data_shelxl_4 _publ_contact_author_name 'Werner Kaminsky' _publ_contact_author_address ; Department of Chemistry, BOX 351700 University of Washington Seattle, WA 98195 USA ; _publ_contact_author_email 'wernerka@u.washington.edu' _publ_requested_journal 'Journal title here' _publ_section_title ; Dinuclear Iridium Complexes Containing Cp* and Carbonyl Ligands: Synthesis, Structure, and Reactivity ; loop_ _publ_author_name _publ_author_address 'Joseph M. Meredith' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'Karen I. Goldberg' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'Werner Kaminsky' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'D. Michael Heinekey' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; _publ_section_abstract ; The synthesis of the monomeric cationic complexes [Cp*(CO)Ir(R)(CH2Cl2)] was attempted (Cp* = ?5-C5Me5, R = Me, H). The target complexes were not obtained; instead, dimeric products were isolated in high yields. The reaction between Cp*(CO)Ir(Me)(Cl) and [Li(Et2O)2.5][BArF4] afforded the cationic complex [{Cp*(CO)Ir(Me)}2(?-Cl)] (4) in high yield. Complex 4 has been characterized by 1H NMR, 13C NMR, and IR spectroscopies. Reaction of Cp*(CO)Ir(H)2 with [CPh3][BArF4] affords the dicationic complex [Cp*(CO)Ir(?-H)]2 (9) in excellent yield. Complex 9 has been characterized by 1H NMR and IR spectroscopies as well as elemental analysis and single crystal X-Ray diffraction. An X-Ray structural determination was also carried out on the related complex [Cp*(Cl)Ir(? -H)]2 (14). The solid-state structures of 9 and 14 are compared briefly. ; _publ_section_comment ; Details and comments here ; _publ_section_exptl_prep ; details of preparation here ; _publ_section_exptl_refinement ; All H atoms were initially located in a difference Fourier map and were refined with a riding model. H atoms were placed in geometrically idealised positions and constrained to ride on their parent atoms with C---H distances in the range 0.95-1.00 \%A. U~iso~ values were fixed such that they were 1.2U~eq~ of their parent atom U~eq~ for CH's and 1.5U~eq~ of their parent atom U~eq~ in case of methyl groups. ; _publ_section_references ; Altomare, A.; Cascarano, G.; Giacovazzo, C.; Burla, M.C.; Polidori, G.; Camalli, M. (1994) J. Appl. Cryst. 27, 435-442. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W. P., Garcia-Granada, S., Gould, R. O., Smits, J. M. M. & Smykalla, C. (1996) The DIRDIF96 Program System. Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. MacKay, S.; Gilmore, C.J.; Edwards, C.; Tremayne, M.; Stewart, N.; Shankland, K. (1998) "maXus: a computer program for the solution and refinement of crystal structures from diffraction data" University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan. Otwinowski, Z.; Minor, W. (1996) Methods in Enzymology, 276, 307-326. Sheldrick, G. M. (1997) SHELXL97 University of G\"ottingen, Germany. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'JMM01175' ; _chemical_name_common 'JMM01175' _chemical_melting_point ? _chemical_formula_moiety '2(C24 H36 Cl Ir2 O2), 2(C24 B F20), 0.86(C H2 Cl2)' _chemical_formula_sum 'C96.86 H73.72 B2 Cl3.72 F40 Ir4 O4' _chemical_formula_weight 2983.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 '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' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3828(6) _cell_length_b 14.1680(5) _cell_length_c 16.8874(8) _cell_angle_alpha 104.1420(16) _cell_angle_beta 99.0600(15) _cell_angle_gamma 115.7881(19) _cell_volume 2465.95(19) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 519 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description prism _exptl_crystal_colour 'pale-yellow' _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.009 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428.1 _exptl_absorpt_coefficient_mu 5.608 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.18 _exptl_absorpt_correction_T_max 0.39 _exptl_absorpt_process_details 'HKL2008' _exptl_special_details ; Data was collected with \w and \f scans in 1.9^o^ increments with 30 second exposures per degree. Crystal-to-detector distance was 30 mm. 72924 full and partial reflection were integrated. ; _diffrn_ambient_temperature 130(2) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 19274 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.1150 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 28.24 _reflns_number_total 11687 _reflns_number_gt 7221 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0585P)^2^+1.3059P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11687 _refine_ls_number_parameters 784 _refine_ls_number_restraints 140 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0524 _refine_ls_wR_factor_ref 0.1307 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.001 _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 Ir1 Ir 1.02903(3) 0.14054(2) 0.472386(19) 0.02869(10) Uani 1 1 d . . . Ir2 Ir 0.15641(3) 0.64765(3) 0.08793(3) 0.05527(14) Uani 1 1 d . . . F1 F 0.3103(4) 0.2402(4) 0.2351(3) 0.0377(10) Uani 1 1 d . . . F2 F 0.1202(4) 0.1374(4) 0.0914(3) 0.0481(12) Uani 1 1 d . A . F3 F 0.1608(4) 0.0849(4) -0.0632(3) 0.0469(12) Uani 1 1 d . . . F4 F 0.3968(4) 0.1343(4) -0.0682(3) 0.0491(12) Uani 1 1 d . A . F5 F 0.5829(4) 0.2233(4) 0.0727(3) 0.0447(12) Uani 1 1 d . . . F6 F 0.4858(5) 0.4139(4) 0.3949(3) 0.0487(13) Uani 1 1 d . . . F7 F 0.4690(6) 0.5951(5) 0.4076(4) 0.0792(19) Uani 1 1 d . A . F8 F 0.5449(5) 0.7122(4) 0.3031(4) 0.0688(17) Uani 1 1 d . . . F9 F 0.6496(5) 0.6438(4) 0.1861(3) 0.0552(14) Uani 1 1 d . A . F10 F 0.6631(4) 0.4578(3) 0.1682(3) 0.0380(11) Uani 1 1 d . . . F11 F 0.5885(4) 0.1058(3) 0.1894(3) 0.0371(11) Uani 1 1 d . . . F12 F 0.7880(4) 0.0893(4) 0.1655(3) 0.0422(11) Uani 1 1 d . A . F13 F 1.0147(4) 0.2760(4) 0.2112(3) 0.0501(13) Uani 1 1 d . . . F14 F 1.0386(4) 0.4791(4) 0.2885(4) 0.0548(14) Uani 1 1 d . A . F15 F 0.8419(4) 0.4995(3) 0.3105(3) 0.0390(11) Uani 1 1 d . . . F16 F 0.7246(4) 0.4107(3) 0.4300(3) 0.0354(10) Uani 1 1 d . . . F17 F 0.7041(4) 0.3362(4) 0.5593(3) 0.0418(11) Uani 1 1 d . A . F18 F 0.5077(5) 0.1339(4) 0.5374(3) 0.0485(12) Uani 1 1 d . . . F19 F 0.3360(4) 0.0056(4) 0.3792(3) 0.0437(11) Uani 1 1 d . A . F20 F 0.3589(4) 0.0726(3) 0.2475(3) 0.0340(10) Uani 1 1 d . . . C1 C 1.0626(7) 0.2384(6) 0.3877(5) 0.0325(18) Uani 1 1 d . . . C2 C 0.9667(7) 0.2433(6) 0.4230(5) 0.0317(18) Uani 1 1 d . . . C3 C 0.8616(6) 0.1312(6) 0.3922(5) 0.0293(16) Uani 1 1 d . . . C4 C 0.8943(7) 0.0584(6) 0.3383(5) 0.0292(16) Uani 1 1 d . . . C5 C 1.0178(7) 0.1252(6) 0.3373(5) 0.0298(17) Uani 1 1 d . . . C6 C 1.1875(8) 0.3372(7) 0.3973(6) 0.048(2) Uani 1 1 d . . . H6A H 1.1762 0.3691 0.3534 0.057 Uiso 1 1 calc R . . H6B H 1.2488 0.3120 0.3906 0.057 Uiso 1 1 calc R . . H6C H 1.2182 0.3943 0.4543 0.057 Uiso 1 1 calc R . . C7 C 0.9711(8) 0.3480(6) 0.4740(6) 0.042(2) Uani 1 1 d . . . H7A H 0.9418 0.3789 0.4350 0.051 Uiso 1 1 calc R . . H7B H 1.0577 0.4029 0.5097 0.051 Uiso 1 1 calc R . . H7C H 0.9165 0.3307 0.5106 0.051 Uiso 1 1 calc R . . C8 C 0.7387(7) 0.0986(7) 0.4090(6) 0.041(2) Uani 1 1 d . . . H8A H 0.6828 0.1050 0.3652 0.049 Uiso 1 1 calc R . . H8B H 0.7514 0.1482 0.4656 0.049 Uiso 1 1 calc R . . H8C H 0.7005 0.0210 0.4074 0.049 Uiso 1 1 calc R . . C9 C 0.8089(7) -0.0646(6) 0.2897(5) 