Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name "Jiann T'suen Lin" _publ_contact_author_address ; Institute of Chemistry Academia Sinica No 128 Sec 2 Yang Chin Yan Road Taipei 115 TAIWAN ; _publ_contact_author_email JTLIN@CHEM.SINICA.EDU.TW _publ_section_title ; Synthesis, structure and electroluminescent properties of cyclometalated iridium complexes possessing sterically hindered ligands ; loop_ _publ_author_name "Jiann T'suen Lin." 'Chih-Hsin Chen.' 'Pi-Tai Chou.' 'Wan-Ting Hsieh.' ; Chin-Hung Lai ; 'K. R. Justin Thomas' 'Marappan Velusamy' 'Yuh-Sheng Wen.' data_i6679 _database_code_depnum_ccdc_archive 'CCDC 294665' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H55 Cl6 Ir N2 O3' _chemical_formula_sum 'C74 H55 Cl6 Ir N2 O3' _chemical_formula_weight 1425.10 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2327(4) _cell_length_b 13.1476(4) _cell_length_c 20.8703(6) _cell_angle_alpha 83.244(2) _cell_angle_beta 73.8030(10) _cell_angle_gamma 77.3430(10) _cell_volume 3139.30(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100.0(1) _cell_measurement_reflns_used 8464 _cell_measurement_theta_min 0 _cell_measurement_theta_max 0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 2.433 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100.0(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11103 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0150 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.02 _diffrn_reflns_theta_max 25.03 _reflns_number_total 11103 _reflns_number_gt 10598 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+9.3493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11103 _refine_ls_number_parameters 687 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0278 _refine_ls_wR_factor_ref 0.0768 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir Ir 0.869732(10) 0.447082(9) 0.332008(6) 0.01293(5) Uani 1 1 d . . . Cl1 Cl 0.9535 0.8266 0.3094 0.039 Uani 1 1 d . . . Cl2 Cl 0.7121 0.9194 0.3182 0.062 Uani 1 1 d . . . Cl3 Cl 1.0358 0.0106 0.4109 0.060 Uani 1 1 d . . . Cl4 Cl 0.7888 0.0919 0.4543 0.062 Uani 1 1 d . . . Cl5 Cl 0.5028 0.6508 0.0307 0.080 Uani 1 1 d . . . Cl6 Cl 0.3172 0.7489 -0.0315 0.078 Uani 1 1 d . . . O1 O 0.9099(2) 0.35072(19) 0.41494(12) 0.0188(5) Uani 1 1 d . . . O2 O 0.8144(2) 0.57968(18) 0.39190(12) 0.0184(5) Uani 1 1 d . . . O3 O 0.4703 1.0731 0.4467 0.110 Uani 1 1 d D . . N1 N 0.6999(2) 0.4402(2) 0.36409(14) 0.0155(6) Uani 1 1 d . . . N2 N 1.0390(2) 0.4545(2) 0.31139(14) 0.0153(6) Uani 1 1 d . . . C1 C 0.8993(3) 0.3847(3) 0.47161(17) 0.0202(7) Uani 1 1 d . . . C2 C 0.8598(3) 0.4881(3) 0.48970(18) 0.0233(8) Uani 1 1 d . . . H2 H 0.8605 0.5000 0.5326 0.028 Uiso 1 1 calc R . . C3 C 0.8197(3) 0.5757(3) 0.45212(17) 0.0202(7) Uani 1 1 d . . . C4 C 0.9295(4) 0.3013(3) 0.52344(19) 0.0301(9) Uani 1 1 d . . . H4A H 0.9888 0.2460 0.5018 0.045 Uiso 1 1 calc R . . H4B H 0.8617 0.2739 0.5471 0.045 Uiso 1 1 calc R . . H4C H 0.9573 0.3308 0.5544 0.045 Uiso 1 1 calc R . . C5 C 0.7757(4) 0.6793(3) 0.4840(2) 0.0284(9) Uani 1 1 d . . . H5A H 0.8172 0.7303 0.4574 0.043 Uiso 1 1 calc R . . H5B H 0.7874 0.6717 0.5281 0.043 Uiso 1 1 calc R . . H5C H 0.6944 0.7016 0.4869 0.043 Uiso 