# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cmpnd_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H47 Ir2 N P2' _chemical_formula_sum 'C40 H47 Ir2 N P2' _chemical_formula_weight 988.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Ir Ir -1.4440 7.9890 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.8643(12) _cell_length_b 29.946(3) _cell_length_c 11.1359(13) _cell_angle_alpha 90.00 _cell_angle_beta 107.334(2) _cell_angle_gamma 90.00 _cell_volume 3458.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9928 _cell_measurement_theta_min 2.349 _cell_measurement_theta_max 29.333 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.148 _exptl_crystal_size_mid 0.141 _exptl_crystal_size_min 0.134 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 7.810 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3173 _exptl_absorpt_correction_T_max 0.4607 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX DUO CCD system' _diffrn_measurement_method 'narrow \w frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 44776 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 29.50 _reflns_number_total 9093 _reflns_number_gt 7517 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, PLATON(Spek, 1998)' _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. Hydrogen atoms of phenyl groups and those bounded to non-olefinic carbon atoms of cod fragments have been included in the model in calculated positions and refined with a riding model. Hydrogen atoms bounded to the olefinic carbon atoms of the cod fragments have been included in observed positions and refined with their isotropic thermal parameters equal to 1.2 those of the Uiso of their parent carbon atoms. One restraint in a C-H distance has been used in the refinement. Hydride atom has been observed in Fourier difference maps. It has been included in the model in this observed position and refined with a restraint in Ir-H distance. At the end of the refinement, nine residual density peaks higher than 1eA^3^ were found. All of them are close to the metal atoms (Ir-Q distance around 0.9 A). They have no chemical sense. ; _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^)+(0.0245P)^2^+6.4701P] 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 9093 _refine_ls_number_parameters 442 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0282 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl223ds in P 21/n CELL 0.71073 10.8643 29.9462 11.1359 90.000 107.334 90.000 ZERR 4.00 0.0012 0.0034 0.0013 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 = 0.86500 51.65125 0.21560 0.003 0.002 11.500 0.770 12.011 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 = 0.04081 57.79977 0.00304 0.000 0.000 0.620 0.320 1.008 SFAC IR 27.30493 1.59279 16.72961 8.86554 15.61152 0.41792 = 5.83378 45.00114 11.47221 -1.444 7.989 33100.000 1.350 192.217 SFAC N 12.21261 0.00570 3.13220 9.89331 2.01250 28.99754 = 1.16630 0.58260 -11.52901 0.006 0.003 19.600 0.700 14.007 SFAC P 6.43451 1.90670 4.17910 27.15704 1.78000 0.52600 = 1.49080 68.16457 1.11490 0.102 0.094 410.000 1.100 30.974 UNIT 160 188 8 4 8 MERG 2 DFIX 1.650 0.020 IR1 H DFIX 0.960 0.020 C14 H14 FMAP 2 PLAN 15 ACTA 55 BOND $H CONF WPDB -2 L.S. 4 TEMP -173.00 WGHT 0.024500 6.470100 FVAR 0.13553 IR1 3 0.191251 0.113188 0.932787 11.00000 0.01352 0.01638 = 0.01204 0.00070 0.00312 -0.00132 IR2 3 0.491155 0.101397 1.111696 11.00000 0.01343 0.01731 = 0.01278 0.00014 0.00344 0.00045 P1 5 0.387710 0.148085 0.932825 11.00000 0.01624 0.01712 = 0.01320 0.00052 0.00482 -0.00197 P2 5 0.297320 0.127996 1.147556 11.00000 0.01435 0.01752 = 0.01242 0.00033 0.00320 0.00076 N 4 0.341716 0.062786 0.987793 11.00000 0.02217 0.01133 = 0.01647 -0.00082 0.00423 -0.00099 C1 1 0.065190 0.120072 0.733773 11.00000 0.02926 0.02755 = 0.01297 0.00222 0.00182 -0.00515 H1 2 0.085378 0.146975 0.702736 11.00000 -1.20000 C2 1 0.141778 0.082794 0.741914 11.00000 0.02168 0.02896 = 0.01027 -0.00291 0.00489 -0.00455 H2 2 0.216280 0.087148 0.712882 11.00000 -1.20000 C3 1 0.098646 0.035247 0.749472 11.00000 0.03353 0.02782 = 0.02601 -0.00773 0.01318 -0.00949 AFIX 23 H3A 2 0.175716 0.015744 0.772996 11.00000 -1.20000 H3B 2 0.044466 0.025938 0.664941 11.00000 -1.20000 AFIX 0 C4 1 0.022722 0.027769 0.843155 11.00000 0.03155 0.02153 = 0.02642 -0.00406 0.01126 -0.00713 AFIX 23 H4A 2 -0.070302 0.031532 0.798915 11.00000 -1.20000 H4B 2 0.036198 -0.003372 0.874152 11.00000 -1.20000 AFIX 0 C5 1 0.060128 0.059138 0.954807 11.00000 0.01925 0.02291 = 0.01552 -0.00034 0.00583 -0.00755 H5 2 0.098383 0.046455 1.030712 11.00000 -1.20000 C6 1 -0.000795 0.099695 0.957521 11.00000 0.01722 0.02499 = 0.02243 0.00151 0.00737 -0.00533 H6 2 0.001244 0.112477 1.031335 11.00000 -1.20000 C7 1 -0.106937 0.118640 0.850249 11.00000 0.01456 0.03323 = 0.03187 0.00733 0.00497 0.00034 AFIX 23 H7A 2 -0.123173 0.149860 0.870553 11.00000 -1.20000 H7B 2 -0.186816 0.101398 0.841842 11.00000 -1.20000 AFIX 0 C8 1 -0.077811 0.117977 0.724042 11.00000 0.02137 0.03364 = 0.03009 0.00275 -0.00124 -0.00042 AFIX 23 H8A 2 -0.114662 0.090364 0.678516 11.00000 -1.20000 H8B 2 -0.122010 0.143628 0.673104 11.00000 -1.20000 AFIX 0 C9 1 0.636648 0.057371 1.096607 11.00000 0.01950 0.02043 = 0.02361 0.00105 0.00959 0.00562 H9 2 0.609956 0.040982 1.017355 11.00000 -1.20000 C10 1 0.581595 0.041837 1.193732 11.00000 0.01759 0.01970 = 0.02335 0.00185 0.00601 0.00207 H10 2 0.531283 0.015851 1.174953 11.00000 -1.20000 C11 1 0.652068 0.044435 1.333363 11.00000 0.02450 0.03975 = 0.01992 0.00679 0.00580 0.00750 AFIX 23 H11A 2 0.592121 0.036542 1.381788 11.00000 -1.20000 H11B 2 0.723765 0.022609 1.354716 11.00000 -1.20000 AFIX 0 C12 1 0.705131 0.090946 1.369790 11.00000 0.01733 0.04592 = 0.01912 -0.00045 0.00259 0.00304 AFIX 23 H12A 2 0.794557 0.092550 1.364980 11.00000 -1.20000 H12B 2 0.707436 0.097095 1.457784 11.00000 -1.20000 AFIX 0 C13 1 0.622581 0.126526 1.283091 11.00000 0.01428 0.03312 = 0.01695 -0.00888 -0.00220 -0.00083 H13 2 0.575225 0.146022 1.321239 11.00000 -1.20000 C14 1 0.653851 0.145323 1.180312 11.00000 0.01703 0.02629 = 0.02428 -0.00574 0.00341 -0.00239 H14 2 0.621343 0.174649 1.161899 11.00000 -1.20000 C15 1 0.764227 0.129637 1.135231 11.00000 0.01566 0.03138 = 0.02625 0.00168 0.00418 -0.00232 AFIX 23 H15A 2 0.846174 0.140424 1.194232 11.00000 -1.20000 H15B 2 0.755671 0.143014 1.051837 11.00000 -1.20000 AFIX 0 C16 1 0.770350 0.078371 1.124599 11.00000 0.01720 0.03494 = 0.02374 0.00019 0.00853 0.00425 AFIX 23 H16A 2 0.808019 0.070550 1.056615 11.00000 -1.20000 H16B 2 0.827224 0.066065 1.204398 11.00000 -1.20000 AFIX 0 C17 1 0.396613 0.209236 0.938506 11.00000 0.02565 0.02102 = 0.01460 0.00246 0.00706 -0.00405 C18 1 0.516986 0.228464 0.950915 11.00000 0.03212 0.02350 = 0.02234 0.00013 0.00733 -0.00629 AFIX 43 H18 2 0.588717 0.209836 0.954280 11.00000 -1.20000 AFIX 0 C19 1 0.532987 0.274736 0.958420 11.00000 0.04625 0.02789 = 0.02830 0.00154 0.00682 -0.01694 AFIX 43 H19 2 0.614970 0.287630 0.966569 11.00000 -1.20000 AFIX 0 C20 1 0.428335 0.301542 0.953864 11.00000 0.06097 0.01524 = 0.03137 0.00116 0.01230 -0.00957 AFIX 43 H20 2 0.438436 0.333064 0.958658 11.00000 -1.20000 AFIX 0 C21 1 0.309270 0.282960 0.942414 11.00000 0.04928 0.02092 = 0.03020 0.00568 0.01252 0.00974 AFIX 43 H21 2 0.238163 0.301656 0.940842 11.00000 -1.20000 AFIX 0 C22 1 0.293142 0.236982 0.933183 11.00000 0.03028 0.02617 = 0.01879 0.00563 0.00705 0.00097 AFIX 43 H22 2 0.210368 0.224430 0.923120 11.00000 -1.20000 AFIX 0 C23 1 0.425651 0.137952 0.785813 11.00000 0.01972 0.02373 = 0.01625 -0.00063 0.00733 -0.00416 C24 1 0.507781 0.103166 0.777801 11.00000 0.02319 0.03564 = 0.02417 -0.00162 0.00796 0.00217 AFIX 43 H24 2 0.550652 0.086598 0.851078 11.00000 -1.20000 AFIX 0 C25 1 0.527818 0.092356 0.662607 11.00000 0.03515 0.04840 = 0.03506 -0.00727 0.01636 0.00486 AFIX 43 H25 2 0.581139 0.067775 0.657075 11.00000 -1.20000 AFIX 0 C26 1 0.469406 0.117728 0.556664 11.00000 0.02918 0.05589 = 0.02171 -0.01103 0.01316 -0.00709 AFIX 43 H26 2 0.483934 0.110780 0.478755 11.00000 -1.20000 AFIX 0 C27 1 0.390286 0.153015 0.564071 11.00000 0.03224 0.04194 = 0.01656 0.00021 0.00412 -0.01418 AFIX 43 H27 2 0.351196 0.170530 0.491601 11.00000 -1.20000 AFIX 0 C28 1 0.368060 0.162812 0.676792 11.00000 0.02530 0.02416 = 0.02097 0.00218 0.00840 -0.00607 AFIX 43 H28 2 0.312543 0.186919 0.680703 11.00000 -1.20000 AFIX 0 C29 1 0.266630 0.185625 1.187231 11.00000 0.02556 0.01656 = 0.01746 0.00052 0.00849 -0.00147 C30 1 0.367804 0.213128 1.249939 11.00000 0.02414 0.02560 = 0.02676 0.00066 0.00585 0.00023 AFIX 43 H30 2 0.453292 0.201732 1.275127 11.00000 -1.20000 AFIX 0 C31 1 0.345605 0.257302 1.276477 11.00000 0.03826 0.02267 = 0.03553 -0.00432 0.00627 -0.00693 AFIX 43 H31 2 0.415896 0.275794 1.319705 11.00000 -1.20000 AFIX 0 C32 1 0.221486 0.274435 1.240150 11.00000 0.04504 0.01653 = 0.04213 -0.00554 0.01638 0.00227 AFIX 43 H32 2 0.206435 0.304531 1.258822 11.00000 -1.20000 AFIX 0 C33 1 0.120268 0.247586 1.176903 11.00000 0.03021 0.02677 = 0.03561 0.00195 0.01278 0.00780 AFIX 43 H33 2 0.034994 0.259170 1.151431 11.00000 -1.20000 AFIX 0 C34 1 0.142541 0.203550 1.150209 11.00000 0.02381 0.02154 = 0.02585 -0.00046 0.00924 0.00173 AFIX 43 H34 2 0.072027 0.185327 1.105967 11.00000 -1.20000 AFIX 0 C35 1 0.234825 0.094696 1.256166 11.00000 0.01394 0.02405 = 0.01077 -0.00146 -0.00050 -0.00180 C36 1 0.140827 0.109397 1.309255 11.00000 0.02295 0.02455 = 0.01823 -0.00115 0.00489 0.00277 AFIX 43 H36 2 0.102532 0.137932 1.287278 11.00000 -1.20000 AFIX 0 C37 1 0.102411 0.082651 1.394301 11.00000 0.01844 0.03272 = 0.02123 -0.00133 0.00871 -0.00046 AFIX 43 H37 2 0.038024 0.092901 1.429643 11.00000 -1.20000 AFIX 0 C38 1 0.157843 0.041581 1.426635 11.00000 0.02677 0.02957 = 0.02021 0.00539 0.00997 -0.00562 AFIX 43 H38 2 0.132638 0.023525 1.485409 11.00000 -1.20000 AFIX 0 C39 1 0.250802 0.026204 1.373843 11.00000 0.03392 0.01879 = 0.01827 0.00393 0.00596 0.00237 AFIX 43 H39 2 0.288177 -0.002473 1.395626 11.00000 -1.20000 AFIX 0 C40 1 0.288477 0.052465 1.290321 11.00000 0.02263 0.02342 = 0.01599 -0.00045 0.00432 0.00248 AFIX 43 H40 2 0.352338 0.041742 1.254948 11.00000 -1.20000 AFIX 0 H 2 0.129104 0.162214 0.925526 11.00000 0.03275 H1N 2 0.358780 0.051989 0.923011 11.00000 0.02689 H2N 2 0.315838 0.035500 1.015395 11.00000 0.04738 HKLF 4 REM fjl223ds in P 21/n REM R1 = 0.0282 for 7517 Fo > 4sig(Fo) and 0.0414 for all 9093 data REM 442 parameters refined using 2 restraints END ; 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 0.191251(14) 0.113188(5) 0.932787(14) 0.01413(4) Uani 1 1 d D . . Ir2 Ir 0.491155(14) 0.101397(5) 1.111696(14) 0.01461(4) Uani 1 1 d . . . P1 P 0.38771(10) 0.14809(3) 0.93283(9) 0.0154(2) Uani 1 1 d . . . P2 P 0.29732(10) 0.12800(3) 1.14756(9) 0.0149(2) Uani 1 1 d . . . N N 0.3417(3) 0.06279(12) 0.9878(3) 0.0170(7) Uani 1 1 d . . . C1 C 0.0652(4) 0.12007(16) 0.7338(4) 0.0242(9) Uani 1 1 d . . . H1 H 0.085(5) 0.1470(17) 0.703(5) 0.029 Uiso 1 1 d . . . C2 C 0.1418(4) 0.08279(15) 0.7419(4) 0.0203(9) Uani 1 1 d . . . H2 H 0.216(5) 0.0871(15) 0.713(4) 0.024 Uiso 1 1 d . . . C3 C 0.0986(5) 0.03525(15) 0.7495(4) 0.0282(10) Uani 1 1 d . . . H3A H 0.1757 0.0157 0.7730 0.034 Uiso 1 1 calc R . . H3B H 0.0445 0.0259 0.6649 0.034 Uiso 1 1 calc R . . C4 C 0.0227(5) 0.02777(15) 0.8432(4) 0.0259(10) Uani 1 1 d . . . H4A H -0.0703 0.0315 0.7989 0.031 Uiso 1 1 calc R . . H4B H 0.0362 -0.0034 0.8742 0.031 Uiso 1 1 calc R . . C5 C 0.0601(4) 0.05914(14) 0.9548(4) 0.0191(8) Uani 1 1 d . . . H5 H 0.098(4) 0.0465(15) 1.031(5) 0.023 Uiso 1 1 d . . . C6 C -0.0008(4) 0.09970(15) 0.9575(4) 0.0212(9) Uani 1 1 d . . . H6 H 0.001(5) 0.1125(15) 1.031(5) 0.025 Uiso 1 1 d . . . C7 C -0.1069(4) 0.11864(16) 0.8502(4) 0.0270(10) Uani 1 1 d . . . H7A H -0.1232 0.1499 0.8706 0.032 Uiso 1 1 calc R . . H7B H -0.1868 0.1014 0.8418 0.032 Uiso 1 1 calc R . . C8 C -0.0778(4) 0.11798(17) 0.7240(5) 0.0303(10) Uani 1 1 d . . . H8A H -0.1147 0.0904 0.6785 0.036 Uiso 1 1 calc R . . H8B H -0.1220 0.1436 0.6731 0.036 Uiso 1 1 calc R . . C9 C 0.6366(4) 0.05737(14) 1.0966(4) 0.0205(9) Uani 1 1 d . . . H9 H 0.610(4) 0.0410(15) 1.017(5) 0.025 Uiso 1 1 d . . . C10 C 0.5816(4) 0.04184(15) 1.1937(4) 0.0202(8) Uani 1 1 d . . . H10 H 0.531(5) 0.0159(16) 1.175(4) 0.024 Uiso 1 1 d . . . C11 C 0.6521(4) 0.04443(16) 1.3334(4) 0.0282(10) Uani 1 1 d . . . H11A H 0.5921 0.0365 1.3818 0.034 Uiso 1 1 calc R . . H11B H 0.7238 0.0226 1.3547 0.034 Uiso 1 1 calc R . . C12 C 0.7051(4) 0.09095(17) 1.3698(4) 0.0281(10) Uani 1 1 d . . . H12A H 0.7946 0.0926 1.3650 0.034 Uiso 1 1 calc R . . H12B H 0.7074 0.0971 1.4578 0.034 Uiso 1 1 calc R . . C13 C 0.6226(4) 0.12653(16) 1.2831(4) 0.0229(9) Uani 1 1 d . . . H13 H 0.575(5) 0.1460(16) 1.321(5) 0.028 Uiso 1 1 d . . . C14 C 0.6539(4) 0.14532(15) 1.1803(4) 0.0231(9) Uani 1 1 d D . . H14 H 0.621(4) 0.1746(9) 1.162(4) 0.028 Uiso 1 1 d D . . C15 C 0.7642(4) 0.12964(15) 1.1352(4) 0.0249(9) Uani 1 1 d . . . H15A H 0.8462 0.1404 1.1942 0.030 Uiso 1 1 calc R . . H15B H 0.7557 0.1430 1.0518 0.030 Uiso 1 1 calc R . . C16 C 0.7703(4) 0.07837(15) 1.1246(4) 0.0248(9) Uani 1 1 d . . . H16A H 0.8080 0.0706 1.0566 0.030 Uiso 1 1 calc R . . H16B H 0.8272 0.0661 1.2044 0.030 Uiso 1 1 calc R . . C17 C 0.3966(4) 0.20924(14) 0.9385(4) 0.0202(9) Uani 1 1 d . . . C18 C 0.5170(5) 0.22846(15) 0.9509(4) 0.0262(10) Uani 1 1 d . . . H18 H 0.5887 0.2098 0.9543 0.031 Uiso 1 1 calc R . . C19 C 0.5330(5) 0.27474(16) 0.9584(5) 0.0351(12) Uani 1 1 d . . . H19 H 0.6150 0.2876 0.9666 0.042 Uiso 1 1 calc R . . C20 C 0.4283(6) 0.30154(16) 0.9539(5) 0.0362(12) Uani 1 1 d . . . H20 H 0.4384 0.3331 0.9587 0.043 Uiso 1 1 calc R . . C21 C 0.3093(5) 0.28296(16) 0.9424(5) 0.0333(11) Uani 1 1 d . . . H21 H 0.2382 0.3017 0.9408 0.040 Uiso 1 1 calc R . . C22 C 0.2931(5) 0.23698(15) 0.9332(4) 0.0251(9) Uani 1 1 d . . . H22 H 0.2104 0.2244 0.9231 0.030 Uiso 1 1 calc R . . C23 C 0.4257(4) 0.13795(14) 0.7858(4) 0.0195(8) Uani 1 1 d . . . C24 C 0.5078(4) 0.10317(16) 0.7778(4) 0.0275(10) Uani 1 1 d . . . H24 H 0.5507 0.0866 0.8511 0.033 Uiso 1 1 calc R . . C25 C 0.5278(5) 0.09236(19) 0.6626(5) 0.0382(12) Uani 1 1 d . . . H25 H 0.5811 0.0678 0.6571 0.046 Uiso 1 1 calc R . . C26 C 0.4694(5) 0.11773(18) 0.5567(4) 0.0344(12) Uani 1 1 d . . . H26 H 0.4839 0.1108 0.4788 0.041 Uiso 1 1 calc R . . C27 C 0.3903(5) 0.15302(17) 0.5641(4) 0.0309(11) Uani 1 1 d . . . H27 H 0.3512 0.1705 0.4916 0.037 Uiso 1 1 calc R . . C28 C 0.3681(4) 0.16281(15) 