# 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_comp2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H26 N6 Rh 1+, F6 P 1-' _chemical_formula_sum 'C22 H26 F6 N6 P Rh' _chemical_formula_weight 622.37 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' F F 0.0171 0.0103 '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' Rh Rh -1.1178 0.9187 '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 1 21/n 1' _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 8.8647(6) _cell_length_b 28.4028(15) _cell_length_c 9.9019(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.770(4) _cell_angle_gamma 90.00 _cell_volume 2487.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6290 _cell_measurement_theta_min 4.14 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.882 _exptl_absorpt_correction_T_max 0.907 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator 'multi-layer mirror' _diffrn_measurement_device_type 'Rigaku Saturn724' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24455 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.0347 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 27.51 _reflns_number_total 5662 _reflns_number_gt 5001 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction 'CrystalStructure 3.8' _computing_structure_solution SIR2004 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for win' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0322P)^2^+2.5384P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5662 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0497 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.32548(3) 0.123719(10) 0.82530(3) 0.02482(10) Uani 1 1 d . . . P1 P 0.75472(14) 0.17205(4) 1.21778(12) 0.0423(3) Uani 1 1 d . . . F1 F 0.7252(6) 0.22176(12) 1.1520(5) 0.123(2) Uani 1 1 d . . . F2 F 0.7931(6) 0.12185(14) 1.2783(5) 0.1085(16) Uani 1 1 d . . . F3 F 0.9234(5) 0.18809(16) 1.2443(5) 0.1063(15) Uani 1 1 d . . . F4A F 0.7754(6) 0.15352(19) 1.0701(5) 0.0729(14) Uiso 0.75 1 d P . . F5A F 0.5878(6) 0.15390(19) 1.2083(6) 0.0804(14) Uiso 0.75 1 d P . . F6A F 0.7422(8) 0.1875(2) 1.3710(7) 0.109(2) Uiso 0.75 1 d P . . F6B F 0.6667(13) 0.2041(4) 1.3224(12) 0.049(3) Uiso 0.25 1 d P . . F5B F 0.5894(12) 0.1621(4) 1.1364(11) 0.040(2) Uiso 0.25 1 d P . . F4B F 0.8365(13) 0.1475(4) 1.0957(11) 0.039(2) Uiso 0.25 1 d P . . N1 N 0.3264(4) 0.03543(12) 0.6479(3) 0.0308(7) Uani 1 1 d . . . N2 N 0.2522(3) 0.06045(11) 0.7382(3) 0.0275(6) Uani 1 1 d . . . N3 N 0.1198(4) 0.04183(13) 0.7568(4) 0.0373(8) Uani 1 1 d . . . N4 N 0.1031(4) 0.00370(13) 0.6771(4) 0.0406(8) Uani 1 1 d . . . N31 N 0.2819(4) 0.09484(11) 1.0147(3) 0.0261(6) Uani 1 1 d . . . N40 N 0.5275(3) 0.08874(10) 0.8830(3) 0.0256(6) Uani 1 1 d . . . C5 C 0.2304(5) 0.00086(14) 0.6128(4) 0.0325(8) Uani 1 1 d . . . C6 C 0.2619(6) -0.03729(16) 0.5149(4) 0.0472(11) Uani 1 1 d . . . H6A H 0.1784 -0.0392 0.4452 0.057 Uiso 1 1 calc R . . H6B H 0.2721 -0.0674 0.5629 0.057 Uiso 1 1 calc R . . H6C H 0.3561 -0.0303 0.4723 0.057 Uiso 1 1 calc R . . C11 C 0.4227(5) 0.19237(15) 0.7832(5) 0.0425(10) Uani 1 1 d . . . C12 C 0.3603(5) 0.17117(16) 0.6613(4) 0.0413(10) Uani 1 1 d . . . C13 C 0.2020(5) 0.16608(15) 0.6717(4) 0.0403(10) Uani 1 1 d . . . C14 C 0.1665(5) 0.18184(14) 0.8020(4) 0.0370(9) Uani 1 1 d . . . C15 C 0.3050(5) 0.19751(14) 0.8727(4) 0.0383(9) Uani 1 1 d . . . C16 C 0.5840(6) 0.2072(2) 0.8108(7) 0.0698(18) Uani 1 1 d . . . H16A H 0.6107 0.2056 0.9083 0.084 Uiso 1 1 calc R . . H16B H 0.5968 0.2395 0.7789 0.084 Uiso 1 1 calc R . . H16C H 0.6499 0.1860 0.7632 0.084 Uiso 1 1 calc R . . C17 C 0.4432(8) 0.1619(2) 0.5358(6) 0.081(2) Uani 1 1 d . . . H17A H 0.4081 0.1321 0.4948 0.098 Uiso 1 1 calc R . . H17B H 0.5520 0.1600 0.5600 0.098 Uiso 1 1 calc R . . H17C H 0.4234 0.1876 0.4710 0.098 Uiso 1 1 calc R . . C18 C 0.0923(8) 0.1471(2) 0.5649(6) 0.0743(19) Uani 1 1 d . . . H18A H 0.1422 0.1232 0.5122 0.089 Uiso 1 1 calc R . . H18B H 0.0560 0.1727 0.5050 0.089 Uiso 1 1 calc R . . H18C H 0.0066 0.1328 0.6075 0.089 Uiso 1 1 calc R . . C19 C 0.0108(6) 0.1872(2) 0.8508(7) 0.0675(17) Uani 1 1 d . . . H19A H 0.0172 0.1884 0.9499 0.081 Uiso 1 1 calc R . . H19B H -0.0516 0.1603 0.8200 0.081 Uiso 1 1 calc R . . H19C H -0.0348 0.2164 0.8144 0.081 Uiso 1 1 calc R . . C20 C 0.3185(8) 0.21813(18) 1.0118(5) 0.0638(16) Uani 1 1 d . . . H20A H 0.2498 0.2017 1.0693 0.077 Uiso 1 1 calc R . . H20B H 0.2919 0.2516 1.0072 0.077 Uiso 1 1 calc R . . H20C H 0.4227 0.2147 1.0500 0.077 Uiso 1 1 calc R . . C31 C 0.1495(5) 0.09831(15) 1.0725(4) 0.0360(9) Uani 1 1 d . . . H31 H 0.0669 0.1133 1.0239 0.043 Uiso 1 1 calc R . . C32 C 0.1291(6) 0.08084(16) 1.2000(4) 0.0441(11) Uani 1 1 d . . . H32 H 0.0344 0.0838 1.2390 0.053 Uiso 1 1 calc R . . C33 C 0.2484(6) 0.05923(16) 1.2689(4) 0.0466(11) Uani 1 1 d . . . H33 H 0.2377 0.0475 1.3576 0.056 Uiso 1 1 calc R . . C34 C 0.3843(5) 0.05430(15) 1.2102(4) 0.0388(9) Uani 1 1 d . . . H34 H 0.4670 0.0388 1.2572 0.047 Uiso 1 1 calc R . . C35 C 0.3985(4) 0.07239(12) 1.0813(3) 0.0262(7) Uani 1 1 d . . . C36 C 0.5353(4) 0.06777(12) 1.0064(4) 0.0258(7) Uani 1 1 d . . . C37 C 0.6634(5) 0.04353(14) 1.0538(4) 0.0344(8) Uani 1 1 d . . . H37 H 0.6672 0.0289 1.1403 0.041 Uiso 1 1 calc R . . C38 C 0.7848(5) 0.04071(15) 0.9751(5) 0.0394(9) Uani 1 1 d . . . H38 H 0.8736 0.0243 1.0067 0.047 Uiso 1 1 calc R . . C39 C 0.7765(5) 0.06193(16) 0.8498(5) 0.0393(9) Uani 1 1 d . . . H39 H 0.8596 0.0605 0.7940 0.047 Uiso 1 1 calc R . . C40 C 0.6466(4) 0.08518(14) 0.8068(4) 0.0333(8) Uani 1 1 d . . . H40 H 0.6407 0.0993 0.7197 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02492(16) 0.02607(16) 0.02388(15) 0.00512(10) 0.00477(10) 0.00515(11) P1 0.0418(6) 0.0395(6) 0.0458(6) -0.0116(5) 0.0041(5) -0.0045(5) F1 0.156(4) 0.0337(18) 0.169(5) -0.011(2) -0.072(4) 0.006(2) F2 0.141(4) 0.075(3) 0.106(3) 0.041(2) -0.014(3) -0.018(3) F3 0.066(2) 0.110(3) 0.140(4) 0.016(3) -0.024(2) -0.039(2) N1 0.0310(17) 0.0357(17) 0.0261(15) 0.0005(12) 0.0058(12) 0.0033(14) N2 0.0244(16) 0.0325(16) 0.0258(14) 0.0039(12) 0.0032(12) 0.0036(13) N3 0.0257(17) 0.0416(19) 0.0452(19) 0.0010(15) 0.0080(14) 0.0012(15) N4 0.036(2) 0.043(2) 0.043(2) 0.0003(15) 0.0001(15) -0.0045(16) N31 0.0290(16) 0.0270(15) 0.0226(14) 0.0037(11) 0.0048(12) 0.0011(13) N40 0.0226(15) 0.0255(15) 0.0288(15) 0.0005(11) 0.0024(12) 0.0038(12) C5 0.040(2) 0.0328(19) 0.0237(17) 0.0056(14) -0.0010(15) 0.0013(17) C6 0.066(3) 0.040(2) 0.035(2) -0.0031(18) 0.002(2) -0.004(2) C11 0.037(2) 0.032(2) 0.059(3) 0.0188(19) 0.004(2) 0.0015(18) C12 0.049(3) 0.042(2) 0.035(2) 0.0217(17) 0.0153(19) 0.012(2) C13 0.050(3) 0.034(2) 0.036(2) 0.0136(16) -0.0066(18) 0.0096(19) C14 0.033(2) 0.032(2) 0.046(2) 0.0163(17) 0.0070(17) 0.0138(17) C15 0.050(3) 0.0239(18) 0.040(2) 0.0063(15) 0.0019(19) 0.0073(18) C16 0.045(3) 0.053(3) 0.111(5) 0.029(3) -0.001(3) -0.010(3) C17 0.108(5) 0.090(5) 0.050(3) 0.033(3) 0.042(3) 0.037(4) C18 0.088(5) 0.062(4) 0.066(4) 0.009(3) -0.044(3) 0.012(3) C19 0.043(3) 0.063(3) 0.099(5) 0.028(3) 0.027(3) 0.027(3) C20 0.100(5) 0.042(3) 0.048(3) -0.006(2) -0.002(3) 0.016(3) C31 0.034(2) 0.039(2) 0.036(2) 0.0043(16) 0.0124(17) 0.0040(17) C32 0.053(3) 0.042(2) 0.040(2) 0.0037(18) 0.022(2) -0.001(2) C33 0.071(3) 0.043(2) 0.0277(19) 0.0075(17) 0.017(2) 0.001(2) C34 0.052(3) 0.036(2) 0.0278(19) 0.0061(15) -0.0006(17) 0.0037(19) C35 0.033(2) 0.0220(16) 0.0228(16) 0.0004(12) 0.0005(14) -0.0002(14) C36 0.0287(19) 0.0212(16) 0.0269(17) -0.0001(13) -0.0029(14) 0.0010(14) C37 0.036(2) 0.0311(19) 0.035(2) 0.0002(15) -0.0079(16) 0.0032(17) C38 0.030(2) 0.037(2) 0.050(2) -0.0062(18) -0.0099(18) 0.0081(17) C39 0.026(2) 0.043(2) 0.051(2) -0.0099(18) 0.0069(17) 0.0055(17) C40 0.028(2) 0.038(2) 0.0345(19) -0.0015(16) 0.0075(15) 0.0029(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 Rh1 N2 2.079(3) . ? Rh1 N40 2.094(3) . ? Rh1 N31 2.106(3) . ? Rh1 C12 2.148(4) . ? Rh1 C15 2.158(4) . ? Rh1 C14 2.173(4) . ? Rh1 C13 2.177(4) . ? Rh1 C11 2.183(4) . ? P1 F5A 1.564(6) . ? P1 F3 1.569(4) . ? P1 F1 1.570(4) . ? P1 F2 1.575(4) . ? P1 F4A 1.576(5) . ? P1 F6A 1.590(7) . ? P1 F4B 1.608(10) . ? P1 F6B 1.618(11) . ? P1 F5B 1.650(11) . ? N1 C5 1.331(5) . ? N1 N2 1.347(4) . ? N2 N3 1.311(5) . ? N3 N4 1.343(5) . ? N4 C5 1.334(5) . ? N31 C31 1.343(5) . ? N31 C35 1.349(5) . ? N40 C40 1.341(5) . ? N40 C36 1.357(4) . ? C5 C6 1.493(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C15 1.420(6) . ? C11 C12 1.428(7) . ? C11 C16 1.498(7) . ? C12 C13 1.422(6) . ? C12 C17 1.507(6) . ? C13 C14 1.420(6) . ? C13 C18 1.490(7) . ? C14 C15 1.443(6) . ? C14 C19 1.500(6) . ? C15 C20 1.494(6) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C31 C32 1.380(6) . ? C31 H31 0.9500 . ? C32 C33 1.366(7) . ? C32 H32 0.9500 . ? C33 C34 1.379(7) . ? C33 H33 0.9500 . ? C34 C35 1.390(5) . ? C34 H34 0.9500 . ? C35 C36 1.468(5) . ? C36 C37 1.383(5) . ? C37 C38 1.372(6) . ? C37 H37 0.9500 . ? C38 C39 1.377(6) . ? C38 H38 0.9500 . ? C39 C40 1.371(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 N2 Rh1 N40 86.63(12) . . ? N2 Rh1 N31 87.82(12) . . ? N40 Rh1 N31 77.06(12) . . ? N2 Rh1 C12 106.58(16) . . ? N40 Rh1 C12 109.92(15) . . ? N31 Rh1 C12 164.05(15) . . ? N2 Rh1 C15 154.34(15) . . ? N40 Rh1 C15 118.95(15) . . ? N31 Rh1 C15 99.31(14) . . ? C12 Rh1 C15 64.74(17) . . ? N2 Rh1 C14 115.47(15) . . ? N40 Rh1 C14 157.87(15) . . ? N31 Rh1 C14 103.59(14) . . ? C12 Rh1 C14 64.37(16) . . ? C15 Rh1 C14 38.92(17) . . ? N2 Rh1 C13 93.39(15) . . ? N40 Rh1 C13 146.54(15) . . ? N31 Rh1 C13 136.39(15) . . ? C12 Rh1 C13 38.37(17) . . ? C15 Rh1 C13 64.50(16) . . ? C14 Rh1 C13 38.10(16) . . ? N2 Rh1 C11 144.06(16) . . ? N40 Rh1 C11 97.72(14) . . ? N31 Rh1 C11 128.00(16) . . ? C12 Rh1 C11 38.48(18) . . ? C15 Rh1 C11 38.18(17) . . ? C14 Rh1 C11 64.06(16) . . ? C13 Rh1 C11 63.89(17) . . ? F5A P1 F3 173.4(3) . . ? F5A P1 F1 98.1(3) . . ? F3 P1 F1 86.5(3) . . ? F5A P1 F2 84.5(3) . . ? F3 P1 F2 91.1(3) . . ? F1 P1 F2 176.4(3) . . ? F5A P1 F4A 90.1(3) . . ? F3 P1 F4A 94.9(3) . . ? F1 P1 F4A 86.6(3) . . ? F2 P1 F4A 90.9(3) . . ? F5A P1 F6A 91.3(3) . . ? F3 P1 F6A 83.4(3) . . ? F1 P1 F6A 97.3(3) . . ? F2 P1 F6A 85.0(3) . . ? F4A P1 F6A 175.6(4) . . ? F3 P1 F4B 77.3(5) . . ? F1 P1 F4B 98.5(5) . . ? F2 P1 F4B 78.3(4) . . ? F3 P1 F6B 102.9(5) . . ? F1 P1 F6B 71.7(5) . . ? F2 P1 F6B 111.5(5) . . ? F4B P1 F6B 170.1(6) . . ? F3 P1 F5B 159.7(4) . . ? F1 P1 F5B 80.4(4) . . ? F2 P1 F5B 101.2(4) . . ? F4B P1 F5B 89.3(6) . . ? F6B P1 F5B 87.6(6) . . ? C5 N1 N2 103.3(3) . . ? N3 N2 N1 111.1(3) . . ? N3 N2 Rh1 123.3(3) . . ? N1 N2 Rh1 125.4(2) . . ? N2 N3 N4 108.0(3) . . ? C5 N4 N3 105.4(3) . . ? C31 N31 C35 119.3(3) . . ? C31 N31 Rh1 124.6(3) . . ? C35 N31 Rh1 116.1(2) . . ? C40 N40 C36 118.6(3) . . ? C40 N40 Rh1 125.0(3) . . ? C36 N40 Rh1 116.5(2) . . ? N1 C5 N4 112.2(4) . . ? N1 C5 C6 124.1(4) . . ? N4 C5 C6 123.7(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C15 C11 C12 108.1(4) . . ? C15 C11 C16 126.1(5) . . ? C12 C11 C16 125.8(5) . . ? C15 C11 Rh1 69.9(2) . . ? C12 C11 Rh1 69.4(2) . . ? C16 C11 Rh1 126.9(3) . . ? C13 C12 C11 108.1(4) . . ? C13 C12 C17 125.4(5) . . ? C11 C12 C17 126.0(5) . . ? C13 C12 Rh1 71.9(2) . . ? C11 C12 Rh1 72.1(2) . . ? C17 C12 Rh1 128.0(3) . . ? C14 C13 C12 108.2(4) . . ? C14 C13 C18 125.9(5) . . ? C12 C13 C18 125.9(5) . . ? C14 C13 Rh1 70.8(2) . . ? C12 C13 Rh1 69.7(2) . . ? C18 C13 Rh1 124.7(3) . . ? C13 C14 C15 107.8(4) . . ? C13 C14 C19 126.0(5) . . ? C15 C14 C19 125.7(5) . . ? C13 C14 Rh1 71.1(2) . . ? C15 C14 Rh1 70.0(2) . . ? C19 C14 Rh1 130.3(3) . . ? C11 C15 C14 107.6(4) . . ? C11 C15 C20 126.7(5) . . ? C14 C15 C20 125.6(5) . . ? C11 C15 Rh1 71.9(2) . . ? C14 C15 Rh1 71.1(2) . . ? C20 C15 Rh1 125.3(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N31 C31 C32 122.3(4) . . ? N31 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C33 C32 C31 118.3(4) . . ? C33 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C32 C33 C34 120.3(4) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C33 C34 C35 118.9(4) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N31 C35 C34 120.8(4) . . ? N31 C35 C36 115.3(3) . . ? C34 C35 C36 123.9(4) . . ? N40 C36 C37 121.1(4) . . ? N40 C36 C35 114.9(3) . . ? C37 C36 C35 124.0(3) . . ? C38 C37 C36 119.5(4) . . ? C38 C37 H37 120.2 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 119.3(4) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C40 C39 C38 119.0(4) . . ? C40 C39 H39 120.5 . . ? C38 C39 H39 120.5 . . ? N40 C40 C39 122.6(4) . . ? N40 C40 H40 118.7 . . ? C39 C40 H40 118.7 . . ? 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 N1 N2 N3 0.3(4) . . . . ? C5 N1 N2 Rh1 -174.4(2) . . . . ? N40 Rh1 N2 N3 132.2(3) . . . . ? N31 Rh1 N2 N3 55.0(3) . . . . ? C12 Rh1 N2 N3 -118.0(3) . . . . ? C15 Rh1 N2 N3 -52.1(5) . . . . ? C14 Rh1 N2 N3 -49.0(3) . . . . ? C13 Rh1 N2 N3 -81.4(3) . . . . ? C11 Rh1 N2 N3 -129.3(3) . . . . ? N40 Rh1 N2 N1 -53.8(3) . . . . ? N31 Rh1 N2 N1 -130.9(3) . . . . ? C12 Rh1 N2 N1 56.0(3) . . . . ? C15 Rh1 N2 N1 121.9(4) . . . . ? C14 Rh1 N2 N1 125.0(3) . . . . ? C13 Rh1 N2 N1 92.7(3) . . . . ? C11 Rh1 N2 N1 44.7(4) . . . . ? N1 N2 N3 N4 -0.4(4) . . . . ? Rh1 N2 N3 N4 174.4(2) . . . . ? N2 N3 N4 C5 0.4(4) . . . . ? N2 Rh1 N31 C31 -90.3(3) . . . . ? N40 Rh1 N31 C31 -177.3(3) . . . . ? C12 Rh1 N31 C31 64.7(7) . . . . ? C15 Rh1 N31 C31 64.9(3) . . . . ? C14 Rh1 N31 C31 25.4(4) . . . . ? C13 Rh1 N31 C31 2.4(4) . . . . ? C11 Rh1 N31 C31 93.0(4) . . . . ? N2 Rh1 N31 C35 91.2(3) . . . . ? N40 Rh1 N31 C35 4.2(2) . . . . ? C12 Rh1 N31 C35 -113.8(6) . . . . ? C15 Rh1 N31 C35 -113.6(3) . . . . ? C14 Rh1 N31 C35 -153.1(3) . . . . ? C13 Rh1 N31 C35 -176.2(3) . . . . ? C11 Rh1 N31 C35 -85.6(3) . . . . ? N2 Rh1 N40 C40 88.0(3) . . . . ? N31 Rh1 N40 C40 176.5(3) . . . . ? C12 Rh1 N40 C40 -18.4(4) . . . . ? C15 Rh1 N40 C40 -89.9(3) . . . . ? C14 Rh1 N40 C40 -89.2(5) . . . . ? C13 Rh1 N40 C40 -3.1(5) . . . . ? C11 Rh1 N40 C40 -56.2(3) . . . . ? N2 Rh1 N40 C36 -91.0(3) . . . . ? N31 Rh1 N40 C36 -2.5(2) . . . . ? C12 Rh1 N40 C36 162.5(3) . . . . ? C15 Rh1 N40 C36 91.1(3) . . . . ? C14 Rh1 N40 C36 91.8(4) . . . . ? C13 Rh1 N40 C36 177.9(3) . . . . ? C11 Rh1 N40 C36 124.8(3) . . . . ? N2 N1 C5 N4 -0.1(4) . . . . ? N2 N1 C5 C6 -179.0(4) . . . . ? N3 N4 C5 N1 -0.2(4) . . . . ? N3 N4 C5 C6 178.8(4) . . . . ? N2 Rh1 C11 C15 136.9(3) . . . . ? N40 Rh1 C11 C15 -128.2(3) . . . . ? N31 Rh1 C11 C15 -48.6(3) . . . . ? C12 Rh1 C11 C15 119.4(4) . . . . ? C14 Rh1 C11 C15 38.6(3) . . . . ? C13 Rh1 C11 C15 81.2(3) . . . . ? N2 Rh1 C11 C12 17.5(4) . . . . ? N40 Rh1 C11 C12 112.5(3) . . . . ? N31 Rh1 C11 C12 -168.0(2) . . . . ? C15 Rh1 C11 C12 -119.4(4) . . . . ? C14 Rh1 C11 C12 -80.7(3) . . . . ? C13 Rh1 C11 C12 -38.1(3) . . . . ? N2 Rh1 C11 C16 -102.4(5) . . . . ? N40 Rh1 C11 C16 -7.5(5) . . . . ? N31 Rh1 C11 C16 72.1(5) . . . . ? C12 Rh1 C11 C16 -119.9(6) . . . . ? C15 Rh1 C11 C16 120.7(6) . . . . ? C14 Rh1 C11 C16 159.3(6) . . . . ? C13 Rh1 C11 C16 -158.1(6) . . . . ? C15 C11 C12 C13 3.9(5) . . . . ? C16 C11 C12 C13 -175.4(4) . . . . ? Rh1 C11 C12 C13 63.3(3) . . . . ? C15 C11 C12 C17 176.1(4) . . . . ? C16 C11 C12 C17 -3.1(7) . . . . ? Rh1 C11 C12 C17 -124.4(5) . . . . ? C15 C11 C12 Rh1 -59.5(3) . . . . ? C16 C11 C12 Rh1 121.3(4) . . . . ? N2 Rh1 C12 C13 73.9(3) . . . . ? N40 Rh1 C12 C13 166.4(2) . . . . ? N31 Rh1 C12 C13 -79.9(6) . . . . ? C15 Rh1 C12 C13 -80.2(3) . . . . ? C14 Rh1 C12 C13 -36.9(3) . . . . ? C11 Rh1 C12 C13 -116.7(4) . . . . ? N2 Rh1 C12 C11 -169.4(2) . . . . ? N40 Rh1 C12 C11 -76.9(3) . . . . ? N31 Rh1 C12 C11 36.8(7) . . . . ? C15 Rh1 C12 C11 36.5(3) . . . . ? C14 Rh1 C12 C11 79.8(3) . . . . ? C13 Rh1 C12 C11 116.7(4) . . . . ? N2 Rh1 C12 C17 -47.3(6) . . . . ? N40 Rh1 C12 C17 45.2(6) . . . . ? N31 Rh1 C12 C17 158.9(5) . . . . ? C15 Rh1 C12 C17 158.7(6) . . . . ? C14 Rh1 C12 C17 -158.0(6) . . . . ? C13 Rh1 C12 C17 -121.2(7) . . . . ? C11 Rh1 C12 C17 122.1(6) . . . . ? C11 C12 C13 C14 -2.8(5) . . . . ? C17 C12 C13 C14 -175.2(4) . . . . ? Rh1 C12 C13 C14 60.6(3) . . . . ? C11 C12 C13 C18 177.7(4) . . . . ? C17 C12 C13 C18 5.4(7) . . . . ? Rh1 C12 C13 C18 -118.8(4) . . . . ? C11 C12 C13 Rh1 -63.4(3) . . . . ? C17 C12 C13 Rh1 124.2(5) . . . . ? N2 Rh1 C13 C14 128.5(3) . . . . ? N40 Rh1 C13 C14 -142.5(3) . . . . ? N31 Rh1 C13 C14 38.1(4) . . . . ? C12 Rh1 C13 C14 -118.8(4) . . . . ? C15 Rh1 C13 C14 -37.9(3) . . . . ? C11 Rh1 C13 C14 -80.5(3) . . . . ? N2 Rh1 C13 C12 -112.7(3) . . . . ? N40 Rh1 C13 C12 -23.7(4) . . . . ? N31 Rh1 C13 C12 156.9(3) . . . . ? C15 Rh1 C13 C12 80.8(3) . . . . ? C14 Rh1 C13 C12 118.8(4) . . . . ? C11 Rh1 C13 C12 38.3(3) . . . . ? N2 Rh1 C13 C18 7.6(5) . . . . ? N40 Rh1 C13 C18 96.6(5) . . . . ? N31 Rh1 C13 C18 -82.8(5) . . . . ? C12 Rh1 C13 C18 120.3(6) . . . . ? C15 Rh1 C13 C18 -158.8(5) . . . . ? C14 Rh1 C13 C18 -120.9(6) . . . . ? C11 Rh1 C13 C18 158.6(5) . . . . ? C12 C13 C14 C15 0.7(4) . . . . ? C18 C13 C14 C15 -179.8(4) . . . . ? Rh1 C13 C14 C15 60.7(3) . . . . ? C12 C13 C14 C19 173.5(4) . . . . ? C18 C13 C14 C19 -7.1(7) . . . . ? Rh1 C13 C14 C19 -126.6(4) . . . . ? C12 C13 C14 Rh1 -59.9(3) . . . . ? C18 C13 C14 Rh1 119.5(4) . . . . ? N2 Rh1 C14 C13 -59.9(3) . . . . ? N40 Rh1 C14 C13 117.0(4) . . . . ? N31 Rh1 C14 C13 -154.0(3) . . . . ? C12 Rh1 C14 C13 37.1(3) . . . . ? C15 Rh1 C14 C13 117.9(4) . . . . ? C11 Rh1 C14 C13 80.0(3) . . . . ? N2 Rh1 C14 C15 -177.9(2) . . . . ? N40 Rh1 C14 C15 -1.0(5) . . . . ? N31 Rh1 C14 C15 88.0(2) . . . . ? C12 Rh1 C14 C15 -80.8(3) . . . . ? C13 Rh1 C14 C15 -117.9(4) . . . . ? C11 Rh1 C14 C15 -37.9(3) . . . . ? N2 Rh1 C14 C19 61.8(5) . . . . ? N40 Rh1 C14 C19 -121.4(5) . . . . ? N31 Rh1 C14 C19 -32.3(5) . . . . ? C12 Rh1 C14 C19 158.8(6) . . . . ? C15 Rh1 C14 C19 -120.4(6) . . . . ? C13 Rh1 C14 C19 121.7(6) . . . . ? C11 Rh1 C14 C19 -158.3(6) . . . . ? C12 C11 C15 C14 -3.4(4) . . . . ? C16 C11 C15 C14 175.9(4) . . . . ? Rh1 C11 C15 C14 -62.5(3) . . . . ? C12 C11 C15 C20 -179.9(4) . . . . ? C16 C11 C15 C20 -0.6(7) . . . . ? Rh1 C11 C15 C20 121.0(4) . . . . ? C12 C11 C15 Rh1 59.1(3) . . . . ? C16 C11 C15 Rh1 -121.6(4) . . . . ? C13 C14 C15 C11 1.6(4) . . . . ? C19 C14 C15 C11 -171.1(4) . . . . ? Rh1 C14 C15 C11 63.0(3) . . . . ? C13 C14 C15 C20 178.2(4) . . . . ? C19 C14 C15 C20 5.4(7) . . . . ? Rh1 C14 C15 C20 -120.4(4) . . . . ? C13 C14 C15 Rh1 -61.4(3) . . . . ? C19 C14 C15 Rh1 125.9(4) . . . . ? N2 Rh1 C15 C11 -112.2(4) . . . . ? N40 Rh1 C15 C11 62.9(3) . . . . ? N31 Rh1 C15 C11 143.2(3) . . . . ? C12 Rh1 C15 C11 -36.8(3) . . . . ? C14 Rh1 C15 C11 -116.6(4) . . . . ? C13 Rh1 C15 C11 -79.5(3) . . . . ? N2 Rh1 C15 C14 4.5(5) . . . . ? N40 Rh1 C15 C14 179.6(2) . . . . ? N31 Rh1 C15 C14 -100.1(2) . . . . ? C12 Rh1 C15 C14 79.8(3) . . . . ? C13 Rh1 C15 C14 37.2(2) . . . . ? C11 Rh1 C15 C14 116.6(4) . . . . ? N2 Rh1 C15 C20 125.3(5) . . . . ? N40 Rh1 C15 C20 -59.7(5) . . . . ? N31 Rh1 C15 C20 20.6(5) . . . . ? C12 Rh1 C15 C20 -159.4(5) . . . . ? C14 Rh1 C15 C20 120.8(6) . . . . ? C13 Rh1 C15 C20 157.9(5) . . . . ? C11 Rh1 C15 C20 -122.6(6) . . . . ? C35 N31 C31 C32 1.9(6) . . . . ? Rh1 N31 C31 C32 -176.6(3) . . . . ? N31 C31 C32 C33 -0.1(7) . . . . ? C31 C32 C33 C34 -1.4(7) . . . . ? C32 C33 C34 C35 1.2(7) . . . . ? C31 N31 C35 C34 -2.1(5) . . . . ? Rh1 N31 C35 C34 176.5(3) . . . . ? C31 N31 C35 C36 176.3(3) . . . . ? Rh1 N31 C35 C36 -5.1(4) . . . . ? C33 C34 C35 N31 0.6(6) . . . . ? C33 C34 C35 C36 -177.6(4) . . . . ? C40 N40 C36 C37 0.6(5) . . . . ? Rh1 N40 C36 C37 179.7(3) . . . . ? C40 N40 C36 C35 -178.4(3) . . . . ? Rh1 N40 C36 C35 0.6(4) . . . . ? N31 C35 C36 N40 3.0(5) . . . . ? C34 C35 C36 N40 -178.7(4) . . . . ? N31 C35 C36 C37 -176.0(3) . . . . ? C34 C35 C36 C37 2.3(6) . . . . ? N40 C36 C37 C38 0.2(6) . . . . ? C35 C36 C37 C38 179.1(4) . . . . ? C36 C37 C38 C39 -0.3(6) . . . . ? C37 C38 C39 C40 -0.3(6) . . . . ? C36 N40 C40 C39 -1.2(6) . . . . ? Rh1 N40 C40 C39 179.8(3) . . . . ? C38 C39 C40 N40 1.1(6) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.323 _refine_diff_density_min -1.074 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 945547' ####################################################################### # # 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_comp3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H26 Ir N5' _chemical_formula_sum 'C23 H26 Ir N5' _chemical_formula_weight 564.69 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _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 8.7519(5) _cell_length_b 14.9783(7) _cell_length_c 31.9899(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4193.5(3) _cell_formula_units_Z 8 _cell_measurement_temperature 192(2) _cell_measurement_reflns_used 252332 _cell_measurement_theta_min 3.00 _cell_measurement_theta_max 27.57 _exptl_crystal_description columnar _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.789 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_absorpt_coefficient_mu 6.387 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.2981 _exptl_absorpt_correction_T_max 0.7005 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 192(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38798 _diffrn_reflns_av_R_equivalents 0.0455 _diffrn_reflns_av_sigmaI/netI 0.0252 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 27.49 _reflns_number_total 4801 _reflns_number_gt 3861 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'RAPID AUTO' _computing_cell_refinement 'RAPID AUTO' _computing_data_reduction 'RAPID AUTO' _computing_structure_solution 'Il Milione (Burla, et al., 2007)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2010)' _computing_molecular_graphics 'Ortep3 for win' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0185P)^2^+4.7222P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4801 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0500 _refine_ls_wR_factor_gt 0.0470 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.375542(13) 0.475666(7) 0.371847(3) 0.02526(5) Uani 1 1 d . . . N1 N 0.4992(3) 0.35626(16) 0.37189(7) 0.0289(5) Uani 1 1 d . . . N2 N 0.5428(3) 0.32157(17) 0.33414(8) 0.0361(6) Uani 1 1 d . . . N3 N 0.6302(3) 0.25342(18) 0.34136(10) 0.0431(7) Uani 1 1 d . . . N4 N 0.6471(3) 0.24126(18) 0.38311(10) 0.0422(7) Uani 1 1 d . . . N21 N 0.2258(3) 0.40643(16) 0.33246(7) 0.0305(5) Uani 1 1 d . . . C5 C 0.5657(4) 0.3058(2) 0.40094(10) 0.0343(7) Uani 1 1 d . . . C6 C 0.5538(4) 0.3192(2) 0.44672(10) 0.0461(8) Uani 1 1 d . . . H6A H 0.6101 0.2718 0.4612 0.055 Uiso 1 1 calc R . . H6B H 0.4462 0.3173 0.4551 0.055 Uiso 1 1 calc R . . H6C H 0.5974 0.3773 0.4542 0.055 Uiso 1 1 calc R . . C11 C 0.3427(4) 0.61000(19) 0.34758(10) 0.0321(7) Uani 1 1 d . . . C12 C 0.3556(4) 0.61374(19) 0.39169(9) 0.0326(7) Uani 1 1 d . . . C13 C 0.5057(4) 0.5804(2) 0.40300(10) 0.0361(7) Uani 1 1 d . . . C14 C 0.5846(4) 0.5599(2) 0.36503(12) 0.0397(8) Uani 1 1 d . . . C15 C 0.4879(4) 0.5783(2) 0.33059(10) 0.0372(7) Uani 1 1 d . . . C16 C 0.2072(4) 0.6384(2) 0.32252(12) 0.0495(9) Uani 1 1 d . . . H16A H 0.2158 0.7021 0.3158 0.059 Uiso 1 1 calc R . . H16B H 0.1138 0.6280 0.3387 0.059 Uiso 1 1 calc R . . H16C H 0.2031 0.6038 0.2966 0.059 Uiso 1 1 calc R . . C17 C 0.2394(5) 0.6510(2) 0.42125(11) 0.0500(9) Uani 1 1 d . . . H17A H 0.1367 0.6413 0.4099 0.060 Uiso 1 1 calc R . . H17B H 0.2570 0.7151 0.4249 0.060 Uiso 1 1 calc R . . H17C H 0.2483 0.6209 0.4483 0.060 Uiso 1 1 calc R . . C18 C 0.5756(5) 0.5829(3) 0.44581(12) 0.0600(11) Uani 1 1 d . . . H18A H 0.6263 0.6405 0.4501 0.072 Uiso 1 1 calc R . . H18B H 0.6507 0.5347 0.4484 0.072 Uiso 1 1 calc R . . H18C H 0.4954 0.5751 0.4669 0.072 Uiso 1 1 calc R . . C19 C 0.7453(4) 0.5248(2) 0.36159(16) 0.0633(12) Uani 1 1 d . . . H19A H 0.8174 0.5748 0.3626 0.076 Uiso 1 1 calc R . . H19B H 0.7572 0.4928 0.3351 0.076 Uiso 1 1 calc R . . H19C H 0.7658 0.4840 0.3849 0.076 Uiso 1 1 calc R . . C20 C 0.5319(6) 0.5747(3) 0.28541(12) 0.0633(12) Uani 1 1 d . . . H20A H 0.5824 0.5177 0.2795 0.076 Uiso 1 1 calc R . . H20B H 0.6020 0.6239 0.2791 0.076 Uiso 1 1 calc R . . H20C H 0.4401 0.5802 0.2681 0.076 Uiso 1 1 calc R . . C21 C 0.2472(4) 0.4002(2) 0.29076(9) 0.0369(7) Uani 1 1 d . . . H21 H 0.3341 0.4280 0.2786 0.044 Uiso 1 1 calc R . . C22 C 0.1465(4) 0.3548(2) 0.26523(10) 0.0427(8) Uani 1 1 d . . . H22 H 0.1631 0.3516 0.2359 0.051 Uiso 1 1 calc R . . C23 C 0.0217(4) 0.3142(2) 0.28320(11) 0.0453(9) Uani 1 1 d . . . H23 H -0.0506 0.2837 0.2663 0.054 Uiso 1 1 calc R . . C24 C 0.0021(4) 0.3180(2) 0.32583(11) 0.0395(8) Uani 1 1 d . . . H24 H -0.0822 0.2885 0.3384 0.047 Uiso 1 1 calc R . . C25 C 0.1047(3) 0.36472(19) 0.35040(10) 0.0305(6) Uani 1 1 d . . . C26 C 0.0992(3) 0.3754(2) 0.39582(9) 0.0312(6) Uani 1 1 d . . . C27 C -0.0172(4) 0.3392(2) 0.42059(11) 0.0409(8) Uani 1 1 d . . . H27 H -0.0969 0.3055 0.4081 0.049 Uiso 1 1 calc R . . C28 C -0.0156(4) 0.3527(2) 0.46316(11) 0.0464(9) Uani 1 1 d . . . H28 H -0.0947 0.3285 0.4800 0.056 Uiso 1 1 calc R . . C29 C 0.0996(4) 0.4011(2) 0.48124(10) 0.0443(9) Uani 1 1 d . . . H29 H 0.0999 0.4105 0.5106 0.053 Uiso 1 1 calc R . . C30 C 0.2165(4) 0.4367(2) 0.45675(9) 0.0368(7) Uani 1 1 d . . . H30 H 0.2956 0.4700 0.4698 0.044 Uiso 1 1 calc R . . C31 C 0.2199(3) 0.42468(19) 0.41353(9) 0.0281(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02327(7) 0.02147(6) 0.03105(7) 0.00087(4) -0.00013(4) -0.00051(5) N1 0.0265(13) 0.0243(12) 0.0359(13) 0.0017(10) 0.0018(10) -0.0011(10) N2 0.0332(15) 0.0309(13) 0.0441(15) -0.0019(12) 0.0086(12) 0.0014(12) N3 0.0328(16) 0.0318(14) 0.0647(19) -0.0058(13) 0.0057(14) 0.0000(13) N4 0.0299(16) 0.0295(14) 0.0671(19) -0.0019(14) -0.0034(13) 0.0020(12) N21 0.0300(14) 0.0270(12) 0.0346(13) 0.0026(10) -0.0046(10) 0.0004(11) C5 0.0239(15) 0.0258(15) 0.0530(19) 0.0049(14) -0.0020(14) -0.0031(13) C6 0.041(2) 0.047(2) 0.050(2) 0.0093(17) -0.0107(16) 0.0063(17) C11 0.0347(18) 0.0185(13) 0.0432(17) 0.0047(12) -0.0011(13) 0.0009(12) C12 0.0369(17) 0.0208(13) 0.0401(16) -0.0017(12) 0.0047(14) 0.0007(13) C13 0.0379(18) 0.0222(14) 0.0481(18) 0.0006(13) -0.0094(14) -0.0064(14) C14 0.0244(16) 0.0223(15) 0.073(2) -0.0010(15) 0.0038(15) -0.0019(13) C15 0.044(2) 0.0219(14) 0.0458(18) 0.0008(13) 0.0168(15) -0.0043(14) C16 0.052(2) 0.0364(18) 0.060(2) 0.0092(17) -0.0135(18) 0.0038(17) C17 0.059(2) 0.0338(17) 0.057(2) -0.0072(16) 0.0203(19) 0.0013(18) C18 0.069(3) 0.046(2) 0.065(2) 0.0001(19) -0.030(2) -0.016(2) C19 0.0261(19) 0.0314(19) 0.132(4) -0.001(2) 0.012(2) 0.0000(15) C20 0.097(4) 0.0360(19) 0.057(2) -0.0012(18) 0.037(2) -0.007(2) C21 0.0426(19) 0.0322(16) 0.0358(16) 0.0022(13) -0.0038(14) 0.0021(15) C22 0.055(2) 0.0346(17) 0.0388(17) -0.0026(14) -0.0155(16) 0.0053(16) C23 0.043(2) 0.0339(17) 0.059(2) -0.0071(16) -0.0198(17) 0.0034(16) C24 0.0316(18) 0.0303(16) 0.057(2) -0.0005(15) -0.0078(15) -0.0008(14) C25 0.0246(16) 0.0229(13) 0.0441(17) 0.0016(12) -0.0059(12) 0.0045(12) C26 0.0244(16) 0.0310(15) 0.0383(16) 0.0034(13) 0.0012(12) 0.0030(12) C27 0.0274(17) 0.0423(18) 0.053(2) 0.0090(16) -0.0012(14) -0.0042(15) C28 0.0306(18) 0.055(2) 0.054(2) 0.0143(18) 0.0103(15) -0.0021(17) C29 0.041(2) 0.055(2) 0.0374(17) 0.0083(15) 0.0055(14) 0.0082(17) C30 0.0307(17) 0.0418(18) 0.0378(16) -0.0001(14) -0.0002(13) 0.0001(15) C31 0.0236(15) 0.0252(14) 0.0356(15) 0.0025(12) 0.0016(11) 0.0031(12) _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 C31 2.053(3) . ? Ir1 N1 2.091(2) . ? Ir1 N21 2.093(2) . ? Ir1 C12 2.170(3) . ? Ir1 C11 2.176(3) . ? Ir1 C13 2.180(3) . ? Ir1 C14 2.233(3) . ? Ir1 C15 2.252(3) . ? N1 C5 1.332(4) . ? N1 N2 1.369(3) . ? N2 N3 1.296(4) . ? N3 N4 1.356(4) . ? N4 C5 1.330(4) . ? N21 C21 1.350(4) . ? N21 C25 1.358(4) . ? C5 C6 1.482(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C12 1.417(4) . ? C11 C15 1.462(4) . ? C11 C16 1.493(4) . ? C12 C13 1.451(4) . ? C12 C17 1.497(4) . ? C13 C14 1.431(5) . ? C13 C18 1.500(4) . ? C14 C15 1.416(5) . ? C14 C19 1.505(5) . ? C15 C20 1.497(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.380(5) . ? C21 H21 0.9500 . ? C22 C23 1.377(5) . ? C22 H22 0.9500 . ? C23 C24 1.376(5) . ? C23 H23 0.9500 . ? C24 C25 1.383(4) . ? C24 H24 0.9500 . ? C25 C26 1.463(4) . ? C26 C27 1.400(4) . ? C26 C31 1.408(4) . ? C27 C28 1.377(5) . ? C27 H27 0.9500 . ? C28 C29 1.370(5) . ? C28 H28 0.9500 . ? C29 C30 1.395(5) . ? C29 H29 0.9500 . ? C30 C31 1.395(4) . ? C30 H30 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 C31 Ir1 N1 91.42(10) . . ? C31 Ir1 N21 77.97(11) . . ? N1 Ir1 N21 84.29(10) . . ? C31 Ir1 C12 96.39(11) . . ? N1 Ir1 C12 148.94(11) . . ? N21 Ir1 C12 126.73(11) . . ? C31 Ir1 C11 119.21(11) . . ? N1 Ir1 C11 149.30(11) . . ? N21 Ir1 C11 99.24(10) . . ? C12 Ir1 C11 38.05(12) . . ? C31 Ir1 C13 108.50(12) . . ? N1 Ir1 C13 110.16(11) . . ? N21 Ir1 C13 163.56(10) . . ? C12 Ir1 C13 38.98(11) . . ? C11 Ir1 C13 64.34(11) . . ? C31 Ir1 C14 144.78(12) . . ? N1 Ir1 C14 93.39(11) . . ? N21 Ir1 C14 137.23(12) . . ? C12 Ir1 C14 63.65(12) . . ? C11 Ir1 C14 63.33(12) . . ? C13 Ir1 C14 37.81(12) . . ? C31 Ir1 C15 157.53(11) . . ? N1 Ir1 C15 110.99(10) . . ? N21 Ir1 C15 105.00(11) . . ? C12 Ir1 C15 63.64(11) . . ? C11 Ir1 C15 38.50(11) . . ? C13 Ir1 C15 63.16(12) . . ? C14 Ir1 C15 36.80(12) . . ? C5 N1 N2 106.2(2) . . ? C5 N1 Ir1 135.4(2) . . ? N2 N1 Ir1 117.94(18) . . ? N3 N2 N1 107.8(3) . . ? N2 N3 N4 110.2(3) . . ? C5 N4 N3 105.5(3) . . ? C21 N21 C25 119.6(3) . . ? C21 N21 Ir1 122.9(2) . . ? C25 N21 Ir1 117.54(19) . . ? N4 C5 N1 110.3(3) . . ? N4 C5 C6 124.1(3) . . ? N1 C5 C6 125.6(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C11 C15 108.3(3) . . ? C12 C11 C16 126.0(3) . . ? C15 C11 C16 125.7(3) . . ? C12 C11 Ir1 70.77(16) . . ? C15 C11 Ir1 73.59(16) . . ? C16 C11 Ir1 124.1(2) . . ? C11 C12 C13 107.9(3) . . ? C11 C12 C17 126.1(3) . . ? C13 C12 C17 125.9(3) . . ? C11 C12 Ir1 71.18(16) . . ? C13 C12 Ir1 70.85(16) . . ? C17 C12 Ir1 126.5(2) . . ? C14 C13 C12 107.4(3) . . ? C14 C13 C18 125.7(3) . . ? C12 C13 C18 126.0(3) . . ? C14 C13 Ir1 73.10(18) . . ? C12 C13 Ir1 70.17(16) . . ? C18 C13 Ir1 130.4(2) . . ? C15 C14 C13 109.3(3) . . ? C15 C14 C19 124.7(3) . . ? C13 C14 C19 126.0(4) . . ? C15 C14 Ir1 72.36(18) . . ? C13 C14 Ir1 69.08(17) . . ? C19 C14 Ir1 125.2(2) . . ? C14 C15 C11 107.1(3) . . ? C14 C15 C20 126.2(3) . . ? C11 C15 C20 126.5(3) . . ? C14 C15 Ir1 70.84(18) . . ? C11 C15 Ir1 67.91(16) . . ? C20 C15 Ir1 130.8(2) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N21 C21 C22 122.0(3) . . ? N21 C21 H21 119.0 . . ? C22 C21 H21 119.0 . . ? C23 C22 C21 118.5(3) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C24 C23 C22 119.6(3) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C23 C24 C25 120.2(3) . . ? C23 C24 H24 119.9 . . ? C25 C24 H24 119.9 . . ? N21 C25 C24 120.0(3) . . ? N21 C25 C26 113.3(2) . . ? C24 C25 C26 126.8(3) . . ? C27 C26 C31 121.4(3) . . ? C27 C26 C25 123.0(3) . . ? C31 C26 C25 115.6(3) . . ? C28 C27 C26 119.7(3) . . ? C28 C27 H27 120.1 . . ? C26 C27 H27 120.1 . . ? C29 C28 C27 120.2(3) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? C28 C29 C30 120.3(3) . . ? C28 C29 H29 119.8 . . ? C30 C29 H29 119.8 . . ? C29 C30 C31 121.6(3) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C30 C31 C26 116.8(3) . . ? C30 C31 Ir1 127.6(2) . . ? C26 C31 Ir1 115.5(2) . . ? 