1 1 calc R . . C6 C 0.8296 0.8201 0.2842 0.041 Uani 1 1 d . . . H6A H 0.8086 0.7526 0.2988 0.049 Uiso 1 1 calc R . . H6B H 0.8470 0.8272 0.2358 0.049 Uiso 1 1 calc R . . C7 C 0.9163 0.0913 0.3892 0.049 Uani 1 1 d . . . H7A H 0.9062 0.0671 0.3495 0.059 Uiso 1 1 calc R . . H7B H 0.9306 0.1619 0.3789 0.059 Uiso 1 1 calc R . . C8 C 0.4284 0.6533 -0.0323 0.083 Uani 1 1 d . . . H8A H 0.4837 0.6566 -0.0757 0.100 Uiso 1 1 calc R . . H8B H 0.4018 0.5878 -0.0279 0.100 Uiso 1 1 calc R . . C11 C 0.8124(3) 0.5403(2) 0.26074(16) 0.0144(6) Uani 1 1 d . . . C12 C 0.8765(3) 0.5749(3) 0.19777(16) 0.0149(7) Uani 1 1 d . . . C13 C 0.8181(3) 0.6443(3) 0.15677(17) 0.0161(7) Uani 1 1 d . . . C14 C 0.6981(3) 0.6896(3) 0.17982(17) 0.0162(7) Uani 1 1 d . . . C15 C 0.6329(3) 0.6567(3) 0.24180(17) 0.0156(7) Uani 1 1 d . . . C16 C 0.6889(3) 0.5771(3) 0.27981(16) 0.0147(7) Uani 1 1 d . . . C17 C 0.8614(3) 0.6876(3) 0.08773(17) 0.0169(7) Uani 1 1 d . . . C18 C 0.9658(3) 0.6731(3) 0.03971(17) 0.0187(7) Uani 1 1 d . . . H18 H 1.0297 0.6254 0.0477 0.022 Uiso 1 1 calc R . . C19 C 0.9739(3) 0.7322(3) -0.02199(18) 0.0218(8) Uani 1 1 d . . . H19 H 1.0442 0.7224 -0.0546 0.026 Uiso 1 1 calc R . . C20 C 0.8815(3) 0.8037(3) -0.03557(18) 0.0236(8) Uani 1 1 d . . . H20 H 0.8903 0.8411 -0.0768 0.028 Uiso 1 1 calc R . . C21 C 0.6715(3) 0.8942(3) 0.00806(19) 0.0266(8) Uani 1 1 d . . . H21 H 0.6705 0.9362 -0.0309 0.032 Uiso 1 1 calc R . . C22 C 0.5751(3) 0.9031(3) 0.0609(2) 0.0275(8) Uani 1 1 d . . . H22 H 0.5097 0.9526 0.0570 0.033 Uiso 1 1 calc R . . C23 C 0.5697(3) 0.8406(3) 0.12136(19) 0.0221(8) Uani 1 1 d . . . H23 H 0.5024 0.8489 0.1562 0.027 Uiso 1 1 calc R . . C24 C 0.6662(3) 0.7674(3) 0.12743(17) 0.0179(7) Uani 1 1 d . . . C25 C 0.7667(3) 0.7601(3) 0.07310(17) 0.0178(7) Uani 1 1 d . . . C26 C 0.7729(3) 0.8206(3) 0.01285(18) 0.0214(7) Uani 1 1 d . . . C31 C 0.6268(3) 0.5172(3) 0.33797(16) 0.0160(7) Uani 1 1 d . . . C33 C 0.6579(3) 0.3749(3) 0.41489(17) 0.0190(7) Uani 1 1 d . . . H33 H 0.7099 0.3226 0.4311 0.023 Uiso 1 1 calc R . . C34 C 0.5412(3) 0.3823(3) 0.44390(18) 0.0228(8) Uani 1 1 d . . . H34 H 0.5143 0.3369 0.4796 0.027 Uiso 1 1 calc R . . C35 C 0.4645(3) 0.4596(3) 0.41850(18) 0.0232(8) Uani 1 1 d . . . H35 H 0.3849 0.4668 0.4370 0.028 Uiso 1 1 calc R . . C36 C 0.5075(3) 0.5256(3) 0.36545(18) 0.0202(7) Uani 1 1 d . . . H36 H 0.4562 0.5764 0.3477 0.024 Uiso 1 1 calc R . . C41 C 1.0046(3) 0.5408(3) 0.17104(16) 0.0157(7) Uani 1 1 d . . . C42 C 1.0514(3) 0.4508(3) 0.13596(18) 0.0203(7) Uani 1 1 d . . . H42 H 1.0031 0.4066 0.1333 0.024 Uiso 1 1 calc R . . C43 C 1.1693(3) 0.4261(3) 0.1049(2) 0.0268(8) Uani 1 1 d . . . H43 H 1.1994 0.3663 0.0810 0.032 Uiso 1 1 calc R . . C44 C 1.2423(3) 0.4905(3) 0.1095(2) 0.0313(9) Uani 1 1 d . . . H44 H 1.3212 0.4739 0.0888 0.038 Uiso 1 1 calc R . . C45 C 1.1973(3) 0.5794(3) 0.1449(2) 0.0282(8) Uani 1 1 d . . . H45 H 1.2463 0.6222 0.1486 0.034 Uiso 1 1 calc R . . C46 C 1.0793(3) 0.6047(3) 0.17483(18) 0.0211(7) Uani 1 1 d . . . H46 H 1.0495 0.6654 0.1978 0.025 Uiso 1 1 calc R . . C51 C 0.5087(3) 0.7083(3) 0.26617(17) 0.0177(7) Uani 1 1 d . . . C52 C 0.4248(3) 0.6931(3) 0.23656(19) 0.0232(8) Uani 1 1 d . . . H52 H 0.4462 0.6512 0.2005 0.028 