0.0337(18) Uani 1 1 d . . . H9A H 0.7668 -0.0761 0.2312 0.040 Uiso 1 1 calc R . . H9B H 0.7458 -0.0952 0.3183 0.040 Uiso 1 1 calc R . . H9C H 0.8586 -0.1029 0.2877 0.040 Uiso 1 1 calc R . . C10 C 1.0836(8) 0.0799(7) 0.2834(6) 0.044(2) Uani 1 1 d . . . H10A H 1.0579 0.0781 0.2249 0.053 Uiso 1 1 calc R . . H10B H 1.0605 0.0039 0.2822 0.053 Uiso 1 1 calc R . . H10C H 1.1749 0.1283 0.3083 0.053 Uiso 1 1 calc R . . C11 C 0.2847(7) 0.8139(6) 0.1837(5) 0.0359(19) Uani 1 1 d . . . C12 C 0.2338(8) 0.8274(6) 0.1083(5) 0.0361(19) Uani 1 1 d . . . C13 C 0.1010(9) 0.7828(7) 0.0948(5) 0.047(2) Uani 1 1 d . . . C14 C 0.0692(8) 0.7388(7) 0.1591(7) 0.053(3) Uani 1 1 d . . . C15 C 0.1827(8) 0.7579(6) 0.2160(6) 0.045(2) Uani 1 1 d . . . C16 C 0.4193(8) 0.8570(7) 0.2258(6) 0.054(3) Uani 1 1 d . . . H16A H 0.4576 0.9350 0.2637 0.065 Uiso 1 1 calc R . . H16B H 0.4623 0.8527 0.1821 0.065 Uiso 1 1 calc R . . H16C H 0.4273 0.8116 0.2594 0.065 Uiso 1 1 calc R . . C17 C 0.3081(11) 0.8921(8) 0.0594(6) 0.064(3) Uani 1 1 d . . . H17A H 0.3342 0.9715 0.0856 0.077 Uiso 1 1 calc R . . H17B H 0.2560 0.8635 -0.0002 0.077 Uiso 1 1 calc R . . H17C H 0.3827 0.8836 0.0607 0.077 Uiso 1 1 calc R . . C18 C 0.0148(10) 0.7862(10) 0.0250(6) 0.077(4) Uani 1 1 d . . . H18A H 0.0183 0.8590 0.0424 0.092 Uiso 1 1 calc R . . H18B H -0.0714 0.7265 0.0134 0.092 Uiso 1 1 calc R . . H18C H 0.0407 0.7754 -0.0270 0.092 Uiso 1 1 calc R . . C19 C -0.0576(10) 0.6894(9) 0.1712(8) 0.090(4) Uani 1 1 d . . . H19A H -0.0728 0.7496 0.1997 0.108 Uiso 1 1 calc R . . H19B H -0.0620 0.6432 0.2067 0.108 Uiso 1 1 calc R . . H19C H -0.1217 0.6429 0.1153 0.108 Uiso 1 1 calc R . . C20 C 0.1952(11) 0.7347(8) 0.2979(7) 0.081(4) Uani 1 1 d . . . H20A H 0.2232 0.8032 0.3462 0.098 Uiso 1 1 calc R . . H20B H 0.2571 0.7093 0.3046 0.098 Uiso 1 1 calc R . . H20C H 0.1136 0.6763 0.2964 0.098 Uiso 1 1 calc R . . C21 C 0.4579(7) 0.2326(6) 0.1638(5) 0.0263(16) Uani 1 1 d . . . C22 C 0.3359(7) 0.2106(6) 0.1612(5) 0.0298(17) Uani 1 1 d . A . C23 C 0.2355(7) 0.1599(7) 0.0882(5) 0.0342(18) Uani 1 1 d . . . C24 C 0.2547(7) 0.1317(6) 0.0096(5) 0.0357(18) Uani 1 1 d . A . C25 C 0.3737(7) 0.1560(6) 0.0068(5) 0.0320(17) Uani 1 1 d . . . C26 C 0.4701(7) 0.2046(6) 0.0828(5) 0.0323(17) Uani 1 1 d . A . C27 C 0.5777(7) 0.4266(6) 0.2808(5) 0.0296(17) Uani 1 1 d . . . C28 C 0.5281(8) 0.4659(6) 0.3399(5) 0.040(2) Uani 1 1 d . A . C29 C 0.5183(9) 0.5603(7) 0.3482(6) 0.048(2) Uani 1 1 d . . . C30 C 0.5555(9) 0.6186(7) 0.2963(7) 0.055(3) Uani 1 1 d . A . C31 C 0.6077(8) 0.5852(6) 0.2373(6) 0.044(2) Uani 1 1 d . . . C32 C 0.6152(7) 0.4887(6) 0.2304(5) 0.0335(18) Uani 1 1 d . A . C33 C 0.7027(7) 0.3030(6) 0.2478(4) 0.0249(16) Uani 1 1 d . . . C34 C 0.6979(6) 0.2017(6) 0.2143(5) 0.0256(15) Uani 1 1 d . A . C35 C 0.8007(7) 0.1920(6) 0.2011(5) 0.0340(18) Uani 1 1 d . . . C36 C 0.9146(7) 0.2833(7) 0.2240(5) 0.0364(19) Uani 1 1 d . A . C37 C 0.9255(7) 0.3875(6) 0.2622(5) 0.0365(19) Uani 1 1 d . . . C38 C 0.8205(7) 0.3944(6) 0.2719(5) 0.0302(17) Uani 1 1 d . A . C39 C 0.5416(6) 0.2481(6) 0.3319(5) 0.0256(15) Uani 1 1 d . . . C40 C 0.6279(7) 0.3097(6) 0.4137(5) 0.0280(17) Uani 1 1 d . A . C41 C 0.6181(7) 0.2744(6) 0.4834(5) 0.0315(17) Uani 1 1 d . . . C42 C 0.5183(7) 0.1715(7) 0.4722(5) 0.0350(18) Uani 1 1 d . A . C43 C 0.4335(7) 0.1071(6) 0.3923(5) 0.0265(16) Uani 1 1 d . . . C44 C 0.4471(7) 0.1448(5) 0.3242(5) 0.0272(16) Uani 1 1 d . A . Cl1 Cl 1.0828(4) -0.0022(3) 0.4666(3) 0.0353(9) Uani 0.50 1 d P . 2 O1 O 1.2682(13) 0.1298(12) 0.5179(9) 0.065(4) Uani 0.50 1 d PU . 2 O2 O 0.9457(15) 0.1374(12) 0.6286(10) 0.077(4) Uani 0.50 1 d PU . 2 C46 C 1.1753(14) 0.1300(12) 0.4991(10) 0.029(3) Uani 0.50 1 d PU . 2 C47 C 0.9834(16) 0.1380(12) 0.5639(11) 0.037(4) Uani 0.50 1 d PU . 2 C48 C 1.2072(18) 0.2514(16) 0.5514(13) 0.064(5) Uani 0.50 1 d PU . 2 H48A H 1.2062 0.3104 0.5933 0.096 Uiso 0.50 1 d PR . 2 H48B H 1.2602 0.2825 0.5183 0.096 Uiso 0.50 1 d PR . 2 H48C H 1.2391 0.2136 0.5798 0.096 Uiso 0.50 1 d PR . 2 C49 C 1.0936(14) 0.2553(12) 0.5987(10) 0.032(3) Uani 0.50 1 d PU . 2 H49A H 1.0230 0.2505 0.6178 0.047 Uiso 0.50 1 d PR . 2 H49B H 1.1443 0.3299 0.5997 0.047 Uiso 0.50 1 d PR . 2 H49C H 1.1431 0.2376 0.6358 0.047 Uiso 0.50 1 d PR . 2 Cl2 Cl 0.0441(7) 0.5367(5) -0.0588(4) 0.0385(14) Uani 0.36 1 d PU . 3 Cl3 Cl 0.0191(17) 0.4730(13) 0.0509(11) 0.040(4) Uani 0.14 1 d PU . 3 O3 O 0.169(3) 0.584(3) -0.086(2) 0.078(9) Uani 0.25 1 d PU . 3 O4 O 0.392(4) 0.619(4) 0.045(3) 0.053(11) Uani 0.14 1 d PU . 3 O5 O 0.256(4) 0.516(4) 0.170(3) 0.113(13) Uani 0.25 1 d PU . 3 O6 O 0.144(2) 0.456(2) 0.1371(16) 0.089(7) Uani 0.36 1 d PU . 3 C50 C 0.166(3) 0.601(2) -0.0202(18) 0.088(7) Uani 0.50 1 d PU . 3 H50A H 0.2504 0.6174 -0.0176 0.132 Uiso 0.25 1 d PR . 3 H50B H 0.1421 0.6395 -0.0528 0.132 Uiso 0.25 1 d PR . 3 H50C H 0.1099 0.5219 -0.0471 0.132 Uiso 0.25 1 d PR . 3 C51 C 0.265(5) 0.622(4) -0.009(3) 0.072(12) Uani 0.25 1 d PU . 3 H51A H 0.2103 0.5559 -0.0581 0.108 Uiso 0.25 1 d PR . 3 H51B H 0.3334 0.6155 0.0193 0.108 Uiso 0.25 1 d PR . 3 H51C H 0.2974 0.6861 -0.0267 0.108 Uiso 0.25 1 d PR . 3 C52 C 0.3028(19) 0.6270(17) 0.0597(15) 0.064(5) Uani 0.50 1 d PU . 3 H52A H 0.2710 0.5623 0.0092 0.097 Uiso 0.36 1 d PR . 3 H52B H 0.3468 0.6179 0.1069 0.097 Uiso 0.36 1 d PR . 3 H52C H 0.3595 0.6924 0.0501 0.097 Uiso 0.36 1 d PR . 3 C53 C 0.247(4) 0.574(3) 0.139(2) 0.047(9) Uani 0.25 1 d PU . 3 C54 C 0.152(2) 0.5266(19) 0.1175(15) 0.069(6) Uani 0.50 1 d PU . 3 H54A H 0.1787 0.4870 0.0781 0.103 Uiso 0.14 1 d PR . 3 H54B H 0.0680 0.4763 0.1161 0.103 Uiso 0.14 1 d PR . 3 H54C H 0.2078 0.5561 0.1743 0.103 Uiso 0.14 1 d PR . 3 B1 B 0.5709(8) 0.3024(6) 0.2557(5) 0.0241(17) Uani 1 1 d . A 3 Cl4 Cl 0.4035(4) 0.4198(3) 0.0262(3) 0.0965(13) Uani 0.86 1 d PD . . C45 C 0.4650(14) 0.5413(11) 0.0057(15) 0.058(6) Uani 0.43 1 d PDU . . H45A H 0.3985 0.5362 -0.0391 0.070 Uiso 0.43 1 calc PR . . H45B H 0.4836 0.6026 0.0582 0.070 Uiso 0.43 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02679(17) 0.02326(15) 0.03020(18) 0.00693(12) 0.00362(12) 0.01049(13) Ir2 0.0465(2) 0.0320(2) 0.0610(3) -0.00972(17) -0.01072(19) 0.01999(18) F1 0.034(2) 0.048(3) 0.041(3) 0.019(2) 0.019(2) 0.023(2) F2 0.030(3) 0.074(3) 0.045(3) 0.023(3) 0.013(2) 0.028(3) F3 0.043(3) 0.060(3) 0.032(3) 0.009(2) 0.002(2) 0.028(3) F4 0.048(3) 0.068(3) 0.028(3) 0.006(2) 0.012(2) 0.032(3) F5 0.039(3) 0.062(3) 0.035(3) 0.008(2) 0.017(2) 0.029(3) F6 0.065(3) 0.047(3) 0.062(3) 0.023(3) 0.041(3) 0.041(3) F7 0.115(5) 0.068(4) 0.093(5) 0.025(3) 0.058(4) 0.071(4) F8 0.086(4) 0.038(3) 0.095(5) 0.022(3) 0.016(3) 0.046(3) F9 0.060(3) 0.039(3) 0.072(4) 0.032(3) 0.014(3) 0.024(3) F10 0.044(3) 0.037(2) 0.046(3) 0.022(2) 0.022(2) 0.024(2) F11 0.031(2) 0.017(2) 0.055(3) 0.006(2) 0.013(2) 0.0084(19) F12 0.049(3) 0.042(3) 0.047(3) 0.012(2) 0.020(2) 0.032(2) F13 0.037(3) 0.060(3) 0.070(4) 0.027(3) 0.027(3) 0.031(3) F14 0.027(3) 0.043(3) 0.087(4) 0.024(3) 0.019(3) 0.010(2) F15 0.030(2) 0.025(2) 0.053(3) 0.010(2) 0.008(2) 0.010(2) F16 0.033(2) 0.025(2) 0.037(3) 0.0070(19) 0.006(2) 0.009(2) F17 0.041(3) 0.056(3) 0.023(2) 0.005(2) 0.006(2) 0.025(2) F18 0.053(3) 0.066(3) 0.041(3) 0.030(3) 0.024(2) 0.033(3) F19 0.043(3) 0.035(2) 0.053(3) 0.023(2) 0.020(2) 0.014(2) F20 0.031(2) 0.030(2) 0.033(3) 0.0079(19) 0.007(2) 0.010(2) C1 0.036(4) 0.026(4) 0.039(5) 0.015(3) 0.011(4) 0.016(4) C2 0.038(4) 