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 C31 Ir1 N1 C5 -56.0(3) . . . . ? N21 Ir1 N1 C5 -133.8(3) . . . . ? C12 Ir1 N1 C5 48.8(4) . . . . ? C11 Ir1 N1 C5 127.7(3) . . . . ? C13 Ir1 N1 C5 54.3(3) . . . . ? C14 Ir1 N1 C5 89.1(3) . . . . ? C15 Ir1 N1 C5 122.3(3) . . . . ? C31 Ir1 N1 N2 133.2(2) . . . . ? N21 Ir1 N1 N2 55.5(2) . . . . ? C12 Ir1 N1 N2 -121.9(2) . . . . ? C11 Ir1 N1 N2 -43.0(3) . . . . ? C13 Ir1 N1 N2 -116.5(2) . . . . ? C14 Ir1 N1 N2 -81.7(2) . . . . ? C15 Ir1 N1 N2 -48.4(2) . . . . ? C5 N1 N2 N3 0.4(3) . . . . ? Ir1 N1 N2 N3 173.6(2) . . . . ? N1 N2 N3 N4 -0.1(3) . . . . ? N2 N3 N4 C5 -0.2(4) . . . . ? C31 Ir1 N21 C21 -177.5(3) . . . . ? N1 Ir1 N21 C21 -84.8(2) . . . . ? C12 Ir1 N21 C21 93.5(3) . . . . ? C11 Ir1 N21 C21 64.4(2) . . . . ? C13 Ir1 N21 C21 67.4(5) . . . . ? C14 Ir1 N21 C21 4.0(3) . . . . ? C15 Ir1 N21 C21 25.4(3) . . . . ? C31 Ir1 N21 C25 1.0(2) . . . . ? N1 Ir1 N21 C25 93.7(2) . . . . ? C12 Ir1 N21 C25 -88.0(2) . . . . ? C11 Ir1 N21 C25 -117.1(2) . . . . ? C13 Ir1 N21 C25 -114.1(4) . . . . ? C14 Ir1 N21 C25 -177.5(2) . . . . ? C15 Ir1 N21 C25 -156.1(2) . . . . ? N3 N4 C5 N1 0.5(4) . . . . ? N3 N4 C5 C6 -178.8(3) . . . . ? N2 N1 C5 N4 -0.5(3) . . . . ? Ir1 N1 C5 N4 -172.0(2) . . . . ? N2 N1 C5 C6 178.7(3) . . . . ? Ir1 N1 C5 C6 7.3(5) . . . . ? C31 Ir1 C11 C12 59.5(2) . . . . ? N1 Ir1 C11 C12 -124.8(2) . . . . ? N21 Ir1 C11 C12 140.82(18) . . . . ? C13 Ir1 C11 C12 -38.24(18) . . . . ? C14 Ir1 C11 C12 -80.5(2) . . . . ? C15 Ir1 C11 C12 -116.7(3) . . . . ? C31 Ir1 C11 C15 176.17(18) . . . . ? N1 Ir1 C11 C15 -8.1(3) . . . . ? N21 Ir1 C11 C15 -102.52(19) . . . . ? C12 Ir1 C11 C15 116.7(3) . . . . ? C13 Ir1 C11 C15 78.4(2) . . . . ? C14 Ir1 C11 C15 36.11(18) . . . . ? C31 Ir1 C11 C16 -61.5(3) . . . . ? N1 Ir1 C11 C16 114.2(3) . . . . ? N21 Ir1 C11 C16 19.8(3) . . . . ? C12 Ir1 C11 C16 -121.0(4) . . . . ? C13 Ir1 C11 C16 -159.2(3) . . . . ? C14 Ir1 C11 C16 158.5(3) . . . . ? C15 Ir1 C11 C16 122.4(4) . . . . ? C15 C11 C12 C13 -2.8(3) . . . . ? C16 C11 C12 C13 -179.6(3) . . . . ? Ir1 C11 C12 C13 61.69(19) . . . . ? C15 C11 C12 C17 173.6(3) . . . . ? C16 C11 C12 C17 -3.3(5) . . . . ? Ir1 C11 C12 C17 -121.9(3) . . . . ? C15 C11 C12 Ir1 -64.5(2) . . . . ? C16 C11 C12 Ir1 118.7(3) . . . . ? C31 Ir1 C12 C11 -130.82(18) . . . . ? N1 Ir1 C12 C11 125.6(2) . . . . ? N21 Ir1 C12 C11 -51.1(2) . . . . ? C13 Ir1 C12 C11 117.5(3) . . . . ? C14 Ir1 C12 C11 79.6(2) . . . . ? C15 Ir1 C12 C11 38.38(18) . . . . ? C31 Ir1 C12 C13 111.67(19) . . . . ? N1 Ir1 C12 C13 8.1(3) . . . . ? N21 Ir1 C12 C13 -168.60(17) . . . . ? C11 Ir1 C12 C13 -117.5(3) . . . . ? C14 Ir1 C12 C13 -37.87(18) . . . . ? C15 Ir1 C12 C13 -79.1(2) . . . . ? C31 Ir1 C12 C17 -9.3(3) . . . . ? N1 Ir1 C12 C17 -112.9(3) . . . . ? N21 Ir1 C12 C17 70.4(3) . . . . ? C11 Ir1 C12 C17 121.5(4) . . . . ? C13 Ir1 C12 C17 -121.0(4) . . . . ? C14 Ir1 C12 C17 -158.9(3) . . . . ? C15 Ir1 C12 C17 159.9(3) . . . . ? C11 C12 C13 C14 2.2(3) . . . . ? C17 C12 C13 C14 -174.2(3) . . . . ? Ir1 C12 C13 C14 64.1(2) . . . . ? C11 C12 C13 C18 171.9(3) . . . . ? C17 C12 C13 C18 -4.5(5) . . . . ? Ir1 C12 C13 C18 -126.2(3) . . . . ? C11 C12 C13 Ir1 -61.90(19) . . . . ? C17 C12 C13 Ir1 121.7(3) . . . . ? C31 Ir1 C13 C14 166.93(18) . . . . ? N1 Ir1 C13 C14 68.3(2) . . . . ? N21 Ir1 C13 C14 -82.2(5) . . . . ? C12 Ir1 C13 C14 -116.2(3) . . . . ? C11 Ir1 C13 C14 -78.9(2) . . . . ? C15 Ir1 C13 C14 -35.74(19) . . . . ? C31 Ir1 C13 C12 -76.88(19) . . . . ? N1 Ir1 C13 C12 -175.55(16) . . . . ? N21 Ir1 C13 C12 34.0(5) . . . . ? C11 Ir1 C13 C12 37.34(17) . . . . ? C14 Ir1 C13 C12 116.2(3) . . . . ? C15 Ir1 C13 C12 80.46(19) . . . . ? C31 Ir1 C13 C18 44.0(4) . . . . ? N1 Ir1 C13 C18 -54.6(4) . . . . ? N21 Ir1 C13 C18 155.0(4) . . . . ? C12 Ir1 C13 C18 120.9(4) . . . . ? C11 Ir1 C13 C18 158.3(4) . . . . ? C14 Ir1 C13 C18 -122.9(4) . . . . ? C15 Ir1 C13 C18 -158.6(4) . . . . ? C12 C13 C14 C15 -0.7(3) . . . . ? C18 C13 C14 C15 -170.5(3) . . . . ? Ir1 C13 C14 C15 61.5(2) . . . . ? C12 C13 C14 C19 178.9(3) . . . . ? C18 C13 C14 C19 9.1(5) . . . . ? Ir1 C13 C14 C19 -119.0(3) . . . . ? C12 C13 C14 Ir1 -62.2(2) . . . . ? C18 C13 C14 Ir1 128.1(3) . . . . ? C31 Ir1 C14 C15 -141.4(2) . . . . ? N1 Ir1 C14 C15 121.32(18) . . . . ? N21 Ir1 C14 C15 36.1(3) . . . . ? C12 Ir1 C14 C15 -80.50(19) . . . . ? C11 Ir1 C14 C15 -37.77(18) . . . . ? C13 Ir1 C14 C15 -119.5(3) . . . . ? C31 Ir1 C14 C13 -21.8(3) . . . . ? N1 Ir1 C14 C13 -119.13(19) . . . . ? N21 Ir1 C14 C13 155.61(17) . . . . ? C12 Ir1 C14 C13 39.04(18) . . . . ? C11 Ir1 C14 C13 81.8(2) . . . . ? C15 Ir1 C14 C13 119.5(3) . . . . ? C31 Ir1 C14 C19 98.2(4) . . . . ? N1 Ir1 C14 C19 0.9(4) . . . . ? N21 Ir1 C14 C19 -84.4(4) . . . . ? C12 Ir1 C14 C19 159.1(4) . . . . ? C11 Ir1 C14 C19 -158.2(4) . . . . ? C13 Ir1 C14 C19 120.0(4) . . . . ? C15 Ir1 C14 C19 -120.4(4) . . . . ? C13 C14 C15 C11 -1.0(3) . . . . ? C19 C14 C15 C11 179.4(3) . . . . ? Ir1 C14 C15 C11 58.5(2) . . . . ? C13 C14 C15 C20 173.5(3) . . . . ? C19 C14 C15 C20 -6.1(5) . . . . ? Ir1 C14 C15 C20 -127.1(3) . . . . ? C13 C14 C15 Ir1 -59.4(2) . . . . ? C19 C14 C15 Ir1 121.0(3) . . . . ? C12 C11 C15 C14 2.4(3) . . . . ? C16 C11 C15 C14 179.2(3) . . . . ? Ir1 C11 C15 C14 -60.3(2) . . . . ? C12 C11 C15 C20 -172.1(3) . . . . ? C16 C11 C15 C20 4.8(5) . . . . ? Ir1 C11 C15 C20 125.2(3) . . . . ? C12 C11 C15 Ir1 62.69(19) . . . . ? C16 C11 C15 Ir1 -120.5(3) . . . . ? C31 Ir1 C15 C14 109.7(3) . . . . ? N1 Ir1 C15 C14 -66.0(2) . . . . ? N21 Ir1 C15 C14 -155.55(18) . . . . ? C12 Ir1 C15 C14 80.5(2) . . . . ? C11 Ir1 C15 C14 118.5(3) . . . . ? C13 Ir1 C15 C14 36.71(19) . . . . ? C31 Ir1 C15 C11 -8.8(4) . . . . ? N1 Ir1 C15 C11 175.57(17) . . . . ? N21 Ir1 C15 C11 86.00(19) . . . . ? C12 Ir1 C15 C11 -37.94(18) . . . . ? C13 Ir1 C15 C11 -81.75(19) . . . . ? C14 Ir1 C15 C11 -118.5(3) . . . . ? C31 Ir1 C15 C20 -128.6(4) . . . . ? N1 Ir1 C15 C20 55.8(4) . . . . ? N21 Ir1 C15 C20 -33.8(4) . . . . ? C12 Ir1 C15 C20 -157.7(4) . . . . ? C11 Ir1 C15 C20 -119.8(4) . . . . ? C13 Ir1 C15 C20 158.5(4) . . . . ? C14 Ir1 C15 C20 121.7(4) . . . . ? C25 N21 C21 C22 2.1(5) . . . . ? Ir1 N21 C21 C22 -179.5(2) . . . . ? N21 C21 C22 C23 -0.5(5) . . . . ? C21 C22 C23 C24 -1.5(5) . . . . ? C22 C23 C24 C25 2.0(5) . . . . ? C21 N21 C25 C24 -1.5(4) . . . . ? Ir1 N21 C25 C24 180.0(2) . . . . ? C21 N21 C25 C26 178.4(3) . . . . ? Ir1 N21 C25 C26 -0.1(3) . . . . ? C23 C24 C25 N21 -0.5(5) . . . . ? C23 C24 C25 C26 179.6(3) . . . . ? N21 C25 C26 C27 178.9(3) . . . . ? C24 C25 C26 C27 -1.2(5) . . . . ? N21 C25 C26 C31 -1.3(4) . . . . ? C24 C25 C26 C31 178.6(3) . . . . ? C31 C26 C27 C28 0.9(5) . . . . ? C25 C26 C27 C28 -179.4(3) . . . . ? C26 C27 C28 C29 -0.3(5) . . . . ? C27 C28 C29 C30 -0.3(5) . . . . ? C28 C29 C30 C31 0.2(5) . . . . ? C29 C30 C31 C26 0.4(5) . . . . ? C29 C30 C31 Ir1 177.2(3) . . . . ? C27 C26 C31 C30 -1.0(4) . . . . ? C25 C26 C31 C30 179.3(3) . . . . ? C27 C26 C31 Ir1 -178.1(2) . . . . ? C25 C26 C31 Ir1 2.1(3) . . . . ? N1 Ir1 C31 C30 97.7(3) . . . . ? N21 Ir1 C31 C30 -178.4(3) . . . . ? C12 Ir1 C31 C30 -52.2(3) . . . . ? C11 Ir1 C31 C30 -84.5(3) . . . . ? C13 Ir1 C31 C30 -14.1(3) . . . . ? C14 Ir1 C31 C30 -0.2(4) . . . . ? C15 Ir1 C31 C30 -78.2(4) . . . . ? N1 Ir1 C31 C26 -85.5(2) . . . . ? N21 Ir1 C31 C26 -1.7(2) . . . . ? C12 Ir1 C31 C26 124.6(2) . . . . ? C11 Ir1 C31 C26 92.3(2) . . . . ? C13 Ir1 C31 C26 162.7(2) . . . . ? C14 Ir1 C31 C26 176.6(2) . . . . ? C15 Ir1 C31 C26 98.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.033 _refine_diff_density_min -0.429 _refine_diff_density_rms 0.086 _database_code_depnum_ccdc_archive 'CCDC 945548' ####################################################################### # # 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_comp4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H26 N5 Rh, C H2 Cl2' _chemical_formula_sum 'C24 H28 Cl2 N5 Rh' _chemical_formula_weight 560.32 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 1 2/c 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.5018(19) _cell_length_b 7.6323(5) _cell_length_c 22.3074(15) _cell_angle_alpha 90.00 _cell_angle_beta 125.421(2) _cell_angle_gamma 90.00 _cell_volume 4787.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 191(2) _cell_measurement_reflns_used 22569 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.555 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7003 _exptl_absorpt_correction_T_max 0.8314 _exptl_absorpt_process_details ; Higashi, T. (1999). Program for Absorption Correction. Rigaku Corporation, Tokyo, Japan. ; _diffrn_ambient_temperature 191(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_reflns_number 22569 _diffrn_reflns_av_R_equivalents 0.0222 _diffrn_reflns_av_sigmaI/netI 0.0188 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5456 _reflns_number_gt 5012 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+8.2116P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5456 _refine_ls_number_parameters 296 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0275 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0618 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.648252(5) 1.049679(18) 0.537811(7) 0.01939(5) Uani 1 1 d . . . Cl1 Cl 0.44398(3) 0.82739(12) 0.28772(5) 0.0775(3) Uani 1 1 d . . . Cl2 Cl 0.43103(4) 0.46678(14) 0.31122(6) 0.0835(3) Uani 1 1 d . . . N1 N 0.62024(6) 0.8115(2) 0.48375(9) 0.0241(3) Uani 1 1 d . . . N2 N 0.63545(6) 0.7519(2) 0.44328(9) 0.0287(4) Uani 1 1 d . . . N3 N 0.60590(6) 0.6315(2) 0.39872(10) 0.0335(4) Uani 1 1 d . . . N4 N 0.57069(6) 0.6085(2) 0.40800(10) 0.0330(4) Uani 1 1 d . . . N21 N 0.71525(6) 0.9345(2) 0.58679(9) 0.0230(3) Uani 1 1 d . . . C1 C 0.45551(9) 0.6066(4) 0.27937(14) 0.0459(6) Uani 1 1 d . . . H1A H 0.4416 0.5800 0.2272 0.055 Uiso 1 1 calc R . . H1B H 0.4903 0.5874 0.3082 0.055 Uiso 1 1 calc R . . C30 C 0.63064(8) 0.9610(3) 0.65598(12) 0.0296(4) Uani 1 1 d . . . H30 H 0.6024 1.0293 0.6286 0.036 Uiso 1 1 calc R . . C31 C 0.66011(7) 0.9495(2) 0.63210(10) 0.0233(4) Uani 1 1 d . . . C5 C 0.58045(7) 0.7213(3) 0.46051(11) 0.0269(4) Uani 1 1 d . . . C6 C 0.55071(8) 0.7426(3) 0.48857(14) 0.0363(5) Uani 1 1 d . . . H6A H 0.5490 0.8670 0.4978 0.044 Uiso 1 1 calc R . . H6B H 0.5649 0.6765 0.5344 0.044 Uiso 1 1 calc R . . H6C H 0.5186 0.6984 0.4519 0.044 Uiso 1 1 calc R . . C29 C 0.64169(8) 0.8746(3) 0.71914(12) 0.0345(5) Uani 1 1 d . . . H29 H 0.6210 0.8847 0.7341 0.041 Uiso 1 1 calc R . . C28 C 0.68259(8) 0.7739(3) 0.76028(11) 0.0336(5) Uani 1 1 d . . . H28 H 0.6895 0.7122 0.8024 0.040 Uiso 1 1 calc R . . C27 C 0.71330(8) 0.7643(3) 0.73948(11) 0.0297(4) Uani 1 1 d . . . H27 H 0.7419 0.6984 0.7681 0.036 Uiso 1 1 calc R . . C26 C 0.70233(7) 0.8516(2) 0.67622(10) 0.0236(4) Uani 1 1 d . . . C11 C 0.66522(7) 1.3168(2) 0.52453(11) 0.0247(4) Uani 1 1 d . . . C12 C 0.63801(7) 1.2391(3) 0.45266(11) 0.0263(4) Uani 1 1 d . . . C13 C 0.59302(7) 1.1952(3) 0.43633(11) 0.0277(4) Uani 1 1 d . . . C14 C 0.59197(7) 1.2427(3) 0.49767(12) 0.0277(4) Uani 1 1 d . . . C15 C 0.63665(7) 1.3217(2) 0.55204(11) 0.0257(4) Uani 1 1 d . . . C16 C 0.71348(8) 1.3970(3) 0.56113(13) 0.0361(5) Uani 1 1 d . . . H16A H 0.7297 1.3970 0.6145 0.043 Uiso 1 1 calc R . . H16B H 0.7103 1.5178 0.5438 0.043 Uiso 1 1 calc R . . H16C H 0.7321 1.3289 0.5490 0.043 Uiso 1 1 calc R . . C17 C 0.65220(9) 1.2214(3) 0.40091(13) 0.0401(5) Uani 1 1 d . . . H17A H 0.6867 1.2348 0.4283 0.048 Uiso 1 1 calc R . . H17B H 0.6363 1.3122 0.3629 0.048 Uiso 1 1 calc R . . H17C H 0.6428 1.1055 0.3777 0.048 Uiso 1 1 calc R . . C18 C 0.55264(9) 1.1175(4) 0.36573(13) 0.0449(6) Uani 1 1 d . . . H18A H 0.5312 1.0564 0.3741 0.054 Uiso 1 1 calc R . . H18B H 0.5650 1.0342 0.3473 0.054 Uiso 1 1 calc R . . H18C H 0.5352 1.2108 0.3295 0.054 Uiso 1 1 calc R . . C19 C 0.54831(8) 1.2429(3) 0.49755(15) 0.0416(6) Uani 1 1 d . . . H19A H 0.5310 1.1324 0.4767 0.050 Uiso 1 1 calc R . . H19B H 0.5277 1.3410 0.4678 0.050 Uiso 1 1 calc R . . H19C H 0.5577 1.2552 0.5481 0.050 Uiso 1 1 calc R . . C20 C 0.64960(9) 1.4100(3) 0.62129(13) 0.0378(5) Uani 1 1 d . . . H20A H 0.6842 1.4076 0.6574 0.045 Uiso 1 1 calc R . . H20B H 0.6345 1.3485 0.6412 0.045 Uiso 1 1 calc R . . H20C H 0.6386 1.5318 0.6106 0.045 Uiso 1 1 calc R . . C21 C 0.74006(7) 0.9350(3) 0.55745(12) 0.0288(4) Uani 1 1 d . . . H21 H 0.7269 0.9934 0.5119 0.035 Uiso 1 1 calc R . . C22 C 0.78377(7) 0.8543(3) 0.59071(12) 0.0323(4) Uani 1 1 d . . . H22 H 0.8008 0.8600 0.5692 0.039 Uiso 1 1 calc R . . C23 C 0.80226(7) 0.7652(3) 0.65582(12) 0.0335(5) Uani 1 1 d . . . H23 H 0.8323 0.7090 0.6800 0.040 Uiso 1 1 calc R . . C24 C 0.77643(7) 0.7587(3) 0.68562(11) 0.0297(4) Uani 1 1 d . . . H24 H 0.7883 0.6954 0.7298 0.036 Uiso 1 1 calc R . . C25 C 0.73296(6) 0.8454(2) 0.65051(10) 0.0230(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02041(8) 0.02000(8) 0.01989(8) 0.00100(5) 0.01291(6) 0.00082(5) Cl1 0.0603(5) 0.0597(5) 0.0775(6) -0.0026(4) 0.0199(4) 0.0002(4) Cl2 0.0824(6) 0.0901(7) 0.0833(6) 0.0064(5) 0.0512(5) -0.0277(5) N1 0.0247(8) 0.0241(8) 0.0258(8) 0.0013(6) 0.0159(7) 0.0022(6) N2 0.0315(8) 0.0288(9) 0.0280(8) -0.0025(7) 0.0185(7) 0.0031(7) N3 0.0350(9) 0.0306(9) 0.0304(9) -0.0040(7) 0.0164(8) 0.0034(8) N4 0.0298(9) 0.0268(9) 0.0337(9) -0.0021(7) 0.0134(8) 0.0010(7) N21 0.0233(7) 0.0236(8) 0.0235(8) 0.0000(6) 0.0143(6) 0.0000(6) C1 0.0364(12) 0.0608(16) 0.0369(12) 0.0019(12) 0.0191(10) -0.0032(12) C30 0.0324(10) 0.0324(11) 0.0302(10) -0.0006(8) 0.0216(9) -0.0008(9) C31 0.0272(9) 0.0233(9) 0.0214(8) -0.0020(7) 0.0153(8) -0.0033(7) C5 0.0246(9) 0.0221(9) 0.0295(10) 0.0014(8) 0.0130(8) 0.0008(8) C6 0.0328(11) 0.0333(11) 0.0492(13) -0.0040(10) 0.0274(10) -0.0065(9) C29 0.0414(11) 0.0406(12) 0.0320(10) -0.0041(9) 0.0273(10) -0.0091(10) C28 0.0444(12) 0.0343(11) 0.0248(10) 0.0008(8) 0.0216(9) -0.0068(10) C27 0.0341(10) 0.0276(10) 0.0238(9) 0.0009(8) 0.0146(8) -0.0012(8) C26 0.0277(9) 0.0210(9) 0.0218(9) -0.0024(7) 0.0141(8) -0.0015(7) C11 0.0273(9) 0.0198(9) 0.0265(9) 0.0055(7) 0.0154(8) 0.0020(7) C12 0.0312(10) 0.0242(9) 0.0240(9) 0.0056(8) 0.0163(8) 0.0052(8) C13 0.0280(9) 0.0219(9) 0.0254(9) 0.0045(7) 0.0111(8) 0.0049(8) C14 0.0281(9) 0.0223(9) 0.0356(11) 0.0050(8) 0.0200(9) 0.0040(8) C15 0.0320(10) 0.0191(9) 0.0274(9) 0.0031(7) 0.0180(8) 0.0037(8) C16 0.0307(10) 0.0331(11) 0.0382(12) 0.0051(9) 0.0165(9) -0.0043(9) C17 0.0546(14) 0.0414(13) 0.0351(12) 0.0098(10) 0.0322(11) 0.0116(11) C18 0.0378(12) 0.0408(13) 0.0301(11) -0.0010(10) 0.0048(10) -0.0016(11) C19 0.0330(11) 0.0371(12) 0.0620(16) 0.0115(11) 0.0316(11) 0.0105(10) C20 0.0529(14) 0.0290(11) 0.0334(11) -0.0020(9) 0.0260(11) 0.0051(10) C21 0.0284(10) 0.0324(10) 0.0298(10) 0.0021(8) 0.0193(8) 0.0003(8) C22 0.0283(10) 0.0365(11) 0.0387(11) -0.0011(9) 0.0232(9) 0.0028(9) C23 0.0242(9) 0.0351(11) 0.0354(11) -0.0023(9) 0.0140(9) 0.0049(9) C24 0.0288(10) 0.0286(10) 0.0251(9) 0.0005(8) 0.0118(8) 0.0036(8) C25 0.0246(8) 0.0197(8) 0.0221(8) -0.0031(7) 0.0121(7) -0.0014(7) _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 Rh1 C31 2.0442(19) . ? Rh1 N1 2.0840(17) . ? Rh1 N21 2.0932(16) . ? Rh1 C15 2.1722(19) . ? Rh1 C14 2.1744(19) . ? Rh1 C11 2.1883(19) . ? Rh1 C13 2.2335(19) . ? Rh1 C12 2.2464(19) . ? Cl1 C1 1.766(3) . ? Cl2 C1 1.747(3) . ? N1 C5 1.343(3) . ? N1 N2 1.359(2) . ? N2 N3 1.303(3) . ? N3 N4 1.357(3) . ? N4 C5 1.330(3) . ? N21 C21 1.345(2) . ? N21 C25 1.360(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C30 C29 1.394(3) . ? C30 C31 1.398(3) . ? C30 H30 0.9500 . ? C31 C26 1.410(3) . ? C5 C6 1.489(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C29 C28 1.386(3) . ? C29 H29 0.9500 . ? C28 C27 1.383(3) . ? C28 H28 0.9500 . ? C27 C26 1.400(3) . ? C27 H27 0.9500 . ? C26 C25 1.467(3) . ? C11 C15 1.432(3) . ? C11 C12 1.435(3) . ? C11 C16 1.496(3) . ? C12 C13 1.414(3) . ? C12 C17 1.498(3) . ? C13 C14 1.436(3) . ? C13 C18 1.493(3) . ? C14 C15 1.429(3) . ? C14 C19 1.505(3) . ? C15 C20 1.497(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.381(3) . ? C21 H21 0.9500 . ? C22 C23 1.380(3) . ? C22 H22 0.9500 . ? C23 C24 1.387(3) . ? C23 H23 0.9500 . ? C24 C25 1.393(3) . ? C24 H24 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 C31 Rh1 N1 91.04(7) . . ? C31 Rh1 N21 78.69(7) . . ? N1 Rh1 N21 86.40(6) . . ? C31 Rh1 C15 98.69(7) . . ? N1 Rh1 C15 148.81(7) . . ? N21 Rh1 C15 124.49(7) . . ? C31 Rh1 C14 106.00(8) . . ? N1 Rh1 C14 110.42(7) . . ? N21 Rh1 C14 162.15(7) . . ? C15 Rh1 C14 38.40(8) . . ? C31 Rh1 C11 125.32(7) . . ? N1 Rh1 C11 143.63(7) . . ? N21 Rh1 C11 99.25(7) . . ? C15 Rh1 C11 38.34(7) . . ? C14 Rh1 C11 63.77(7) . . ? C31 Rh1 C13 140.65(8) . . ? N1 Rh1 C13 90.58(7) . . ? N21 Rh1 C13 140.63(7) . . ? C15 Rh1 C13 63.37(7) . . ? C14 Rh1 C13 38.01(7) . . ? C11 Rh1 C13 62.46(7) . . ? C31 Rh1 C12 161.90(7) . . ? N1 Rh1 C12 106.22(7) . . ? N21 Rh1 C12 107.25(7) . . ? C15 Rh1 C12 63.66(7) . . ? C14 Rh1 C12 63.28(7) . . ? C11 Rh1 C12 37.72(7) . . ? C13 Rh1 C12 36.80(7) . . ? C5 N1 N2 105.92(16) . . ? C5 N1 Rh1 134.28(13) . . ? N2 N1 Rh1 116.62(12) . . ? N3 N2 N1 108.06(16) . . ? N2 N3 N4 110.42(16) . . ? C5 N4 N3 104.98(17) . . ? C21 N21 C25 118.85(17) . . ? C21 N21 Rh1 124.49(13) . . ? C25 N21 Rh1 116.55(12) . . ? Cl2 C1 Cl1 110.40(15) . . ? Cl2 C1 H1A 109.6 . . ? Cl1 C1 H1A 109.6 . . ? Cl2 C1 H1B 109.6 . . ? Cl1 C1 H1B 109.6 . . ? H1A C1 H1B 108.1 . . ? C29 C30 C31 121.5(2) . . ? C29 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C30 C31 C26 116.92(17) . . ? C30 C31 Rh1 127.79(15) . . ? C26 C31 Rh1 115.24(13) . . ? N4 C5 N1 110.61(18) . . ? N4 C5 C6 123.83(19) . . ? N1 C5 C6 125.55(19) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C28 C29 C30 120.57(19) . . ? C28 C29 H29 119.7 . . ? C30 C29 H29 119.7 . . ? C27 C28 C29 119.40(19) . . ? C27 C28 H28 120.3 . . ? C29 C28 H28 120.3 . . ? C28 C27 C26 120.1(2) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C27 C26 C31 121.50(18) . . ? C27 C26 C25 122.95(18) . . ? C31 C26 C25 115.54(16) . . ? C15 C11 C12 108.82(17) . . ? C15 C11 C16 125.47(19) . . ? C12 C11 C16 125.40(18) . . ? C15 C11 Rh1 70.22(10) . . ? C12 C11 Rh1 73.34(11) . . ? C16 C11 Rh1 127.43(14) . . ? C13 C12 C11 107.18(17) . . ? C13 C12 C17 125.46(19) . . ? C11 C12 C17 127.15(19) . . ? C13 C12 Rh1 71.10(11) . . ? C11 C12 Rh1 68.94(10) . . ? C17 C12 Rh1 129.18(15) . . ? C12 C13 C14 108.95(17) . . ? C12 C13 C18 125.4(2) . . ? C14 C13 C18 125.6(2) . . ? C12 C13 Rh1 72.10(11) . . ? C14 C13 Rh1 68.77(11) . . ? C18 C13 Rh1 126.72(15) . . ? C15 C14 C13 107.73(17) . . ? C15 C14 C19 126.0(2) . . ? C13 C14 C19 125.2(2) . . ? C15 C14 Rh1 70.71(11) . . ? C13 C14 Rh1 73.22(11) . . ? C19 C14 Rh1 130.94(15) . . ? C14 C15 C11 107.29(17) . . ? C14 C15 C20 126.55(19) . . ? C11 C15 C20 125.88(19) . . ? C14 C15 Rh1 70.89(11) . . ? C11 C15 Rh1 71.44(10) . . ? C20 C15 Rh1 127.68(14) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N21 C21 C22 122.81(19) . . ? N21 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C23 C22 C21 118.68(19) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C22 C23 C24 119.24(19) . . ? C22 C23 H23 120.4 . . ? C24 C23 H23 120.4 . . ? C23 C24 C25 119.65(19) . . ? C23 C24 H24 120.2 . . ? C25 C24 H24 120.2 . . ? N21 C25 C24 120.72(17) . . ? N21 C25 C26 113.80(16) . . ? C24 C25 C26 125.48(18) . . ? 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 C31 Rh1 N1 C5 68.94(19) . . . . ? N21 Rh1 N1 C5 147.55(19) . . . . ? C15 Rh1 N1 C5 -39.8(3) . . . . ? C14 Rh1 N1 C5 -38.6(2) . . . . ? C11 Rh1 N1 C5 -111.72(19) . . . . ? C13 Rh1 N1 C5 -71.74(19) . . . . ? C12 Rh1 N1 C5 -105.53(19) . . . . ? C31 Rh1 N1 N2 -134.48(14) . . . . ? N21 Rh1 N1 N2 -55.88(13) . . . . ? C15 Rh1 N1 N2 116.73(16) . . . . ? C14 Rh1 N1 N2 118.00(13) . . . . ? C11 Rh1 N1 N2 44.85(19) . . . . ? C13 Rh1 N1 N2 84.84(14) . . . . ? C12 Rh1 N1 N2 51.04(14) . . . . ? C5 N1 N2 N3 -0.4(2) . . . . ? Rh1 N1 N2 N3 -163.13(13) . . . . ? N1 N2 N3 N4 0.2(2) . . . . ? N2 N3 N4 C5 0.0(2) . . . . ? C31 Rh1 N21 C21 179.62(17) . . . . ? N1 Rh1 N21 C21 87.83(16) . . . . ? C15 Rh1 N21 C21 -87.53(17) . . . . ? C14 Rh1 N21 C21 -73.2(3) . . . . ? C11 Rh1 N21 C21 -55.99(17) . . . . ? C13 Rh1 N21 C21 1.3(2) . . . . ? C12 Rh1 N21 C21 -18.04(18) . . . . ? C31 Rh1 N21 C25 3.50(13) . . . . ? N1 Rh1 N21 C25 -88.29(14) . . . . ? C15 Rh1 N21 C25 96.34(14) . . . . ? C14 Rh1 N21 C25 110.7(2) . . . . ? C11 Rh1 N21 C25 127.89(14) . . . . ? C13 Rh1 N21 C25 -174.81(13) . . . . ? C12 Rh1 N21 C25 165.84(13) . . . . ? C29 C30 C31 C26 -2.2(3) . . . . ? C29 C30 C31 Rh1 175.06(16) . . . . ? N1 Rh1 C31 C30 -94.98(18) . . . . ? N21 Rh1 C31 C30 178.90(19) . . . . ? C15 Rh1 C31 C30 55.29(19) . . . . ? C14 Rh1 C31 C30 16.6(2) . . . . ? C11 Rh1 C31 C30 85.51(19) . . . . ? C13 Rh1 C31 C30 -2.8(2) . . . . ? C12 Rh1 C31 C30 67.7(3) . . . . ? N1 Rh1 C31 C26 82.30(14) . . . . ? N21 Rh1 C31 C26 -3.82(14) . . . . ? C15 Rh1 C31 C26 -127.44(14) . . . . ? C14 Rh1 C31 C26 -166.09(14) . . . . ? C11 Rh1 C31 C26 -97.22(15) . . . . ? C13 Rh1 C31 C26 174.48(13) . . . . ? C12 Rh1 C31 C26 -115.0(2) . . . . ? N3 N4 C5 N1 -0.2(2) . . . . ? N3 N4 C5 C6 179.59(19) . . . . ? N2 N1 C5 N4 0.4(2) . . . . ? Rh1 N1 C5 N4 158.67(15) . . . . ? N2 N1 C5 C6 -179.45(19) . . . . ? Rh1 N1 C5 C6 -21.1(3) . . . . ? C31 C30 C29 C28 0.0(3) . . . . ? C30 C29 C28 C27 2.1(3) . . . . ? C29 C28 C27 C26 -1.8(3) . . . . ? C28 C27 C26 C31 -0.5(3) . . . . ? C28 C27 C26 C25 -179.30(19) . . . . ? C30 C31 C26 C27 2.4(3) . . . . ? Rh1 C31 C26 C27 -175.17(15) . . . . ? C30 C31 C26 C25 -178.66(17) . . . . ? Rh1 C31 C26 C25 3.8(2) . . . . ? C31 Rh1 C11 C15 -53.32(15) . . . . ? N1 Rh1 C11 C15 127.50(13) . . . . ? N21 Rh1 C11 C15 -135.97(12) . . . . ? C14 Rh1 C11 C15 38.25(12) . . . . ? C13 Rh1 C11 C15 81.05(13) . . . . ? C12 Rh1 C11 C15 117.75(17) . . . . ? C31 Rh1 C11 C12 -171.07(11) . . . . ? N1 Rh1 C11 C12 9.75(17) . . . . ? N21 Rh1 C11 C12 106.29(11) . . . . ? C15 Rh1 C11 C12 -117.75(17) . . . . ? C14 Rh1 C11 C12 -79.50(12) . . . . ? C13 Rh1 C11 C12 -36.70(11) . . . . ? C31 Rh1 C11 C16 66.8(2) . . . . ? N1 Rh1 C11 C16 -112.42(19) . . . . ? N21 Rh1 C11 C16 -15.88(19) . . . . ? C15 Rh1 C11 C16 120.1(2) . . . . ? C14 Rh1 C11 C16 158.3(2) . . . . ? C13 Rh1 C11 C16 -158.9(2) . . . . ? C12 Rh1 C11 C16 -122.2(2) . . . . ? C15 C11 C12 C13 -0.5(2) . . . . ? C16 C11 C12 C13 -174.39(19) . . . . ? Rh1 C11 C12 C13 61.17(13) . . . . ? C15 C11 C12 C17 174.49(19) . . . . ? C16 C11 C12 C17 0.6(3) . . . . ? Rh1 C11 C12 C17 -123.9(2) . . . . ? C15 C11 C12 Rh1 -61.63(13) . . . . ? C16 C11 C12 Rh1 124.4(2) . . . . ? C31 Rh1 C12 C13 -93.8(3) . . . . ? N1 Rh1 C12 C13 68.20(12) . . . . ? N21 Rh1 C12 C13 159.45(11) . . . . ? C15 Rh1 C12 C13 -80.02(13) . . . . ? C14 Rh1 C12 C13 -36.89(12) . . . . ? C11 Rh1 C12 C13 -117.80(16) . . . . ? C31 Rh1 C12 C11 24.0(3) . . . . ? N1 Rh1 C12 C11 -174.00(11) . . . . ? N21 Rh1 C12 C11 -82.75(12) . . . . ? C15 Rh1 C12 C11 37.78(11) . . . . ? C14 Rh1 C12 C11 80.91(12) . . . . ? C13 Rh1 C12 C11 117.80(16) . . . . ? C31 Rh1 C12 C17 145.5(2) . . . . ? N1 Rh1 C12 C17 -52.6(2) . . . . ? N21 Rh1 C12 C17 38.7(2) . . . . ? C15 Rh1 C12 C17 159.2(2) . . . . ? C14 Rh1 C12 C17 -157.7(2) . . . . ? C11 Rh1 C12 C17 121.4(2) . . . . ? C13 Rh1 C12 C17 -120.8(3) . . . . ? C11 C12 C13 C14 -0.7(2) . . . . ? C17 C12 C13 C14 -175.71(19) . . . . ? Rh1 C12 C13 C14 59.12(14) . . . . ? C11 C12 C13 C18 177.4(2) . . . . ? C17 C12 C13 C18 2.4(3) . . . . ? Rh1 C12 C13 C18 -122.8(2) . . . . ? C11 C12 C13 Rh1 -59.78(13) . . . . ? C17 C12 C13 Rh1 125.2(2) . . . . ? C31 Rh1 C13 C12 150.72(12) . . . . ? N1 Rh1 C13 C12 -116.93(12) . . . . ? N21 Rh1 C13 C12 -31.90(17) . . . . ? C15 Rh1 C13 C12 80.90(13) . . . . ? C14 Rh1 C13 C12 119.44(17) . . . . ? C11 Rh1 C13 C12 37.62(11) . . . . ? C31 Rh1 C13 C14 31.28(17) . . . . ? N1 Rh1 C13 C14 123.63(12) . . . . ? N21 Rh1 C13 C14 -151.34(12) . . . . ? C15 Rh1 C13 C14 -38.55(12) . . . . ? C11 Rh1 C13 C14 -81.82(12) . . . . ? C12 Rh1 C13 C14 -119.44(17) . . . . ? C31 Rh1 C13 C18 -88.0(2) . . . . ? N1 Rh1 C13 C18 4.4(2) . . . . ? N21 Rh1 C13 C18 89.4(2) . . . . ? C15 Rh1 C13 C18 -157.8(2) . . . . ? C14 Rh1 C13 C18 -119.3(2) . . . . ? C11 Rh1 C13 C18 158.9(2) . . . . ? C12 Rh1 C13 C18 121.3(2) . . . . ? C12 C13 C14 C15 1.5(2) . . . . ? C18 C13 C14 C15 -176.6(2) . . . . ? Rh1 C13 C14 C15 62.71(13) . . . . ? C12 C13 C14 C19 170.14(19) . . . . ? C18 C13 C14 C19 -8.0(3) . . . . ? Rh1 C13 C14 C19 -128.7(2) . . . . ? C12 C13 C14 Rh1 -61.18(14) . . . . ? C18 C13 C14 Rh1 120.7(2) . . . . ? C31 Rh1 C14 C15 83.76(12) . . . . ? N1 Rh1 C14 C15 -178.94(11) . . . . ? N21 Rh1 C14 C15 -19.2(3) . . . . ? C11 Rh1 C14 C15 -38.19(11) . . . . ? C13 Rh1 C14 C15 -116.26(16) . . . . ? C12 Rh1 C14 C15 -80.53(12) . . . . ? C31 Rh1 C14 C13 -159.97(11) . . . . ? N1 Rh1 C14 C13 -62.68(12) . . . . ? N21 Rh1 C14 C13 97.0(2) . . . . ? C15 Rh1 C14 C13 116.26(16) . . . . ? C11 Rh1 C14 C13 78.07(12) . . . . ? C12 Rh1 C14 C13 35.73(11) . . . . ? C31 Rh1 C14 C19 -37.6(2) . . . . ? N1 Rh1 C14 C19 59.7(2) . . . . ? N21 Rh1 C14 C19 -140.6(2) . . . . ? C15 Rh1 C14 C19 -121.4(3) . . . . ? C11 Rh1 C14 C19 -159.5(2) . . . . ? C13 Rh1 C14 C19 122.4(3) . . . . ? C12 Rh1 C14 C19 158.1(2) . . . . ? C13 C14 C15 C11 -1.8(2) . . . . ? C19 C14 C15 C11 -170.28(19) . . . . ? Rh1 C14 C15 C11 62.57(13) . . . . ? C13 C14 C15 C20 172.40(19) . . . . ? C19 C14 C15 C20 3.9(3) . . . . ? Rh1 C14 C15 C20 -123.3(2) . . . . ? C13 C14 C15 Rh1 -64.35(13) . . . . ? C19 C14 C15 Rh1 127.1(2) . . . . ? C12 C11 C15 C14 1.4(2) . . . . ? C16 C11 C15 C14 175.32(19) . . . . ? Rh1 C11 C15 C14 -62.21(13) . . . . ? C12 C11 C15 C20 -172.83(19) . . . . ? C16 C11 C15 C20 1.1(3) . . . . ? Rh1 C11 C15 C20 123.6(2) . . . . ? C12 C11 C15 Rh1 63.60(13) . . . . ? C16 C11 C15 Rh1 -122.47(19) . . . . ? C31 Rh1 C15 C14 -104.83(12) . . . . ? N1 Rh1 C15 C14 1.92(19) . . . . ? N21 Rh1 C15 C14 172.96(11) . . . . ? C11 Rh1 C15 C14 116.62(17) . . . . ? C13 Rh1 C15 C14 38.15(11) . . . . ? C12 Rh1 C15 C14 79.45(12) . . . . ? C31 Rh1 C15 C11 138.55(12) . . . . ? N1 Rh1 C15 C11 -114.70(15) . . . . ? N21 Rh1 C15 C11 56.34(14) . . . . ? C14 Rh1 C15 C11 -116.62(17) . . . . ? C13 Rh1 C15 C11 -78.47(12) . . . . ? C12 Rh1 C15 C11 -37.17(11) . . . . ? C31 Rh1 C15 C20 17.1(2) . . . . ? N1 Rh1 C15 C20 123.84(19) . . . . ? N21 Rh1 C15 C20 -65.1(2) . . . . ? C14 Rh1 C15 C20 121.9(2) . . . . ? C11 Rh1 C15 C20 -121.5(2) . . . . ? C13 Rh1 C15 C20 160.1(2) . . . . ? C12 Rh1 C15 C20 -158.6(2) . . . . ? C25 N21 C21 C22 -2.5(3) . . . . ? Rh1 N21 C21 C22 -178.57(16) . . . . ? N21 C21 C22 C23 1.8(3) . . . . ? C21 C22 C23 C24 0.3(3) . . . . ? C22 C23 C24 C25 -1.6(3) . . . . ? C21 N21 C25 C24 1.1(3) . . . . ? Rh1 N21 C25 C24 177.50(14) . . . . ? C21 N21 C25 C26 -178.84(17) . . . . ? Rh1 N21 C25 C26 -2.5(2) . . . . ? C23 C24 C25 N21 0.9(3) . . . . ? C23 C24 C25 C26 -179.14(19) . . . . ? C27 C26 C25 N21 178.10(18) . . . . ? C31 C26 C25 N21 -0.8(2) . . . . ? C27 C26 C25 C24 -1.9(3) . . . . ? C31 C26 C25 C24 179.22(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.889 _refine_diff_density_min -0.748 _refine_diff_density_rms 0.071 _database_code_depnum_ccdc_archive 'CCDC 945549' ####################################################################### # # 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_comp6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H49 N8 Rh2 3+, 3(F6 P 1-), C2 H3 N' _chemical_formula_sum 'C44 H52 F18 N9 P3 Rh2' _chemical_formula_weight 1347.68 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' Rh Rh -1.1178 0.9187 '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' F F 0.0171 0.0103 '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 1 21/c 1' _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 12.9484(6) _cell_length_b 21.5240(9) _cell_length_c 20.3894(9) _cell_angle_alpha 90.00 _cell_angle_beta 108.669(1) _cell_angle_gamma 90.00 _cell_volume 5383.