Uiso 1 1 calc R . . C53 C 0.3093(3) 0.7406(3) 0.2609(2) 0.0287(9) Uani 1 1 d . . . H53 H 0.2538 0.7305 0.2408 0.034 Uiso 1 1 calc R . . C54 C 0.2766(3) 0.8024(3) 0.3143(2) 0.0313(9) Uani 1 1 d . . . H54 H 0.1992 0.8338 0.3304 0.038 Uiso 1 1 calc R . . C55 C 0.3587(4) 0.8177(3) 0.3441(2) 0.0330(9) Uani 1 1 d . . . H55 H 0.3364 0.8592 0.3805 0.040 Uiso 1 1 calc R . . C56 C 0.4745(3) 0.7714(3) 0.3199(2) 0.0246(8) Uani 1 1 d . . . H56 H 0.5295 0.7827 0.3398 0.030 Uiso 1 1 calc R . . C61 C 0.9395(3) 0.3219(3) 0.27813(16) 0.0146(7) Uani 1 1 d . . . C62 C 0.8843(3) 0.2642(3) 0.24815(16) 0.0156(7) Uani 1 1 d . . . C63 C 0.9467(3) 0.1715(3) 0.21897(16) 0.0159(7) Uani 1 1 d . . . C64 C 1.0644(3) 0.1336(3) 0.21974(16) 0.0159(7) Uani 1 1 d . . . C65 C 1.1240(3) 0.1922(3) 0.24392(17) 0.0170(7) Uani 1 1 d . . . C66 C 1.0613(3) 0.2872(3) 0.27242(16) 0.0154(7) Uani 1 1 d . . . C67 C 0.9132(3) 0.0996(3) 0.18163(17) 0.0180(7) Uani 1 1 d . . . C68 C 0.8176(3) 0.0980(3) 0.15930(19) 0.0228(8) Uani 1 1 d . . . H68 H 0.7510 0.1495 0.1704 0.027 Uiso 1 1 calc R . . C69 C 0.8227(3) 0.0166(3) 0.1192(2) 0.0286(9) Uani 1 1 d . . . H69 H 0.7581 0.0155 0.1043 0.034 Uiso 1 1 calc R . . C70 C 0.9186(3) -0.0605(3) 0.1014(2) 0.0276(8) Uani 1 1 d . . . H70 H 0.9186 -0.1123 0.0747 0.033 Uiso 1 1 calc R . . C71 C 1.1256(3) -0.1330(3) 0.10711(19) 0.0253(8) Uani 1 1 d . . . H71 H 1.1340 -0.1888 0.0814 0.030 Uiso 1 1 calc R . . C72 C 1.2171(3) -0.1195(3) 0.12909(19) 0.0245(8) Uani 1 1 d . . . H72 H 1.2869 -0.1671 0.1178 0.029 Uiso 1 1 calc R . . C73 C 1.2092(3) -0.0358(3) 0.16829(18) 0.0208(7) Uani 1 1 d . . . H73 H 1.2728 -0.0286 0.1823 0.025 Uiso 1 1 calc R . . C74 C 1.1061(3) 0.0346(3) 0.18525(17) 0.0170(7) Uani 1 1 d . . . C75 C 1.0118(3) 0.0191(3) 0.16311(17) 0.0181(7) Uani 1 1 d . . . C76 C 1.0184(3) -0.0615(3) 0.12371(18) 0.0220(8) Uani 1 1 d . . . C81 C 1.1151(3) 0.3634(3) 0.29321(16) 0.0169(7) Uani 1 1 d . . . C83 C 1.0748(3) 0.5348(3) 0.32773(16) 0.0174(7) Uani 1 1 d . . . H83 H 1.0215 0.5966 0.3384 0.021 Uiso 1 1 calc R . . C84 C 1.1874(3) 0.5291(3) 0.32928(17) 0.0201(7) Uani 1 1 d . . . H84 H 1.2106 0.5860 0.3405 0.024 Uiso 1 1 calc R . . C85 C 1.2652(3) 0.4369(3) 0.31386(19) 0.0252(8) Uani 1 1 d . . . H85 H 1.3414 0.4300 0.3160 0.030 Uiso 1 1 calc R . . C86 C 1.2300(3) 0.3547(3) 0.29516(19) 0.0240(8) Uani 1 1 d . . . H86 H 1.2832 0.2931 0.2838 0.029 Uiso 1 1 calc R . . C91 C 0.7627(3) 0.3007(3) 0.24179(18) 0.0187(7) Uani 1 1 d . . . C92 C 0.7411(3) 0.3731(3) 0.19042(18) 0.0211(7) Uani 1 1 d . . . H92 H 0.8010 0.4038 0.1633 0.025 Uiso 1 1 calc R . . C93 C 0.6319(3) 0.4001(3) 0.1790(2) 0.0277(8) Uani 1 1 d . . . H93 H 0.6188 0.4490 0.1446 0.033 Uiso 1 1 calc R . . C94 C 0.5423(3) 0.3547(3) 0.2187(2) 0.0322(9) Uani 1 1 d . . . H94 H 0.4693 0.3719 0.2105 0.039 Uiso 1 1 calc R . . C95 C 0.5617(3) 0.2838(3) 0.2704(2) 0.0307(9) Uani 1 1 d . . . H95 H 0.5013 0.2538 0.2975 0.037 Uiso 1 1 calc R . . C96 C 0.6714(3) 0.2566(3) 0.28220(19) 0.0248(8) Uani 1 1 d . . . H96 H 0.6837 0.2088 0.3173 0.030 Uiso 1 1 calc R . . C101 C 1.2516(3) 0.1528(3) 0.2339(2) 0.0217(8) Uani 1 1 d . . . C102 C 1.3269(3) 0.1715(3) 0.1719(2) 0.0290(9) Uani 1 1 d . . . H102 H 1.2978 0.2110 0.1382 