0.023(4) 0.033(5) 0.009(3) 0.004(4) 0.016(4) C3 0.021(4) 0.028(4) 0.032(4) 0.007(3) 0.007(3) 0.010(3) C4 0.033(4) 0.029(4) 0.026(4) 0.010(3) 0.012(3) 0.014(3) C5 0.025(4) 0.034(4) 0.037(5) 0.020(4) 0.016(3) 0.014(3) C6 0.036(5) 0.038(5) 0.061(6) 0.027(4) 0.008(4) 0.010(4) C7 0.050(5) 0.027(4) 0.046(5) 0.009(4) 0.009(4) 0.020(4) C8 0.029(4) 0.044(5) 0.048(6) 0.015(4) 0.014(4) 0.016(4) C9 0.032(4) 0.023(4) 0.030(4) -0.001(3) 0.001(3) 0.008(3) C10 0.053(6) 0.050(5) 0.050(6) 0.024(4) 0.035(5) 0.032(5) C11 0.033(4) 0.025(4) 0.039(5) 0.004(3) -0.005(4) 0.014(4) C12 0.050(5) 0.032(4) 0.028(4) 0.003(3) 0.001(4) 0.029(4) C13 0.055(6) 0.040(5) 0.032(5) -0.014(4) -0.005(4) 0.032(5) C14 0.024(5) 0.034(5) 0.075(7) -0.003(5) 0.009(5) 0.005(4) C15 0.054(6) 0.023(4) 0.044(5) 0.008(4) 0.000(4) 0.014(4) C16 0.040(5) 0.040(5) 0.077(7) 0.015(5) 0.003(5) 0.023(4) C17 0.100(9) 0.072(7) 0.032(5) 0.013(5) 0.029(6) 0.052(7) C18 0.077(8) 0.100(9) 0.046(7) 0.001(6) -0.019(5) 0.062(7) C19 0.056(7) 0.052(7) 0.115(11) -0.004(7) 0.026(7) 0.003(6) C20 0.101(9) 0.039(6) 0.087(9) 0.037(6) 0.024(7) 0.014(6) C21 0.029(4) 0.027(4) 0.032(4) 0.011(3) 0.014(3) 0.020(3) C22 0.038(5) 0.029(4) 0.030(4) 0.011(3) 0.021(4) 0.019(4) C23 0.024(4) 0.045(5) 0.034(5) 0.012(4) 0.008(4) 0.019(4) C24 0.024(4) 0.041(5) 0.031(5) 0.007(4) -0.002(3) 0.014(4) C25 0.035(4) 0.036(4) 0.034(5) 0.012(4) 0.017(4) 0.023(4) C26 0.025(4) 0.041(4) 0.032(5) 0.008(4) 0.012(3) 0.018(4) C27 0.025(4) 0.026(4) 0.033(5) 0.007(3) 0.001(3) 0.013(3) C28 0.054(5) 0.038(4) 0.045(5) 0.014(4) 0.024(4) 0.034(4) C29 0.079(7) 0.041(5) 0.055(6) 0.020(4) 0.039(5) 0.049(5) C30 0.067(7) 0.035(5) 0.065(7) 0.011(5) 0.011(5) 0.035(5) C31 0.049(5) 0.027(4) 0.051(6) 0.020(4) 0.004(4) 0.015(4) C32 0.032(4) 0.028(4) 0.047(5) 0.017(4) 0.015(4) 0.017(4) C33 0.032(4) 0.027(4) 0.024(4) 0.014(3) 0.013(3) 0.019(3) C34 0.019(4) 0.030(4) 0.023(4) 0.006(3) 0.009(3) 0.009(3) C35 0.041(5) 0.028(4) 0.039(5) 0.010(4) 0.013(4) 0.022(4) C36 0.027(4) 0.047(5) 0.045(5) 0.019(4) 0.014(4) 0.024(4) C37 0.032(4) 0.038(5) 0.042(5) 0.022(4) 0.013(4) 0.015(4) C38 0.028(4) 0.022(4) 0.036(5) 0.010(3) 0.010(3) 0.009(3) C39 0.025(4) 0.031(4) 0.030(4) 0.009(3) 0.014(3) 0.020(3) C40 0.032(4) 0.030(4) 0.036(5) 0.008(3) 0.016(4) 0.027(4) C41 0.024(4) 0.035(4) 0.040(5) 0.010(4) 0.012(4) 0.019(4) C42 0.041(5) 0.050(5) 0.033(5) 0.021(4) 0.019(4) 0.032(4) C43 0.028(4) 0.025(4) 0.037(5) 0.017(3) 0.018(4) 0.016(3) C44 0.026(4) 0.022(4) 0.026(4) -0.001(3) 0.002(3) 0.012(3) Cl1 0.033(2) 0.040(2) 0.047(2) 0.0261(19) 0.0181(18) 0.0229(18) O1 0.060(6) 0.074(6) 0.064(6) 0.022(5) 0.018(5) 0.038(5) O2 0.087(7) 0.077(6) 0.076(7) 0.026(5) 0.020(5) 0.051(5) C46 0.029(6) 0.028(5) 0.036(6) 0.013(5) 0.011(5) 0.019(5) C47 0.053(7) 0.033(6) 0.033(6) 0.017(5) 0.011(5) 0.026(5) C48 0.060(8) 0.064(8) 0.062(8) 0.030(6) 0.004(5) 0.025(6) C49 0.038(6) 0.032(6) 0.037(6) 0.021(5) 0.007(5) 0.024(5) Cl2 0.048(4) 0.028(3) 0.026(3) 0.004(2) 0.010(3) 0.011(3) Cl3 0.043(7) 0.033(6) 0.035(7) 0.012(5) 0.004(5) 0.015(5) O3 0.080(10) 0.078(10) 0.074(10) 0.028(6) 0.029(5) 0.034(6) O4 0.053(12) 0.053(12) 0.057(12) 0.014(6) 0.016(6) 0.031(7) O5 0.113(13) 0.113(13) 0.116(13) 0.039(7) 0.037(6) 0.057(8) O6 0.101(8) 0.081(8) 0.089(8) 0.033(5) 0.018(5) 0.050(5) C50 0.084(9) 0.087(9) 0.085(10) 0.013(6) 0.045(7) 0.038(7) C51 0.072(14) 0.071(14) 0.073(14) 0.027(8) 0.026(8) 0.033(9) C52 0.055(7) 0.065(8) 0.073(8) 0.004(5) 0.019(6) 0.040(6) C53 0.051(11) 0.041(10) 0.050(11) 0.012(7) 0.008(7) 0.027(7) C54 0.081(9) 0.064(8) 0.070(8) 0.033(6) 0.018(6) 0.040(6) B1 0.027(4) 0.022(4) 0.023(5) 0.005(3) 0.006(4) 0.015(4) Cl4 0.088(3) 0.080(2) 0.087(3) 0.043(2) -0.010(2) 0.019(2) C45 0.055(8) 0.065(8) 0.055(8) 0.022(6) 0.017(6) 0.028(6) _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 Ir1 C47 1.731(17) . ? Ir1 C46 1.875(14) . ? Ir1 C48 2.037(19) . ? Ir1 C49 2.114(15) . ? Ir1 C2 2.186(7) . ? Ir1 C1 2.190(7) . ? Ir1 C5 2.214(7) . ? Ir1 C3 2.223(7) . ? Ir1 C4 2.257(7) . ? Ir1 Cl1 2.375(3) . ? Ir1 Cl1 2.427(4) 2_756 ? Ir2 C50 1.82(3) . ? Ir2 C54 1.88(2) . ? Ir2 C53 2.06(4) . ? Ir2 C52 2.065(18) . ? Ir2 Cl3 2.158(17) . ? Ir2 C11 2.183(7) . ? Ir2 C12 2.206(7) . ? Ir2 C15 2.216(9) . ? Ir2 C14 2.267(9) . ? Ir2 C13 2.283(8) . ? Ir2 C51 2.33(5) . ? Ir2 Cl2 2.378(6) . ? F1 C22 1.348(8) . ? F2 C23 1.335(8) . ? F3 C24 1.335(8) . ? F4 C25 1.336(8) . ? F5 C26 1.351(8) . ? F6 C28 1.354(9) . ? F7 C29 1.356(9) . ? F8 C30 1.368(9) . ? F9 C31 1.350(9) . ? F10 C32 1.358(9) . ? F11 C34 1.341(8) . ? F12 C35 1.359(8) . ? F13 C36 1.333(8) . ? F14 C37 1.336(9) . ? F15 C38 1.358(8) . ? F16 C40 1.330(8) . ? F17 C41 1.324(9) . ? F18 C42 1.336(8) . ? F19 C43 1.351(8) . ? F20 C44 1.361(8) . ? C1 C5 1.420(10) . ? C1 C2 1.429(11) . ? C1 C6 1.518(10) . ? C2 C3 1.439(10) . ? C2 C7 1.495(10) . ? C3 C4 1.441(10) . ? C3 C8 1.483(10) . ? C4 C5 1.411(10) . ? C4 C9 1.502(10) . ? C5 C10 1.519(10) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.424(10) . ? C11 C15 1.442(12) . ? C11 C16 1.478(11) . ? C12 C13 1.436(12) . ? C12 C17 1.498(12) . ? C13 C14 1.406(13) . ? C13 C18 1.486(12) . ? C14 C15 1.446(12) . ? C14 C19 1.488(13) . ? C15 C20 1.497(13) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.380(10) . ? C21 C22 1.395(10) . ? C21 B1 1.645(11) . ? C22 C23 1.375(10) . ? C23 C24 1.378(11) . ? C24 C25 1.370(10) . ? C25 C26 1.384(11) . ? C27 C32 1.361(10) . ? C27 C28 1.378(10) . ? C27 B1 1.668(10) . ? C28 C29 1.370(10) . ? C29 C30 1.346(12) . ? C30 C31 1.368(13) . ? C31 C32 1.388(10) . ? C33 C38 1.372(10) . ? C33 C34 1.378(9) . ? C33 B1 1.656(10) . ? C34 C35 1.384(10) . ? C35 C36 1.345(11) . ? C36 C37 1.395(11) . ? C37 C38 1.377(10) . ? C39 C44 1.377(10) . ? C39 C40 1.394(10) . ? C39 B1 1.663(11) . ? C40 C41 1.390(10) . ? C41 C42 1.383(11) . ? C42 C43 1.368(11) . ? C43 C44 1.385(10) . ? Cl1 C46 1.599(15) . ? Cl1 C47 1.627(15) 2_756 ? Cl1 O2 2.026(16) 2_756 ? Cl1 O1 2.089(15) . ? Cl1 Ir1 2.427(4) 2_756 ? O1 C46 1.147(18) . ? O2 C47 1.25(2) . ? O2 Cl1 2.026(16) 2_756 ? C48 H48A 0.9602 . ? C48 H48B 0.9599 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? Cl2 Cl3 0.773(16) 2_565 ? Cl2 C50 1.32(3) . ? Cl2 O3 1.59(3) . ? Cl2 C54 2.14(3) 2_565 ? Cl2 Cl3 2.257(17) . ? Cl2 Ir2 2.563(7) 2_565 ? Cl2 H50B 1.3990 . ? Cl2 H50C 0.9300 . ? Cl3 Cl2 0.773(16) 2_565 ? Cl3 C54 1.56(3) . ? Cl3 C50 1.97(3) 2_565 ? Cl3 O6 2.08(3) . ? Cl3 Cl3 2.11(3) 2_565 ? Cl3 Ir2 2.519(17) 2_565 ? Cl3 H54B 1.1494 . ? O3 C50 1.08(3) . ? O4 C52 1.21(4) . ? O5 C53 1.11(5) . ? O6 C54 1.09(3) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9599 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9599 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9601 . ? Cl4 C45 1.699(5) 2_665 ? Cl4 C45 1.703(5) . ? C45 Cl4 1.699(5) 2_665 ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? 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 C47 Ir1 C46 101.9(7) . . ? C47 Ir1 C2 105.4(5) . . ? C46 Ir1 C2 138.8(5) . . ? C48 Ir1 C2 104.3(6) . . ? C49 Ir1 C2 90.7(4) . . ? C47 Ir1 C1 140.2(5) . . ? C46 Ir1 C1 104.0(5) . . ? C49 Ir1 C1 107.0(4) . . ? C47 Ir1 C5 160.1(6) . . ? C46 Ir1 C5 96.7(5) . . ? C48 Ir1 C5 111.1(6) . . ? C49 Ir1 C5 144.3(4) . . ? C47 Ir1 C3 98.3(6) . . ? C46 Ir1 C3 158.5(5) . . ? C48 Ir1 C3 142.2(6) . . ? C49 Ir1 C3 112.2(4) . . ? C47 Ir1 C4 124.3(6) . . ? C46 Ir1 C4 122.1(5) . . ? C48 Ir1 C4 147.7(6) . . ? C49 Ir1 C4 149.7(4) . . ? C47 Ir1 Cl1 94.9(5) . . ? C49 Ir1 Cl1 111.6(4) . . ? C2 Ir1 Cl1 157.0(2) . . ? C1 Ir1 Cl1 124.5(2) . . ? C5 Ir1 Cl1 94.2(2) . . ? C3 Ir1 Cl1 129.1(2) . . ? C4 Ir1 Cl1 96.5(2) . . ? C46 Ir1 Cl1 93.0(4) . 