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 68266 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.50 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2704 _exptl_absorpt_coefficient_mu 0.806 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6886 _exptl_absorpt_correction_T_max 0.9237 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85510 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12324 _reflns_number_gt 10876 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0437P)^2^+5.9061P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12324 _refine_ls_number_parameters 682 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0375 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0883 _refine_ls_wR_factor_gt 0.0856 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.041980(14) 0.136630(8) 0.325550(9) 0.02095(5) Uani 1 1 d . . . Rh2 Rh 0.364180(14) 0.326360(8) 0.482850(10) 0.02229(5) Uani 1 1 d . . . P1 P -0.13828(6) 0.38672(3) 0.49069(4) 0.03136(15) Uani 1 1 d . . . P2 P -0.03269(6) 0.11204(3) 0.63335(4) 0.03124(15) Uani 1 1 d . . . P3 P 0.53509(6) -0.00504(4) 0.28890(4) 0.04429(19) Uani 1 1 d . . . F11 F -0.2149(2) 0.32978(11) 0.49093(16) 0.0824(8) Uani 1 1 d . . . F12 F -0.03741(18) 0.34974(11) 0.54090(12) 0.0645(6) Uani 1 1 d . . . F13 F -0.1094(2) 0.36030(11) 0.42664(11) 0.0708(7) Uani 1 1 d . . . F14 F -0.23775(17) 0.42566(11) 0.44198(12) 0.0669(6) Uani 1 1 d . . . F15 F -0.1633(2) 0.41496(11) 0.55666(11) 0.0677(6) Uani 1 1 d . . . F16 F -0.06234(16) 0.44501(9) 0.49133(12) 0.0550(5) Uani 1 1 d . . . F21 F -0.12822(19) 0.08600(14) 0.56950(12) 0.0782(8) Uani 1 1 d . . . F22 F -0.0594(2) 0.18000(9) 0.60206(13) 0.0659(6) Uani 1 1 d . . . F23 F -0.11771(15) 0.12111(9) 0.67459(10) 0.0481(4) Uani 1 1 d . . . F24 F -0.0078(2) 0.04440(11) 0.66422(17) 0.0879(9) Uani 1 1 d . . . F25 F 0.05203(15) 0.10323(9) 0.59158(10) 0.0460(4) Uani 1 1 d . . . F26 F 0.06092(18) 0.14039(14) 0.69644(11) 0.0769(8) Uani 1 1 d . . . F31 F 0.4440(2) -0.04621(15) 0.23652(14) 0.0871(8) Uani 1 1 d . . . F32 F 0.44609(19) 0.04700(12) 0.28223(15) 0.0796(7) Uani 1 1 d . . . F33 F 0.50421(19) -0.03572(12) 0.35136(11) 0.0657(6) Uani 1 1 d . . . F34 F 0.6251(2) -0.05593(15) 0.29637(16) 0.1039(11) Uani 1 1 d . . . F35 F 0.56448(19) 0.02169(15) 0.22403(13) 0.0858(9) Uani 1 1 d . . . F36 F 0.6238(2) 0.03661(17) 0.34096(17) 0.1041(10) Uani 1 1 d . . . N1 N 0.18204(17) 0.19491(10) 0.34356(10) 0.0254(4) Uani 1 1 d . . . N2 N 0.20321(17) 0.23061(10) 0.40036(11) 0.0274(4) Uani 1 1 d . . . N3 N 0.29474(16) 0.25942(9) 0.40715(11) 0.0249(4) Uani 1 1 d . . . N4 N 0.33608(18) 0.24427(10) 0.35678(12) 0.0311(5) Uani 1 1 d . . . N5 N 0.5866(5) 0.1963(3) 0.2070(3) 0.132(2) Uiso 1 1 d . . . N31 N 0.10082(17) 0.07521(10) 0.26545(10) 0.0257(4) Uani 1 1 d . . . N40 N 0.15407(17) 0.08110(9) 0.40058(10) 0.0251(4) Uani 1 1 d . . . N41 N 0.30838(17) 0.27155(10) 0.54955(11) 0.0293(4) Uani 1 1 d . . . N50 N 0.49171(17) 0.26226(10) 0.52230(12) 0.0291(4) Uani 1 1 d . . . C1 C 0.6098(5) 0.1980(3) 0.3356(3) 0.0987(17) Uiso 1 1 d . . . H1A H 0.5824 0.1589 0.3483 0.118 Uiso 1 1 calc R . . H1B H 0.5685 0.2328 0.3457 0.118 Uiso 1 1 calc R . . H1C H 0.6871 0.2027 0.3624 0.118 Uiso 1 1 calc R . . C2 C 0.5974(4) 0.1974(2) 0.2636(3) 0.0795(13) Uiso 1 1 d . . . C5 C 0.2647(2) 0.20370(12) 0.31782(13) 0.0271(5) Uani 1 1 d . . . C6 C 0.2790(3) 0.17329(14) 0.25577(16) 0.0405(7) Uani 1 1 d . . . H6A H 0.2089 0.1723 0.2185 0.049 Uiso 1 1 calc R . . H6B H 0.3054 0.1307 0.2674 0.049 Uiso 1 1 calc R . . H6C H 0.3320 0.1968 0.2405 0.049 Uiso 1 1 calc R . . C11 C -0.1287(2) 0.11390(12) 0.28050(13) 0.0273(5) Uani 1 1 d . . . C12 C -0.1023(2) 0.11727(12) 0.35378(13) 0.0267(5) Uani 1 1 d . . . C13 C -0.0643(2) 0.17959(12) 0.37513(13) 0.0260(5) Uani 1 1 d . . . C14 C -0.0706(2) 0.21448(12) 0.31417(13) 0.0272(5) Uani 1 1 d . . . C15 C -0.1086(2) 0.17429(12) 0.25566(13) 0.0277(5) Uani 1 1 d . . . C16 C -0.1756(2) 0.05874(14) 0.23661(15) 0.0375(6) Uani 1 1 d . . . H16A H -0.1603 0.0617 0.1926 0.045 Uiso 1 1 calc R . . H16B H -0.2546 0.0576 0.2275 0.045 Uiso 1 1 calc R . . H16C H -0.1427 0.0207 0.2609 0.045 Uiso 1 1 calc R . . C17 C -0.1145(2) 0.06621(13) 0.40061(15) 0.0363(6) Uani 1 1 d . . . H17A H -0.0570 0.0699 0.4455 0.044 Uiso 1 1 calc R . . H17B H -0.1083 0.0259 0.3798 0.044 Uiso 1 1 calc R . . H17C H -0.1860 0.0694 0.4072 0.044 Uiso 1 1 calc R . . C18 C -0.0369(2) 0.20582(14) 0.44679(13) 0.0345(6) Uani 1 1 d . . . H18A H -0.0199 0.1718 0.4806 0.041 Uiso 1 1 calc R . . H18B H -0.0993 0.2294 0.4509 0.041 Uiso 1 1 calc R . . H18C H 0.0264 0.2334 0.4558 0.041 Uiso 1 1 calc R . . C19 C -0.0430(3) 0.28154(13) 0.31190(16) 0.0395(6) Uani 1 1 d . . . H19A H 0.0123 0.2932 0.3555 0.047 Uiso 1 1 calc R . . H19B H -0.1087 0.3067 0.3053 0.047 Uiso 1 1 calc R . . H19C H -0.0146 0.2888 0.2734 0.047 Uiso 1 1 calc R . . C20 C -0.1370(3) 0.19469(15) 0.18209(14) 0.0409(7) Uani 1 1 d . . . H20A H -0.1427 0.1583 0.1523 0.049 Uiso 1 1 calc R . . H20B H -0.0801 0.2225 0.1771 0.049 Uiso 1 1 calc R . . H20C H -0.2069 0.2167 0.1686 0.049 Uiso 1 1 calc R . . C21 C 0.4565(2) 0.41116(11) 0.51380(15) 0.0320(6) Uani 1 1 d . . . C22 C 0.3569(2) 0.41631(12) 0.52883(15) 0.0344(6) Uani 1 1 d . . . C23 C 0.2685(2) 0.41068(12) 0.46443(16) 0.0339(6) Uani 1 1 d . . . C24 C 0.3149(2) 0.40319(12) 0.41032(15) 0.0332(6) Uani 1 1 d . . . C25 C 0.4312(2) 0.40184(12) 0.44020(15) 0.0315(5) Uani 1 1 d . . . C26 C 0.5690(2) 0.41622(14) 0.56494(18) 0.0453(7) Uani 1 1 d . . . H26A H 0.6187 0.3892 0.5505 0.054 Uiso 1 1 calc R . . H26B H 0.5677 0.4035 0.6108 0.054 Uiso 1 1 calc R . . H26C H 0.5941 0.4593 0.5669 0.054 Uiso 1 1 calc R . . C27 C 0.3455(3) 0.42681(16) 0.59857(18) 0.0518(8) Uani 1 1 d . . . H27A H 0.2822 0.4038 0.6021 0.062 Uiso 1 1 calc R . . H27B H 0.3354 0.4713 0.6050 0.062 Uiso 1 1 calc R . . H27C H 0.4114 0.4123 0.6344 0.062 Uiso 1 1 calc R . . C28 C 0.1502(2) 0.41921(15) 0.4551(2) 0.0506(8) Uani 1 1 d . . . H28A H 0.1374 0.4123 0.4994 0.061 Uiso 1 1 calc R . . H28B H 0.1073 0.3894 0.4209 0.061 Uiso 1 1 calc R . . H28C H 0.1281 0.4616 0.4390 0.061 Uiso 1 1 calc R . . C29 C 0.2541(3) 0.39775(16) 0.33510(17) 0.0517(8) Uani 1 1 d . . . H29A H 0.2898 0.3670 0.3142 0.062 Uiso 1 1 calc R . . H29B H 0.2532 0.4381 0.3127 0.062 Uiso 1 1 calc R . . H29C H 0.1791 0.3845 0.3288 0.062 Uiso 1 1 calc R . . C30 C 0.5090(3) 0.39845(17) 0.39997(19) 0.0508(8) Uani 1 1 d . . . H30A H 0.5823 0.3894 0.4314 0.061 Uiso 1 1 calc R . . H30B H 0.5096 0.4383 0.3768 0.061 Uiso 1 1 calc R . . H30C H 0.4862 0.3654 0.3652 0.061 Uiso 1 1 calc R . . C31 C 0.0630(2) 0.07140(13) 0.19587(13) 0.0312(5) Uani 1 1 d . . . H31 H 0.0089 0.1001 0.1710 0.037 Uiso 1 1 calc R . . C32 C 0.0996(2) 0.02734(14) 0.15931(14) 0.0369(6) Uani 1 1 d . . . H32 H 0.0706 0.0254 0.1103 0.044 Uiso 1 1 calc R . . C33 C 0.1794(2) -0.01389(14) 0.19549(16) 0.0396(6) Uani 1 1 d . . . H33 H 0.2060 -0.0447 0.1716 0.047 Uiso 1 1 calc R . . C34 C 0.2201(2) -0.00990(13) 0.26658(15) 0.0343(6) Uani 1 1 d . . . H34 H 0.2755 -0.0376 0.2921 0.041 Uiso 1 1 calc R . . C35 C 0.1793(2) 0.03500(11) 0.30065(13) 0.0262(5) Uani 1 1 d . . . C36 C 0.2149(2) 0.04165(11) 0.37632(13) 0.0264(5) Uani 1 1 d . . . C37 C 0.3028(2) 0.01022(13) 0.42071(15) 0.0368(6) Uani 1 1 d . . . H37 H 0.3469 -0.0157 0.4029 0.044 Uiso 1 1 calc R . . C38 C 0.3256(3) 0.01697(15) 0.49138(16) 0.0429(7) Uani 1 1 d . . . H38 H 0.3853 -0.0045 0.5227 0.052 Uiso 1 1 calc R . . C39 C 0.2608(3) 0.05529(14) 0.51584(14) 0.0393(6) Uani 1 1 d . . . H39 H 0.2736 0.0594 0.5642 0.047 Uiso 1 1 calc R . . C40 C 0.1770(2) 0.08756(13) 0.46914(13) 0.0332(6) Uani 1 1 d . . . H40 H 0.1344 0.1152 0.4861 0.040 Uiso 1 1 calc R . . C41 C 0.2112(2) 0.27807(14) 0.55931(14) 0.0364(6) Uani 1 1 d . . . H41 H 0.1638 0.3102 0.5353 0.044 Uiso 1 1 calc R . . C42 C 0.1778(3) 0.23976(17) 0.60296(16) 0.0454(8) Uani 1 1 d . . . H42 H 0.1080 0.2450 0.6082 0.054 Uiso 1 1 calc R . . C43 C 0.2472(3) 0.19370(18) 0.63879(16) 0.0508(9) Uani 1 1 d . . . H43 H 0.2265 0.1673 0.6698 0.061 Uiso 1 1 calc R . . C44 C 0.3467(3) 0.18659(16) 0.62902(17) 0.0468(8) Uani 1 1 d . . . H44 H 0.3957 0.1553 0.6534 0.056 Uiso 1 1 calc R . . C45 C 0.3749(2) 0.22561(13) 0.58312(14) 0.0334(6) Uani 1 1 d . . . C46 C 0.4776(2) 0.21957(13) 0.56685(15) 0.0352(6) Uani 1 1 d . . . C47 C 0.5545(3) 0.17355(16) 0.5933(2) 0.0564(9) Uani 1 1 d . . . H47 H 0.5420 0.1428 0.6233 0.068 Uiso 1 1 calc R . . C48 C 0.6490(3) 0.17252(17) 0.5761(2) 0.0623(11) Uani 1 1 d . . . H48 H 0.7030 0.1417 0.5948 0.075 Uiso 1 1 calc R . . C49 C 0.6638(3) 0.21645(15) 0.5317(2) 0.0513(8) Uani 1 1 d . . . H49 H 0.7286 0.2169 0.5194 0.062 Uiso 1 1 calc R . . C50 C 0.5836(2) 0.26035(13) 0.50486(16) 0.0375(6) Uani 1 1 d . . . H50 H 0.5935 0.2902 0.4731 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02121(9) 0.02277(9) 0.01810(9) -0.00249(7) 0.00522(7) -0.00238(7) Rh2 0.01703(9) 0.02198(9) 0.02681(10) -0.00170(7) 0.00553(7) -0.00251(6) P1 0.0272(3) 0.0366(4) 0.0321(3) 0.0069(3) 0.0119(3) 0.0002(3) P2 0.0316(3) 0.0329(3) 0.0310(3) 0.0020(3) 0.0125(3) -0.0018(3) P3 0.0304(4) 0.0585(5) 0.0432(4) 0.0201(4) 0.0108(3) 0.0065(3) F11 0.0638(15) 0.0630(14) 0.119(2) 0.0208(14) 0.0267(15) -0.0267(12) F12 0.0527(12) 0.0719(14) 0.0656(13) 0.0247(11) 0.0146(10) 0.0266(11) F13 0.108(2) 0.0628(14) 0.0527(12) -0.0140(10) 0.0417(13) -0.0023(13) F14 0.0420(11) 0.0851(16) 0.0653(13) 0.0347(12) 0.0056(10) 0.0122(11) F15 0.0886(17) 0.0767(15) 0.0557(12) 0.0168(11) 0.0482(12) 0.0271(13) F16 0.0497(11) 0.0441(10) 0.0791(14) -0.0028(10) 0.0318(11) -0.0110(8) F21 0.0561(14) 0.119(2) 0.0594(13) -0.0357(14) 0.0186(11) -0.0353(14) F22 0.0803(16) 0.0476(11) 0.0879(16) 0.0234(11) 0.0524(14) 0.0166(10) F23 0.0420(10) 0.0645(12) 0.0460(10) 0.0060(9) 0.0256(8) -0.0002(9) F24 0.0935(19) 0.0575(14) 0.142(2) 0.0489(15) 0.0788(19) 0.0305(13) F25 0.0477(10) 0.0493(10) 0.0503(10) -0.0059(8) 0.0286(9) -0.0013(8) F26 0.0448(12) 0.147(2) 0.0392(11) -0.0233(13) 0.0144(9) -0.0261(14) F31 0.0759(17) 0.120(2) 0.0769(17) -0.0337(16) 0.0411(14) -0.0273(16) F32 0.0522(13) 0.0700(15) 0.113(2) 0.0253(14) 0.0216(14) 0.0175(11) F33 0.0662(14) 0.0872(16) 0.0531(12) 0.0259(11) 0.0321(11) 0.0116(12) F34 0.094(2) 0.126(2) 0.118(2) 0.069(2) 0.0709(19) 0.0690(19) F35 0.0480(13) 0.135(2) 0.0741(15) 0.0618(16) 0.0193(11) 0.0056(14) F36 0.0541(15) 0.135(3) 0.104(2) -0.003(2) -0.0013(15) -0.0304(17) N1 0.0264(10) 0.0260(10) 0.0241(10) -0.0044(8) 0.0084(8) -0.0049(8) N2 0.0253(10) 0.0295(11) 0.0280(10) -0.0078(9) 0.0094(8) -0.0065(8) N3 0.0219(10) 0.0254(10) 0.0280(10) -0.0009(8) 0.0087(8) -0.0033(8) N4 0.0318(11) 0.0317(11) 0.0335(11) -0.0023(9) 0.0158(9) -0.0043(9) N31 0.0246(10) 0.0289(10) 0.0242(10) -0.0051(8) 0.0088(8) -0.0053(8) N40 0.0246(10) 0.0262(10) 0.0234(9) 0.0001(8) 0.0059(8) -0.0021(8) N41 0.0265(11) 0.0338(11) 0.0270(10) -0.0051(9) 0.0076(9) -0.0090(9) N50 0.0220(10) 0.0258(10) 0.0363(11) 0.0007(9) 0.0049(9) -0.0018(8) C5 0.0310(13) 0.0263(12) 0.0262(12) 0.0022(10) 0.0121(10) -0.0007(10) C6 0.0489(18) 0.0439(16) 0.0372(15) -0.0055(13) 0.0255(14) -0.0092(13) C11 0.0198(11) 0.0307(12) 0.0306(12) -0.0046(10) 0.0068(9) -0.0003(9) C12 0.0209(11) 0.0295(12) 0.0304(12) -0.0008(10) 0.0091(10) -0.0013(9) C13 0.0243(12) 0.0297(12) 0.0247(11) -0.0020(10) 0.0086(9) 0.0003(9) C14 0.0274(12) 0.0286(12) 0.0256(11) -0.0002(10) 0.0085(10) 0.0053(10) C15 0.0257(12) 0.0303(12) 0.0244(12) -0.0007(10) 0.0042(9) 0.0042(10) C16 0.0280(13) 0.0405(15) 0.0390(15) -0.0114(12) 0.0037(11) -0.0074(11) C17 0.0342(14) 0.0362(14) 0.0422(15) 0.0060(12) 0.0172(12) -0.0044(11) C18 0.0394(15) 0.0405(15) 0.0247(12) -0.0029(11) 0.0119(11) 0.0030(12) C19 0.0544(18) 0.0276(13) 0.0382(15) 0.0013(11) 0.0171(13) 0.0019(12) C20 0.0493(18) 0.0453(16) 0.0251(13) 0.0031(12) 0.0077(12) 0.0123(14) C21 0.0251(12) 0.0207(11) 0.0460(15) -0.0017(11) 0.0057(11) -0.0055(9) C22 0.0318(14) 0.0244(12) 0.0462(16) -0.0081(11) 0.0112(12) -0.0035(10) C23 0.0253(13) 0.0213(12) 0.0520(16) -0.0030(11) 0.0080(12) 0.0000(9) C24 0.0299(13) 0.0220(12) 0.0417(15) 0.0058(11) 0.0029(11) 0.0002(10) C25 0.0283(13) 0.0249(12) 0.0403(14) 0.0064(11) 0.0097(11) -0.0011(10) C26 0.0281(14) 0.0376(15) 0.0592(19) -0.0033(14) -0.0014(13) -0.0101(12) C27 0.058(2) 0.0463(18) 0.055(2) -0.0230(16) 0.0239(17) -0.0065(15) C28 0.0262(15) 0.0386(16) 0.084(3) -0.0067(16) 0.0131(15) 0.0053(12) C29 0.055(2) 0.0437(17) 0.0429(17) 0.0105(14) -0.0039(15) 0.0042(15) C30 0.0455(18) 0.0527(19) 0.064(2) 0.0195(17) 0.0308(17) 0.0031(15) C31 0.0265(12) 0.0410(14) 0.0253(12) -0.0054(11) 0.0074(10) -0.0034(11) C32 0.0344(14) 0.0510(17) 0.0275(13) -0.0135(12) 0.0127(11) -0.0079(12) C33 0.0424(16) 0.0422(16) 0.0419(15) -0.0137(13) 0.0245(13) -0.0033(13) C34 0.0339(14) 0.0334(14) 0.0403(14) -0.0024(12) 0.0185(12) 0.0015(11) C35 0.0238(12) 0.0277(12) 0.0292(12) -0.0014(10) 0.0115(10) -0.0041(9) C36 0.0239(12) 0.0256(12) 0.0297(12) -0.0011(10) 0.0083(10) -0.0033(9) C37 0.0322(14) 0.0371(15) 0.0382(14) 0.0004(12) 0.0073(12) 0.0063(11) C38 0.0380(16) 0.0443(16) 0.0377(15) 0.0055(13) -0.0002(12) 0.0085(13) C39 0.0434(16) 0.0424(16) 0.0262(13) 0.0023(12) 0.0026(12) 0.0014(13) C40 0.0344(14) 0.0372(14) 0.0257(12) -0.0022(11) 0.0064(11) 0.0001(11) C41 0.0294(14) 0.0479(16) 0.0326(13) -0.0104(12) 0.0110(11) -0.0115(12) C42 0.0406(17) 0.064(2) 0.0353(15) -0.0105(14) 0.0174(13) -0.0231(15) C43 0.055(2) 0.064(2) 0.0338(15) 0.0021(15) 0.0146(14) -0.0279(17) C44 0.0501(19) 0.0475(18) 0.0392(16) 0.0090(14) 0.0093(14) -0.0138(14) C45 0.0327(14) 0.0315(13) 0.0323(13) 0.0009(11) 0.0053(11) -0.0091(11) C46 0.0301(14) 0.0307(13) 0.0401(15) 0.0041(11) 0.0047(11) -0.0050(11) C47 0.047(2) 0.0410(18) 0.075(2) 0.0239(17) 0.0108(18) 0.0040(14) C48 0.0379(18) 0.0451(19) 0.097(3) 0.0218(19) 0.0111(19) 0.0140(15) C49 0.0269(15) 0.0441(17) 0.081(2) 0.0076(17) 0.0143(15) 0.0070(13) C50 0.0266(13) 0.0339(14) 0.0523(17) 0.0034(13) 0.0130(12) 0.0023(11) _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 Rh1 N31 2.104(2) . ? Rh1 N40 2.110(2) . ? Rh1 N1 2.138(2) . ? Rh1 C13 2.159(2) . ? Rh1 C11 2.160(2) . ? Rh1 C12 2.165(2) . ? Rh1 C15 2.171(2) . ? Rh1 C14 2.184(2) . ? Rh2 N3 2.092(2) . ? Rh2 N41 2.096(2) . ? Rh2 N50 2.104(2) . ? Rh2 C25 2.152(3) . ? Rh2 C23 2.161(3) . ? Rh2 C21 2.162(2) . ? Rh2 C22 2.166(3) . ? Rh2 C24 2.174(3) . ? P1 F13 1.575(2) . ? P1 F11 1.578(2) . ? P1 F14 1.590(2) . ? P1 F12 1.591(2) . ? P1 F16 1.5915(19) . ? P1 F15 1.601(2) . ? P2 F24 1.578(2) . ? P2 F26 1.581(2) . ? P2 F21 1.584(2) . ? P2 F22 1.589(2) . ? P2 F23 1.5968(18) . ? P2 F25 1.6009(18) . ? P3 F34 1.571(2) . ? P3 F36 1.571(3) . ? P3 F32 1.581(2) . ? P3 F31 1.584(3) . ? P3 F33 1.595(2) . ? P3 F35 1.596(2) . ? N1 N2 1.343(3) . ? N1 C5 1.347(3) . ? N2 N3 1.305(3) . ? N3 N4 1.341(3) . ? N4 C5 1.334(3) . ? N5 C2 1.118(7) . ? N31 C31 1.347(3) . ? N31 C35 1.353(3) . ? N40 C40 1.340(3) . ? N40 C36 1.355(3) . ? N41 C41 1.343(3) . ? N41 C45 1.345(4) . ? N50 C46 1.345(4) . ? N50 C50 1.347(3) . ? C1 C2 1.425(7) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C5 C6 1.488(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C12 1.424(4) . ? C11 C15 1.448(4) . ? C11 C16 1.494(4) . ? C12 C13 1.447(3) . ? C12 C17 1.497(4) . ? C13 C14 1.432(3) . ? C13 C18 1.499(3) . ? C14 C15 1.428(3) . ? C14 C19 1.491(4) . ? C15 C20 1.492(4) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.422(4) . ? C21 C25 1.444(4) . ? C21 C26 1.500(4) . ? C22 C23 1.445(4) . ? C22 C27 1.493(4) . ? C23 C24 1.424(4) . ? C23 C28 1.494(4) . ? C24 C25 1.433(4) . ? C24 C29 1.488(4) . ? C25 C30 1.490(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.381(4) . ? C31 H31 0.9500 . ? C32 C33 1.383(4) . ? C32 H32 0.9500 . ? C33 C34 1.377(4) . ? C33 H33 0.9500 . ? C34 C35 1.389(4) . ? C34 H34 0.9500 . ? C35 C36 1.469(3) . ? C36 C37 1.382(4) . ? C37 C38 1.383(4) . ? C37 H37 0.9500 . ? C38 C39 1.379(4) . ? C38 H38 0.9500 . ? C39 C40 1.380(4) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.381(4) . ? C41 H41 0.9500 . ? C42 C43 1.380(5) . ? C42 H42 0.9500 . ? C43 C44 1.374(5) . ? C43 H43 0.9500 . ? C44 C45 1.391(4) . ? C44 H44 0.9500 . ? C45 C46 1.476(4) . ? C46 C47 1.386(4) . ? C47 C48 1.378(5) . ? C47 H47 0.9500 . ? C48 C49 1.364(5) . ? C48 H48 0.9500 . ? C49 C50 1.381(4) . ? C49 H49 0.9500 . ? C50 H50 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 N31 Rh1 N40 76.89(8) . . ? N31 Rh1 N1 91.33(8) . . ? N40 Rh1 N1 81.90(8) . . ? N31 Rh1 C13 161.01(9) . . ? N40 Rh1 C13 107.26(9) . . ? N1 Rh1 C13 107.53(9) . . ? N31 Rh1 C11 97.00(9) . . ? N40 Rh1 C11 123.54(9) . . ? N1 Rh1 C11 154.41(9) . . ? C13 Rh1 C11 65.00(9) . . ? N31 Rh1 C12 122.56(9) . . ? N40 Rh1 C12 98.64(9) . . ? N1 Rh1 C12 145.52(9) . . ? C13 Rh1 C12 39.10(9) . . ? C11 Rh1 C12 38.45(9) . . ? N31 Rh1 C15 105.60(9) . . ? N40 Rh1 C15 162.22(9) . . ? N1 Rh1 C15 115.35(9) . . ? C13 Rh1 C15 64.79(9) . . ? C11 Rh1 C15 39.07(10) . . ? C12 Rh1 C15 64.90(10) . . ? N31 Rh1 C14 140.71(9) . . ? N40 Rh1 C14 142.40(9) . . ? N1 Rh1 C14 93.93(9) . . ? C13 Rh1 C14 38.50(9) . . ? C11 Rh1 C14 64.64(10) . . ? C12 Rh1 C14 64.69(10) . . ? C15 Rh1 C14 38.28(9) . . ? N3 Rh2 N41 86.28(8) . . ? N3 Rh2 N50 85.98(8) . . ? N41 Rh2 N50 76.95(9) . . ? N3 Rh2 C25 110.82(9) . . ? N41 Rh2 C25 162.65(10) . . ? N50 Rh2 C25 106.30(9) . . ? N3 Rh2 C23 111.28(9) . . ? N41 Rh2 C23 106.73(10) . . ? N50 Rh2 C23 162.38(9) . . ? C25 Rh2 C23 65.10(10) . . ? N3 Rh2 C21 149.70(10) . . ? N41 Rh2 C21 123.99(10) . . ? N50 Rh2 C21 98.57(9) . . ? C25 Rh2 C21 39.10(11) . . ? C23 Rh2 C21 64.82(10) . . ? N3 Rh2 C22 150.07(10) . . ? N41 Rh2 C22 98.65(10) . . ? N50 Rh2 C22 123.93(10) . . ? C25 Rh2 C22 65.12(11) . . ? C23 Rh2 C22 39.00(11) . . ? C21 Rh2 C22 38.36(10) . . ? N3 Rh2 C24 93.37(9) . . ? N41 Rh2 C24 141.51(10) . . ? N50 Rh2 C24 141.49(10) . . ? C25 Rh2 C24 38.68(10) . . ? C23 Rh2 C24 38.36(11) . . ? C21 Rh2 C24 64.58(10) . . ? C22 Rh2 C24 64.57(11) . . ? F13 P1 F11 92.21(15) . . ? F13 P1 F14 91.85(14) . . ? F11 P1 F14 91.55(14) . . ? F13 P1 F12 89.36(14) . . ? F11 P1 F12 89.82(14) . . ? F14 P1 F12 178.13(15) . . ? F13 P1 F16 88.93(12) . . ? F11 P1 F16 178.77(15) . . ? F14 P1 F16 87.96(12) . . ? F12 P1 F16 90.65(13) . . ? F13 P1 F15 177.80(15) . . ? F11 P1 F15 89.77(15) . . ? F14 P1 F15 89.05(13) . . ? F12 P1 F15 89.68(12) . . ? F16 P1 F15 89.10(13) . . ? F24 P2 F26 91.49(18) . . ? F24 P2 F21 90.43(17) . . ? F26 P2 F21 177.99(17) . . ? F24 P2 F22 179.26(14) . . ? F26 P2 F22 89.03(16) . . ? F21 P2 F22 89.04(16) . . ? F24 P2 F23 89.43(12) . . ? F26 P2 F23 90.15(11) . . ? F21 P2 F23 89.28(12) . . ? F22 P2 F23 90.03(11) . . ? F24 P2 F25 90.89(12) . . ? F26 P2 F25 90.07(11) . . ? F21 P2 F25 90.50(11) . . ? F22 P2 F25 89.64(11) . . ? F23 P2 F25 179.61(12) . . ? F34 P3 F36 88.5(2) . . ? F34 P3 F32 179.0(2) . . ? F36 P3 F32 90.51(17) . . ? F34 P3 F31 92.53(19) . . ? F36 P3 F31 178.98(19) . . ? F32 P3 F31 88.49(16) . . ? F34 P3 F33 90.09(13) . . ? F36 P3 F33 90.73(16) . . ? F32 P3 F33 89.99(14) . . ? F31 P3 F33 89.08(14) . . ? F34 P3 F35 88.02(14) . . ? F36 P3 F35 92.15(17) . . ? F32 P3 F35 91.94(15) . . ? F31 P3 F35 88.07(15) . . ? F33 P3 F35 176.52(17) . . ? N2 N1 C5 106.7(2) . . ? N2 N1 Rh1 114.30(15) . . ? C5 N1 Rh1 138.69(17) . . ? N3 N2 N1 106.92(19) . . ? N2 N3 N4 112.0(2) . . ? N2 N3 Rh2 124.52(16) . . ? N4 N3 Rh2 123.34(16) . . ? C5 N4 N3 104.2(2) . . ? C31 N31 C35 118.6(2) . . ? C31 N31 Rh1 125.03(18) . . ? C35 N31 Rh1 116.33(16) . . ? C40 N40 C36 119.0(2) . . ? C40 N40 Rh1 124.68(18) . . ? C36 N40 Rh1 115.82(16) . . ? C41 N41 C45 118.6(2) . . ? C41 N41 Rh2 124.8(2) . . ? C45 N41 Rh2 116.52(18) . . ? C46 N50 C50 118.7(2) . . ? C46 N50 Rh2 116.50(18) . . ? C50 N50 Rh2 124.78(19) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N5 C2 C1 179.1(7) . . ? N4 C5 N1 110.2(2) . . ? N4 C5 C6 122.9(2) . . ? N1 C5 C6 126.9(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C11 C15 108.2(2) . . ? C12 C11 C16 125.7(2) . . ? C15 C11 C16 126.0(2) . . ? C12 C11 Rh1 70.96(14) . . ? C15 C11 Rh1 70.86(14) . . ? C16 C11 Rh1 126.84(18) . . ? C11 C12 C13 107.9(2) . . ? C11 C12 C17 126.4(2) . . ? C13 C12 C17 125.7(2) . . ? C11 C12 Rh1 70.60(14) . . ? C13 C12 Rh1 70.25(14) . . ? C17 C12 Rh1 125.92(18) . . ? C14 C13 C12 107.8(2) . . ? C14 C13 C18 125.3(2) . . ? C12 C13 C18 126.4(2) . . ? C14 C13 Rh1 71.67(14) . . ? C12 C13 Rh1 70.65(14) . . ? C18 C13 Rh1 129.04(18) . . ? C15 C14 C13 108.4(2) . . ? C15 C14 C19 125.6(2) . . ? C13 C14 C19 125.9(2) . . ? C15 C14 Rh1 70.37(14) . . ? C13 C14 Rh1 69.83(14) . . ? C19 C14 Rh1 126.02(19) . . ? C14 C15 C11 107.7(2) . . ? C14 C15 C20 124.8(2) . . ? C11 C15 C20 127.0(2) . . ? C14 C15 Rh1 71.36(14) . . ? C11 C15 Rh1 70.07(14) . . ? C20 C15 Rh1 130.6(2) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 108.4(2) . . ? C22 C21 C26 126.2(3) . . ? C25 C21 C26 125.4(3) . . ? C22 C21 Rh2 70.97(14) . . ? C25 C21 Rh2 70.08(14) . . ? C26 C21 Rh2 125.98(19) . . ? C21 C22 C23 107.9(3) . . ? C21 C22 C27 126.1(3) . . ? C23 C22 C27 126.0(3) . . ? C21 C22 Rh2 70.67(15) . . ? C23 C22 Rh2 70.32(15) . . ? C27 C22 Rh2 125.4(2) . . ? C24 C23 C22 107.8(2) . . ? C24 C23 C28 125.9(3) . . ? C22 C23 C28 125.9(3) . . ? C24 C23 Rh2 71.28(15) . . ? C22 C23 Rh2 70.68(15) . . ? C28 C23 Rh2 129.3(2) . . ? C23 C24 C25 108.6(2) . . ? C23 C24 C29 126.3(3) . . ? C25 C24 C29 125.1(3) . . ? C23 C24 Rh2 70.36(15) . . ? C25 C24 Rh2 69.86(14) . . ? C29 C24 Rh2 125.8(2) . . ? C24 C25 C21 107.3(2) . . ? C24 C25 C30 124.8(3) . . ? C21 C25 C30 127.6(3) . . ? C24 C25 Rh2 71.46(15) . . ? C21 C25 Rh2 70.82(14) . . ? C30 C25 Rh2 128.1(2) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N31 C31 C32 122.6(3) . . ? N31 C31 H31 118.7 . . ? C32 C31 H31 118.7 . . ? C31 C32 C33 118.7(3) . . ? C31 C32 H32 120.7 . . ? C33 C32 H32 120.7 . . ? C34 C33 C32 119.3(3) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 119.4(3) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? N31 C35 C34 121.4(2) . . ? N31 C35 C36 115.1(2) . . ? C34 C35 C36 123.4(2) . . ? N40 C36 C37 121.4(2) . . ? N40 C36 C35 114.9(2) . . ? C37 C36 C35 123.8(2) . . ? C36 C37 C38 119.2(3) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 119.2(3) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 119.1(3) . . ? C38 C39 H39 120.4 . . ? C40 C39 H39 120.4 . . ? N40 C40 C39 122.1(3) . . ? N40 C40 H40 119.0 . . ? C39 C40 H40 119.0 . . ? N41 C41 C42 122.4(3) . . ? N41 C41 H41 118.8 . . ? C42 C41 H41 118.8 . . ? C43 C42 C41 119.0(3) . . ? C43 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? C44 C43 C42 119.0(3) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C43 C44 C45 119.4(3) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? N41 C45 C44 121.5(3) . . ? N41 C45 C46 115.2(2) . . ? C44 C45 C46 123.2(3) . . ? N50 C46 C47 121.0(3) . . ? N50 C46 C45 114.8(2) . . ? C47 C46 C45 124.2(3) . . ? C48 C47 C46 119.9(3) . . ? C48 C47 H47 120.0 . . ? C46 C47 H47 120.0 . . ? C49 C48 C47 118.9(3) . . ? C49 C48 H48 120.6 . . ? C47 C48 H48 120.6 . . ? C48 C49 C50 119.3(3) . . ? C48 C49 H49 120.3 . . ? C50 C49 H49 120.3 . . ? N50 C50 C49 122.1(3) . . ? N50 C50 H50 118.9 . . ? C49 C50 H50 118.9 . . ? 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 N31 Rh1 N1 N2 -157.23(17) . . . . ? N40 Rh1 N1 N2 -80.67(17) . . . . ? C13 Rh1 N1 N2 24.95(19) . . . . ? C11 Rh1 N1 N2 93.5(2) . . . . ? C12 Rh1 N1 N2 12.8(3) . . . . ? C15 Rh1 N1 N2 94.79(18) . . . . ? C14 Rh1 N1 N2 61.74(18) . . . . ? N31 Rh1 N1 C5 15.2(3) . . . . ? N40 Rh1 N1 C5 91.8(3) . . . . ? C13 Rh1 N1 C5 -162.6(3) . . . . ? C11 Rh1 N1 C5 -94.1(3) . . . . ? C12 Rh1 N1 C5 -174.8(2) . . . . ? C15 Rh1 N1 C5 -92.8(3) . . . . ? C14 Rh1 N1 C5 -125.8(3) . . . . ? C5 N1 N2 N3 0.3(3) . . . . ? Rh1 N1 N2 N3 175.13(15) . . . . ? N1 N2 N3 N4 -0.1(3) . . . . ? N1 N2 N3 Rh2 175.69(15) . . . . ? N41 Rh2 N3 N2 37.6(2) . . . . ? N50 Rh2 N3 N2 114.7(2) . . . . ? C25 Rh2 N3 N2 -139.36(19) . . . . ? C23 Rh2 N3 N2 -69.0(2) . . . . ? C21 Rh2 N3 N2 -145.2(2) . . . . ? C22 Rh2 N3 N2 -63.3(3) . . . . ? C24 Rh2 N3 N2 -103.9(2) . . . . ? N41 Rh2 N3 N4 -147.2(2) . . . . ? N50 Rh2 N3 N4 -70.0(2) . . . . ? C25 Rh2 N3 N4 35.9(2) . . . . ? C23 Rh2 N3 N4 106.3(2) . . . . ? C21 Rh2 N3 N4 30.1(3) . . . . ? C22 Rh2 N3 N4 111.9(2) . . . . ? C24 Rh2 N3 N4 71.4(2) . . . . ? N2 N3 N4 C5 -0.3(3) . . . . ? Rh2 N3 N4 C5 -176.05(16) . . . . ? N40 Rh1 N31 C31 174.1(2) . . . . ? N1 Rh1 N31 C31 -104.6(2) . . . . ? C13 Rh1 N31 C31 69.0(4) . . . . ? C11 Rh1 N31 C31 51.2(2) . . . . ? C12 Rh1 N31 C31 82.1(2) . . . . ? C15 Rh1 N31 C31 12.2(2) . . . . ? C14 Rh1 N31 C31 -6.7(3) . . . . ? N40 Rh1 N31 C35 -2.82(17) . . . . ? N1 Rh1 N31 C35 78.55(17) . . . . ? C13 Rh1 N31 C35 -107.9(3) . . . . ? C11 Rh1 N31 C35 -125.70(18) . . . . ? C12 Rh1 N31 C35 -94.78(19) . . . . ? C15 Rh1 N31 C35 -164.64(17) . . . . ? C14 Rh1 N31 C35 176.41(16) . . . . ? N31 Rh1 N40 C40 179.6(2) . . . . ? N1 Rh1 N40 C40 86.3(2) . . . . ? C13 Rh1 N40 C40 -19.6(2) . . . . ? C11 Rh1 N40 C40 -90.7(2) . . . . ? C12 Rh1 N40 C40 -58.9(2) . . . . ? C15 Rh1 N40 C40 -80.2(4) . . . . ? C14 Rh1 N40 C40 0.4(3) . . . . ? N31 Rh1 N40 C36 7.70(17) . . . . ? N1 Rh1 N40 C36 -85.58(17) . . . . ? C13 Rh1 N40 C36 168.49(17) . . . . ? C11 Rh1 N40 C36 97.45(18) . . . . ? C12 Rh1 N40 C36 129.28(17) . . . . ? C15 Rh1 N40 C36 108.0(3) . . . . ? C14 Rh1 N40 C36 -171.49(17) . . . . ? N3 Rh2 N41 C41 -91.2(2) . . . . ? N50 Rh2 N41 C41 -177.9(2) . . . . ? C25 Rh2 N41 C41 79.1(4) . . . . ? C23 Rh2 N41 C41 20.0(2) . . . . ? C21 Rh2 N41 C41 90.5(2) . . . . ? C22 Rh2 N41 C41 59.1(2) . . . . ? C24 Rh2 N41 C41 -0.4(3) . . . . ? N3 Rh2 N41 C45 86.92(19) . . . . ? N50 Rh2 N41 C45 0.20(18) . . . . ? C25 Rh2 N41 C45 -102.8(3) . . . . ? C23 Rh2 N41 C45 -161.96(19) . . . . ? C21 Rh2 N41 C45 -91.4(2) . . . . ? C22 Rh2 N41 C45 -122.78(19) . . . . ? C24 Rh2 N41 C45 177.66(18) . . . . ? N3 Rh2 N50 C46 -86.1(2) . . . . ? N41 Rh2 N50 C46 0.97(19) . . . . ? C25 Rh2 N50 C46 163.34(19) . . . . ? C23 Rh2 N50 C46 105.2(4) . . . . ? C21 Rh2 N50 C46 124.0(2) . . . . ? C22 Rh2 N50 C46 92.7(2) . . . . ? C24 Rh2 N50 C46 -176.49(19) . . . . ? N3 Rh2 N50 C50 92.2(2) . . . . ? N41 Rh2 N50 C50 179.3(2) . . . . ? C25 Rh2 N50 C50 -18.3(2) . . . . ? C23 Rh2 N50 C50 -76.4(4) . . . . ? C21 Rh2 N50 C50 -57.6(2) . . . . ? C22 Rh2 N50 C50 -89.0(2) . . . . ? C24 Rh2 N50 C50 1.8(3) . . . . ? N3 N4 C5 N1 0.5(3) . . . . ? N3 N4 C5 C6 -178.9(2) . . . . ? N2 N1 C5 N4 -0.5(3) . . . . ? Rh1 N1 C5 N4 -173.32(19) . . . . ? N2 N1 C5 C6 178.8(3) . . . . ? Rh1 N1 C5 C6 6.0(4) . . . . ? N31 Rh1 C11 C12 135.85(15) . . . . ? N40 Rh1 C11 C12 56.97(17) . . . . ? N1 Rh1 C11 C12 -116.1(2) . . . . ? C13 Rh1 C11 C12 -37.83(14) . . . . ? C15 Rh1 C11 C12 -118.0(2) . . . . ? C14 Rh1 C11 C12 -80.57(15) . . . . ? N31 Rh1 C11 C15 -106.19(14) . . . . ? N40 Rh1 C11 C15 174.93(13) . . . . ? N1 Rh1 C11 C15 1.9(3) . . . . ? C13 Rh1 C11 C15 80.13(15) . . . . ? C12 Rh1 C11 C15 118.0(2) . . . . ? C14 Rh1 C11 C15 37.40(14) . . . . ? N31 Rh1 C11 C16 15.0(2) . . . . ? N40 Rh1 C11 C16 -63.9(3) . . . . ? N1 Rh1 C11 C16 123.1(3) . . . . ? C13 Rh1 C11 C16 -158.7(3) . . . . ? C12 Rh1 C11 C16 -120.9(3) . . . . ? C15 Rh1 C11 C16 121.2(3) . . . . ? C14 Rh1 C11 C16 158.6(3) . . . . ? C15 C11 C12 C13 -0.8(3) . . . . ? C16 C11 C12 C13 -177.1(2) . . . . ? Rh1 C11 C12 C13 60.66(17) . . . . ? C15 C11 C12 C17 177.7(2) . . . . ? C16 C11 C12 C17 1.3(4) . . . . ? Rh1 C11 C12 C17 -120.9(3) . . . . ? C15 C11 C12 Rh1 -61.42(17) . . . . ? C16 C11 C12 Rh1 122.2(3) . . . . ? N31 Rh1 C12 C11 -55.12(17) . . . . ? N40 Rh1 C12 C11 -135.02(15) . . . . ? N1 Rh1 C12 C11 136.73(16) . . . . ? C13 Rh1 C12 C11 118.2(2) . . . . ? C15 Rh1 C12 C11 37.94(15) . . . . ? C14 Rh1 C12 C11 80.42(16) . . . . ? N31 Rh1 C12 C13 -173.30(13) . . . . ? N40 Rh1 C12 C13 106.80(14) . . . . ? N1 Rh1 C12 C13 18.6(2) . . . . ? C11 Rh1 C12 C13 -118.2(2) . . . . ? C15 Rh1 C12 C13 -80.24(15) . . . . ? C14 Rh1 C12 C13 -37.76(14) . . . . ? N31 Rh1 C12 C17 66.3(2) . . . . ? N40 Rh1 C12 C17 -13.6(2) . . . . ? N1 Rh1 C12 C17 -101.8(2) . . . . ? C13 Rh1 C12 C17 -120.4(3) . . . . ? C11 Rh1 C12 C17 121.4(3) . . . . ? C15 Rh1 C12 C17 159.4(3) . . . . ? C14 Rh1 C12 C17 -158.1(3) . . . . ? C11 C12 C13 C14 1.5(3) . . . . ? C17 C12 C13 C14 -176.9(2) . . . . ? Rh1 C12 C13 C14 62.42(17) . . . . ? C11 C12 C13 C18 174.3(2) . . . . ? C17 C12 C13 C18 -4.2(4) . . . . ? Rh1 C12 C13 C18 -124.8(3) . . . . ? C11 C12 C13 Rh1 -60.88(17) . . . . ? C17 C12 C13 Rh1 120.6(3) . . . . ? N31 Rh1 C13 C14 -99.6(3) . . . . ? N40 Rh1 C13 C14 160.40(14) . . . . ? N1 Rh1 C13 C14 73.65(15) . . . . ? C11 Rh1 C13 C14 -80.03(16) . . . . ? C12 Rh1 C13 C14 -117.2(2) . . . . ? C15 Rh1 C13 C14 -36.69(15) . . . . ? N31 Rh1 C13 C12 17.6(3) . . . . ? N40 Rh1 C13 C12 -82.36(15) . . . . ? N1 Rh1 C13 C12 -169.11(14) . . . . ? C11 Rh1 C13 C12 37.21(14) . . . . ? C15 Rh1 C13 C12 80.56(15) . . . . ? C14 Rh1 C13 C12 117.2(2) . . . . ? N31 Rh1 C13 C18 139.3(3) . . . . ? N40 Rh1 C13 C18 39.4(2) . . . . ? N1 Rh1 C13 C18 -47.4(2) . . . . ? C11 Rh1 C13 C18 158.9(3) . . . . ? C12 Rh1 C13 C18 121.7(3) . . . . ? C15 Rh1 C13 C18 -157.7(3) . . . . ? C14 Rh1 C13 C18 -121.0(3) . . . . ? C12 C13 C14 C15 -1.7(3) . . . . ? C18 C13 C14 C15 -174.6(2) . . . . ? Rh1 C13 C14 C15 60.03(17) . . . . ? C12 C13 C14 C19 177.7(3) . . . . ? C18 C13 C14 C19 4.8(4) . . . . ? Rh1 C13 C14 C19 -120.5(3) . . . . ? C12 C13 C14 Rh1 -61.77(17) . . . . ? C18 C13 C14 Rh1 125.3(3) . . . . ? N31 Rh1 C14 C15 30.3(2) . . . . ? N40 Rh1 C14 C15 -150.91(15) . . . . ? N1 Rh1 C14 C15 127.28(15) . . . . ? C13 Rh1 C14 C15 -119.2(2) . . . . ? C11 Rh1 C14 C15 -38.17(15) . . . . ? C12 Rh1 C14 C15 -80.90(16) . . . . ? N31 Rh1 C14 C13 149.57(14) . . . . ? N40 Rh1 C14 C13 -31.7(2) . . . . ? N1 Rh1 C14 C13 -113.49(15) . . . . ? C11 Rh1 C14 C13 81.07(16) . . . . ? C12 Rh1 C14 C13 38.34(14) . . . . ? C15 Rh1 C14 C13 119.2(2) . . . . ? N31 Rh1 C14 C19 -90.0(3) . . . . ? N40 Rh1 C14 C19 88.7(3) . . . . ? N1 Rh1 C14 C19 6.9(2) . . . . ? C13 Rh1 C14 C19 120.4(3) . . . . ? C11 Rh1 C14 C19 -158.5(3) . . . . ? C12 Rh1 C14 C19 158.7(3) . . . . ? C15 Rh1 C14 C19 -120.4(3) . . . . ? C13 C14 C15 C11 1.3(3) . . . . ? C19 C14 C15 C11 -178.2(3) . . . . ? Rh1 C14 C15 C11 60.96(17) . . . . ? C13 C14 C15 C20 173.3(3) . . . . ? C19 C14 C15 C20 -6.2(4) . . . . ? Rh1 C14 C15 C20 -127.0(3) . . . . ? C13 C14 C15 Rh1 -59.69(17) . . . . ? C19 C14 C15 Rh1 120.8(3) . . . . ? C12 C11 C15 C14 -0.3(3) . . . . ? C16 C11 C15 C14 176.1(2) . . . . ? Rh1 C11 C15 C14 -61.79(17) . . . . ? C12 C11 C15 C20 -172.1(3) . . . . ? C16 C11 C15 C20 4.2(4) . . . . ? Rh1 C11 C15 C20 126.4(3) . . . . ? C12 C11 C15 Rh1 61.48(17) . . . . ? C16 C11 C15 Rh1 -122.2(3) . . . . ? N31 Rh1 C15 C14 -160.60(14) . . . . ? N40 Rh1 C15 C14 103.7(3) . . . . ? N1 Rh1 C15 C14 -61.45(17) . . . . ? C13 Rh1 C15 C14 36.90(15) . . . . ? C11 Rh1 C15 C14 117.6(2) . . . . ? C12 Rh1 C15 C14 80.30(16) . . . . ? N31 Rh1 C15 C11 81.76(15) . . . . ? N40 Rh1 C15 C11 -14.0(4) . . . . ? N1 Rh1 C15 C11 -179.09(13) . . . . ? C13 Rh1 C15 C11 -80.73(15) . . . . ? C12 Rh1 C15 C11 -37.34(14) . . . . ? C14 Rh1 C15 C11 -117.6(2) . . . . ? N31 Rh1 C15 C20 -40.4(3) . . . . ? N40 Rh1 C15 C20 -136.1(3) . . . . ? N1 Rh1 C15 C20 58.8(3) . . . . ? C13 Rh1 C15 C20 