0.035 Uiso 1 1 calc R . . C103 C 1.4453(4) 0.1314(4) 0.1602(3) 0.0425(12) Uani 1 1 d . . . H103 H 1.4951 0.1441 0.1187 0.051 Uiso 1 1 calc R . . C104 C 1.4890(4) 0.0730(3) 0.2098(3) 0.0476(14) Uani 1 1 d . . . H104 H 1.5683 0.0463 0.2020 0.057 Uiso 1 1 calc R . . C105 C 1.4157(4) 0.0540(3) 0.2709(3) 0.0467(13) Uani 1 1 d . . . H105 H 1.4455 0.0147 0.3044 0.056 Uiso 1 1 calc R . . C106 C 1.2967(4) 0.0933(3) 0.2832(2) 0.0324(9) Uani 1 1 d . . . H106 H 1.2475 0.0794 0.3247 0.039 Uiso 1 1 calc R . . H3A H 0.4682 1.0682 0.4911 0.165 Uiso 1 1 d D . . H3B H 0.4190 1.0750 0.4326 0.165 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir 0.01149(7) 0.01408(7) 0.01304(7) -0.00001(5) -0.00362(5) -0.00200(5) Cl1 0.035 0.033 0.050 0.000 -0.015 -0.007 Cl2 0.032 0.045 0.107 -0.015 -0.012 -0.002 Cl3 0.056 0.062 0.046 0.008 -0.004 0.005 Cl4 0.053 0.052 0.072 0.009 -0.009 -0.005 Cl5 0.073 0.093 0.079 -0.041 -0.013 -0.017 Cl6 0.078 0.085 0.055 -0.013 0.002 -0.004 O1 0.0167(12) 0.0220(12) 0.0169(12) 0.0020(10) -0.0052(10) -0.0027(10) O2 0.0178(12) 0.0197(12) 0.0176(12) -0.0027(10) -0.0044(10) -0.0030(10) O3 0.047 0.122 0.116 -0.037 0.021 0.037 N1 0.0156(14) 0.0157(14) 0.0153(14) -0.0015(11) -0.0058(11) -0.0011(11) N2 0.0164(14) 0.0166(14) 0.0131(13) -0.0001(11) -0.0048(11) -0.0029(11) C1 0.0123(17) 0.032(2) 0.0154(17) 0.0026(15) -0.0034(13) -0.0062(15) C2 0.0208(18) 0.034(2) 0.0159(17) -0.0033(15) -0.0045(14) -0.0067(16) C3 0.0131(17) 0.0283(19) 0.0191(18) -0.0048(14) 0.0006(14) -0.0083(14) C4 0.029(2) 0.038(2) 0.0215(19) 0.0040(17) -0.0099(16) -0.0023(18) C5 0.030(2) 0.030(2) 0.025(2) -0.0081(16) -0.0012(16) -0.0092(17) C6 0.034 0.044 0.046 -0.014 -0.011 -0.005 C7 0.066 0.037 0.037 0.007 -0.011 -0.003 C8 0.102 0.111 0.051 0.002 -0.025 -0.049 C11 0.0151(16) 0.0131(15) 0.0154(16) -0.0022(12) -0.0051(13) -0.0018(13) C12 0.0157(17) 0.0144(16) 0.0160(16) -0.0028(13) -0.0049(13) -0.0037(13) C13 0.0167(17) 0.0161(16) 0.0161(16) -0.0023(13) -0.0035(13) -0.0046(13) C14 0.0183(17) 0.0155(16) 0.0167(16) -0.0016(13) -0.0070(14) -0.0039(13) C15 0.0147(17) 0.0161(16) 0.0167(16) -0.0028(13) -0.0043(13) -0.0033(13) C16 0.0143(16) 0.0158(16) 0.0147(16) -0.0027(13) -0.0045(13) -0.0027(13) C17 0.0211(18) 0.0156(16) 0.0166(17) -0.0015(13) -0.0066(14) -0.0064(14) C18 0.0210(18) 0.0181(17) 0.0178(17) -0.0025(14) -0.0056(14) -0.0040(14) C19 0.026(2) 0.0240(19) 0.0156(17) -0.0024(14) -0.0024(15) -0.0090(15) C20 0.032(2) 0.0259(19) 0.0163(17) 0.0056(14) -0.0091(15) -0.0129(16) C21 0.031(2) 0.027(2) 0.0248(19) 0.0096(16) -0.0150(17) -0.0085(17) C22 0.025(2) 0.027(2) 0.032(2) 0.0071(16) -0.0149(17) -0.0033(16) C23 0.0193(18) 0.0217(18) 0.0248(19) 0.0017(15) -0.0074(15) -0.0024(15) C24 0.0202(18) 0.0186(17) 0.0179(17) 0.0013(14) -0.0086(14) -0.0067(14) C25 0.0221(18) 0.0166(16) 0.0175(17) -0.0003(13) -0.0077(14) -0.0069(14) C26 0.027(2) 0.0221(18) 0.0195(18) 0.0024(14) -0.0108(15) -0.0108(15) C31 0.0171(17) 0.0172(16) 0.0144(16) -0.0021(13) -0.0048(13) -0.0033(13) C33 0.0179(18) 0.0186(17) 0.0193(17) 0.0035(14) -0.0059(14) -0.0021(14) C34 0.0214(19) 0.0255(19) 0.0200(18) 0.0060(14) -0.0027(15) -0.0087(15) C35 0.0146(17) 0.028(2) 0.0245(19) 0.0001(15) -0.0012(14) -0.0052(15) C36 