0.6768(4) 0.0231(9) Uani 1 1 d . . . H28 H 0.3125 0.1869 0.6807 0.028 Uiso 1 1 calc R . . C29 C 0.2666(4) 0.18562(14) 1.1872(4) 0.0194(8) Uani 1 1 d . . . C30 C 0.3678(4) 0.21313(15) 1.2499(4) 0.0259(10) Uani 1 1 d . . . H30 H 0.4533 0.2017 1.2751 0.031 Uiso 1 1 calc R . . C31 C 0.3456(5) 0.25730(16) 1.2765(5) 0.0332(11) Uani 1 1 d . . . H31 H 0.4159 0.2758 1.3197 0.040 Uiso 1 1 calc R . . C32 C 0.2215(5) 0.27443(16) 1.2401(5) 0.0338(11) Uani 1 1 d . . . H32 H 0.2064 0.3045 1.2588 0.041 Uiso 1 1 calc R . . C33 C 0.1203(5) 0.24759(16) 1.1769(5) 0.0302(10) Uani 1 1 d . . . H33 H 0.0350 0.2592 1.1514 0.036 Uiso 1 1 calc R . . C34 C 0.1425(4) 0.20355(14) 1.1502(4) 0.0233(9) Uani 1 1 d . . . H34 H 0.0720 0.1853 1.1060 0.028 Uiso 1 1 calc R . . C35 C 0.2348(4) 0.09470(14) 1.2562(4) 0.0172(8) Uani 1 1 d . . . C36 C 0.1408(4) 0.10940(15) 1.3093(4) 0.0222(9) Uani 1 1 d . . . H36 H 0.1025 0.1379 1.2873 0.027 Uiso 1 1 calc R . . C37 C 0.1024(4) 0.08265(15) 1.3943(4) 0.0235(9) Uani 1 1 d . . . H37 H 0.0380 0.0929 1.4296 0.028 Uiso 1 1 calc R . . C38 C 0.1578(4) 0.04158(15) 1.4266(4) 0.0249(9) Uani 1 1 d . . . H38 H 0.1326 0.0235 1.4854 0.030 Uiso 1 1 calc R . . C39 C 0.2508(4) 0.02620(15) 1.3738(4) 0.0241(9) Uani 1 1 d . . . H39 H 0.2882 -0.0025 1.3956 0.029 Uiso 1 1 calc R . . C40 C 0.2885(4) 0.05247(14) 1.2903(4) 0.0210(9) Uani 1 1 d . . . H40 H 0.3523 0.0417 1.2549 0.025 Uiso 1 1 calc R . . H H 0.129(4) 0.1622(9) 0.926(5) 0.033(14) Uiso 1 1 d D . . H1N H 0.359(5) 0.0520(16) 0.923(5) 0.027(13) Uiso 1 1 d . . . H2N H 0.316(5) 0.036(2) 1.015(5) 0.047(17) Uiso 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 0.01352(7) 0.01638(8) 0.01204(7) 0.00070(6) 0.00312(5) -0.00132(5) Ir2 0.01343(7) 0.01731(8) 0.01278(7) 0.00014(6) 0.00344(5) 0.00045(5) P1 0.0162(5) 0.0171(5) 0.0132(5) 0.0005(4) 0.0048(4) -0.0020(4) P2 0.0144(5) 0.0175(5) 0.0124(5) 0.0003(4) 0.0032(4) 0.0008(4) N 0.0222(18) 0.0113(17) 0.0165(17) -0.0008(13) 0.0042(14) -0.0010(13) C1 0.029(2) 0.028(2) 0.013(2) 0.0022(17) 0.0018(17) -0.0052(19) C2 0.022(2) 0.029(2) 0.0103(19) -0.0029(16) 0.0049(16) -0.0046(17) C3 0.034(3) 0.028(3) 0.026(2) -0.0077(19) 0.013(2) -0.009(2) C4 0.032(2) 0.022(2) 0.026(2) -0.0041(18) 0.0113(19) -0.0071(18) C5 0.019(2) 0.023(2) 0.016(2) -0.0003(16) 0.0058(16) -0.0075(16) C6 0.017(2) 0.025(2) 0.022(2) 0.0015(18) 0.0074(17) -0.0053(16) C7 0.015(2) 0.033(3) 0.032(3) 0.007(2) 0.0050(18) 0.0003(18) C8 0.021(2) 0.034(3) 0.030(3) 0.003(2) -0.0012(19) -0.0004(19) C9 0.020(2) 0.020(2) 0.024(2) 0.0010(17) 0.0096(17) 0.0056(16) C10 0.018(2) 0.020(2) 0.023(2) 0.0019(17) 0.0060(17) 0.0021(16) C11 0.025(2) 0.040(3) 0.020(2) 0.0068(19) 0.0058(18) 0.007(2) C12 0.017(2) 0.046(3) 0.019(2) 0.000(2) 0.0026(17) 0.0030(19) C13 0.014(2) 0.033(3) 0.017(2) -0.0089(18) -0.0022(16) -0.0008(17) C14 0.017(2) 0.026(2) 0.024(2) -0.0057(18) 0.0034(17) -0.0024(17) C15 0.016(2) 0.031(3) 0.026(2) 0.0017(19) 0.0042(17) -0.0023(17) C16 0.017(2) 0.035(3) 0.024(2) 0.0002(19) 0.0085(17) 0.0043(18) C17 0.026(2) 0.021(2) 0.0146(19) 0.0025(16) 0.0071(17) -0.0040(17) C18 0.032(3) 0.024(2) 0.022(2) 0.0001(18) 0.0073(19) -0.0063(18) C19 0.046(3) 0.028(3) 0.028(3) 0.002(2) 0.007(2) -0.017(2) C20 0.061(4) 0.015(2) 0.031(3) 0.0012(19) 0.012(2) -0.010(2) C21 0.049(3) 0.021(2) 0.030(3) 0.006(2) 0.013(2) 0.010(2) C22 0.030(2) 0.026(2) 0.019(2) 0.0056(17) 0.0070(18) 0.0010(18) C23 0.020(2) 0.024(2) 0.016(2) -0.0006(16) 0.0073(16) -0.0042(16) C24 0.023(2) 0.036(3) 0.024(2) -0.0016(19) 0.0080(18) 0.0022(19) C25 0.035(3) 0.048(3) 0.035(3) -0.007(2) 0.016(2) 0.005(2) C26 0.029(3) 0.056(3) 0.022(2) -0.011(2) 0.013(2) -0.007(2) C27 0.032(3) 0.042(3) 0.017(2) 0.0002(19) 0.0041(19) -0.014(2) C28 0.025(2) 0.024(2) 0.021(2) 0.0022(17) 0.0084(18) -0.0061(17) C29 0.026(2) 0.017(2) 0.017(2) 0.0005(16) 0.0085(17) -0.0015(16) C30 0.024(2) 0.026(2) 0.027(2) 0.0007(18) 0.0059(19) 0.0002(18) C31 0.038(3) 0.023(3) 0.036(3) -0.004(2) 0.006(2) -0.007(2) C32 0.045(3) 0.017(2) 0.042(3) -0.006(2) 0.016(2) 0.002(2) C33 0.030(3) 0.027(3) 0.036(3) 0.002(2) 0.013(2) 0.0078(19) C34 0.024(2) 0.022(2) 0.026(2) -0.0005(17) 0.0092(18) 0.0017(17) C35 0.0139(18) 0.024(2) 0.0108(18) -0.0015(15) -0.0005(14) -0.0018(15) C36 0.023(2) 0.025(2) 0.018(2) -0.0012(17) 0.0049(17) 0.0028(17) C37 0.018(2) 0.033(3) 0.021(2) -0.0013(18) 0.0087(17) -0.0005(18) C38 0.027(2) 0.030(3) 0.020(2) 0.0054(18) 0.0100(18) -0.0056(18) C39 0.034(2) 0.019(2) 0.018(2) 0.0039(16) 0.0060(18) 0.0024(18) C40 0.023(2) 0.023(2) 0.016(2) -0.0005(16) 0.0043(16) 0.0025(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 N 2.175(3) . ? Ir1 C5 2.218(4) . ? Ir1 C6 2.221(4) . ? Ir1 C2 2.226(4) . ? Ir1 C1 2.241(4) . ? Ir1 P2 2.3669(10) . ? Ir1 P1 2.3764(10) . ? Ir1 H 1.608(19) . ? Ir2 C9 2.103(4) . ? Ir2 C10 2.109(4) . ? Ir2 N 2.131(3) . ? Ir2 C13 2.150(4) . ? Ir2 C14 2.153(4) . ? Ir2 P2 2.3937(10) . ? Ir2 P1 2.4190(10) . ? P1 C23 1.829(4) . ? P1 C17 1.834(4) . ? P2 C29 1.836(4) . ? P2 C35 1.846(4) . ? N H1N 0.86(5) . ? N H2N 0.94(6) . ? C1 C2 1.379(6) . ? C1 C8 1.526(6) . ? C1 H1 0.93(5) . ? C2 C3 1.509(6) . ? C2 H2 0.97(5) . ? C3 C4 1.527(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.514(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.388(6) . ? C5 H5 0.91(5) . ? C6 C7 1.503(6) . ? C6 H6 0.90(5) . ? C7 C8 1.530(7) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.459(6) . ? C9 C16 1.527(6) . ? C9 H9 0.98(5) . ? C10 C11 1.517(6) . ? C10 H10 0.94(5) . ? C11 C12 1.516(7) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.535(6) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.405(6) . ? C13 H13 0.96(5) . ? C14 C15 1.506(6) . ? C14 H14 0.946(19) . ? C15 C16 1.543(6) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.385(6) . ? C17 C18 1.398(6) . ? C18 C19 1.396(6) . ? C18 H18 0.9500 . ? C19 C20 1.380(8) . ? C19 H19 0.9500 . ? C20 C21 1.379(7) . ? C20 H20 0.9500 . ? C21 C22 1.388(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.392(6) . ? C23 C28 1.402(6) . ? C24 C25 1.401(7) . ? C24 H24 0.9500 . ? C25 C26 1.388(8) . ? C25 H25 0.9500 . ? C26 C27 1.380(7) . ? C26 H26 0.9500 . ? C27 C28 1.379(6) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.384(6) . ? C29 C34 1.394(6) . ? C30 C31 1.392(7) . ? C30 H30 0.9500 . ? C31 C32 1.386(7) . ? C31 H31 0.9500 . ? C32 C33 1.375(7) . ? C32 H32 0.9500 . ? C33 C34 1.389(6) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.395(6) . ? C35 C40 1.397(6) . ? C36 C37 1.396(6) . ? C36 H36 0.9500 . ? C37 C38 1.370(6) . ? C37 H37 0.9500 . ? C38 C39 1.390(6) . ? C38 H38 0.9500 . ? C39 C40 1.370(6) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 N Ir1 C5 85.18(15) . . ? N Ir1 C6 119.59(15) . . ? C5 Ir1 C6 36.44(16) . . ? N Ir1 C2 86.13(15) . . ? C5 Ir1 C2 80.03(15) . . ? C6 Ir1 C2 94.33(16) . . ? N Ir1 C1 121.94(16) . . ? C5 Ir1 C1 87.31(16) . . ? C6 Ir1 C1 79.60(17) . . ? C2 Ir1 C1 35.97(16) . . ? N Ir1 P2 75.32(10) . . ? C5 Ir1 P2 99.23(11) . . ? C6 Ir1 P2 95.81(12) . . ? C2 Ir1 P2 161.42(12) . . ? C1 Ir1 P2 162.22(13) . . ? N Ir1 P1 72.87(10) . . ? C5 Ir1 P1 158.05(12) . . ? C6 Ir1 P1 163.07(12) . . ? C2 Ir1 P1 98.12(11) . . ? C1 Ir1 P1 104.12(12) . . ? P2 Ir1 P1 75.56(4) . . ? N Ir1 H 156.5(18) . . ? C5 Ir1 H 113.5(17) . . ? C6 Ir1 H 77.1(17) . . ? C2 Ir1 H 110.3(18) . . ? C1 Ir1 H 75.1(18) . . ? P2 Ir1 H 87.2(18) . . ? P1 Ir1 H 87.8(17) . . ? C9 Ir2 C10 40.54(16) . . ? C9 Ir2 N 93.09(16) . . ? C10 Ir2 N 89.33(15) . . ? C9 Ir2 C13 88.52(17) . . ? C10 Ir2 C13 79.11(18) . . ? N Ir2 C13 160.19(16) . . ? C9 Ir2 C14 81.62(17) . . ? C10 Ir2 C14 97.80(17) . . ? N Ir2 C14 161.43(16) . . ? C13 Ir2 C14 38.11(17) . . ? C9 Ir2 P2 160.29(12) . . ? C10 Ir2 P2 121.92(12) . . ? N Ir2 P2 75.53(10) . . ? C13 Ir2 P2 96.89(12) . . ? C14 Ir2 P2 114.06(12) . . ? C9 Ir2 P1 118.19(12) . . ? C10 Ir2 P1 152.60(12) . . ? N Ir2 P1 72.73(10) . . ? C13 Ir2 P1 123.46(13) . . ? C14 Ir2 P1 94.01(13) . . ? P2 Ir2 P1 74.28(3) . . ? C23 P1 C17 99.96(19) . . ? C23 P1 Ir1 111.65(14) . . ? C17 P1 Ir1 118.51(14) . . ? C23 P1 Ir2 117.90(14) . . ? C17 P1 Ir2 122.82(14) . . ? Ir1 P1 Ir2 86.73(3) . . ? C29 P2 C35 102.79(19) . . ? C29 P2 Ir1 110.52(14) . . ? C35 P2 Ir1 113.42(13) . . ? C29 P2 Ir2 125.78(14) . . ? C35 P2 Ir2 116.31(13) . . ? Ir1 P2 Ir2 87.52(3) . . ? Ir2 N Ir1 99.76(14) . . ? Ir2 N H1N 116(3) . . ? Ir1 N H1N 111(3) . . ? Ir2 N H2N 120(3) . . ? Ir1 N H2N 115(3) . . ? H1N N H2N 96(4) . . ? C2 C1 C8 123.6(4) . . ? C2 C1 Ir1 71.4(2) . . ? C8 C1 Ir1 112.1(3) . . ? C2 C1 H1 121(3) . . ? C8 C1 H1 111(3) . . ? Ir1 C1 H1 108(3) . . ? C1 C2 C3 125.2(4) . . ? C1 C2 Ir1 72.6(2) . . ? C3 C2 Ir1 108.9(3) . . ? C1 C2 H2 115(3) . . ? C3 C2 H2 117(3) . . ? Ir1 C2 H2 106(3) . . ? C2 C3 C4 114.6(4) . . ? C2 C3 H3A 108.6 . . ? C4 C3 H3A 108.6 . . ? C2 C3 H3B 108.6 . . ? C4 C3 H3B 108.6 . . ? H3A C3 H3B 107.6 . . ? C5 C4 C3 113.7(4) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? C6 C5 C4 123.2(4) . . ? C6 C5 Ir1 71.9(2) . . ? C4 C5 Ir1 112.7(3) . . ? C6 C5 H5 116(3) . . ? C4 C5 H5 116(3) . . ? Ir1 C5 H5 106(3) . . ? C5 C6 C7 124.8(4) . . ? C5 C6 Ir1 71.6(2) . . ? C7 C6 Ir1 111.1(3) . . ? C5 C6 H6 121(3) . . ? C7 C6 H6 112(3) . . ? Ir1 C6 H6 105(3) . . ? C6 C7 C8 113.9(4) . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C1 C8 C7 114.8(4) . . ? C1 C8 H8A 108.6 . . ? C7 C8 H8A 108.6 . . ? C1 C8 H8B 108.6 . . ? C7 C8 H8B 108.6 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C16 123.7(4) . . ? C10 C9 Ir2 69.9(2) . . ? C16 C9 Ir2 114.7(3) . . ? C10 C9 H9 116(3) . . ? C16 C9 H9 114(3) . . ? Ir2 C9 H9 111(3) . . ? C9 C10 C11 123.4(4) . . ? C9 C10 Ir2 69.5(2) . . ? C11 C10 Ir2 115.4(3) . . ? C9 C10 H10 116(3) . . ? C11 C10 H10 111(3) . . ? Ir2 C10 H10 116(3) . . ? C12 C11 C10 110.9(4) . . ? C12 C11 H11A 109.5 . . ? C10 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 111.4(4) . . ? C11 C12 H12A 109.3 . . ? C13 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? C13 C12 H12B 109.3 . . ? H12A C12 H12B 108.0 . . ? C14 C13 C12 123.6(4) . . ? C14 C13 Ir2 71.0(2) . . ? C12 C13 Ir2 115.1(3) . . ? C14 C13 H13 114(3) . . ? C12 C13 H13 116(3) . . ? Ir2 C13 H13 108(3) . . ? C13 C14 C15 123.8(4) . . ? C13 C14 Ir2 70.9(2) . . ? C15 C14 Ir2 110.0(3) . . ? C13 C14 H14 113(3) . . ? C15 C14 H14 120(3) . . ? Ir2 C14 H14 106(3) . . ? C14 C15 C16 113.1(4) . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C9 C16 C15 111.4(3) . . ? C9 C16 H16A 109.3 . . ? C15 C16 H16A 109.3 . . ? C9 C16 H16B 109.3 . . ? C15 C16 H16B 109.3 . . ? H16A C16 H16B 108.0 . . ? C22 C17 C18 118.7(4) . . ? C22 C17 P1 124.3(3) . . ? C18 C17 P1 116.9(3) . . ? C19 C18 C17 120.7(5) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C20 C19 C18 119.2(5) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C21 C20 C19 120.6(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 120.1(5) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C17 C22 C21 120.6(4) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C24 C23 C28 118.1(4) . . ? C24 C23 P1 120.1(3) . . ? C28 C23 P1 121.7(3) . . ? C23 C24 C25 120.6(5) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 119.7(5) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C27 C26 C25 120.2(4) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 119.9(5) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C28 C23 121.4(4) . . ? C27 C28 H28 119.3 . . ? C23 C28 H28 119.3 . . ? C30 C29 C34 118.2(4) . . ? C30 C29 P2 120.4(3) . . ? C34 C29 P2 121.3(3) . . ? C29 C30 C31 120.7(4) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 120.3(5) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C33 C32 C31 119.6(4) . . ? C33 C32 H32 120.2 . . ? C31 C32 H32 120.2 . . ? C32 C33 C34 120.1(4) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 C29 121.1(4) . . ? C33 C34 H34 119.4 . . ? C29 C34 H34 119.4 . . ? C36 C35 C40 118.0(4) . . ? C36 C35 P2 124.5(3) . . ? C40 C35 P2 117.5(3) . . ? C35 C36 C37 120.7(4) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C38 C37 C36 119.8(4) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C37 C38 C39 120.3(4) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C40 C39 C38 119.9(4) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C35 121.3(4) . . ? C39 C40 H40 119.4 . . ? C35 C40 H40 119.4 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N Ir1 P1 C23 83.19(18) . . . . ? C5 Ir1 P1 C23 83.3(3) . . . . ? C6 Ir1 P1 C23 -137.2(4) . . . . ? C2 Ir1 P1 C23 -0.19(19) . . . . ? C1 Ir1 P1 C23 -36.4(2) . . . . ? P2 Ir1 P1 C23 161.97(16) . . . . ? N Ir1 P1 C17 -161.52(18) . . . . ? C5 Ir1 P1 C17 -161.4(3) . . . . ? C6 Ir1 P1 C17 -21.9(4) . . . . ? C2 Ir1 P1 C17 115.10(19) . . . . ? C1 Ir1 P1 C17 78.9(2) . . . . ? P2 Ir1 P1 C17 -82.73(15) . . . . ? N Ir1 P1 Ir2 -35.60(10) . . . . ? C5 Ir1 P1 Ir2 -35.5(3) . . . . ? C6 Ir1 P1 Ir2 104.0(4) . . . . ? C2 Ir1 P1 Ir2 -118.98(12) . . . . ? C1 Ir1 P1 Ir2 -155.16(13) . . . . ? P2 Ir1 P1 Ir2 43.19(3) . . . . ? C9 Ir2 P1 C23 7.8(2) . . . . ? C10 Ir2 P1 C23 -25.1(3) . . . . ? N Ir2 P1 C23 -76.34(18) . . . . ? C13 Ir2 P1 C23 116.4(2) . . . . ? C14 Ir2 P1 C23 90.40(19) . . . . ? P2 Ir2 P1 C23 -155.72(16) . . . . ? C9 Ir2 P1 C17 -117.3(2) . . . . ? C10 Ir2 P1 C17 -150.2(3) . . . . ? N Ir2 P1 C17 158.6(2) . . . . ? C13 Ir2 P1 C17 -8.7(2) . . . . ? C14 Ir2 P1 C17 -34.6(2) . . . . ? P2 Ir2 P1 C17 79.23(17) . . . . ? C9 Ir2 P1 Ir1 120.58(14) . . . . ? C10 Ir2 P1 Ir1 87.7(3) . . . . ? N Ir2 P1 Ir1 36.47(11) . . . . ? C13 Ir2 P1 Ir1 -130.81(14) . . . . ? C14 Ir2 P1 Ir1 -156.78(12) . . . . ? P2 Ir2 P1 Ir1 -42.91(3) . . . . ? N Ir1 P2 C29 159.47(18) . . . . ? C5 Ir1 P2 C29 -118.03(18) . . . . ? C6 Ir1 P2 C29 -81.42(19) . . . . ? C2 Ir1 P2 C29 155.8(4) . . . . ? C1 Ir1 P2 C29 -7.5(4) . . . . ? P1 Ir1 P2 C29 83.77(15) . . . . ? N Ir1 P2 C35 -85.71(18) . . . . ? C5 Ir1 P2 C35 -3.21(19) . . . . ? C6 Ir1 P2 C35 33.40(19) . . . . ? C2 Ir1 P2 C35 -89.4(4) . . . . ? C1 Ir1 P2 C35 107.3(4) . . . . ? P1 Ir1 P2 C35 -161.41(15) . . . . ? N Ir1 P2 Ir2 31.98(10) . . . . ? C5 Ir1 P2 Ir2 114.48(12) . . . . ? C6 Ir1 P2 Ir2 151.08(12) . . . . ? C2 Ir1 P2 Ir2 28.3(4) . . . . ? C1 Ir1 P2 Ir2 -135.0(4) . . . . ? P1 Ir1 P2 Ir2 -43.72(3) . . . . ? C9 Ir2 P2 C29 157.4(4) . . . . ? C10 Ir2 P2 C29 133.7(2) . . . . ? N Ir2 P2 C29 -146.33(19) . . . . ? C13 Ir2 P2 C29 52.3(2) . . . . ? C14 Ir2 P2 C29 16.8(2) . . . . ? P1 Ir2 P2 C29 -70.57(17) . . . . ? C9 Ir2 P2 C35 26.0(4) . . . . ? C10 Ir2 P2 C35 2.4(2) . . . . ? N Ir2 P2 C35 82.31(17) . . . . ? C13 Ir2 P2 C35 -79.05(19) . . . . ? C14 Ir2 P2 C35 -114.6(2) . . . . ? P1 Ir2 P2 