2_756 ? C48 Ir1 Cl1 110.8(5) . 2_756 ? C2 Ir1 Cl1 127.7(2) . 2_756 ? C1 Ir1 Cl1 159.8(2) . 2_756 ? C5 Ir1 Cl1 130.5(2) . 2_756 ? C3 Ir1 Cl1 97.3(2) . 2_756 ? C4 Ir1 Cl1 99.2(2) . 2_756 ? C50 Ir2 C54 97.2(11) . . ? C50 Ir2 C53 96.1(14) . . ? C52 Ir2 Cl3 97.8(8) . . ? C50 Ir2 C11 124.4(9) . . ? C54 Ir2 C11 116.0(8) . . ? C53 Ir2 C11 93.8(11) . . ? C52 Ir2 C11 92.4(6) . . ? Cl3 Ir2 C11 152.1(5) . . ? C50 Ir2 C12 98.4(9) . . ? C54 Ir2 C12 153.5(8) . . ? C53 Ir2 C12 127.0(11) . . ? C52 Ir2 C12 99.7(6) . . ? Cl3 Ir2 C12 159.2(5) . . ? C50 Ir2 C15 161.3(9) . . ? C54 Ir2 C15 98.6(7) . . ? C53 Ir2 C15 92.7(11) . . ? C52 Ir2 C15 120.8(7) . . ? Cl3 Ir2 C15 116.2(5) . . ? C50 Ir2 C14 138.8(10) . . ? C54 Ir2 C14 116.2(8) . . ? C53 Ir2 C14 124.9(11) . . ? C52 Ir2 C14 155.2(6) . . ? Cl3 Ir2 C14 103.9(6) . . ? C50 Ir2 C13 106.4(9) . . ? C54 Ir2 C13 151.7(8) . . ? C53 Ir2 C13 153.7(11) . . ? C52 Ir2 C13 134.6(7) . . ? Cl3 Ir2 C13 122.4(5) . . ? C54 Ir2 C51 90.7(13) . . ? Cl3 Ir2 C51 96.2(13) . . ? C11 Ir2 C51 105.2(12) . . ? C12 Ir2 C51 93.4(11) . . ? C15 Ir2 C51 142.2(13) . . ? C14 Ir2 C51 153.1(12) . . ? C13 Ir2 C51 117.4(12) . . ? C54 Ir2 Cl2 93.8(7) . . ? C53 Ir2 Cl2 109.0(10) . . ? C11 Ir2 Cl2 147.7(3) . . ? C12 Ir2 Cl2 110.9(2) . . ? C15 Ir2 Cl2 153.7(3) . . ? C14 Ir2 Cl2 116.2(3) . . ? C13 Ir2 Cl2 97.3(3) . . ? C5 C1 C2 108.1(6) . . ? C5 C1 C6 125.4(7) . . ? C2 C1 C6 126.4(7) . . ? C6 C1 Ir1 125.6(5) . . ? C1 C2 C3 107.3(6) . . ? C1 C2 C7 125.5(7) . . ? C3 C2 C7 126.9(7) . . ? C7 C2 Ir1 127.1(5) . . ? C2 C3 C4 108.0(6) . . ? C2 C3 C8 125.5(7) . . ? C4 C3 C8 126.3(7) . . ? C8 C3 Ir1 126.3(5) . . ? C5 C4 C3 107.3(6) . . ? C5 C4 C9 127.1(7) . . ? C3 C4 C9 125.5(6) . . ? C9 C4 Ir1 127.5(5) . . ? C4 C5 C1 109.3(6) . . ? C4 C5 C10 123.3(7) . . ? C1 C5 C10 127.3(7) . . ? C10 C5 Ir1 126.7(5) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 108.0(7) . . ? C12 C11 C16 126.4(8) . . ? C15 C11 C16 125.4(8) . . ? C16 C11 Ir2 125.0(5) . . ? C11 C12 C13 108.0(8) . . ? C11 C12 C17 125.8(8) . . ? C13 C12 C17 125.6(8) . . ? C17 C12 Ir2 128.1(6) . . ? C14 C13 C12 108.5(7) . . ? C14 C13 C18 126.9(9) . . ? C12 C13 C18 124.6(9) . . ? C18 C13 Ir2 126.8(6) . . ? C13 C14 C15 108.5(7) . . ? C13 C14 C19 126.0(10) . . ? C15 C14 C19 125.4(10) . . ? C19 C14 Ir2 127.8(7) . . ? C11 C15 C14 107.0(7) . . ? C11 C15 C20 125.9(8) . . ? C14 C15 C20 126.8(9) . . ? C20 C15 Ir2 126.9(6) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 111.9(6) . . ? C26 C21 B1 127.5(6) . . ? C22 C21 B1 119.9(6) . . ? F1 C22 C23 115.3(6) . . ? F1 C22 C21 119.3(6) . . ? C23 C22 C21 125.4(7) . . ? F2 C23 C24 119.2(7) . . ? F2 C23 C22 121.7(7) . . ? C24 C23 C22 119.1(7) . . ? F3 C24 C25 119.9(7) . . ? F3 C24 C23 121.2(7) . . ? C25 C24 C23 118.9(7) . . ? F4 C25 C24 120.5(7) . . ? F4 C25 C26 120.2(6) . . ? C24 C25 C26 119.3(7) . . ? F5 C26 C21 120.2(7) . . ? F5 C26 C25 114.4(6) . . ? C21 C26 C25 125.4(7) . . ? C32 C27 C28 114.4(7) . . ? C32 C27 B1 118.8(7) . . ? C28 C27 B1 125.7(7) . . ? F6 C28 C29 114.7(7) . . ? F6 C28 C27 122.2(6) . . ? C29 C28 C27 123.1(8) . . ? C30 C29 F7 119.1(7) . . ? C30 C29 C28 120.4(8) . . ? F7 C29 C28 120.5(8) . . ? C29 C30 F8 121.1(8) . . ? C29 C30 C31 119.3(7) . . ? F8 C30 C31 119.5(8) . . ? F9 C31 C30 120.9(7) . . ? F9 C31 C32 120.6(8) . . ? C30 C31 C32 118.5(7) . . ? F10 C32 C27 120.4(6) . . ? F10 C32 C31 115.5(7) . . ? C27 C32 C31 124.1(8) . . ? C38 C33 C34 114.2(6) . . ? C38 C33 B1 127.4(6) . . ? C34 C33 B1 118.3(6) . . ? F11 C34 C33 120.1(6) . . ? F11 C34 C35 116.4(6) . . ? C33 C34 C35 123.4(6) . . ? C36 C35 F12 118.9(7) . . ? C36 C35 C34 120.9(7) . . ? F12 C35 C34 120.2(7) . . ? F13 C36 C35 121.9(7) . . ? F13 C36 C37 120.4(7) . . ? C35 C36 C37 117.7(7) . . ? F14 C37 C38 121.2(7) . . ? F14 C37 C36 118.9(7) . . ? C38 C37 C36 119.9(7) . . ? F15 C38 C33 121.2(6) . . ? F15 C38 C37 115.0(6) . . ? C33 C38 C37 123.7(7) . . ? C44 C39 C40 114.2(7) . . ? C44 C39 B1 128.5(7) . . ? C40 C39 B1 117.2(6) . . ? F16 C40 C41 115.5(7) . . ? F16 C40 C39 120.5(6) . . ? C41 C40 C39 124.0(7) . . ? F17 C41 C42 119.8(7) . . ? F17 C41 C40 121.2(7) . . ? C42 C41 C40 119.0(7) . . ? F18 C42 C43 120.7(7) . . ? F18 C42 C41 120.5(7) . . ? C43 C42 C41 118.8(7) . . ? F19 C43 C42 120.1(6) . . ? F19 C43 C44 119.4(7) . . ? C42 C43 C44 120.5(6) . . ? F20 C44 C39 121.2(6) . . ? F20 C44 C43 115.3(6) . . ? C39 C44 C43 123.5(7) . . ? C46 Cl1 C47 167.6(8) . 2_756 ? C46 Cl1 O2 135.7(7) . 2_756 ? C47 Cl1 O1 134.8(7) 2_756 . ? O2 Cl1 O1 115.4(6) 2_756 . ? C47 Cl1 Ir1 140.3(6) 2_756 . ? O2 Cl1 Ir1 134.3(4) 2_756 . ? C46 Cl1 Ir1 137.5(6) . 2_756 ? C47 Cl1 Ir1 45.4(6) 2_756 2_756 ? O1 Cl1 Ir1 127.8(4) . 2_756 ? Ir1 Cl1 Ir1 117.08(15) . 2_756 ? O1 C46 C48 104.3(15) . . ? O1 C46 Cl1 97.8(11) . . ? C48 C46 Cl1 149.3(13) . . ? O1 C46 Ir1 176.2(14) . . ? Cl1 C46 H48C 133.7 . . ? Ir1 C46 H48C 100.2 . . ? O2 C47 C49 99.2(14) . . ? O2 C47 Cl1 88.4(11) . 2_756 ? C49 C47 Cl1 154.5(12) . 2_756 ? O2 C47 Ir1 176.8(14) . . ? C49 C47 Ir1 81.2(10) . . ? Cl1 C47 Ir1 92.5(8) 2_756 . ? Cl1 C47 H49A 157.8 2_756 . ? Ir1 C47 H49A 109.7 . . ? C46 C48 C49 113.6(13) . . ? C46 C48 H48A 159.0 . . ? Ir1 C48 H48A 109.4 . . ? C46 C48 H48B 91.5 . . ? C49 C48 H48B 145.5 . . ? Ir1 C48 H48B 109.4 . . ? H48A C48 H48B 109.5 . . ? C49 C48 H48C 103.3 . . ? Ir1 C48 H48C 109.6 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 C48 106.6(12) . . ? C47 C49 H48A 139.7 . . ? C48 C49 H49A 172.6 . . ? Ir1 C49 H49A 109.6 . . ? H48A C49 H49A 152.8 . . ? C47 C49 H49B 156.1 . . ? Ir1 C49 H49B 109.4 . . ? H48A C49 H49B 45.8 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 93.3 . . ? Ir1 C49 H49C 109.3 . . ? H48A C49 H49C 76.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? Cl3 Cl2 C50 139.8(19) 2_565 . ? Cl3 Cl2 O3 162(2) 2_565 . ? C50 Cl2 C54 164.9(14) . 2_565 ? O3 Cl2 C54 136.5(14) . 2_565 ? C50 Cl2 Cl3 90.9(13) . . ? O3 Cl2 Cl3 125.8(14) . . ? C54 Cl2 Cl3 96.0(9) 2_565 . ? Cl3 Cl2 Ir2 91.5(14) 2_565 . ? C50 Cl2 Ir2 49.6(11) . . ? O3 Cl2 Ir2 91.8(13) . . ? C54 Cl2 Ir2 125.5(7) 2_565 . ? C50 Cl2 Ir2 147.6(13) . 2_565 ? O3 Cl2 Ir2 140.7(12) . 2_565 ? C54 Cl2 Ir2 46.0(6) 2_565 2_565 ? Ir2 Cl2 Ir2 115.8(3) . 2_565 ? Cl3 Cl2 H50B 125.2 2_565 . ? C54 Cl2 H50B 125.4 2_565 . ? Cl3 Cl2 H50B 125.1 . . ? Ir2 Cl2 H50B 171.0 2_565 . ? Cl3 Cl2 H50C 144.5 2_565 . ? C54 Cl2 H50C 148.1 2_565 . ? Ir2 Cl2 H50C 105.4 2_565 . ? Cl2 Cl3 C54 129(2) 2_565 . ? C54 Cl3 C50 151.4(17) . 2_565 ? Cl2 Cl3 O6 118.5(19) 2_565 . ? C50 Cl3 O6 129.0(14) 2_565 . ? Cl2 Cl3 Cl3 90.5(17) 2_565 2_565 ? C54 Cl3 Cl3 124.6(17) . 2_565 ? O6 Cl3 Cl3 150.3(17) . 2_565 ? Cl2 Cl3 Ir2 113.3(16) 2_565 . ? C50 Cl3 Ir2 130.0(12) 2_565 . ? Cl2 Cl3 Cl2 110.5(16) 2_565 . ? C54 Cl3 Cl2 108.4(13) . . ? C50 Cl3 Cl2 98.5(11) 2_565 . ? O6 Cl3 Cl2 130.5(13) . . ? C54 Cl3 Ir2 158.5(14) . 2_565 ? O6 Cl3 Ir2 138.1(10) . 2_565 ? Ir2 Cl3 Ir2 126.9(7) . 2_565 ? Cl2 Cl3 H54B 98.0 2_565 . ? C50 Cl3 H54B 114.8 2_565 . ? Cl3 Cl3 H54B 159.5 2_565 . ? Cl2 Cl3 H54B 146.1 . . ? Ir2 Cl3 H54B 145.9 2_565 . ? C51 O3 Cl2 103(3) . . ? Cl2 O3 H50A 101.7 . . ? Cl2 O3 H51A 99.4 . . ? H50B O3 H51A 122.2 . . ? O5 O6 Cl3 130(3) . . ? O5 O6 H54B 131.2 . . ? C53 O6 H54B 90.0 . . ? C51 C50 Cl2 154(4) . . ? O3 C50 Ir2 171(3) . . ? C51 C50 Ir2 103(3) . . ? Cl2 C50 Ir2 97.1(14) . . ? O3 C50 C52 116(3) . . ? Cl2 C50 C52 147(2) . . ? O3 C50 Cl3 95(3) . 