0.0163(17) 0.0203(18) 0.0225(18) 0.0012(14) -0.0052(14) -0.0018(14) C41 0.0150(17) 0.0175(16) 0.0131(16) 0.0017(13) -0.0045(13) -0.0006(13) C42 0.0193(18) 0.0197(17) 0.0212(18) -0.0003(14) -0.0041(14) -0.0043(14) C43 0.0209(19) 0.0250(19) 0.029(2) -0.0083(16) -0.0009(16) 0.0027(15) C44 0.0136(18) 0.040(2) 0.035(2) -0.0097(18) 0.0009(16) 0.0002(17) C45 0.0189(19) 0.036(2) 0.031(2) -0.0062(17) -0.0042(16) -0.0096(17) C46 0.0202(18) 0.0244(19) 0.0182(17) -0.0046(14) -0.0026(14) -0.0050(15) C51 0.0167(17) 0.0151(16) 0.0193(17) 0.0044(13) -0.0045(14) -0.0023(13) C52 0.0190(18) 0.0269(19) 0.0229(18) 0.0053(15) -0.0065(15) -0.0050(15) C53 0.0190(19) 0.032(2) 0.033(2) 0.0161(17) -0.0110(16) -0.0065(16) C54 0.0143(18) 0.023(2) 0.047(3) 0.0067(18) -0.0001(17) 0.0012(15) C55 0.028(2) 0.022(2) 0.041(2) -0.0087(17) 0.0049(18) -0.0018(17) C56 0.0179(18) 0.0239(19) 0.032(2) -0.0047(16) -0.0035(16) -0.0053(15) C61 0.0154(16) 0.0156(16) 0.0118(15) 0.0018(12) -0.0021(13) -0.0040(13) C62 0.0141(16) 0.0177(17) 0.0148(16) 0.0006(13) -0.0029(13) -0.0045(13) C63 0.0158(17) 0.0178(17) 0.0146(16) 0.0025(13) -0.0039(13) -0.0061(13) C64 0.0153(17) 0.0160(16) 0.0141(16) 0.0010(13) -0.0023(13) -0.0016(13) C65 0.0159(17) 0.0182(17) 0.0168(16) 0.0015(13) -0.0057(13) -0.0029(14) C66 0.0146(17) 0.0173(16) 0.0142(16) 0.0013(13) -0.0048(13) -0.0026(13) C67 0.0199(18) 0.0163(16) 0.0177(17) 0.0002(13) -0.0030(14) -0.0068(14) C68 0.0177(18) 0.0226(18) 0.029(2) -0.0056(15) -0.0060(15) -0.0042(15) C69 0.026(2) 0.032(2) 0.034(2) -0.0075(17) -0.0117(17) -0.0100(17) C70 0.031(2) 0.0243(19) 0.032(2) -0.0074(16) -0.0100(17) -0.0111(17) C71 0.032(2) 0.0156(17) 0.028(2) -0.0046(15) -0.0063(16) -0.0046(15) C72 0.028(2) 0.0157(17) 0.0272(19) -0.0011(15) -0.0068(16) 0.0009(15) C73 0.0218(18) 0.0177(17) 0.0234(18) 0.0015(14) -0.0080(15) -0.0035(14) C74 0.0213(18) 0.0142(16) 0.0153(16) 0.0025(13) -0.0048(14) -0.0049(14) C75 0.0201(18) 0.0175(17) 0.0169(17) 0.0016(13) -0.0038(14) -0.0071(14) C76 0.025(2) 0.0174(17) 0.0238(18) 0.0003(14) -0.0054(15) -0.0075(15) C81 0.0162(17) 0.0200(17) 0.0147(16) -0.0009(13) -0.0046(13) -0.0032(14) C83 0.0197(18) 0.0182(17) 0.0145(16) 0.0004(13) -0.0044(13) -0.0050(14) C84 0.0206(18) 0.0251(18) 0.0168(17) -0.0038(14) -0.0031(14) -0.0098(15) C85 0.0153(18) 0.034(2) 0.029(2) -0.0093(16) -0.0059(15) -0.0050(16) C86 0.0151(18) 0.0269(19) 0.031(2) -0.0100(16) -0.0071(15) 0.0001(15) C91 0.0154(17) 0.0190(17) 0.0230(18) -0.0094(14) -0.0044(14) -0.0026(14) C92 0.0192(18) 0.0215(18) 0.0243(19) -0.0065(15) -0.0076(15) -0.0022(14) C93 0.024(2) 0.033(2) 0.029(2) -0.0088(17) -0.0142(17) 0.0029(16) C94 0.0156(19) 0.046(2) 0.038(2) -0.019(2) -0.0107(17) 0.0031(17) C95 0.0162(19) 0.040(2) 0.036(2) -0.0146(19) 0.0001(16) -0.0095(17) C96 0.0211(19) 0.028(2) 0.0261(19) -0.0070(16) -0.0034(15) -0.0071(16) C101 0.0178(18) 0.0138(16) 0.035(2) -0.0087(15) -0.0094(16) 0.0003(14) C102 0.0201(19) 0.027(2) 0.038(2) -0.0116(17) -0.0012(17) -0.0034(16) C103 0.022(2) 0.033(2) 0.066(3) -0.020(2) 0.006(2) -0.0062(18) C104 0.017(2) 0.026(2) 0.100(4) -0.015(3) -0.013(2) -0.0010(18) C105 0.032(3) 0.024(2) 0.093(4) 0.006(2) -0.038(3) -0.0031(19) C106 0.024(2) 0.025(2) 0.051(3) 