157.1(3) . . . . ? C11 Rh1 C15 C20 -122.2(3) . . . . ? C12 Rh1 C15 C20 -159.5(3) . . . . ? C14 Rh1 C15 C20 120.2(3) . . . . ? N3 Rh2 C21 C22 127.3(2) . . . . ? N41 Rh2 C21 C22 -56.0(2) . . . . ? N50 Rh2 C21 C22 -135.98(17) . . . . ? C25 Rh2 C21 C22 118.7(2) . . . . ? C23 Rh2 C21 C22 37.84(17) . . . . ? C24 Rh2 C21 C22 80.46(18) . . . . ? N3 Rh2 C21 C25 8.6(3) . . . . ? N41 Rh2 C21 C25 -174.66(14) . . . . ? N50 Rh2 C21 C25 105.35(15) . . . . ? C23 Rh2 C21 C25 -80.83(17) . . . . ? C22 Rh2 C21 C25 -118.7(2) . . . . ? C24 Rh2 C21 C25 -38.21(15) . . . . ? N3 Rh2 C21 C26 -111.3(3) . . . . ? N41 Rh2 C21 C26 65.5(3) . . . . ? N50 Rh2 C21 C26 -14.5(3) . . . . ? C25 Rh2 C21 C26 -119.9(3) . . . . ? C23 Rh2 C21 C26 159.3(3) . . . . ? C22 Rh2 C21 C26 121.4(3) . . . . ? C24 Rh2 C21 C26 -158.1(3) . . . . ? C25 C21 C22 C23 -0.4(3) . . . . ? C26 C21 C22 C23 178.0(2) . . . . ? Rh2 C21 C22 C23 -60.78(18) . . . . ? C25 C21 C22 C27 -179.4(3) . . . . ? C26 C21 C22 C27 -1.0(4) . . . . ? Rh2 C21 C22 C27 120.2(3) . . . . ? C25 C21 C22 Rh2 60.37(18) . . . . ? C26 C21 C22 Rh2 -121.2(3) . . . . ? N3 Rh2 C22 C21 -126.4(2) . . . . ? N41 Rh2 C22 C21 135.95(16) . . . . ? N50 Rh2 C22 C21 55.9(2) . . . . ? C25 Rh2 C22 C21 -37.59(16) . . . . ? C23 Rh2 C22 C21 -118.1(2) . . . . ? C24 Rh2 C22 C21 -80.50(18) . . . . ? N3 Rh2 C22 C23 -8.3(3) . . . . ? N41 Rh2 C22 C23 -105.96(17) . . . . ? N50 Rh2 C22 C23 174.00(15) . . . . ? C25 Rh2 C22 C23 80.51(18) . . . . ? C21 Rh2 C22 C23 118.1(2) . . . . ? C24 Rh2 C22 C23 37.59(16) . . . . ? N3 Rh2 C22 C27 112.4(3) . . . . ? N41 Rh2 C22 C27 14.8(3) . . . . ? N50 Rh2 C22 C27 -65.2(3) . . . . ? C25 Rh2 C22 C27 -158.7(3) . . . . ? C23 Rh2 C22 C27 120.7(3) . . . . ? C21 Rh2 C22 C27 -121.2(3) . . . . ? C24 Rh2 C22 C27 158.3(3) . . . . ? C21 C22 C23 C24 -1.0(3) . . . . ? C27 C22 C23 C24 178.0(3) . . . . ? Rh2 C22 C23 C24 -61.99(18) . . . . ? C21 C22 C23 C28 -174.0(3) . . . . ? C27 C22 C23 C28 5.0(5) . . . . ? Rh2 C22 C23 C28 125.0(3) . . . . ? C21 C22 C23 Rh2 61.00(18) . . . . ? C27 C22 C23 Rh2 -120.0(3) . . . . ? N3 Rh2 C23 C24 -67.02(16) . . . . ? N41 Rh2 C23 C24 -159.56(15) . . . . ? N50 Rh2 C23 C24 100.8(3) . . . . ? C25 Rh2 C23 C24 36.85(15) . . . . ? C21 Rh2 C23 C24 80.20(17) . . . . ? C22 Rh2 C23 C24 117.4(2) . . . . ? N3 Rh2 C23 C22 175.55(15) . . . . ? N41 Rh2 C23 C22 83.01(17) . . . . ? N50 Rh2 C23 C22 -16.6(4) . . . . ? C25 Rh2 C23 C22 -80.58(17) . . . . ? C21 Rh2 C23 C22 -37.23(16) . . . . ? C24 Rh2 C23 C22 -117.4(2) . . . . ? N3 Rh2 C23 C28 54.4(3) . . . . ? N41 Rh2 C23 C28 -38.1(3) . . . . ? N50 Rh2 C23 C28 -137.8(3) . . . . ? C25 Rh2 C23 C28 158.3(3) . . . . ? C21 Rh2 C23 C28 -158.4(3) . . . . ? C22 Rh2 C23 C28 -121.1(4) . . . . ? C24 Rh2 C23 C28 121.4(4) . . . . ? C22 C23 C24 C25 2.0(3) . . . . ? C28 C23 C24 C25 175.0(3) . . . . ? Rh2 C23 C24 C25 -59.58(18) . . . . ? C22 C23 C24 C29 -177.9(3) . . . . ? C28 C23 C24 C29 -4.9(4) . . . . ? Rh2 C23 C24 C29 120.5(3) . . . . ? C22 C23 C24 Rh2 61.60(18) . . . . ? C28 C23 C24 Rh2 -125.4(3) . . . . ? N3 Rh2 C24 C23 120.76(15) . . . . ? N41 Rh2 C24 C23 32.5(2) . . . . ? N50 Rh2 C24 C23 -151.47(16) . . . . ? C25 Rh2 C24 C23 -119.5(2) . . . . ? C21 Rh2 C24 C23 -80.87(17) . . . . ? C22 Rh2 C24 C23 -38.20(15) . . . . ? N3 Rh2 C24 C25 -119.74(16) . . . . ? N41 Rh2 C24 C25 152.00(16) . . . . ? N50 Rh2 C24 C25 -32.0(2) . . . . ? C23 Rh2 C24 C25 119.5(2) . . . . ? C21 Rh2 C24 C25 38.63(16) . . . . ? C22 Rh2 C24 C25 81.30(17) . . . . ? N3 Rh2 C24 C29 -0.4(3) . . . . ? N41 Rh2 C24 C29 -88.7(3) . . . . ? N50 Rh2 C24 C29 87.4(3) . . . . ? C25 Rh2 C24 C29 119.3(3) . . . . ? C23 Rh2 C24 C29 -121.2(3) . . . . ? C21 Rh2 C24 C29 158.0(3) . . . . ? C22 Rh2 C24 C29 -159.4(3) . . . . ? C23 C24 C25 C21 -2.3(3) . . . . ? C29 C24 C25 C21 177.6(3) . . . . ? Rh2 C24 C25 C21 -62.16(17) . . . . ? C23 C24 C25 C30 -176.1(3) . . . . ? C29 C24 C25 C30 3.7(4) . . . . ? Rh2 C24 C25 C30 124.0(3) . . . . ? C23 C24 C25 Rh2 59.89(18) . . . . ? C29 C24 C25 Rh2 -120.2(3) . . . . ? C22 C21 C25 C24 1.6(3) . . . . ? C26 C21 C25 C24 -176.8(2) . . . . ? Rh2 C21 C25 C24 62.58(17) . . . . ? C22 C21 C25 C30 175.3(3) . . . . ? C26 C21 C25 C30 -3.2(4) . . . . ? Rh2 C21 C25 C30 -123.8(3) . . . . ? C22 C21 C25 Rh2 -60.93(18) . . . . ? C26 C21 C25 Rh2 120.6(3) . . . . ? N3 Rh2 C25 C24 68.02(18) . . . . ? N41 Rh2 C25 C24 -101.6(3) . . . . ? N50 Rh2 C25 C24 159.91(16) . . . . ? C23 Rh2 C25 C24 -36.55(16) . . . . ? C21 Rh2 C25 C24 -116.6(2) . . . . ? C22 Rh2 C25 C24 -79.73(18) . . . . ? N3 Rh2 C25 C21 -175.36(14) . . . . ? N41 Rh2 C25 C21 15.0(4) . . . . ? N50 Rh2 C25 C21 -83.47(16) . . . . ? C23 Rh2 C25 C21 80.07(17) . . . . ? C22 Rh2 C25 C21 36.89(15) . . . . ? C24 Rh2 C25 C21 116.6(2) . . . . ? N3 Rh2 C25 C30 -52.1(3) . . . . ? N41 Rh2 C25 C30 138.3(3) . . . . ? N50 Rh2 C25 C30 39.8(3) . . . . ? C23 Rh2 C25 C30 -156.7(3) . . . . ? C21 Rh2 C25 C30 123.3(3) . . . . ? C22 Rh2 C25 C30 160.2(3) . . . . ? C24 Rh2 C25 C30 -120.1(3) . . . . ? C35 N31 C31 C32 1.3(4) . . . . ? Rh1 N31 C31 C32 -175.5(2) . . . . ? N31 C31 C32 C33 -0.9(4) . . . . ? C31 C32 C33 C34 -0.1(4) . . . . ? C32 C33 C34 C35 0.7(4) . . . . ? C31 N31 C35 C34 -0.6(4) . . . . ? Rh1 N31 C35 C34 176.49(19) . . . . ? C31 N31 C35 C36 -179.1(2) . . . . ? Rh1 N31 C35 C36 -2.0(3) . . . . ? C33 C34 C35 N31 -0.4(4) . . . . ? C33 C34 C35 C36 178.0(3) . . . . ? C40 N40 C36 C37 -2.9(4) . . . . ? Rh1 N40 C36 C37 169.5(2) . . . . ? C40 N40 C36 C35 176.5(2) . . . . ? Rh1 N40 C36 C35 -11.1(3) . . . . ? N31 C35 C36 N40 8.7(3) . . . . ? C34 C35 C36 N40 -169.8(2) . . . . ? N31 C35 C36 C37 -171.9(2) . . . . ? C34 C35 C36 C37 9.6(4) . . . . ? N40 C36 C37 C38 3.1(4) . . . . ? C35 C36 C37 C38 -176.2(3) . . . . ? C36 C37 C38 C39 -0.5(5) . . . . ? C37 C38 C39 C40 -2.2(5) . . . . ? C36 N40 C40 C39 0.0(4) . . . . ? Rh1 N40 C40 C39 -171.6(2) . . . . ? C38 C39 C40 N40 2.5(5) . . . . ? C45 N41 C41 C42 0.6(4) . . . . ? Rh2 N41 C41 C42 178.7(2) . . . . ? N41 C41 C42 C43 1.1(4) . . . . ? C41 C42 C43 C44 -1.2(5) . . . . ? C42 C43 C44 C45 -0.3(5) . . . . ? C41 N41 C45 C44 -2.2(4) . . . . ? Rh2 N41 C45 C44 179.6(2) . . . . ? C41 N41 C45 C46 177.0(2) . . . . ? Rh2 N41 C45 C46 -1.2(3) . . . . ? C43 C44 C45 N41 2.1(5) . . . . ? C43 C44 C45 C46 -177.0(3) . . . . ? C50 N50 C46 C47 -1.4(4) . . . . ? Rh2 N50 C46 C47 177.0(3) . . . . ? C50 N50 C46 C45 179.7(2) . . . . ? Rh2 N50 C46 C45 -1.9(3) . . . . ? N41 C45 C46 N50 2.0(4) . . . . ? C44 C45 C46 N50 -178.8(3) . . . . ? N41 C45 C46 C47 -176.8(3) . . . . ? C44 C45 C46 C47 2.4(5) . . . . ? N50 C46 C47 C48 2.5(5) . . . . ? C45 C46 C47 C48 -178.7(3) . . . . ? C46 C47 C48 C49 -1.4(6) . . . . ? C47 C48 C49 C50 -0.5(6) . . . . ? C46 N50 C50 C49 -0.6(4) . . . . ? Rh2 N50 C50 C49 -178.9(2) . . . . ? C48 C49 C50 N50 1.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.817 _refine_diff_density_min -1.221 _refine_diff_density_rms 0.080 _database_code_depnum_ccdc_archive 'CCDC 945550' ####################################################################### # # 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_comp8 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H49 N6 Ph2 1+, F6 P 1-' _chemical_formula_sum 'C44 H49 F6 N6 P Rh2' _chemical_formula_weight 1012.68 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' F F 0.0171 0.0103 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.0022(7) _cell_length_b 13.3883(8) _cell_length_c 14.0886(8) _cell_angle_alpha 71.928(3) _cell_angle_beta 80.972(2) _cell_angle_gamma 63.631(2) _cell_volume 2088.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 12861 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.53 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 0.896 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.8412 _exptl_absorpt_correction_T_max 0.9158 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20608 _diffrn_reflns_av_R_equivalents 0.0653 _diffrn_reflns_av_sigmaI/netI 0.0871 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9454 _reflns_number_gt 5977 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0532P)^2^+11.2250P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9454 _refine_ls_number_parameters 522 _refine_ls_number_restraints 55 _refine_ls_R_factor_all 0.1100 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1833 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.24906(5) 0.56738(5) 0.31893(4) 0.02907(16) Uani 1 1 d . . . Rh2 Rh 0.20755(4) 0.18343(5) 0.17809(4) 0.02794(16) Uani 1 1 d . . . P1 P 0.72498(19) 0.1184(2) 0.32598(17) 0.0472(6) Uani 1 1 d D . . F1A F 0.8335(9) 0.0029(9) 0.3753(8) 0.062(3) Uiso 0.50 1 d PD . . F1B F 0.7835(9) -0.0143(8) 0.3855(8) 0.056(3) Uiso 0.50 1 d PD . . F2A F 0.8061(10) 0.1805(11) 0.3348(10) 0.069(3) Uiso 0.50 1 d PD . . F3 F 0.6865(5) 0.1449(6) 0.4307(5) 0.0846(19) Uiso 1 1 d D . . F4A F 0.6560(15) 0.0529(15) 0.3164(14) 0.117(5) Uiso 0.50 1 d PD . . F4B F 0.6034(11) 0.1082(15) 0.3507(12) 0.104(5) Uiso 0.50 1 d PD . . F5A F 0.7327(12) 0.0799(12) 0.2273(9) 0.084(4) Uiso 0.50 1 d PD . . F5B F 0.7921(9) 0.1046(9) 0.2218(7) 0.055(3) Uiso 0.50 1 d PD . . F6A F 0.6543(9) 0.2536(8) 0.2650(8) 0.044(3) Uiso 0.50 1 d PD . . F2B F 0.8355(14) 0.1379(19) 0.3010(16) 0.142(7) Uiso 0.50 1 d PD . . F6B F 0.6249(10) 0.2358(10) 0.2734(10) 0.072(4) Uiso 0.50 1 d PD . . N1 N 0.2041(5) 0.4519(5) 0.2804(4) 0.0291(13) Uani 1 1 d . . . N2 N 0.0975(5) 0.4541(5) 0.3087(5) 0.0367(14) Uani 1 1 d . . . N3 N 0.0868(5) 0.3766(5) 0.2786(5) 0.0352(14) Uani 1 1 d . . . N4 N 0.1869(5) 0.3233(5) 0.2289(5) 0.0336(14) Uani 1 1 d . . . N31 N 0.0952(6) 0.6943(5) 0.2554(5) 0.0441(17) Uani 1 1 d . . . N42 N 0.0440(5) 0.2882(5) 0.1184(4) 0.0304(13) Uani 1 1 d . . . C5 C 0.2565(6) 0.3693(6) 0.2335(5) 0.0307(15) Uani 1 1 d . . . C6 C 0.3754(6) 0.3350(7) 0.1933(6) 0.0385(18) Uani 1 1 d . . . H6A H 0.4249 0.3296 0.2422 0.046 Uiso 1 1 calc R . . H6B H 0.3775 0.3930 0.1312 0.046 Uiso 1 1 calc R . . H6C H 0.4028 0.2595 0.1800 0.046 Uiso 1 1 calc R . . C11 C 0.4063(6) 0.5109(6) 0.4001(5) 0.0323(16) Uani 1 1 d . . . C12 C 0.3304(7) 0.6278(6) 0.3976(6) 0.0373(17) Uani 1 1 d . . . C13 C 0.2281(7) 0.6234(8) 0.4550(6) 0.048(2) Uani 1 1 d . . . C14 C 0.2389(7) 0.5101(8) 0.4840(6) 0.0423(19) Uani 1 1 d . . . C15 C 0.3501(6) 0.4396(6) 0.4483(6) 0.0353(17) Uani 1 1 d . . . C16 C 0.5302(7) 0.4715(9) 0.3638(7) 0.054(2) Uani 1 1 d . . . H16A H 0.5376 0.5312 0.3054 0.065 Uiso 1 1 calc R . . H16B H 0.5547 0.3993 0.3453 0.065 Uiso 1 1 calc R . . H16C H 0.5787 0.4583 0.4171 0.065 Uiso 1 1 calc R . . C17 C 0.3587(10) 0.7294(8) 0.3584(8) 0.071(3) Uani 1 1 d . . . H17A H 0.2876 0.8005 0.3432 0.086 Uiso 1 1 calc R . . H17B H 0.4063 0.7226 0.2975 0.086 Uiso 1 1 calc R . . H17C H 0.4007 0.7323 0.4088 0.086 Uiso 1 1 calc R . . C18 C 0.1323(9) 0.7278(10) 0.4810(9) 0.090(4) Uani 1 1 d . . . H18A H 0.1149 0.7950 0.4224 0.108 Uiso 1 1 calc R . . H18B H 0.1558 0.7434 0.5357 0.108 Uiso 1 1 calc R . . H18C H 0.0638 0.7128 0.5020 0.108 Uiso 1 1 calc R . . C19 C 0.1569(9) 0.4625(11) 0.5466(8) 0.078(4) Uani 1 1 d . . . H19A H 0.1415 0.4176 0.5118 0.094 Uiso 1 1 calc R . . H19B H 0.0848 0.5266 0.5573 0.094 Uiso 1 1 calc R . . H19C H 0.1912 0.4122 0.6111 0.094 Uiso 1 1 calc R . . C20 C 0.3981(8) 0.3102(7) 0.4696(7) 0.053(2) Uani 1 1 d . . . H20A H 0.3428 0.2893 0.4499 0.064 Uiso 1 1 calc R . . H20B H 0.4126 0.2745 0.5411 0.064 Uiso 1 1 calc R . . H20C H 0.4702 0.2823 0.4315 0.064 Uiso 1 1 calc R . . C21 C 0.3622(5) 0.0243(5) 0.2261(6) 0.0345(17) Uani 1 1 d . . . C22 C 0.3000(6) 0.0525(6) 0.3121(6) 0.0357(17) Uani 1 1 d . . . C23 C 0.1901(6) 0.0510(6) 0.3145(5) 0.0295(15) Uani 1 1 d . . . C24 C 0.1848(6) 0.0226(6) 0.2258(6) 0.0315(16) Uani 1 1 d . . . C25 C 0.2914(6) 0.0073(6) 0.1711(6) 0.0352(17) Uani 1 1 d . . . C26 C 0.4889(7) -0.0029(8) 0.2049(7) 0.055(2) Uani 1 1 d . . . H26A H 0.5055 0.0056 0.1333 0.066 Uiso 1 1 calc R . . H26B H 0.5354 -0.0826 0.2424 0.066 Uiso 1 1 calc R . . H26C H 0.5072 0.0508 0.2255 0.066 Uiso 1 1 calc R . . C27 C 0.3434(7) 0.0768(7) 0.3913(6) 0.044(2) Uani 1 1 d . . . H27A H 0.2795 0.1351 0.4188 0.053 Uiso 1 1 calc R . . H27B H 0.4017 0.1059 0.3621 0.053 Uiso 1 1 calc R . . H27C H 0.3774 0.0053 0.4448 0.053 Uiso 1 1 calc R . . C28 C 0.1019(7) 0.0677(8) 0.3957(6) 0.049(2) Uani 1 1 d . . . H28A H 0.0294 0.0793 0.3719 0.059 Uiso 1 1 calc R . . H28B H 0.0906 0.1357 0.4158 0.059 Uiso 1 1 calc R . . H28C H 0.1274 -0.0010 0.4530 0.059 Uiso 1 1 calc R . . C29 C 0.0878(7) 0.0070(7) 0.1972(7) 0.048(2) Uani 1 1 d . . . H29A H 0.0147 0.0625 0.2179 0.057 Uiso 1 1 calc R . . H29B H 0.0957 -0.0720 0.2304 0.057 Uiso 1 1 calc R . . H29C H 0.0896 0.0203 0.1247 0.057 Uiso 1 1 calc R . . C30 C 0.3227(8) -0.0330(7) 0.0779(7) 0.052(2) Uani 1 1 d . . . H30A H 0.2557 0.0056 0.0351 0.063 Uiso 1 1 calc R . . H30B H 0.3476 -0.1171 0.0959 0.063 Uiso 1 1 calc R . . H30C H 0.3853 -0.0139 0.0419 0.063 Uiso 1 1 calc R . . C31 C -0.0082(6) 0.7204(7) 0.3027(7) 0.048(2) Uani 1 1 d . . . H31 H -0.0126 0.6782 0.3701 0.058 Uiso 1 1 calc R . . C32 C -0.1068(8) 0.8054(9) 0.2568(9) 0.068(3) Uani 1 1 d . . . H32 H -0.1780 0.8248 0.2927 0.082 Uiso 1 1 calc R . . C33 C -0.1018(10) 0.8618(8) 0.1593(10) 0.075(4) Uani 1 1 d . . . H33 H -0.1700 0.9202 0.1263 0.090 Uiso 1 1 calc R . . C34 C 0.0021(10) 0.8347(8) 0.1078(9) 0.070(3) Uani 1 1 d . . . H34 H 0.0052 0.8739 0.0393 0.084 Uiso 1 1 calc R . . C35 C 0.1026(8) 0.7498(6) 0.1564(6) 0.044(2) Uani 1 1 d . . . C36 C 0.2181(8) 0.7137(7) 0.1132(6) 0.046(2) Uani 1 1 d . . . C37 C 0.2448(10) 0.7605(8) 0.0131(7) 0.059(3) Uani 1 1 d . . . H37 H 0.1859 0.8205 -0.0303 0.071 Uiso 1 1 calc R . . C38 C 0.3557(11) 0.7190(11) -0.0205(7) 0.071(3) Uani 1 1 d . . . H38 H 0.3747 0.7531 -0.0867 0.086 Uiso 1 1 calc R . . C39 C 0.4396(10) 0.6289(10) 0.0400(7) 0.062(3) Uani 1 1 d . . . H39 H 0.5163 0.5986 0.0151 0.074 Uiso 1 1 calc R . . C40 C 0.4131(8) 0.5815(8) 0.1378(6) 0.047(2) Uani 1 1 d . . . H40 H 0.4725 0.5198 0.1798 0.056 Uiso 1 1 calc R . . C41 C 0.3031(7) 0.6222(7) 0.1747(5) 0.0351(17) Uani 1 1 d . . . C42 C -0.0542(6) 0.3019(6) 0.1716(7) 0.0386(18) Uani 1 1 d . . . H42 H -0.0503 0.2641 0.2410 0.046 Uiso 1 1 calc R . . C43 C -0.1588(6) 0.3676(7) 0.1298(7) 0.044(2) Uani 1 1 d . . . H43 H -0.2271 0.3744 0.1686 0.053 Uiso 1 1 calc R . . C44 C -0.1635(7) 0.4246(7) 0.0293(7) 0.047(2) Uani 1 1 d . . . H44 H -0.2357 0.4727 -0.0015 0.057 Uiso 1 1 calc R . . C45 C -0.0646(6) 0.4119(6) -0.0260(6) 0.0400(18) Uani 1 1 d . . . H45 H -0.0677 0.4507 -0.0953 0.048 Uiso 1 1 calc R . . C46 C 0.0415(6) 0.3413(6) 0.0202(6) 0.0337(16) Uani 1 1 d . . . C47 C 0.1535(6) 0.3209(6) -0.0291(5) 0.0328(16) Uani 1 1 d . . . C48 C 0.1684(7) 0.3668(7) -0.1312(6) 0.0422(19) Uani 1 1 d . . . H48 H 0.1038 0.4117 -0.1731 0.051 Uiso 1 1 calc R . . C49 C 0.2770(8) 0.3465(8) -0.1704(6) 0.046(2) Uani 1 1 d . . . H49 H 0.2874 0.3770 -0.2399 0.056 Uiso 1 1 calc R . . C50 C 0.3702(7) 0.2832(7) -0.1108(6) 0.045(2) Uani 1 1 d . . . H50 H 0.4450 0.2698 -0.1388 0.054 Uiso 1 1 calc R . . C51 C 0.3557(7) 0.2382(7) -0.0096(6) 0.0419(19) Uani 1 1 d . . . H51 H 0.4210 0.1953 0.0317 0.050 Uiso 1 1 calc R . . C52 C 0.2469(6) 0.2548(6) 0.0328(5) 0.0305(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0336(3) 0.0257(3) 0.0297(3) -0.0086(2) -0.0026(2) -0.0127(2) Rh2 0.0295(3) 0.0222(3) 0.0323(3) -0.0084(2) -0.0028(2) -0.0096(2) P1 0.0451(12) 0.0475(13) 0.0409(13) -0.0136(11) -0.0027(10) -0.0108(10) N1 0.035(3) 0.025(3) 0.034(3) -0.011(3) -0.002(3) -0.016(2) N2 0.036(3) 0.038(4) 0.043(4) -0.017(3) 0.001(3) -0.019(3) N3 0.030(3) 0.033(3) 0.036(4) -0.011(3) 0.005(3) -0.008(3) N4 0.034(3) 0.030(3) 0.035(3) -0.010(3) -0.003(3) -0.011(3) N31 0.049(4) 0.028(3) 0.055(5) -0.010(3) -0.024(3) -0.010(3) N42 0.026(3) 0.028(3) 0.032(3) -0.003(3) -0.016(3) -0.006(2) C5 0.037(4) 0.024(4) 0.032(4) -0.006(3) -0.005(3) -0.013(3) C6 0.029(4) 0.046(5) 0.045(5) -0.018(4) 0.008(3) -0.019(3) C11 0.032(4) 0.037(4) 0.029(4) -0.004(3) -0.014(3) -0.015(3) C12 0.049(4) 0.031(4) 0.039(4) -0.008(3) -0.017(4) -0.019(3) C13 0.055(5) 0.061(6) 0.034(4) -0.038(4) -0.016(4) -0.008(4) C14 0.036(4) 0.064(6) 0.025(4) -0.012(4) 0.001(3) -0.021(4) C15 0.041(4) 0.031(4) 0.031(4) -0.006(3) -0.012(3) -0.010(3) C16 0.043(5) 0.072(7) 0.046(5) -0.015(5) -0.007(4) -0.023(5) C17 0.107(8) 0.048(6) 0.073(7) -0.002(5) -0.045(6) -0.041(6) C18 0.062(6) 0.093(9) 0.103(10) -0.074(8) -0.020(6) 0.015(6) C19 0.057(6) 0.134(11) 0.051(6) -0.019(7) 0.015(5) -0.057(7) C20 0.071(6) 0.037(5) 0.052(6) -0.001(4) -0.024(5) -0.022(4) C21 0.019(3) 0.011(3) 0.056(5) -0.006(3) -0.006(3) 0.009(2) C22 0.040(4) 0.025(4) 0.031(4) -0.004(3) -0.003(3) -0.006(3) C23 0.041(4) 0.026(4) 0.030(4) -0.006(3) 0.001(3) -0.023(3) C24 0.043(4) 0.018(3) 0.042(4) -0.006(3) -0.008(3) -0.019(3) C25 0.047(4) 0.020(4) 0.040(4) -0.010(3) -0.005(4) -0.014(3) C26 0.043(5) 0.048(5) 0.062(6) -0.004(5) -0.016(4) -0.012(4) C27 0.069(5) 0.053(5) 0.024(4) -0.009(4) -0.017(4) -0.033(4) C28 0.051(5) 0.047(5) 0.045(5) -0.013(4) 0.000(4) -0.016(4) C29 0.056(5) 0.039(5) 0.059(6) -0.016(4) -0.016(4) -0.022(4) C30 0.061(5) 0.039(5) 0.050(5) -0.021(4) -0.005(4) -0.008(4) C31 0.028(4) 0.037(5) 0.073(6) -0.023(4) -0.008(4) -0.001(3) C32 0.050(5) 0.059(6) 0.096(9) -0.037(7) -0.031(6) -0.003(5) C33 0.081(8) 0.034(5) 0.096(9) -0.020(6) -0.061(7) 0.009(5) C34 0.095(8) 0.032(5) 0.076(8) -0.009(5) -0.043(6) -0.011(5) C35 0.068(6) 0.021(4) 0.045(5) -0.005(3) -0.030(4) -0.015(4) C36 0.075(6) 0.034(4) 0.041(5) -0.009(4) -0.012(4) -0.029(4) C37 0.103(8) 0.047(5) 0.047(6) -0.002(4) -0.018(6) -0.052(6) C38 0.120(10) 0.101(9) 0.029(5) -0.009(6) 0.003(6) -0.085(8) C39 0.089(7) 0.090(8) 0.043(5) -0.022(6) 0.008(5) -0.070(7) C40 0.062(5) 0.073(6) 0.025(4) -0.013(4) 0.002(4) -0.045(5) C41 0.056(5) 0.038(4) 0.029(4) -0.014(3) 0.007(4) -0.034(4) C42 0.031(4) 0.033(4) 0.053(5) -0.012(4) -0.005(4) -0.013(3) C43 0.027(4) 0.031(4) 0.068(6) -0.014(4) -0.001(4) -0.007(3) C44 0.037(4) 0.030(4) 0.067(6) -0.004(4) -0.024(4) -0.007(3) C45 0.045(4) 0.028(4) 0.041(5) -0.003(3) -0.016(4) -0.010(3) C46 0.036(4) 0.024(4) 0.038(4) -0.007(3) -0.017(3) -0.005(3) C47 0.043(4) 0.027(4) 0.034(4) -0.011(3) -0.004(3) -0.017(3) C48 0.055(5) 0.040(5) 0.036(4) -0.005(4) -0.013(4) -0.024(4) C49 0.068(6) 0.050(5) 0.030(4) -0.008(4) -0.003(4) -0.033(5) C50 0.040(4) 0.049(5) 0.045(5) -0.017(4) 0.014(4) -0.020(4) C51 0.042(4) 0.040(5) 0.044(5) -0.018(4) 0.006(4) -0.016(4) C52 0.038(4) 0.023(3) 0.030(4) -0.006(3) -0.001(3) -0.012(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 Rh1 C41 2.061(7) . ? Rh1 N31 2.071(6) . ? Rh1 N1 2.110(5) . ? Rh1 C12 2.165(7) . ? Rh1 C15 2.190(7) . ? Rh1 C13 2.204(7) . ? Rh1 C11 2.210(7) . ? Rh1 C14 2.213(8) . ? Rh2 C52 2.064(7) . ? Rh2 N42 2.092(5) . ? Rh2 N4 2.101(6) . ? Rh2 C25 2.141(7) . ? Rh2 C21 2.183(6) . ? Rh2 C24 2.187(6) . ? Rh2 C22 2.207(7) . ? Rh2 C23 2.235(7) . ? P1 F2B 1.541(12) . ? P1 F4A 1.549(11) . ? P1 F6B 1.574(10) . ? P1 F3 1.578(6) . ? P1 F1B 1.585(9) . ? P1 F5A 1.601(10) . ? P1 F5B 1.604(9) . ? P1 F1A 1.603(9) . ? P1 F6A 1.632(9) . ? P1 F4B 1.621(11) . ? P1 F2A 1.644(10) . ? N1 C5 1.329(8) . ? N1 N2 1.371(8) . ? N2 N3 1.302(8) . ? N3 N4 1.375(8) . ? N4 C5 1.319(9) . ? N31 C31 1.349(10) . ? N31 C35 1.373(11) . ? N42 C42 1.343(9) . ? N42 C46 1.343(9) . ? C5 C6 1.476(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C15 1.403(10) . ? C11 C12 1.424(10) . ? C11 C16 1.514(10) . ? C12 C13 1.459(12) . ? C12 C17 1.485(11) . ? C13 C14 1.389(12) . ? C13 C18 1.506(11) . ? C14 C15 1.444(10) . ? C14 C19 1.511(12) . ? C15 C20 1.502(11) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.403(10) . ? C21 C25 1.420(10) . ? C21 C26 1.522(10) . ? C22 C23 1.433(10) . ? C22 C27 1.502(10) . ? C23 C24 1.435(10) . ? C23 C28 1.480(10) . ? C24 C25 1.437(10) . ? C24 C29 1.497(10) . ? C25 C30 1.504(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.366(12) . ? C31 H31 0.9500 . ? C32 C33 1.353(16) . ? C32 H32 0.9500 . ? C33 C34 1.379(16) . ? C33 H33 0.9500 . ? C34 C35 1.395(12) . ? C34 H34 0.9500 . ? C35 C36 1.453(12) . ? C36 C41 1.382(11) . ? C36 C37 1.412(12) . ? C37 C38 1.359(15) . ? C37 H37 0.9500 . ? C38 C39 1.362(15) . ? C38 H38 0.9500 . ? C39 C40 1.387(11) . ? C39 H39 0.9500 . ? C40 C41 1.365(11) . ? C40 H40 0.9500 . ? C42 C43 1.355(10) . ? C42 H42 0.9500 . ? C43 C44 1.381(12) . ? C43 H43 0.9500 . ? C44 C45 1.364(11) . ? C44 H44 0.9500 . ? C45 C46 1.401(10) . ? C45 H45 0.9500 . ? C46 C47 1.457(10) . ? C47 C52 1.384(10) . ? C47 C48 1.399(10) . ? C48 C49 1.371(11) . ? C48 H48 0.9500 . ? C49 C50 1.363(12) . ? C49 H49 0.9500 . ? C50 C51 1.384(11) . ? C50 H50 0.9500 . ? C51 C52 1.395(10) . ? C51 H51 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 C41 Rh1 N31 79.2(3) . . ? C41 Rh1 N1 91.8(2) . . ? N31 Rh1 N1 85.3(2) . . ? C41 Rh1 C12 100.2(3) . . ? N31 Rh1 C12 113.5(3) . . ? N1 Rh1 C12 159.1(3) . . ? C41 Rh1 C15 129.4(3) . . ? N31 Rh1 C15 151.2(3) . . ? N1 Rh1 C15 95.4(3) . . ? C12 Rh1 C15 63.8(3) . . ? C41 Rh1 C13 133.6(3) . . ? N31 Rh1 C13 96.7(3) . . ? N1 Rh1 C13 134.3(3) . . ? C12 Rh1 C13 39.0(3) . . ? C15 Rh1 C13 62.6(3) . . ? C41 Rh1 C11 100.1(3) . . ? N31 Rh1 C11 151.3(3) . . ? N1 Rh1 C11 123.2(3) . . ? C12 Rh1 C11 38.0(3) . . ? C15 Rh1 C11 37.2(3) . . ? C13 Rh1 C11 62.8(3) . . ? C41 Rh1 C14 162.6(3) . . ? N31 Rh1 C14 113.3(3) . . ? N1 Rh1 C14 101.1(3) . . ? C12 Rh1 C14 64.1(3) . . ? C15 Rh1 C14 38.3(3) . . ? C13 Rh1 C14 36.7(3) . . ? C11 Rh1 C14 63.0(3) . . ? C52 Rh2 N42 78.4(3) . . ? C52 Rh2 N4 94.4(3) . . ? N42 Rh2 N4 86.4(2) . . ? C52 Rh2 C25 96.0(3) . . ? N42 Rh2 C25 119.1(3) . . ? N4 Rh2 C25 154.0(3) . . ? C52 Rh2 C21 103.6(3) . . ? N42 Rh2 C21 157.1(3) . . ? N4 Rh2 C21 115.9(3) . . ? C25 Rh2 C21 38.3(3) . . ? C52 Rh2 C24 123.4(3) . . ? N42 Rh2 C24 95.5(2) . . ? N4 Rh2 C24 141.8(3) . . ? C25 Rh2 C24 38.8(3) . . ? C21 Rh2 C24 64.0(3) . . ? C52 Rh2 C22 137.8(3) . . ? N42 Rh2 C22 143.5(3) . . ? N4 Rh2 C22 93.5(3) . . ? C25 Rh2 C22 63.2(3) . . ? C21 Rh2 C22 37.3(3) . . ? C24 Rh2 C22 63.2(3) . . ? C52 Rh2 C23 159.6(3) . . ? N42 Rh2 C23 107.4(2) . . ? N4 Rh2 C23 105.3(2) . . ? C25 Rh2 C23 63.9(3) . . ? C21 Rh2 C23 63.3(3) . . ? C24 Rh2 C23 37.8(3) . . ? C22 Rh2 C23 37.6(3) . . ? F2B P1 F6B 106.1(10) . . ? F2B P1 F3 102.7(9) . . ? F4A P1 F3 104.7(7) . . ? F6B P1 F3 91.0(6) . . ? F2B P1 F1B 97.1(9) . . ? F6B P1 F1B 156.5(7) . . ? F3 P1 F1B 87.0(5) . . ? F4A P1 F5A 58.1(8) . . ? F3 P1 F5A 162.6(6) . . ? F1B P1 F5A 88.8(6) . . ? F2B P1 F5B 60.2(9) . . ? F6B P1 F5B 92.2(7) . . ? F3 P1 F5B 162.9(5) . . ? F1B P1 F5B 96.6(5) . . ? F4A P1 F1A 94.4(8) . . ? F3 P1 F1A 90.5(5) . . ? F5A P1 F1A 93.6(6) . . ? F4A P1 F6A 106.3(8) . . ? F3 P1 F6A 92.7(5) . . ? F5A P1 F6A 89.9(6) . . ? F1A P1 F6A 157.4(6) . . ? F2B P1 F4B 175.7(10) . . ? F6B P1 F4B 70.0(8) . . ? F3 P1 F4B 75.9(6) . . ? F1B P1 F4B 86.9(7) . . ? F5B P1 F4B 120.9(7) . . ? F4A P1 F2A 176.1(9) . . ? F3 P1 F2A 77.5(5) . . ? F5A P1 F2A 119.7(7) . . ? F1A P1 F2A 82.4(6) . . ? F6A P1 F2A 76.5(6) . . ? C5 N1 N2 106.2(5) . . ? C5 N1 Rh1 135.4(5) . . ? N2 N1 Rh1 118.4(4) . . ? N3 N2 N1 108.9(5) . . ? N2 N3 N4 107.9(5) . . ? C5 N4 N3 106.9(6) . . ? C5 N4 Rh2 133.5(5) . . ? N3 N4 Rh2 119.2(4) . . ? C31 N31 C35 119.8(7) . . ? C31 N31 Rh1 124.8(6) . . ? C35 N31 Rh1 115.3(6) . . ? C42 N42 C46 120.3(6) . . ? C42 N42 Rh2 124.0(5) . . ? C46 N42 Rh2 115.6(5) . . ? N4 C5 N1 110.0(6) . . ? N4 C5 C6 125.7(6) . . ? N1 C5 C6 124.3(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C15 C11 C12 108.9(6) . . ? C15 C11 C16 126.5(7) . . ? C12 C11 C16 124.4(7) . . ? C15 C11 Rh1 70.6(4) . . ? C12 C11 Rh1 69.3(4) . . ? C16 C11 Rh1 129.9(5) . . ? C11 C12 C13 105.8(7) . . ? C11 C12 C17 126.1(8) . . ? C13 C12 C17 127.4(8) . . ? C11 C12 Rh1 72.7(4) . . ? C13 C12 Rh1 71.9(4) . . ? C17 C12 Rh1 127.4(6) . . ? C14 C13 C12 109.3(7) . . ? C14 C13 C18 127.9(10) . . ? C12 C13 C18 122.7(9) . . ? C14 C13 Rh1 72.0(4) . . ? C12 C13 Rh1 69.0(4) . . ? C18 C13 Rh1 127.7(6) . . ? C13 C14 C15 107.3(7) . . ? C13 C14 C19 128.7(8) . . ? C15 C14 C19 123.9(9) . . ? C13 C14 Rh1 71.3(4) . . ? C15 C14 Rh1 70.0(4) . . ? C19 C14 Rh1 126.8(6) . . ? C11 C15 C14 108.4(7) . . ? C11 C15 C20 127.3(7) . . ? C14 C15 C20 124.1(7) . . ? C11 C15 Rh1 72.2(4) . . ? C14 C15 Rh1 71.7(4) . . ? C20 C15 Rh1 126.3(6) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 107.7(6) . . ? C22 C21 C26 125.6(7) . . ? C25 C21 C26 125.9(7) . . ? C22 C21 Rh2 72.3(4) . . ? C25 C21 Rh2 69.2(4) . . ? C26 C21 Rh2 131.5(6) . . ? C21 C22 C23 109.6(7) . . ? C21 C22 C27 125.2(7) . . ? C23 C22 C27 125.1(7) . . ? C21 C22 Rh2 70.5(4) . . ? C23 C22 Rh2 72.3(4) . . ? C27 C22 Rh2 125.2(5) . . ? C22 C23 C24 106.7(6) . . ? C22 C23 C28 126.9(7) . . ? C24 C23 C28 126.3(7) . . ? C22 C23 Rh2 70.1(4) . . ? C24 C23 Rh2 69.3(4) . . ? C28 C23 Rh2 128.5(5) . . ? C23 C24 C25 107.6(6) . . ? C23 C24 C29 126.3(7) . . ? C25 C24 C29 126.1(7) . . ? C23 C24 Rh2 72.9(4) . . ? C25 C24 Rh2 68.9(4) . . ? C29 C24 Rh2 125.4(5) . . ? C21 C25 C24 108.4(6) . . ? C21 C25 C30 127.7(7) . . ? C24 C25 C30 123.6(7) . . ? C21 C25 Rh2 72.5(4) . . ? C24 C25 Rh2 72.4(4) . . ? C30 C25 Rh2 126.3(6) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N31 C31 C32 122.1(10) . . ? N31 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C33 C32 C31 119.2(10) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C32 C33 C34 120.2(9) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 120.0(10) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? N31 C35 C34 118.6(9) . . ? N31 C35 C36 114.9(7) . . ? C34 C35 C36 126.5(9) . . ? C41 C36 C37 120.1(9) . . ? C41 C36 C35 115.7(7) . . ? C37 C36 C35 124.0(9) . . ? C38 C37 C36 119.4(10) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C37 C38 C39 120.5(9) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C38 C39 C40 120.1(10) . . ? C38 C39 H39 119.9 . . ? C40 C39 H39 119.9 . . ? C41 C40 C39 121.0(9) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.5 . . ? C40 C41 C36 118.8(7) . . ? C40 C41 Rh1 126.4(6) . . ? C36 C41 Rh1 114.7(6) . . ? N42 C42 C43 122.5(8) . . ? N42 C42 H42 118.8 . . ? C43 C42 H42 118.8 . . ? C42 C43 C44 118.2(8) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C45 C44 C43 120.2(7) . . ? C45 C44 H44 119.9 . . ? C43 C44 H44 119.9 . . ? C44 C45 C46 119.4(8) . . ? C44 C45 H45 120.3 . . ? C46 C45 H45 120.3 . . ? N42 C46 C45 119.3(7) . . ? N42 C46 C47 115.2(6) . . ? C45 C46 C47 125.4(7) . . ? C52 C47 C48 120.9(7) . . ? C52 C47 C46 115.5(6) . . ? C48 C47 C46 123.6(7) . . ? C49 C48 C47 119.5(8) . . ? C49 C48 H48 120.3 . . ? C47 C48 H48 120.3 . . ? C50 C49 C48 120.8(8) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? C49 C50 C51 119.9(7) . . ? C49 C50 H50 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 C52 121.0(8) . . ? C50 C51 H51 119.5 . . ? C52 C51 H51 119.5 . . ? C47 C52 C51 117.9(7) . . ? C47 C52 Rh2 114.7(5) . . ? C51 C52 Rh2 127.3(6) . . ? 