2_565 ? C51 C50 Cl3 167(3) . 2_565 ? C52 C50 Cl3 141.5(18) . 2_565 ? Cl2 C50 H50A 149.3 . . ? Ir2 C50 H50A 109.7 . . ? Cl3 C50 H50A 163.4 2_565 . ? C51 C50 H50B 113.7 . . ? Ir2 C50 H50B 109.3 . . ? C52 C50 H50B 138.9 . . ? H50A C50 H50B 109.5 . . ? C51 C50 H50C 111.8 . . ? Ir2 C50 H50C 109.4 . . ? C52 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Cl2 C50 H51A 104.0 . . ? Ir2 C50 H51A 140.4 . . ? Cl3 C50 H51A 118.1 2_565 . ? H50B C50 H51A 108.6 . . ? C50 C51 C52 108(4) . . ? C52 C51 O3 154(5) . . ? C50 C51 O4 149(5) . . ? O3 C51 O4 149(4) . . ? O3 C51 Ir2 99(3) . . ? O4 C51 Ir2 107(3) . . ? C52 C51 H50A 144.5 . . ? C52 C51 H51A 126.9 . . ? O4 C51 H51A 113.0 . . ? Ir2 C51 H51A 110.5 . . ? C50 C51 H51B 147.9 . . ? Ir2 C51 H51B 108.4 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 100.9 . . ? C52 C51 H51C 122.7 . . ? O4 C51 H51C 106.9 . . ? Ir2 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C51 H52A 105.6 . . ? O3 C51 H52A 115.0 . . ? Ir2 C51 H52A 91.5 . . ? H51C C51 H52A 153.1 . . ? C50 C51 H52C 132.0 . . ? H51A C51 H52C 159.0 . . ? C51 C52 O4 93(4) . . ? C51 C52 C53 140(3) . . ? O4 C52 C53 116(3) . . ? O4 C52 C50 126(3) . . ? C53 C52 C50 106.8(18) . . ? O4 C52 Ir2 177(3) . . ? O4 C52 H50A 96.7 . . ? C53 C52 H50A 135.1 . . ? C53 C52 H51B 143.2 . . ? Ir2 C52 H51B 142.7 . . ? C53 C52 H52A 105.4 . . ? Ir2 C52 H52A 110.0 . . ? C51 C52 H52B 160.8 . . ? C50 C52 H52B 156.1 . . ? Ir2 C52 H52B 109.8 . . ? H50A C52 H52B 162.9 . . ? H51B C52 H52B 106.9 . . ? H52A C52 H52B 109.5 . . ? C53 C52 H52C 144.5 . . ? Ir2 C52 H52C 108.6 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 O5 92(4) . . ? C54 C53 C52 110(3) . . ? O5 C53 C52 136(4) . . ? O6 C53 C52 135(3) . . ? O5 C53 Ir2 156(4) . . ? O6 C53 Ir2 108(2) . . ? C54 C53 H52B 139.3 . . ? O5 C53 H52B 109.6 . . ? O6 C53 H52B 139.7 . . ? Ir2 C53 H52B 93.9 . . ? H52B C53 H54A 98.3 . . ? C52 C53 H54C 165.0 . . ? Ir2 C53 H54C 100.3 . . ? H52B C53 H54C 159.2 . . ? H54A C53 H54C 97.1 . . ? C53 C54 O6 98(3) . . ? C53 C54 Cl3 154(3) . . ? O6 C54 Cl3 102(2) . . ? O5 C54 Cl3 151(2) . . ? C53 C54 Ir2 85(3) . . ? O6 C54 Ir2 176(3) . . ? O5 C54 Ir2 130(2) . . ? C53 C54 Cl2 164(3) . 2_565 ? O6 C54 Cl2 98(2) . 2_565 ? O5 C54 Cl2 150(2) . 2_565 ? Cl3 C54 H54A 92.2 . . ? Ir2 C54 H54A 109.6 . . ? Cl2 C54 H54A 106.9 2_565 . ? C53 C54 H54B 158.9 . . ? O5 C54 H54B 114.9 . . ? Ir2 C54 H54B 110.8 . . ? H54A C54 H54B 109.5 . . ? Cl3 C54 H54C 153.7 . . ? Ir2 C54 H54C 108.0 . . ? Cl2 C54 H54C 137.6 2_565 . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C21 B1 C33 112.4(6) . . ? C21 B1 C39 114.6(6) . . ? C33 B1 C39 102.4(5) . . ? C21 B1 C27 101.0(5) . . ? C33 B1 C27 115.9(6) . . ? C39 B1 C27 111.1(6) . . ? C45 Cl4 C45 61.1(6) 2_665 . ? Cl4 C45 Cl4 118.9(6) 2_665 . ? Cl4 C45 H45A 107.6 2_665 . ? Cl4 C45 H45A 107.6 . . ? Cl4 C45 H45B 107.6 2_665 . ? Cl4 C45 H45B 107.6 . . ? H45A C45 H45B 107.0 . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.536 _refine_diff_density_min -2.179 _refine_diff_density_rms 0.172 #===END data_shelxl_9 _publ_contact_author_name 'Werner Kaminsky' _publ_contact_author_address ; Department of Chemistry, BOX 351700 University of Washington Seattle, WA 98195 USA ; _publ_contact_author_email 'wernerka@u.washington.edu' _publ_requested_journal 'Journal title here' _publ_section_title ; title here ; loop_ _publ_author_name _publ_author_address 'Joe Meredith' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'Werner Kaminsky' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'Michael Heinekey' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; _publ_section_abstract ; Abstract here ; _publ_section_comment ; Details and comments here ; _publ_section_exptl_prep ; details of preparation here ; _publ_section_exptl_refinement ; All H atoms were initially located in a difference Fourier map and were refined with a riding model. H atoms were placed in geometrically idealised positions and constrained to ride on their parent atoms with C---H distances in the range 0.95-1.00 \%A. U~iso~ values were fixed such that they were 1.2U~eq~ of their parent atom U~eq~ for CH's and 1.5U~eq~ of their parent atom U~eq~ in case of methyl groups. ; _publ_section_references ; Altomare, A.; Cascarano, G.; Giacovazzo, C.; Burla, M.C.; Polidori, G.; Camalli, M. (1994) J. Appl. Cryst. 27, 435-442. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W. P., Garcia-Granada, S., Gould, R. O., Smits, J. M. M. & Smykalla, C. (1996) The DIRDIF96 Program System. Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. MacKay, S.; Gilmore, C.J.; Edwards, C.; Tremayne, M.; Stewart, N.; Shankland, K. (1998) "maXus: a computer program for the solution and refinement of crystal structures from diffraction data" University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan. Otwinowski, Z.; Minor, W. (1996) Methods in Enzymology, 276, 307-326. Sheldrick, G. M. (1997) SHELXL97 University of G\"ottingen, Germany. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'JMM1052' ; _chemical_name_common 'JMM1052' _chemical_melting_point ? _chemical_formula_moiety 'C22 H32 Ir2 O2, 2(C24 B F20)' _chemical_formula_sum 'C70 H32 B2 F40 Ir2 O2' _chemical_formula_weight 2070.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P -1 ' _symmetry_cell_setting 'Triclinic' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2595(2) _cell_length_b 12.5616(3) _cell_length_c 13.0354(2) _cell_angle_alpha 84.3822(10) _cell_angle_beta 65.2489(11) _cell_angle_gamma 87.8949(8) _cell_volume 1666.26(6) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 925 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 992 _exptl_absorpt_coefficient_mu 4.151 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.317 _exptl_absorpt_correction_T_max 0.605 _exptl_absorpt_process_details 'HKL2000' _exptl_special_details ; Data was collected with \w and \f scans in 2^o^ increments with 20 second exposures per degree. Crystal-to-detector distance was 30 mm. 44279 full and partial reflection were integrated. ; _diffrn_ambient_temperature 130(2) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 15395 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0808 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 31.98 _reflns_number_total 10236 _reflns_number_gt 8630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0584P)^2^+0.0000P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10236 _refine_ls_number_parameters 529 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.003 _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 Ir1 Ir 1.029489(15) 0.097581(12) 0.018964(12) 0.01858(6) Uani 1 1 d . . . H1A H 1.0635 -0.0546 0.0627 0.054(19) Uiso 1 1 d R . . F1 F 0.1471(2) 0.4851(2) 0.4306(2) 0.0223(5) Uani 1 1 d . . . F2 F 0.2527(3) 0.3117(2) 0.3205(2) 0.0281(6) Uani 1 1 d . . . F3 F 0.4769(3) 0.3303(2) 0.1249(2) 0.0291(6) Uani 1 1 d . . . F4 F 0.5957(3) 0.5233(2) 0.0468(2) 0.0236(5) Uani 1 1 d . . . F5 F 0.4953(3) 0.6959(2) 0.1510(2) 0.0235(5) Uani 1 1 d . . . F6 F 0.0674(3) 0.5933(2) 0.2751(2) 0.0234(5) Uani 1 1 d . . . F7 F -0.1720(3) 0.6520(2) 0.3072(2) 0.0302(6) Uani 1 1 d . . . F8 F -0.2936(3) 0.8134(2) 0.4380(2) 0.0321(6) Uani 1 1 d . . . F9 F -0.1657(3) 0.9150(2) 0.5385(2) 0.0265(6) Uani 1 1 d . . . F10 F 0.0760(3) 0.8582(2) 0.5081(2) 0.0232(5) Uani 1 1 d . . . F11 F 0.0300(2) 0.6452(2) 0.6150(2) 0.0233(5) Uani 1 1 d . . . F12 F 0.0773(3) 0.5726(2) 0.7908(2) 0.0273(6) Uani 1 1 d . . . F13 F 0.3243(3) 0.5509(3) 0.7728(2) 0.0407(8) Uani 1 1 d . . . F14 F 0.5309(3) 0.6015(3) 0.5677(2) 0.0384(8) Uani 1 1 d . . . F15 F 0.4865(3) 0.6737(2) 0.3875(2) 0.0283(6) Uani 1 1 d . . . F16 F 0.3686(3) 0.8720(2) 0.4495(2) 0.0261(6) Uani 1 1 d . . . F17 F 0.4597(3) 1.0589(2) 0.3384(2) 0.0306(6) Uani 1 1 d . . . F18 F 0.4479(3) 1.1176(2) 0.1353(2) 0.0295(6) Uani 1 1 d . . . F19 F 0.3434(3) 0.9816(2) 0.0463(2) 0.0276(6) Uani 1 1 d . . . F20 F 0.2565(3) 0.7886(2) 0.1537(2) 0.0250(5) Uani 1 1 d . . . O1 O 1.2965(4) 0.1162(3) -0.1765(3) 0.0432(10) Uani 1 1 d . . . C1 C 1.1966(5) 0.1041(4) -0.1047(4) 0.0286(10) Uani 1 1 d . . . C2 C 1.0624(4) 0.2586(4) 0.0682(3) 0.0248(10) Uani 1 1 d . . . C3 C 0.9478(4) 0.2589(3) 0.0430(3) 0.0210(8) Uani 1 1 d . . . C4 C 0.8490(4) 0.1864(3) 0.1245(3) 0.0197(8) Uani 1 1 d . . . C5 C 0.9013(4) 0.1339(3) 0.1974(3) 0.0199(8) Uani 1 1 d . . . C6 C 1.0334(4) 0.1720(3) 0.1624(3) 0.0179(8) Uani 1 1 d . . . C7 C 1.1804(5) 0.3237(4) 0.0149(5) 0.0360(11) Uani 1 1 d . . . H7A H 1.1704 0.3862 0.0573 0.043 Uiso 1 1 calc R . . H7B H 1.1951 0.3475 -0.0634 0.043 Uiso 1 1 calc R . . H7C H 1.2552 0.2813 0.0149 0.043 Uiso 1 1 calc R . . C8 C 0.9255(6) 0.3388(4) -0.0391(4) 0.0322(11) Uani 1 1 d . . . H8A H 0.8776 0.3999 0.0004 0.039 Uiso 1 1 calc R . . H8B H 0.8744 0.3059 -0.0728 0.039 Uiso 1 1 calc R . . H8C H 1.0099 0.3633 -0.0990 0.039 Uiso 1 1 calc R . . C9 C 0.7137(4) 0.1756(4) 0.1336(4) 0.0277(10) Uani 1 1 d . . . H9A H 0.6597 0.2339 0.1742 0.033 Uiso 1 1 calc R . . H9B H 0.6765 0.1068 0.1752 0.033 Uiso 1 1 calc R . . H9C H 0.7158 0.1789 0.0574 0.033 Uiso 1 1 calc R . . C10 C 0.8315(5) 0.0563(4) 0.2996(4) 0.0284(10) Uani 1 1 d . . . H10A H 0.8054 0.0930 0.3687 0.034 Uiso 1 1 calc R . . H10B H 0.8901 -0.0030 0.3010 0.034 Uiso 1 1 calc R . . H10C H 0.7536 0.0282 0.2956 0.034 Uiso 1 1 calc R . . C11 C 1.1191(5) 0.1449(4) 0.2221(4) 0.0318(11) Uani 1 1 d . . . H11A H 1.0933 0.1871 0.2874 0.038 Uiso 1 1 calc R . . H11B H 1.2102 0.1610 0.1700 0.038 Uiso 1 1 calc R . . H11C H 1.1102 0.0685 0.2484 0.038 Uiso 1 1 calc R . . C12 C 0.3102(4) 0.6005(3) 0.2940(3) 0.0169(7) Uani 1 1 d . . . C13 C 0.2580(4) 0.4988(3) 0.3327(3) 0.0184(8) Uani 1 1 d . . . C14 C 0.3089(4) 0.4083(3) 0.2785(4) 0.0196(8) Uani 1 1 d . . . C15 C 0.4227(4) 0.4170(3) 0.1808(4) 0.0203(8) Uani 1 1 d . . . C16 C 0.4825(4) 0.5160(3) 0.1398(3) 0.0185(8) Uani 1 1 d . . . C17 C 0.4255(4) 0.6039(3) 0.1969(3) 0.0190(8) Uani 1 1 d . . . C18 C 0.0863(4) 0.7218(3) 0.3912(3) 0.0177(8) Uani 1 1 d . . . C19 C 0.0156(4) 0.6731(3) 0.3425(3) 0.0192(8) Uani 1 1 d . . . C20 C -0.1096(5) 0.7025(4) 0.3569(4) 0.0228(8) Uani 1 1 d . . . C21 C -0.1722(5) 0.7847(4) 0.4230(4) 0.0244(9) Uani 1 1 d . . . C22 C -0.1063(4) 0.8357(3) 0.4724(3) 0.0209(8) Uani 1 1 d . . . C23 C 0.0181(4) 0.8042(3) 0.4558(3) 0.0187(8) Uani 1 1 d . . . C24 C 0.2573(4) 0.6663(3) 0.4905(3) 0.0188(8) Uani 1 1 d . . . C25 C 0.1571(4) 0.6384(3) 0.5969(3) 0.0177(7) Uani 1 1 d . . . C26 C 0.1796(4) 0.6007(3) 0.6904(3) 0.0206(8) Uani 1 1 d . . . C27 C 0.3041(5) 0.5877(4) 0.6815(4) 0.0255(9) Uani 1 1 d . . . C28 C 0.4072(5) 0.6143(4) 0.5782(4) 0.0263(9) Uani 1 1 d . . . C29 C 0.3810(4) 0.6511(4) 0.4863(4) 0.0219(8) Uani 1 1 d . . . C30 C 0.3089(4) 0.8173(3) 0.3071(3) 0.0189(8) Uani 1 1 d . . . C31 C 0.3628(4) 0.8923(3) 0.3477(3) 0.0205(8) Uani 1 1 d . . . C32 C 0.4106(4) 0.9917(3) 0.2924(4) 0.0232(9) Uani 1 1 d . . . C33 C 0.4058(4) 1.0213(3) 0.1898(4) 0.0231(9) Uani 1 1 d . . . C34 C 0.3525(5) 0.9513(3) 0.1453(4) 0.0219(8) Uani 1 1 d . . . C35 C 0.3062(4) 0.8522(3) 0.2029(3) 0.0197(8) Uani 1 1 d . . . B1 B 0.2400(5) 0.7013(4) 0.3714(4) 0.0173(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01546(9) 0.02053(9) 0.01930(8) -0.00538(6) -0.00578(6) -0.00342(6) F1 0.0180(13) 0.0234(12) 0.0206(11) 0.0021(9) -0.0036(10) -0.0079(10) F2 0.0323(16) 0.0149(12) 0.0367(14) 0.0015(10) -0.0143(12) -0.0064(11) F3 0.0304(16) 0.0163(12) 0.0398(15) -0.0090(11) -0.0125(13) 0.0018(11) F4 0.0181(13) 0.0265(13) 0.0225(11) -0.0045(10) -0.0044(10) -0.0024(10) F5 0.0224(14) 0.0172(11) 0.0248(12) -0.0021(9) -0.0032(10) -0.0072(10) F6 0.0283(14) 0.0218(12) 0.0268(12) -0.0086(10) -0.0168(11) 0.0007(11) F7 0.0270(15) 0.0349(15) 0.0386(15) -0.0074(12) -0.0222(13) -0.0031(12) F8 0.0209(14) 0.0363(16) 0.0418(15) -0.0046(13) -0.0159(12) 0.0022(12) F9 0.0231(14) 0.0253(13) 0.0298(13) -0.0094(11) -0.0088(11) 0.0042(11) F10 0.0225(14) 0.0234(12) 0.0257(12) -0.0072(10) -0.0108(11) -0.0020(10) F11 0.0173(13) 0.0308(14) 0.0208(11) 0.0042(10) -0.0080(10) -0.0033(11) F12 0.0349(16) 0.0259(13) 0.0201(11) 0.0003(10) -0.0107(11) -0.0056(12) F13 0.045(2) 0.055(2) 0.0305(14) 0.0018(14) -0.0251(14) 0.0054(16) F14 0.0233(16) 0.063(2) 0.0367(15) -0.0047(14) -0.0207(13) 0.0070(15) F15 0.0203(14) 0.0402(16) 0.0255(12) -0.0051(11) -0.0102(11) -0.0010(12) F16 0.0311(15) 0.0291(14) 0.0210(11) -0.0061(10) -0.0122(11) -0.0093(11) F17 0.0270(15) 0.0257(14) 0.0384(15) -0.0086(11) -0.0109(12) -0.0119(11) F18 0.0228(14) 0.0174(12) 0.0427(15) 0.0047(11) -0.0093(12) -0.0080(11) F19 0.0323(16) 0.0249(13) 0.0261(12) 0.0059(10) -0.0141(12) -0.0035(12) F20 0.0334(15) 0.0235(13) 0.0224(11) 0.0021(10) -0.0159(11) -0.0100(11) O1 0.025(2) 0.046(2) 0.041(2) -0.0100(17) 0.0054(16) -0.0128(17) C1 0.027(3) 0.024(2) 0.033(2) -0.0050(18) -0.010(2) -0.0088(18) C2 0.018(2) 0.045(3) 0.0139(16) -0.0152(17) -0.0087(16) 0.019(2) C3 0.019(2) 0.0196(19) 0.0217(18) -0.0024(15) -0.0061(16) -0.0034(16) C4 0.022(2) 0.0204(19) 0.0222(18) -0.0040(15) -0.0138(17) -0.0010(16) C5 0.019(2) 0.0175(18) 0.0246(19) -0.0080(15) -0.0089(17) 0.0012(16) C6 0.019(2) 0.0179(18) 0.0234(18) -0.0076(15) -0.0141(16) -0.0010(15) C7 0.031(3) 0.031(3) 0.043(3) -0.012(2) -0.011(2) -0.007(2) C8 0.043(3) 0.023(2) 0.032(2) 0.0039(19) -0.019(2) -0.006(2) C9 0.019(2) 0.035(2) 0.036(2) -0.009(2) -0.0167(19) 0.0026(19) C10 0.034(3) 0.030(2) 0.0199(19) -0.0019(17) -0.0088(19) -0.007(2) C11 0.029(3) 0.040(3) 0.034(2) -0.015(2) -0.019(2) 0.008(2) C12 0.020(2) 0.0157(17) 0.0192(17) -0.0033(14) -0.0113(16) -0.0035(15) C13 0.018(2) 0.0211(19) 0.0170(17) 0.0023(14) -0.0087(15) -0.0054(16) C14 0.019(2) 0.0165(18) 0.028(2) -0.0010(15) -0.0149(17) -0.0049(15) C15 0.024(2) 0.0152(18) 0.0248(19) -0.0034(15) -0.0132(17) -0.0025(16) C16 0.0148(19) 0.023(2) 0.0178(17) -0.0002(15) -0.0069(15) -0.0024(15) C17 0.021(2) 0.0165(18) 0.0189(17) 0.0014(14) -0.0086(16) -0.0052(15) C18 0.018(2) 0.0206(19) 0.0157(16) 0.0006(14) -0.0081(15) -0.0024(15) C19 0.019(2) 0.0170(18) 0.0223(18) -0.0034(14) -0.0094(16) -0.0020(15) C20 0.023(2) 0.025(2) 0.026(2) -0.0006(16) -0.0154(18) -0.0034(17) C21 0.021(2) 0.025(2) 0.029(2) 0.0016(17) -0.0121(18) -0.0009(17) C22 0.021(2) 0.0169(18) 0.0232(19) 0.0007(15) -0.0085(17) -0.0018(16) C23 0.021(2) 0.0170(18) 0.0204(17) -0.0003(14) -0.0106(16) -0.0037(15) C24 0.020(2) 0.0171(18) 0.0222(18) -0.0048(15) -0.0110(16) -0.0028(15) C25 0.018(2) 0.0159(17) 0.0202(17) -0.0035(14) -0.0085(15) -0.0026(15) C26 0.024(2) 0.0204(19) 