C35 158.07(15) . . . . ? C9 Ir2 P2 Ir1 -88.9(4) . . . . ? C10 Ir2 P2 Ir1 -112.60(14) . . . . ? N Ir2 P2 Ir1 -32.68(10) . . . . ? C13 Ir2 P2 Ir1 165.97(13) . . . . ? C14 Ir2 P2 Ir1 130.45(14) . . . . ? P1 Ir2 P2 Ir1 43.09(3) . . . . ? C9 Ir2 N Ir1 -159.75(16) . . . . ? C10 Ir2 N Ir1 159.87(17) . . . . ? C13 Ir2 N Ir1 106.0(4) . . . . ? C14 Ir2 N Ir1 -87.1(5) . . . . ? P2 Ir2 N Ir1 36.56(10) . . . . ? P1 Ir2 N Ir1 -41.15(10) . . . . ? C5 Ir1 N Ir2 -137.95(16) . . . . ? C6 Ir1 N Ir2 -125.46(17) . . . . ? C2 Ir1 N Ir2 141.75(17) . . . . ? C1 Ir1 N Ir2 138.25(16) . . . . ? P2 Ir1 N Ir2 -37.09(10) . . . . ? P1 Ir1 N Ir2 42.02(10) . . . . ? N Ir1 C1 C2 5.9(3) . . . . ? C5 Ir1 C1 C2 -76.7(3) . . . . ? C6 Ir1 C1 C2 -112.6(3) . . . . ? P2 Ir1 C1 C2 171.0(3) . . . . ? P1 Ir1 C1 C2 84.3(3) . . . . ? N Ir1 C1 C8 125.5(3) . . . . ? C5 Ir1 C1 C8 42.9(3) . . . . ? C6 Ir1 C1 C8 7.0(3) . . . . ? C2 Ir1 C1 C8 119.5(5) . . . . ? P2 Ir1 C1 C8 -69.4(6) . . . . ? P1 Ir1 C1 C8 -156.1(3) . . . . ? C8 C1 C2 C3 -3.5(7) . . . . ? Ir1 C1 C2 C3 101.2(4) . . . . ? C8 C1 C2 Ir1 -104.6(4) . . . . ? N Ir1 C2 C1 -174.9(3) . . . . ? C5 Ir1 C2 C1 99.3(3) . . . . ? C6 Ir1 C2 C1 65.6(3) . . . . ? P2 Ir1 C2 C1 -171.4(3) . . . . ? P1 Ir1 C2 C1 -102.9(3) . . . . ? N Ir1 C2 C3 63.0(3) . . . . ? C5 Ir1 C2 C3 -22.8(3) . . . . ? C6 Ir1 C2 C3 -56.4(3) . . . . ? C1 Ir1 C2 C3 -122.1(4) . . . . ? P2 Ir1 C2 C3 66.5(5) . . . . ? P1 Ir1 C2 C3 135.0(3) . . . . ? C1 C2 C3 C4 -46.2(6) . . . . ? Ir1 C2 C3 C4 35.4(5) . . . . ? C2 C3 C4 C5 -30.2(6) . . . . ? C3 C4 C5 C6 91.8(5) . . . . ? C3 C4 C5 Ir1 9.2(5) . . . . ? N Ir1 C5 C6 161.5(3) . . . . ? C2 Ir1 C5 C6 -111.5(3) . . . . ? C1 Ir1 C5 C6 -76.1(3) . . . . ? P2 Ir1 C5 C6 87.3(2) . . . . ? P1 Ir1 C5 C6 161.5(2) . . . . ? N Ir1 C5 C4 -79.2(3) . . . . ? C6 Ir1 C5 C4 119.2(4) . . . . ? C2 Ir1 C5 C4 7.7(3) . . . . ? C1 Ir1 C5 C4 43.1(3) . . . . ? P2 Ir1 C5 C4 -153.5(3) . . . . ? P1 Ir1 C5 C4 -79.3(4) . . . . ? C4 C5 C6 C7 -2.5(7) . . . . ? Ir1 C5 C6 C7 103.3(4) . . . . ? C4 C5 C6 Ir1 -105.8(4) . . . . ? N Ir1 C6 C5 -21.3(3) . . . . ? C2 Ir1 C6 C5 66.7(3) . . . . ? C1 Ir1 C6 C5 99.7(3) . . . . ? P2 Ir1 C6 C5 -97.7(2) . . . . ? P1 Ir1 C6 C5 -155.9(3) . . . . ? N Ir1 C6 C7 -142.4(3) . . . . ? C5 Ir1 C6 C7 -121.1(4) . . . . ? C2 Ir1 C6 C7 -54.4(3) . . . . ? C1 Ir1 C6 C7 -21.4(3) . . . . ? P2 Ir1 C6 C7 141.2(3) . . . . ? P1 Ir1 C6 C7 83.0(5) . . . . ? C5 C6 C7 C8 -48.9(6) . . . . ? Ir1 C6 C7 C8 32.9(5) . . . . ? C2 C1 C8 C7 90.3(5) . . . . ? Ir1 C1 C8 C7 8.6(5) . . . . ? C6 C7 C8 C1 -27.7(6) . . . . ? N Ir2 C9 C10 -85.4(3) . . . . ? C13 Ir2 C9 C10 74.9(3) . . . . ? C14 Ir2 C9 C10 112.5(3) . . . . ? P2 Ir2 C9 C10 -31.6(5) . . . . ? P1 Ir2 C9 C10 -157.4(2) . . . . ? C10 Ir2 C9 C16 -118.8(4) . . . . ? N Ir2 C9 C16 155.8(3) . . . . ? C13 Ir2 C9 C16 -43.9(3) . . . . ? C14 Ir2 C9 C16 -6.3(3) . . . . ? P2 Ir2 C9 C16 -150.4(3) . . . . ? P1 Ir2 C9 C16 83.8(3) . . . . ? C16 C9 C10 C11 -0.7(7) . . . . ? Ir2 C9 C10 C11 -107.6(4) . . . . ? C16 C9 C10 Ir2 106.9(4) . . . . ? N Ir2 C10 C9 95.5(3) . . . . ? C13 Ir2 C10 C9 -100.6(3) . . . . ? C14 Ir2 C10 C9 -67.3(3) . . . . ? P2 Ir2 C10 C9 168.0(2) . . . . ? P1 Ir2 C10 C9 47.4(4) . . . . ? C9 Ir2 C10 C11 118.2(4) . . . . ? N Ir2 C10 C11 -146.2(3) . . . . ? C13 Ir2 C10 C11 17.6(3) . . . . ? C14 Ir2 C10 C11 51.0(3) . . . . ? P2 Ir2 C10 C11 -73.8(3) . . . . ? P1 Ir2 C10 C11 165.7(2) . . . . ? C9 C10 C11 C12 50.3(6) . . . . ? Ir2 C10 C11 C12 -31.0(5) . . . . ? C10 C11 C12 C13 28.9(5) . . . . ? C11 C12 C13 C14 -98.4(5) . . . . ? C11 C12 C13 Ir2 -15.3(5) . . . . ? C9 Ir2 C13 C14 78.3(3) . . . . ? C10 Ir2 C13 C14 118.0(3) . . . . ? N Ir2 C13 C14 173.3(4) . . . . ? P2 Ir2 C13 C14 -120.7(2) . . . . ? P1 Ir2 C13 C14 -45.1(3) . . . . ? C9 Ir2 C13 C12 -40.7(3) . . . . ? C10 Ir2 C13 C12 -1.0(3) . . . . ? N Ir2 C13 C12 54.3(6) . . . . ? C14 Ir2 C13 C12 -119.0(4) . . . . ? P2 Ir2 C13 C12 120.3(3) . . . . ? P1 Ir2 C13 C12 -164.0(3) . . . . ? C12 C13 C14 C15 6.4(7) . . . . ? Ir2 C13 C14 C15 -101.7(4) . . . . ? C12 C13 C14 Ir2 108.1(4) . . . . ? C9 Ir2 C14 C13 -98.4(3) . . . . ? C10 Ir2 C14 C13 -61.1(3) . . . . ? N Ir2 C14 C13 -172.8(4) . . . . ? P2 Ir2 C14 C13 69.1(3) . . . . ? P1 Ir2 C14 C13 143.7(3) . . . . ? C9 Ir2 C14 C15 21.6(3) . . . . ? C10 Ir2 C14 C15 58.9(3) . . . . ? N Ir2 C14 C15 -52.8(6) . . . . ? C13 Ir2 C14 C15 120.0(4) . . . . ? P2 Ir2 C14 C15 -170.8(3) . . . . ? P1 Ir2 C14 C15 -96.3(3) . . . . ? C13 C14 C15 C16 46.3(6) . . . . ? Ir2 C14 C15 C16 -33.6(4) . . . . ? C10 C9 C16 C15 -91.6(5) . . . . ? Ir2 C9 C16 C15 -10.1(5) . . . . ? C14 C15 C16 C9 28.8(5) . . . . ? C23 P1 C17 C22 116.3(4) . . . . ? Ir1 P1 C17 C22 -5.1(4) . . . . ? Ir2 P1 C17 C22 -111.0(3) . . . . ? C23 P1 C17 C18 -64.7(4) . . . . ? Ir1 P1 C17 C18 173.9(3) . . . . ? Ir2 P1 C17 C18 68.0(4) . . . . ? C22 C17 C18 C19 0.3(6) . . . . ? P1 C17 C18 C19 -178.8(3) . . . . ? C17 C18 C19 C20 0.2(7) . . . . ? C18 C19 C20 C21 0.2(7) . . . . ? C19 C20 C21 C22 -1.1(7) . . . . ? C18 C17 C22 C21 -1.2(6) . . . . ? P1 C17 C22 C21 177.8(3) . . . . ? C20 C21 C22 C17 1.6(7) . . . . ? C17 P1 C23 C24 138.1(4) . . . . ? Ir1 P1 C23 C24 -95.6(4) . . . . ? Ir2 P1 C23 C24 2.5(4) . . . . ? C17 P1 C23 C28 -45.7(4) . . . . ? Ir1 P1 C23 C28 80.6(4) . . . . ? Ir2 P1 C23 C28 178.7(3) . . . . ? C28 C23 C24 C25 -2.5(7) . . . . ? P1 C23 C24 C25 173.8(4) . . . . ? C23 C24 C25 C26 2.7(8) . . . . ? C24 C25 C26 C27 -1.0(8) . . . . ? C25 C26 C27 C28 -0.7(7) . . . . ? C26 C27 C28 C23 0.8(7) . . . . ? C24 C23 C28 C27 0.8(6) . . . . ? P1 C23 C28 C27 -175.5(3) . . . . ? C35 P2 C29 C30 108.8(4) . . . . ? Ir1 P2 C29 C30 -129.9(3) . . . . ? Ir2 P2 C29 C30 -27.6(4) . . . . ? C35 P2 C29 C34 -74.3(4) . . . . ? Ir1 P2 C29 C34 47.0(4) . . . . ? Ir2 P2 C29 C34 149.3(3) . . . . ? C34 C29 C30 C31 0.8(7) . . . . ? P2 C29 C30 C31 177.8(4) . . . . ? C29 C30 C31 C32 -0.1(7) . . . . ? C30 C31 C32 C33 -0.4(8) . . . . ? C31 C32 C33 C34 0.3(8) . . . . ? C32 C33 C34 C29 0.4(7) . . . . ? C30 C29 C34 C33 -0.9(6) . . . . ? P2 C29 C34 C33 -177.9(3) . . . . ? C29 P2 C35 C36 24.4(4) . . . . ? Ir1 P2 C35 C36 -94.9(4) . . . . ? Ir2 P2 C35 C36 165.8(3) . . . . ? C29 P2 C35 C40 -153.5(3) . . . . ? Ir1 P2 C35 C40 87.2(3) . . . . ? Ir2 P2 C35 C40 -12.1(4) . . . . ? C40 C35 C36 C37 0.3(6) . . . . ? P2 C35 C36 C37 -177.6(3) . . . . ? C35 C36 C37 C38 0.3(7) . . . . ? C36 C37 C38 C39 -0.9(7) . . . . ? C37 C38 C39 C40 0.9(7) . . . . ? C38 C39 C40 C35 -0.3(7) . . . . ? C36 C35 C40 C39 -0.3(6) . . . . ? P2 C35 C40 C39 177.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.838 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.157 _database_code_depnum_ccdc_archive 'CCDC 951633' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cmpnd_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H47 Ir2 N P2, C6 D6' _chemical_formula_sum 'C46 H47 D6 Ir2 N P2' _chemical_formula_weight 1072.35 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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P bca' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 21.7209(10) _cell_length_b 10.3274(5) _cell_length_c 33.4874(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7511.9(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 22992 _cell_measurement_theta_min 2.235 _cell_measurement_theta_max 28.20 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.258 _exptl_crystal_size_mid 0.111 _exptl_crystal_size_min 0.110 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.896 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4160 _exptl_absorpt_coefficient_mu 7.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.242 _exptl_absorpt_correction_T_max 0.446 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX DUO CCD system' _diffrn_measurement_method 'narrow \w frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 85822 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 28.54 _reflns_number_total 9153 _reflns_number_gt 8274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.12, BrukerAXS; PARST(Nardelli, 1995)' _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. A disorder has been observed in 4 carbon atoms of both cod-based ligands (C8H12 and C8H13 fragments). They have been included in the model in two sets of positions with complementary occupancy factors (0.7/0.3). They have been refined with geometrical restrains (using the SAME command). Hydrogen atoms of the non-olefinic carbons of these fragments, and those of the phenyl groups have been included in the model in calculated positions and refined with a riding model. Hydrogen atoms bonded to olefinic carbons (of the major component) have been included in observed positions and refined with a restrain in the C-H distances, their thermal parameters have been restrained to be -1.2 times those of their carbon parent atoms. Hydrogen atoms of the NH2 bridging group have been included in observed positions and refined with a restrain in N-H distances. There are very large solvent accessible voids in the structure and a zone where residual density peaks are observed. The solvent is highly disordered and it could not be modelled even with several restraints. Therefore, SQUEEZE corrections have been applied. The total potential solvent accesible void volume (959 \A3) and the electron count (328 e in the unit cell) may agree with the presence of eight C6D6 molecules. They have been included in the chemical formula, F000 and density. Results of the SQUEEZE calculations are included at the end of this cif file. ; _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^)+(0.0219P)^2^+62.5186P] 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 9153 _refine_ls_number_parameters 431 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0488 _refine_ls_R_factor_gt 0.0419 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0847 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.036 _refine_ls_shift/su_mean 0.001 _iucr_refine_instructions_details ; TITL fjl231as in Pbca CELL 0.71073 21.7209 10.3274 33.4874 90.000 90.000 90.000 ZERR 8.00 0.0010 0.0005 0.0016 0.000 0.000 0.000 LATT 1 SYMM 1/2 + X, 1/2 - Y, - Z SYMM - X, 1/2 + Y, 1/2 - Z SYMM 1/2 - X, - Y, 1/2 + Z SFAC C H IR N P UNIT 368 376 16 8 16 MERG 2 OMIT 0 0 2 OMIT 2 0 2 OMIT 1 0 4 OMIT 5 0 4 OMIT 4 0 0 OMIT 5 0 2 OMIT 3 0 2 OMIT 0 0 6 OMIT 2 0 8 dfix 1.54 0.02 c11 C12B dfix 0.96 0.02 C1 H1 C2 H2 C9 H9 C10 H10 DFIX 0.96 0.02 C6A H6 C14A H14 DFIX 0.87 0.02 N1 H1N N1 H2N FMAP 2 PLAN 10 ACTA 55.00 BOND $H CONF WPDB -2 L.S. 4 TEMP -173.00 WGHT 0.021900 62.518597 FVAR 0.20974 IR1 3 0.403498 0.707578 0.115327 11.00000 0.01911 0.01530 = 0.01619 0.00163 -0.00026 -0.00197 IR2 3 0.500306 0.759113 0.162304 11.00000 0.01982 0.01515 = 0.01717 0.00209 -0.00130 -0.00141 P1 5 0.505905 0.669233 0.098070 11.00000 0.01703 0.01728 = 0.01977 0.00350 0.00214 0.00221 P2 5 0.399492 0.847891 0.168859 11.00000 0.01725 0.01690 = 0.01869 0.00213 0.00240 0.00091 N1 4 0.441257 0.595299 0.164704 11.00000 0.04072 0.01445 = 0.01429 0.00186 0.00788 -0.00170 C1 1 0.359022 0.565893 0.079538 11.00000 0.02060 0.01548 = 0.02511 -0.00105 -0.00113 -0.00201 C2 1 0.318021 0.611943 0.109834 11.00000 0.01456 0.01455 = 0.02200 0.00152 -0.00141 -0.00347 C3 1 0.259823 0.689812 0.103804 11.00000 0.01974 0.02319 = 0.03235 -0.00406 -0.00013 0.00124 AFIX 23 H3A 2 0.226085 0.628068 0.098100 11.00000 -1.20000 H3B 2 0.249912 0.732405 0.129497 11.00000 -1.20000 AFIX 0 PART 1 C4A 1 0.258599 0.791144 0.072169 10.70000 0.02325 AFIX 23 H4A1 2 0.219749 0.840664 0.074573 10.70000 -1.20000 H4A2 2 0.258494 0.748122 0.045750 10.70000 -1.20000 AFIX 0 C5A 1 0.311752 0.884452 0.073736 10.70000 0.01900 AFIX 23 H5A1 2 0.311248 0.928459 0.099999 10.70000 -1.20000 H5A2 2 0.305408 0.951476 0.053005 10.70000 -1.20000 AFIX 0 C6A 1 0.374735 0.824675 0.067659 10.70000 0.01386 H6 2 0.408383 0.882053 0.061283 10.70000 -1.20000 C7A 1 0.378535 0.747977 0.028836 10.70000 0.02400 AFIX 23 H7A1 2 0.421798 0.744526 0.019595 10.70000 -1.20000 H7A2 2 0.353749 0.791489 0.007968 10.70000 -1.20000 AFIX 0 PART 2 SAME 0.03 0.03 C4A C5A C6A C7A C15B 1 0.655025 0.850341 0.179561 10.30000 0.03523 AFIX 23 H15A 2 0.654717 0.904503 0.203953 10.30000 -1.20000 H15B 2 0.697979 0.846595 0.169742 10.30000 -1.20000 AFIX 0 C14B 1 0.616157 0.914112 0.148616 10.30000 0.04669 AFIX 23 H14A 2 0.617542 0.860780 0.124066 10.30000 -1.20000 H14B 2 0.634666 0.999158 0.142139 10.30000 -1.20000 AFIX 0 C13B 1 0.549079 0.935473 0.159800 10.30000 0.01437 C12B 1 0.544736 1.000850 0.201435 10.30000 0.03019 AFIX 23 H12A 2 0.505287 1.048484 0.203293 10.30000 -1.20000 H12B 2 0.578517 1.064623 0.204097 10.30000 -1.20000 AFIX 0 PART 0 C8 1 0.353119 0.603077 0.035757 11.00000 0.02484 0.02836 = 0.02566 -0.00800 -0.00272 0.00202 AFIX 23 H8A 2 0.309400 0.598180 0.027537 11.00000 -1.20000 H8B 2 0.376905 0.541581 0.019135 11.00000 -1.20000 AFIX 0 C9 1 0.566770 0.679154 0.201113 11.00000 0.02279 0.02875 = 0.02666 0.00131 -0.01036 0.00433 C10 1 0.527997 0.766433 0.223133 11.00000 0.02537 0.03095 = 0.01219 0.00214 -0.00212 0.00246 C11 1 0.548803 0.900469 0.237232 11.00000 0.02245 0.04025 = 0.02745 -0.01506 -0.00136 0.00002 AFIX 23 H11A 2 0.526921 0.922162 0.262288 11.00000 -1.20000 H11B 2 0.593412 0.897585 0.243229 11.00000 -1.20000 AFIX 0 PART 1 C12A 1 0.537051 1.005322 0.207122 10.70000 0.02285 AFIX 23 H12C 2 0.496513 1.045287 0.212661 10.70000 -1.20000 H12D 2 0.568839 1.073348 0.210079 10.70000 -1.20000 AFIX 0 C13A 1 0.537759 0.956815 0.165325 10.70000 0.01826 H13A 2 0.523165 0.998343 0.149979 10.70000 -1.20000 C14A 1 0.583183 0.875500 0.149683 10.70000 0.01904 H14 2 0.590783 0.882919 0.121532 10.70000 -1.20000 C15A 1 0.641392 0.835009 0.172168 10.70000 0.02402 AFIX 23 H15C 2 0.676506 0.831654 0.153348 10.70000 -1.20000 H15D 2 0.650937 0.900205 0.192938 10.70000 -1.20000 AFIX 0 PART 2 SAME 0.03 0.03 C12A C13A C14A C15A C4B 1 0.277071 0.824580 0.079523 10.30000 0.04566 AFIX 23 H4B1 2 0.267613 0.813060 0.050823 10.30000 -1.20000 H4B2 2 0.251148 0.896118 0.089747 10.30000 -1.20000 AFIX 0 C5B 1 0.342134 0.859550 0.084005 10.30000 0.02632 C6B 1 0.389763 0.816867 0.059711 10.30000 0.02700 C7B 1 0.382461 0.720253 0.026105 10.30000 0.02248 AFIX 23 H7B1 2 0.358907 0.762274 0.004365 10.30000 -1.20000 H7B2 2 0.423878 0.699924 0.015474 10.30000 -1.20000 AFIX 0 PART 0 C16 1 0.633214 0.705325 0.191303 11.00000 0.02552 0.02953 = 0.02682 -0.00086 -0.00230 0.00227 AFIX 23 H16A 2 0.657959 0.701524 0.216102 11.00000 -1.20000 H16B 2 0.648555 0.637291 0.173006 11.00000 -1.20000 AFIX 0 C17 1 0.548491 0.742554 0.057362 11.00000 0.01730 0.01985 = 0.02221 -0.00099 0.00006 0.00004 C18 1 0.539032 0.875130 0.048882 11.00000 0.02446 0.02476 = 0.01943 0.00344 0.00385 0.00295 AFIX 43 H18 2 0.509918 0.923268 0.063975 11.00000 -1.20000 AFIX 0 C19 1 0.571837 0.935139 0.018797 11.00000 0.02880 0.02538 = 0.02981 0.00620 0.00084 -0.00098 AFIX 43 H19 2 0.564653 1.024080 0.013253 11.00000 -1.20000 AFIX 0 C20 1 0.614906 0.868014 -0.003359 11.00000 0.02975 0.03077 = 0.02731 0.00741 0.00790 -0.00393 AFIX 43 H20 2 0.637163 0.910472 -0.023973 11.00000 -1.20000 AFIX 0 C21 1 0.625489 0.737652 0.004723 11.00000 0.03800 0.02539 = 0.03365 -0.00407 0.01542 -0.00094 AFIX 43 H21 2 0.654992 0.690797 -0.010436 11.00000 -1.20000 AFIX 0 C22 1 0.592962 0.676208 0.034903 11.00000 0.02593 0.01955 = 0.03287 -0.00087 0.00789 -0.00057 AFIX 43 H22 2 0.600938 0.587582 0.040470 11.00000 -1.20000 AFIX 0 C23 1 0.523787 0.498128 0.092481 11.00000 0.01548 0.01960 = 0.01638 0.00077 0.00011 -0.00056 C24 1 0.557517 0.431207 0.120954 11.00000 0.03844 0.02095 = 0.02685 -0.00175 -0.01270 0.00335 AFIX 43 H24 2 0.572048 0.475451 0.143971 11.00000 -1.20000 AFIX 0 C25 1 0.570442 0.299115 0.116202 11.00000 0.05029 0.02258 = 0.03981 -0.00008 -0.01207 0.00803 AFIX 43 H25 2 0.593202 0.253960 0.136025 11.00000 -1.20000 AFIX 0 C26 1 0.550089 0.235494 0.082833 11.00000 0.04368 0.01682 = 0.03016 -0.00306 0.00408 -0.00066 AFIX 43 H26 2 0.559674 0.146515 0.079208 11.00000 -1.20000 AFIX 0 C27 1 0.515708 0.300044 0.054439 11.00000 0.02604 0.02606 = 0.02170 -0.00439 0.00594 -0.00642 AFIX 43 H27 2 0.501074 0.255180 0.031564 11.00000 -1.20000 AFIX 0 C28 1 0.502692 0.429286 0.059320 11.00000 0.02103 0.02505 = 0.02011 0.00142 0.00333 0.00274 AFIX 43 H28 2 0.478811 0.472747 0.039694 11.00000 -1.20000 AFIX 0 C29 1 0.385057 1.021036 0.166323 11.00000 0.01443 0.01664 = 0.02150 -0.00114 -0.00214 0.00037 C30 1 0.350466 1.089480 0.194408 11.00000 0.02153 0.02146 = 0.02312 0.00024 -0.00035 -0.00064 AFIX 43 H30 2 0.331492 1.044441 0.215865 11.00000 -1.20000 AFIX 0 C31 1 0.343490 1.223383 0.191271 11.00000 0.03093 0.02149 = 0.02853 -0.00597 -0.00172 0.00582 AFIX 43 H31 2 0.320101 1.269187 0.210639 11.00000 -1.20000 AFIX 0 C32 1 0.370546 1.289174 0.160064 11.00000 0.02446 0.01722 = 0.03828 0.00020 -0.00613 0.00127 AFIX 43 H32 2 0.366829 1.380664 0.158365 11.00000 -1.20000 AFIX 0 C33 1 0.402802 1.222747 0.131483 11.00000 0.02462 0.02382 = 0.03878 0.01026 0.00420 -0.00021 AFIX 43 H33 2 0.420290 1.267924 0.109529 11.00000 -1.20000 AFIX 0 C34 1 0.409974 1.089495 0.134555 11.00000 0.02019 0.02171 = 0.02730 0.00285 0.00612 0.00490 AFIX 43 H34 2 0.432351 1.044401 0.114537 11.00000 -1.20000 AFIX 0 C35 1 0.363234 0.797420 0.215459 11.00000 0.02012 0.01978 = 0.01962 0.00317 -0.00176 0.00401 C36 1 0.320493 0.696849 0.216113 11.00000 0.01933 0.02536 = 0.02161 0.00187 -0.00153 -0.00394 AFIX 43 H36 2 0.309136 0.656055 0.191776 11.00000 -1.20000 AFIX 0 C37 1 0.294181 0.655088 0.251618 11.00000 0.02178 0.03517 = 0.02671 0.00676 0.00325 -0.00716 AFIX 43 H37 2 0.266087 0.584588 0.251504 11.00000 -1.20000 AFIX 0 C38 1 0.308808 0.715993 0.287185 11.00000 0.03453 0.04023 = 0.01640 0.00519 0.00463 0.00231 AFIX 43 H38 2 0.290450 0.688463 0.311494 11.00000 -1.20000 AFIX 0 C39 1 0.350910 0.818526 0.286978 11.00000 0.03647 0.03125 = 0.02040 -0.00185 -0.00506 0.00339 AFIX 43 H39 2 0.360355 0.862803 0.311078 11.00000 -1.20000 AFIX 0 C40 1 0.378525 0.854972 0.251881 11.00000 0.02988 0.02124 = 0.02456 0.00043 -0.00188 -0.00341 AFIX 43 H40 2 0.408881 0.921175 0.252366 11.00000 -1.20000 AFIX 0 H1N 2 0.456932 0.519514 0.160954 11.00000 0.01707 H2N 2 0.422533 0.585110 0.187042 11.00000 0.01392 PART 1 PART 0 H1 2 0.376179 0.480490 0.079138 11.00000 0.04165 H2 2 0.309615 0.554425 0.131917 11.00000 0.03155 H9 2 0.559494 0.587203 0.204253 11.00000 0.02281 H10 2 0.499960 0.723459 0.240708 11.00000 0.02725 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM fjl231as in Pbca REM R1 = 0.0419 for 8274 Fo > 4sig(Fo) and 0.0488 for all 9153 data REM 431 parameters refined using 19 restraints END ; 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 0.403498(10) 0.70758(2) 0.115327(6) 0.01687(6) Uani 1 1 d . . . Ir2 Ir 0.500306(11) 0.75911(2) 0.162304(6) 0.01738(6) Uani 1 1 d . B . P1 P 0.50590(7) 0.66923(14) 0.09807(5) 0.0180(3) Uani 1 1 d . B . P2 P 0.39949(7) 0.84789(14) 0.16886(4) 0.0176(3) Uani 1 1 d . B . N1 N 0.4413(3) 0.5953(5) 0.16470(15) 0.0232(11) Uani 1 1 d D B . C1 C 0.3590(3) 0.5659(6) 0.07954(19) 0.0204(12) Uani 1 1 d D B . C2 C 0.3180(3) 0.6119(5) 0.10983(17) 0.0170(11) Uani 1 1 d D B . C3 C 0.2598(3) 0.6898(6) 0.1038(2) 0.0251(13) Uani 1 1 d . . . H3A H 0.2261 0.6281 0.0981 0.030 Uiso 1 1 calc R A 1 H3B H 0.2499 0.7324 0.1295 0.030 Uiso 1 1 calc R A 1 C4A C 0.2586(5) 0.7911(9) 0.0722(3) 0.0232(19) Uiso 0.70 1 d PD B 1 H4A1 H 0.2197 0.8407 0.0746 0.028 Uiso 0.70 1 calc PR B 1 H4A2 H 0.2585 0.7481 0.0458 0.028 Uiso 0.70 1 calc PR B 1 C5A C 0.3118(4) 0.8845(8) 0.0737(3) 0.0190(16) Uiso 0.70 1 d PD B 1 H5A1 H 0.3112 0.9285 0.1000 0.023 Uiso 0.70 1 calc PR B 1 H5A2 H 0.3054 0.9515 0.0530 0.023 Uiso 0.70 1 calc PR B 1 C6A C 0.3747(4) 0.8247(8) 0.0677(3) 0.0139(18) Uiso 0.70 1 d PD B 1 H6 H 0.408(3) 0.882(7) 0.061(3) 0.017 Uiso 0.70 1 d PD C 1 C7A C 0.3785(6) 0.7480(12) 0.0288(4) 0.024(3) Uiso 0.70 1 d PD B 1 H7A1 H 0.4218 0.7445 0.0196 0.029 Uiso 0.70 1 calc PR B 1 H7A2 H 0.3537 0.7915 0.0080 0.029 Uiso 0.70 1 calc PR B 1 C15B C 0.6550(12) 0.850(3) 0.1796(9) 0.035(7) Uiso 0.30 1 d PD B 2 H15A H 0.6547 0.9045 0.2040 0.042 Uiso 0.30 1 calc PR B 2 H15B H 0.6980 0.8466 0.1697 0.042 Uiso 0.30 1 calc PR B 2 C14B C 0.6162(11) 0.914(3) 0.1486(7) 0.047(7) Uiso 0.30 1 d PD B 2 H14A H 0.6175 0.8608 0.1241 0.056 Uiso 0.30 1 calc PR B 2 H14B H 0.6347 0.9992 0.1421 0.056 Uiso 0.30 1 calc PR B 2 C13B C 0.5491(9) 0.935(2) 0.1598(6) 0.014(5) Uiso 0.30 1 d PD B 2 C12B C 0.5447(16) 1.001(3) 0.2014(7) 0.030(10) Uiso 0.30 1 d PD B 2 H12A H 0.5053 1.0485 0.2033 0.036 Uiso 0.30 1 calc PR B 2 H12B H 0.5785 1.0646 0.2041 0.036 Uiso 0.30 1 calc PR B 2 C8 C 0.3531(3) 0.6031(6) 0.03576(19) 0.0263(14) Uani 1 1 d . . . H8A H 0.3094 0.5982 0.0275 0.032 Uiso 1 1 calc R B 1 H8B H 0.3769 0.5416 0.0191 0.032 Uiso 1 1 calc R B 1 C9 C 0.5668(3) 0.6792(6) 0.2011(2) 0.0261(14) Uani 1 1 d D . . C10 C 0.5280(3) 0.7664(6) 0.22313(17) 0.0228(13) Uani 1 1 d D B . C11 C 0.5488(3) 0.9005(7) 0.2372(2) 0.0301(15) Uani 1 1 d D . . H11A H 0.5269 0.9222 0.2623 0.036 Uiso 1 1 calc R B 1 H11B H 0.5934 0.8976 0.2432 0.036 Uiso 1 1 calc R B 1 C12A C 0.5371(7) 1.0053(12) 0.2071(4) 0.023(3) Uiso 0.70 1 d PD B 1 H12C H 0.4965 1.0453 0.2127 0.027 Uiso 0.70 1 calc PR B 1 H12D H 0.5688 1.0733 0.2101 0.027 Uiso 0.70 1 calc PR B 1 C13A C 0.5378(5) 0.9568(11) 0.1653(3) 0.018(2) Uiso 0.70 1 d PD B 1 H13A H 0.523(5) 0.998(10) 0.150(3) 0.022 Uiso 0.70 1 d P D 1 C14A C 0.5832(4) 0.8755(8) 0.1497(3) 0.0190(17) Uiso 0.70 1 d PD B 1 H14 H 0.591(4) 0.883(9) 0.1215(8) 0.023 Uiso 0.70 1 d PD E 1 C15A C 0.6414(5) 0.8350(10) 0.1722(3) 0.024(2) Uiso 0.70 1 d PD B 1 H15C H 0.6765 0.8317 0.1533 0.029 Uiso 0.70 1 calc PR B 1 H15D H 0.6509 0.9002 0.1929 0.029 Uiso 0.70 1 calc PR B 1 C4B C 0.2771(11) 0.825(3) 0.0795(9) 0.046(7) Uiso 0.30 1 d PD B 2 H4B1 H 0.2676 0.8131 0.0508 0.055 Uiso 0.30 1 calc PR B 2 H4B2 H 0.2511 0.8961 0.0897 0.055 Uiso 0.30 1 calc PR B 2 C5B C 0.3421(10) 0.860(2) 0.0840(6) 0.026(5) Uiso 0.30 1 d PD B 2 C6B C 0.3898(11) 0.817(2) 0.0597(7) 0.027(6) Uiso 0.30 1 d PD B 2 C7B C 0.3825(13) 0.720(3) 0.0261(7) 0.022(7) Uiso 0.30 1 d PD B 2 H7B1 H 0.3589 0.7623 0.0044 0.027 Uiso 0.30 1 calc PR B 2 H7B2 H 0.4239 0.6999 0.0155 0.027 Uiso 0.30 1 calc PR B 2 C16 C 0.6332(3) 0.7053(7) 0.1913(2) 0.0273(13) Uani 1 1 d . B . H16A H 0.6580 0.7015 0.2161 0.033 Uiso 1 1 calc R F 1 H16B H 0.6486 0.6373 0.1730 0.033 Uiso 1 1 calc R F 1 C17 C 0.5485(3) 0.7426(6) 0.05736(18) 0.0198(12) Uani 1 1 d . . . C18 C 0.5390(3) 0.8751(6) 0.04888(18) 0.0229(13) Uani 1 1 d . B . H18 H 0.5099 0.9233 0.0640 0.027 Uiso 1 1 calc R . . C19 C 0.5718(3) 0.9351(6) 0.0188(2) 0.0280(14) Uani 1 1 d . . . H19 H 0.5647 1.0241 0.0133 0.034 Uiso 1 1 calc R B . C20 C 0.6149(3) 0.8680(7) -0.0034(2) 0.0293(14) Uani 1 1 d . B . H20 H 0.6372 0.9105 -0.0240 0.035 Uiso 1 1 calc R . . C21 C 0.6255(3) 0.7377(7) 0.0047(2) 0.0323(15) Uani 1 1 d . . . H21 H 0.6550 0.6908 -0.0104 0.039 Uiso 1 1 calc R B . C22 C 0.5930(3) 0.6762(6) 0.0349(2) 0.0261(13) Uani 1 1 d . B . H22 H 0.6009 0.5876 0.0405 0.031 Uiso 1 1 calc R . . C23 C 0.5238(3) 0.4981(6) 0.09248(17) 0.0172(11) Uani 1 1 d . . . C24 C 0.5575(3) 0.4312(6) 0.1210(2) 0.0287(14) Uani 1 1 d . B . H24 H 0.5720 0.4755 0.1440 0.034 Uiso 1 1 calc R . . C25 C 0.5704(4) 0.2991(7) 0.1162(2) 0.0376(17) Uani 1 1 d . . . H25 H 0.5932 0.2540 0.1360 0.045 Uiso 1 1 calc R B . C26 C 0.5501(3) 0.2355(6) 0.0828(2) 0.0302(15) Uani 1 1 d . B . H26 H 0.5597 0.1465 0.0792 0.036 Uiso 1 1 calc R . . C27 C 0.5157(3) 0.3000(6) 0.05444(19) 0.0246(13) Uani 1 1 d . . . H27 H 0.5011 0.2552 0.0316 0.030 Uiso 1 1 calc R B . C28 C 0.5027(3) 0.4293(6) 0.05932(18) 0.0221(12) Uani 1 1 d . B . H28 H 0.4788 0.4727 0.0397 0.026 Uiso 1 1 calc R . . C29 C 0.3851(3) 1.0210(5) 0.16632(17) 0.0175(11) Uani 1 1 d . . . C30 C 0.3505(3) 1.0895(6) 0.19441(19) 0.0220(12) Uani 1 1 d . B . H30 H 0.3315 1.0444 0.2159 0.026 Uiso 1 1 calc R . . C31 C 0.3435(3) 1.2234(6) 0.1913(2) 0.0270(14) Uani 1 1 d . . . H31 H 0.3201 1.2692 0.2106 0.032 Uiso 1 1 calc R B . C32 C 0.3705(3) 1.2892(6) 0.1601(2) 0.0267(13) Uani 1 1 d . B . H32 H 0.3668 1.3807 0.1584 0.032 Uiso 1 1 calc R . . C33 C 0.4028(3) 1.2227(6) 0.1315(2) 0.0291(14) Uani 1 1 d . . . H33 H 0.4203 1.2679 0.1095 0.035 Uiso 1 1 calc R B . C34 C 0.4100(3) 1.0895(6) 0.13456(19) 0.0231(13) Uani 1 1 d . B . H34 H 0.4324 1.0444 0.1145 0.028 Uiso 1 1 calc R . . C35 C 0.3632(3) 0.7974(6) 0.21546(17) 0.0198(11) Uani 1 1 d . . . C36 C 0.3205(3) 0.6968(6) 0.21611(18) 0.0221(12) Uani 1 1 d . B . H36 H 0.3091 0.6561 0.1918 0.027 Uiso 1 1 calc R . . C37 C 0.2942(3) 0.6551(7) 0.25162(19) 0.0279(14) Uani 1 1 d . . . H37 H 0.2661 0.5846 0.2515 0.033 Uiso 1 1 calc R B . C38 C 0.3088(3) 0.7160(7) 0.28719(19) 0.0304(14) Uani 1 1 d . B . H38 H 0.2905 0.6885 0.3115 0.036 Uiso 1 1 calc R . . C39 C 0.3509(3) 0.8185(7) 0.28698(19) 0.0294(14) Uani 1 1 d . . . H39 H 0.3604 0.8628 0.3111 0.035 Uiso 1 1 calc R B . C40 C 0.3785(3) 0.8550(6) 0.25188(19) 0.0252(13) Uani 1 1 d . B . H40 H 0.4089 0.9212 0.2524 0.030 Uiso 1 1 calc R . . H1N H 0.457(3) 0.520(3) 0.1610(19) 0.017(17) Uiso 1 1 d D . . H2N H 0.423(3) 0.585(6) 0.1870(11) 0.014(16) Uiso 1 1 d D . . H1 H 0.376(3) 0.480(4) 0.079(2) 0.04(2) Uiso 1 1 d D . . H2 H 0.310(3) 0.554(6) 0.1319(15) 0.03(2) Uiso 1 1 d D . . H9 H 0.559(3) 0.587(2) 0.204(2) 0.023(18) Uiso 1 1 d D . . H10 H 0.500(3) 0.723(6) 0.2407(17) 0.027(19) 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 Ir1 0.01911(11) 0.01530(10) 0.01619(10) 0.00163(8) -0.00026(9) -0.00197(8) Ir2 0.01982(11) 0.01515(10) 0.01717(11) 0.00209(8) -0.00130(8) -0.00141(8) P1 0.0170(7) 0.0173(7) 0.0198(7) 0.0035(5) 0.0021(6) 0.0022(6) P2 0.0173(7) 0.0169(7) 0.0187(7) 0.0021(5) 0.0024(6) 0.0009(6) N1 0.041(3) 0.014(2) 0.014(2) 0.0019(19) 0.008(2) -0.002(2) C1 0.021(3) 0.015(3) 0.025(3) -0.001(2) -0.001(2) -0.002(2) C2 0.015(3) 0.015(3) 0.022(3) 0.002(2) -0.001(2) -0.003(2) C3 0.020(3) 0.023(3) 0.032(3) -0.004(3) 0.000(2) 0.001(2) C8 0.025(3) 0.028(3) 0.026(3) -0.008(3) -0.003(3) 0.002(3) C9 0.023(3) 0.029(3) 0.027(3) 0.001(3) -0.010(3) 0.004(3) C10 0.025(3) 0.031(3) 0.012(3) 0.002(2) -0.002(2) 0.002(3) C11 0.022(3) 0.040(4) 0.027(3) -0.015(3) -0.001(3) 0.000(3) C16 0.026(3) 0.030(3) 0.027(3) -0.001(3) -0.002(3) 0.002(3) C17 0.017(3) 0.020(3) 0.022(3) -0.001(2) 0.000(2) 0.000(2) C18 0.024(3) 0.025(3) 0.019(3) 0.003(2) 0.004(2) 0.003(2) C19 0.029(3) 0.025(3) 0.030(3) 0.006(3) 0.001(3) -0.001(3) C20 0.030(4) 0.031(3) 0.027(3) 0.007(3) 0.008(3) -0.004(3) C21 0.038(4) 0.025(3) 0.034(4) -0.004(3) 0.015(3) -0.001(3) C22 0.026(3) 0.020(3) 0.033(3) -0.001(3) 0.008(3) -0.001(2) C23 0.015(3) 0.020(3) 0.016(3) 0.001(2) 0.000(2) -0.001(2) C24 0.038(4) 0.021(3) 0.027(3) -0.002(3) -0.013(3) 0.003(3) C25 0.050(4) 0.023(3) 0.040(4) 0.000(3) -0.012(4) 0.008(3) C26 0.044(4) 0.017(3) 0.030(3) -0.003(3) 0.004(3) -0.001(3) C27 0.026(3) 0.026(3) 0.022(3) -0.004(3) 0.006(2) -0.006(2) C28 0.021(3) 0.025(3) 0.020(3) 0.001(2) 0.003(2) 0.003(2) C29 0.014(3) 0.017(3) 0.021(3) -0.001(2) -0.002(2) 0.000(2) C30 0.022(3) 0.021(3) 0.023(3) 0.000(2) 0.000(2) -0.001(2) C31 0.031(3) 0.021(3) 0.029(3) -0.006(3) -0.002(3) 0.006(3) C32 0.024(3) 0.017(3) 0.038(4) 0.000(3) -0.006(3) 0.001(2) C33 0.025(3) 0.024(3) 0.039(4) 0.010(3) 0.004(3) 0.000(3) C34 0.020(3) 0.022(3) 0.027(3) 0.003(2) 0.006(2) 0.005(2) C35 0.020(3) 0.020(3) 0.020(3) 0.003(2) -0.002(2) 0.004(2) C36 0.019(3) 0.025(3) 0.022(3) 0.002(2) -0.002(2) -0.004(2) C37 0.022(3) 0.035(3) 0.027(3) 0.007(3) 0.003(3) -0.007(3) C38 0.035(4) 0.040(4) 0.016(3) 0.005(3) 0.005(3) 0.002(3) C39 0.036(4) 0.031(4) 0.020(3) -0.002(3) -0.005(3) 0.003(3) C40 0.030(3) 0.021(3) 0.025(3) 0.000(2) -0.002(3) -0.003(3) _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 C6A 2.098(9) . ? Ir1 C2 2.111(5) . ? Ir1 C1 2.124(6) . ? Ir1 N1 2.180(5) . ? Ir1 C6B 2.20(3) . ? Ir1 C5B 2.31(2) . ? Ir1 P2 2.3067(15) . ? Ir1 P1 2.3321(15) . ? Ir1 Ir2 2.6795(3) . ? Ir2 C13B 2.11(2) . ? Ir2 C9 2.111(6) . ? Ir2 C10 2.125(6) . ? Ir2 N1 2.125(5) . ? Ir2 C13A 2.200(10) . ? Ir2 C14A 2.205(9) . ? Ir2 P1 2.3459(15) . ? Ir2 P2 2.3841(15) . ? P1 C17 1.813(6) . ? P1 C23 1.819(6) . ? P2 C29 1.817(6) . ? P2 C35 1.824(6) . ? N1 H1N 0.86(2) . ? N1 H2N 0.86(2) . ? C1 C2 1.431(8) . ? C1 C8 1.521(9) . ? C1 H1 0.96(2) . ? C2 C3 1.512(8) . ? C2 H2 0.97(2) . ? C3 C4A 1.489(11) . ? C3 C4B 1.65(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4A C5A 1.505(12) . ? C4A H4A1 0.9900 . ? C4A H4A2 0.9900 . ? C5A C6A 1.515(12) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C6A C7A 1.525(15) . ? C6A H6 0.96(2) . ? C7A C8 1.612(14) . ? C7A H7A1 0.9900 . ? C7A H7A2 0.9900 . ? C15B C14B 1.49(3) . ? C15B C16 1.62(3) . ? C15B H15A 0.9900 . ? C15B H15B 0.9900 . ? C14B C13B 1.52(2) . ? C14B H14A 0.9900 . ? C14B H14B 0.9900 . ? C14B H14 1.11(7) . ? C13B C12B 1.55(3) . ? C13B H13A 0.92(10) . ? C12B C11 1.587(18) . ? C12B H12A 0.9900 . ? C12B H12B 0.9900 . ? C8 C7B 1.41(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.437(9) . ? C9 C16 1.505(9) . ? C9 H9 0.97(2) . ? C10 C11 1.531(9) . ? C10 H10 0.96(2) . ? C11 C12A 1.501(14) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12A C13A 1.487(16) . ? C12A H12C 0.9900 . ? C12A H12D 0.9900 . ? C13A C14A 1.398(13) . ? C13A H13A 0.74(10) . ? C14A C15A 1.530(14) . ? C14A H14 0.96(2) . ? C15A C16 1.495(12) . ? C15A H15C 0.9900 . ? C15A H15D 0.9900 . ? C4B C5B 1.47(3) . ? C4B H4B1 0.9900 . ? C4B H4B2 0.9900 . ? C5B C6B 1.39(2) . ? C6B C7B 1.51(2) . ? C6B H6 0.79(5) . ? C7B H7B1 0.9900 . ? C7B H7B2 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C22 1.403(8) . ? C17 C18 1.413(8) . ? C18 C19 1.381(9) . ? C18 H18 0.9500 . ? C19 C20 1.381(9) . ? C19 H19 0.9500 . ? C20 C21 1.392(9) . ? C20 H20 0.9500 . ? C21 C22 1.387(9) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.387(8) . ? C23 C28 1.396(8) . ? C24 C25 1.402(9) . ? C24 H24 0.9500 . ? C25 C26 1.370(10) . ? C25 H25 0.9500 . ? C26 C27 1.381(9) . ? C26 H26 0.9500 . ? C27 C28 1.374(9) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C34 1.387(8) . ? C29 C30 1.396(8) . ? C30 C31 1.395(8) . ? C30 H30 0.9500 . ? C31 C32 1.378(9) . ? C31 H31 0.9500 . ? C32 C33 1.370(9) . ? C32 H32 0.9500 . ? C33 C34 1.389(8) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 C36 1.393(8) . ? C35 C40 1.397(8) . ? C36 C37 1.388(8) . ? C36 H36 0.9500 . ? C37 C38 1.384(9) . ? C37 H37 0.9500 . ? C38 C39 1.399(10) . ? C38 H38 0.9500 . ? C39 C40 1.372(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? 