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 C41 Rh1 N1 C5 51.2(7) . . . . ? N31 Rh1 N1 C5 130.2(7) . . . . ? C12 Rh1 N1 C5 -74.3(11) . . . . ? C15 Rh1 N1 C5 -78.7(7) . . . . ? C13 Rh1 N1 C5 -135.1(7) . . . . ? C11 Rh1 N1 C5 -52.2(8) . . . . ? C14 Rh1 N1 C5 -117.0(7) . . . . ? C41 Rh1 N1 N2 -130.3(5) . . . . ? N31 Rh1 N1 N2 -51.3(5) . . . . ? C12 Rh1 N1 N2 104.2(8) . . . . ? C15 Rh1 N1 N2 99.8(5) . . . . ? C13 Rh1 N1 N2 43.4(7) . . . . ? C11 Rh1 N1 N2 126.3(5) . . . . ? C14 Rh1 N1 N2 61.5(5) . . . . ? C5 N1 N2 N3 -0.8(8) . . . . ? Rh1 N1 N2 N3 -179.7(4) . . . . ? N1 N2 N3 N4 -0.6(8) . . . . ? N2 N3 N4 C5 1.7(8) . . . . ? N2 N3 N4 Rh2 175.4(5) . . . . ? C52 Rh2 N4 C5 -61.7(7) . . . . ? N42 Rh2 N4 C5 -139.8(7) . . . . ? C25 Rh2 N4 C5 51.6(10) . . . . ? C21 Rh2 N4 C5 45.7(8) . . . . ? C24 Rh2 N4 C5 125.9(7) . . . . ? C22 Rh2 N4 C5 76.8(7) . . . . ? C23 Rh2 N4 C5 113.1(7) . . . . ? C52 Rh2 N4 N3 126.5(5) . . . . ? N42 Rh2 N4 N3 48.4(5) . . . . ? C25 Rh2 N4 N3 -120.1(7) . . . . ? C21 Rh2 N4 N3 -126.0(5) . . . . ? C24 Rh2 N4 N3 -45.8(7) . . . . ? C22 Rh2 N4 N3 -94.9(5) . . . . ? C23 Rh2 N4 N3 -58.6(5) . . . . ? C41 Rh1 N31 C31 176.3(7) . . . . ? N1 Rh1 N31 C31 83.6(6) . . . . ? C12 Rh1 N31 C31 -87.2(7) . . . . ? C15 Rh1 N31 C31 -9.2(10) . . . . ? C13 Rh1 N31 C31 -50.5(7) . . . . ? C11 Rh1 N31 C31 -92.4(8) . . . . ? C14 Rh1 N31 C31 -16.5(7) . . . . ? C41 Rh1 N31 C35 -0.4(5) . . . . ? N1 Rh1 N31 C35 -93.1(5) . . . . ? C12 Rh1 N31 C35 96.1(6) . . . . ? C15 Rh1 N31 C35 174.1(5) . . . . ? C13 Rh1 N31 C35 132.8(6) . . . . ? C11 Rh1 N31 C35 91.0(7) . . . . ? C14 Rh1 N31 C35 166.8(5) . . . . ? C52 Rh2 N42 C42 -176.9(6) . . . . ? N4 Rh2 N42 C42 -81.7(6) . . . . ? C25 Rh2 N42 C42 92.6(6) . . . . ? C21 Rh2 N42 C42 85.4(9) . . . . ? C24 Rh2 N42 C42 60.0(6) . . . . ? C22 Rh2 N42 C42 9.2(8) . . . . ? C23 Rh2 N42 C42 23.3(6) . . . . ? C52 Rh2 N42 C46 4.5(5) . . . . ? N4 Rh2 N42 C46 99.8(5) . . . . ? C25 Rh2 N42 C46 -85.9(6) . . . . ? C21 Rh2 N42 C46 -93.2(8) . . . . ? C24 Rh2 N42 C46 -118.5(5) . . . . ? C22 Rh2 N42 C46 -169.3(5) . . . . ? C23 Rh2 N42 C46 -155.3(5) . . . . ? N3 N4 C5 N1 -2.2(8) . . . . ? Rh2 N4 C5 N1 -174.7(5) . . . . ? N3 N4 C5 C6 177.5(7) . . . . ? Rh2 N4 C5 C6 5.1(12) . . . . ? N2 N1 C5 N4 1.9(8) . . . . ? Rh1 N1 C5 N4 -179.5(5) . . . . ? N2 N1 C5 C6 -177.9(7) . . . . ? Rh1 N1 C5 C6 0.7(12) . . . . ? C41 Rh1 C11 C15 -146.3(4) . . . . ? N31 Rh1 C11 C15 127.8(6) . . . . ? N1 Rh1 C11 C15 -47.4(5) . . . . ? C12 Rh1 C11 C15 120.0(6) . . . . ? C13 Rh1 C11 C15 79.6(5) . . . . ? C14 Rh1 C11 C15 38.3(5) . . . . ? C41 Rh1 C11 C12 93.7(5) . . . . ? N31 Rh1 C11 C12 7.7(8) . . . . ? N1 Rh1 C11 C12 -167.4(4) . . . . ? C15 Rh1 C11 C12 -120.0(6) . . . . ? C13 Rh1 C11 C12 -40.4(5) . . . . ? C14 Rh1 C11 C12 -81.8(5) . . . . ? C41 Rh1 C11 C16 -24.5(8) . . . . ? N31 Rh1 C11 C16 -110.4(8) . . . . ? N1 Rh1 C11 C16 74.4(8) . . . . ? C12 Rh1 C11 C16 -118.1(9) . . . . ? C15 Rh1 C11 C16 121.8(9) . . . . ? C13 Rh1 C11 C16 -158.5(8) . . . . ? C14 Rh1 C11 C16 160.1(8) . . . . ? C15 C11 C12 C13 5.1(8) . . . . ? C16 C11 C12 C13 -170.3(7) . . . . ? Rh1 C11 C12 C13 64.8(5) . . . . ? C15 C11 C12 C17 176.2(8) . . . . ? C16 C11 C12 C17 0.8(12) . . . . ? Rh1 C11 C12 C17 -124.1(8) . . . . ? C15 C11 C12 Rh1 -59.7(5) . . . . ? C16 C11 C12 Rh1 124.9(7) . . . . ? C41 Rh1 C12 C11 -93.4(5) . . . . ? N31 Rh1 C12 C11 -176.0(4) . . . . ? N1 Rh1 C12 C11 30.8(10) . . . . ? C15 Rh1 C12 C11 35.7(4) . . . . ? C13 Rh1 C12 C11 113.7(7) . . . . ? C14 Rh1 C12 C11 78.5(5) . . . . ? C41 Rh1 C12 C13 152.9(5) . . . . ? N31 Rh1 C12 C13 70.3(5) . . . . ? N1 Rh1 C12 C13 -82.9(9) . . . . ? C15 Rh1 C12 C13 -78.0(5) . . . . ? C11 Rh1 C12 C13 -113.7(7) . . . . ? C14 Rh1 C12 C13 -35.2(5) . . . . ? C41 Rh1 C12 C17 29.2(9) . . . . ? N31 Rh1 C12 C17 -53.3(9) . . . . ? N1 Rh1 C12 C17 153.4(8) . . . . ? C15 Rh1 C12 C17 158.3(9) . . . . ? C13 Rh1 C12 C17 -123.7(10) . . . . ? C11 Rh1 C12 C17 122.6(10) . . . . ? C14 Rh1 C12 C17 -158.9(9) . . . . ? C11 C12 C13 C14 -4.3(8) . . . . ? C17 C12 C13 C14 -175.3(8) . . . . ? Rh1 C12 C13 C14 61.1(5) . . . . ? C11 C12 C13 C18 172.4(8) . . . . ? C17 C12 C13 C18 1.5(13) . . . . ? Rh1 C12 C13 C18 -122.2(8) . . . . ? C11 C12 C13 Rh1 -65.4(5) . . . . ? C17 C12 C13 Rh1 123.7(8) . . . . ? C41 Rh1 C13 C14 -158.0(5) . . . . ? N31 Rh1 C13 C14 120.6(5) . . . . ? N1 Rh1 C13 C14 30.7(6) . . . . ? C12 Rh1 C13 C14 -119.8(7) . . . . ? C15 Rh1 C13 C14 -38.4(5) . . . . ? C11 Rh1 C13 C14 -80.4(5) . . . . ? C41 Rh1 C13 C12 -38.2(6) . . . . ? N31 Rh1 C13 C12 -119.6(5) . . . . ? N1 Rh1 C13 C12 150.4(4) . . . . ? C15 Rh1 C13 C12 81.4(5) . . . . ? C11 Rh1 C13 C12 39.3(4) . . . . ? C14 Rh1 C13 C12 119.8(7) . . . . ? C41 Rh1 C13 C18 77.5(11) . . . . ? N31 Rh1 C13 C18 -3.8(10) . . . . ? N1 Rh1 C13 C18 -93.8(11) . . . . ? C12 Rh1 C13 C18 115.8(12) . . . . ? C15 Rh1 C13 C18 -162.8(11) . . . . ? C11 Rh1 C13 C18 155.1(11) . . . . ? C14 Rh1 C13 C18 -124.5(12) . . . . ? C12 C13 C14 C15 1.9(9) . . . . ? C18 C13 C14 C15 -174.7(8) . . . . ? Rh1 C13 C14 C15 61.1(5) . . . . ? C12 C13 C14 C19 178.2(8) . . . . ? C18 C13 C14 C19 1.7(15) . . . . ? Rh1 C13 C14 C19 -122.6(9) . . . . ? C12 C13 C14 Rh1 -59.2(5) . . . . ? C18 C13 C14 Rh1 124.3(9) . . . . ? C41 Rh1 C14 C13 64.8(12) . . . . ? N31 Rh1 C14 C13 -68.5(5) . . . . ? N1 Rh1 C14 C13 -158.2(5) . . . . ? C12 Rh1 C14 C13 37.4(5) . . . . ? C15 Rh1 C14 C13 117.2(7) . . . . ? C11 Rh1 C14 C13 80.0(5) . . . . ? C41 Rh1 C14 C15 -52.4(12) . . . . ? N31 Rh1 C14 C15 174.3(4) . . . . ? N1 Rh1 C14 C15 84.6(5) . . . . ? C12 Rh1 C14 C15 -79.8(5) . . . . ? C13 Rh1 C14 C15 -117.2(7) . . . . ? C11 Rh1 C14 C15 -37.2(4) . . . . ? C41 Rh1 C14 C19 -170.4(10) . . . . ? N31 Rh1 C14 C19 56.3(9) . . . . ? N1 Rh1 C14 C19 -33.4(9) . . . . ? C12 Rh1 C14 C19 162.2(10) . . . . ? C15 Rh1 C14 C19 -118.0(11) . . . . ? C13 Rh1 C14 C19 124.8(11) . . . . ? C11 Rh1 C14 C19 -155.2(10) . . . . ? C12 C11 C15 C14 -4.1(8) . . . . ? C16 C11 C15 C14 171.2(7) . . . . ? Rh1 C11 C15 C14 -63.0(5) . . . . ? C12 C11 C15 C20 -178.7(7) . . . . ? C16 C11 C15 C20 -3.4(13) . . . . ? Rh1 C11 C15 C20 122.4(8) . . . . ? C12 C11 C15 Rh1 58.9(5) . . . . ? C16 C11 C15 Rh1 -125.8(7) . . . . ? C13 C14 C15 C11 1.4(9) . . . . ? C19 C14 C15 C11 -175.2(8) . . . . ? Rh1 C14 C15 C11 63.3(5) . . . . ? C13 C14 C15 C20 176.2(7) . . . . ? C19 C14 C15 C20 -0.4(13) . . . . ? Rh1 C14 C15 C20 -121.9(8) . . . . ? C13 C14 C15 Rh1 -61.9(5) . . . . ? C19 C14 C15 Rh1 121.6(8) . . . . ? C41 Rh1 C15 C11 45.0(6) . . . . ? N31 Rh1 C15 C11 -128.0(6) . . . . ? N1 Rh1 C15 C11 141.8(4) . . . . ? C12 Rh1 C15 C11 -36.4(4) . . . . ? C13 Rh1 C15 C11 -80.4(5) . . . . ? C14 Rh1 C15 C11 -117.1(7) . . . . ? C41 Rh1 C15 C14 162.1(4) . . . . ? N31 Rh1 C15 C14 -10.9(8) . . . . ? N1 Rh1 C15 C14 -101.1(5) . . . . ? C12 Rh1 C15 C14 80.7(5) . . . . ? C13 Rh1 C15 C14 36.7(5) . . . . ? C11 Rh1 C15 C14 117.1(7) . . . . ? C41 Rh1 C15 C20 -78.6(8) . . . . ? N31 Rh1 C15 C20 108.4(8) . . . . ? N1 Rh1 C15 C20 18.2(7) . . . . ? C12 Rh1 C15 C20 -160.0(8) . . . . ? C13 Rh1 C15 C20 156.0(8) . . . . ? C11 Rh1 C15 C20 -123.6(9) . . . . ? C14 Rh1 C15 C20 119.3(9) . . . . ? C52 Rh2 C21 C22 160.1(5) . . . . ? N42 Rh2 C21 C22 -107.3(7) . . . . ? N4 Rh2 C21 C22 58.2(5) . . . . ? C25 Rh2 C21 C22 -117.6(6) . . . . ? C24 Rh2 C21 C22 -79.1(5) . . . . ? C23 Rh2 C21 C22 -36.6(4) . . . . ? C52 Rh2 C21 C25 -82.3(5) . . . . ? N42 Rh2 C21 C25 10.3(9) . . . . ? N4 Rh2 C21 C25 175.8(4) . . . . ? C24 Rh2 C21 C25 38.5(4) . . . . ? C22 Rh2 C21 C25 117.6(6) . . . . ? C23 Rh2 C21 C25 81.0(5) . . . . ? C52 Rh2 C21 C26 37.9(8) . . . . ? N42 Rh2 C21 C26 130.4(8) . . . . ? N4 Rh2 C21 C26 -64.0(8) . . . . ? C25 Rh2 C21 C26 120.1(10) . . . . ? C24 Rh2 C21 C26 158.7(9) . . . . ? C22 Rh2 C21 C26 -122.3(10) . . . . ? C23 Rh2 C21 C26 -158.9(9) . . . . ? C25 C21 C22 C23 1.5(8) . . . . ? C26 C21 C22 C23 -169.2(7) . . . . ? Rh2 C21 C22 C23 62.0(5) . . . . ? C25 C21 C22 C27 179.7(7) . . . . ? C26 C21 C22 C27 8.9(12) . . . . ? Rh2 C21 C22 C27 -119.9(7) . . . . ? C25 C21 C22 Rh2 -60.4(5) . . . . ? C26 C21 C22 Rh2 128.8(7) . . . . ? C52 Rh2 C22 C21 -29.5(6) . . . . ? N42 Rh2 C22 C21 141.5(5) . . . . ? N4 Rh2 C22 C21 -130.0(4) . . . . ? C25 Rh2 C22 C21 38.0(4) . . . . ? C24 Rh2 C22 C21 81.7(5) . . . . ? C23 Rh2 C22 C21 119.2(6) . . . . ? C52 Rh2 C22 C23 -148.7(4) . . . . ? N42 Rh2 C22 C23 22.3(6) . . . . ? N4 Rh2 C22 C23 110.8(4) . . . . ? C25 Rh2 C22 C23 -81.2(4) . . . . ? C21 Rh2 C22 C23 -119.2(6) . . . . ? C24 Rh2 C22 C23 -37.5(4) . . . . ? C52 Rh2 C22 C27 90.5(7) . . . . ? N42 Rh2 C22 C27 -98.6(7) . . . . ? N4 Rh2 C22 C27 -10.0(7) . . . . ? C25 Rh2 C22 C27 157.9(7) . . . . ? C21 Rh2 C22 C27 119.9(8) . . . . ? C24 Rh2 C22 C27 -158.4(7) . . . . ? C23 Rh2 C22 C27 -120.9(8) . . . . ? C21 C22 C23 C24 -1.0(8) . . . . ? C27 C22 C23 C24 -179.1(7) . . . . ? Rh2 C22 C23 C24 59.9(5) . . . . ? C21 C22 C23 C28 175.3(7) . . . . ? C27 C22 C23 C28 -2.8(12) . . . . ? Rh2 C22 C23 C28 -123.8(8) . . . . ? C21 C22 C23 Rh2 -60.9(5) . . . . ? C27 C22 C23 Rh2 121.0(7) . . . . ? C52 Rh2 C23 C22 89.7(8) . . . . ? N42 Rh2 C23 C22 -166.3(4) . . . . ? N4 Rh2 C23 C22 -75.3(4) . . . . ? C25 Rh2 C23 C22 79.3(4) . . . . ? C21 Rh2 C23 C22 36.3(4) . . . . ? C24 Rh2 C23 C22 117.6(6) . . . . ? C52 Rh2 C23 C24 -27.9(10) . . . . ? N42 Rh2 C23 C24 76.1(4) . . . . ? N4 Rh2 C23 C24 167.1(4) . . . . ? C25 Rh2 C23 C24 -38.3(4) . . . . ? C21 Rh2 C23 C24 -81.3(4) . . . . ? C22 Rh2 C23 C24 -117.6(6) . . . . ? C52 Rh2 C23 C28 -148.4(8) . . . . ? N42 Rh2 C23 C28 -44.4(7) . . . . ? N4 Rh2 C23 C28 46.6(7) . . . . ? C25 Rh2 C23 C28 -158.8(8) . . . . ? C21 Rh2 C23 C28 158.2(8) . . . . ? C24 Rh2 C23 C28 -120.5(8) . . . . ? C22 Rh2 C23 C28 121.9(8) . . . . ? C22 C23 C24 C25 0.0(8) . . . . ? C28 C23 C24 C25 -176.3(7) . . . . ? Rh2 C23 C24 C25 60.4(5) . . . . ? C22 C23 C24 C29 177.8(7) . . . . ? C28 C23 C24 C29 1.5(12) . . . . ? Rh2 C23 C24 C29 -121.7(7) . . . . ? C22 C23 C24 Rh2 -60.4(5) . . . . ? C28 C23 C24 Rh2 123.2(7) . . . . ? C52 Rh2 C24 C23 168.7(4) . . . . ? N42 Rh2 C24 C23 -111.5(4) . . . . ? N4 Rh2 C24 C23 -20.4(6) . . . . ? C25 Rh2 C24 C23 117.2(6) . . . . ? C21 Rh2 C24 C23 79.1(4) . . . . ? C22 Rh2 C24 C23 37.3(4) . . . . ? C52 Rh2 C24 C25 51.5(5) . . . . ? N42 Rh2 C24 C25 131.3(4) . . . . ? N4 Rh2 C24 C25 -137.7(5) . . . . ? C21 Rh2 C24 C25 -38.1(4) . . . . ? C22 Rh2 C24 C25 -79.9(5) . . . . ? C23 Rh2 C24 C25 -117.2(6) . . . . ? C52 Rh2 C24 C29 -68.6(7) . . . . ? N42 Rh2 C24 C29 11.2(7) . . . . ? N4 Rh2 C24 C29 102.3(7) . . . . ? C25 Rh2 C24 C29 -120.1(8) . . . . ? C21 Rh2 C24 C29 -158.2(8) . . . . ? C22 Rh2 C24 C29 160.1(8) . . . . ? C23 Rh2 C24 C29 122.7(8) . . . . ? C22 C21 C25 C24 -1.5(8) . . . . ? C26 C21 C25 C24 169.2(7) . . . . ? Rh2 C21 C25 C24 -63.9(5) . . . . ? C22 C21 C25 C30 -174.9(7) . . . . ? C26 C21 C25 C30 -4.2(12) . . . . ? Rh2 C21 C25 C30 122.7(8) . . . . ? C22 C21 C25 Rh2 62.4(5) . . . . ? C26 C21 C25 Rh2 -126.9(8) . . . . ? C23 C24 C25 C21 0.9(8) . . . . ? C29 C24 C25 C21 -176.9(7) . . . . ? Rh2 C24 C25 C21 64.0(5) . . . . ? C23 C24 C25 C30 174.7(7) . . . . ? C29 C24 C25 C30 -3.2(12) . . . . ? Rh2 C24 C25 C30 -122.3(7) . . . . ? C23 C24 C25 Rh2 -63.0(5) . . . . ? C29 C24 C25 Rh2 119.1(7) . . . . ? C52 Rh2 C25 C21 104.5(5) . . . . ? N42 Rh2 C25 C21 -175.5(4) . . . . ? N4 Rh2 C25 C21 -8.6(8) . . . . ? C24 Rh2 C25 C21 -116.6(6) . . . . ? C22 Rh2 C25 C21 -36.9(4) . . . . ? C23 Rh2 C25 C21 -79.2(5) . . . . ? C52 Rh2 C25 C24 -139.0(4) . . . . ? N42 Rh2 C25 C24 -58.9(5) . . . . ? N4 Rh2 C25 C24 108.0(6) . . . . ? C21 Rh2 C25 C24 116.6(6) . . . . ? C22 Rh2 C25 C24 79.6(5) . . . . ? C23 Rh2 C25 C24 37.4(4) . . . . ? C52 Rh2 C25 C30 -19.9(7) . . . . ? N42 Rh2 C25 C30 60.2(8) . . . . ? N4 Rh2 C25 C30 -132.9(7) . . . . ? C21 Rh2 C25 C30 -124.3(9) . . . . ? C24 Rh2 C25 C30 119.1(9) . . . . ? C22 Rh2 C25 C30 -161.3(8) . . . . ? C23 Rh2 C25 C30 156.5(8) . . . . ? C35 N31 C31 C32 -3.6(12) . . . . ? Rh1 N31 C31 C32 179.9(7) . . . . ? N31 C31 C32 C33 3.2(14) . . . . ? C31 C32 C33 C34 -1.1(15) . . . . ? C32 C33 C34 C35 -0.6(15) . . . . ? C31 N31 C35 C34 1.8(11) . . . . ? Rh1 N31 C35 C34 178.6(6) . . . . ? C31 N31 C35 C36 -179.3(7) . . . . ? Rh1 N31 C35 C36 -2.5(8) . . . . ? C33 C34 C35 N31 0.3(13) . . . . ? C33 C34 C35 C36 -178.5(8) . . . . ? N31 C35 C36 C41 5.3(10) . . . . ? C34 C35 C36 C41 -175.9(8) . . . . ? N31 C35 C36 C37 -179.3(7) . . . . ? C34 C35 C36 C37 -0.5(13) . . . . ? C41 C36 C37 C38 -3.6(12) . . . . ? C35 C36 C37 C38 -178.7(8) . . . . ? C36 C37 C38 C39 3.5(14) . . . . ? C37 C38 C39 C40 -2.4(15) . . . . ? C38 C39 C40 C41 1.3(13) . . . . ? C39 C40 C41 C36 -1.4(12) . . . . ? C39 C40 C41 Rh1 -177.2(6) . . . . ? C37 C36 C41 C40 2.5(11) . . . . ? C35 C36 C41 C40 178.0(7) . . . . ? C37 C36 C41 Rh1 178.8(6) . . . . ? C35 C36 C41 Rh1 -5.6(9) . . . . ? N31 Rh1 C41 C40 179.3(7) . . . . ? N1 Rh1 C41 C40 -95.8(7) . . . . ? C12 Rh1 C41 C40 67.1(7) . . . . ? C15 Rh1 C41 C40 2.7(8) . . . . ? C13 Rh1 C41 C40 90.4(7) . . . . ? C11 Rh1 C41 C40 28.5(7) . . . . ? C14 Rh1 C41 C40 42.2(14) . . . . ? N31 Rh1 C41 C36 3.3(5) . . . . ? N1 Rh1 C41 C36 88.2(6) . . . . ? C12 Rh1 C41 C36 -108.9(6) . . . . ? C15 Rh1 C41 C36 -173.3(5) . . . . ? C13 Rh1 C41 C36 -85.6(7) . . . . ? C11 Rh1 C41 C36 -147.5(5) . . . . ? C14 Rh1 C41 C36 -133.8(10) . . . . ? C46 N42 C42 C43 0.6(11) . . . . ? Rh2 N42 C42 C43 -177.9(6) . . . . ? N42 C42 C43 C44 -1.7(12) . . . . ? C42 C43 C44 C45 1.5(12) . . . . ? C43 C44 C45 C46 -0.4(12) . . . . ? C42 N42 C46 C45 0.6(10) . . . . ? Rh2 N42 C46 C45 179.2(5) . . . . ? C42 N42 C46 C47 179.3(6) . . . . ? Rh2 N42 C46 C47 -2.1(8) . . . . ? C44 C45 C46 N42 -0.7(11) . . . . ? C44 C45 C46 C47 -179.3(7) . . . . ? N42 C46 C47 C52 -3.3(9) . . . . ? C45 C46 C47 C52 175.3(7) . . . . ? N42 C46 C47 C48 178.7(7) . . . . ? C45 C46 C47 C48 -2.7(11) . . . . ? C52 C47 C48 C49 -0.4(11) . . . . ? C46 C47 C48 C49 177.6(7) . . . . ? C47 C48 C49 C50 -0.6(12) . . . . ? C48 C49 C50 C51 0.2(13) . . . . ? C49 C50 C51 C52 1.2(12) . . . . ? C48 C47 C52 C51 1.7(10) . . . . ? C46 C47 C52 C51 -176.5(6) . . . . ? C48 C47 C52 Rh2 -174.8(5) . . . . ? C46 C47 C52 Rh2 7.1(8) . . . . ? C50 C51 C52 C47 -2.1(11) . . . . ? C50 C51 C52 Rh2 173.9(6) . . . . ? N42 Rh2 C52 C47 -6.2(5) . . . . ? N4 Rh2 C52 C47 -91.6(5) . . . . ? C25 Rh2 C52 C47 112.3(5) . . . . ? C21 Rh2 C52 C47 150.5(5) . . . . ? C24 Rh2 C52 C47 82.8(6) . . . . ? C22 Rh2 C52 C47 168.3(5) . . . . ? C23 Rh2 C52 C47 102.9(8) . . . . ? N42 Rh2 C52 C51 177.7(7) . . . . ? N4 Rh2 C52 C51 92.4(7) . . . . ? C25 Rh2 C52 C51 -63.8(7) . . . . ? C21 Rh2 C52 C51 -25.6(7) . . . . ? C24 Rh2 C52 C51 -93.3(7) . . . . ? C22 Rh2 C52 C51 -7.7(9) . . . . ? C23 Rh2 C52 C51 -73.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.452 _refine_diff_density_min -1.588 _refine_diff_density_rms 0.195 _database_code_depnum_ccdc_archive 'CCDC 945551' ####################################################################### # # 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_comp8CH2Cl2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H49 N6 Rh2 1+, F6 P 1-, C H2 Cl2, C4 H10 O' _chemical_formula_sum 'C49 H61 Cl2 F6 N6 O P Rh2' _chemical_formula_weight 1171.73 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.8507(12) _cell_length_b 14.1135(12) _cell_length_c 14.1254(12) _cell_angle_alpha 114.573(2) _cell_angle_beta 96.515(3) _cell_angle_gamma 95.075(3) _cell_volume 2466.7(4) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 18468 _cell_measurement_theta_min 3.1 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1196 _exptl_absorpt_coefficient_mu 0.876 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7790 _exptl_absorpt_correction_T_max 0.8442 _exptl_absorpt_process_details NUMABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24373 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0331 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11230 _reflns_number_gt 9533 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+7.5883P] 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 11230 _refine_ls_number_parameters 579 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1291 _refine_ls_wR_factor_gt 0.1210 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.18587(2) 0.34666(2) 0.41037(2) 0.01972(8) Uani 1 1 d . . . Rh2 Rh 0.275798(19) 0.56391(2) 0.88309(2) 0.01876(8) Uani 1 1 d . . . Cl2 Cl 0.5582(6) -0.0270(6) 0.8322(10) 0.519(11) Uani 1 1 d . . . Cl1 Cl 0.4910(4) 0.0452(4) 0.6726(5) 0.229(2) Uani 1 1 d . . . P1 P 0.19287(10) 0.06657(10) 0.84488(11) 0.0425(3) Uani 1 1 d . . . F1 F 0.1543(4) 0.1722(4) 0.8579(6) 0.131(2) Uani 1 1 d . . . F2 F 0.2535(3) 0.0765(4) 0.7593(4) 0.0869(13) Uani 1 1 d . . . F3 F 0.1026(4) 0.0046(4) 0.7552(4) 0.1116(19) Uani 1 1 d . . . F4 F 0.2317(4) -0.0399(3) 0.8268(4) 0.0929(14) Uani 1 1 d . . . F5 F 0.1318(3) 0.0563(4) 0.9287(4) 0.0874(13) Uani 1 1 d . . . F6 F 0.2841(3) 0.1273(5) 0.9311(4) 0.1144(19) Uani 1 1 d . . . O1 O 0.8084(7) 0.1308(7) 0.6053(8) 0.154(3) Uiso 1 1 d D . . N1 N 0.2572(2) 0.5670(3) 0.5815(2) 0.0254(7) Uani 1 1 d . . . N2 N 0.2162(2) 0.4696(2) 0.5624(2) 0.0215(6) Uani 1 1 d . . . N3 N 0.2102(2) 0.4591(2) 0.6495(2) 0.0215(6) Uani 1 1 d . . . N4 N 0.2483(2) 0.5535(2) 0.7301(2) 0.0206(6) Uani 1 1 d . . . N31 N 0.1510(2) 0.2442(3) 0.4776(2) 0.0257(7) Uani 1 1 d . . . N42 N 0.2007(3) 0.6921(3) 0.9419(3) 0.0293(7) Uani 1 1 d . . . C1 C 0.8714(7) 0.0552(8) 0.7055(8) 0.099(3) Uiso 1 1 d D . . C2 C 0.7681(10) 0.0878(12) 0.6791(12) 0.164(5) Uiso 1 1 d D . . C3 C 0.7358(10) 0.1651(11) 0.5657(10) 0.144(4) Uiso 1 1 d D . . C4 C 0.7713(9) 0.1882(10) 0.4722(10) 0.131(4) Uiso 1 1 d D . . C5 C 0.2761(3) 0.6169(3) 0.6862(3) 0.0232(7) Uani 1 1 d . . . C6 C 0.3245(3) 0.7282(3) 0.7454(3) 0.0336(9) Uani 1 1 d . . . H6A H 0.3628 0.7375 0.8123 0.040 Uiso 1 1 calc R . . H6B H 0.2744 0.7749 0.7598 0.040 Uiso 1 1 calc R . . H6C H 0.3684 0.7456 0.7033 0.040 Uiso 1 1 calc R . . C7 C 0.4613(13) -0.0280(11) 0.7398(19) 0.219(9) Uani 1 1 d . . . C11 C 0.0925(3) 0.4249(3) 0.3321(3) 0.0250(8) Uani 1 1 d . . . C12 C 0.1920(3) 0.4243(3) 0.3073(3) 0.0240(7) Uani 1 1 d . . . C13 C 0.2042(3) 0.3172(3) 0.2491(3) 0.0270(8) Uani 1 1 d . . . C14 C 0.1183(3) 0.2525(3) 0.2474(3) 0.0277(8) Uani 1 1 d . . . C15 C 0.0473(3) 0.3206(3) 0.2947(3) 0.0263(8) Uani 1 1 d . . . C16 C 0.0493(3) 0.5234(3) 0.3870(3) 0.0327(9) Uani 1 1 d . . . H16A H 0.0988 0.5760 0.4442 0.039 Uiso 1 1 calc R . . H16B H -0.0074 0.5072 0.4164 0.039 Uiso 1 1 calc R . . H16C H 0.0280 0.5513 0.3364 0.039 Uiso 1 1 calc R . . C17 C 0.2608(3) 0.5216(3) 0.3267(3) 0.0318(9) Uani 1 1 d . . . H17A H 0.2623 0.5751 0.3988 0.038 Uiso 1 1 calc R . . H17B H 0.2378 0.5492 0.2763 0.038 Uiso 1 1 calc R . . H17C H 0.3270 0.5039 0.3175 0.038 Uiso 1 1 calc R . . C18 C 0.2891(3) 0.2772(4) 0.1961(3) 0.0357(10) Uani 1 1 d . . . H18A H 0.3459 0.3333 0.2246 0.043 Uiso 1 1 calc R . . H18B H 0.2715 0.2551 0.1200 0.043 Uiso 1 1 calc R . . H18C H 0.3057 0.2170 0.2089 0.043 Uiso 1 1 calc R . . C19 C 0.0979(4) 0.1343(4) 0.1923(4) 0.0409(11) Uani 1 1 d . . . H19A H 0.0513 0.1082 0.2263 0.049 Uiso 1 1 calc R . . H19B H 0.1594 0.1058 0.1966 0.049 Uiso 1 1 calc R . . H19C H 0.0699 0.1119 0.1180 0.049 Uiso 1 1 calc R . . C20 C -0.0570(3) 0.2833(4) 0.2957(3) 0.0345(9) Uani 1 1 d . . . H20A H -0.0615 0.2145 0.2976 0.041 Uiso 1 1 calc R . . H20B H -0.0988 0.2770 0.2319 0.041 Uiso 1 1 calc R . . H20C H -0.0791 0.3341 0.3581 0.041 Uiso 1 1 calc R . . C21 C 0.3762(3) 0.6005(3) 1.0277(3) 0.0256(8) Uani 1 1 d . . . C22 C 0.4325(3) 0.6239(3) 0.9584(3) 0.0270(8) Uani 1 1 d . . . C23 C 0.4276(3) 0.5281(3) 0.8665(3) 0.0264(8) Uani 1 1 d . . . C24 C 0.3708(3) 0.4451(3) 0.8778(3) 0.0248(8) Uani 1 1 d . . . C25 C 0.3401(3) 0.4912(3) 0.9796(3) 0.0232(7) Uani 1 1 d . . . C26 C 0.3644(3) 0.6777(4) 1.1364(3) 0.0371(10) Uani 1 1 d . . . H26A H 0.3634 0.7477 1.1381 0.044 Uiso 1 1 calc R . . H26B H 0.4195 0.6806 1.1881 0.044 Uiso 1 1 calc R . . H26C H 0.3026 0.6549 1.1537 0.044 Uiso 1 1 calc R . . C27 C 0.4937(3) 0.7273(4) 0.9842(4) 0.0400(11) Uani 1 1 d . . . H27A H 0.4624 0.7850 1.0302 0.048 Uiso 1 1 calc R . . H27B H 0.4994 0.7344 0.9189 0.048 Uiso 1 1 calc R . . H27C H 0.5593 0.7299 1.0204 0.048 Uiso 1 1 calc R . . C28 C 0.4731(3) 0.5136(4) 0.7702(4) 0.0360(10) Uani 1 1 d . . . H28A H 0.4798 0.5800 0.7633 0.043 Uiso 1 1 calc R . . H28B H 0.4310 0.4587 0.7073 0.043 Uiso 1 1 calc R . . H28C H 0.5382 0.4926 0.7776 0.043 Uiso 1 1 calc R . . C29 C 0.3544(3) 0.3311(3) 0.8019(4) 0.0362(10) Uani 1 1 d . . . H29A H 0.3020 0.2933 0.8197 0.043 Uiso 1 1 calc R . . H29B H 0.4152 0.3013 0.8062 0.043 Uiso 1 1 calc R . . H29C H 0.3353 0.3240 0.7300 0.043 Uiso 1 1 calc R . . C30 C 0.2842(3) 0.4310(4) 1.0274(3) 0.0325(9) Uani 1 1 d . . . H30A H 0.2387 0.3721 0.9715 0.039 Uiso 1 1 calc R . . H30B H 0.2471 0.4779 1.0778 0.039 Uiso 1 1 calc R . . H30C H 0.3305 0.4038 1.0641 0.039 Uiso 1 1 calc R . . C31 C 0.0606(3) 0.2172(3) 0.4923(3) 0.0329(9) Uani 1 1 d . . . H31 H 0.0075 0.2446 0.4687 0.040 Uiso 1 1 calc R . . C32 C 0.0410(4) 0.1520(4) 0.5395(4) 0.0409(11) Uani 1 1 d . . . H32 H -0.0243 0.1343 0.5479 0.049 Uiso 1 1 calc R . . C33 C 0.1177(4) 0.1125(4) 0.5749(4) 0.0452(12) Uani 1 1 d . . . H33 H 0.1062 0.0673 0.6082 0.054 Uiso 1 1 calc R . . C34 C 0.2113(4) 0.1397(4) 0.5611(4) 0.0391(10) Uani 1 1 d . . . H34 H 0.2650 0.1135 0.5851 0.047 Uiso 1 1 calc R . . C35 C 0.2270(3) 0.2054(3) 0.5121(3) 0.0282(8) Uani 1 1 d . . . C36 C 0.3227(3) 0.2449(3) 0.4960(3) 0.0316(9) Uani 1 1 d . . . C37 C 0.4121(4) 0.2184(4) 0.5278(4) 0.0419(11) Uani 1 1 d . . . H37 H 0.4124 0.1688 0.5573 0.050 Uiso 1 1 calc R . . C38 C 0.4989(4) 0.2639(5) 0.5164(4) 0.0498(13) Uani 1 1 d . . . H38 H 0.5593 0.2453 0.5371 0.060 Uiso 1 1 calc R . . C39 C 0.4986(3) 0.3371(4) 0.4749(4) 0.0426(11) Uani 1 1 d . . . H39 H 0.5591 0.3695 0.4684 0.051 Uiso 1 1 calc R . . C40 C 0.4103(3) 0.3635(4) 0.4424(3) 0.0349(9) Uani 1 1 d . . . H40 H 0.4110 0.4140 0.4142 0.042 Uiso 1 1 calc R . . C41 C 0.3216(3) 0.3168(3) 0.4511(3) 0.0268(8) Uani 1 1 d . . . C42 C 0.2402(3) 0.7951(3) 0.9814(3) 0.0320(9) Uani 1 1 d . . . H42 H 0.3084 0.8128 0.9830 0.038 Uiso 1 1 calc R . . C43 C 0.1843(4) 0.8748(4) 1.0193(4) 0.0447(12) Uani 1 1 d . . . H43 H 0.2138 0.9462 1.0454 0.054 Uiso 1 1 calc R . . C44 C 0.0859(4) 0.8513(4) 1.0195(4) 0.0454(12) Uani 1 1 d . . . H44 H 0.0473 0.9061 1.0464 0.054 Uiso 1 1 calc R . . C45 C 0.0439(4) 0.7466(4) 0.9800(4) 0.0416(11) Uani 1 1 d . . . H45 H -0.0240 0.7290 0.9799 0.050 Uiso 1 1 calc R . . C46 C 0.1019(3) 0.6670(3) 0.9402(3) 0.0286(8) Uani 1 1 d . . . C47 C 0.0648(3) 0.5546(3) 0.8946(3) 0.0272(8) Uani 1 1 d . . . C48 C -0.0316(3) 0.5129(4) 0.8862(3) 0.0362(10) Uani 1 1 d . . . H48 H -0.0791 0.5583 0.9102 0.043 Uiso 1 1 calc R . . C49 C -0.0583(3) 0.4055(4) 0.8428(4) 0.0424(11) Uani 1 1 d . . . H49 H -0.1239 0.3764 0.8392 0.051 Uiso 1 1 calc R . . C50 C 0.0102(3) 0.3394(4) 0.8043(4) 0.0390(10) Uani 1 1 d . . . H50 H -0.0084 0.2651 0.7735 0.047 Uiso 1 1 calc R . . C51 C 0.1059(3) 0.3824(3) 0.8111(3) 0.0303(8) Uani 1 1 d . . . H51 H 0.1525 0.3372 0.7829 0.036 Uiso 1 1 calc R . . C52 C 0.1346(2) 0.4896(3) 0.8581(3) 0.0193(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01821(14) 0.02286(15) 0.01768(14) 0.00824(11) 0.00388(10) 0.00241(10) Rh2 0.01536(14) 0.02267(14) 0.01773(14) 0.00822(11) 0.00309(10) 0.00217(10) Cl2 0.269(8) 0.212(6) 0.75(2) -0.036(9) -0.266(11) 0.098(6) Cl1 0.231(5) 0.147(4) 0.297(7) 0.086(4) 0.055(5) 0.001(3) P1 0.0473(7) 0.0345(6) 0.0452(7) 0.0191(6) 0.0040(6) -0.0023(5) F1 0.110(4) 0.074(3) 0.249(7) 0.094(4) 0.065(4) 0.044(3) F2 0.083(3) 0.116(4) 0.089(3) 0.070(3) 0.027(2) 0.003(3) F3 0.093(3) 0.141(4) 0.093(3) 0.069(3) -0.035(3) -0.051(3) F4 0.124(4) 0.063(2) 0.119(4) 0.053(3) 0.054(3) 0.038(2) F5 0.077(3) 0.132(4) 0.090(3) 0.073(3) 0.042(2) 0.036(3) F6 0.067(3) 0.150(5) 0.067(3) 0.004(3) -0.014(2) -0.025(3) N1 0.0272(16) 0.0267(16) 0.0222(15) 0.0104(13) 0.0052(13) 0.0027(13) N2 0.0222(15) 0.0229(15) 0.0197(14) 0.0089(12) 0.0064(12) 0.0028(12) N3 0.0198(14) 0.0239(15) 0.0181(14) 0.0061(12) 0.0034(12) 0.0035(12) N4 0.0185(14) 0.0223(14) 0.0197(14) 0.0080(12) 0.0029(12) 0.0023(12) N31 0.0299(17) 0.0251(16) 0.0199(15) 0.0077(13) 0.0039(13) 0.0029(13) N42 0.0305(18) 0.0330(18) 0.0211(16) 0.0086(14) 0.0041(14) 0.0046(14) C5 0.0205(17) 0.0247(18) 0.0236(18) 0.0098(15) 0.0038(14) 0.0024(14) C6 0.042(2) 0.0262(19) 0.029(2) 0.0100(17) 0.0063(18) -0.0040(17) C7 0.197(17) 0.106(10) 0.36(3) 0.103(14) 0.103(18) -0.003(10) C11 0.0259(19) 0.033(2) 0.0176(17) 0.0126(16) 0.0023(14) 0.0066(16) C12 0.0250(18) 0.0295(19) 0.0177(17) 0.0107(15) 0.0028(14) 0.0032(15) C13 0.0265(19) 0.037(2) 0.0181(17) 0.0118(16) 0.0062(15) 0.0047(16) C14 0.0270(19) 0.032(2) 0.0193(18) 0.0084(16) 0.0017(15) -0.0009(16) C15 0.0229(18) 0.035(2) 0.0177(17) 0.0096(16) 0.0001(14) 0.0005(15) C16 0.035(2) 0.039(2) 0.028(2) 0.0150(18) 0.0086(17) 0.0142(18) C17 0.035(2) 0.035(2) 0.031(2) 0.0194(18) 0.0092(17) 0.0005(17) C18 0.037(2) 0.043(2) 0.026(2) 0.0107(19) 0.0135(18) 0.0102(19) C19 0.046(3) 0.032(2) 0.032(2) 0.0025(19) 0.004(2) 0.0010(19) C20 0.024(2) 0.047(3) 0.030(2) 0.0159(19) 0.0017(17) -0.0006(18) C21 0.0200(17) 0.033(2) 0.0200(17) 0.0087(16) -0.0018(14) 0.0038(15) C22 0.0167(17) 0.031(2) 0.033(2) 0.0144(17) 0.0033(15) 0.0049(15) C23 0.0148(16) 0.039(2) 0.0274(19) 0.0150(17) 0.0060(14) 0.0056(15) C24 0.0210(17) 0.0297(19) 0.0224(18) 0.0096(16) 0.0056(14) 0.0042(15) C25 0.0193(17) 0.0314(19) 0.0218(17) 0.0145(16) 0.0008(14) 0.0060(15) C26 0.031(2) 0.045(2) 0.023(2) 0.0047(19) 0.0009(17) 0.0065(19) C27 0.025(2) 0.035(2) 0.054(3) 0.018(2) 0.000(2) -0.0051(18) C28 0.027(2) 0.052(3) 0.036(2) 0.022(2) 0.0140(18) 0.0095(19) C29 0.031(2) 0.035(2) 0.036(2) 0.0083(19) 0.0089(18) 0.0059(18) C30 0.029(2) 0.046(2) 0.030(2) 0.0232(19) 0.0079(17) 0.0070(18) C31 0.033(2) 0.036(2) 0.030(2) 0.0157(18) 0.0052(17) -0.0010(17) C32 0.043(3) 0.042(2) 0.035(2) 0.017(2) 0.007(2) -0.011(2) C33 0.064(3) 0.034(2) 0.037(2) 0.020(2) 0.000(2) -0.009(2) C34 0.051(3) 0.032(2) 0.032(2) 0.0149(19) -0.003(2) 0.002(2) C35 0.037(2) 0.0215(17) 0.0216(18) 0.0070(15) -0.0019(16) 0.0021(16) C36 0.033(2) 0.029(2) 0.026(2) 0.0051(17) 0.0033(17) 0.0078(17) C37 0.042(3) 0.041(2) 0.040(3) 0.014(2) 0.000(2) 0.018(2) C38 0.030(2) 0.063(3) 0.049(3) 0.016(3) 0.001(2) 0.022(2) C39 0.023(2) 0.059(3) 0.037(2) 0.011(2) 0.0054(18) 0.009(2) C40 0.024(2) 0.045(2) 0.029(2) 0.0106(19) 0.0056(17) 0.0038(18) C41 0.0248(19) 0.0310(19) 0.0213(18) 0.0072(16) 0.0046(15) 0.0069(15) C42 0.033(2) 0.029(2) 0.030(2) 0.0087(17) 0.0055(17) 0.0042(17) C43 0.051(3) 0.032(2) 0.041(3) 0.005(2) 0.007(2) 0.013(2) C44 0.047(3) 0.042(3) 0.040(3) 0.007(2) 0.010(2) 0.024(2) C45 0.032(2) 0.058(3) 0.034(2) 0.015(2) 0.0111(19) 0.019(2) C46 0.0252(19) 0.042(2) 0.0202(18) 0.0130(17) 0.0077(15) 0.0097(17) C47 0.0198(18) 0.046(2) 0.0221(18) 0.0191(17) 0.0054(14) 0.0082(16) C48 0.0220(19) 0.056(3) 0.033(2) 0.021(2) 0.0087(17) 0.0052(19) C49 0.023(2) 0.070(3) 0.042(3) 0.034(3) 0.0056(18) -0.004(2) C50 0.033(2) 0.042(2) 0.044(3) 0.026(2) -0.001(2) -0.0091(19) C51 0.0250(19) 0.032(2) 0.034(2) 0.0157(18) 0.0012(17) 0.0003(16) C52 0.0158(16) 0.0274(17) 0.0193(16) 0.0146(14) 0.0034(13) 0.0019(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 Rh1 C41 2.035(4) . ? Rh1 N31 2.086(3) . ? Rh1 N2 2.090(3) . ? Rh1 C12 2.160(4) . ? Rh1 C14 2.166(4) . ? Rh1 C13 2.189(4) . ? Rh1 C11 2.249(4) . ? Rh1 C15 2.270(4) . ? Rh2 C52 2.055(3) . ? Rh2 N42 2.079(3) . ? Rh2 N4 2.092(3) . ? Rh2 C21 2.173(4) . ? Rh2 C25 2.180(4) . ? Rh2 C24 2.204(4) . ? Rh2 C23 2.221(4) . ? Rh2 C22 2.227(4) . ? Cl2 C7 1.76(2) . ? Cl1 C7 1.722(18) . ? P1 F6 1.551(4) . ? P1 F3 1.568(4) . ? P1 F4 1.570(4) . ? P1 F1 1.574(4) . ? P1 F5 1.577(4) . ? P1 F2 1.592(4) . ? O1 C3 1.320(12) . ? O1 C2 1.537(13) . ? N1 C5 1.327(5) . ? N1 N2 1.342(4) . ? N2 N3 1.310(4) . ? N3 N4 1.352(4) . ? N4 C5 1.337(5) . ? N31 C31 1.341(5) . ? N31 C35 1.361(5) . ? N42 C42 1.357(5) . ? N42 C46 1.378(5) . ? C1 C2 1.592(13) . ? C3 C4 1.604(13) . ? C5 C6 1.488(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C15 1.398(6) . ? C11 C12 1.460(5) . ? C11 C16 1.500(5) . ? C12 C13 1.426(6) . ? C12 C17 1.504(5) . ? C13 C14 1.427(6) . ? C13 C18 1.492(6) . ? C14 C15 1.454(6) . ? C14 C19 1.502(6) . ? C15 C20 1.497(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C25 1.417(5) . ? C21 C22 1.440(6) . ? C21 C26 1.506(5) . ? C22 C23 1.422(6) . ? C22 C27 1.499(6) . ? C23 C24 1.427(6) . ? C23 C28 1.509(5) . ? C24 C25 1.443(5) . ? C24 C29 1.495(6) . ? C25 C30 1.501(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.369(6) . ? C31 H31 0.9500 . ? C32 C33 1.381(7) . ? C32 H32 0.9500 . ? C33 C34 1.377(7) . ? C33 H33 0.9500 . ? C34 C35 1.385(6) . ? C34 H34 0.9500 . ? C35 C36 1.470(6) . ? C36 C37 1.404(6) . ? C36 C41 1.405(6) . ? C37 C38 1.371(8) . ? C37 H37 0.9500 . ? C38 C39 1.384(8) . ? C38 H38 0.9500 . ? C39 C40 1.393(6) . ? C39 H39 0.9500 . ? C40 C41 1.384(6) . ? C40 H40 0.9500 . ? C42 C43 1.378(6) . ? C42 H42 0.9500 . ? C43 C44 1.374(7) . ? C43 H43 0.9500 . ? C44 C45 1.387(7) . ? C44 H44 0.9500 . ? C45 C46 1.400(6) . ? C45 H45 0.9500 . ? C46 C47 1.459(6) . ? C47 C48 1.382(6) . ? C47 C52 1.384(5) . ? C48 C49 1.375(7) . ? C48 H48 0.9500 . ? C49 C50 1.384(7) . ? C49 H49 0.9500 . ? C50 C51 1.384(6) . ? C50 H50 0.9500 . ? C51 C52 1.373(5) . ? C51 H51 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 C41 Rh1 N31 78.99(15) . . ? C41 Rh1 N2 83.29(14) . . ? N31 Rh1 N2 88.25(12) . . ? C41 Rh1 C12 110.35(16) . . ? N31 Rh1 C12 164.85(14) . . ? N2 Rh1 C12 104.37(13) . . ? C41 Rh1 C14 115.15(15) . . ? N31 Rh1 C14 101.18(14) . . ? N2 Rh1 C14 160.44(14) . . ? C12 Rh1 C14 64.29(15) . . ? C41 Rh1 C13 95.26(15) . . ? N31 Rh1 C13 131.59(14) . . ? N2 Rh1 C13 139.30(14) . . ? C12 Rh1 C13 38.26(15) . . ? C14 Rh1 C13 38.24(15) . . ? C41 Rh1 C11 148.48(16) . . ? N31 Rh1 C11 132.43(14) . . ? N2 Rh1 C11 98.12(13) . . ? C12 Rh1 C11 38.60(14) . . ? C14 Rh1 C11 62.87(15) . . ? C13 Rh1 C11 63.29(14) . . ? C41 Rh1 C15 153.35(15) . . ? N31 Rh1 C15 103.12(14) . . ? N2 Rh1 C15 123.14(13) . . ? C12 Rh1 C15 63.06(14) . . ? C14 Rh1 C15 38.20(15) . . ? C13 Rh1 C15 63.12(14) . . ? C11 Rh1 C15 36.05(14) . . ? C52 Rh2 N42 78.77(14) . . ? C52 Rh2 N4 88.13(12) . . ? N42 Rh2 N4 92.12(12) . . ? C52 Rh2 C21 120.81(14) . . ? N42 Rh2 C21 97.56(14) . . ? N4 Rh2 C21 150.72(14) . . ? C52 Rh2 C25 95.89(14) . . ? N42 Rh2 C25 123.18(14) . . ? N4 Rh2 C25 144.61(13) . . ? C21 Rh2 C25 37.98(14) . . ? C52 Rh2 C24 105.37(14) . . ? N42 Rh2 C24 160.75(14) . . ? N4 Rh2 C24 106.68(13) . . ? C21 Rh2 C24 63.96(14) . . ? C25 Rh2 C24 38.43(13) . . ? C52 Rh2 C23 140.80(15) . . ? N42 Rh2 C23 140.32(15) . . ? N4 Rh2 C23 92.12(13) . . ? C21 Rh2 C23 63.16(14) . . ? C25 Rh2 C23 63.14(14) . . ? C24 Rh2 C23 37.63(14) . . ? C52 Rh2 C22 158.21(14) . . ? N42 Rh2 C22 106.08(14) . . ? N4 Rh2 C22 112.55(14) . . ? C21 Rh2 C22 38.18(15) . . ? C25 Rh2 C22 63.41(15) . . ? C24 Rh2 C22 63.29(14) . . ? C23 Rh2 C22 37.28(15) . . ? F6 P1 F3 178.4(3) . . ? F6 P1 F4 89.5(3) . . ? F3 P1 F4 90.1(3) . . ? F6 P1 F1 91.7(4) . . ? F3 P1 F1 88.7(3) . . ? F4 P1 F1 177.5(3) . . ? F6 P1 F5 91.7(3) . . ? F3 P1 F5 89.9(3) . . ? F4 P1 F5 90.4(2) . . ? F1 P1 F5 91.8(3) . . ? F6 P1 F2 88.9(3) . . ? F3 P1 F2 89.5(3) . . ? F4 P1 F2 89.7(3) . . ? F1 P1 F2 88.1(3) . . ? F5 P1 F2 179.4(2) . . ? C3 O1 C2 107.5(10) . . ? C5 N1 N2 103.7(3) . . ? N3 N2 N1 112.2(3) . . ? N3 N2 Rh1 125.1(2) . . ? N1 N2 Rh1 122.2(2) . . ? N2 N3 N4 106.4(3) . . ? C5 N4 N3 106.4(3) . . ? C5 N4 Rh2 133.7(3) . . ? N3 N4 Rh2 118.7(2) . . ? C31 N31 C35 118.4(4) . . ? C31 N31 Rh1 124.8(3) . . ? C35 N31 Rh1 116.8(3) . . ? C42 N42 C46 118.7(4) . . ? C42 N42 Rh2 126.1(3) . . ? C46 N42 Rh2 115.2(3) . . ? O1 C2 C1 91.6(9) . . ? O1 C3 C4 107.4(11) . . ? N1 C5 N4 111.3(3) . . ? N1 C5 C6 123.6(4) . . ? N4 C5 C6 125.1(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Cl1 C7 Cl2 114.7(10) . . ? C15 C11 C12 108.4(3) . . ? C15 C11 C16 127.7(4) . . ? C12 C11 C16 123.8(4) . . ? C15 C11 Rh1 72.8(2) . . ? C12 C11 Rh1 67.4(2) . . ? C16 C11 Rh1 126.2(3) . . ? C13 C12 C11 107.6(3) . . ? C13 C12 C17 127.6(4) . . ? C11 C12 C17 124.2(4) . . ? C13 C12 Rh1 72.0(2) . . ? C11 C12 Rh1 74.0(2) . . ? C17 C12 Rh1 126.8(3) . . ? C12 C13 C14 107.6(3) . . ? C12 C13 C18 127.5(4) . . ? C14 C13 C18 124.9(4) . . ? C12 C13 Rh1 69.8(2) . . ? C14 C13 Rh1 70.0(2) . . ? C18 C13 Rh1 126.8(3) . . ? C13 C14 C15 108.2(3) . . ? C13 C14 C19 126.0(4) . . ? C15 C14 C19 125.2(4) . . ? C13 C14 Rh1 71.8(2) . . ? C15 C14 Rh1 74.8(2) . . ? C19 C14 Rh1 126.1(3) . . ? C11 C15 C14 107.7(3) . . ? C11 C15 C20 127.0(4) . . ? C14 C15 C20 125.1(4) . . ? C11 C15 Rh1 71.2(2) . . ? C14 C15 Rh1 67.0(2) . . ? C20 C15 Rh1 130.1(3) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 108.4(3) . . ? C25 C21 C26 125.8(4) . . ? C22 C21 C26 125.7(4) . . ? C25 C21 Rh2 71.3(2) . . ? C22 C21 Rh2 72.9(2) . . ? C26 C21 Rh2 125.2(3) . . ? C23 C22 C21 107.1(3) . . ? C23 C22 C27 126.7(4) . . ? C21 C22 C27 125.9(4) . . ? C23 C22 Rh2 71.1(2) . . ? C21 C22 Rh2 68.9(2) . . ? C27 C22 Rh2 130.2(3) . . ? C22 C23 C24 109.4(3) . . ? C22 C23 C28 126.6(4) . . ? C24 C23 C28 124.0(4) . . ? C22 C23 Rh2 71.6(2) . . ? C24 C23 Rh2 70.6(2) . . ? C28 C23 Rh2 123.5(3) . . ? C23 C24 C25 106.8(3) . . ? C23 C24 C29 125.9(4) . . ? C25 C24 C29 127.1(4) . . ? C23 C24 Rh2 71.8(2) . . ? C25 C24 Rh2 69.9(2) . . ? C29 C24 Rh2 127.2(3) . . ? C21 C25 C24 108.3(3) . . ? C21 C25 C30 126.6(4) . . ? C24 C25 C30 125.0(4) . . ? C21 C25 Rh2 70.7(2) . . ? C24 C25 Rh2 71.7(2) . . ? C30 C25 Rh2 125.9(3) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N31 C31 C32 123.1(4) . . ? N31 C31 H31 118.4 . . ? C32 C31 H31 118.4 . . ? C31 C32 C33 118.9(5) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.6 . . ? C34 C33 C32 118.9(4) . . ? C34 C33 H33 120.6 . . ? C32 C33 H33 120.6 . . ? C33 C34 C35 120.0(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? N31 C35 C34 120.8(4) . . ? N31 C35 C36 113.0(4) . . ? C34 C35 C36 126.1(4) . . ? C37 C36 C41 120.3(4) . . ? C37 C36 C35 123.5(4) . . ? C41 C36 C35 116.1(4) . . ? C38 C37 C36 120.0(5) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C37 C38 C39 120.1(4) . . ? C37 C38 H38 119.9 . . ? C39 C38 H38 119.9 . . ? C38 C39 C40 120.4(5) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 120.5(5) . . ? C41 C40 H40 119.8 . . ? C39 C40 H40 119.8 . . ? C40 C41 C36 118.7(4) . . ? C40 C41 Rh1 126.3(3) . . ? C36 C41 Rh1 115.0(3) . . ? N42 C42 C43 121.9(4) . . ? N42 C42 H42 119.1 . . ? C43 C42 H42 119.1 . . ? C44 C43 C42 120.2(5) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.1(4) . . ? C43 C44 H44 120.5 . . ? C45 C44 H44 120.5 . . ? C44 C45 C46 119.6(4) . . ? C44 C45 H45 120.2 . . ? C46 C45 H45 120.2 . . ? N42 C46 C45 120.5(4) . . ? N42 C46 C47 115.3(3) . . ? C45 C46 C47 124.2(4) . . ? C48 C47 C52 121.0(4) . . ? C48 C47 C46 124.4(4) . . ? C52 C47 C46 114.6(3) . . ? C49 C48 C47 119.5(4) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 120.2(4) . . ? C48 C49 H49 119.9 . . ? C50 C49 H49 119.9 . . ? C51 C50 C49 119.4(4) . . ? C51 C50 H50 120.3 . . ? C49 C50 H50 120.3 . . ? C52 C51 C50 121.0(4) . . ? C52 C51 H51 119.5 . . ? C50 C51 H51 119.5 . . ? C51 C52 C47 118.8(4) . . ? C51 C52 Rh2 125.1(3) . . ? C47 C52 Rh2 116.1(3) . . ? 