0.0170(17) -0.0035(15) -0.0076(16) -0.0002(16) C27 0.033(3) 0.027(2) 0.0233(19) -0.0024(17) -0.0189(19) 0.0031(19) C28 0.021(2) 0.031(2) 0.033(2) -0.0044(18) -0.0178(19) 0.0042(19) C29 0.020(2) 0.025(2) 0.0223(18) -0.0072(16) -0.0092(16) -0.0001(17) C30 0.018(2) 0.0180(18) 0.0203(18) -0.0022(14) -0.0078(16) -0.0016(15) C31 0.021(2) 0.0212(19) 0.0203(18) -0.0067(15) -0.0081(16) -0.0019(16) C32 0.018(2) 0.0192(19) 0.031(2) -0.0085(16) -0.0070(18) -0.0021(16) C33 0.018(2) 0.0133(18) 0.035(2) -0.0010(16) -0.0077(18) -0.0027(15) C34 0.022(2) 0.0187(19) 0.0244(19) 0.0015(15) -0.0099(17) -0.0020(16) C35 0.020(2) 0.0189(19) 0.0220(18) -0.0037(15) -0.0097(16) -0.0025(16) B1 0.020(2) 0.0150(19) 0.0183(19) -0.0037(15) -0.0085(18) -0.0058(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 Ir1 C1 1.895(5) . ? Ir1 C6 2.188(4) . ? Ir1 C3 2.190(4) . ? Ir1 C5 2.247(4) . ? Ir1 C4 2.249(4) . ? Ir1 C2 2.269(5) . ? Ir1 Ir1 2.7069(3) 2_755 ? Ir1 H1A 2.0111 . ? F1 C13 1.362(5) . ? F2 C14 1.345(5) . ? F3 C15 1.351(5) . ? F4 C16 1.339(5) . ? F5 C17 1.359(5) . ? F6 C19 1.348(4) . ? F7 C20 1.345(5) . ? F8 C21 1.338(5) . ? F9 C22 1.348(5) . ? F10 C23 1.358(5) . ? F11 C25 1.351(5) . ? F12 C26 1.356(5) . ? F13 C27 1.339(5) . ? F14 C28 1.347(5) . ? F15 C29 1.350(5) . ? F16 C31 1.355(5) . ? F17 C32 1.337(5) . ? F18 C33 1.336(5) . ? F19 C34 1.353(5) . ? F20 C35 1.342(5) . ? O1 C1 1.125(6) . ? C2 C7 1.454(7) . ? C2 C3 1.459(6) . ? C2 C6 1.492(6) . ? C3 C4 1.446(6) . ? C3 C8 1.488(6) . ? C4 C5 1.414(6) . ? C4 C9 1.488(6) . ? C5 C6 1.446(6) . ? C5 C10 1.506(6) . ? C6 C11 1.485(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C17 1.380(6) . ? C12 C13 1.384(6) . ? C12 B1 1.660(6) . ? C13 C14 1.374(6) . ? C14 C15 1.375(6) . ? C15 C16 1.384(6) . ? C16 C17 1.377(6) . ? C18 C23 1.393(6) . ? C18 C19 1.395(6) . ? C18 B1 1.653(6) . ? C19 C20 1.383(6) . ? C20 C21 1.385(6) . ? C21 C22 1.375(6) . ? C22 C23 1.374(6) . ? C24 C29 1.378(6) . ? C24 C25 1.394(6) . ? C24 B1 1.660(6) . ? C25 C26 1.382(6) . ? C26 C27 1.362(6) . ? C27 C28 1.380(7) . ? C28 C29 1.383(6) . ? C30 C31 1.394(6) . ? C30 C35 1.398(6) . ? C30 B1 1.652(6) . ? C31 C32 1.385(6) . ? C32 C33 1.375(6) . ? C33 C34 1.379(6) . ? C34 C35 1.386(6) . ? 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 C1 Ir1 C6 110.89(18) . . ? C1 Ir1 C3 109.46(18) . . ? C6 Ir1 C3 64.06(15) . . ? C1 Ir1 C5 148.93(18) . . ? C6 Ir1 C5 38.04(15) . . ? C3 Ir1 C5 62.82(15) . . ? C1 Ir1 C4 147.34(18) . . ? C6 Ir1 C4 63.15(15) . . ? C3 Ir1 C4 37.98(16) . . ? C5 Ir1 C4 36.67(15) . . ? C1 Ir1 C2 91.19(18) . . ? C6 Ir1 C2 39.07(15) . . ? C3 Ir1 C2 38.14(15) . . ? C5 Ir1 C2 63.92(15) . . ? C4 Ir1 C2 63.70(15) . . ? C1 Ir1 Ir1 94.29(14) . 2_755 ? C6 Ir1 Ir1 136.49(11) . 2_755 ? C3 Ir1 Ir1 140.10(12) . 2_755 ? C5 Ir1 Ir1 110.38(11) . 2_755 ? C4 Ir1 Ir1 111.75(11) . 2_755 ? C2 Ir1 Ir1 174.29(11) . 2_755 ? C1 Ir1 H1A 89.8 . . ? C6 Ir1 H1A 98.9 . . ? C3 Ir1 H1A 157.5 . . ? C5 Ir1 H1A 94.7 . . ? C4 Ir1 H1A 122.5 . . ? C2 Ir1 H1A 134.0 . . ? Ir1 Ir1 H1A 44.5 2_755 . ? O1 C1 Ir1 174.5(4) . . ? C7 C2 C3 129.8(4) . . ? C7 C2 C6 126.5(4) . . ? C3 C2 C6 103.8(4) . . ? C7 C2 Ir1 126.8(3) . . ? C3 C2 Ir1 68.0(3) . . ? C6 C2 Ir1 67.5(2) . . ? C4 C3 C2 110.4(4) . . ? C4 C3 C8 124.5(4) . . ? C2 C3 C8 123.9(4) . . ? C4 C3 Ir1 73.2(2) . . ? C2 C3 Ir1 73.9(3) . . ? C8 C3 Ir1 129.6(3) . . ? C5 C4 C3 107.9(4) . . ? C5 C4 C9 126.7(4) . . ? C3 C4 C9 125.3(4) . . ? C5 C4 Ir1 71.6(2) . . ? C3 C4 Ir1 68.8(2) . . ? C9 C4 Ir1 128.2(3) . . ? C4 C5 C6 108.7(4) . . ? C4 C5 C10 127.0(4) . . ? C6 C5 C10 124.2(4) . . ? C4 C5 Ir1 71.8(2) . . ? C6 C5 Ir1 68.8(2) . . ? C10 C5 Ir1 128.2(3) . . ? C5 C6 C11 126.2(4) . . ? C5 C6 C2 108.9(3) . . ? C11 C6 C2 124.1(4) . . ? C5 C6 Ir1 73.2(2) . . ? C11 C6 Ir1 127.8(3) . . ? C2 C6 Ir1 73.4(2) . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C17 C12 C13 113.8(4) . . ? C17 C12 B1 126.9(4) . . ? C13 C12 B1 119.0(4) . . ? F1 C13 C14 116.3(4) . . ? F1 C13 C12 119.0(4) . . ? C14 C13 C12 124.8(4) . . ? F2 C14 C13 121.7(4) . . ? F2 C14 C15 119.5(4) . . ? C13 C14 C15 118.7(4) . . ? F3 C15 C14 120.9(4) . . ? F3 C15 C16 119.7(4) . . ? C14 C15 C16 119.4(4) . . ? F4 C16 C17 121.7(4) . . ? F4 C16 C15 119.1(4) . . ? C17 C16 C15 119.1(4) . . ? F5 C17 C16 113.8(4) . . ? F5 C17 C12 122.0(4) . . ? C16 C17 C12 124.1(4) . . ? C23 C18 C19 113.1(4) . . ? C23 C18 B1 118.4(4) . . ? C19 C18 B1 128.3(3) . . ? F6 C19 C20 114.8(4) . . ? F6 C19 C18 121.3(4) . . ? C20 C19 C18 123.9(4) . . ? F7 C20 C21 119.3(4) . . ? F7 C20 C19 120.7(4) . . ? C21 C20 C19 120.0(4) . . ? F8 C21 C22 121.1(4) . . ? F8 C21 C20 120.5(4) . . ? C22 C21 C20 118.3(4) . . ? F9 C22 C21 119.5(4) . . ? F9 C22 C23 120.7(4) . . ? C21 C22 C23 119.8(4) . . ? F10 C23 C22 116.2(4) . . ? F10 C23 C18 119.0(4) . . ? C22 C23 C18 124.9(4) . . ? C29 C24 C25 113.9(4) . . ? C29 C24 B1 119.4(4) . . ? C25 C24 B1 126.3(4) . . ? F11 C25 C26 115.3(4) . . ? F11 C25 C24 121.6(3) . . ? C26 C25 C24 123.1(4) . . ? F12 C26 C27 119.6(4) . . ? F12 C26 C25 119.9(4) . . ? C27 C26 C25 120.4(4) . . ? F13 C27 C26 119.7(4) . . ? F13 C27 C28 121.3(4) . . ? C26 C27 C28 119.0(4) . . ? F14 C28 C27 119.8(4) . . ? F14 C28 C29 121.2(4) . . ? C27 C28 C29 119.0(4) . . ? F15 C29 C24 119.7(4) . . ? F15 C29 C28 115.8(4) . . ? C24 C29 C28 124.5(4) . . ? C31 C30 C35 113.3(4) . . ? C31 C30 B1 128.0(4) . . ? C35 C30 B1 118.5(4) . . ? F16 C31 C32 114.7(4) . . ? F16 C31 C30 120.5(4) . . ? C32 C31 C30 124.8(4) . . ? F17 C32 C33 120.2(4) . . ? F17 C32 C31 120.6(4) . . ? C33 C32 C31 119.2(4) . . ? F18 C33 C32 120.9(4) . . ? F18 C33 C34 120.1(4) . . ? C32 C33 C34 119.0(4) . . ? F19 C34 C33 119.1(4) . . ? F19 C34 C35 120.8(4) . . ? C33 C34 C35 120.1(4) . . ? F20 C35 C34 116.5(4) . . ? F20 C35 C30 120.0(4) . . ? C34 C35 C30 123.6(4) . . ? C30 B1 C18 101.9(3) . . ? C30 B1 C12 111.9(3) . . ? C18 B1 C12 113.8(3) . . ? C30 B1 C24 113.7(3) . . ? C18 B1 C24 113.5(3) . . ? C12 B1 C24 102.5(3) . . ? _diffrn_measured_fraction_theta_max 0.884 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.430 _refine_diff_density_min -3.589 _refine_diff_density_rms 0.204 #===END data_shelxl_14 _publ_contact_author_name 'Werner Kaminsky' _publ_contact_author_address ; Department of Chemistry, BOX 351700 University of Washington Seattle, WA 98195 USA ; _publ_contact_author_email 'wernerka@u.washington.edu' _publ_requested_journal 'Journal title here' _publ_section_title ; title here ; loop_ _publ_author_name _publ_author_address 'Joe Meredith' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'Werner Kaminsky' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; 'Mike Heinekey' ; Department of Chemistry Univ. of Washington Seattle, WA 98195 USA ; _publ_section_abstract ; Abstract here ; _publ_section_comment ; Details and comments here ; _publ_section_exptl_prep ; details of preparation here ; _publ_section_exptl_refinement ; All H atoms were initially located in a difference Fourier map and were refined with a riding model. H atoms were placed in geometrically idealised positions and constrained to ride on their parent atoms with C---H distances in the range 0.95-1.00 \%A. U~iso~ values were fixed such that they were 1.2U~eq~ of their parent atom U~eq~ for CH's and 1.5U~eq~ of their parent atom U~eq~ in case of methyl groups. ; _publ_section_references ; Altomare, A.; Cascarano, G.; Giacovazzo, C.; Burla, M.C.; Polidori, G.; Camalli, M. (1994) J. Appl. Cryst. 