0.0044(18) -0.0171(19) -0.0057(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir C11 1.996(3) . ? Ir C61 1.996(3) . ? Ir N1 2.016(3) . ? Ir N2 2.016(3) . ? Ir O1 2.128(2) . ? Ir O2 2.141(2) . ? Cl1 C6 1.7573 . ? Cl2 C6 1.7604 . ? Cl3 C7 1.7447 . ? Cl4 C7 1.7585 . ? Cl5 C8 1.7901 . ? Cl6 C8 1.6344 . ? O1 C1 1.276(4) . ? O2 C3 1.271(4) . ? O3 H3A 0.9140 . ? O3 H3B 0.7589 . ? N1 C33 1.341(4) . ? N1 C31 1.366(4) . ? N2 C83 1.339(4) . ? N2 C81 1.366(4) . ? C1 C2 1.399(5) . ? C1 C4 1.509(5) . ? C2 C3 1.391(5) . ? C2 H2 0.9300 . ? C3 C5 1.510(5) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C11 C12 1.411(5) . ? C11 C16 1.437(5) . ? C12 C13 1.395(5) . ? C12 C41 1.494(5) . ? C13 C14 1.425(5) . ? C13 C17 1.481(5) . ? C14 C15 1.393(5) . ? C14 C24 1.481(5) . ? C15 C16 1.410(5) . ? C15 C51 1.492(5) . ? C16 C31 1.480(5) . ? C17 C18 1.377(5) . ? C17 C25 1.411(5) . ? C18 C19 1.414(5) . ? C18 H18 0.9300 . ? C19 C20 1.375(5) . ? C19 H19 0.9300 . ? C20 C26 1.417(5) . ? C20 H20 0.9300 . ? C21 C22 1.365(6) . ? C21 C26 1.416(5) . ? C21 H21 0.9300 . ? C22 C23 1.416(5) . ? C22 H22 0.9300 . ? C23 C24 1.376(5) . ? C23 H23 0.9300 . ? C24 C25 1.415(5) . ? C25 C26 1.399(5) . ? C31 C36 1.396(5) . ? C33 C34 1.373(5) . ? C33 H33 0.9300 . ? C34 C35 1.388(5) . ? C34 H34 0.9300 . ? C35 C36 1.380(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C41 C42 1.392(5) . ? C41 C46 1.393(5) . ? C42 C43 1.389(5) . ? C42 H42 0.9300 . ? C43 C44 1.385(6) . ? C43 H43 0.9300 . ? C44 C45 1.381(6) . ? C44 H44 0.9300 . ? C45 C46 1.386(5) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C51 C56 1.387(5) . ? C51 C52 1.396(5) . ? C52 C53 1.389(5) . ? C52 H52 0.9300 . ? C53 C54 1.373(6) . ? C53 H53 0.9300 . ? C54 C55 1.378(6) . ? C54 H54 0.9300 . ? C55 C56 1.388(5) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C61 C62 1.414(5) . ? C61 C66 1.434(5) . ? C62 C63 1.395(5) . ? C62 C91 1.497(5) . ? C63 C64 1.420(5) . ? C63 C67 1.480(5) . ? C64 C65 1.387(5) . ? C64 C74 1.482(5) . ? C65 C66 1.415(5) . ? C65 C101 1.496(5) . ? C66 C81 1.475(5) . ? C67 C68 1.380(5) . ? C67 C75 1.415(5) . ? C68 C69 1.415(5) . ? C68 H68 0.9300 . ? C69 C70 1.366(6) . ? C69 H69 0.9300 . ? C70 C76 1.420(5) . ? C70 H70 0.9300 . ? C71 C72 1.373(6) . ? C71 C76 1.416(5) . ? C71 H71 0.9300 . ? C72 C73 1.418(5) . ? C72 H72 0.9300 . ? C73 C74 1.374(5) . ? C73 H73 0.9300 . ? C74 C75 1.417(5) . ? C75 C76 1.392(5) . ? C81 C86 1.396(5) . ? C83 C84 1.372(5) . ? C83 H83 0.9300 . ? C84 C85 1.376(5) . ? C84 H84 0.9300 . ? C85 C86 1.379(5) . ? C85 H85 0.9300 . ? C86 H86 0.9300 . ? C91 C92 1.390(5) . ? C91 C96 1.392(5) . ? C92 C93 1.385(5) . ? C92 H92 0.9300 . ? C93 C94 1.381(6) . ? C93 H93 0.9300 . ? C94 C95 1.379(6) . ? C94 H94 0.9300 . ? C95 C96 1.394(6) . ? C95 H95 0.9300 . ? C96 H96 0.9300 . ? C101 C106 1.383(6) . ? C101 C102 1.394(6) . ? C102 C103 1.390(6) . ? C102 H102 0.9300 . ? C103 C104 1.375(8) . ? C103 H103 0.9300 . ? C104 C105 1.369(8) . ? C104 H104 0.9300 . ? C105 C106 1.395(6) . ? C105 H105 0.9300 . ? C106 H106 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Ir C61 96.76(13) . . ? C11 Ir N1 80.71(12) . . ? C61 Ir N1 103.69(12) . . ? C11 Ir N2 104.49(12) . . ? C61 Ir N2 80.24(12) . . ? N1 Ir N2 173.22(11) . . ? C11 