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 N1 N2 N3 -0.2(4) . . . . ? C5 N1 N2 Rh1 -172.0(2) . . . . ? C41 Rh1 N2 N3 -78.0(3) . . . . ? N31 Rh1 N2 N3 1.1(3) . . . . ? C12 Rh1 N2 N3 172.7(3) . . . . ? C14 Rh1 N2 N3 120.7(4) . . . . ? C13 Rh1 N2 N3 -168.3(3) . . . . ? C11 Rh1 N2 N3 133.8(3) . . . . ? C15 Rh1 N2 N3 105.7(3) . . . . ? C41 Rh1 N2 N1 92.7(3) . . . . ? N31 Rh1 N2 N1 171.8(3) . . . . ? C12 Rh1 N2 N1 -16.6(3) . . . . ? C14 Rh1 N2 N1 -68.6(5) . . . . ? C13 Rh1 N2 N1 2.5(4) . . . . ? C11 Rh1 N2 N1 -55.5(3) . . . . ? C15 Rh1 N2 N1 -83.6(3) . . . . ? N1 N2 N3 N4 0.3(4) . . . . ? Rh1 N2 N3 N4 171.8(2) . . . . ? N2 N3 N4 C5 -0.3(4) . . . . ? N2 N3 N4 Rh2 -169.3(2) . . . . ? C52 Rh2 N4 C5 143.9(4) . . . . ? N42 Rh2 N4 C5 65.2(4) . . . . ? C21 Rh2 N4 C5 -44.4(5) . . . . ? C25 Rh2 N4 C5 -118.6(4) . . . . ? C24 Rh2 N4 C5 -110.6(3) . . . . ? C23 Rh2 N4 C5 -75.3(4) . . . . ? C22 Rh2 N4 C5 -43.2(4) . . . . ? C52 Rh2 N4 N3 -50.7(3) . . . . ? N42 Rh2 N4 N3 -129.4(3) . . . . ? C21 Rh2 N4 N3 121.0(3) . . . . ? C25 Rh2 N4 N3 46.8(4) . . . . ? C24 Rh2 N4 N3 54.8(3) . . . . ? C23 Rh2 N4 N3 90.1(3) . . . . ? C22 Rh2 N4 N3 122.2(3) . . . . ? C41 Rh1 N31 C31 176.0(3) . . . . ? N2 Rh1 N31 C31 92.5(3) . . . . ? C12 Rh1 N31 C31 -54.4(7) . . . . ? C14 Rh1 N31 C31 -70.2(3) . . . . ? C13 Rh1 N31 C31 -96.7(4) . . . . ? C11 Rh1 N31 C31 -6.9(4) . . . . ? C15 Rh1 N31 C31 -31.2(3) . . . . ? C41 Rh1 N31 C35 -1.6(3) . . . . ? N2 Rh1 N31 C35 -85.1(3) . . . . ? C12 Rh1 N31 C35 128.0(5) . . . . ? C14 Rh1 N31 C35 112.1(3) . . . . ? C13 Rh1 N31 C35 85.6(3) . . . . ? C11 Rh1 N31 C35 175.4(2) . . . . ? C15 Rh1 N31 C35 151.2(3) . . . . ? C52 Rh2 N42 C42 -178.0(4) . . . . ? N4 Rh2 N42 C42 -90.3(3) . . . . ? C21 Rh2 N42 C42 62.0(4) . . . . ? C25 Rh2 N42 C42 92.3(4) . . . . ? C24 Rh2 N42 C42 77.5(6) . . . . ? C23 Rh2 N42 C42 5.6(4) . . . . ? C22 Rh2 N42 C42 23.9(4) . . . . ? C52 Rh2 N42 C46 2.7(3) . . . . ? N4 Rh2 N42 C46 90.3(3) . . . . ? C21 Rh2 N42 C46 -117.4(3) . . . . ? C25 Rh2 N42 C46 -87.1(3) . . . . ? C24 Rh2 N42 C46 -101.9(5) . . . . ? C23 Rh2 N42 C46 -173.8(3) . . . . ? C22 Rh2 N42 C46 -155.5(3) . . . . ? C3 O1 C2 C1 179.0(10) . . . . ? C2 O1 C3 C4 -168.9(10) . . . . ? N2 N1 C5 N4 0.1(4) . . . . ? N2 N1 C5 C6 178.6(4) . . . . ? N3 N4 C5 N1 0.1(4) . . . . ? Rh2 N4 C5 N1 166.8(3) . . . . ? N3 N4 C5 C6 -178.4(4) . . . . ? Rh2 N4 C5 C6 -11.7(6) . . . . ? C41 Rh1 C11 C15 131.7(3) . . . . ? N31 Rh1 C11 C15 -42.9(3) . . . . ? N2 Rh1 C11 C15 -137.9(2) . . . . ? C12 Rh1 C11 C15 119.2(3) . . . . ? C14 Rh1 C11 C15 37.2(2) . . . . ? C13 Rh1 C11 C15 80.3(2) . . . . ? C41 Rh1 C11 C12 12.5(4) . . . . ? N31 Rh1 C11 C12 -162.0(2) . . . . ? N2 Rh1 C11 C12 102.9(2) . . . . ? C14 Rh1 C11 C12 -82.0(2) . . . . ? C13 Rh1 C11 C12 -38.9(2) . . . . ? C15 Rh1 C11 C12 -119.2(3) . . . . ? C41 Rh1 C11 C16 -103.8(4) . . . . ? N31 Rh1 C11 C16 81.7(4) . . . . ? N2 Rh1 C11 C16 -13.4(4) . . . . ? C12 Rh1 C11 C16 -116.3(4) . . . . ? C14 Rh1 C11 C16 161.7(4) . . . . ? C13 Rh1 C11 C16 -155.2(4) . . . . ? C15 Rh1 C11 C16 124.5(5) . . . . ? C15 C11 C12 C13 3.0(4) . . . . ? C16 C11 C12 C13 -176.0(3) . . . . ? Rh1 C11 C12 C13 64.6(3) . . . . ? C15 C11 C12 C17 174.5(3) . . . . ? C16 C11 C12 C17 -4.6(6) . . . . ? Rh1 C11 C12 C17 -123.9(4) . . . . ? C15 C11 C12 Rh1 -61.5(3) . . . . ? C16 C11 C12 Rh1 119.4(4) . . . . ? C41 Rh1 C12 C13 71.8(3) . . . . ? N31 Rh1 C12 C13 -54.4(6) . . . . ? N2 Rh1 C12 C13 159.9(2) . . . . ? C14 Rh1 C12 C13 -37.1(2) . . . . ? C11 Rh1 C12 C13 -115.1(3) . . . . ? C15 Rh1 C12 C13 -79.9(2) . . . . ? C41 Rh1 C12 C11 -173.1(2) . . . . ? N31 Rh1 C12 C11 60.7(6) . . . . ? N2 Rh1 C12 C11 -85.0(2) . . . . ? C14 Rh1 C12 C11 78.0(2) . . . . ? C13 Rh1 C12 C11 115.1(3) . . . . ? C15 Rh1 C12 C11 35.2(2) . . . . ? C41 Rh1 C12 C17 -52.0(4) . . . . ? N31 Rh1 C12 C17 -178.3(4) . . . . ? N2 Rh1 C12 C17 36.0(4) . . . . ? C14 Rh1 C12 C17 -161.0(4) . . . . ? C13 Rh1 C12 C17 -123.8(4) . . . . ? C11 Rh1 C12 C17 121.0(4) . . . . ? C15 Rh1 C12 C17 156.2(4) . . . . ? C11 C12 C13 C14 -5.9(4) . . . . ? C17 C12 C13 C14 -177.0(4) . . . . ? Rh1 C12 C13 C14 60.0(3) . . . . ? C11 C12 C13 C18 172.6(4) . . . . ? C17 C12 C13 C18 1.5(7) . . . . ? Rh1 C12 C13 C18 -121.4(4) . . . . ? C11 C12 C13 Rh1 -65.9(2) . . . . ? C17 C12 C13 Rh1 123.0(4) . . . . ? C41 Rh1 C13 C12 -116.6(2) . . . . ? N31 Rh1 C13 C12 163.5(2) . . . . ? N2 Rh1 C13 C12 -30.8(3) . . . . ? C14 Rh1 C13 C12 118.5(3) . . . . ? C11 Rh1 C13 C12 39.2(2) . . . . ? C15 Rh1 C13 C12 79.8(2) . . . . ? C41 Rh1 C13 C14 124.9(3) . . . . ? N31 Rh1 C13 C14 45.0(3) . . . . ? N2 Rh1 C13 C14 -149.2(2) . . . . ? C12 Rh1 C13 C14 -118.5(3) . . . . ? C11 Rh1 C13 C14 -79.3(3) . . . . ? C15 Rh1 C13 C14 -38.7(2) . . . . ? C41 Rh1 C13 C18 5.7(4) . . . . ? N31 Rh1 C13 C18 -74.2(4) . . . . ? N2 Rh1 C13 C18 91.5(4) . . . . ? C12 Rh1 C13 C18 122.3(5) . . . . ? C14 Rh1 C13 C18 -119.2(5) . . . . ? C11 Rh1 C13 C18 161.5(4) . . . . ? C15 Rh1 C13 C18 -157.9(4) . . . . ? C12 C13 C14 C15 6.5(4) . . . . ? C18 C13 C14 C15 -172.0(4) . . . . ? Rh1 C13 C14 C15 66.4(3) . . . . ? C12 C13 C14 C19 178.3(4) . . . . ? C18 C13 C14 C19 -0.3(7) . . . . ? Rh1 C13 C14 C19 -121.8(4) . . . . ? C12 C13 C14 Rh1 -59.9(3) . . . . ? C18 C13 C14 Rh1 121.5(4) . . . . ? C41 Rh1 C14 C13 -64.4(3) . . . . ? N31 Rh1 C14 C13 -147.4(2) . . . . ? N2 Rh1 C14 C13 95.0(4) . . . . ? C12 Rh1 C14 C13 37.2(2) . . . . ? C11 Rh1 C14 C13 80.4(3) . . . . ? C15 Rh1 C14 C13 115.6(3) . . . . ? C41 Rh1 C14 C15 -179.9(2) . . . . ? N31 Rh1 C14 C15 97.1(2) . . . . ? N2 Rh1 C14 C15 -20.6(5) . . . . ? C12 Rh1 C14 C15 -78.4(2) . . . . ? C13 Rh1 C14 C15 -115.6(3) . . . . ? C11 Rh1 C14 C15 -35.1(2) . . . . ? C41 Rh1 C14 C19 57.4(4) . . . . ? N31 Rh1 C14 C19 -25.6(4) . . . . ? N2 Rh1 C14 C19 -143.2(4) . . . . ? C12 Rh1 C14 C19 158.9(4) . . . . ? C13 Rh1 C14 C19 121.8(5) . . . . ? C11 Rh1 C14 C19 -157.8(4) . . . . ? C15 Rh1 C14 C19 -122.7(5) . . . . ? C12 C11 C15 C14 1.0(4) . . . . ? C16 C11 C15 C14 -180.0(4) . . . . ? Rh1 C11 C15 C14 -57.2(3) . . . . ? C12 C11 C15 C20 -175.3(4) . . . . ? C16 C11 C15 C20 3.7(6) . . . . ? Rh1 C11 C15 C20 126.5(4) . . . . ? C12 C11 C15 Rh1 58.2(2) . . . . ? C16 C11 C15 Rh1 -122.8(4) . . . . ? C13 C14 C15 C11 -4.7(4) . . . . ? C19 C14 C15 C11 -176.5(4) . . . . ? Rh1 C14 C15 C11 59.8(3) . . . . ? C13 C14 C15 C20 171.7(4) . . . . ? C19 C14 C15 C20 -0.1(6) . . . . ? Rh1 C14 C15 C20 -123.9(4) . . . . ? C13 C14 C15 Rh1 -64.5(3) . . . . ? C19 C14 C15 Rh1 123.7(4) . . . . ? C41 Rh1 C15 C11 -119.5(4) . . . . ? N31 Rh1 C15 C11 149.0(2) . . . . ? N2 Rh1 C15 C11 52.4(3) . . . . ? C12 Rh1 C15 C11 -37.7(2) . . . . ? C14 Rh1 C15 C11 -119.6(3) . . . . ? C13 Rh1 C15 C11 -80.8(2) . . . . ? C41 Rh1 C15 C14 0.1(5) . . . . ? N31 Rh1 C15 C14 -91.5(2) . . . . ? N2 Rh1 C15 C14 171.9(2) . . . . ? C12 Rh1 C15 C14 81.9(2) . . . . ? C13 Rh1 C15 C14 38.8(2) . . . . ? C11 Rh1 C15 C14 119.6(3) . . . . ? C41 Rh1 C15 C20 117.5(4) . . . . ? N31 Rh1 C15 C20 25.9(4) . . . . ? N2 Rh1 C15 C20 -70.7(4) . . . . ? C12 Rh1 C15 C20 -160.7(4) . . . . ? C14 Rh1 C15 C20 117.4(5) . . . . ? C13 Rh1 C15 C20 156.2(4) . . . . ? C11 Rh1 C15 C20 -123.0(5) . . . . ? C52 Rh2 C21 C25 55.3(3) . . . . ? N42 Rh2 C21 C25 136.7(2) . . . . ? N4 Rh2 C21 C25 -115.1(3) . . . . ? C24 Rh2 C21 C25 -37.7(2) . . . . ? C23 Rh2 C21 C25 -79.9(2) . . . . ? C22 Rh2 C21 C25 -116.9(3) . . . . ? C52 Rh2 C21 C22 172.1(2) . . . . ? N42 Rh2 C21 C22 -106.5(2) . . . . ? N4 Rh2 C21 C22 1.8(4) . . . . ? C25 Rh2 C21 C22 116.9(3) . . . . ? C24 Rh2 C21 C22 79.2(2) . . . . ? C23 Rh2 C21 C22 36.9(2) . . . . ? C52 Rh2 C21 C26 -65.9(4) . . . . ? N42 Rh2 C21 C26 15.5(4) . . . . ? N4 Rh2 C21 C26 123.7(4) . . . . ? C25 Rh2 C21 C26 -121.1(5) . . . . ? C24 Rh2 C21 C26 -158.9(4) . . . . ? C23 Rh2 C21 C26 158.9(4) . . . . ? C22 Rh2 C21 C26 122.0(5) . . . . ? C25 C21 C22 C23 1.7(4) . . . . ? C26 C21 C22 C23 177.3(4) . . . . ? Rh2 C21 C22 C23 -61.2(3) . . . . ? C25 C21 C22 C27 -172.0(4) . . . . ? C26 C21 C22 C27 3.6(6) . . . . ? Rh2 C21 C22 C27 125.1(4) . . . . ? C25 C21 C22 Rh2 62.9(3) . . . . ? C26 C21 C22 Rh2 -121.5(4) . . . . ? C52 Rh2 C22 C23 99.3(4) . . . . ? N42 Rh2 C22 C23 -160.7(2) . . . . ? N4 Rh2 C22 C23 -61.4(3) . . . . ? C21 Rh2 C22 C23 117.7(3) . . . . ? C25 Rh2 C22 C23 79.8(2) . . . . ? C24 Rh2 C22 C23 36.6(2) . . . . ? C52 Rh2 C22 C21 -18.4(5) . . . . ? N42 Rh2 C22 C21 81.7(2) . . . . ? N4 Rh2 C22 C21 -179.1(2) . . . . ? C25 Rh2 C22 C21 -37.9(2) . . . . ? C24 Rh2 C22 C21 -81.1(2) . . . . ? C23 Rh2 C22 C21 -117.7(3) . . . . ? C52 Rh2 C22 C27 -138.2(4) . . . . ? N42 Rh2 C22 C27 -38.1(4) . . . . ? N4 Rh2 C22 C27 61.2(4) . . . . ? C21 Rh2 C22 C27 -119.8(5) . . . . ? C25 Rh2 C22 C27 -157.6(5) . . . . ? C24 Rh2 C22 C27 159.2(5) . . . . ? C23 Rh2 C22 C27 122.5(5) . . . . ? C21 C22 C23 C24 -0.9(4) . . . . ? C27 C22 C23 C24 172.7(4) . . . . ? Rh2 C22 C23 C24 -60.7(3) . . . . ? C21 C22 C23 C28 178.3(4) . . . . ? C27 C22 C23 C28 -8.1(7) . . . . ? Rh2 C22 C23 C28 118.5(4) . . . . ? C21 C22 C23 Rh2 59.8(3) . . . . ? C27 C22 C23 Rh2 -126.6(4) . . . . ? C52 Rh2 C23 C22 -144.6(2) . . . . ? N42 Rh2 C23 C22 29.9(3) . . . . ? N4 Rh2 C23 C22 125.8(2) . . . . ? C21 Rh2 C23 C22 -37.8(2) . . . . ? C25 Rh2 C23 C22 -80.6(2) . . . . ? C24 Rh2 C23 C22 -119.2(3) . . . . ? C52 Rh2 C23 C24 -25.3(3) . . . . ? N42 Rh2 C23 C24 149.1(2) . . . . ? N4 Rh2 C23 C24 -115.0(2) . . . . ? C21 Rh2 C23 C24 81.4(2) . . . . ? C25 Rh2 C23 C24 38.6(2) . . . . ? C22 Rh2 C23 C24 119.2(3) . . . . ? C52 Rh2 C23 C28 93.2(4) . . . . ? N42 Rh2 C23 C28 -92.4(4) . . . . ? N4 Rh2 C23 C28 3.5(4) . . . . ? C21 Rh2 C23 C28 -160.1(4) . . . . ? C25 Rh2 C23 C28 157.1(4) . . . . ? C24 Rh2 C23 C28 118.5(4) . . . . ? C22 Rh2 C23 C28 -122.3(5) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? C28 C23 C24 C25 -179.4(4) . . . . ? Rh2 C23 C24 C25 -61.5(3) . . . . ? C22 C23 C24 C29 -175.4(4) . . . . ? C28 C23 C24 C29 5.3(6) . . . . ? Rh2 C23 C24 C29 123.2(4) . . . . ? C22 C23 C24 Rh2 61.4(3) . . . . ? C28 C23 C24 Rh2 -117.9(4) . . . . ? C52 Rh2 C24 C23 163.7(2) . . . . ? N42 Rh2 C24 C23 -96.2(5) . . . . ? N4 Rh2 C24 C23 71.0(2) . . . . ? C21 Rh2 C24 C23 -79.1(2) . . . . ? C25 Rh2 C24 C23 -116.4(3) . . . . ? C22 Rh2 C24 C23 -36.3(2) . . . . ? C52 Rh2 C24 C25 -79.9(2) . . . . ? N42 Rh2 C24 C25 20.1(5) . . . . ? N4 Rh2 C24 C25 -172.6(2) . . . . ? C21 Rh2 C24 C25 37.3(2) . . . . ? C23 Rh2 C24 C25 116.4(3) . . . . ? C22 Rh2 C24 C25 80.1(2) . . . . ? C52 Rh2 C24 C29 42.1(4) . . . . ? N42 Rh2 C24 C29 142.1(4) . . . . ? N4 Rh2 C24 C29 -50.6(4) . . . . ? C21 Rh2 C24 C29 159.2(4) . . . . ? C25 Rh2 C24 C29 122.0(4) . . . . ? C23 Rh2 C24 C29 -121.7(4) . . . . ? C22 Rh2 C24 C29 -157.9(4) . . . . ? C22 C21 C25 C24 -1.7(4) . . . . ? C26 C21 C25 C24 -177.4(4) . . . . ? Rh2 C21 C25 C24 62.2(3) . . . . ? C22 C21 C25 C30 175.1(4) . . . . ? C26 C21 C25 C30 -0.6(6) . . . . ? Rh2 C21 C25 C30 -121.0(4) . . . . ? C22 C21 C25 Rh2 -63.9(3) . . . . ? C26 C21 C25 Rh2 120.4(4) . . . . ? C23 C24 C25 C21 1.2(4) . . . . ? C29 C24 C25 C21 176.4(4) . . . . ? Rh2 C24 C25 C21 -61.6(3) . . . . ? C23 C24 C25 C30 -175.7(4) . . . . ? C29 C24 C25 C30 -0.5(6) . . . . ? Rh2 C24 C25 C30 121.5(4) . . . . ? C23 C24 C25 Rh2 62.8(3) . . . . ? C29 C24 C25 Rh2 -122.0(4) . . . . ? C52 Rh2 C25 C21 -134.8(2) . . . . ? N42 Rh2 C25 C21 -54.4(3) . . . . ? N4 Rh2 C25 C21 130.1(2) . . . . ? C24 Rh2 C25 C21 117.8(3) . . . . ? C23 Rh2 C25 C21 80.0(2) . . . . ? C22 Rh2 C25 C21 38.1(2) . . . . ? C52 Rh2 C25 C24 107.4(2) . . . . ? N42 Rh2 C25 C24 -172.2(2) . . . . ? N4 Rh2 C25 C24 12.3(3) . . . . ? C21 Rh2 C25 C24 -117.8(3) . . . . ? C23 Rh2 C25 C24 -37.8(2) . . . . ? C22 Rh2 C25 C24 -79.7(2) . . . . ? C52 Rh2 C25 C30 -13.1(4) . . . . ? N42 Rh2 C25 C30 67.3(4) . . . . ? N4 Rh2 C25 C30 -108.2(4) . . . . ? C21 Rh2 C25 C30 121.7(4) . . . . ? C24 Rh2 C25 C30 -120.5(4) . . . . ? C23 Rh2 C25 C30 -158.3(4) . . . . ? C22 Rh2 C25 C30 159.8(4) . . . . ? C35 N31 C31 C32 -0.4(6) . . . . ? Rh1 N31 C31 C32 -178.0(3) . . . . ? N31 C31 C32 C33 0.6(7) . . . . ? C31 C32 C33 C34 -0.2(7) . . . . ? C32 C33 C34 C35 -0.2(7) . . . . ? C31 N31 C35 C34 0.0(6) . . . . ? Rh1 N31 C35 C34 177.8(3) . . . . ? C31 N31 C35 C36 -177.2(4) . . . . ? Rh1 N31 C35 C36 0.6(4) . . . . ? C33 C34 C35 N31 0.3(6) . . . . ? C33 C34 C35 C36 177.1(4) . . . . ? N31 C35 C36 C37 178.2(4) . . . . ? C34 C35 C36 C37 1.2(7) . . . . ? N31 C35 C36 C41 1.5(5) . . . . ? C34 C35 C36 C41 -175.5(4) . . . . ? C41 C36 C37 C38 0.9(7) . . . . ? C35 C36 C37 C38 -175.6(4) . . . . ? C36 C37 C38 C39 0.8(8) . . . . ? C37 C38 C39 C40 -1.2(8) . . . . ? C38 C39 C40 C41 -0.2(7) . . . . ? C39 C40 C41 C36 1.9(6) . . . . ? C39 C40 C41 Rh1 179.0(3) . . . . ? C37 C36 C41 C40 -2.3(6) . . . . ? C35 C36 C41 C40 174.5(4) . . . . ? C37 C36 C41 Rh1 -179.7(3) . . . . ? C35 C36 C41 Rh1 -2.9(5) . . . . ? N31 Rh1 C41 C40 -174.8(4) . . . . ? N2 Rh1 C41 C40 -85.3(4) . . . . ? C12 Rh1 C41 C40 17.6(4) . . . . ? C14 Rh1 C41 C40 87.9(4) . . . . ? C13 Rh1 C41 C40 53.8(4) . . . . ? C11 Rh1 C41 C40 9.3(5) . . . . ? C15 Rh1 C41 C40 87.9(5) . . . . ? N31 Rh1 C41 C36 2.4(3) . . . . ? N2 Rh1 C41 C36 91.9(3) . . . . ? C12 Rh1 C41 C36 -165.2(3) . . . . ? C14 Rh1 C41 C36 -94.9(3) . . . . ? C13 Rh1 C41 C36 -129.0(3) . . . . ? C11 Rh1 C41 C36 -173.5(3) . . . . ? C15 Rh1 C41 C36 -95.0(4) . . . . ? C46 N42 C42 C43 -0.2(6) . . . . ? Rh2 N42 C42 C43 -179.6(3) . . . . ? N42 C42 C43 C44 1.1(7) . . . . ? C42 C43 C44 C45 -0.8(8) . . . . ? C43 C44 C45 C46 -0.4(7) . . . . ? C42 N42 C46 C45 -1.0(6) . . . . ? Rh2 N42 C46 C45 178.5(3) . . . . ? C42 N42 C46 C47 178.8(3) . . . . ? Rh2 N42 C46 C47 -1.7(4) . . . . ? C44 C45 C46 N42 1.3(7) . . . . ? C44 C45 C46 C47 -178.5(4) . . . . ? N42 C46 C47 C48 179.4(4) . . . . ? C45 C46 C47 C48 -0.8(6) . . . . ? N42 C46 C47 C52 -1.0(5) . . . . ? C45 C46 C47 C52 178.8(4) . . . . ? C52 C47 C48 C49 1.2(6) . . . . ? C46 C47 C48 C49 -179.2(4) . . . . ? C47 C48 C49 C50 -2.3(7) . . . . ? C48 C49 C50 C51 0.8(7) . . . . ? C49 C50 C51 C52 1.8(7) . . . . ? C50 C51 C52 C47 -2.9(6) . . . . ? C50 C51 C52 Rh2 175.4(3) . . . . ? C48 C47 C52 C51 1.4(6) . . . . ? C46 C47 C52 C51 -178.2(3) . . . . ? C48 C47 C52 Rh2 -177.1(3) . . . . ? C46 C47 C52 Rh2 3.3(4) . . . . ? N42 Rh2 C52 C51 178.3(3) . . . . ? N4 Rh2 C52 C51 85.8(3) . . . . ? C21 Rh2 C52 C51 -89.5(3) . . . . ? C25 Rh2 C52 C51 -58.9(3) . . . . ? C24 Rh2 C52 C51 -21.0(4) . . . . ? C23 Rh2 C52 C51 -5.3(4) . . . . ? C22 Rh2 C52 C51 -76.3(5) . . . . ? N42 Rh2 C52 C47 -3.2(3) . . . . ? N4 Rh2 C52 C47 -95.8(3) . . . . ? C21 Rh2 C52 C47 88.9(3) . . . . ? C25 Rh2 C52 C47 119.5(3) . . . . ? C24 Rh2 C52 C47 157.4(3) . . . . ? C23 Rh2 C52 C47 173.2(2) . . . . ? C22 Rh2 C52 C47 102.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.647 _refine_diff_density_min -1.192 _refine_diff_density_rms 0.128 _database_code_depnum_ccdc_archive 'CCDC 945552' ####################################################################### # # 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_comp8b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H49 N6 Rh2 1+, B F4 1-, 0.5(C2 H3 N), 0.25(H2 O)' _chemical_formula_sum 'C45 H51 B F4 N6.50 O0.25 Rh2' _chemical_formula_weight 979.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6756(8) _cell_length_b 14.2627(9) _cell_length_c 14.4068(8) _cell_angle_alpha 99.704(2) _cell_angle_beta 111.325(2) _cell_angle_gamma 96.083(2) _cell_volume 2166.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 185(2) _cell_measurement_reflns_used 23327 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.55 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.502 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 999 _exptl_absorpt_coefficient_mu 0.820 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7351 _exptl_absorpt_correction_T_max 0.8532 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 185(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20536 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9821 _reflns_number_gt 8407 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+3.1209P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9821 _refine_ls_number_parameters 515 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0490 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh -0.17335(2) 0.486787(17) 0.232458(17) 0.03369(8) Uani 1 1 d . . . Rh2 Rh 0.16352(2) 0.196871(17) 0.258202(17) 0.03313(8) Uani 1 1 d . . . F1 F 0.3955(3) 0.1757(3) 0.7850(3) 0.0935(10) Uiso 1 1 d D . . F2A F 0.3725(5) 0.0758(4) 0.8980(4) 0.0699(14) Uiso 0.50 1 d PD . . F2B F 0.4510(7) 0.0731(6) 0.8721(6) 0.104(2) Uiso 0.50 1 d PD . . F3A F 0.2224(6) 0.1027(4) 0.7795(5) 0.1595(19) Uiso 1 1 d D . . F4A F 0.3574(6) 0.0212(5) 0.7136(5) 0.0809(16) Uiso 0.50 1 d PD . . F4B F 0.2906(8) 0.0080(5) 0.7334(6) 0.105(2) Uiso 0.50 1 d PD . . O1 O 0.5000 1.0000 0.5000 0.127(5) Uiso 0.50 2 d SP . . N1 N 0.1043(3) 0.48852(19) 0.2903(2) 0.0387(6) Uani 1 1 d . . . N2 N -0.0063(3) 0.43301(18) 0.26990(19) 0.0335(5) Uani 1 1 d . . . N3 N 0.0034(2) 0.34194(18) 0.26746(19) 0.0338(5) Uani 1 1 d . . . N4 N 0.1238(2) 0.33646(18) 0.28639(19) 0.0328(5) Uani 1 1 d . . . N5 N 0.2396(12) 0.9077(9) 0.4185(10) 0.109(4) Uiso 0.50 1 d PD . . N31 N -0.2661(3) 0.3465(2) 0.2071(2) 0.0441(7) Uani 1 1 d . . . N42 N 0.1025(3) 0.16772(19) 0.3720(2) 0.0416(6) Uani 1 1 d . . . C1 C 0.4308(17) 0.9848(15) 0.5724(13) 0.149(7) Uiso 0.50 1 d PD . . C2 C 0.3226(11) 0.9438(9) 0.4759(9) 0.082(3) Uiso 0.50 1 d PD . . C5 C 0.1832(3) 0.4259(2) 0.2996(2) 0.0358(7) Uani 1 1 d . . . C6 C 0.3168(4) 0.4548(3) 0.3197(3) 0.0488(9) Uani 1 1 d . . . H6A H 0.3411 0.4072 0.2763 0.059 Uiso 1 1 calc R . . H6B H 0.3674 0.4580 0.3917 0.059 Uiso 1 1 calc R . . H6C H 0.3306 0.5185 0.3044 0.059 Uiso 1 1 calc R . . C11 C -0.1105(4) 0.6126(2) 0.3673(2) 0.0411(8) Uani 1 1 d . . . C12 C -0.1153(4) 0.6426(2) 0.2740(3) 0.0446(8) Uani 1 1 d . . . C13 C -0.2421(4) 0.6201(3) 0.2036(3) 0.0473(9) Uani 1 1 d . . . C14 C -0.3132(4) 0.5690(3) 0.2471(3) 0.0461(8) Uani 1 1 d . . . C15 C -0.2310(4) 0.5688(2) 0.3511(3) 0.0423(8) Uani 1 1 d . . . C16 C 0.0041(4) 0.6272(3) 0.4626(3) 0.0555(10) Uani 1 1 d . . . H16A H 0.0222 0.6942 0.5012 0.067 Uiso 1 1 calc R . . H16B H 0.0750 0.6137 0.4447 0.067 Uiso 1 1 calc R . . H16C H -0.0096 0.5832 0.5045 0.067 Uiso 1 1 calc R . . C17 C -0.0075(5) 0.6994(3) 0.2627(4) 0.0659(12) Uani 1 1 d . . . H17A H -0.0234 0.7647 0.2569 0.079 Uiso 1 1 calc R . . H17B H 0.0024 0.6671 0.2011 0.079 Uiso 1 1 calc R . . H17C H 0.0691 0.7035 0.3227 0.079 Uiso 1 1 calc R . . C18 C -0.2946(6) 0.6472(4) 0.1015(3) 0.0722(14) Uani 1 1 d . . . H18A H -0.3560 0.6889 0.1019 0.087 Uiso 1 1 calc R . . H18B H -0.3351 0.5885 0.0474 0.087 Uiso 1 1 calc R . . H18C H -0.2266 0.6819 0.0888 0.087 Uiso 1 1 calc R . . C19 C -0.4519(4) 0.5335(4) 0.2007(4) 0.0723(13) Uani 1 1 d . . . H19A H -0.4746 0.4879 0.1351 0.087 Uiso 1 1 calc R . . H19B H -0.4950 0.5884 0.1897 0.087 Uiso 1 1 calc R . . H19C H -0.4766 0.5009 0.2470 0.087 Uiso 1 1 calc R . . C20 C -0.2733(5) 0.5327(3) 0.4281(4) 0.0626(12) Uani 1 1 d . . . H20A H -0.3059 0.5835 0.4605 0.075 Uiso 1 1 calc R . . H20B H -0.2024 0.5159 0.4804 0.075 Uiso 1 1 calc R . . H20C H -0.3392 0.4754 0.3934 0.075 Uiso 1 1 calc R . . C21 C 0.0994(4) 0.0525(2) 0.1589(3) 0.0439(8) Uani 1 1 d . . . C22 C 0.0146(3) 0.1121(3) 0.1091(2) 0.0429(8) Uani 1 1 d . . . C23 C 0.0868(3) 0.1868(3) 0.0900(2) 0.0406(7) Uani 1 1 d . . . C24 C 0.2153(3) 0.1746(3) 0.1257(2) 0.0403(7) Uani 1 1 d . . . C25 C 0.2222(3) 0.0895(2) 0.1674(3) 0.0407(7) Uani 1 1 d . . . C26 C 0.0619(5) -0.0378(3) 0.1894(3) 0.0606(11) Uani 1 1 d . . . H26A H 0.1101 -0.0320 0.2624 0.073 Uiso 1 1 calc R . . H26B H 0.0786 -0.0936 0.1497 0.073 Uiso 1 1 calc R . . H26C H -0.0275 -0.0466 0.1760 0.073 Uiso 1 1 calc R . . C27 C -0.1241(4) 0.0954(4) 0.0769(3) 0.0598(11) Uani 1 1 d . . . H27A H -0.1500 0.0428 0.1049 0.072 Uiso 1 1 calc R . . H27B H -0.1642 0.0779 0.0021 0.072 Uiso 1 1 calc R . . H27C H -0.1492 0.1546 0.1024 0.072 Uiso 1 1 calc R . . C28 C 0.0380(4) 0.2674(3) 0.0413(3) 0.0514(9) Uani 1 1 d . . . H28A H 0.0016 0.3053 0.0831 0.062 Uiso 1 1 calc R . . H28B H -0.0262 0.2401 -0.0273 0.062 Uiso 1 1 calc R . . H28C H 0.1068 0.3093 0.0365 0.062 Uiso 1 1 calc R . . C29 C 0.3173(4) 0.2303(3) 0.1064(3) 0.0524(9) Uani 1 1 d . . . H29A H 0.3982 0.2310 0.1606 0.063 Uiso 1 1 calc R . . H29B H 0.3034 0.2968 0.1058 0.063 Uiso 1 1 calc R . . H29C H 0.3172 0.1995 0.0402 0.063 Uiso 1 1 calc R . . C30 C 0.3355(4) 0.0437(3) 0.2040(3) 0.0565(10) Uani 1 1 d . . . H30A H 0.3220 -0.0032 0.2432 0.068 Uiso 1 1 calc R . . H30B H 0.4083 0.0938 0.2477 0.068 Uiso 1 1 calc R . . H30C H 0.3502 0.0106 0.1451 0.068 Uiso 1 1 calc R . . C31 C -0.2760(4) 0.3043(3) 0.2820(3) 0.0509(9) Uani 1 1 d . . . H31 H -0.2425 0.3409 0.3506 0.061 Uiso 1 1 calc R . . C32 C -0.3342(4) 0.2086(3) 0.2607(5) 0.0658(13) Uani 1 1 d . . . H32 H -0.3385 0.1793 0.3141 0.079 Uiso 1 1 calc R . . C33 C -0.3858(4) 0.1568(3) 0.1600(5) 0.0757(16) Uani 1 1 d . . . H33 H -0.4269 0.0915 0.1438 0.091 Uiso 1 1 calc R . . C34 C -0.3776(4) 0.2001(3) 0.0836(4) 0.0669(14) Uani 1 1 d . . . H34 H -0.4158 0.1658 0.0142 0.080 Uiso 1 1 calc R . . C35 C -0.3128(3) 0.2948(3) 0.1088(3) 0.0501(9) Uani 1 1 d . . . C36 C -0.2788(4) 0.3432(3) 0.0387(3) 0.0519(10) Uani 1 1 d . . . C37 C -0.3082(4) 0.3013(4) -0.0653(3) 0.0715(15) Uani 1 1 d . . . H37 H -0.3630 0.2406 -0.0963 0.086 Uiso 1 1 calc R . . C38 C -0.2579(5) 0.3477(5) -0.1221(3) 0.0808(18) Uani 1 1 d . . . H38 H -0.2772 0.3188 -0.1917 0.097 Uiso 1 1 calc R . . C39 C -0.1803(5) 0.4353(4) -0.0778(3) 0.0717(15) Uani 1 1 d . . . H39 H -0.1450 0.4669 -0.1169 0.086 Uiso 1 1 calc R . . C40 C -0.1517(4) 0.4796(3) 0.0244(3) 0.0571(11) Uani 1 1 d . . . H40 H -0.0980 0.5409 0.0537 0.068 Uiso 1 1 calc R . . C41 C -0.2014(3) 0.4344(3) 0.0834(2) 0.0438(8) Uani 1 1 d . . . C42 C -0.0170(4) 0.1335(2) 0.3549(3) 0.0464(8) Uani 1 1 d . . . H42 H -0.0796 0.1260 0.2884 0.056 Uiso 1 1 calc R . . C43 C -0.0514(5) 0.1089(3) 0.4313(3) 0.0527(9) Uani 1 1 d . . . H43 H -0.1360 0.0832 0.4170 0.063 Uiso 1 1 calc R . . C44 C 0.0392(5) 0.1224(3) 0.5286(3) 0.0566(11) Uani 1 1 d . . . H44 H 0.0174 0.1056 0.5819 0.068 Uiso 1 1 calc R . . C45 C 0.1608(5) 0.1601(3) 0.5480(3) 0.0540(10) Uani 1 1 d . . . H45 H 0.2232 0.1712 0.6151 0.065 Uiso 1 1 calc R . . C46 C 0.1926(4) 0.1821(2) 0.4685(2) 0.0443(8) Uani 1 1 d . . . C47 C 0.3184(4) 0.2185(2) 0.4762(3) 0.0463(9) Uani 1 1 d . . . C48 C 0.4245(5) 0.2385(3) 0.5688(3) 0.0612(12) Uani 1 1 d . . . H48 H 0.4163 0.2293 0.6300 0.073 Uiso 1 1 calc R . . C49 C 0.5397(5) 0.2713(3) 0.5694(3) 0.0682(13) Uani 1 1 d . . . H49 H 0.6112 0.2855 0.6317 0.082 Uiso 1 1 calc R . . C50 C 0.5529(4) 0.2841(3) 0.4798(3) 0.0624(11) Uani 1 1 d . . . H50 H 0.6331 0.3062 0.4808 0.075 Uiso 1 1 calc R . . C51 C 0.4472(4) 0.2641(3) 0.3883(3) 0.0513(9) Uani 1 1 d . . . H51 H 0.4565 0.2730 0.3274 0.062 Uiso 1 1 calc R . . C52 C 0.3287(3) 0.2316(2) 0.3846(2) 0.0410(8) Uani 1 1 d . . . B1 B 0.3443(7) 0.0903(4) 0.7979(4) 0.106(3) Uani 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 Rh1 0.04378(15) 0.02782(12) 0.02787(12) 0.00480(9) 0.01047(10) 0.01482(10) Rh2 0.04122(14) 0.02898(13) 0.02487(12) 0.00309(9) 0.00699(10) 0.01447(10) N1 0.0463(15) 0.0295(13) 0.0400(14) 0.0067(11) 0.0159(13) 0.0106(11) N2 0.0418(14) 0.0287(12) 0.0283(12) 0.0049(10) 0.0111(11) 0.0110(11) N3 0.0410(14) 0.0286(12) 0.0305(12) 0.0055(10) 0.0114(11) 0.0121(11) N4 0.0398(14) 0.0296(12) 0.0275(12) 0.0046(10) 0.0109(11) 0.0117(10) N31 0.0406(15) 0.0342(14) 0.0521(17) 0.0047(13) 0.0118(13) 0.0147(12) N42 0.0628(19) 0.0259(12) 0.0324(13) 0.0053(11) 0.0136(13) 0.0130(12) C5 0.0449(17) 0.0302(14) 0.0309(15) 0.0039(12) 0.0137(13) 0.0095(13) C6 0.047(2) 0.0372(18) 0.066(2) 0.0124(17) 0.0261(19) 0.0099(15) C11 0.060(2) 0.0280(15) 0.0323(16) 0.0017(12) 0.0134(15) 0.0200(14) C12 0.066(2) 0.0287(15) 0.0424(18) 0.0065(14) 0.0233(17) 0.0176(15) C13 0.073(2) 0.0388(18) 0.0374(17) 0.0133(14) 0.0217(17) 0.0314(17) C14 0.054(2) 0.0410(18) 0.0468(19) 0.0092(15) 0.0187(17) 0.0265(16) C15 0.063(2) 0.0318(16) 0.0392(17) 0.0072(13) 0.0245(16) 0.0229(15) C16 0.070(3) 0.0361(18) 0.044(2) -0.0044(15) 0.0066(19) 0.0180(17) C17 0.092(3) 0.037(2) 0.082(3) 0.012(2) 0.051(3) 0.010(2) C18 0.113(4) 0.071(3) 0.047(2) 0.028(2) 0.030(3) 0.058(3) C19 0.054(3) 0.079(3) 0.079(3) 0.008(3) 0.019(2) 0.031(2) C20 0.097(3) 0.053(2) 0.067(3) 0.025(2) 0.053(3) 0.039(2) C21 0.057(2) 0.0352(17) 0.0356(17) -0.0032(13) 0.0161(15) 0.0151(15) C22 0.0451(18) 0.0471(19) 0.0288(15) -0.0038(14) 0.0088(14) 0.0157(15) C23 0.0493(19) 0.0451(18) 0.0234(14) 0.0012(13) 0.0091(13) 0.0206(15) C24 0.0480(19) 0.0439(18) 0.0277(15) 0.0025(13) 0.0126(14) 0.0194(15) C25 0.0461(18) 0.0360(16) 0.0332(16) -0.0008(13) 0.0082(14) 0.0183(14) C26 0.082(3) 0.0324(18) 0.061(3) -0.0023(17) 0.028(2) 0.0073(19) C27 0.047(2) 0.081(3) 0.040(2) -0.0039(19) 0.0106(17) 0.014(2) C28 0.063(2) 0.059(2) 0.0329(17) 0.0128(16) 0.0134(17) 0.0319(19) C29 0.053(2) 0.064(2) 0.043(2) 0.0111(18) 0.0198(17) 0.0197(19) C30 0.057(2) 0.047(2) 0.059(2) 0.0070(18) 0.0128(19) 0.0292(18) C31 0.0439(19) 0.0380(18) 0.069(3) 0.0140(18) 0.0172(18) 0.0161(15) C32 0.050(2) 0.043(2) 0.115(4) 0.029(3) 0.036(3) 0.0173(18) C33 0.045(2) 0.035(2) 0.139(5) -0.002(3) 0.036(3) 0.0068(17) C34 0.039(2) 0.047(2) 0.094(4) -0.019(2) 0.018(2) 0.0060(17) C35 0.0338(17) 0.0430(19) 0.057(2) -0.0080(17) 0.0051(16) 0.0157(14) C36 0.0435(19) 0.059(2) 0.0389(18) -0.0044(17) 0.0018(15) 0.0270(17) C37 0.056(2) 0.083(3) 0.044(2) -0.020(2) -0.0074(19) 0.032(2) C38 0.089(4) 0.115(5) 0.0268(19) 0.000(2) 0.004(2) 0.059(3) C39 0.092(4) 0.101(4) 0.034(2) 0.023(2) 0.024(2) 0.059(3) C40 0.074(3) 0.068(3) 0.0369(18) 0.0175(18) 0.0201(19) 0.039(2) C41 0.0486(19) 0.050(2) 0.0289(15) 0.0053(14) 0.0072(14) 0.0273(16) C42 0.065(2) 0.0322(16) 0.0391(18) 0.0029(14) 0.0181(17) 0.0111(16) C43 0.082(3) 0.0339(17) 0.052(2) 0.0099(16) 0.036(2) 0.0126(18) C44 0.105(4) 0.0333(17) 0.048(2) 0.0154(16) 0.042(2) 0.024(2) C45 0.093(3) 0.0363(18) 0.0334(17) 0.0094(14) 0.0198(19) 0.027(2) C46 0.072(2) 0.0265(15) 0.0300(15) 0.0052(12) 0.0128(16) 0.0203(15) C47 0.065(2) 0.0305(16) 0.0304(16) 0.0036(13) 0.0019(16) 0.0190(15) C48 0.085(3) 0.045(2) 0.0320(18) 0.0048(16) -0.0020(19) 0.018(2) C49 0.067(3) 0.058(3) 0.046(2) 0.0066(19) -0.015(2) 0.014(2) C50 0.054(2) 0.052(2) 0.054(2) 0.0056(19) -0.0075(19) 0.0112(18) C51 0.049(2) 0.047(2) 0.044(2) 0.0062(16) 0.0026(16) 0.0153(16) C52 0.0500(19) 0.0314(15) 0.0306(15) 0.0038(12) 0.0018(14) 0.0176(14) B1 0.148(7) 0.043(3) 0.061(3) 0.001(2) -0.032(4) 0.030(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C41 2.042(3) . ? Rh1 N31 2.077(3) . ? Rh1 N2 2.092(3) . ? Rh1 C14 2.158(3) . ? Rh1 C12 2.167(3) . ? Rh1 C13 2.186(3) . ? Rh1 C11 2.245(3) . ? Rh1 C15 2.253(3) . ? Rh2 C52 2.054(3) . ? Rh2 N42 2.093(3) . ? Rh2 N4 2.098(2) . ? Rh2 C25 2.174(3) . ? Rh2 C21 2.179(3) . ? Rh2 C24 2.188(3) . ? Rh2 C23 2.230(3) . ? Rh2 C22 2.249(3) . ? F1 B1 1.370(7) . ? F2A B1 1.414(7) . ? F2B B1 1.392(8) . ? F3A B1 1.387(8) . ? F4A B1 1.494(8) . ? F4B B1 1.300(8) . ? O1 C1 1.56(2) . ? N1 C5 1.338(4) . ? N1 N2 1.345(4) . ? N2 N3 1.311(3) . ? N3 N4 1.345(4) . ? N4 C5 1.334(4) . ? N5 C2 1.027(12) . ? N31 C31 1.356(5) . ? N31 C35 1.359(5) . ? N42 C42 1.346(5) . ? N42 C46 1.369(4) . ? C1 C2 1.471(15) . ? C5 C6 1.477(5) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C15 1.396(5) . ? C11 C12 1.462(5) . ? C11 C16 1.493(5) . ? C12 C13 1.422(6) . ? C12 C17 1.498(6) . ? C13 C14 1.419(6) . ? C13 C18 1.509(5) . ? C14 C15 1.457(5) . ? C14 C19 1.500(6) . ? C15 C20 1.509(5) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C25 1.429(5) . ? C21 C22 1.444(5) . ? C21 C26 1.501(5) . ? C22 C23 1.414(5) . ? C22 C27 1.493(5) . ? C23 C24 1.440(5) . ? C23 C28 1.503(5) . ? C24 C25 1.440(5) . ? C24 C29 1.497(6) . ? C25 C30 1.497(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.388(5) . ? C31 H31 0.9500 . ? C32 C33 1.386(8) . ? C32 H32 0.9500 . ? C33 C34 1.378(8) . ? C33 H33 0.9500 . ? C34 C35 1.395(6) . ? C34 H34 0.9500 . ? C35 C36 1.456(6) . ? C36 C41 1.403(6) . ? C36 C37 1.414(5) . ? C37 C38 1.379(8) . ? C37 H37 0.9500 . ? C38 C39 1.364(8) . ? C38 H38 0.9500 . ? C39 C40 1.402(6) . ? C39 H39 0.9500 . ? C40 C41 1.392(6) . ? C40 H40 0.9500 . ? C42 C43 