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 C6A Ir1 C2 86.6(3) . . ? C6A Ir1 C1 80.3(3) . . ? C2 Ir1 C1 39.5(2) . . ? C6A Ir1 N1 174.8(3) . . ? C2 Ir1 N1 98.5(2) . . ? C1 Ir1 N1 103.5(2) . . ? C6A Ir1 C6B 11.1(6) . . ? C2 Ir1 C6B 92.7(6) . . ? C1 Ir1 C6B 79.3(6) . . ? N1 Ir1 C6B 165.2(6) . . ? C6A Ir1 C5B 24.7(5) . . ? C2 Ir1 C5B 76.8(5) . . ? C1 Ir1 C5B 87.1(5) . . ? N1 Ir1 C5B 157.3(5) . . ? C6B Ir1 C5B 35.7(6) . . ? C6A Ir1 P2 102.6(3) . . ? C2 Ir1 P2 109.17(16) . . ? C1 Ir1 P2 148.67(17) . . ? N1 Ir1 P2 76.05(14) . . ? C6B Ir1 P2 109.3(6) . . ? C5B Ir1 P2 84.5(5) . . ? C6A Ir1 P1 101.1(3) . . ? C2 Ir1 P1 137.55(16) . . ? C1 Ir1 P1 100.20(17) . . ? N1 Ir1 P1 74.86(15) . . ? C6B Ir1 P1 90.4(6) . . ? C5B Ir1 P1 123.6(5) . . ? P2 Ir1 P1 109.59(5) . . ? C6A Ir1 Ir2 124.5(2) . . ? C2 Ir1 Ir2 146.54(16) . . ? C1 Ir1 Ir2 145.60(17) . . ? N1 Ir1 Ir2 50.58(14) . . ? C6B Ir1 Ir2 120.1(6) . . ? C5B Ir1 Ir2 125.7(5) . . ? P2 Ir1 Ir2 56.53(4) . . ? P1 Ir1 Ir2 55.30(4) . . ? C13B Ir2 C9 91.1(6) . . ? C13B Ir2 C10 82.3(6) . . ? C9 Ir2 C10 39.7(2) . . ? C13B Ir2 N1 173.0(6) . . ? C9 Ir2 N1 94.5(2) . . ? C10 Ir2 N1 99.4(2) . . ? C13B Ir2 C13A 9.8(6) . . ? C9 Ir2 C13A 94.7(3) . . ? C10 Ir2 C13A 79.5(3) . . ? N1 Ir2 C13A 163.8(3) . . ? C13B Ir2 C14A 27.3(6) . . ? C9 Ir2 C14A 76.9(3) . . ? C10 Ir2 C14A 86.2(3) . . ? N1 Ir2 C14A 159.1(3) . . ? C13A Ir2 C14A 37.0(3) . . ? C13B Ir2 P1 106.2(6) . . ? C9 Ir2 P1 111.98(19) . . ? C10 Ir2 P1 151.43(18) . . ? N1 Ir2 P1 75.58(14) . . ? C13A Ir2 P1 113.0(3) . . ? C14A Ir2 P1 89.9(2) . . ? C13B Ir2 P2 97.6(6) . . ? C9 Ir2 P2 136.22(19) . . ? C10 Ir2 P2 99.09(18) . . ? N1 Ir2 P2 75.42(16) . . ? C13A Ir2 P2 88.8(3) . . ? C14A Ir2 P2 123.9(2) . . ? P1 Ir2 P2 106.51(5) . . ? C13B Ir2 Ir1 122.9(5) . . ? C9 Ir2 Ir1 145.14(18) . . ? C10 Ir2 Ir1 142.36(18) . . ? N1 Ir2 Ir1 52.43(15) . . ? C13A Ir2 Ir1 120.1(3) . . ? C14A Ir2 Ir1 129.5(2) . . ? P1 Ir2 Ir1 54.81(4) . . ? P2 Ir2 Ir1 53.82(4) . . ? C17 P1 C23 102.7(3) . . ? C17 P1 Ir1 127.0(2) . . ? C23 P1 Ir1 113.21(19) . . ? C17 P1 Ir2 123.4(2) . . ? C23 P1 Ir2 119.33(19) . . ? Ir1 P1 Ir2 69.89(4) . . ? C29 P2 C35 104.3(3) . . ? C29 P2 Ir1 126.0(2) . . ? C35 P2 Ir1 120.1(2) . . ? C29 P2 Ir2 122.2(2) . . ? C35 P2 Ir2 111.43(19) . . ? Ir1 P2 Ir2 69.65(4) . . ? Ir2 N1 Ir1 76.99(16) . . ? Ir2 N1 H1N 119(4) . . ? Ir1 N1 H1N 121(4) . . ? Ir2 N1 H2N 115(4) . . ? Ir1 N1 H2N 123(4) . . ? H1N N1 H2N 102(6) . . ? C2 C1 C8 123.2(5) . . ? C2 C1 Ir1 69.8(3) . . ? C8 C1 Ir1 114.1(4) . . ? C2 C1 H1 124(5) . . ? C8 C1 H1 105(5) . . ? Ir1 C1 H1 118(5) . . ? C1 C2 C3 127.0(5) . . ? C1 C2 Ir1 70.7(3) . . ? C3 C2 Ir1 119.9(4) . . ? C1 C2 H2 117(4) . . ? C3 C2 H2 106(4) . . ? Ir1 C2 H2 113(4) . . ? C4A C3 C2 118.9(6) . . ? C2 C3 C4B 108.9(10) . . ? C4A C3 H3A 107.6 . . ? C2 C3 H3A 107.6 . . ? C4B C3 H3A 127.9 . . ? C4A C3 H3B 107.6 . . ? C2 C3 H3B 107.6 . . ? C4B C3 H3B 95.9 . . ? H3A C3 H3B 107.0 . . ? C3 C4A C5A 114.3(7) . . ? C3 C4A H4A1 108.7 . . ? C5A C4A H4A1 108.7 . . ? C3 C4A H4A2 108.7 . . ? C5A C4A H4A2 108.7 . . ? H4A1 C4A H4A2 107.6 . . ? C4A C5A C6A 115.3(7) . . ? C4A C5A H5A1 108.4 . . ? C6A C5A H5A1 108.5 . . ? C4A C5A H5A2 108.5 . . ? C6A C5A H5A2 108.4 . . ? H5A1 C5A H5A2 107.5 . . ? C5A C6A C7A 112.0(8) . . ? C5A C6A Ir1 113.7(7) . . ? C7A C6A Ir1 109.5(7) . . ? C5A C6A H6 118(6) . . ? C7A C6A H6 95(6) . . ? Ir1 C6A H6 107(5) . . ? C6A C7A C8 109.9(9) . . ? C6A C7A H7A1 109.7 . . ? C8 C7A H7A1 109.7 . . ? C6A C7A H7A2 109.7 . . ? C8 C7A H7A2 109.7 . . ? H7A1 C7A H7A2 108.2 . . ? C14B C15B C16 114(2) . . ? C14B C15B H15A 108.7 . . ? C16 C15B H15A 108.7 . . ? C14B C15B H15B 108.7 . . ? C16 C15B H15B 108.7 . . ? H15A C15B H15B 107.6 . . ? C15B C14B C13B 115.8(19) . . ? C15B C14B H14A 108.3 . . ? C13B C14B H14A 108.3 . . ? C15B C14B H14B 108.3 . . ? C13B C14B H14B 108.3 . . ? H14A C14B H14B 107.4 . . ? C15B C14B H14 136(6) . . ? C13B C14B H14 77(4) . . ? H14B C14B H14 106.3 . . ? C14B C13B C12B 110.0(18) . . ? C14B C13B Ir2 111.5(17) . . ? C12B C13B Ir2 108.0(16) . . ? C14B C13B H13A 127(7) . . ? C12B C13B H13A 89(7) . . ? Ir2 C13B H13A 108(6) . . ? C13B C12B C11 113.0(18) . . ? C13B C12B H12A 109.0 . . ? C11 C12B H12A 109.0 . . ? C13B C12B H12B 109.0 . . ? C11 C12B H12B 109.0 . . ? H12A C12B H12B 107.8 . . ? C7B C8 C1 113.6(11) . . ? C1 C8 C7A 110.1(6) . . ? C7B C8 H8A 114.5 . . ? C1 C8 H8A 109.6 . . ? C7A C8 H8A 109.6 . . ? C7B C8 H8B 100.7 . . ? C1 C8 H8B 109.6 . . ? C7A C8 H8B 109.6 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C16 124.2(6) . . ? C10 C9 Ir2 70.7(3) . . ? C16 C9 Ir2 116.8(4) . . ? C10 C9 H9 118(4) . . ? C16 C9 H9 111(4) . . ? Ir2 C9 H9 110(4) . . ? C9 C10 C11 123.5(6) . . ? C9 C10 Ir2 69.6(3) . . ? C11 C10 Ir2 114.3(4) . . ? C9 C10 H10 113(4) . . ? C11 C10 H10 115(4) . . ? Ir2 C10 H10 113(4) . . ? C12A C11 C10 113.3(7) . . ? C10 C11 C12B 110.0(13) . . ? C12A C11 H11A 108.9 . . ? C10 C11 H11A 108.9 . . ? C12B C11 H11A 117.7 . . ? C12A C11 H11B 108.9 . . ? C10 C11 H11B 108.9 . . ? C12B C11 H11B 103.1 . . ? H11A C11 H11B 107.7 . . ? C13A C12A C11 112.8(10) . . ? C13A C12A H12C 109.0 . . ? C11 C12A H12C 109.0 . . ? C13A C12A H12D 109.0 . . ? C11 C12A H12D 109.0 . . ? H12C C12A H12D 107.8 . . ? C14A C13A C12A 124.2(9) . . ? C14A C13A Ir2 71.7(6) . . ? C12A C13A Ir2 110.6(7) . . ? C14A C13A H13A 113(8) . . ? C12A C13A H13A 117(8) . . ? Ir2 C13A H13A 110(8) . . ? C13A C14A C15A 124.3(8) . . ? C13A C14A Ir2 71.3(6) . . ? C15A C14A Ir2 115.5(6) . . ? C13A C14A H14 116(6) . . ? C15A C14A H14 111(6) . . ? Ir2 C14A H14 112(6) . . ? C16 C15A C14A 111.0(8) . . ? C16 C15A H15C 109.4 . . ? C14A C15A H15C 109.4 . . ? C16 C15A H15D 109.5 . . ? C14A C15A H15D 109.4 . . ? H15C C15A H15D 108.0 . . ? C5B C4B C3 112(2) . . ? C5B C4B H4B1 109.2 . . ? C3 C4B H4B1 109.2 . . ? C5B C4B H4B2 109.2 . . ? C3 C4B H4B2 109.2 . . ? H4B1 C4B H4B2 107.9 . . ? C6B C5B C4B 125.5(19) . . ? C6B C5B Ir1 67.7(14) . . ? C4B C5B Ir1 115.8(17) . . ? C5B C6B C7B 124.6(19) . . ? C5B C6B Ir1 76.6(15) . . ? C7B C6B Ir1 107.8(17) . . ? C5B C6B H6 94(7) . . ? C7B C6B H6 132(7) . . ? Ir1 C6B H6 108(7) . . ? C8 C7B C6B 116(2) . . ? C8 C7B H7B1 108.2 . . ? C6B C7B H7B1 108.2 . . ? C8 C7B H7B2 108.2 . . ? C6B C7B H7B2 108.2 . . ? H7B1 C7B H7B2 107.3 . . ? C15A C16 C9 111.6(7) . . ? C9 C16 C15B 120.0(10) . . ? C15A C16 H16A 109.3 . . ? C9 C16 H16A 109.3 . . ? C15B C16 H16A 94.7 . . ? C15A C16 H16B 109.3 . . ? C9 C16 H16B 109.3 . . ? C15B C16 H16B 114.1 . . ? H16A C16 H16B 108.0 . . ? C22 C17 C18 117.7(6) . . ? C22 C17 P1 123.4(5) . . ? C18 C17 P1 118.8(5) . . ? C19 C18 C17 120.4(6) . . ? C19 C18 H18 119.8 . . ? C17 C18 H18 119.8 . . ? C18 C19 C20 121.1(6) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C19 C20 C21 119.5(6) . . ? C19 C20 H20 120.2 . . ? C21 C20 H20 120.2 . . ? C22 C21 C20 120.0(6) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C17 121.2(6) . . ? C21 C22 H22 119.4 . . ? C17 C22 H22 119.4 . . ? C24 C23 C28 117.8(6) . . ? C24 C23 P1 121.7(5) . . ? C28 C23 P1 120.4(4) . . ? C23 C24 C25 120.8(6) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 119.7(7) . . ? C26 C25 H25 120.2 . . ? C24 C25 H25 120.2 . . ? C25 C26 C27 120.3(6) . . ? C25 C26 H26 119.8 . . ? C27 C26 H26 119.8 . . ? C28 C27 C26 119.9(6) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C27 C28 C23 121.5(6) . . ? C27 C28 H28 119.3 . . ? C23 C28 H28 119.3 . . ? C34 C29 C30 117.9(5) . . ? C34 C29 P2 118.0(4) . . ? C30 C29 P2 124.0(5) . . ? C31 C30 C29 120.6(6) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C32 C31 C30 120.0(6) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C33 C32 C31 120.1(6) . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.1(6) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C29 C34 C33 121.2(6) . . ? C29 C34 H34 119.4 . . ? C33 C34 H34 119.4 . . ? C36 C35 C40 117.5(6) . . ? C36 C35 P2 120.9(5) . . ? C40 C35 P2 121.5(5) . . ? C37 C36 C35 121.3(6) . . ? C37 C36 H36 119.4 . . ? C35 C36 H36 119.4 . . ? C38 C37 C36 120.1(6) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 119.3(6) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C40 C39 C38 119.8(6) . . ? C40 C39 H39 120.1 . . ? C38 C39 H39 120.1 . . ? C39 C40 C35 121.8(6) . . ? C39 C40 H40 119.1 . . ? C35 C40 H40 119.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6A Ir1 Ir2 C13B 8.2(8) . . . . ? C2 Ir1 Ir2 C13B -147.3(8) . . . . ? C1 Ir1 Ir2 C13B 138.2(8) . . . . ? N1 Ir1 Ir2 C13B -173.7(7) . . . . ? C6B Ir1 Ir2 C13B 20.3(10) . . . . ? C5B Ir1 Ir2 C13B -22.1(9) . . . . ? P2 Ir1 Ir2 C13B -74.0(7) . . . . ? P1 Ir1 Ir2 C13B 87.2(7) . . . . ? C6A Ir1 Ir2 C9 -156.9(5) . . . . ? C2 Ir1 Ir2 C9 47.6(4) . . . . ? C1 Ir1 Ir2 C9 -26.9(4) . . . . ? N1 Ir1 Ir2 C9 21.3(4) . . . . ? C6B Ir1 Ir2 C9 -144.7(8) . . . . ? C5B Ir1 Ir2 C9 172.9(7) . . . . ? P2 Ir1 Ir2 C9 121.0(3) . . . . ? P1 Ir1 Ir2 C9 -77.8(3) . . . . ? C6A Ir1 Ir2 C10 133.2(4) . . . . ? C2 Ir1 Ir2 C10 -22.3(4) . . . . ? C1 Ir1 Ir2 C10 -96.8(4) . . . . ? N1 Ir1 Ir2 C10 -48.6(3) . . . . ? C6B Ir1 Ir2 C10 145.4(7) . . . . ? C5B Ir1 Ir2 C10 103.0(7) . . . . ? P2 Ir1 Ir2 C10 51.1(3) . . . . ? P1 Ir1 Ir2 C10 -147.7(3) . . . . ? C6A Ir1 Ir2 N1 -178.1(4) . . . . ? C2 Ir1 Ir2 N1 26.4(3) . . . . ? C1 Ir1 Ir2 N1 -48.1(3) . . . . ? C6B Ir1 Ir2 N1 -166.0(7) . . . . ? C5B Ir1 Ir2 N1 151.6(6) . . . . ? P2 Ir1 Ir2 N1 99.74(19) . . . . ? P1 Ir1 Ir2 N1 -99.08(19) . . . . ? C6A Ir1 Ir2 C13A 19.2(5) . . . . ? C2 Ir1 Ir2 C13A -136.3(4) . . . . ? C1 Ir1 Ir2 C13A 149.2(5) . . . . ? N1 Ir1 Ir2 C13A -162.7(4) . . . . ? C6B Ir1 Ir2 C13A 31.3(8) . . . . ? C5B Ir1 Ir2 C13A -11.1(7) . . . . ? P2 Ir1 Ir2 C13A -63.0(3) . . . . ? P1 Ir1 Ir2 C13A 98.2(3) . . . . ? C6A Ir1 Ir2 C14A -24.9(4) . . . . ? C2 Ir1 Ir2 C14A 179.6(4) . . . . ? C1 Ir1 Ir2 C14A 105.1(4) . . . . ? N1 Ir1 Ir2 C14A 153.3(3) . . . . ? C6B Ir1 Ir2 C14A -12.7(7) . . . . ? C5B Ir1 Ir2 C14A -55.1(7) . . . . ? P2 Ir1 Ir2 C14A -107.0(3) . . . . ? P1 Ir1 Ir2 C14A 54.2(3) . . . . ? C6A Ir1 Ir2 P1 -79.0(3) . . . . ? C2 Ir1 Ir2 P1 125.4(3) . . . . ? C1 Ir1 Ir2 P1 50.9(3) . . . . ? N1 Ir1 Ir2 P1 99.08(19) . . . . ? C6B Ir1 Ir2 P1 -66.9(7) . . . . ? C5B Ir1 Ir2 P1 -109.3(6) . . . . ? P2 Ir1 Ir2 P1 -161.18(6) . . . . ? C6A Ir1 Ir2 P2 82.1(3) . . . . ? C2 Ir1 Ir2 P2 -73.4(3) . . . . ? C1 Ir1 Ir2 P2 -147.9(3) . . . . ? N1 Ir1 Ir2 P2 -99.74(19) . . . . ? C6B Ir1 Ir2 P2 94.3(7) . . . . ? C5B Ir1 Ir2 P2 51.9(6) . . . . ? P1 Ir1 Ir2 P2 161.18(6) . . . . ? C6A Ir1 P1 C17 7.1(4) . . . . ? C2 Ir1 P1 C17 104.4(3) . . . . ? C1 Ir1 P1 C17 89.2(3) . . . . ? N1 Ir1 P1 C17 -169.5(3) . . . . ? C6B Ir1 P1 C17 10.0(6) . . . . ? C5B Ir1 P1 C17 -4.1(6) . . . . ? P2 Ir1 P1 C17 -100.7(3) . . . . ? Ir2 Ir1 P1 C17 -117.3(3) . . . . ? C6A Ir1 P1 C23 -121.3(3) . . . . ? C2 Ir1 P1 C23 -24.0(3) . . . . ? C1 Ir1 P1 C23 -39.3(3) . . . . ? N1 Ir1 P1 C23 62.0(2) . . . . ? C6B Ir1 P1 C23 -118.5(6) . . . . ? C5B Ir1 P1 C23 -132.6(6) . . . . ? P2 Ir1 P1 C23 130.8(2) . . . . ? Ir2 Ir1 P1 C23 114.2(2) . . . . ? C6A Ir1 P1 Ir2 124.4(2) . . . . ? C2 Ir1 P1 Ir2 -138.3(2) . . . . ? C1 Ir1 P1 Ir2 -153.53(17) . . . . ? N1 Ir1 P1 Ir2 -52.21(14) . . . . ? C6B Ir1 P1 Ir2 127.3(6) . . . . ? C5B Ir1 P1 Ir2 113.2(6) . . . . ? P2 Ir1 P1 Ir2 16.60(5) . . . . ? C13B Ir2 P1 C17 2.7(6) . . . . ? C9 Ir2 P1 C17 -95.3(3) . . . . ? C10 Ir2 P1 C17 -101.2(4) . . . . ? N1 Ir2 P1 C17 175.7(3) . . . . ? C13A Ir2 P1 C17 10.2(4) . . . . ? C14A Ir2 P1 C17 -19.5(3) . . . . ? P2 Ir2 P1 C17 106.0(2) . . . . ? Ir1 Ir2 P1 C17 121.8(2) . . . . ? C13B Ir2 P1 C23 134.9(6) . . . . ? C9 Ir2 P1 C23 36.9(3) . . . . ? C10 Ir2 P1 C23 31.0(4) . . . . ? N1 Ir2 P1 C23 -52.1(3) . . . . ? C13A Ir2 P1 C23 142.4(4) . . . . ? C14A Ir2 P1 C23 112.7(3) . . . . ? P2 Ir2 P1 C23 -121.8(2) . . . . ? Ir1 Ir2 P1 C23 -106.0(2) . . . . ? C13B Ir2 P1 Ir1 -119.1(6) . . . . ? C9 Ir2 P1 Ir1 142.9(2) . . . . ? C10 Ir2 P1 Ir1 137.0(4) . . . . ? N1 Ir2 P1 Ir1 53.91(16) . . . . ? C13A Ir2 P1 Ir1 -111.6(3) . . . . ? C14A Ir2 P1 Ir1 -141.3(2) . . . . ? P2 Ir2 P1 Ir1 -15.76(5) . . . . ? C6A Ir1 P2 C29 -7.6(4) . . . . ? C2 Ir1 P2 C29 -98.4(3) . . . . ? C1 Ir1 P2 C29 -99.7(4) . . . . ? N1 Ir1 P2 C29 167.3(3) . . . . ? C6B Ir1 P2 C29 1.7(7) . . . . ? C5B Ir1 P2 C29 -24.5(6) . . . . ? P1 Ir1 P2 C29 99.3(2) . . . . ? Ir2 Ir1 P2 C29 115.6(2) . . . . ? C6A Ir1 P2 C35 133.2(4) . . . . ? C2 Ir1 P2 C35 42.4(3) . . . . ? C1 Ir1 P2 C35 41.1(4) . . . . ? N1 Ir1 P2 C35 -51.9(3) . . . . ? C6B Ir1 P2 C35 142.4(7) . . . . ? C5B Ir1 P2 C35 116.3(6) . . . . ? P1 Ir1 P2 C35 -120.0(2) . . . . ? Ir2 Ir1 P2 C35 -103.6(2) . . . . ? C6A Ir1 P2 Ir2 -123.2(3) . . . . ? C2 Ir1 P2 Ir2 145.99(16) . . . . ? C1 Ir1 P2 Ir2 144.7(3) . . . . ? N1 Ir1 P2 Ir2 51.68(16) . . . . ? C6B Ir1 P2 Ir2 -113.9(6) . . . . ? C5B Ir1 P2 Ir2 -140.1(5) . . . . ? P1 Ir1 P2 Ir2 -16.35(5) . . . . ? C13B Ir2 P2 C29 4.9(6) . . . . ? C9 Ir2 P2 C29 104.6(4) . . . . ? C10 Ir2 P2 C29 88.2(3) . . . . ? N1 Ir2 P2 C29 -174.3(3) . . . . ? C13A Ir2 P2 C29 9.1(4) . . . . ? C14A Ir2 P2 C29 -3.2(4) . . . . ? P1 Ir2 P2 C29 -104.6(2) . . . . ? Ir1 Ir2 P2 C29 -120.5(2) . . . . ? C13B