27, 435-442. Beurskens, P.T., Admiraal, G., Beurskens, G., Bosman, W. P., Garcia-Granada, S., Gould, R. O., Smits, J. M. M. & Smykalla, C. (1996) The DIRDIF96 Program System. Technical Report of the Crystallography Laboratory, University of Nijmegen, The Netherlands. MacKay, S.; Gilmore, C.J.; Edwards, C.; Tremayne, M.; Stewart, N.; Shankland, K. (1998) "maXus: a computer program for the solution and refinement of crystal structures from diffraction data" University of Glasgow, Scotland, UK, Nonius BV, Delft, The Netherlands and MacScience Co. Ltd., Yokohama, Japan. Otwinowski, Z.; Minor, W. (1996) Methods in Enzymology, 276, 307-326. Sheldrick, G. M. (1997) SHELXL97 University of G\"ottingen, Germany. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; 'JMM01047' ; _chemical_name_common 'JMM01047' _chemical_melting_point ? _chemical_formula_moiety 'C20 H32 Cl2 Ir2' _chemical_formula_sum 'C20 H32 Cl2 Ir2' _chemical_formula_weight 727.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ir' 'Ir' -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.2699(7) _cell_length_b 14.969(2) _cell_length_c 10.4680(13) _cell_angle_alpha 90.00 _cell_angle_beta 114.200(7) _cell_angle_gamma 90.00 _cell_volume 1039.1(2) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 228 _cell_measurement_theta_min 3 _cell_measurement_theta_max 20 _exptl_crystal_description 'cut block' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.326 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_absorpt_coefficient_mu 13.052 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.175 _exptl_absorpt_correction_T_max 0.212 _exptl_absorpt_process_details 'HKL2008' _exptl_special_details ; Data was collected with \w and \f scans in 2^o^ increments with 10 second exposures per degree. Crystal-to-detector distance was 30 mm. 19465 full and partial reflection were integrated. ; _diffrn_ambient_temperature 130(2) _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 'Nonius KappaCCD' _diffrn_measurement_method '\f and \w scans' _diffrn_reflns_number 3885 _diffrn_reflns_av_R_equivalents 0.0661 _diffrn_reflns_av_sigmaI/netI 0.0892 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.07 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2072 _reflns_number_gt 1459 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'KappaCCD' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SIR97' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'maXus, Zortep' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0255P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2072 _refine_ls_number_parameters 120 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0808 _refine_ls_wR_factor_gt 0.0726 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _refine_ls_shift/su_max 0.045 _refine_ls_shift/su_mean 0.002 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 Ir1 Ir 0.59028(5) 0.06459(2) 0.59753(4) 0.0335(6) Uani 1 1 d . . . H1 H 0.624(11) 0.017(5) 0.436(8) 0.03(2) Uiso 1 1 d . . . Cl1 Cl 0.3467(3) 0.17268(15) 0.4619(2) 0.0432(8) Uani 1 1 d . . . C1 C 0.7422(12) 0.1649(5) 0.7603(9) 0.037(2) Uani 1 1 d . . . C2 C 0.8765(12) 0.1332(6) 0.7047(9) 0.038(2) Uani 1 1 d . . . C3 C 0.9024(12) 0.0383(6) 0.7304(10) 0.042(2) Uani 1 1 d . . . C4 C 0.7778(13) 0.0139(5) 0.8036(9) 0.036(2) Uani 1 1 d . . . C5 C 0.6749(13) 0.0932(6) 0.8176(10) 0.041(2) Uani 1 1 d . . . C6 C 0.6789(14) 0.2613(6) 0.7574(11) 0.050(3) Uani 1 1 d . . . H6A H 0.7899 0.2955 0.8268 0.060 Uiso 1 1 calc R . . H6B H 0.5606 0.2646 0.7797 0.060 Uiso 1 1 calc R . . H6C H 0.6452 0.2862 0.6639 0.060 Uiso 1 1 calc R . . C7 C 0.9879(13) 0.1898(7) 0.6411(10) 0.049(2) Uani 1 1 d . . . H7A H 1.1096 0.2143 0.7157 0.059 Uiso 1 1 calc R . . H7B H 0.9008 0.2388 0.5881 0.059 Uiso 1 1 calc R . . H7C H 1.0258 0.1531 0.5782 0.059 Uiso 1 1 calc R . . C8 C 1.0446(13) -0.0228(7) 0.7020(11) 0.051(3) Uani 1 1 d . . . H8A H 1.1723 -0.0260 0.7853 0.062 Uiso 1 1 calc R . . H8B H 1.0694 0.0003 0.6229 0.062 Uiso 1 1 calc R . . H8C H 0.9850 -0.0826 0.6794 0.062 Uiso 1 1 calc R . . C9 C 0.7711(13) -0.0746(5) 0.8564(12) 0.059(3) Uani 1 1 d . . . H9A H 0.8758 -0.0802 0.9518 0.070 Uiso 1 1 calc R . . H9B H 0.7944 -0.1190 0.7959 0.070 Uiso 1 1 calc R . . H9C H 0.6385 -0.0847 0.8574 0.070 Uiso 1 1 calc R . . C10 C 0.5442(14) 0.0990(7) 0.8956(10) 0.046(2) Uani 1 1 d . . . H10A H 0.6285 0.0994 0.9965 0.055 Uiso 1 1 calc R . . H10B H 0.4536 0.0472 0.8724 0.055 Uiso 1 1 calc R . . H10C H 0.4642 0.1540 0.8694 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.0340(6) 0.0340(6) 0.0312(6) 0.00060(17) 0.0122(3) -0.00078(16) Cl1 0.0420(13) 0.0380(13) 0.0422(15) 0.0000(10) 0.0100(10) 0.0060(9) C1 0.039(5) 0.028(4) 0.034(5) 0.001(4) 0.006(4) -0.002(4) C2 0.038(5) 0.050(5) 0.022(5) 0.003(4) 0.008(4) -0.010(4) C3 0.029(4) 0.043(5) 0.040(6) 0.000(4) 0.001(4) 0.002(4) C4 0.039(4) 0.029(4) 0.031(5) -0.002(4) 0.007(4) -0.006(4) C5 0.041(5) 0.045(5) 0.039(6) -0.002(4) 0.018(4) -0.001(4) C6 0.052(6) 0.035(5) 0.060(7) 0.005(5) 0.019(5) 0.001(4) C7 0.047(5) 0.060(6) 0.038(6) -0.004(5) 0.016(4) -0.012(5) C8 0.036(5) 0.057(6) 0.059(7) -0.014(5) 0.018(5) 0.003(4) C9 0.029(4) 0.026(5) 0.092(9) -0.023(5) -0.003(5) -0.001(4) C10 0.046(5) 0.056(6) 0.036(6) -0.003(5) 0.018(4) -0.004(4) _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 Ir1 C3 2.156(8) . ? Ir1 C4 2.162(8) . ? Ir1 C5 2.170(10) . ? Ir1 C2 2.174(8) . ? Ir1 C1 2.198(8) . ? Ir1 Cl1 2.389(2) . ? Ir1 Ir1 2.7265(7) 3_656 ? Ir1 H1 1.94(8) . ? C1 C2 1.408(13) . ? C1 C5 1.411(12) . ? C1 C6 1.511(12) . ? C2 C3 1.443(13) . ? C2 C7 1.503(12) . ? C3 C4 1.453(14) . ? C3 C8 1.498(12) . ? C4 C5 1.442(12) . ? C4 C9 1.444(12) . ? C5 C10 1.488(13) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 C3 Ir1 C4 39.3(4) . . ? C3 Ir1 C5 65.5(4) . . ? C4 Ir1 C5 38.9(3) . . ? C3 Ir1 C2 38.9(3) . . ? C4 Ir1 C2 64.7(3) . . ? C5 Ir1 C2 64.1(3) . . ? C3 Ir1 C1 64.1(3) . . ? C4 Ir1 C1 63.6(3) . . ? C5 Ir1 C1 37.7(3) . . ? C2 Ir1 C1 37.6(3) . . ? C3 Ir1 Cl1 146.5(3) . . ? C4 Ir1 Cl1 147.2(3) . . ? C5 Ir1 Cl1 108.4(2) . . ? C2 Ir1 Cl1 107.8(2) . . ? C1 Ir1 Cl1 90.7(2) . . ? C3 Ir1 Ir1 114.2(2) . 3_656 ? C4 Ir1 Ir1 114.3(2) . 3_656 ? C5 Ir1 Ir1 140.8(2) . 3_656 ? C2 Ir1 Ir1 141.9(3) . 3_656 ? C1 Ir1 Ir1 177.9(2) . 3_656 ? Cl1 Ir1 Ir1 91.34(6) . 3_656 ? C3 Ir1 H1 91(2) . . ? C4 Ir1 H1 119(2) . . ? C5 Ir1 H1 156(2) . . ? C2 Ir1 H1 101(2) . . ? C1 Ir1 H1 136(2) . . ? Cl1 Ir1 H1 93(2) . . ? Ir1 Ir1 H1 44(2) 3_656 . ? C2 C1 C5 109.8(8) . . ? C2 C1 C6 124.8(8) . . ? C5 C1 C6 125.3(9) . . ? C2 C1 Ir1 70.3(5) . . ? C5 C1 Ir1 70.1(5) . . ? C6 C1 Ir1 125.8(6) . . ? C1 C2 C3 108.3(8) . . ? C1 C2 C7 125.7(9) . . ? C3 C2 C7 125.8(9) . . ? C1 C2 Ir1 72.1(5) . . ? C3 C2 Ir1 69.9(5) . . ? C7 C2 Ir1 127.8(6) . . ? C2 C3 C4 106.5(8) . . ? C2 C3 C8 127.7(9) . . ? C4 C3 C8 125.5(8) . . ? C2 C3 Ir1 71.2(5) . . ? C4 C3 Ir1 70.6(5) . . ? C8 C3 Ir1 127.8(7) . . ? C5 C4 C9 128.0(9) . . ? C5 C4 C3 107.9(7) . . ? C9 C4 C3 124.0(9) . . ? C5 C4 Ir1 70.8(5) . . ? C9 C4 Ir1 126.7(6) . . ? C3 C4 Ir1 70.1(5) . . ? C1 C5 C4 107.3(8) . . ? C1 C5 C10 126.9(9) . . ? C4 C5 C10 125.3(9) . . ? C1 C5 Ir1 72.2(5) . . ? C4 C5 Ir1 70.3(5) . . ? C10 C5 Ir1 128.8(6) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.169 _refine_diff_density_min -0.463 _refine_diff_density_rms 0.088 #===END