1.385(5) . ? C42 H42 0.9500 . ? C43 C44 1.382(6) . ? C43 H43 0.9500 . ? C44 C45 1.372(7) . ? C44 H44 0.9500 . ? C45 C46 1.397(5) . ? C45 H45 0.9500 . ? C46 C47 1.464(6) . ? C47 C52 1.409(5) . ? C47 C48 1.410(5) . ? C48 C49 1.373(7) . ? C48 H48 0.9500 . ? C49 C50 1.394(7) . ? C49 H49 0.9500 . ? C50 C51 1.399(5) . ? C50 H50 0.9500 . ? C51 C52 1.390(6) . ? C51 H51 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 C41 Rh1 N31 78.83(15) . . ? C41 Rh1 N2 86.23(12) . . ? N31 Rh1 N2 87.92(11) . . ? C41 Rh1 C14 112.42(14) . . ? N31 Rh1 C14 101.04(13) . . ? N2 Rh1 C14 160.44(12) . . ? C41 Rh1 C12 110.59(15) . . ? N31 Rh1 C12 164.46(13) . . ? N2 Rh1 C12 104.65(13) . . ? C14 Rh1 C12 64.24(15) . . ? C41 Rh1 C13 93.91(13) . . ? N31 Rh1 C13 131.81(14) . . ? N2 Rh1 C13 139.59(14) . . ? C14 Rh1 C13 38.13(15) . . ? C12 Rh1 C13 38.12(15) . . ? C41 Rh1 C11 149.06(15) . . ? N31 Rh1 C11 131.76(13) . . ? N2 Rh1 C11 97.86(11) . . ? C14 Rh1 C11 63.20(14) . . ? C12 Rh1 C11 38.66(13) . . ? C13 Rh1 C11 63.34(13) . . ? C41 Rh1 C15 150.90(13) . . ? N31 Rh1 C15 102.52(13) . . ? N2 Rh1 C15 122.78(12) . . ? C14 Rh1 C15 38.49(13) . . ? C12 Rh1 C15 63.10(13) . . ? C13 Rh1 C15 63.17(13) . . ? C11 Rh1 C15 36.17(14) . . ? C52 Rh2 N42 78.73(14) . . ? C52 Rh2 N4 92.32(11) . . ? N42 Rh2 N4 87.95(10) . . ? C52 Rh2 C25 96.40(13) . . ? N42 Rh2 C25 123.26(12) . . ? N4 Rh2 C25 148.66(12) . . ? C52 Rh2 C21 121.77(13) . . ? N42 Rh2 C21 97.54(13) . . ? N4 Rh2 C21 145.90(12) . . ? C25 Rh2 C21 38.32(14) . . ? C52 Rh2 C24 105.99(14) . . ? N42 Rh2 C24 160.81(12) . . ? N4 Rh2 C24 110.13(11) . . ? C25 Rh2 C24 38.54(13) . . ? C21 Rh2 C24 63.94(14) . . ? C52 Rh2 C23 141.73(15) . . ? N42 Rh2 C23 139.47(13) . . ? N4 Rh2 C23 91.55(11) . . ? C25 Rh2 C23 63.52(12) . . ? C21 Rh2 C23 62.75(13) . . ? C24 Rh2 C23 38.02(12) . . ? C52 Rh2 C22 159.06(13) . . ? N42 Rh2 C22 105.81(13) . . ? N4 Rh2 C22 108.12(11) . . ? C25 Rh2 C22 63.76(12) . . ? C21 Rh2 C22 38.01(13) . . ? C24 Rh2 C22 63.29(13) . . ? C23 Rh2 C22 36.79(14) . . ? C5 N1 N2 103.9(3) . . ? N3 N2 N1 111.7(3) . . ? N3 N2 Rh1 125.5(2) . . ? N1 N2 Rh1 122.58(19) . . ? N2 N3 N4 106.9(2) . . ? C5 N4 N3 106.9(2) . . ? C5 N4 Rh2 135.3(2) . . ? N3 N4 Rh2 116.17(19) . . ? C31 N31 C35 120.0(3) . . ? C31 N31 Rh1 124.1(3) . . ? C35 N31 Rh1 115.8(3) . . ? C42 N42 C46 119.3(3) . . ? C42 N42 Rh2 124.1(2) . . ? C46 N42 Rh2 116.6(3) . . ? N5 C2 C1 167.3(16) . . ? N4 C5 N1 110.7(3) . . ? N4 C5 C6 126.2(3) . . ? N1 C5 C6 123.1(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C15 C11 C12 108.1(3) . . ? C15 C11 C16 126.6(3) . . ? C12 C11 C16 125.3(4) . . ? C15 C11 Rh1 72.22(19) . . ? C12 C11 Rh1 67.77(18) . . ? C16 C11 Rh1 125.7(2) . . ? C13 C12 C11 107.6(3) . . ? C13 C12 C17 127.1(4) . . ? C11 C12 C17 124.8(4) . . ? C13 C12 Rh1 71.7(2) . . ? C11 C12 Rh1 73.58(19) . . ? C17 C12 Rh1 126.9(3) . . ? C14 C13 C12 108.1(3) . . ? C14 C13 C18 125.2(4) . . ? C12 C13 C18 126.7(4) . . ? C14 C13 Rh1 69.87(19) . . ? C12 C13 Rh1 70.18(19) . . ? C18 C13 Rh1 126.7(3) . . ? C13 C14 C15 107.9(3) . . ? C13 C14 C19 126.4(4) . . ? C15 C14 C19 125.2(4) . . ? C13 C14 Rh1 72.0(2) . . ? C15 C14 Rh1 74.26(19) . . ? C19 C14 Rh1 125.9(3) . . ? C11 C15 C14 108.0(3) . . ? C11 C15 C20 127.1(4) . . ? C14 C15 C20 124.8(4) . . ? C11 C15 Rh1 71.60(19) . . ? C14 C15 Rh1 67.25(18) . . ? C20 C15 Rh1 129.4(2) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C25 C21 C22 108.9(3) . . ? C25 C21 C26 125.8(3) . . ? C22 C21 C26 125.1(4) . . ? C25 C21 Rh2 70.67(19) . . ? C22 C21 Rh2 73.64(19) . . ? C26 C21 Rh2 125.2(3) . . ? C23 C22 C21 106.9(3) . . ? C23 C22 C27 125.7(3) . . ? C21 C22 C27 127.2(4) . . ? C23 C22 Rh2 70.84(19) . . ? C21 C22 Rh2 68.35(19) . . ? C27 C22 Rh2 128.9(2) . . ? C22 C23 C24 109.4(3) . . ? C22 C23 C28 125.6(3) . . ? C24 C23 C28 125.0(4) . . ? C22 C23 Rh2 72.37(19) . . ? C24 C23 Rh2 69.44(18) . . ? C28 C23 Rh2 123.9(2) . . ? C25 C24 C23 107.3(3) . . ? C25 C24 C29 126.4(3) . . ? C23 C24 C29 125.6(3) . . ? C25 C24 Rh2 70.20(19) . . ? C23 C24 Rh2 72.54(18) . . ? C29 C24 Rh2 130.2(2) . . ? C21 C25 C24 107.4(3) . . ? C21 C25 C30 126.6(3) . . ? C24 C25 C30 125.8(4) . . ? C21 C25 Rh2 71.02(18) . . ? C24 C25 Rh2 71.26(18) . . ? C30 C25 Rh2 127.2(2) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N31 C31 C32 121.3(4) . . ? N31 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C33 C32 C31 118.8(5) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C34 C33 C32 119.9(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 119.5(5) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? N31 C35 C34 120.3(4) . . ? N31 C35 C36 114.4(3) . . ? C34 C35 C36 125.1(4) . . ? C41 C36 C37 119.7(5) . . ? C41 C36 C35 115.2(3) . . ? C37 C36 C35 124.8(4) . . ? C38 C37 C36 120.6(5) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C39 C38 C37 119.7(4) . . ? C39 C38 H38 120.2 . . ? C37 C38 H38 120.2 . . ? C38 C39 C40 121.0(5) . . ? C38 C39 H39 119.5 . . ? C40 C39 H39 119.5 . . ? C41 C40 C39 120.6(5) . . ? C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C40 C41 C36 118.5(3) . . ? C40 C41 Rh1 126.7(3) . . ? C36 C41 Rh1 114.8(3) . . ? N42 C42 C43 122.0(4) . . ? N42 C42 H42 119.0 . . ? C43 C42 H42 119.0 . . ? C44 C43 C42 119.0(4) . . ? C44 C43 H43 120.5 . . ? C42 C43 H43 120.5 . . ? C45 C44 C43 119.7(4) . . ? C45 C44 H44 120.1 . . ? C43 C44 H44 120.1 . . ? C44 C45 C46 119.7(4) . . ? C44 C45 H45 120.1 . . ? C46 C45 H45 120.1 . . ? N42 C46 C45 120.3(4) . . ? N42 C46 C47 113.7(3) . . ? C45 C46 C47 126.0(3) . . ? C52 C47 C48 121.2(4) . . ? C52 C47 C46 116.0(3) . . ? C48 C47 C46 122.8(4) . . ? C49 C48 C47 119.3(4) . . ? C49 C48 H48 120.4 . . ? C47 C48 H48 120.4 . . ? C48 C49 C50 120.8(4) . . ? C48 C49 H49 119.6 . . ? C50 C49 H49 119.6 . . ? C49 C50 C51 119.4(5) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C52 C51 C50 121.5(4) . . ? C52 C51 H51 119.2 . . ? C50 C51 H51 119.2 . . ? C51 C52 C47 117.7(3) . . ? C51 C52 Rh2 127.2(3) . . ? C47 C52 Rh2 115.0(3) . . ? F4B B1 F1 130.8(7) . . ? F4B B1 F3A 83.6(6) . . ? F1 B1 F3A 101.9(4) . . ? F4B B1 F2B 106.4(6) . . ? F1 B1 F2B 98.3(6) . . ? F1 B1 F2A 119.3(5) . . ? F3A B1 F2A 95.8(6) . . ? F1 B1 F4A 99.8(6) . . ? F3A B1 F4A 114.0(5) . . ? F2A B1 F4A 124.5(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 N1 N2 N3 0.5(3) . . . . ? C5 N1 N2 Rh1 -173.7(2) . . . . ? C41 Rh1 N2 N3 -77.3(3) . . . . ? N31 Rh1 N2 N3 1.7(2) . . . . ? C14 Rh1 N2 N3 119.7(4) . . . . ? C12 Rh1 N2 N3 172.4(2) . . . . ? C13 Rh1 N2 N3 -168.9(2) . . . . ? C11 Rh1 N2 N3 133.6(2) . . . . ? C15 Rh1 N2 N3 105.3(3) . . . . ? C41 Rh1 N2 N1 96.1(3) . . . . ? N31 Rh1 N2 N1 175.1(2) . . . . ? C14 Rh1 N2 N1 -66.9(5) . . . . ? C12 Rh1 N2 N1 -14.2(3) . . . . ? C13 Rh1 N2 N1 4.5(3) . . . . ? C11 Rh1 N2 N1 -53.0(2) . . . . ? C15 Rh1 N2 N1 -81.4(3) . . . . ? N1 N2 N3 N4 -0.2(3) . . . . ? Rh1 N2 N3 N4 173.77(18) . . . . ? N2 N3 N4 C5 -0.1(3) . . . . ? N2 N3 N4 Rh2 -167.81(18) . . . . ? C52 Rh2 N4 C5 55.3(3) . . . . ? N42 Rh2 N4 C5 133.9(3) . . . . ? C25 Rh2 N4 C5 -51.0(4) . . . . ? C21 Rh2 N4 C5 -125.6(3) . . . . ? C24 Rh2 N4 C5 -52.7(3) . . . . ? C23 Rh2 N4 C5 -86.6(3) . . . . ? C22 Rh2 N4 C5 -120.1(3) . . . . ? C52 Rh2 N4 N3 -141.6(2) . . . . ? N42 Rh2 N4 N3 -63.0(2) . . . . ? C25 Rh2 N4 N3 112.1(3) . . . . ? C21 Rh2 N4 N3 37.5(3) . . . . ? C24 Rh2 N4 N3 110.4(2) . . . . ? C23 Rh2 N4 N3 76.5(2) . . . . ? C22 Rh2 N4 N3 43.0(2) . . . . ? C41 Rh1 N31 C31 168.6(3) . . . . ? N2 Rh1 N31 C31 82.0(3) . . . . ? C14 Rh1 N31 C31 -80.5(3) . . . . ? C12 Rh1 N31 C31 -62.5(6) . . . . ? C13 Rh1 N31 C31 -106.2(3) . . . . ? C11 Rh1 N31 C31 -16.7(3) . . . . ? C15 Rh1 N31 C31 -41.2(3) . . . . ? C41 Rh1 N31 C35 -8.0(2) . . . . ? N2 Rh1 N31 C35 -94.6(2) . . . . ? C14 Rh1 N31 C35 102.9(3) . . . . ? C12 Rh1 N31 C35 120.9(5) . . . . ? C13 Rh1 N31 C35 77.2(3) . . . . ? C11 Rh1 N31 C35 166.7(2) . . . . ? C15 Rh1 N31 C35 142.3(2) . . . . ? C52 Rh2 N42 C42 -178.9(3) . . . . ? N4 Rh2 N42 C42 88.3(3) . . . . ? C25 Rh2 N42 C42 -88.6(3) . . . . ? C21 Rh2 N42 C42 -57.9(3) . . . . ? C24 Rh2 N42 C42 -72.6(5) . . . . ? C23 Rh2 N42 C42 -1.7(3) . . . . ? C22 Rh2 N42 C42 -20.0(3) . . . . ? C52 Rh2 N42 C46 -1.1(2) . . . . ? N4 Rh2 N42 C46 -93.9(2) . . . . ? C25 Rh2 N42 C46 89.2(2) . . . . ? C21 Rh2 N42 C46 119.9(2) . . . . ? C24 Rh2 N42 C46 105.3(4) . . . . ? C23 Rh2 N42 C46 176.1(2) . . . . ? C22 Rh2 N42 C46 157.9(2) . . . . ? N3 N4 C5 N1 0.4(3) . . . . ? Rh2 N4 C5 N1 164.6(2) . . . . ? N3 N4 C5 C6 -178.4(3) . . . . ? Rh2 N4 C5 C6 -14.2(5) . . . . ? N2 N1 C5 N4 -0.6(3) . . . . ? N2 N1 C5 C6 178.4(3) . . . . ? C41 Rh1 C11 C15 126.7(3) . . . . ? N31 Rh1 C11 C15 -43.2(3) . . . . ? N2 Rh1 C11 C15 -137.48(19) . . . . ? C14 Rh1 C11 C15 37.4(2) . . . . ? C12 Rh1 C11 C15 118.9(3) . . . . ? C13 Rh1 C11 C15 80.3(2) . . . . ? C41 Rh1 C11 C12 7.8(4) . . . . ? N31 Rh1 C11 C12 -162.1(2) . . . . ? N2 Rh1 C11 C12 103.7(2) . . . . ? C14 Rh1 C11 C12 -81.5(2) . . . . ? C13 Rh1 C11 C12 -38.6(2) . . . . ? C15 Rh1 C11 C12 -118.9(3) . . . . ? C41 Rh1 C11 C16 -110.5(4) . . . . ? N31 Rh1 C11 C16 79.5(4) . . . . ? N2 Rh1 C11 C16 -14.7(4) . . . . ? C14 Rh1 C11 C16 160.1(4) . . . . ? C12 Rh1 C11 C16 -118.4(4) . . . . ? C13 Rh1 C11 C16 -157.0(4) . . . . ? C15 Rh1 C11 C16 122.8(4) . . . . ? C15 C11 C12 C13 2.8(4) . . . . ? C16 C11 C12 C13 -177.0(3) . . . . ? Rh1 C11 C12 C13 64.1(2) . . . . ? C15 C11 C12 C17 174.9(3) . . . . ? C16 C11 C12 C17 -4.9(5) . . . . ? Rh1 C11 C12 C17 -123.8(4) . . . . ? C15 C11 C12 Rh1 -61.3(2) . . . . ? C16 C11 C12 Rh1 118.9(3) . . . . ? C41 Rh1 C12 C13 68.9(2) . . . . ? N31 Rh1 C12 C13 -56.5(6) . . . . ? N2 Rh1 C12 C13 160.3(2) . . . . ? C14 Rh1 C12 C13 -36.9(2) . . . . ? C11 Rh1 C12 C13 -115.4(3) . . . . ? C15 Rh1 C12 C13 -80.0(2) . . . . ? C41 Rh1 C12 C11 -175.7(2) . . . . ? N31 Rh1 C12 C11 58.9(6) . . . . ? N2 Rh1 C12 C11 -84.2(2) . . . . ? C14 Rh1 C12 C11 78.6(2) . . . . ? C13 Rh1 C12 C11 115.4(3) . . . . ? C15 Rh1 C12 C11 35.4(2) . . . . ? C41 Rh1 C12 C17 -54.2(4) . . . . ? N31 Rh1 C12 C17 -179.6(4) . . . . ? N2 Rh1 C12 C17 37.3(4) . . . . ? C14 Rh1 C12 C17 -159.9(4) . . . . ? C13 Rh1 C12 C17 -123.1(5) . . . . ? C11 Rh1 C12 C17 121.5(5) . . . . ? C15 Rh1 C12 C17 156.9(4) . . . . ? C11 C12 C13 C14 -5.5(4) . . . . ? C17 C12 C13 C14 -177.3(3) . . . . ? Rh1 C12 C13 C14 59.8(2) . . . . ? C11 C12 C13 C18 173.1(3) . . . . ? C17 C12 C13 C18 1.3(6) . . . . ? Rh1 C12 C13 C18 -121.6(4) . . . . ? C11 C12 C13 Rh1 -65.3(2) . . . . ? C17 C12 C13 Rh1 122.8(4) . . . . ? C41 Rh1 C13 C14 122.1(2) . . . . ? N31 Rh1 C13 C14 43.6(3) . . . . ? N2 Rh1 C13 C14 -149.1(2) . . . . ? C12 Rh1 C13 C14 -118.9(3) . . . . ? C11 Rh1 C13 C14 -79.8(2) . . . . ? C15 Rh1 C13 C14 -39.1(2) . . . . ? C41 Rh1 C13 C12 -118.9(2) . . . . ? N31 Rh1 C13 C12 162.6(2) . . . . ? N2 Rh1 C13 C12 -30.2(3) . . . . ? C14 Rh1 C13 C12 118.9(3) . . . . ? C11 Rh1 C13 C12 39.1(2) . . . . ? C15 Rh1 C13 C12 79.8(2) . . . . ? C41 Rh1 C13 C18 2.6(4) . . . . ? N31 Rh1 C13 C18 -75.9(5) . . . . ? N2 Rh1 C13 C18 91.4(5) . . . . ? C14 Rh1 C13 C18 -119.5(5) . . . . ? C12 Rh1 C13 C18 121.6(5) . . . . ? C11 Rh1 C13 C18 160.7(5) . . . . ? C15 Rh1 C13 C18 -158.6(5) . . . . ? C12 C13 C14 C15 6.1(4) . . . . ? C18 C13 C14 C15 -172.5(3) . . . . ? Rh1 C13 C14 C15 66.1(2) . . . . ? C12 C13 C14 C19 178.2(4) . . . . ? C18 C13 C14 C19 -0.4(6) . . . . ? Rh1 C13 C14 C19 -121.8(4) . . . . ? C12 C13 C14 Rh1 -60.0(2) . . . . ? C18 C13 C14 Rh1 121.3(4) . . . . ? C41 Rh1 C14 C13 -66.0(3) . . . . ? N31 Rh1 C14 C13 -148.4(2) . . . . ? N2 Rh1 C14 C13 95.6(4) . . . . ? C12 Rh1 C14 C13 36.9(2) . . . . ? C11 Rh1 C14 C13 80.2(2) . . . . ? C15 Rh1 C14 C13 115.3(3) . . . . ? C41 Rh1 C14 C15 178.7(2) . . . . ? N31 Rh1 C14 C15 96.3(2) . . . . ? N2 Rh1 C14 C15 -19.7(5) . . . . ? C12 Rh1 C14 C15 -78.4(2) . . . . ? C13 Rh1 C14 C15 -115.3(3) . . . . ? C11 Rh1 C14 C15 -35.1(2) . . . . ? C41 Rh1 C14 C19 56.3(4) . . . . ? N31 Rh1 C14 C19 -26.1(4) . . . . ? N2 Rh1 C14 C19 -142.1(4) . . . . ? C12 Rh1 C14 C19 159.2(4) . . . . ? C13 Rh1 C14 C19 122.3(5) . . . . ? C11 Rh1 C14 C19 -157.5(4) . . . . ? C15 Rh1 C14 C19 -122.4(5) . . . . ? C12 C11 C15 C14 1.0(3) . . . . ? C16 C11 C15 C14 -179.3(3) . . . . ? Rh1 C11 C15 C14 -57.5(2) . . . . ? C12 C11 C15 C20 -175.5(3) . . . . ? C16 C11 C15 C20 4.3(5) . . . . ? Rh1 C11 C15 C20 126.0(3) . . . . ? C12 C11 C15 Rh1 58.5(2) . . . . ? C16 C11 C15 Rh1 -121.7(3) . . . . ? C13 C14 C15 C11 -4.4(4) . . . . ? C19 C14 C15 C11 -176.6(3) . . . . ? Rh1 C14 C15 C11 60.3(2) . . . . ? C13 C14 C15 C20 172.2(3) . . . . ? C19 C14 C15 C20 0.0(6) . . . . ? Rh1 C14 C15 C20 -123.2(3) . . . . ? C13 C14 C15 Rh1 -64.6(2) . . . . ? C19 C14 C15 Rh1 123.1(4) . . . . ? C41 Rh1 C15 C11 -122.1(3) . . . . ? N31 Rh1 C15 C11 148.45(19) . . . . ? N2 Rh1 C15 C11 52.8(2) . . . . ? C14 Rh1 C15 C11 -119.5(3) . . . . ? C12 Rh1 C15 C11 -37.8(2) . . . . ? C13 Rh1 C15 C11 -80.8(2) . . . . ? C41 Rh1 C15 C14 -2.6(4) . . . . ? N31 Rh1 C15 C14 -92.0(2) . . . . ? N2 Rh1 C15 C14 172.3(2) . . . . ? C12 Rh1 C15 C14 81.7(2) . . . . ? C13 Rh1 C15 C14 38.7(2) . . . . ? C11 Rh1 C15 C14 119.5(3) . . . . ? C41 Rh1 C15 C20 114.6(4) . . . . ? N31 Rh1 C15 C20 25.1(4) . . . . ? N2 Rh1 C15 C20 -70.6(4) . . . . ? C14 Rh1 C15 C20 117.1(5) . . . . ? C12 Rh1 C15 C20 -161.2(4) . . . . ? C13 Rh1 C15 C20 155.9(4) . . . . ? C11 Rh1 C15 C20 -123.4(5) . . . . ? C52 Rh2 C21 C25 -55.1(3) . . . . ? N42 Rh2 C21 C25 -136.5(2) . . . . ? N4 Rh2 C21 C25 126.0(2) . . . . ? C24 Rh2 C21 C25 38.2(2) . . . . ? C23 Rh2 C21 C25 81.0(2) . . . . ? C22 Rh2 C21 C25 117.5(3) . . . . ? C52 Rh2 C21 C22 -172.5(2) . . . . ? N42 Rh2 C21 C22 106.1(2) . . . . ? N4 Rh2 C21 C22 8.6(3) . . . . ? C25 Rh2 C21 C22 -117.5(3) . . . . ? C24 Rh2 C21 C22 -79.2(2) . . . . ? C23 Rh2 C21 C22 -36.5(2) . . . . ? C52 Rh2 C21 C26 65.7(4) . . . . ? N42 Rh2 C21 C26 -15.7(4) . . . . ? N4 Rh2 C21 C26 -113.2(4) . . . . ? C25 Rh2 C21 C26 120.8(4) . . . . ? C24 Rh2 C21 C26 159.0(4) . . . . ? C23 Rh2 C21 C26 -158.3(4) . . . . ? C22 Rh2 C21 C26 -121.8(4) . . . . ? C25 C21 C22 C23 -1.6(4) . . . . ? C26 C21 C22 C23 -177.4(3) . . . . ? Rh2 C21 C22 C23 60.7(2) . . . . ? C25 C21 C22 C27 174.5(3) . . . . ? C26 C21 C22 C27 -1.3(6) . . . . ? Rh2 C21 C22 C27 -123.2(3) . . . . ? C25 C21 C22 Rh2 -62.3(2) . . . . ? C26 C21 C22 Rh2 121.9(3) . . . . ? C52 Rh2 C22 C23 -100.0(4) . . . . ? N42 Rh2 C22 C23 160.10(19) . . . . ? N4 Rh2 C22 C23 67.0(2) . . . . ? C25 Rh2 C22 C23 -80.2(2) . . . . ? C21 Rh2 C22 C23 -118.0(3) . . . . ? C24 Rh2 C22 C23 -36.90(19) . . . . ? C52 Rh2 C22 C21 18.0(5) . . . . ? N42 Rh2 C22 C21 -81.9(2) . . . . ? N4 Rh2 C22 C21 -175.0(2) . . . . ? C25 Rh2 C22 C21 37.8(2) . . . . ? C24 Rh2 C22 C21 81.1(2) . . . . ? C23 Rh2 C22 C21 118.0(3) . . . . ? C52 Rh2 C22 C27 139.1(4) . . . . ? N42 Rh2 C22 C27 39.2(4) . . . . ? N4 Rh2 C22 C27 -53.9(4) . . . . ? C25 Rh2 C22 C27 158.9(4) . . . . ? C21 Rh2 C22 C27 121.1(5) . . . . ? C24 Rh2 C22 C27 -157.8(4) . . . . ? C23 Rh2 C22 C27 -120.9(5) . . . . ? C21 C22 C23 C24 0.7(4) . . . . ? C27 C22 C23 C24 -175.4(3) . . . . ? Rh2 C22 C23 C24 59.8(2) . . . . ? C21 C22 C23 C28 -178.5(3) . . . . ? C27 C22 C23 C28 5.3(5) . . . . ? Rh2 C22 C23 C28 -119.4(3) . . . . ? C21 C22 C23 Rh2 -59.1(2) . . . . ? C27 C22 C23 Rh2 124.7(3) . . . . ? C52 Rh2 C23 C22 145.4(2) . . . . ? N42 Rh2 C23 C22 -30.3(3) . . . . ? N4 Rh2 C23 C22 -118.9(2) . . . . ? C25 Rh2 C23 C22 80.9(2) . . . . ? C21 Rh2 C23 C22 37.7(2) . . . . ? C24 Rh2 C23 C22 119.5(3) . . . . ? C52 Rh2 C23 C24 25.9(3) . . . . ? N42 Rh2 C23 C24 -149.7(2) . . . . ? N4 Rh2 C23 C24 121.6(2) . . . . ? C25 Rh2 C23 C24 -38.6(2) . . . . ? C21 Rh2 C23 C24 -81.8(2) . . . . ? C22 Rh2 C23 C24 -119.5(3) . . . . ? C52 Rh2 C23 C28 -93.1(4) . . . . ? N42 Rh2 C23 C28 91.2(4) . . . . ? N4 Rh2 C23 C28 2.6(3) . . . . ? C25 Rh2 C23 C28 -157.6(4) . . . . ? C21 Rh2 C23 C28 159.2(4) . . . . ? C24 Rh2 C23 C28 -119.0(4) . . . . ? C22 Rh2 C23 C28 121.5(4) . . . . ? C22 C23 C24 C25 0.4(4) . . . . ? C28 C23 C24 C25 179.6(3) . . . . ? Rh2 C23 C24 C25 62.0(2) . . . . ? C22 C23 C24 C29 171.0(3) . . . . ? C28 C23 C24 C29 -9.8(5) . . . . ? Rh2 C23 C24 C29 -127.4(3) . . . . ? C22 C23 C24 Rh2 -61.6(2) . . . . ? C28 C23 C24 Rh2 117.6(3) . . . . ? C52 Rh2 C24 C25 80.0(2) . . . . ? N42 Rh2 C24 C25 -21.8(5) . . . . ? N4 Rh2 C24 C25 178.62(19) . . . . ? C21 Rh2 C24 C25 -38.0(2) . . . . ? C23 Rh2 C24 C25 -116.4(3) . . . . ? C22 Rh2 C24 C25 -80.6(2) . . . . ? C52 Rh2 C24 C23 -163.6(2) . . . . ? N42 Rh2 C24 C23 94.5(4) . . . . ? N4 Rh2 C24 C23 -65.0(2) . . . . ? C25 Rh2 C24 C23 116.4(3) . . . . ? C21 Rh2 C24 C23 78.3(2) . . . . ? C22 Rh2 C24 C23 35.7(2) . . . . ? C52 Rh2 C24 C29 -41.4(3) . . . . ? N42 Rh2 C24 C29 -143.2(4) . . . . ? N4 Rh2 C24 C29 57.2(3) . . . . ? C25 Rh2 C24 C29 -121.4(4) . . . . ? C21 Rh2 C24 C29 -159.4(4) . . . . ? C23 Rh2 C24 C29 122.2(4) . . . . ? C22 Rh2 C24 C29 158.0(4) . . . . ? C22 C21 C25 C24 1.8(4) . . . . ? C26 C21 C25 C24 177.6(3) . . . . ? Rh2 C21 C25 C24 -62.3(2) . . . . ? C22 C21 C25 C30 -173.1(3) . . . . ? C26 C21 C25 C30 2.6(6) . . . . ? Rh2 C21 C25 C30 122.7(4) . . . . ? C22 C21 C25 Rh2 64.2(2) . . . . ? C26 C21 C25 Rh2 -120.1(3) . . . . ? C23 C24 C25 C21 -1.3(3) . . . . ? C29 C24 C25 C21 -171.9(3) . . . . ? Rh2 C24 C25 C21 62.2(2) . . . . ? C23 C24 C25 C30 173.7(3) . . . . ? C29 C24 C25 C30 3.2(5) . . . . ? Rh2 C24 C25 C30 -122.8(3) . . . . ? C23 C24 C25 Rh2 -63.5(2) . . . . ? C29 C24 C25 Rh2 126.0(3) . . . . ? C52 Rh2 C25 C21 135.5(2) . . . . ? N42 Rh2 C25 C21 54.8(2) . . . . ? N4 Rh2 C25 C21 -119.3(3) . . . . ? C24 Rh2 C25 C21 -116.8(3) . . . . ? C23 Rh2 C25 C21 -78.8(2) . . . . ? C22 Rh2 C25 C21 -37.5(2) . . . . ? C52 Rh2 C25 C24 -107.7(2) . . . . ? N42 Rh2 C25 C24 171.60(19) . . . . ? N4 Rh2 C25 C24 -2.5(3) . . . . ? C21 Rh2 C25 C24 116.8(3) . . . . ? C23 Rh2 C25 C24 38.1(2) . . . . ? C22 Rh2 C25 C24 79.3(2) . . . . ? C52 Rh2 C25 C30 13.5(4) . . . . ? N42 Rh2 C25 C30 -67.2(4) . . . . ? N4 Rh2 C25 C30 118.7(3) . . . . ? C21 Rh2 C25 C30 -122.0(4) . . . . ? C24 Rh2 C25 C30 121.2(4) . . . . ? C23 Rh2 C25 C30 159.2(4) . . . . ? C22 Rh2 C25 C30 -159.5(4) . . . . ? C35 N31 C31 C32 -0.5(5) . . . . ? Rh1 N31 C31 C32 -176.9(3) . . . . ? N31 C31 C32 C33 -1.8(6) . . . . ? C31 C32 C33 C34 0.7(6) . . . . ? C32 C33 C34 C35 2.6(6) . . . . ? C31 N31 C35 C34 3.8(5) . . . . ? Rh1 N31 C35 C34 -179.4(3) . . . . ? C31 N31 C35 C36 -170.7(3) . . . . ? Rh1 N31 C35 C36 6.1(4) . . . . ? C33 C34 C35 N31 -4.9(6) . . . . ? C33 C34 C35 C36 169.0(4) . . . . ? N31 C35 C36 C41 1.2(4) . . . . ? C34 C35 C36 C41 -173.0(3) . . . . ? N31 C35 C36 C37 175.0(3) . . . . ? C34 C35 C36 C37 0.9(6) . . . . ? C41 C36 C37 C38 2.3(6) . . . . ? C35 C36 C37 C38 -171.3(4) . . . . ? C36 C37 C38 C39 -0.7(7) . . . . ? C37 C38 C39 C40 -0.7(7) . . . . ? C38 C39 C40 C41 0.5(6) . . . . ? C39 C40 C41 C36 1.0(6) . . . . ? C39 C40 C41 Rh1 -179.3(3) . . . . ? C37 C36 C41 C40 -2.4(5) . . . . ? C35 C36 C41 C40 171.8(3) . . . . ? C37 C36 C41 Rh1 177.9(3) . . . . ? C35 C36 C41 Rh1 -8.0(4) . . . . ? N31 Rh1 C41 C40 -171.2(3) . . . . ? N2 Rh1 C41 C40 -82.6(3) . . . . ? C14 Rh1 C41 C40 91.3(3) . . . . ? C12 Rh1 C41 C40 21.6(4) . . . . ? C13 Rh1 C41 C40 56.9(3) . . . . ? C11 Rh1 C41 C40 16.4(5) . . . . ? C15 Rh1 C41 C40 93.0(4) . . . . ? N31 Rh1 C41 C36 8.5(2) . . . . ? N2 Rh1 C41 C36 97.1(3) . . . . ? C14 Rh1 C41 C36 -89.0(3) . . . . ? C12 Rh1 C41 C36 -158.7(2) . . . . ? C13 Rh1 C41 C36 -123.4(3) . . . . ? C11 Rh1 C41 C36 -163.9(2) . . . . ? C15 Rh1 C41 C36 -87.3(4) . . . . ? C46 N42 C42 C43 -2.4(5) . . . . ? Rh2 N42 C42 C43 175.4(3) . . . . ? N42 C42 C43 C44 1.8(5) . . . . ? C42 C43 C44 C45 0.3(5) . . . . ? C43 C44 C45 C46 -1.7(5) . . . . ? C42 N42 C46 C45 0.9(5) . . . . ? Rh2 N42 C46 C45 -177.0(2) . . . . ? C42 N42 C46 C47 179.5(3) . . . . ? Rh2 N42 C46 C47 1.5(3) . . . . ? C44 C45 C46 N42 1.1(5) . . . . ? C44 C45 C46 C47 -177.2(3) . . . . ? N42 C46 C47 C52 -1.1(4) . . . . ? C45 C46 C47 C52 177.3(3) . . . . ? N42 C46 C47 C48 179.8(3) . . . . ? C45 C46 C47 C48 -1.8(5) . . . . ? C52 C47 C48 C49 0.1(6) . . . . ? C46 C47 C48 C49 179.1(4) . . . . ? C47 C48 C49 C50 -0.7(7) . . . . ? C48 C49 C50 C51 0.7(7) . . . . ? C49 C50 C51 C52 -0.1(6) . . . . ? C50 C51 C52 C47 -0.5(5) . . . . ? C50 C51 C52 Rh2 -179.1(3) . . . . ? C48 C47 C52 C51 0.5(5) . . . . ? C46 C47 C52 C51 -178.6(3) . . . . ? C48 C47 C52 Rh2 179.3(3) . . . . ? C46 C47 C52 Rh2 0.2(4) . . . . ? N42 Rh2 C52 C51 179.2(3) . . . . ? N4 Rh2 C52 C51 -93.4(3) . . . . ? C25 Rh2 C52 C51 56.5(3) . . . . ? C21 Rh2 C52 C51 87.2(3) . . . . ? C24 Rh2 C52 C51 18.3(3) . . . . ? C23 Rh2 C52 C51 2.1(4) . . . . ? C22 Rh2 C52 C51 74.3(5) . . . . ? N42 Rh2 C52 C47 0.5(2) . . . . ? N4 Rh2 C52 C47 87.9(2) . . . . ? C25 Rh2 C52 C47 -122.3(2) . . . . ? C21 Rh2 C52 C47 -91.5(3) . . . . ? C24 Rh2 C52 C47 -160.4(2) . . . . ? C23 Rh2 C52 C47 -176.6(2) . . . . ? C22 Rh2 C52 C47 -104.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.405 _refine_diff_density_min -0.700 _refine_diff_density_rms 0.084 _database_code_depnum_ccdc_archive 'CCDC 945553' ####################################################################### # # 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_comp9 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H49 Ir N8 Rh 3+, 3(F6 P 1-), C2 H3 N' _chemical_formula_sum 'C44 H52 F18 Ir N9 P3 Rh' _chemical_formula_weight 1436.97 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' F F 0.0171 0.0103 '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' Rh Rh -1.1178 0.9187 '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 1 21/c 1' _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 12.9890(4) _cell_length_b 21.3738(5) _cell_length_c 20.4689(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.3110(10) _cell_angle_gamma 90.00 _cell_volume 5363.0(2) _cell_formula_units_Z 4 _cell_measurement_temperature 183(2) _cell_measurement_reflns_used 53615 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 2.981 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5871 _exptl_absorpt_correction_T_max 0.7548 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 183(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 85347 _diffrn_reflns_av_R_equivalents 0.0842 _diffrn_reflns_av_sigmaI/netI 0.0499 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12261 _reflns_number_gt 9389 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0671P)^2^+6.2915P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12261 _refine_ls_number_parameters 670 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1354 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.126 _refine_ls_restrained_S_all 1.126 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.364957(19) 0.326180(12) 0.482250(13) 0.02665(9) Uani 0.57 1 d P . . Ir2 Ir 0.04183(2) 0.136533(14) 0.325901(14) 0.02866(9) Uani 0.43 1 d P . . Rh1 Rh 0.04183(2) 0.136533(14) 0.325901(14) 0.02866(9) Uani 0.57 1 d P . . Rh2 Rh 0.364957(19) 0.326180(12) 0.482250(13) 0.02665(9) Uani 0.43 1 d P . . P1 P 0.53440(14) -0.00395(10) 0.28953(10) 0.0558(5) Uani 1 1 d . . . P2 P 0.96805(13) 0.11197(7) 0.63345(8) 0.0361(3) Uani 1 1 d . . . P3 P 0.13806(12) 0.61377(8) 0.50987(8) 0.0365(3) Uani 1 1 d . . . F1 F 0.5639(4) 0.0237(3) 0.2258(3) 0.102(2) Uani 1 1 d . . . F2 F 0.4461(4) 0.0478(2) 0.2846(3) 0.0860(15) Uani 1 1 d . . . F3 F 0.4436(4) -0.0442(3) 0.2365(3) 0.0935(17) Uani 1 1 d . . . F4 F 0.5035(4) -0.0356(2) 0.3515(2) 0.0732(13) Uani 1 1 d . . . F5 F 0.6242(5) -0.0547(3) 0.2968(3) 0.117(2) Uani 1 1 d . . . F6 F 0.6218(4) 0.0376(3) 0.3428(3) 0.117(2) Uani 1 1 d . . . F7 F 0.9413(4) 0.17999(18) 0.6023(3) 0.0719(13) Uani 1 1 d . . . F8 F 0.8721(4) 0.0865(3) 0.5695(2) 0.0855(16) Uani 1 1 d . . . F9 F 0.8833(3) 0.12128(19) 0.67459(19) 0.0526(9) Uani 1 1 d . . . F10 F 0.9920(4) 0.0444(2) 0.6640(3) 0.0937(18) Uani 1 1 d . . . F11 F 1.0616(3) 0.1402(3) 0.6963(2) 0.0840(16) Uani 1 1 d . . . F12 F 1.0522(3) 0.10297(17) 0.59162(19) 0.0514(9) Uani 1 1 d . . . F13 F 0.1092(4) 0.6395(2) 0.5735(2) 0.0738(13) Uani 1 1 d . . . F14 F 0.2147(4) 0.6707(2) 0.5099(3) 0.0888(16) Uani 1 1 d . . . F15 F 0.2369(3) 0.5748(2) 0.5585(2) 0.0751(13) Uani 1 1 d . . . F16 F 0.1628(4) 0.5861(2) 0.4440(2) 0.0751(13) Uani 1 1 d . . . F17 F 0.0619(3) 0.55520(18) 0.5085(2) 0.0613(11) Uani 1 1 d . . . F18 F 0.0376(3) 0.6507(2) 0.4594(2) 0.0679(12) Uani 1 1 d . . . N1 N 0.3341(4) 0.2439(2) 0.3553(2) 0.0408(12) Uani 1 1 d . . . N2 N 0.2947(3) 0.25833(19) 0.4069(2) 0.0288(9) Uani 1 1 d . . . N3 N 0.2041(3) 0.2301(2) 0.4014(2) 0.0326(10) Uani 1 1 d . . . N4 N 0.1816(4) 0.1950(2) 0.3443(2) 0.0323(10) Uani 1 1 d . . . N5 N 0.5831(10) 0.1987(6) 0.2040(7) 0.147(4) Uiso 1 1 d . . . N31 N 0.4922(3) 0.2616(2) 0.5216(2) 0.0323(10) Uani 1 1 d . . . N40 N 0.3087(4) 0.2702(2) 0.5486(2) 0.0332(10) Uani 1 1 d . . . N41 N 0.1535(3) 0.0810(2) 0.4004(2) 0.0301(10) Uani 1 1 d . . . N50 N 0.1017(3) 0.0758(2) 0.2657(2) 0.0303(10) Uani 1 1 d . . . C1 C 0.6089(14) 0.1967(8) 0.3372(8) 0.169(6) Uiso 1 1 d . . . H1A H 0.6351 0.2365 0.3605 0.203 Uiso 1 1 calc R . . H1B H 0.6611 0.1635 0.3587 0.203 Uiso 1 1 calc R . . H1C H 0.5378 0.1866 0.3415 0.203 Uiso 1 1 calc R . . C2 C 0.5976(13) 0.2021(8) 0.2610(10) 0.149(5) Uiso 1 1 d . . . C5 C 0.2620(5) 0.2030(3) 0.3164(3) 0.0335(12) Uani 1 1 d . . . C6 C 0.2773(6) 0.1735(3) 0.2551(3) 0.0517(17) Uani 1 1 d . . . H6A H 0.2097 0.1769 0.2157 0.062 Uiso 1 1 calc R . . H6B H 0.2960 0.1293 0.2649 0.062 Uiso 1 1 calc R . . H6C H 0.3364 0.1948 0.2441 0.062 Uiso 1 1 calc R . . C11 C 0.4314(5) 0.4022(3) 0.4400(3) 0.0393(14) Uani 1 1 d . . . C12 C 0.4567(5) 0.4120(2) 0.5140(3) 0.0391(14) Uani 1 1 d . . . C13 C 0.3566(5) 0.4168(3) 0.5282(3) 0.0406(14) Uani 1 1 d . . . C14 C 0.2689(5) 0.4109(2) 0.4643(3) 0.0411(15) Uani 1 1 d . . . C15 C 0.3158(5) 0.4035(2) 0.4101(3) 0.0393(14) Uani 1 1 d . . . C16 C 0.5112(6) 0.4006(3) 0.4007(4) 0.0574(19) Uani 1 1 d . . . H16A H 0.5822 0.3859 0.4313 0.069 Uiso 1 1 calc R . . H16B H 0.5191 0.4428 0.3841 0.069 Uiso 1 1 calc R . . H16C H 0.4842 0.3722 0.3611 0.069 Uiso 1 1 calc R . . C17 C 0.5693(5) 0.4160(3) 0.5656(4) 0.0549(18) Uani 1 1 d . . . H17A H 0.6177 0.3875 0.5519 0.066 Uiso 1 1 calc R . . H17B H 0.5675 0.4042 0.6114 0.066 Uiso 1 1 calc R . . H17C H 0.5964 0.4589 0.5671 0.066 Uiso 1 1 calc R . . C18 C 0.3448(7) 0.4266(4) 0.5983(4) 0.064(2) Uani 1 1 d . . . H18A H 0.2813 0.4032 0.6009 0.076 Uiso 1 1 calc R . . H18B H 0.3347 0.4712 0.6052 0.076 Uiso 1 1 calc R . . H18C H 0.4106 0.4116 0.6343 0.076 Uiso 1 1 calc R . . C19 C 0.1502(5) 0.4199(3) 0.4539(4) 0.0582(19) Uani 1 1 d . . . H19A H 0.1065 0.3970 0.4125 0.070 Uiso 1 1 calc R . . H19B H 0.1323 0.4645 0.4479 0.070 Uiso 1 1 calc R . . H19C H 0.1341 0.4041 0.4944 0.070 Uiso 1 1 calc R . . C20 C 0.2556(6) 0.3979(3) 0.3346(4) 0.0594(19) Uani 1 1 d . . . H20A H 0.1809 0.3838 0.3276 0.071 Uiso 1 1 calc R . . H20B H 0.2925 0.3675 0.3142 0.071 Uiso 1 1 calc R . . H20C H 0.2537 0.4388 0.3125 0.071 Uiso 1 1 calc R . . C21 C -0.1079(5) 0.1750(3) 0.2558(3) 0.0334(12) Uani 1 1 d . . . C22 C -0.0692(5) 0.2148(2) 0.3146(3) 0.0332(12) Uani 1 1 d . . . C23 C -0.0641(4) 0.1798(2) 0.3751(3) 0.0309(12) Uani 1 1 d . . . C24 C -0.1026(4) 0.1177(3) 0.3541(3) 0.0334(12) Uani 1 1 d . . . C25 C -0.1285(4) 0.1142(3) 0.2801(3) 0.0332(12) Uani 1 1 d . . . C26 C -0.1363(6) 0.1955(3) 0.1821(3) 0.0472(16) Uani 1 1 d . . . H26A H -0.1385 0.1590 0.1527 0.057 Uiso 1 1 calc R . . H26B H -0.0811 0.2250 0.1779 0.057 Uiso 1 1 calc R . . H26C H -0.2079 0.2159 0.1674 0.057 Uiso 1 1 calc R . . C27 C -0.0410(6) 0.2814(3) 0.3123(3) 0.0484(16) Uani 1 1 d . . . H27A H 0.0140 0.2932 0.3563 0.058 Uiso 1 1 calc R . . H27B H -0.1065 0.3070 0.3046 0.058 Uiso 1 1 calc R . . H27C H -0.0117 0.2881 0.2744 0.058 Uiso 1 1 calc R . . C28 C -0.0386(5) 0.2064(3) 0.4463(3) 0.0423(14) Uani 1 1 d . . . H28A H 0.0175 0.2388 0.4538 0.051 Uiso 1 1 calc R . . H28B H -0.0119 0.1730 0.4806 0.051 Uiso 1 1 calc R . . H28C H -0.1048 0.2248 0.4512 0.051 Uiso 1 1 calc R . . C29 C -0.1162(5) 0.0665(3) 0.3998(3) 0.0428(14) Uani 1 1 d . . . H29A H -0.0611 0.0708 0.4458 0.051 Uiso 1 1 calc R . . H29B H -0.1074 0.0260 0.3799 0.051 Uiso 1 1 calc R . . H29C H -0.1892 0.0690 0.4039 0.051 Uiso 1 1 calc R . . C30 C -0.1753(5) 0.0588(3) 0.2370(3) 0.0446(15) Uani 1 1 d . . . H30A H -0.1530 0.0589 0.1956 0.054 Uiso 1 1 calc R . . H30B H -0.2550 0.0603 0.2230 0.054 Uiso 1 1 calc R . . H30C H -0.1486 0.0206 0.2637 0.054 Uiso 1 1 calc R . . C31 C 0.5836(5) 0.2605(3) 0.5042(3) 0.0401(14) Uani 1 1 d . . . H31 H 0.5928 0.2906 0.4724 0.048 Uiso 1 1 calc R . . C32 C 0.6636(5) 0.2169(3) 0.5315(4) 0.0549(18) Uani 1 1 d . . . H32 H 0.7291 0.2178 0.5204 0.066 Uiso 1 1 calc R . . C33 C 0.6481(6) 0.1718(4) 0.5750(5) 0.070(2) Uani 1 1 d . . . H33 H 0.7015 0.1403 0.5933 0.084 Uiso 1 1 calc R . . C34 C 0.5549(6) 0.1731(3) 0.5913(4) 0.059(2) Uani 1 1 d . . . H34 H 0.5433 0.1418 0.6211 0.071 Uiso 1 1 calc R . . C35 C 0.4774(5) 0.2182(3) 0.5658(3) 0.0393(13) Uani 1 1 d . . . C36 C 0.3759(5) 0.2250(3) 0.5817(3) 0.0386(13) Uani 1 1 d . . . C37 C 0.3468(6) 0.1859(3) 0.6278(4) 0.0519(17) Uani 1 1 d . . . H37 H 0.3955 0.1541 0.6521 0.062 Uiso 1 1 calc R . . C38 C 0.2484(6) 0.1933(4) 0.6380(3) 0.0569(19) Uani 1 1 d . . . H38 H 0.2287 0.1669 0.6692 0.068 Uiso 1 1 calc R . . C39 C 0.1781(5) 0.2398(3) 0.6021(3) 0.0500(17) Uani 1 1 d . . . H39 H 0.1087 0.2455 0.6073 0.060 Uiso 1 1 calc R . . C40 C 0.2128(5) 0.2782(3) 0.5581(3) 0.0423(14) Uani 1 1 d . . . H40 H 0.1664 0.3111 0.5342 0.051 Uiso 1 1 calc R . . C41 C 0.1752(5) 0.0870(3) 0.4687(3) 0.0372(13) Uani 1 1 d . . . H41 H 0.1318 0.1146 0.4850 0.045 Uiso 1 1 calc R . . C42 C 0.2585(5) 0.0546(3) 0.5160(3) 0.0441(15) Uani 1 1 d . . . H42 H 0.2713 0.0585 0.5643 0.053 Uiso 1 1 calc R . . C43 C 0.3232(5) 0.0161(3) 0.4913(3) 0.0495(16) Uani 1 1 d . . . H43 H 0.3825 -0.0059 0.5228 0.059 Uiso 1 1 calc R . . C44 C 0.3016(5) 0.0096(3) 0.4207(3) 0.0415(14) Uani 1 1 d . . . H44 H 0.3459 -0.0163 0.4033 0.050 Uiso 1 1 calc R . . C45 C 0.2141(4) 0.0417(2) 0.3764(3) 0.0309(12) Uani 1 1 d . . . C46 C 0.1790(4) 0.0356(3) 0.3007(3) 0.0336(12) Uani 1 1 d . . . C47 C 0.2198(5) -0.0093(3) 0.2665(3) 0.0411(14) Uani 1 1 d . . . H47 H 0.2752 -0.0373 