Ir2 P2 C35 -119.1(6) . . . . ? C9 Ir2 P2 C35 -19.5(4) . . . . ? C10 Ir2 P2 C35 -35.8(3) . . . . ? N1 Ir2 P2 C35 61.6(3) . . . . ? C13A Ir2 P2 C35 -115.0(3) . . . . ? C14A Ir2 P2 C35 -127.3(3) . . . . ? P1 Ir2 P2 C35 131.4(2) . . . . ? Ir1 Ir2 P2 C35 115.4(2) . . . . ? C13B Ir2 P2 Ir1 125.5(6) . . . . ? C9 Ir2 P2 Ir1 -134.9(3) . . . . ? C10 Ir2 P2 Ir1 -151.23(18) . . . . ? N1 Ir2 P2 Ir1 -53.82(14) . . . . ? C13A Ir2 P2 Ir1 129.6(3) . . . . ? C14A Ir2 P2 Ir1 117.3(3) . . . . ? P1 Ir2 P2 Ir1 15.96(5) . . . . ? C9 Ir2 N1 Ir1 -168.0(2) . . . . ? C10 Ir2 N1 Ir1 152.3(2) . . . . ? C13A Ir2 N1 Ir1 67.6(11) . . . . ? C14A Ir2 N1 Ir1 -103.6(7) . . . . ? P1 Ir2 N1 Ir1 -56.44(10) . . . . ? P2 Ir2 N1 Ir1 55.28(11) . . . . ? C2 Ir1 N1 Ir2 -165.67(18) . . . . ? C1 Ir1 N1 Ir2 154.36(19) . . . . ? C6B Ir1 N1 Ir2 55(2) . . . . ? C5B Ir1 N1 Ir2 -89.7(14) . . . . ? P2 Ir1 N1 Ir2 -57.91(11) . . . . ? P1 Ir1 N1 Ir2 57.25(11) . . . . ? C6A Ir1 C1 C2 -96.5(4) . . . . ? N1 Ir1 C1 C2 87.1(4) . . . . ? C6B Ir1 C1 C2 -107.8(7) . . . . ? C5B Ir1 C1 C2 -72.6(6) . . . . ? P2 Ir1 C1 C2 1.9(5) . . . . ? P1 Ir1 C1 C2 163.8(3) . . . . ? Ir2 Ir1 C1 C2 123.4(3) . . . . ? C6A Ir1 C1 C8 21.8(5) . . . . ? C2 Ir1 C1 C8 118.3(6) . . . . ? N1 Ir1 C1 C8 -154.6(4) . . . . ? C6B Ir1 C1 C8 10.5(7) . . . . ? C5B Ir1 C1 C8 45.7(7) . . . . ? P2 Ir1 C1 C8 120.2(4) . . . . ? P1 Ir1 C1 C8 -77.9(4) . . . . ? Ir2 Ir1 C1 C8 -118.4(4) . . . . ? C8 C1 C2 C3 7.2(9) . . . . ? Ir1 C1 C2 C3 113.4(6) . . . . ? C8 C1 C2 Ir1 -106.2(6) . . . . ? C6A Ir1 C2 C1 78.9(4) . . . . ? N1 Ir1 C2 C1 -100.8(3) . . . . ? C6B Ir1 C2 C1 69.5(7) . . . . ? C5B Ir1 C2 C1 101.8(6) . . . . ? P2 Ir1 C2 C1 -179.0(3) . . . . ? P1 Ir1 C2 C1 -24.0(4) . . . . ? Ir2 Ir1 C2 C1 -121.1(3) . . . . ? C6A Ir1 C2 C3 -43.5(5) . . . . ? C1 Ir1 C2 C3 -122.3(6) . . . . ? N1 Ir1 C2 C3 136.8(5) . . . . ? C6B Ir1 C2 C3 -52.8(7) . . . . ? C5B Ir1 C2 C3 -20.6(7) . . . . ? P2 Ir1 C2 C3 58.7(5) . . . . ? P1 Ir1 C2 C3 -146.4(4) . . . . ? Ir2 Ir1 C2 C3 116.5(4) . . . . ? C1 C2 C3 C4A -37.9(9) . . . . ? Ir1 C2 C3 C4A 49.6(8) . . . . ? C1 C2 C3 C4B -57.6(14) . . . . ? Ir1 C2 C3 C4B 29.9(13) . . . . ? C2 C3 C4A C5A -50.8(10) . . . . ? C4B C3 C4A C5A 14(3) . . . . ? C3 C4A C5A C6A 62.3(10) . . . . ? C4A C5A C6A C7A 55.0(11) . . . . ? C4A C5A C6A Ir1 -69.8(8) . . . . ? C2 Ir1 C6A C5A 51.6(6) . . . . ? C1 Ir1 C6A C5A 90.8(6) . . . . ? C6B Ir1 C6A C5A 174(4) . . . . ? C5B Ir1 C6A C5A -13.5(13) . . . . ? P2 Ir1 C6A C5A -57.4(6) . . . . ? P1 Ir1 C6A C5A -170.6(5) . . . . ? Ir2 Ir1 C6A C5A -115.2(5) . . . . ? C2 Ir1 C6A C7A -74.6(7) . . . . ? C1 Ir1 C6A C7A -35.3(7) . . . . ? C6B Ir1 C6A C7A 48(4) . . . . ? C5B Ir1 C6A C7A -139.6(16) . . . . ? P2 Ir1 C6A C7A 176.5(7) . . . . ? P1 Ir1 C6A C7A 63.3(7) . . . . ? Ir2 Ir1 C6A C7A 118.7(6) . . . . ? C5A C6A C7A C8 -84.8(10) . . . . ? Ir1 C6A C7A C8 42.2(10) . . . . ? C16 C15B C14B C13B 62(3) . . . . ? C15B C14B C13B C12B 50(3) . . . . ? C15B C14B C13B Ir2 -70(3) . . . . ? C9 Ir2 C13B C14B 52.4(14) . . . . ? C10 Ir2 C13B C14B 91.2(14) . . . . ? C13A Ir2 C13B C14B 164(5) . . . . ? C14A Ir2 C13B C14B -5.5(12) . . . . ? P1 Ir2 C13B C14B -60.9(14) . . . . ? P2 Ir2 C13B C14B -170.6(13) . . . . ? Ir1 Ir2 C13B C14B -119.1(13) . . . . ? C9 Ir2 C13B C12B -68.6(15) . . . . ? C10 Ir2 C13B C12B -29.8(14) . . . . ? C13A Ir2 C13B C12B 43(4) . . . . ? C14A Ir2 C13B C12B -127(2) . . . . ? P1 Ir2 C13B C12B 178.1(14) . . . . ? P2 Ir2 C13B C12B 68.4(15) . . . . ? Ir1 Ir2 C13B C12B 119.9(14) . . . . ? C14B C13B C12B C11 -84(3) . . . . ? Ir2 C13B C12B C11 38(2) . . . . ? C2 C1 C8 C7B 85.5(14) . . . . ? Ir1 C1 C8 C7B 4.7(14) . . . . ? C2 C1 C8 C7A 76.6(8) . . . . ? Ir1 C1 C8 C7A -4.1(8) . . . . ? C6A C7A C8 C7B -139(10) . . . . ? C6A C7A C8 C1 -24.4(10) . . . . ? C13B Ir2 C9 C10 76.5(7) . . . . ? N1 Ir2 C9 C10 -99.3(4) . . . . ? C13A Ir2 C9 C10 67.4(5) . . . . ? C14A Ir2 C9 C10 100.0(4) . . . . ? P1 Ir2 C9 C10 -175.5(3) . . . . ? P2 Ir2 C9 C10 -25.8(5) . . . . ? Ir1 Ir2 C9 C10 -116.0(4) . . . . ? C13B Ir2 C9 C16 -42.8(8) . . . . ? C10 Ir2 C9 C16 -119.3(7) . . . . ? N1 Ir2 C9 C16 141.4(5) . . . . ? C13A Ir2 C9 C16 -51.9(6) . . . . ? C14A Ir2 C9 C16 -19.3(5) . . . . ? P1 Ir2 C9 C16 65.1(5) . . . . ? P2 Ir2 C9 C16 -145.1(4) . . . . ? Ir1 Ir2 C9 C16 124.6(4) . . . . ? C16 C9 C10 C11 3.6(10) . . . . ? Ir2 C9 C10 C11 -106.3(6) . . . . ? C16 C9 C10 Ir2 109.9(6) . . . . ? C13B Ir2 C10 C9 -101.2(7) . . . . ? N1 Ir2 C10 C9 85.7(4) . . . . ? C13A Ir2 C10 C9 -110.7(5) . . . . ? C14A Ir2 C10 C9 -74.0(4) . . . . ? P1 Ir2 C10 C9 8.7(6) . . . . ? P2 Ir2 C10 C9 162.3(4) . . . . ? Ir1 Ir2 C10 C9 122.8(4) . . . . ? C13B Ir2 C10 C11 17.4(7) . . . . ? C9 Ir2 C10 C11 118.6(6) . . . . ? N1 Ir2 C10 C11 -155.7(5) . . . . ? C13A Ir2 C10 C11 7.9(5) . . . . ? C14A Ir2 C10 C11 44.6(5) . . . . ? P1 Ir2 C10 C11 127.3(4) . . . . ? P2 Ir2 C10 C11 -79.1(4) . . . . ? Ir1 Ir2 C10 C11 -118.6(4) . . . . ? C9 C10 C11 C12A 89.2(9) . . . . ? Ir2 C10 C11 C12A 8.4(9) . . . . ? C9 C10 C11 C12B 80.2(14) . . . . ? Ir2 C10 C11 C12B -0.7(14) . . . . ? C13B C12B C11 C12A -138(13) . . . . ? C13B C12B C11 C10 -25(3) . . . . ? C10 C11 C12A C13A -28.4(13) . . . . ? C12B C11 C12A C13A 42(11) . . . . ? C11 C12A C13A C14A -47.0(15) . . . . ? C11 C12A C13A Ir2 34.4(12) . . . . ? C13B Ir2 C13A C14A -8(4) . . . . ? C9 Ir2 C13A C14A 60.8(5) . . . . ? C10 Ir2 C13A C14A 97.6(5) . . . . ? N1 Ir2 C13A C14A -174.8(9) . . . . ? P1 Ir2 C13A C14A -55.5(6) . . . . ? P2 Ir2 C13A C14A -162.9(5) . . . . ? Ir1 Ir2 C13A C14A -116.9(5) . . . . ? C13B Ir2 C13A C12A -128(5) . . . . ? C9 Ir2 C13A C12A -59.8(8) . . . . ? C10 Ir2 C13A C12A -23.0(8) . . . . ? N1 Ir2 C13A C12A 64.6(15) . . . . ? C14A Ir2 C13A C12A -120.6(10) . . . . ? P1 Ir2 C13A C12A -176.0(7) . . . . ? P2 Ir2 C13A C12A 76.5(8) . . . . ? Ir1 Ir2 C13A C12A 122.5(7) . . . . ? C12A C13A C14A C15A -5.8(16) . . . . ? Ir2 C13A C14A C15A -108.7(9) . . . . ? C12A C13A C14A Ir2 102.9(11) . . . . ? C13B Ir2 C14A C13A 2.9(15) . . . . ? C9 Ir2 C14A C13A -116.7(6) . . . . ? C10 Ir2 C14A C13A -77.6(6) . . . . ? N1 Ir2 C14A C13A 176.0(7) . . . . ? P1 Ir2 C14A C13A 130.7(5) . . . . ? P2 Ir2 C14A C13A 20.7(6) . . . . ? Ir1 Ir2 C14A C13A 89.2(6) . . . . ? C13B Ir2 C14A C15A 122.7(15) . . . . ? C9 Ir2 C14A C15A 3.1(6) . . . . ? C10 Ir2 C14A C15A 42.2(7) . . . . ? N1 Ir2 C14A C15A -64.2(11) . . . . ? C13A Ir2 C14A C15A 119.8(9) . . . . ? P1 Ir2 C14A C15A -109.5(7) . . . . ? P2 Ir2 C14A C15A 140.6(6) . . . . ? Ir1 Ir2 C14A C15A -151.0(6) . . . . ? C13A C14A C15A C16 96.9(11) . . . . ? Ir2 C14A C15A C16 12.9(10) . . . . ? C4A C3 C4B C5B -146(5) . . . . ? C2 C3 C4B C5B -23(2) . . . . ? C3 C4B C5B C6B 88(3) . . . . ? C3 C4B C5B Ir1 8(3) . . . . ? C6A Ir1 C5B C6B -2.6(15) . . . . ? C2 Ir1 C5B C6B -114.2(12) . . . . ? C1 Ir1 C5B C6B -75.6(12) . . . . ? N1 Ir1 C5B C6B 165.5(13) . . . . ? P2 Ir1 C5B C6B 134.6(12) . . . . ? P1 Ir1 C5B C6B 24.7(14) . . . . ? Ir2 Ir1 C5B C6B 93.4(12) . . . . ? C6A Ir1 C5B C4B 117(2) . . . . ? C2 Ir1 C5B C4B 5.7(16) . . . . ? C1 Ir1 C5B C4B 44.3(17) . . . . ? N1 Ir1 C5B C4B -75(2) . . . . ? C6B Ir1 C5B C4B 120(2) . . . . ? P2 Ir1 C5B C4B -105.5(17) . . . . ? P1 Ir1 C5B C4B 144.6(16) . . . . ? Ir2 Ir1 C5B C4B -146.8(15) . . . . ? C4B C5B C6B C7B -4(4) . . . . ? Ir1 C5B C6B C7B 103(3) . . . . ? C4B C5B C6B Ir1 -107(3) . . . . ? C6A Ir1 C6B C5B 6(3) . . . . ? C2 Ir1 C6B C5B 62.7(12) . . . . ? C1 Ir1 C6B C5B 100.1(12) . . . . ? N1 Ir1 C6B C5B -157.8(18) . . . . ? P2 Ir1 C6B C5B -48.7(12) . . . . ? P1 Ir1 C6B C5B -159.6(11) . . . . ? Ir2 Ir1 C6B C5B -110.5(11) . . . . ? C6A Ir1 C6B C7B -117(4) . . . . ? C2 Ir1 C6B C7B -59.7(15) . . . . ? C1 Ir1 C6B C7B -22.3(15) . . . . ? N1 Ir1 C6B C7B 80(3) . . . . ? C5B Ir1 C6B C7B -122(2) . . . . ? P2 Ir1 C6B C7B -171.1(14) . . . . ? P1 Ir1 C6B C7B 78.0(15) . . . . ? Ir2 Ir1 C6B C7B 127.1(14) . . . . ? C1 C8 C7B C6B -26(3) . . . . ? C7A C8 C7B C6B 43(8) . . . . ? C5B C6B C7B C8 -52(4) . . . . ? Ir1 C6B C7B C8 33(2) . . . . ? C14A C15A C16 C9 -27.8(10) . . . . ? C14A C15A C16 C15B -155(6) . . . . ? C10 C9 C16 C15A -51.5(9) . . . . ? Ir2 C9 C16 C15A 32.5(8) . . . . ? C10 C9 C16 C15B -38.0(15) . . . . ? Ir2 C9 C16 C15B 46.0(14) . . . . ? C14B C15B C16 C15A 9(4) . . . . ? C14B C15B C16 C9 -49(2) . . . . ? C23 P1 C17 C22 -11.8(6) . . . . ? Ir1 P1 C17 C22 -144.3(5) . . . . ? Ir2 P1 C17 C22 126.8(5) . . . . ? C23 P1 C17 C18 171.6(5) . . . . ? Ir1 P1 C17 C18 39.1(6) . . . . ? Ir2 P1 C17 C18 -49.9(6) . . . . ? C22 C17 C18 C19 1.4(9) . . . . ? P1 C17 C18 C19 178.3(5) . . . . ? C17 C18 C19 C20 -0.7(10) . . . . ? C18 C19 C20 C21 0.0(11) . . . . ? C19 C20 C21 C22 -0.1(11) . . . . ? C20 C21 C22 C17 0.9(11) . . . . ? C18 C17 C22 C21 -1.6(10) . . . . ? P1 C17 C22 C21 -178.3(5) . . . . ? C17 P1 C23 C24 114.2(6) . . . . ? Ir1 P1 C23 C24 -105.6(5) . . . . ? Ir2 P1 C23 C24 -26.5(6) . . . . ? C17 P1 C23 C28 -67.0(5) . . . . ? Ir1 P1 C23 C28 73.2(5) . . . . ? Ir2 P1 C23 C28 152.3(4) . . . . ? C28 C23 C24 C25 0.7(10) . . . . ? P1 C23 C24 C25 179.6(6) . . . . ? C23 C24 C25 C26 0.7(12) . . . . ? C24 C25 C26 C27 -1.6(12) . . . . ? C25 C26 C27 C28 1.1(10) . . . . ? C26 C27 C28 C23 0.3(9) . . . . ? C24 C23 C28 C27 -1.2(9) . . . . ? P1 C23 C28 C27 179.9(5) . . . . ? C35 P2 C29 C34 177.0(5) . . . . ? Ir1 P2 C29 C34 -37.4(6) . . . . ? Ir2 P2 C29 C34 49.7(5) . . . . ? C35 P2 C29 C30 -3.0(6) . . . . ? Ir1 P2 C29 C30 142.7(4) . . . . ? Ir2 P2 C29 C30 -130.2(5) . . . . ? C34 C29 C30 C31 -2.5(9) . . . . ? P2 C29 C30 C31 177.4(5) . . . . ? C29 C30 C31 C32 0.4(10) . . . . ? C30 C31 C32 C33 1.9(10) . . . . ? C31 C32 C33 C34 -2.0(10) . . . . ? C30 C29 C34 C33 2.4(9) . . . . ? P2 C29 C34 C33 -177.6(5) . . . . ? C32 C33 C34 C29 -0.1(10) . . . . ? C29 P2 C35 C36 126.3(5) . . . . ? Ir1 P2 C35 C36 -21.8(6) . . . . ? Ir2 P2 C35 C36 -100.0(5) . . . . ? C29 P2 C35 C40 -55.7(6) . . . . ? Ir1 P2 C35 C40 156.2(4) . . . . ? Ir2 P2 C35 C40 78.0(5) . . . . ? C40 C35 C36 C37 -0.2(9) . . . . ? P2 C35 C36 C37 177.9(5) . . . . ? C35 C36 C37 C38 1.9(10) . . . . ? C36 C37 C38 C39 -0.9(10) . . . . ? C37 C38 C39 C40 -1.9(10) . . . . ? C38 C39 C40 C35 3.8(10) . . . . ? C36 C35 C40 C39 -2.7(9) . . . . ? P2 C35 C40 C39 179.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.674 _refine_diff_density_min -1.435 _refine_diff_density_rms 0.168 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.750 -0.032 0.078 239 82 ' ' 2 0.250 -0.027 0.422 239 82 ' ' 3 0.750 -0.016 0.578 239 82 ' ' 4 0.250 -0.013 0.922 239 82 ' ' _platon_squeeze_details ; There are very large solvent accessible voids in the structure and a zone where residual density peaks are observed. The solvent is highly disordered and it cannot be modelled even with several restraints. Therefore, SQUEEZE corrections have been applied. The total potential solvent accesible void volume (959 \A3) and the electron count (328 e in the unit cell) may agree with the presence of eight C6D6 molecules. They have been included in the chemical formula, F000 and density. Results of the SQUEEZE calculations are included at the end of this cif file. ; # start Validation Reply Form _vrf_CHEMW03_cmpnd_3 ; PROBLEM: ALERT: The ratio of given/expected molecular weight as RESPONSE: The calculated molecular weight is calculated from the moiety formula, which does not include 8 C6D6 molecules. They have not been included in the structural model, but their presence has been estimated via SQUEEZE calculation and included in the calculation of crystal parameters (molecular weight, density, F000, etc). ; _database_code_depnum_ccdc_archive 'CCDC 951634' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_cmpnd_7 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H52 Ir2 P2' _chemical_formula_sum 'C28 H52 Ir2 P2' _chemical_formula_weight 835.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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' Ir Ir -1.4440 7.9890 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1020 0.0940 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' 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 12.0438(6) _cell_length_b 13.3654(6) _cell_length_c 17.5773(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.2757(6) _cell_angle_gamma 90.00 _cell_volume 2817.4(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9945 _cell_measurement_theta_min 2.281 _cell_measurement_theta_max 27.457 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.281 _exptl_crystal_size_mid 0.114 _exptl_crystal_size_min 0.111 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.968 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 9.559 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.185 _exptl_absorpt_correction_T_max 0.331 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. (1996) Bruker-AXS within APEX2 package. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX DUO CCD system' _diffrn_measurement_method 'narrow \w frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27939 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.48 _reflns_number_total 6455 _reflns_number_gt 5340 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 v2008, Bruker AXS' _computing_cell_refinement 'SAINT+ in APEX2 v2008, Bruker AXS' _computing_data_reduction 'SAINT+ in APEX2 v2008, Bruker AXS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material 'XCIF program, SHELXTLv6.12, BrukerAXS; PARST(Nardelli, 1995)' _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. Hydrogen atom of methyl groups have been included in the model in calculated positions and refined with a riding model. The rest of the hydrogen atoms have been included in the model in observed positions and freely refined; only one geometrical restraint in a C-H distance has been included in the refinement. ; _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^)+(0.0147P)^2^+1.3531P] 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 6455 _refine_ls_number_parameters 409 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0264 _refine_ls_R_factor_gt 0.0173 _refine_ls_wR_factor_ref 0.0400 _refine_ls_wR_factor_gt 0.0369 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl212ds in P 1 21/c 1 CELL 0.71073 12.0438 13.3654 17.5773 90.000 95.2757 90.000 ZERR 4.00 0.0006 0.0006 0.0008 0.000 0.0006 0.000 LATT 1 SYMM - X, 1/2 + Y, 1/2 - Z SFAC C 2.31000 20.84392 1.02000 10.20751 1.58860 0.56870 = 0.86500 51.65125 0.21560 0.003 0.002 11.500 0.770 12.011 SFAC H 0.49300 10.51091 0.32291 26.12573 0.14019 3.14236 = 0.04081 57.79977 0.00304 0.000 0.000 0.620 0.320 1.008 SFAC IR 27.30493 1.59279 16.72961 8.86554 15.61152 0.41792 = 5.83378 45.00114 11.47221 -1.444 7.989 33100.000 1.350 192.217 SFAC P 6.43451 1.90670 4.17910 27.15704 1.78000 0.52600 = 1.49080 68.16457 1.11490 0.102 0.094 410.000 1.100 30.974 UNIT 112 208 8 8 MERG 2 FMAP 2 BOND $H DFIX 0.96 0.04 C7 H7B CONF ACTA 55 WPDB -2 PLAN 20 L.S. 4 TEMP -173.00 WGHT 0.014700 1.353100 FVAR 0.14204 IR1 3 0.140002 0.049768 0.264697 11.00000 0.01102 0.01277 = 0.01602 0.00080 0.00139 0.00021 IR2 3 0.351113 0.052763 0.242757 11.00000 0.01123 0.01197 = 0.01557 0.00057 0.00198 0.00044 P1 4 0.206901 0.063915 0.147925 11.00000 0.01542 0.01479 = 0.01528 0.00090 0.00054 0.00066 P2 4 0.281396 0.038724 0.359759 11.00000 0.01367 0.01437 = 0.01564 0.00139 0.00101 0.00042 C1 1 0.006141 -0.057396 0.236172 11.00000 0.01745 0.02214 = 0.02859 -0.00652 0.00104 -0.00616 C2 1 0.025243 -0.050918 0.316828 11.00000 0.01298 0.01495 = 0.03021 0.00271 0.00315 -0.00324 C3 1 -0.054687 -0.000254 0.367234 11.00000 0.01699 0.02551 = 0.02592 0.00278 0.00521 -0.00354 C4 1 -0.022505 0.108872 0.383444 11.00000 0.02261 0.02727 = 0.03790 -0.00917 0.01355 -0.00234 C5 1 0.035738 0.154796 0.319652 11.00000 0.02099 0.01488 = 0.04151 -0.00352 0.01334 -0.00089 C6 1 -0.004457 0.148733 0.241326 11.00000 0.01870 0.01907 = 0.03890 0.00926 0.00913 0.00540 C7 1 -0.112128 0.097416 0.212590 11.00000 0.01321 0.04342 = 0.04157 0.01020 0.00191 0.00464 C8 1 -0.093526 -0.011957 0.190550 11.00000 0.01861 0.04309 = 0.02991 -0.00312 -0.00469 -0.00434 C9 1 0.465019 -0.062996 0.213788 11.00000 0.01720 0.01449 = 0.03202 0.00101 0.00441 0.00378 C10 1 0.503084 -0.025814 0.287666 11.00000 0.01438 0.01861 = 0.02794 0.00528 0.00195 0.00596 C11 1 0.606499 0.038514 0.302806 11.00000 0.01515 0.02830 = 0.02889 0.00302 -0.00201 0.00351 C12 1 0.578236 0.150814 0.298468 11.00000 0.01751 0.02528 = 0.02549 -0.00386 0.00050 -0.00494 C13 1 0.473764 0.171535 0.246298 11.00000 0.01696 0.01602 = 0.02855 0.00073 0.00681 -0.00335 C14 1 0.458310 0.135294 0.170406 11.00000 0.01435 0.01843 = 0.02380 0.00374 0.00562 -0.00161 C15 1 0.544266 0.071852 0.133175 11.00000 0.01980 0.02915 = 0.02968 0.00016 0.00880 0.00015 C16 1 0.526683 -0.040350 0.144066 11.00000 0.02367 0.02564 = 0.03111 -0.00412 0.00918 0.00565 C17 1 0.182000 -0.032194 0.071286 11.00000 0.01782 0.02339 = 0.02535 -0.00520 -0.00181 0.00004 C18 1 0.207737 -0.137551 0.102722 11.00000 0.04075 0.01814 = 0.03493 -0.00385 0.00905 -0.00006 AFIX 137 H18A 2 0.177950 -0.187399 0.065366 11.00000 -1.50000 H18B 2 0.173073 -0.146507 0.150566 11.00000 -1.50000 H18C 2 0.288632 -0.146061 0.112320 11.00000 -1.50000 AFIX 0 C19 1 0.247650 -0.012649 0.002665 11.00000 0.03832 0.03178 = 0.02147 -0.00660 0.00250 -0.00024 AFIX 137 H19A 2 0.326350 -0.001884 0.020201 11.00000 -1.50000 H19B 2 0.217951 0.046959 -0.024575 11.00000 -1.50000 H19C 2 0.240855 -0.070456 -0.031748 11.00000 -1.50000 AFIX 0 C20 1 0.189722 0.181906 0.092199 11.00000 0.02116 0.02228 = 0.01947 0.00581 0.00209 0.00146 C21 1 0.211817 0.274792 0.142304 11.00000 0.02579 0.01767 = 0.03060 0.00497 0.00415 0.00338 AFIX 137 H21A 2 0.215890 0.333939 0.109727 11.00000 -1.50000 H21B 2 0.282562 0.266701 0.173978 11.00000 -1.50000 H21C 2 0.151139 0.283184 0.175276 11.00000 -1.50000 AFIX 0 C22 1 0.076173 0.189141 0.045577 11.00000 0.03033 0.03093 = 0.03125 0.01076 -0.00668 0.00388 AFIX 137 H22A 2 0.016727 0.184293 0.079909 11.00000 -1.50000 H22B 2 0.068630 0.134388 0.008377 11.00000 -1.50000 H22C 2 0.070494 0.253372 0.018609 11.00000 -1.50000 AFIX 0 C23 1 0.305594 -0.077527 0.416607 11.00000 0.01596 0.02043 = 0.02266 0.00367 0.00084 -0.00132 C24 1 0.229857 -0.086340 0.481634 11.00000 0.02892 0.02789 = 0.02234 0.00839 0.00575 -0.00308 AFIX 137 H24A 2 0.152203 -0.093281 0.460202 11.00000 -1.50000 H24B 2 0.237461 -0.026160 0.513539 11.00000 -1.50000 H24C 2 0.251427 -0.145220 0.512783 11.00000 -1.50000 AFIX 0 C25 1 0.296841 -0.171817 0.366786 11.00000 0.02645 0.01652 = 0.03426 0.00356 0.00639 0.00048 AFIX 137 H25A 2 0.312148 -0.230947 0.399021 11.00000 -1.50000 H25B 2 0.351270 -0.168114 0.328725 11.00000 -1.50000 H25C 2 0.221507 -0.176677 0.340757 11.00000 -1.50000 AFIX 0 C26 1 0.303545 0.137656 0.434329 11.00000 0.01877 0.02320 = 0.01630 -0.00309 0.00302 -0.00072 C27 1 0.406948 0.121200 0.490202 11.00000 0.02581 0.02840 = 0.02432 -0.00326 -0.00346 -0.00374 AFIX 137 H27A 2 0.472744 0.114592 0.461668 11.00000 -1.50000 H27B 2 0.397597 0.060046 0.519704 11.00000 -1.50000 H27C 2 0.416764 0.178417 0.525037 11.00000 -1.50000 AFIX 0 C28 1 0.311038 0.240379 0.397072 11.00000 0.03055 0.01825 = 0.02659 -0.00490 0.00301 -0.00155 AFIX 137 H28A 2 0.306979 0.292605 0.435853 11.00000 -1.50000 H28B 2 0.249046 0.248468 0.357366 11.00000 -1.50000 H28C 2 0.381895 0.245975 0.374093 11.00000 -1.50000 AFIX 0 H1 2 0.029327 -0.116791 0.214772 11.00000 0.03284 H2 2 0.068651 -0.103842 0.342826 11.00000 0.02033 H3A 2 -0.055928 -0.033912 0.415358 11.00000 0.02419 H3B 2 -0.127060 -0.000839 0.342240 11.00000 0.02002 H4A 2 0.027892 0.110280 0.431154 11.00000 0.03394 H4B 2 -0.086304 0.149354 0.392091 11.00000 0.04128 H5 2 0.075500 0.213136 0.332382 11.00000 0.03444 H6 2 0.016375 0.199968 0.211751 11.00000 0.01977 H7A 2 -0.162866 0.097931 0.250071 11.00000 0.03888 H7B 2 -0.149442 0.138509 0.166741 11.00000 0.03953 H8A 2 -0.159987 -0.050608 0.195831 11.00000 0.03058 H8B 2 -0.078779 -0.015297 0.136913 11.00000 0.03485 H9 2 0.425160 -0.124293 0.212256 11.00000 0.01539 H10 2 0.488928 -0.068727 0.330051 11.00000 0.01813 H11A 2 0.647436 0.022135 0.351864 11.00000 0.03715 H11B 2 0.654059 0.019768 0.264362 11.00000 0.01517 H13 2 0.441342 0.230843 0.255951 11.00000 0.02092 H12A 2 0.571233 0.171630 0.348021 11.00000 0.01113 H12B 2 0.640335 0.192269 0.282211 11.00000 0.01900 H14 2 0.410274 0.176795 0.133500 11.00000 0.01444 H15A 2 0.618866 0.090738 0.152666 11.00000 0.03198 H15B 2 0.539558 0.086172 0.080012 11.00000 0.02601 H16A 2 0.596600 -0.076664 0.148373 11.00000 0.02263 H16B 2 0.480844 -0.072058 0.100665 11.00000 0.03891 H17 2 0.111754 -0.024936 0.058441 11.00000 0.02599 H20 2 0.242888 0.180368 0.058647 11.00000 0.02876 H23 2 0.377161 -0.076268 0.438497 11.00000 0.01744 H26 2 0.239264 0.131817 0.460854 11.00000 0.02209 HKLF 4 REM fjl212ds in P 1 21/c 1 REM R1 = 0.0173 for 5340 Fo > 4sig(Fo) and 0.0264 for all 6455 data REM 409 parameters refined using 1 restraints END ; 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 0.140002(8) 0.049768(8) 0.264697(6) 0.01326(3) Uani 1 1 d . . . Ir2 Ir 0.351113(8) 0.052763(8) 0.242757(6) 0.01288(3) Uani 1 1 d . . . P1 P 0.20690(6) 0.06392(5) 0.14792(4) 0.01522(14) Uani 1 1 d . . . P2 P 0.28140(6) 0.03872(5) 0.35976(4) 0.01458(14) Uani 1 1 d . . . C1 C 0.0061(2) -0.0574(2) 0.23617(18) 0.0228(7) Uani 1 1 d . . . C2 C 0.0252(2) -0.0509(2) 0.31683(18) 0.0193(6) Uani 1 1 d . . . C3 C -0.0547(3) -0.0003(2) 0.36723(19) 0.0226(6) Uani 1 1 d . . . C4 C -0.0225(3) 0.1089(2) 0.3834(2) 0.0286(8) Uani 1 1 d . . . C5 C 0.0357(3) 0.1548(2) 0.31965(19) 0.0251(7) Uani 1 1 d . . . C6 C -0.0045(2) 0.1487(2) 0.2413(2) 0.0252(7) Uani 1 1 d . . . C7 C -0.1121(3) 0.0974(3) 0.2126(2) 0.0328(8) Uani 1 1 d D . . C8 C -0.0935(3) -0.0120(3) 0.1905(2) 0.0310(8) Uani 1 1 d . . . C9 C 0.4650(2) -0.0630(2) 0.21379(18) 0.0211(6) Uani 1 1 d . . . C10 C 0.5031(2) -0.0258(2) 0.28767(18) 0.0203(6) Uani 1 1 d . . . C11 C 0.6065(3) 0.0385(2) 0.3028(2) 0.0244(7) Uani 1 1 d . . . C12 C 0.5782(2) 0.1508(2) 0.29847(18) 0.0229(6) Uani 1 1 d . . . C13 C 0.4738(2) 0.1715(2) 0.24630(18) 0.0202(6) Uani 1 1 d . . . C14 C 0.4583(2) 0.1353(2) 0.17041(17) 0.0186(6) Uani 1 1 d . . . C15 C 0.5443(3) 0.0719(2) 0.1332(2) 0.0258(7) Uani 1 1 d . . . C16 C 0.5267(3) -0.0403(2) 0.1441(2) 0.0264(7) Uani 1 1 d . . . C17 C 0.1820(3) -0.0322(2) 0.07129(18) 0.0224(6) Uani 1 1 d . . . C18 C 0.2077(3) -0.1376(2) 0.10272(19) 0.0309(8) Uani 1 1 d . . . H18A H 0.1779 -0.1874 0.0654 0.046 Uiso 1 1 calc R . . H18B H 0.1731 -0.1465 0.1506 0.046 Uiso 1 1 calc R . . H18C H 0.2886 -0.1461 0.1123 0.046 Uiso 1 1 calc R . . C19 C 0.2477(3) -0.0126(2) 0.00266(18) 0.0305(7) Uani 1 1 d . . . H19A H 0.3264 -0.0019 0.0202 0.046 Uiso 1 1 calc R . . H19B H 0.2180 0.0470 -0.0246 0.046 Uiso 1 1 calc R . . H19C H 0.2409 -0.0705 -0.0317 0.046 Uiso 1 1 calc R . . C20 C 0.1897(3) 0.1819(2) 0.09220(17) 0.0210(6) Uani 1 1 d . . . C21 C 0.2118(3) 0.2748(2) 0.14230(18) 0.0246(7) Uani 1 1 d . . . H21A H 0.2159 0.3339 0.1097 0.037 Uiso 1 1 calc R . . H21B H 0.2826 0.2667 0.1740 0.037 Uiso 1 1 calc R . . H21C H 0.1511 0.2832 0.1753 0.037 Uiso 1 1 calc R . . C22 C 0.0762(3) 0.1891(2) 0.04558(19) 0.0314(8) Uani 1 1 d . . . H22A H 0.0167 0.1843 0.0799 0.047 Uiso 1 1 calc R . . H22B H 0.0686 0.1344 0.0084 0.047 Uiso 1 1 calc R . . H22C H 0.0705 0.2534 0.0186 0.047 Uiso 1 1 calc R . . C23 C 0.3056(3) -0.0775(2) 0.41661(17) 0.0197(6) Uani 1 1 d . . . C24 C 0.2299(3) -0.0863(2) 0.48163(17) 0.0262(7) Uani 1 1 d . . . H24A H 0.1522 -0.0933 0.4602 0.039 Uiso 1 1 calc R . . H24B H 0.2375 -0.0262 0.5135 0.039 Uiso 1 1 calc R . . H24C H 0.2514 -0.1452 0.5128 0.039 Uiso 1 1 calc R . . C25 C 0.2968(3) -0.1718(2) 0.36679(18) 0.0255(7) Uani 1 1 d . . . H25A H 0.3121 -0.2309 0.3990 0.038 Uiso 1 1 calc R . . H25B H 0.3513 -0.1681 0.3287 0.038 Uiso 1 1 calc R . . H25C H 0.2215 -0.1767 0.3408 0.038 Uiso 1 1 calc R . . C26 C 0.3035(2) 0.1377(2) 0.43433(16) 0.0193(6) Uani 1 1 d . . . C27 C 0.4069(3) 0.1212(2) 0.49020(18) 0.0265(7) Uani 1 1 d . . . H27A H 0.4727 0.1146 0.4617 0.040 Uiso 1 1 calc R . . H27B H 0.3976 0.0600 0.5197 0.040 Uiso 1 1 calc R . . H27C H 0.4168 0.1784 0.5250 0.040 Uiso 1 1 calc R . . C28 C 0.3110(3) 0.2404(2) 0.39707(18) 0.0251(7) Uani 1 1 d . . . H28A H 0.3070 0.2926 0.4359 0.038 Uiso 1 1 calc R . . H28B H 0.2490 0.2485 0.3574 0.038 Uiso 1 1 calc R . . H28C H 0.3819 0.2460 0.3741 0.038 Uiso 1 1 calc R . . H1 H 0.029(3) -0.117(3) 0.2148(19) 0.033(9) Uiso 1 1 d . . . H2 H 0.069(2) -0.104(2) 0.3428(17) 0.020(8) Uiso 1 1 d . . . H3A H -0.056(3) -0.034(2) 0.4154(19) 0.024(8) Uiso 1 1 d . . . H3B H -0.127(3) -0.001(2) 0.3422(17) 0.020(8) Uiso 1 1 d . . . H4A H 0.028(3) 0.110(2) 0.431(2) 0.034(10) Uiso 1 1 d . . . H4B H -0.086(3) 0.149(3) 0.392(2) 0.041(10) Uiso 1 1 d . . . H5 H 0.075(3) 0.213(3) 0.3324(19) 0.034(10) Uiso 1 1 d . . . H6 H 0.016(2) 0.200(2) 0.2118(17) 0.020(8) Uiso 1 1 d . . . H7A H -0.163(3) 0.098(3) 0.250(2) 0.039(10) Uiso 1 1 d . . . H7B H -0.149(3) 0.139(2) 0.1667(17) 0.040(10) Uiso 1 1 d D . . H8A H -0.160(3) -0.051(2) 0.1958(19) 0.031(9) Uiso 1 1 d . . . H8B H -0.079(3) -0.015(2) 0.137(2) 0.035(10) Uiso 1 1 d . . . H9 H 0.425(2) -0.124(2) 0.2123(16) 0.015(8) Uiso 1 1 d . . . H10 H 0.489(2) -0.069(2) 0.3301(17) 0.018(8) Uiso 1 1 d . . . H11A H 0.647(3) 0.022(3) 0.352(2) 0.037(10) Uiso 1 1 d . . . H11B H 0.654(2) 0.020(2) 0.2644(16) 0.015(8) Uiso 1 1 d . . . H13 H 0.441(2) 0.231(2) 0.2560(17) 0.021(8) Uiso 1 1 d . . . H12A H 0.571(2) 0.172(2) 0.3480(17) 0.011(7) Uiso 1 1 d . . . H12B H 0.640(2) 0.192(2) 0.2822(17) 0.019(8) Uiso 1 1 d . . . H14 H 0.410(2) 0.177(2) 0.1335(17) 0.014(7) Uiso 1 1 d . . . H15A H 0.619(3) 0.091(2) 0.1527(19) 0.032(9) Uiso 1 1 d . . . H15B H 0.540(3) 0.086(2) 0.080(2) 0.026(9) Uiso 1 1 d . . . H16A H 0.597(3) -0.077(2) 0.1484(18) 0.023(8) Uiso 1 1 d . . . H16B H 0.481(3) -0.072(3) 0.101(2) 0.039(10) Uiso 1 1 d . . . H17 H 0.112(3) -0.025(2) 0.0584(19) 0.026(9) Uiso 1 1 d . . . H20 H 0.243(3) 0.180(2) 0.0586(19) 0.029(9) Uiso 1 1 d . . . H23 H 0.377(3) -0.076(2) 0.4385(17) 0.017(8) Uiso 1 1 d . . . H26 H 0.239(3) 0.132(2) 0.4609(17) 0.022(8) Uiso 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 0.01102(6) 0.01277(6) 0.01602(6) 0.00080(4) 0.00139(4) 0.00021(4) Ir2 0.01123(6) 0.01197(6) 0.01557(6) 0.00057(4) 0.00198(4) 0.00044(4) P1 0.0154(3) 0.0148(3) 0.0153(3) 0.0009(3) 0.0005(3) 0.0007(3) P2 0.0137(3) 0.0144(3) 0.0156(4) 0.0014(3) 0.0010(3) 0.0004(3) C1 0.0174(15) 0.0221(16) 0.0286(17) -0.0065(13) 0.0010(13) -0.0062(12) C2 0.0130(14) 0.0150(14) 0.0302(17) 0.0027(12) 0.0031(12) -0.0032(11) C3 0.0170(16) 0.0255(16) 0.0259(17) 0.0028(13) 0.0052(13) -0.0035(13) C4 0.0226(17) 0.0273(18) 0.038(2) -0.0092(14) 0.0135(16) -0.0023(14) C5 0.0210(16) 0.0149(15) 0.042(2) -0.0035(13) 0.0133(14) -0.0009(13) C6 0.0187(15) 0.0191(16) 0.039(2) 0.0093(14) 0.0091(14) 0.0054(12) C7 0.0132(16) 0.043(2) 0.042(2) 0.0102(17) 0.0019(15) 0.0046(14) C8 0.0186(17) 0.043(2) 0.030(2) -0.0031(15) -0.0047(14) -0.0043(15) C9 0.0172(15) 0.0145(15) 0.0320(18) 0.0010(12) 0.0044(13) 0.0038(12) C10 0.0144(14) 0.0186(15) 0.0279(17) 0.0053(12) 0.0019(12) 0.0060(11) C11 0.0151(15) 0.0283(17) 0.0289(18) 0.0030(14) -0.0020(13) 0.0035(13) C12 0.0175(15) 0.0253(16) 0.0255(17) -0.0039(13) 0.0005(13) -0.0049(13) C13 0.0170(14) 0.0160(15) 0.0286(17) 0.0007(12) 0.0068(13) -0.0034(12) C14 0.0144(14) 0.0184(15) 0.0238(16) 0.0037(12) 0.0056(12) -0.0016(11) C15 0.0198(16) 0.0291(17) 0.0297(19) 0.0002(14) 0.0088(14) 0.0002(13) C16 0.0237(17) 0.0256(17) 0.0311(18) -0.0041(14) 0.0092(14) 0.0057(14) C17 0.0178(16) 0.0234(16) 0.0254(17) -0.0052(12) -0.0018(13) 0.0000(13) C18 0.041(2) 0.0181(16) 0.0349(19) -0.0038(13) 0.0091(16) -0.0001(14) C19 0.0383(19) 0.0318(18) 0.0215(17) -0.0066(14) 0.0025(14) -0.0002(15) C20 0.0212(16) 0.0223(16) 0.0195(16) 0.0058(12) 0.0021(12) 0.0015(12) C21 0.0258(17) 0.0177(15) 0.0306(18) 0.0050(12) 0.0042(13) 0.0034(13) C22 0.0303(18) 0.0309(18) 0.0312(19) 0.0108(14) -0.0067(15) 0.0039(14) C23 0.0160(15) 0.0204(15) 0.0227(16) 0.0037(12) 0.0008(12) -0.0013(12) C24 0.0289(18) 0.0279(17) 0.0223(17) 0.0084(13) 0.0058(13) -0.0031(14) C25 0.0264(17) 0.0165(15) 0.0343(19) 0.0036(12) 0.0064(14) 0.0005(13) C26 0.0188(15) 0.0232(15) 0.0163(15) -0.0031(11) 0.0030(12) -0.0007(12) C27 0.0258(17) 0.0284(17) 0.0243(17) -0.0033(13) -0.0035(13) -0.0037(13) C28 0.0306(18) 0.0182(15) 0.0266(17) -0.0049(12) 0.0030(13) -0.0016(13) _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 C5 2.169(3) . ? Ir1 C1 2.180(3) . ? Ir1 C2 2.189(3) . ? Ir1 C6 2.194(3) . ? Ir1 P2 2.2783(7) . ? Ir1 P1 2.2808(7) . ? Ir1 Ir2 2.60679(18) . ? Ir2 C9 2.160(3) . ? Ir2 C13 2.165(3) . ? Ir2 C14 2.192(3) . ? Ir2 C10 2.193(3) . ? Ir2 P1 2.2989(8) . ? Ir2 P2 2.2994(7) . ? P1 C20 1.858(3) . ? P1 C17 1.866(3) . ? P2 C23 1.856(3) . ? P2 C26 1.864(3) . ? C1 C2 1.418(4) . ? C1 C8 1.509(5) . ? C1 H1 0.93(3) . ? C2 C3 1.525(4) . ? C2 H2 0.97(3) . ? C3 C4 1.529(4) . ? C3 H3A 0.96(3) . ? C3 H3B 0.94(3) . ? C4 C5 1.507(4) . ? C4 H4A 0.99(3) . ? C4 H4B 0.96(3) . ? C5 C6 1.419(5) . ? C5 H5 0.93(3) . ? C6 C7 1.512(5) . ? C6 H6 0.91(3) . ? C7 C8 1.534(5) . ? C7 H7A 0.94(3) . ? C7 H7B 1.04(3) . ? C8 H8A 0.96(3) . ? C8 H8B 0.98(3) . ? C9 C10 1.426(4) . ? C9 C16 1.521(4) . ? C9 H9 0.95(3) . ? C10 C11 1.517(4) . ? C10 H10 0.97(3) . ? C11 C12 1.539(4) . ? C11 H11A 0.98(4) . ? C11 H11B 0.96(3) . ? C12 C13 1.513(4) . ? C12 H12A 0.93(3) . ? C12 H12B 0.99(3) . ? C13 C14 1.415(4) . ? C13 H13 0.91(3) . ? C14 C15 1.531(4) . ? C14 H14 1.00(3) . ? C15 C16 1.529(4) . ? C15 H15A 0.97(3) . ? C15 H15B 0.95(3) . ? C16 H16A 0.97(3) . ? C16 H16B 0.99(4) . ? C17 C19 1.524(4) . ? C17 C18 1.534(4) . ? C17 H17 0.86(3) . ? 