Ir O1 173.17(11) . . ? C61 Ir O1 86.83(11) . . ? N1 Ir O1 92.82(10) . . ? N2 Ir O1 81.81(10) . . ? C11 Ir O2 87.13(11) . . ? C61 Ir O2 173.29(11) . . ? N1 Ir O2 82.28(10) . . ? N2 Ir O2 93.52(10) . . ? O1 Ir O2 89.87(9) . . ? C1 O1 Ir 123.9(2) . . ? C3 O2 Ir 123.5(2) . . ? H3A O3 H3B 125.735(3) . . ? C33 N1 C31 120.8(3) . . ? C33 N1 Ir 122.8(2) . . ? C31 N1 Ir 115.6(2) . . ? C83 N2 C81 120.9(3) . . ? C83 N2 Ir 122.4(2) . . ? C81 N2 Ir 115.3(2) . . ? O1 C1 C2 126.7(3) . . ? O1 C1 C4 114.4(3) . . ? C2 C1 C4 118.9(3) . . ? C3 C2 C1 128.7(3) . . ? C3 C2 H2 115.6 . . ? C1 C2 H2 115.6 . . ? O2 C3 C2 127.1(3) . . ? O2 C3 C5 113.9(3) . . ? C2 C3 C5 119.0(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Cl1 C6 Cl2 111.062(2) . . ? Cl1 C6 H6A 109.4 . . ? Cl2 C6 H6A 109.4 . . ? Cl1 C6 H6B 109.4 . . ? Cl2 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? Cl3 C7 Cl4 111.429(2) . . ? Cl3 C7 H7A 109.3 . . ? Cl4 C7 H7A 109.3 . . ? Cl3 C7 H7B 109.3 . . ? Cl4 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? Cl6 C8 Cl5 116.255(2) . . ? Cl6 C8 H8A 108.2 . . ? Cl5 C8 H8A 108.2 . . ? Cl6 C8 H8B 108.2 . . ? Cl5 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? C12 C11 C16 118.5(3) . . ? C12 C11 Ir 128.9(2) . . ? C16 C11 Ir 112.6(2) . . ? C13 C12 C11 119.0(3) . . ? C13 C12 C41 117.0(3) . . ? C11 C12 C41 124.0(3) . . ? C12 C13 C14 121.5(3) . . ? C12 C13 C17 130.4(3) . . ? C14 C13 C17 108.1(3) . . ? C15 C14 C13 120.3(3) . . ? C15 C14 C24 131.7(3) . . ? C13 C14 C24 108.0(3) . . ? C14 C15 C16 118.0(3) . . ? C14 C15 C51 119.3(3) . . ? C16 C15 C51 122.7(3) . . ? C15 C16 C11 121.8(3) . . ? C15 C16 C31 123.9(3) . . ? C11 C16 C31 114.0(3) . . ? C18 C17 C25 118.6(3) . . ? C18 C17 C13 135.5(3) . . ? C25 C17 C13 105.9(3) . . ? C17 C18 C19 118.6(3) . . ? C17 C18 H18 120.7 . . ? C19 C18 H18 120.7 . . ? C20 C19 C18 122.4(3) . . ? C20 C19 H19 118.8 . . ? C18 C19 H19 118.8 . . ? C19 C20 C26 120.4(3) . . ? C19 C20 H20 119.8 . . ? C26 C20 H20 119.8 . . ? C22 C21 C26 119.8(3) . . ? C22 C21 H21 120.1 . . ? C26 C21 H21 120.1 . . ? C21 C22 C23 123.2(4) . . ? C21 C22 H22 118.4 . . ? C23 C22 H22 118.4 . . ? C24 C23 C22 118.6(3) . . ? C24 C23 H23 120.7 . . ? C22 C23 H23 120.7 . . ? C23 C24 C25 117.9(3) . . ? C23 C24 C14 136.2(3) . . ? C25 C24 C14 105.8(3) . . ? C26 C25 C17 123.8(3) . . ? C26 C25 C24 124.1(3) . . ? C17 C25 C24 112.1(3) . . ? C25 C26 C21 116.4(3) . . ? C25 C26 C20 116.1(3) . . ? C21 C26 C20 127.4(3) . . ? N1 C31 C36 118.1(3) . . ? N1 C31 C16 112.9(3) . . ? C36 C31 C16 128.9(3) . . ? N1 C33 C34 122.6(3) . . ? N1 C33 H33 118.7 . . ? C34 C33 H33 118.7 . . ? C33 C34 C35 118.1(3) . . ? C33 C34 H34 120.9 . . ? C35 C34 H34 120.9 . . ? C36 C35 C34 119.3(3) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C31 121.0(3) . . ? C35 C36 H36 119.5 . . ? C31 C36 H36 119.5 . . ? C42 C41 C46 118.3(3) . . ? C42 C41 C12 121.3(3) . . ? C46 C41 C12 120.0(3) . . ? C43 C42 C41 120.7(3) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 120.1(4) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 119.8(4) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 120.0(4) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 121.0(3) . . ? C45 C46 H46 119.5 . . ? C41 C46 H46 119.5 . . ? C56 C51 C52 118.8(3) . . ? C56 C51 C15 120.0(3) . . ? C52 C51 C15 121.2(3) . . ? C53 C52 C51 120.1(4) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C54 C53 C52 120.4(4) . . ? C54 C53 H53 119.8 . . ? C52 C53 H53 119.8 . . ? C53 C54 C55 120.0(4) . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C54 C55 C56 120.1(4) . . ? C54 C55 H55 119.9 . . ? C56 C55 H55 119.9 . . ? C51 C56 C55 120.5(4) . . ? C51 C56 H56 119.7 . . ? C55 C56 H56 119.7 . . ? C62 C61 C66 118.2(3) . . ? C62 C61 Ir 128.6(3) . . ? C66 C61 Ir 113.1(2) . . ? C63 C62 C61 119.4(3) . . ? C63 C62 C91 117.2(3) . . ? C61 C62 C91 123.3(3) . . ? C62 C63 C64 121.1(3) . . ? C62 C63 C67 130.7(3) . . ? C64 C63 C67 108.1(3) . . ? C65 C64 C63 121.0(3) . . ? C65 C64 C74 130.5(3) . . ? C63 C64 C74 108.2(3) . . ? C64 C65 C66 117.8(3) . . ? C64 C65 C101 117.0(3) . . ? C66 C65 C101 125.1(3) . . ? C65 C66 C61 122.0(3) . . ? C65 C66 C81 124.0(3) . . ? C61 C66 C81 113.8(3) . . ? C68 C67 C75 117.9(3) . . ? C68 C67 C63 136.0(3) . . ? C75 C67 C63 105.9(3) . . ? C67 C68 C69 118.8(3) . . ? C67 C68 H68 120.6 . . ? C69 C68 H68 120.6 . . ? C70 C69 C68 122.8(4) . . ? C70 C69 H69 118.6 . . ? C68 C69 H69 118.6 . . ? C69 C70 C76 120.0(3) . . ? C69 C70 H70 120.0 . . ? C76 C70 H70 120.0 . . ? C72 C71 C76 119.7(3) . . ? C72 C71 H71 120.1 . . ? C76 C71 H71 120.1 . . ? C71 C72 C73 122.5(4) . . ? C71 C72 H72 118.7 . . ? C73 C72 H72 118.7 . . ? C74 C73 C72 118.9(3) . . ? C74 C73 H73 120.5 . . ? C72 C73 H73 120.5 . . ? C73 C74 C75 118.0(3) . . ? C73 C74 C64 136.1(3) . . ? C75 C74 C64 105.8(3) . . ? C76 C75 C67 124.1(3) . . ? C76 C75 C74 123.9(3) . . ? C67 C75 C74 111.9(3) . . ? C75 C76 C71 116.9(3) . . ? C75 C76 C70 116.4(3) . . ? C71 C76 C70 126.6(3) . . ? N2 C81 C86 118.1(3) . . ? N2 C81 C66 112.9(3) . . ? C86 C81 C66 129.0(3) . . ? N2 C83 C84 122.3(3) . . ? N2 C83 H83 118.8 . . ? C84 C83 H83 118.8 . . ? C83 C84 C85 118.2(3) . . ? C83 C84 H84 120.9 . . ? C85 C84 H84 120.9 . . ? C84 C85 C86 119.9(3) . . ? C84 C85 H85 120.0 . . ? C86 C85 H85 120.0 . . ? C85 C86 C81 120.5(3) . . ? C85 C86 H86 119.7 . . ? C81 C86 H86 119.7 . . ? C92 C91 C96 118.4(3) . . ? C92 C91 C62 119.8(3) . . ? C96 C91 C62 121.5(3) . . ? C93 C92 C91 121.0(4) . . ? C93 C92 H92 119.5 . . ? C91 C92 H92 119.5 . . ? C94 C93 C92 120.2(4) . . ? C94 C93 H93 119.9 . . ? C92 C93 H93 119.9 . . ? C95 C94 C93 119.6(4) . . ? C95 C94 H94 120.2 . . ? C93 C94 H94 120.2 . . ? C94 C95 C96 120.4(4) . . ? C94 C95 H95 119.8 . . ? C96 C95 H95 119.8 . . ? C91 C96 C95 120.3(4) . . ? C91 C96 H96 119.8 . . ? C95 C96 H96 119.8 . . ? C106 C101 C102 118.8(4) . . ? C106 C101 C65 121.9(4) . . ? C102 C101 C65 119.2(3) . . ? C103 C102 C101 120.4(4) . . ? C103 C102 H102 119.8 . . ? C101 C102 H102 119.8 . . ? C104 C103 C102 120.2(5) . . ? C104 C103 H103 119.9 . . ? C102 C103 H103 119.9 . . ? C105 C104 C103 119.9(4) . . ? C105 C104 H104 120.1 . . ? C103 C104 H104 120.1 . . ? C104 C105 C106 120.6(5) . . ? C104 C105 H105 119.7 . . ? C106 C105 H105 119.7 . . ? C101 C106 C105 120.1(4) . . ? C101 C106 H106 119.9 . . ? C105 C106 H106 119.9 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.951 _refine_diff_density_min -1.786 _refine_diff_density_rms 0.104