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 C21 1.531(4) . ? C20 C22 1.531(4) . ? C20 H20 0.91(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.531(4) . ? C23 C25 1.533(4) . ? C23 H23 0.91(3) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C28 1.527(4) . ? C26 C27 1.529(4) . ? C26 H26 0.94(3) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 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 C5 Ir1 C1 94.67(12) . . ? C5 Ir1 C2 78.33(11) . . ? C1 Ir1 C2 37.87(11) . . ? C5 Ir1 C6 37.96(12) . . ? C1 Ir1 C6 78.24(12) . . ? C2 Ir1 C6 85.91(11) . . ? C5 Ir1 P2 98.03(10) . . ? C1 Ir1 P2 127.82(9) . . ? C2 Ir1 P2 96.39(9) . . ? C6 Ir1 P2 134.65(9) . . ? C5 Ir1 P1 127.89(9) . . ? C1 Ir1 P1 99.35(8) . . ? C2 Ir1 P1 135.76(8) . . ? C6 Ir1 P1 96.96(8) . . ? P2 Ir1 P1 111.30(3) . . ? C5 Ir1 Ir2 131.95(8) . . ? C1 Ir1 Ir2 133.37(8) . . ? C2 Ir1 Ir2 137.15(8) . . ? C6 Ir1 Ir2 136.93(8) . . ? P2 Ir1 Ir2 55.671(17) . . ? P1 Ir1 Ir2 55.634(19) . . ? C9 Ir2 C13 94.91(11) . . ? C9 Ir2 C14 78.63(11) . . ? C13 Ir2 C14 37.91(11) . . ? C9 Ir2 C10 38.24(12) . . ? C13 Ir2 C10 78.24(11) . . ? C14 Ir2 C10 86.17(11) . . ? C9 Ir2 P1 109.24(9) . . ? C13 Ir2 P1 116.18(9) . . ? C14 Ir2 P1 89.58(8) . . ? C10 Ir2 P1 147.34(8) . . ? C9 Ir2 P2 116.40(8) . . ? C13 Ir2 P2 109.78(8) . . ? C14 Ir2 P2 147.47(8) . . ? C10 Ir2 P2 90.02(8) . . ? P1 Ir2 P2 109.88(2) . . ? C9 Ir2 Ir1 132.32(8) . . ? C13 Ir2 Ir1 132.77(8) . . ? C14 Ir2 Ir1 136.74(8) . . ? C10 Ir2 Ir1 137.09(8) . . ? P1 Ir2 Ir1 54.978(17) . . ? P2 Ir2 Ir1 54.906(18) . . ? C20 P1 C17 101.60(14) . . ? C20 P1 Ir1 120.89(10) . . ? C17 P1 Ir1 123.10(10) . . ? C20 P1 Ir2 118.51(10) . . ? C17 P1 Ir2 122.65(11) . . ? Ir1 P1 Ir2 69.39(2) . . ? C23 P2 C26 102.13(14) . . ? C23 P2 Ir1 121.26(10) . . ? C26 P2 Ir1 121.26(10) . . ? C23 P2 Ir2 119.85(9) . . ? C26 P2 Ir2 122.05(9) . . ? Ir1 P2 Ir2 69.42(2) . . ? C2 C1 C8 123.7(3) . . ? C2 C1 Ir1 71.42(16) . . ? C8 C1 Ir1 113.2(2) . . ? C2 C1 H1 115(2) . . ? C8 C1 H1 112(2) . . ? Ir1 C1 H1 114(2) . . ? C1 C2 C3 123.7(3) . . ? C1 C2 Ir1 70.71(16) . . ? C3 C2 Ir1 115.25(19) . . ? C1 C2 H2 117.3(18) . . ? C3 C2 H2 113.1(17) . . ? Ir1 C2 H2 108.2(17) . . ? C2 C3 C4 111.6(2) . . ? C2 C3 H3A 111.5(18) . . ? C4 C3 H3A 107.9(19) . . ? C2 C3 H3B 109.4(19) . . ? C4 C3 H3B 107.7(19) . . ? H3A C3 H3B 109(3) . . ? C5 C4 C3 112.2(3) . . ? C5 C4 H4A 109(2) . . ? C3 C4 H4A 108(2) . . ? C5 C4 H4B 109(2) . . ? C3 C4 H4B 112(2) . . ? H4A C4 H4B 107(3) . . ? C6 C5 C4 123.9(3) . . ? C6 C5 Ir1 71.99(17) . . ? C4 C5 Ir1 113.3(2) . . ? C6 C5 H5 114(2) . . ? C4 C5 H5 115(2) . . ? Ir1 C5 H5 110(2) . . ? C5 C6 C7 123.7(3) . . ? C5 C6 Ir1 70.05(17) . . ? C7 C6 Ir1 115.5(2) . . ? C5 C6 H6 115(2) . . ? C7 C6 H6 115(2) . . ? Ir1 C6 H6 107.8(19) . . ? C6 C7 C8 112.1(3) . . ? C6 C7 H7A 111(2) . . ? C8 C7 H7A 108(2) . . ? C6 C7 H7B 108.3(19) . . ? C8 C7 H7B 111.7(19) . . ? H7A C7 H7B 106(3) . . ? C1 C8 C7 112.1(3) . . ? C1 C8 H8A 111(2) . . ? C7 C8 H8A 110.1(19) . . ? C1 C8 H8B 107(2) . . ? C7 C8 H8B 109(2) . . ? H8A C8 H8B 107(3) . . ? C10 C9 C16 121.6(3) . . ? C10 C9 Ir2 72.16(16) . . ? C16 C9 Ir2 114.5(2) . . ? C10 C9 H9 116.5(18) . . ? C16 C9 H9 115.6(17) . . ? Ir2 C9 H9 107.1(17) . . ? C9 C10 C11 123.2(3) . . ? C9 C10 Ir2 69.60(16) . . ? C11 C10 Ir2 115.87(19) . . ? C9 C10 H10 115.5(18) . . ? C11 C10 H10 113.6(19) . . ? Ir2 C10 H10 111.1(17) . . ? C10 C11 C12 111.7(2) . . ? C10 C11 H11A 112(2) . . ? C12 C11 H11A 111(2) . . ? C10 C11 H11B 105.2(17) . . ? C12 C11 H11B 111.3(18) . . ? H11A C11 H11B 106(3) . . ? C13 C12 C11 112.1(3) . . ? C13 C12 H12A 111.9(18) . . ? C11 C12 H12A 106.6(17) . . ? C13 C12 H12B 109.3(17) . . ? C11 C12 H12B 112.9(16) . . ? H12A C12 H12B 104(2) . . ? C14 C13 C12 122.6(3) . . ? C14 C13 Ir2 72.05(16) . . ? C12 C13 Ir2 114.2(2) . . ? C14 C13 H13 117(2) . . ? C12 C13 H13 113(2) . . ? Ir2 C13 H13 110.0(19) . . ? C13 C14 C15 123.8(3) . . ? C13 C14 Ir2 70.05(15) . . ? C15 C14 Ir2 115.27(19) . . ? C13 C14 H14 116.2(16) . . ? C15 C14 H14 113.9(16) . . ? Ir2 C14 H14 108.7(16) . . ? C16 C15 C14 112.5(2) . . ? C16 C15 H15A 110(2) . . ? C14 C15 H15A 110(2) . . ? C16 C15 H15B 108.9(19) . . ? C14 C15 H15B 109.1(19) . . ? H15A C15 H15B 105(3) . . ? C9 C16 C15 112.3(2) . . ? C9 C16 H16A 108.8(18) . . ? C15 C16 H16A 111.8(18) . . ? C9 C16 H16B 105(2) . . ? C15 C16 H16B 113(2) . . ? H16A C16 H16B 105(3) . . ? C19 C17 C18 109.9(3) . . ? C19 C17 P1 113.1(2) . . ? C18 C17 P1 111.0(2) . . ? C19 C17 H17 110(2) . . ? C18 C17 H17 111(2) . . ? P1 C17 H17 102(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C22 110.9(2) . . ? C21 C20 P1 112.3(2) . . ? C22 C20 P1 112.7(2) . . ? C21 C20 H20 107(2) . . ? C22 C20 H20 108(2) . . ? P1 C20 H20 106(2) . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 110.4(2) . . ? C24 C23 P2 113.0(2) . . ? C25 C23 P2 112.4(2) . . ? C24 C23 H23 107.0(19) . . ? C25 C23 H23 105.6(19) . . ? P2 C23 H23 107.9(18) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C27 109.1(2) . . ? C28 C26 P2 110.3(2) . . ? C27 C26 P2 113.9(2) . . ? C28 C26 H26 111.7(18) . . ? C27 C26 H26 109.1(19) . . ? P2 C26 H26 102.6(18) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 Ir1 Ir2 C9 162.71(17) . . . . ? C1 Ir1 Ir2 C9 -16.65(16) . . . . ? C2 Ir1 Ir2 C9 38.01(16) . . . . ? C6 Ir1 Ir2 C9 -143.51(18) . . . . ? P2 Ir1 Ir2 C9 95.45(12) . . . . ? P1 Ir1 Ir2 C9 -84.60(12) . . . . ? C5 Ir1 Ir2 C13 -17.77(17) . . . . ? C1 Ir1 Ir2 C13 162.87(16) . . . . ? C2 Ir1 Ir2 C13 -142.47(16) . . . . ? C6 Ir1 Ir2 C13 36.01(18) . . . . ? P2 Ir1 Ir2 C13 -85.03(11) . . . . ? P1 Ir1 Ir2 C13 94.92(11) . . . . ? C5 Ir1 Ir2 C14 -71.94(17) . . . . ? C1 Ir1 Ir2 C14 108.70(16) . . . . ? C2 Ir1 Ir2 C14 163.36(16) . . . . ? C6 Ir1 Ir2 C14 -18.16(18) . . . . ? P2 Ir1 Ir2 C14 -139.20(12) . . . . ? P1 Ir1 Ir2 C14 40.75(12) . . . . ? C5 Ir1 Ir2 C10 108.21(17) . . . . ? C1 Ir1 Ir2 C10 -71.16(17) . . . . ? C2 Ir1 Ir2 C10 -16.50(17) . . . . ? C6 Ir1 Ir2 C10 161.98(18) . . . . ? P2 Ir1 Ir2 C10 40.94(12) . . . . ? P1 Ir1 Ir2 C10 -139.11(12) . . . . ? C5 Ir1 Ir2 P1 -112.68(12) . . . . ? C1 Ir1 Ir2 P1 67.95(12) . . . . ? C2 Ir1 Ir2 P1 122.61(12) . . . . ? C6 Ir1 Ir2 P1 -58.90(14) . . . . ? P2 Ir1 Ir2 P1 -179.94(3) . . . . ? C5 Ir1 Ir2 P2 67.26(12) . . . . ? C1 Ir1 Ir2 P2 -112.10(12) . . . . ? C2 Ir1 Ir2 P2 -57.44(12) . . . . ? C6 Ir1 Ir2 P2 121.04(14) . . . . ? P1 Ir1 Ir2 P2 179.94(3) . . . . ? C5 Ir1 P1 C20 7.94(17) . . . . ? C1 Ir1 P1 C20 111.39(14) . . . . ? C2 Ir1 P1 C20 123.51(16) . . . . ? C6 Ir1 P1 C20 32.23(15) . . . . ? P2 Ir1 P1 C20 -111.62(12) . . . . ? Ir2 Ir1 P1 C20 -111.67(12) . . . . ? C5 Ir1 P1 C17 -124.10(17) . . . . ? C1 Ir1 P1 C17 -20.65(15) . . . . ? C2 Ir1 P1 C17 -8.53(17) . . . . ? C6 Ir1 P1 C17 -99.81(15) . . . . ? P2 Ir1 P1 C17 116.34(13) . . . . ? Ir2 Ir1 P1 C17 116.29(13) . . . . ? C5 Ir1 P1 Ir2 119.61(11) . . . . ? C1 Ir1 P1 Ir2 -136.94(9) . . . . ? C2 Ir1 P1 Ir2 -124.81(11) . . . . ? C6 Ir1 P1 Ir2 143.90(9) . . . . ? P2 Ir1 P1 Ir2 0.05(3) . . . . ? C9 Ir2 P1 C20 -116.40(14) . . . . ? C13 Ir2 P1 C20 -10.59(14) . . . . ? C14 Ir2 P1 C20 -38.60(13) . . . . ? C10 Ir2 P1 C20 -120.84(18) . . . . ? P2 Ir2 P1 C20 114.78(11) . . . . ? Ir1 Ir2 P1 C20 114.83(11) . . . . ? C9 Ir2 P1 C17 11.90(15) . . . . ? C13 Ir2 P1 C17 117.72(14) . . . . ? C14 Ir2 P1 C17 89.70(14) . . . . ? C10 Ir2 P1 C17 7.47(19) . . . . ? P2 Ir2 P1 C17 -116.92(12) . . . . ? Ir1 Ir2 P1 C17 -116.87(12) . . . . ? C9 Ir2 P1 Ir1 128.77(8) . . . . ? C13 Ir2 P1 Ir1 -125.41(9) . . . . ? C14 Ir2 P1 Ir1 -153.43(8) . . . . ? C10 Ir2 P1 Ir1 124.34(14) . . . . ? P2 Ir2 P1 Ir1 -0.05(3) . . . . ? C5 Ir1 P2 C23 110.64(13) . . . . ? C1 Ir1 P2 C23 8.31(15) . . . . ? C2 Ir1 P2 C23 31.57(13) . . . . ? C6 Ir1 P2 C23 122.13(15) . . . . ? P1 Ir1 P2 C23 -113.26(11) . . . . ? Ir2 Ir1 P2 C23 -113.20(11) . . . . ? C5 Ir1 P2 C26 -20.36(13) . . . . ? C1 Ir1 P2 C26 -122.69(14) . . . . ? C2 Ir1 P2 C26 -99.42(13) . . . . ? C6 Ir1 P2 C26 -8.86(16) . . . . ? P1 Ir1 P2 C26 115.75(11) . . . . ? Ir2 Ir1 P2 C26 115.80(11) . . . . ? C5 Ir1 P2 Ir2 -136.16(8) . . . . ? C1 Ir1 P2 Ir2 121.51(10) . . . . ? C2 Ir1 P2 Ir2 144.78(8) . . . . ? C6 Ir1 P2 Ir2 -124.67(11) . . . . ? P1 Ir1 P2 Ir2 -0.05(3) . . . . ? C9 Ir2 P2 C23 -9.68(15) . . . . ? C13 Ir2 P2 C23 -115.93(14) . . . . ? C14 Ir2 P2 C23 -121.33(18) . . . . ? C10 Ir2 P2 C23 -38.44(14) . . . . ? P1 Ir2 P2 C23 115.11(12) . . . . ? Ir1 Ir2 P2 C23 115.07(12) . . . . ? C9 Ir2 P2 C26 120.49(15) . . . . ? C13 Ir2 P2 C26 14.24(15) . . . . ? C14 Ir2 P2 C26 8.85(19) . . . . ? C10 Ir2 P2 C26 91.74(14) . . . . ? P1 Ir2 P2 C26 -114.71(12) . . . . ? Ir1 Ir2 P2 C26 -114.76(12) . . . . ? C9 Ir2 P2 Ir1 -124.74(10) . . . . ? C13 Ir2 P2 Ir1 129.00(9) . . . . ? C14 Ir2 P2 Ir1 123.61(15) . . . . ? C10 Ir2 P2 Ir1 -153.50(8) . . . . ? P1 Ir2 P2 Ir1 0.05(3) . . . . ? C5 Ir1 C1 C2 -64.17(19) . . . . ? C6 Ir1 C1 C2 -98.58(18) . . . . ? P2 Ir1 C1 C2 39.8(2) . . . . ? P1 Ir1 C1 C2 166.19(15) . . . . ? Ir2 Ir1 C1 C2 115.35(16) . . . . ? C5 Ir1 C1 C8 55.4(2) . . . . ? C2 Ir1 C1 C8 119.5(3) . . . . ? C6 Ir1 C1 C8 21.0(2) . . . . ? P2 Ir1 C1 C8 159.30(18) . . . . ? P1 Ir1 C1 C8 -74.3(2) . . . . ? Ir2 Ir1 C1 C8 -125.1(2) . . . . ? C8 C1 C2 C3 2.1(5) . . . . ? Ir1 C1 C2 C3 108.1(3) . . . . ? C8 C1 C2 Ir1 -105.9(3) . . . . ? C5 Ir1 C2 C1 113.6(2) . . . . ? C6 Ir1 C2 C1 76.05(19) . . . . ? P2 Ir1 C2 C1 -149.44(16) . . . . ? P1 Ir1 C2 C1 -19.7(2) . . . . ? Ir2 Ir1 C2 C1 -104.99(18) . . . . ? C5 Ir1 C2 C3 -5.4(2) . . . . ? C1 Ir1 C2 C3 -119.0(3) . . . . ? C6 Ir1 C2 C3 -42.9(2) . . . . ? P2 Ir1 C2 C3 91.6(2) . . . . ? P1 Ir1 C2 C3 -138.73(19) . . . . ? Ir2 Ir1 C2 C3 136.01(19) . . . . ? C1 C2 C3 C4 -94.1(4) . . . . ? Ir1 C2 C3 C4 -11.2(4) . . . . ? C2 C3 C4 C5 29.1(4) . . . . ? C3 C4 C5 C6 49.0(4) . . . . ? C3 C4 C5 Ir1 -34.3(4) . . . . ? C1 Ir1 C5 C6 -64.07(19) . . . . ? C2 Ir1 C5 C6 -98.41(19) . . . . ? P2 Ir1 C5 C6 166.68(16) . . . . ? P1 Ir1 C5 C6 41.6(2) . . . . ? Ir2 Ir1 C5 C6 116.40(17) . . . . ? C1 Ir1 C5 C4 55.9(3) . . . . ? C2 Ir1 C5 C4 21.5(2) . . . . ? C6 Ir1 C5 C4 119.9(3) . . . . ? P2 Ir1 C5 C4 -73.4(2) . . . . ? P1 Ir1 C5 C4 161.5(2) . . . . ? Ir2 Ir1 C5 C4 -123.7(2) . . . . ? C4 C5 C6 C7 1.5(5) . . . . ? Ir1 C5 C6 C7 107.9(3) . . . . ? C4 C5 C6 Ir1 -106.4(3) . . . . ? C1 Ir1 C6 C5 113.72(19) . . . . ? C2 Ir1 C6 C5 76.23(18) . . . . ? P2 Ir1 C6 C5 -18.7(2) . . . . ? P1 Ir1 C6 C5 -148.13(16) . . . . ? Ir2 Ir1 C6 C5 -102.73(18) . . . . ? C5 Ir1 C6 C7 -118.8(3) . . . . ? C1 Ir1 C6 C7 -5.1(2) . . . . ? C2 Ir1 C6 C7 -42.6(2) . . . . ? P2 Ir1 C6 C7 -137.5(2) . . . . ? P1 Ir1 C6 C7 93.1(2) . . . . ? Ir2 Ir1 C6 C7 138.47(19) . . . . ? C5 C6 C7 C8 -93.4(4) . . . . ? Ir1 C6 C7 C8 -11.2(4) . . . . ? C2 C1 C8 C7 49.0(4) . . . . ? Ir1 C1 C8 C7 -33.5(3) . . . . ? C6 C7 C8 C1 28.7(4) . . . . ? C13 Ir2 C9 C10 63.93(18) . . . . ? C14 Ir2 C9 C10 98.34(18) . . . . ? P1 Ir2 C9 C10 -176.13(15) . . . . ? P2 Ir2 C9 C10 -51.01(18) . . . . ? Ir1 Ir2 C9 C10 -116.42(16) . . . . ? C13 Ir2 C9 C16 -53.4(3) . . . . ? C14 Ir2 C9 C16 -19.0(2) . . . . ? C10 Ir2 C9 C16 -117.3(3) . . . . ? P1 Ir2 C9 C16 66.6(2) . . . . ? P2 Ir2 C9 C16 -168.3(2) . . . . ? Ir1 Ir2 C9 C16 126.3(2) . . . . ? C16 C9 C10 C11 0.1(4) . . . . ? Ir2 C9 C10 C11 -108.2(3) . . . . ? C16 C9 C10 Ir2 108.3(3) . . . . ? C13 Ir2 C10 C9 -113.91(19) . . . . ? C14 Ir2 C10 C9 -76.45(18) . . . . ? P1 Ir2 C10 C9 6.8(3) . . . . ? P2 Ir2 C10 C9 135.88(16) . . . . ? Ir1 Ir2 C10 C9 103.45(17) . . . . ? C9 Ir2 C10 C11 117.9(3) . . . . ? C13 Ir2 C10 C11 4.0(2) . . . . ? C14 Ir2 C10 C11 41.5(2) . . . . ? P1 Ir2 C10 C11 124.7(2) . . . . ? P2 Ir2 C10 C11 -106.2(2) . . . . ? Ir1 Ir2 C10 C11 -138.60(18) . . . . ? C9 C10 C11 C12 93.0(3) . . . . ? Ir2 C10 C11 C12 11.4(3) . . . . ? C10 C11 C12 C13 -27.2(4) . . . . ? C11 C12 C13 C14 -52.0(4) . . . . ? C11 C12 C13 Ir2 31.5(3) . . . . ? C9 Ir2 C13 C14 64.39(19) . . . . ? C10 Ir2 C13 C14 98.99(18) . . . . ? P1 Ir2 C13 C14 -49.86(18) . . . . ? P2 Ir2 C13 C14 -175.28(15) . . . . ? Ir1 Ir2 C13 C14 -115.26(16) . . . . ? C9 Ir2 C13 C12 -54.0(2) . . . . ? C14 Ir2 C13 C12 -118.4(3) . . . . ? C10 Ir2 C13 C12 -19.4(2) . . . . ? P1 Ir2 C13 C12 -168.23(18) . . . . ? P2 Ir2 C13 C12 66.4(2) . . . . ? Ir1 Ir2 C13 C12 126.38(18) . . . . ? C12 C13 C14 C15 0.1(4) . . . . ? Ir2 C13 C14 C15 -107.7(3) . . . . ? C12 C13 C14 Ir2 107.8(3) . . . . ? C9 Ir2 C14 C13 -113.59(19) . . . . ? C10 Ir2 C14 C13 -75.73(18) . . . . ? P1 Ir2 C14 C13 136.68(17) . . . . ? P2 Ir2 C14 C13 8.3(3) . . . . ? Ir1 Ir2 C14 C13 104.37(18) . . . . ? C9 Ir2 C14 C15 5.3(2) . . . . ? C13 Ir2 C14 C15 118.9(3) . . . . ? C10 Ir2 C14 C15 43.2(2) . . . . ? P1 Ir2 C14 C15 -104.4(2) . . . . ? P2 Ir2 C14 C15 127.2(2) . . . . ? Ir1 Ir2 C14 C15 -136.7(2) . . . . ? C13 C14 C15 C16 90.9(4) . . . . ? Ir2 C14 C15 C16 8.8(4) . . . . ? C10 C9 C16 C15 -54.0(4) . . . . ? Ir2 C9 C16 C15 29.5(4) . . . . ? C14 C15 C16 C9 -24.3(4) . . . . ? C20 P1 C17 C19 48.2(3) . . . . ? Ir1 P1 C17 C19 -172.42(19) . . . . ? Ir2 P1 C17 C19 -87.1(2) . . . . ? C20 P1 C17 C18 172.2(2) . . . . ? Ir1 P1 C17 C18 -48.4(3) . . . . ? Ir2 P1 C17 C18 37.0(3) . . . . ? C17 P1 C20 C21 -177.3(2) . . . . ? Ir1 P1 C20 C21 42.2(2) . . . . ? Ir2 P1 C20 C21 -39.7(2) . . . . ? C17 P1 C20 C22 56.6(2) . . . . ? Ir1 P1 C20 C22 -83.9(2) . . . . ? Ir2 P1 C20 C22 -165.79(18) . . . . ? C26 P2 C23 C24 56.5(2) . . . . ? Ir1 P2 C23 C24 -82.2(2) . . . . ? Ir2 P2 C23 C24 -164.95(18) . . . . ? C26 P2 C23 C25 -177.6(2) . . . . ? Ir1 P2 C23 C25 43.7(2) . . . . ? Ir2 P2 C23 C25 -39.1(2) . . . . ? C23 P2 C26 C28 168.3(2) . . . . ? Ir1 P2 C26 C28 -53.0(2) . . . . ? Ir2 P2 C26 C28 31.0(2) . . . . ? C23 P2 C26 C27 45.2(2) . . . . ? Ir1 P2 C26 C27 -176.07(17) . . . . ? Ir2 P2 C26 C27 -92.1(2) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.974 _refine_diff_density_min -0.480 _refine_diff_density_rms 0.109 _database_code_depnum_ccdc_archive 'CCDC 951635'