0.2920 0.049 Uiso 1 1 calc R . . C48 C 0.1793(5) -0.0126(3) 0.1953(3) 0.0460(15) Uani 1 1 d . . . H48 H 0.2063 -0.0432 0.1714 0.055 Uiso 1 1 calc R . . C49 C 0.0996(5) 0.0285(3) 0.1592(3) 0.0438(15) Uani 1 1 d . . . H49 H 0.0702 0.0266 0.1102 0.053 Uiso 1 1 calc R . . C50 C 0.0633(5) 0.0726(3) 0.1958(3) 0.0379(13) Uani 1 1 d . . . H50 H 0.0094 0.1018 0.1710 0.046 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01934(13) 0.02667(15) 0.03214(16) -0.00260(10) 0.00608(10) -0.00277(10) Ir2 0.02937(17) 0.03003(17) 0.02479(16) -0.00265(11) 0.00655(12) -0.00366(12) Rh1 0.02937(17) 0.03003(17) 0.02479(16) -0.00265(11) 0.00655(12) -0.00366(12) Rh2 0.01934(13) 0.02667(15) 0.03214(16) -0.00260(10) 0.00608(10) -0.00277(10) P1 0.0342(9) 0.0752(13) 0.0550(11) 0.0281(10) 0.0106(8) 0.0053(9) P2 0.0370(8) 0.0369(8) 0.0357(8) 0.0013(6) 0.0135(6) -0.0014(6) P3 0.0319(8) 0.0413(9) 0.0370(8) 0.0071(6) 0.0123(6) 0.0000(6) F1 0.053(3) 0.161(5) 0.090(3) 0.079(4) 0.023(3) 0.009(3) F2 0.061(3) 0.073(3) 0.119(4) 0.027(3) 0.025(3) 0.015(2) F3 0.076(3) 0.131(5) 0.083(3) -0.028(3) 0.038(3) -0.021(3) F4 0.073(3) 0.096(3) 0.059(3) 0.030(2) 0.033(2) 0.010(3) F5 0.104(4) 0.138(5) 0.138(5) 0.083(4) 0.080(4) 0.074(4) F6 0.059(3) 0.149(6) 0.121(5) 0.014(4) -0.002(3) -0.029(3) F7 0.092(3) 0.048(2) 0.096(3) 0.026(2) 0.058(3) 0.017(2) F8 0.062(3) 0.129(4) 0.065(3) -0.042(3) 0.021(2) -0.034(3) F9 0.045(2) 0.068(3) 0.052(2) 0.0060(19) 0.0262(18) 0.0001(19) F10 0.103(4) 0.059(3) 0.151(5) 0.053(3) 0.085(4) 0.032(3) F11 0.047(2) 0.158(5) 0.046(2) -0.027(3) 0.014(2) -0.027(3) F12 0.055(2) 0.053(2) 0.057(2) -0.0071(18) 0.0327(19) 0.0010(18) F13 0.114(4) 0.062(3) 0.055(3) -0.013(2) 0.043(3) -0.006(3) F14 0.072(3) 0.065(3) 0.128(4) 0.023(3) 0.032(3) -0.025(2) F15 0.049(2) 0.090(3) 0.074(3) 0.036(3) 0.004(2) 0.011(2) F16 0.101(4) 0.082(3) 0.063(3) 0.018(2) 0.055(3) 0.029(3) F17 0.058(3) 0.051(2) 0.084(3) -0.001(2) 0.035(2) -0.0088(19) F18 0.054(3) 0.074(3) 0.072(3) 0.022(2) 0.016(2) 0.024(2) N1 0.050(3) 0.041(3) 0.040(3) -0.002(2) 0.025(2) -0.001(2) N2 0.030(2) 0.024(2) 0.032(2) -0.0061(18) 0.0094(19) -0.0088(18) N3 0.029(2) 0.032(2) 0.037(3) -0.015(2) 0.012(2) -0.013(2) N4 0.035(3) 0.031(2) 0.031(2) -0.0012(19) 0.012(2) -0.006(2) N31 0.023(2) 0.032(2) 0.039(3) -0.001(2) 0.0062(19) -0.0003(19) N40 0.029(2) 0.038(3) 0.033(2) -0.005(2) 0.0097(19) -0.007(2) N41 0.029(2) 0.030(2) 0.029(2) -0.0003(19) 0.0074(19) -0.0033(19) N50 0.027(2) 0.035(2) 0.032(2) -0.0086(19) 0.0126(19) -0.0032(19) C5 0.043(3) 0.031(3) 0.031(3) -0.004(2) 0.017(2) -0.009(2) C6 0.065(5) 0.051(4) 0.048(4) -0.005(3) 0.031(3) -0.013(3) C11 0.028(3) 0.029(3) 0.057(4) 0.009(3) 0.009(3) -0.004(2) C12 0.036(3) 0.015(2) 0.059(4) -0.009(2) 0.006(3) -0.016(2) C13 0.041(3) 0.022(3) 0.062(4) -0.017(3) 0.021(3) -0.007(2) C14 0.030(3) 0.019(3) 0.071(4) -0.006(3) 0.012(3) 0.009(2) C15 0.036(3) 0.018(3) 0.056(4) 0.008(2) 0.004(3) 0.002(2) C16 0.049(4) 0.056(4) 0.071(5) 0.018(4) 0.024(4) -0.005(3) C17 0.033(3) 0.047(4) 0.069(5) -0.006(3) -0.005(3) -0.012(3) C18 0.071(5) 0.060(5) 0.065(5) -0.029(4) 0.028(4) -0.010(4) C19 0.030(3) 0.046(4) 0.095(6) -0.006(4) 0.016(3) 0.008(3) C20 0.060(5) 0.050(4) 0.054(4) 0.018(3) -0.001(3) 0.009(3) C21 0.031(3) 0.037(3) 0.028(3) -0.004(2) 0.004(2) 0.007(2) C22 0.043(3) 0.026(3) 0.033(3) -0.002(2) 0.015(2) 0.008(2) C23 0.033(3) 0.032(3) 0.029(3) -0.001(2) 0.013(2) 0.005(2) C24 0.024(3) 0.041(3) 0.037(3) 0.000(2) 0.012(2) 0.002(2) C25 0.029(3) 0.034(3) 0.035(3) -0.005(2) 0.007(2) -0.001(2) C26 0.063(4) 0.046(4) 0.029(3) -0.001(3) 0.010(3) 0.012(3) C27 0.066(4) 0.037(3) 0.043(4) 0.000(3) 0.019(3) 0.005(3) C28 0.050(4) 0.043(3) 0.034(3) -0.005(3) 0.015(3) 0.001(3) C29 0.041(3) 0.041(3) 0.049(4) 0.008(3) 0.018(3) 0.000(3) C30 0.035(3) 0.042(3) 0.050(4) -0.013(3) 0.004(3) -0.008(3) C31 0.030(3) 0.040(3) 0.051(4) 0.004(3) 0.014(3) -0.001(3) C32 0.030(3) 0.044(4) 0.087(5) 0.007(4) 0.014(3) 0.004(3) C33 0.043(4) 0.054(5) 0.105(7) 0.017(4) 0.014(4) 0.013(3) C34 0.048(4) 0.048(4) 0.073(5) 0.024(4) 0.009(4) 0.008(3) C35 0.037(3) 0.031(3) 0.046(3) 0.003(3) 0.009(3) -0.006(3) C36 0.037(3) 0.035(3) 0.039(3) -0.002(3) 0.007(3) -0.009(3) C37 0.054(4) 0.049(4) 0.048(4) 0.009(3) 0.011(3) -0.016(3) C38 0.061(5) 0.072(5) 0.039(4) 0.001(3) 0.018(3) -0.030(4) C39 0.044(4) 0.069(5) 0.042(4) -0.012(3) 0.020(3) -0.023(3) C40 0.033(3) 0.057(4) 0.037(3) -0.010(3) 0.011(3) -0.011(3) C41 0.046(3) 0.036(3) 0.027(3) -0.001(2) 0.008(2) -0.005(3) C42 0.051(4) 0.046(4) 0.030(3) 0.005(3) 0.006(3) 0.002(3) C43 0.041(4) 0.057(4) 0.041(3) 0.014(3) 0.001(3) 0.007(3) C44 0.039(3) 0.042(3) 0.043(3) 0.003(3) 0.013(3) 0.002(3) C45 0.026(3) 0.029(3) 0.037(3) -0.004(2) 0.009(2) -0.004(2) C46 0.028(3) 0.036(3) 0.037(3) -0.004(2) 0.011(2) -0.004(2) C47 0.037(3) 0.040(3) 0.050(4) -0.003(3) 0.019(3) -0.003(3) C48 0.050(4) 0.043(4) 0.054(4) -0.017(3) 0.029(3) -0.004(3) C49 0.037(3) 0.064(4) 0.030(3) -0.015(3) 0.011(3) -0.007(3) C50 0.035(3) 0.048(3) 0.026(3) -0.011(3) 0.004(2) -0.004(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 N2 2.094(4) . ? Ir1 N31 2.099(4) . ? Ir1 N40 2.113(5) . ? Ir1 C11 2.151(6) . ? Ir1 C14 2.160(5) . ? Ir1 C12 2.166(5) . ? Ir1 C15 2.168(5) . ? Ir1 C13 2.172(5) . ? Ir2 N41 2.092(4) . ? Ir2 N50 2.108(4) . ? Ir2 N4 2.133(4) . ? Ir2 C25 2.152(5) . ? Ir2 C21 2.162(5) . ? Ir2 C23 2.163(5) . ? Ir2 C22 2.171(5) . ? Ir2 C24 2.175(5) . ? P1 F5 1.563(5) . ? P1 F6 1.564(6) . ? P1 F3 1.569(5) . ? P1 F2 1.572(5) . ? P1 F1 1.589(5) . ? P1 F4 1.602(4) . ? P2 F10 1.564(4) . ? P2 F11 1.570(4) . ? P2 F8 1.576(4) . ? P2 F7 1.579(4) . ? P2 F9 1.604(4) . ? P2 F12 1.608(4) . ? P3 F13 1.569(4) . ? P3 F14 1.572(4) . ? P3 F15 1.577(4) . ? P3 F18 1.581(4) . ? P3 F17 1.590(4) . ? P3 F16 1.598(4) . ? N1 C5 1.334(7) . ? N1 N2 1.352(6) . ? N2 N3 1.294(6) . ? N3 N4 1.338(6) . ? N4 C5 1.356(7) . ? N5 C2 1.120(17) . ? N31 C31 1.348(7) . ? N31 C35 1.353(7) . ? N40 C36 1.329(7) . ? N40 C40 1.334(7) . ? N41 C41 1.337(7) . ? N41 C45 1.351(7) . ? N50 C46 1.336(7) . ? N50 C50 1.352(7) . ? C1 C2 1.52(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C5 C6 1.474(8) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C15 1.421(8) . ? C11 C12 1.455(9) . ? C11 C16 1.508(9) . ? C12 C13 1.426(8) . ? C12 C17 1.497(8) . ? C13 C14 1.428(9) . ? C13 C18 1.507(9) . ? C14 C15 1.439(9) . ? C14 C19 1.498(8) . ? C15 C20 1.487(9) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.424(7) . ? C21 C25 1.447(8) . ? C21 C26 1.495(8) . ? C22 C23 1.432(8) . ? C22 C27 1.473(8) . ? C23 C24 1.433(8) . ? C23 C28 1.496(7) . ? C24 C25 1.440(8) . ? C24 C29 1.488(8) . ? C25 C30 1.482(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.371(8) . ? C31 H31 0.9500 . ? C32 C33 1.370(10) . ? C32 H32 0.9500 . ? C33 C34 1.359(11) . ? C33 H33 0.9500 . ? C34 C35 1.367(9) . ? C34 H34 0.9500 . ? C35 C36 1.466(8) . ? C36 C37 1.402(9) . ? C37 C38 1.370(10) . ? C37 H37 0.9500 . ? C38 C39 1.384(10) . ? C38 H38 0.9500 . ? C39 C40 1.398(9) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.377(8) . ? C41 H41 0.9500 . ? C42 C43 1.385(9) . ? C42 H42 0.9500 . ? C43 C44 1.384(9) . ? C43 H43 0.9500 . ? C44 C45 1.379(8) . ? C44 H44 0.9500 . ? C45 C46 1.469(8) . ? C46 C47 1.391(8) . ? C47 C48 1.377(9) . ? C47 H47 0.9500 . ? C48 C49 1.372(9) . ? C48 H48 0.9500 . ? C49 C50 1.381(8) . ? C49 H49 0.9500 . ? C50 H50 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 N2 Ir1 N31 85.62(17) . . ? N2 Ir1 N40 85.56(17) . . ? N31 Ir1 N40 77.12(18) . . ? N2 Ir1 C11 111.2(2) . . ? N31 Ir1 C11 106.3(2) . . ? N40 Ir1 C11 162.9(2) . . ? N2 Ir1 C14 111.6(2) . . ? N31 Ir1 C14 162.5(2) . . ? N40 Ir1 C14 106.3(2) . . ? C11 Ir1 C14 65.4(2) . . ? N2 Ir1 C12 150.4(2) . . ? N31 Ir1 C12 99.0(2) . . ? N40 Ir1 C12 124.0(2) . . ? C11 Ir1 C12 39.4(2) . . ? C14 Ir1 C12 64.6(2) . . ? N2 Ir1 C15 93.9(2) . . ? N31 Ir1 C15 141.3(2) . . ? N40 Ir1 C15 141.5(2) . . ? C11 Ir1 C15 38.4(2) . . ? C14 Ir1 C15 38.9(2) . . ? C12 Ir1 C15 64.4(2) . . ? N2 Ir1 C13 149.9(2) . . ? N31 Ir1 C13 124.5(2) . . ? N40 Ir1 C13 98.6(2) . . ? C11 Ir1 C13 65.4(2) . . ? C14 Ir1 C13 38.5(2) . . ? C12 Ir1 C13 38.4(2) . . ? C15 Ir1 C13 64.5(2) . . ? N41 Ir2 N50 77.06(17) . . ? N41 Ir2 N4 81.91(17) . . ? N50 Ir2 N4 90.36(17) . . ? N41 Ir2 C25 123.83(19) . . ? N50 Ir2 C25 97.70(19) . . ? N4 Ir2 C25 154.1(2) . . ? N41 Ir2 C21 162.6(2) . . ? N50 Ir2 C21 105.70(19) . . ? N4 Ir2 C21 114.9(2) . . ? C25 Ir2 C21 39.2(2) . . ? N41 Ir2 C23 107.29(19) . . ? N50 Ir2 C23 161.80(19) . . ? N4 Ir2 C23 107.66(19) . . ? C25 Ir2 C23 65.0(2) . . ? C21 Ir2 C23 64.9(2) . . ? N41 Ir2 C22 142.32(19) . . ? N50 Ir2 C22 140.58(19) . . ? N4 Ir2 C22 93.7(2) . . ? C25 Ir2 C22 64.7(2) . . ? C21 Ir2 C22 38.4(2) . . ? C23 Ir2 C22 38.6(2) . . ? N41 Ir2 C24 98.76(19) . . ? N50 Ir2 C24 123.96(19) . . ? N4 Ir2 C24 145.15(19) . . ? C25 Ir2 C24 38.9(2) . . ? C21 Ir2 C24 65.2(2) . . ? C23 Ir2 C24 38.6(2) . . ? C22 Ir2 C24 64.6(2) . . ? F5 P1 F6 88.9(4) . . ? F5 P1 F3 93.0(4) . . ? F6 P1 F3 178.1(4) . . ? F5 P1 F2 178.2(4) . . ? F6 P1 F2 89.5(3) . . ? F3 P1 F2 88.6(3) . . ? F5 P1 F1 87.8(3) . . ? F6 P1 F1 92.6(3) . . ? F3 P1 F1 88.1(3) . . ? F2 P1 F1 93.1(3) . . ? F5 P1 F4 90.4(3) . . ? F6 P1 F4 90.1(3) . . ? F3 P1 F4 89.3(3) . . ? F2 P1 F4 88.8(3) . . ? F1 P1 F4 176.7(4) . . ? F10 P2 F11 91.7(3) . . ? F10 P2 F8 90.6(3) . . ? F11 P2 F8 177.5(3) . . ? F10 P2 F7 178.8(3) . . ? F11 P2 F7 89.1(3) . . ? F8 P2 F7 88.6(3) . . ? F10 P2 F9 89.2(2) . . ? F11 P2 F9 90.1(2) . . ? F8 P2 F9 89.3(2) . . ? F7 P2 F9 90.0(2) . . ? F10 P2 F12 91.3(2) . . ? F11 P2 F12 90.2(2) . . ? F8 P2 F12 90.4(2) . . ? F7 P2 F12 89.6(2) . . ? F9 P2 F12 179.5(2) . . ? F13 P3 F14 93.1(3) . . ? F13 P3 F15 91.6(3) . . ? F14 P3 F15 91.4(3) . . ? F13 P3 F18 89.8(3) . . ? F14 P3 F18 90.0(3) . . ? F15 P3 F18 177.9(3) . . ? F13 P3 F17 88.4(2) . . ? F14 P3 F17 178.5(3) . . ? F15 P3 F17 88.1(2) . . ? F18 P3 F17 90.4(2) . . ? F13 P3 F16 177.7(3) . . ? F14 P3 F16 89.0(3) . . ? F15 P3 F16 89.4(3) . . ? F18 P3 F16 89.2(2) . . ? F17 P3 F16 89.5(3) . . ? C5 N1 N2 104.1(4) . . ? N3 N2 N1 113.2(4) . . ? N3 N2 Ir1 123.3(3) . . ? N1 N2 Ir1 123.2(3) . . ? N2 N3 N4 105.5(4) . . ? N3 N4 C5 108.7(4) . . ? N3 N4 Ir2 114.2(3) . . ? C5 N4 Ir2 136.8(4) . . ? C31 N31 C35 119.8(5) . . ? C31 N31 Ir1 124.1(4) . . ? C35 N31 Ir1 116.1(4) . . ? C36 N40 C40 120.4(5) . . ? C36 N40 Ir1 115.6(4) . . ? C40 N40 Ir1 124.1(4) . . ? C41 N41 C45 119.6(5) . . ? C41 N41 Ir2 124.3(4) . . ? C45 N41 Ir2 115.7(3) . . ? C46 N50 C50 119.0(5) . . ? C46 N50 Ir2 116.1(3) . . ? C50 N50 Ir2 124.8(4) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N5 C2 C1 171.0(19) . . ? N1 C5 N4 108.5(5) . . ? N1 C5 C6 121.5(5) . . ? N4 C5 C6 130.0(5) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C15 C11 C12 106.8(5) . . ? C15 C11 C16 125.8(6) . . ? C12 C11 C16 126.9(5) . . ? C15 C11 Ir1 71.4(3) . . ? C12 C11 Ir1 70.9(3) . . ? C16 C11 Ir1 129.4(4) . . ? C13 C12 C11 108.4(5) . . ? C13 C12 C17 126.6(6) . . ? C11 C12 C17 125.0(6) . . ? C13 C12 Ir1 71.0(3) . . ? C11 C12 Ir1 69.7(3) . . ? C17 C12 Ir1 124.9(4) . . ? C12 C13 C14 108.1(5) . . ? C12 C13 C18 126.2(6) . . ? C14 C13 C18 125.7(6) . . ? C12 C13 Ir1 70.6(3) . . ? C14 C13 Ir1 70.3(3) . . ? C18 C13 Ir1 124.8(5) . . ? C13 C14 C15 107.7(5) . . ? C13 C14 C19 126.2(6) . . ? C15 C14 C19 125.6(6) . . ? C13 C14 Ir1 71.2(3) . . ? C15 C14 Ir1 70.9(3) . . ? C19 C14 Ir1 129.9(4) . . ? C11 C15 C14 109.0(5) . . ? C11 C15 C20 124.3(6) . . ? C14 C15 C20 126.7(6) . . ? C11 C15 Ir1 70.2(3) . . ? C14 C15 Ir1 70.3(3) . . ? C20 C15 Ir1 125.6(4) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 107.5(5) . . ? C22 C21 C26 125.2(5) . . ? C25 C21 C26 126.8(5) . . ? C22 C21 Ir2 71.2(3) . . ? C25 C21 Ir2 70.0(3) . . ? C26 C21 Ir2 130.5(4) . . ? C21 C22 C23 108.7(5) . . ? C21 C22 C27 125.0(5) . . ? C23 C22 C27 126.3(5) . . ? C21 C22 Ir2 70.5(3) . . ? C23 C22 Ir2 70.4(3) . . ? C27 C22 Ir2 125.8(4) . . ? C24 C23 C22 108.2(5) . . ? C24 C23 C28 126.0(5) . . ? C22 C23 C28 125.2(5) . . ? C24 C23 Ir2 71.1(3) . . ? C22 C23 Ir2 71.0(3) . . ? C28 C23 Ir2 130.3(4) . . ? C23 C24 C25 107.5(5) . . ? C23 C24 C29 126.4(5) . . ? C25 C24 C29 126.1(5) . . ? C23 C24 Ir2 70.3(3) . . ? C25 C24 Ir2 69.7(3) . . ? C29 C24 Ir2 126.6(4) . . ? C24 C25 C21 108.1(5) . . ? C24 C25 C30 125.1(5) . . ? C21 C25 C30 126.7(5) . . ? C24 C25 Ir2 71.4(3) . . ? C21 C25 Ir2 70.8(3) . . ? C30 C25 Ir2 126.6(4) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N31 C31 C32 121.3(6) . . ? N31 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C33 C32 C31 119.2(7) . . ? C33 C32 H32 120.4 . . ? C31 C32 H32 120.4 . . ? C34 C33 C32 118.7(7) . . ? C34 C33 H33 120.7 . . ? C32 C33 H33 120.7 . . ? C33 C34 C35 121.6(7) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? N31 C35 C34 119.3(6) . . ? N31 C35 C36 114.7(5) . . ? C34 C35 C36 126.0(6) . . ? N40 C36 C37 119.9(6) . . ? N40 C36 C35 116.5(5) . . ? C37 C36 C35 123.6(6) . . ? C38 C37 C36 120.4(7) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 119.2(6) . . ? C37 C38 H38 120.4 . . ? C39 C38 H38 120.4 . . ? C38 C39 C40 117.7(6) . . ? C38 C39 H39 121.1 . . ? C40 C39 H39 121.1 . . ? N40 C40 C39 122.4(6) . . ? N40 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? N41 C41 C42 122.1(6) . . ? N41 C41 H41 118.9 . . ? C42 C41 H41 118.9 . . ? C41 C42 C43 118.2(6) . . ? C41 C42 H42 120.9 . . ? C43 C42 H42 120.9 . . ? C44 C43 C42 120.1(6) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C45 C44 C43 118.5(6) . . ? C45 C44 H44 120.8 . . ? C43 C44 H44 120.8 . . ? N41 C45 C44 121.4(5) . . ? N41 C45 C46 115.1(5) . . ? C44 C45 C46 123.5(5) . . ? N50 C46 C47 121.2(5) . . ? N50 C46 C45 115.1(5) . . ? C47 C46 C45 123.7(5) . . ? C48 C47 C46 119.4(6) . . ? C48 C47 H47 120.3 . . ? C46 C47 H47 120.3 . . ? C49 C48 C47 119.5(6) . . ? C49 C48 H48 120.2 . . ? C47 C48 H48 120.2 . . ? C48 C49 C50 118.5(5) . . ? C48 C49 H49 120.7 . . ? C50 C49 H49 120.7 . . ? N50 C50 C49 122.3(6) . . ? N50 C50 H50 118.8 . . ? C49 C50 H50 118.8 . . ? 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 N1 N2 N3 -1.0(6) . . . . ? C5 N1 N2 Ir1 -175.2(4) . . . . ? N31 Ir1 N2 N3 114.6(4) . . . . ? N40 Ir1 N2 N3 37.2(4) . . . . ? C11 Ir1 N2 N3 -139.5(4) . . . . ? C14 Ir1 N2 N3 -68.6(5) . . . . ? C12 Ir1 N2 N3 -144.9(4) . . . . ? C15 Ir1 N2 N3 -104.2(4) . . . . ? C13 Ir1 N2 N3 -62.2(6) . . . . ? N31 Ir1 N2 N1 -71.7(4) . . . . ? N40 Ir1 N2 N1 -149.1(4) . . . . ? C11 Ir1 N2 N1 34.1(5) . . . . ? C14 Ir1 N2 N1 105.1(4) . . . . ? C12 Ir1 N2 N1 28.8(7) . . . . ? C15 Ir1 N2 N1 69.4(4) . . . . ? C13 Ir1 N2 N1 111.4(5) . . . . ? N1 N2 N3 N4 0.4(6) . . . . ? Ir1 N2 N3 N4 174.6(3) . . . . ? N2 N3 N4 C5 0.3(6) . . . . ? N2 N3 N4 Ir2 175.3(3) . . . . ? N41 Ir2 N4 N3 -79.8(4) . . . . ? N50 Ir2 N4 N3 -156.7(4) . . . . ? C25 Ir2 N4 N3 94.6(5) . . . . ? C21 Ir2 N4 N3 95.7(4) . . . . ? C23 Ir2 N4 N3 25.8(4) . . . . ? C22 Ir2 N4 N3 62.5(4) . . . . ? C24 Ir2 N4 N3 13.9(6) . . . . ? N41 Ir2 N4 C5 93.1(6) . . . . ? N50 Ir2 N4 C5 16.3(6) . . . . ? C25 Ir2 N4 C5 -92.4(7) . . . . ? C21 Ir2 N4 C5 -91.3(6) . . . . ? C23 Ir2 N4 C5 -161.2(5) . . . . ? C22 Ir2 N4 C5 -124.5(6) . . . . ? C24 Ir2 N4 C5 -173.1(5) . . . . ? N2 Ir1 N31 C31 93.0(5) . . . . ? N40 Ir1 N31 C31 179.5(5) . . . . ? C11 Ir1 N31 C31 -17.8(5) . . . . ? C14 Ir1 N31 C31 -77.1(9) . . . . ? C12 Ir1 N31 C31 -57.6(5) . . . . ? C15 Ir1 N31 C31 2.3(6) . . . . ? C13 Ir1 N31 C31 -88.9(5) . . . . ? N2 Ir1 N31 C35 -85.3(4) . . . . ? N40 Ir1 N31 C35 1.1(4) . . . . ? C11 Ir1 N31 C35 163.8(4) . . . . ? C14 Ir1 N31 C35 104.6(8) . . . . ? C12 Ir1 N31 C35 124.1(4) . . . . ? C15 Ir1 N31 C35 -176.1(4) . . . . ? C13 Ir1 N31 C35 92.8(4) . . . . ? N2 Ir1 N40 C36 87.2(4) . . . . ? N31 Ir1 N40 C36 0.7(4) . . . . ? C11 Ir1 N40 C36 -103.1(7) . . . . ? C14 Ir1 N40 C36 -161.5(4) . . . . ? C12 Ir1 N40 C36 -91.5(4) . . . . ? C15 Ir1 N40 C36 177.9(4) . . . . ? C13 Ir1 N40 C36 -122.8(4) . . . . ? N2 Ir1 N40 C40 -92.7(4) . . . . ? N31 Ir1 N40 C40 -179.2(5) . . . . ? C11 Ir1 N40 C40 77.0(8) . . . . ? C14 Ir1 N40 C40 18.6(5) . . . . ? C12 Ir1 N40 C40 88.6(5) . . . . ? C15 Ir1 N40 C40 -2.0(6) . . . . ? C13 Ir1 N40 C40 57.2(5) . . . . ? N50 Ir2 N41 C41 179.8(5) . . . . ? N4 Ir2 N41 C41 87.5(4) . . . . ? C25 Ir2 N41 C41 -89.6(5) . . . . ? C21 Ir2 N41 C41 -78.9(8) . . . . ? C23 Ir2 N41 C41 -18.5(5) . . . . ? C22 Ir2 N41 C41 2.0(6) . . . . ? C24 Ir2 N41 C41 -57.2(5) . . . . ? N50 Ir2 N41 C45 7.1(4) . . . . ? N4 Ir2 N41 C45 -85.1(4) . . . . ? C25 Ir2 N41 C45 97.8(4) . . . . ? C21 Ir2 N41 C45 108.4(7) . . . . ? C23 Ir2 N41 C45 168.8(4) . . . . ? C22 Ir2 N41 C45 -170.6(4) . . . . ? C24 Ir2 N41 C45 130.1(4) . . . . ? N41 Ir2 N50 C46 -2.3(4) . . . . ? N4 Ir2 N50 C46 79.3(4) . . . . ? C25 Ir2 N50 C46 -125.3(4) . . . . ? C21 Ir2 N50 C46 -164.6(4) . . . . ? C23 Ir2 N50 C46 -108.4(6) . . . . ? C22 Ir2 N50 C46 175.6(4) . . . . ? C24 Ir2 N50 C46 -94.2(4) . . . . ? N41 Ir2 N50 C50 173.8(5) . . . . ? N4 Ir2 N50 C50 -104.6(5) . . . . ? C25 Ir2 N50 C50 50.7(5) . . . . ? C21 Ir2 N50 C50 11.5(5) . . . . ? C23 Ir2 N50 C50 67.6(8) . . . . ? C22 Ir2 N50 C50 -8.4(6) . . . . ? C24 Ir2 N50 C50 81.8(5) . . . . ? N2 N1 C5 N4 1.1(6) . . . . ? N2 N1 C5 C6 -177.7(5) . . . . ? N3 N4 C5 N1 -1.0(6) . . . . ? Ir2 N4 C5 N1 -174.2(4) . . . . ? N3 N4 C5 C6 177.8(6) . . . . ? Ir2 N4 C5 C6 4.5(10) . . . . ? N2 Ir1 C11 C15 68.1(4) . . . . ? N31 Ir1 C11 C15 159.8(3) . . . . ? N40 Ir1 C11 C15 -100.8(7) . . . . ? C14 Ir1 C11 C15 -36.8(4) . . . . ? C12 Ir1 C11 C15 -116.0(5) . . . . ? C13 Ir1 C11 C15 -79.3(4) . . . . ? N2 Ir1 C11 C12 -175.8(3) . . . . ? N31 Ir1 C11 C12 -84.2(4) . . . . ? N40 Ir1 C11 C12 15.2(8) . . . . ? C14 Ir1 C11 C12 79.2(4) . . . . ? C15 Ir1 C11 C12 116.0(5) . . . . ? C13 Ir1 C11 C12 36.7(3) . . . . ? N2 Ir1 C11 C16 -53.4(6) . . . . ? N31 Ir1 C11 C16 38.3(6) . . . . ? N40 Ir1 C11 C16 137.7(7) . . . . ? C14 Ir1 C11 C16 -158.3(6) . . . . ? C12 Ir1 C11 C16 122.5(7) . . . . ? C15 Ir1 C11 C16 -121.5(7) . . . . ? C13 Ir1 C11 C16 159.2(6) . . . . ? C15 C11 C12 C13 2.0(6) . . . . ? C16 C11 C12 C13 173.7(6) . . . . ? Ir1 C11 C12 C13 -60.8(4) . . . . ? C15 C11 C12 C17 -178.1(5) . . . . ? C16 C11 C12 C17 -6.4(9) . . . . ? Ir1 C11 C12 C17 119.1(6) . . . . ? C15 C11 C12 Ir1 62.8(4) . . . . ? C16 C11 C12 Ir1 -125.5(6) . . . . ? N2 Ir1 C12 C13 126.7(5) . . . . ? N31 Ir1 C12 C13 -136.3(4) . . . . ? N40 Ir1 C12 C13 -55.9(4) . . . . ? C11 Ir1 C12 C13 118.8(5) . . . . ? C14 Ir1 C12 C13 37.3(4) . . . . ? C15 Ir1 C12 C13 80.5(4) . . . . ? N2 Ir1 C12 C11 7.9(6) . . . . ? N31 Ir1 C12 C11 104.9(3) . . . . ? N40 Ir1 C12 C11 -174.7(3) . . . . ? C14 Ir1 C12 C11 -81.5(4) . . . . ? C15 Ir1 C12 C11 -38.3(3) . . . . ? C13 Ir1 C12 C11 -118.8(5) . . . . ? N2 Ir1 C12 C17 -111.4(6) . . . . ? N31 Ir1 C12 C17 -14.4(6) . . . . ? N40 Ir1 C12 C17 66.1(6) . . . . ? C11 Ir1 C12 C17 -119.3(7) . . . . ? C14 Ir1 C12 C17 159.2(7) . . . . ? C15 Ir1 C12 C17 -157.5(7) . . . . ? C13 Ir1 C12 C17 121.9(8) . . . . ? C11 C12 C13 C14 -0.5(6) . . . . ? C17 C12 C13 C14 179.6(5) . . . . ? Ir1 C12 C13 C14 -60.5(4) . . . . ? C11 C12 C13 C18 179.4(6) . . . . ? C17 C12 C13 C18 -0.4(10) . . . . ? Ir1 C12 C13 C18 119.4(6) . . . . ? C11 C12 C13 Ir1 60.0(4) . . . . ? C17 C12 C13 Ir1 -119.9(6) . . . . ? N2 Ir1 C13 C12 -128.0(4) . . . . ? N31 Ir1 C13 C12 55.8(4) . . . . ? N40 Ir1 C13 C12 136.1(4) . . . . ? C11 Ir1 C13 C12 -37.7(4) . . . . ? C14 Ir1 C13 C12 -118.5(5) . . . . ? C15 Ir1 C13 C12 -80.3(4) . . . . ? N2 Ir1 C13 C14 -9.5(6) . . . . ? N31 Ir1 C13 C14 174.3(3) . . . . ? N40 Ir1 C13 C14 -105.5(4) . . . . ? C11 Ir1 C13 C14 80.8(4) . . . . ? C12 Ir1 C13 C14 118.5(5) . . . . ? C15 Ir1 C13 C14 38.2(4) . . . . ? N2 Ir1 C13 C18 110.8(6) . . . . ? N31 Ir1 C13 C18 -65.3(6) . . . . ? N40 Ir1 C13 C18 14.9(6) . . . . ? C11 Ir1 C13 C18 -158.8(6) . . . . ? C14 Ir1 C13 C18 120.4(7) . . . . ? C12 Ir1 C13 C18 -121.2(7) . . . . ? C15 Ir1 C13 C18 158.6(6) . . . . ? C12 C13 C14 C15 -1.1(6) . . . . ? C18 C13 C14 C15 178.9(6) . . . . ? Ir1 C13 C14 C15 -61.9(4) . . . . ? C12 C13 C14 C19 -173.1(6) . . . . ? C18 C13 C14 C19 7.0(10) . . . . ? Ir1 C13 C14 C19 126.2(6) . . . . ? C12 C13 C14 Ir1 60.7(4) . . . . ? C18 C13 C14 Ir1 -119.2(6) . . . . ? N2 Ir1 C14 C13 174.9(3) . . . . ? N31 Ir1 C14 C13 -15.7(9) . . . . ? N40 Ir1 C14 C13 83.2(4) . . . . ? C11 Ir1 C14 C13 -80.8(4) . . . . ? C12 Ir1 C14 C13 -37.2(4) . . . . ? C15 Ir1 C14 C13 -117.2(5) . . . . ? N2 Ir1 C14 C15 -67.9(4) . . . . ? N31 Ir1 C14 C15 101.5(8) . . . . ? N40 Ir1 C14 C15 -159.6(3) . . . . ? C11 Ir1 C14 C15 36.4(3) . . . . ? C12 Ir1 C14 C15 80.0(4) . . . . ? C13 Ir1 C14 C15 117.2(5) . . . . ? N2 Ir1 C14 C19 53.0(7) . . . . ? N31 Ir1 C14 C19 -137.6(7) . . . . ? N40 Ir1 C14 C19 -38.7(7) . . . . ? C11 Ir1 C14 C19 157.3(7) . . . . ? C12 Ir1 C14 C19 -159.1(7) . . . . ? C15 Ir1 C14 C19 120.9(8) . . . . ? C13 Ir1 C14 C19 -121.9(8) . . . . ? C12 C11 C15 C14 -2.7(6) . . . . ? C16 C11 C15 C14 -174.5(6) . . . . ? Ir1 C11 C15 C14 59.7(4) . . . . ? C12 C11 C15 C20 177.4(5) . . . . ? C16 C11 C15 C20 5.6(9) . . . . ? Ir1 C11 C15 C20 -120.1(6) . . . . ? C12 C11 C15 Ir1 -62.5(4) . . . . ? C16 C11 C15 Ir1 125.7(6) . . . . ? C13 C14 C15 C11 2.4(6) . . . . ? C19 C14 C15 C11 174.4(6) . . . . ? Ir1 C14 C15 C11 -59.7(4) . . . . ? C13 C14 C15 C20 -177.7(5) . . . . ? C19 C14 C15 C20 -5.7(9) . . . . ? Ir1 C14 C15 C20 120.2(6) . . . . ? C13 C14 C15 Ir1 62.1(4) . . . . ? C19 C14 C15 Ir1 -125.9(6) . . . . ? N2 Ir1 C15 C11 -119.9(4) . . . . ? N31 Ir1 C15 C11 -32.0(5) . . . . ? N40 Ir1 C15 C11 152.4(4) . . . . ? C14 Ir1 C15 C11 119.8(5) . . . . ? C12 Ir1 C15 C11 39.2(4) . . . . ? C13 Ir1 C15 C11 82.0(4) . . . . ? N2 Ir1 C15 C14 120.3(3) . . . . ? N31 Ir1 C15 C14 -151.8(3) . . . . ? N40 Ir1 C15 C14 32.5(5) . . . . ? C11 Ir1 C15 C14 -119.8(5) . . . . ? C12 Ir1 C15 C14 -80.6(4) . . . . ? C13 Ir1 C15 C14 -37.8(3) . . . . ? N2 Ir1 C15 C20 -1.3(6) . . . . ? N31 Ir1 C15 C20 86.6(6) . . . . ? N40 Ir1 C15 C20 -89.1(6) . . . . ? C11 Ir1 C15 C20 118.6(7) . . . . ? C14 Ir1 C15 C20 -121.6(7) . . . . ? C12 Ir1 C15 C20 157.8(7) . . . . ? C13 Ir1 C15 C20 -159.4(6) . . . . ? N41 Ir2 C21 C22 103.5(6) . . . . ? N50 Ir2 C21 C22 -159.7(3) . . . . ? N4 Ir2 C21 C22 -61.8(4) . . . . ? C25 Ir2 C21 C22 117.5(5) . . . . ? C23 Ir2 C21 C22 37.0(3) . . . . ? C24 Ir2 C21 C22 79.7(4) . . . . ? N41 Ir2 C21 C25 -14.0(8) . . . . ? N50 Ir2 C21 C25 82.9(3) . . . . ? N4 Ir2 C21 C25 -179.2(3) . . . . ? C23 Ir2 C21 C25 -80.5(3) . . . . ? C22 Ir2 C21 C25 -117.5(5) . . . . ? C24 Ir2 C21 C25 -37.8(3) . . . . ? N41 Ir2 C21 C26 -135.9(6) . . . . ? N50 Ir2 C21 C26 -39.0(6) . . . . ? N4 Ir2 C21 C26 58.9(6) . . . . ? C25 Ir2 C21 C26 -121.8(7) . . . . ? C23 Ir2 C21 C26 157.7(6) . . . . ? C22 Ir2 C21 C26 120.7(7) . . . . ? C24 Ir2 C21 C26 -159.6(6) . . . . ? C25 C21 C22 C23 0.6(6) . . . . ? C26 C21 C22 C23 172.9(6) . . . . ? Ir2 C21 C22 C23 -60.3(4) . . . . ? C25 C21 C22 C27 -178.5(6) . . . . ? C26 C21 C22 C27 -6.2(10) . . . . ? Ir2 C21 C22 C27 120.6(6) . . . . ? C25 C21 C22 Ir2 61.0(4) . . . . ? C26 C21 C22 Ir2 -126.8(6) . . . . ? N41 Ir2 C22 C21 -151.7(3) . . . . ? N50 Ir2 C22 C21 31.8(5) . . . . ? N4 Ir2 C22 C21 126.8(3) . . . . ? C25 Ir2 C22 C21 -38.3(3) . . . . ? C23 Ir2 C22 C21 -119.2(5) . . . . ? C24 Ir2 C22 C21 -81.5(4) . . . . ? N41 Ir2 C22 C23 -32.5(5) . . . . ? N50 Ir2 C22 C23 150.9(3) . . . . ? N4 Ir2 C22 C23 -114.0(3) . . . . ? C25 Ir2 C22 C23 80.8(3) . . . . ? C21 Ir2 C22 C23 119.2(5) . . . . ? C24 Ir2 C22 C23 37.6(3) . . . . ? N41 Ir2 C22 C27 88.7(6) . . . . ? N50 Ir2 C22 C27 -87.8(6) . . . . ? N4 Ir2 C22 C27 7.2(5) . . . . ? C25 Ir2 C22 C27 -157.9(6) . . . . ? C21 Ir2 C22 C27 -119.6(6) . . . . ? C23 Ir2 C22 C27 121.2(6) . . . . ? C24 Ir2 C22 C27 158.9(6) . . . . ? C21 C22 C23 C24 -1.4(6) . . . . ? C27 C22 C23 C24 177.7(6) . . . . ? Ir2 C22 C23 C24 -61.7(4) . . . . ? C21 C22 C23 C28 -173.3(5) . . . . ? C27 C22 C23 C28 5.8(9) . . . . ? Ir2 C22 C23 C28 126.4(6) . . . . ? C21 C22 C23 Ir2 60.3(4) . . . . ? C27 C22 C23 Ir2 -120.6(6) . . . . ? N41 Ir2 C23 C24 -82.3(3) . . . . ? N50 Ir2 C23 C24 19.0(8) . . . . ? N4 Ir2 C23 C24 -169.1(3) . . . . ? C25 Ir2 C23 C24 37.6(3) . . . . ? C21 Ir2 C23 C24 81.1(3) . . . . ? C22 Ir2 C23 C24 117.8(5) . . . . ? N41 Ir2 C23 C22 159.9(3) . . . . ? N50 Ir2 C23 C22 -98.8(6) . . . . ? N4 Ir2 C23 C22 73.1(3) . . . . ? C25 Ir2 C23 C22 -80.2(3) . . . . ? C21 Ir2 C23 C22 -36.8(3) . . . . ? C24 Ir2 C23 C22 -117.8(5) . . . . ? N41 Ir2 C23 C28 39.4(5) . . . . ? N50 Ir2 C23 C28 140.7(6) . . . . ? N4 Ir2 C23 C28 -47.5(5) . . . . ? C25 Ir2 C23 C28 159.2(6) . . . . ? C21 Ir2 C23 C28 -157.3(6) . . . . ? C22 Ir2 C23 C28 -120.5(7) . . . . ? C24 Ir2 C23 C28 121.6(6) . . . . ? C22 C23 C24 C25 1.6(6) . . . . ? C28 C23 C24 C25 173.4(5) . . . . ? Ir2 C23 C24 C25 -60.0(4) . . . . ? C22 C23 C24 C29 -176.9(5) . . . . ? C28 C23 C24 C29 -5.1(9) . . . . ? Ir2 C23 C24 C29 121.5(6) . . . . ? C22 C23 C24 Ir2 61.6(4) . . . . ? C28 C23 C24 Ir2 -126.6(6) . . . . ? N41 Ir2 C24 C23 106.8(3) . . . . ? N50 Ir2 C24 C23 -173.0(3) . . . . ? N4 Ir2 C24 C23 18.4(5) . . . . ? C25 Ir2 C24 C23 -118.3(5) . . . . ? C21 Ir2 C24 C23 -80.2(3) . . . . ? C22 Ir2 C24 C23 -37.6(3) . . . . ? N41 Ir2 C24 C25 -134.9(3) . . . . ? N50 Ir2 C24 C25 -54.7(4) . . . . ? N4 Ir2 C24 C25 136.7(4) . . . . ? C21 Ir2 C24 C25 38.1(3) . . . . ? C23 Ir2 C24 C25 118.3(5) . . . . ? C22 Ir2 C24 C25 80.6(3) . . . . ? N41 Ir2 C24 C29 -14.5(5) . . . . ? N50 Ir2 C24 C29 65.8(6) . . . . ? N4 Ir2 C24 C29 -102.9(6) . . . . ? C25 Ir2 C24 C29 120.5(6) . . . . ? C21 Ir2 C24 C29 158.5(6) . . . . ? C23 Ir2 C24 C29 -121.3(6) . . . . ? C22 Ir2 C24 C29 -158.9(6) . . . . ? C23 C24 C25 C21 -1.2(6) . . . . ? C29 C24 C25 C21 177.3(5) . . . . ? Ir2 C24 C25 C21 -61.6(4) . . . . ? C23 C24 C25 C30 -177.4(5) . . . . ? C29 C24 C25 C30 1.1(9) . . . . ? Ir2 C24 C25 C30 122.2(6) . . . . ? C23 C24 C25 Ir2 60.4(4) . . . . ? C29 C24 C25 Ir2 -121.1(6) . . . . ? C22 C21 C25 C24 0.4(6) . . . . ? C26 C21 C25 C24 -171.8(6) . . . . ? Ir2 C21 C25 C24 62.0(4) . . . . ? C22 C21 C25 C30 176.5(5) . . . . ? C26 C21 C25 C30 4.4(10) . . . . ? Ir2 C21 C25 C30 -121.8(6) . . . . ? C22 C21 C25 Ir2 -61.7(4) . . . . ? C26 C21 C25 Ir2 126.2(6) . . . . ? N41 Ir2 C25 C24 57.4(4) . . . . ? N50 Ir2 C25 C24 136.9(3) . . . . ? N4 Ir2 C25 C24 -116.0(5) . . . . ? C21 Ir2 C25 C24 -117.6(5) . . . . ? C23 Ir2 C25 C24 -37.3(3) . . . . ? C22 Ir2 C25 C24 -80.1(3) . . . . ? N41 Ir2 C25 C21 175.0(3) . . . . ? N50 Ir2 C25 C21 -105.4(3) . . . . ? N4 Ir2 C25 C21 1.6(6) . . . . ? C23 Ir2 C25 C21 80.3(3) . . . . ? C22 Ir2 C25 C21 37.5(3) . . . . ? C24 Ir2 C25 C21 117.6(5) . . . . ? N41 Ir2 C25 C30 -63.0(6) . . . . ? N50 Ir2 C25 C30 16.5(5) . . . . ? N4 Ir2 C25 C30 123.6(5) . . . . ? C21 Ir2 C25 C30 121.9(6) . . . . ? C23 Ir2 C25 C30 -157.7(6) . . . . ? C22 Ir2 C25 C30 159.5(6) . . . . ? C24 Ir2 C25 C30 -120.4(7) . . . . ? C35 N31 C31 C32 -1.4(9) . . . . ? Ir1 N31 C31 C32 -179.6(5) . . . . ? N31 C31 C32 C33 2.9(11) . . . . ? C31 C32 C33 C34 -2.0(12) . . . . ? C32 C33 C34 C35 -0.4(13) . . . . ? C31 N31 C35 C34 -1.0(9) . . . . ? Ir1 N31 C35 C34 177.3(5) . . . . ? C31 N31 C35 C36 178.9(5) . . . . ? Ir1 N31 C35 C36 -2.7(6) . . . . ? C33 C34 C35 N31 1.9(11) . . . . ? C33 C34 C35 C36 -178.0(7) . . . . ? C40 N40 C36 C37 -1.1(8) . . . . ? Ir1 N40 C36 C37 179.0(4) . . . . ? C40 N40 C36 C35 177.6(5) . . . . ? Ir1 N40 C36 C35 -2.4(6) . . . . ? N31 C35 C36 N40 3.3(8) . . . . ? C34 C35 C36 N40 -176.7(6) . . . . ? N31 C35 C36 C37 -178.1(5) . . . . ? C34 C35 C36 C37 1.9(10) . . . . ? N40 C36 C37 C38 1.3(10) . . . . ? C35 C36 C37 C38 -177.3(6) . . . . ? C36 C37 C38 C39 0.1(10) . . . . ? C37 C38 C39 C40 -1.5(10) . . . . ? C36 N40 C40 C39 -0.4(9) . . . . ? Ir1 N40 C40 C39 179.5(4) . . . . ? C38 C39 C40 N40 1.8(9) . . . . ? C45 N41 C41 C42 0.4(8) . . . . ? Ir2 N41 C41 C42 -172.0(4) . . . . ? N41 C41 C42 C43 2.0(9) . . . . ? C41 C42 C43 C44 -1.8(10) . . . . ? C42 C43 C44 C45 -0.7(10) . . . . ? C41 N41 C45 C44 -3.0(8) . . . . ? Ir2 N41 C45 C44 170.0(4) . . . . ? C41 N41 C45 C46 176.4(5) . . . . ? Ir2 N41 C45 C46 -10.6(6) . . . . ? C43 C44 C45 N41 3.2(9) . . . . ? C43 C44 C45 C46 -176.2(6) . . . . ? C50 N50 C46 C47 -0.3(8) . . . . ? Ir2 N50 C46 C47 176.0(4) . . . . ? C50 N50 C46 C45 -178.8(5) . . . . ? Ir2 N50 C46 C45 -2.5(6) . . . . ? N41 C45 C46 N50 8.6(7) . . . . ? C44 C45 C46 N50 -172.0(5) . . . . ? N41 C45 C46 C47 -169.8(5) . . . . ? C44 C45 C46 C47 9.6(9) . . . . ? N50 C46 C47 C48 -0.4(9) . . . . ? C45 C46 C47 C48 177.9(5) . . . . ? C46 C47 C48 C49 0.3(9) . . . . ? C47 C48 C49 C50 0.6(9) . . . . ? C46 N50 C50 C49 1.3(8) . . . . ? Ir2 N50 C50 C49 -174.7(4) . . . . ? C48 C49 C50 N50 -1.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.402 _refine_diff_density_min -1.560 _refine_diff_density_rms 0.162 _database_code_depnum_ccdc_archive 'CCDC 945554' ####################################################################### # # 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_comp10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H49 Ir N7 Rh 2+, 2(F6 P 1-), H2 O' _chemical_formula_sum 'C43 H51 F12 Ir N7 O P2 Rh' _chemical_formula_weight 1266.96 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 26.1251(10) _cell_length_b 26.1251(10) _cell_length_c 14.4637(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9871.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 77682 _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5008 _exptl_absorpt_coefficient_mu 3.179 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4489 _exptl_absorpt_correction_T_max 0.6471 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 93022 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.0434 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11301 _reflns_number_gt 10694 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _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. # 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 -0.000 -0.000 0.000 195 19 ' ' 2 0.500 0.500 0.500 195 19 ' ' _platon_squeeze_details ? ; _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^)+(0.0692P)^2^+45.2215P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Hooft y Parameter Value . 0.150( 1)' _refine_ls_abs_structure_Flack 0.135(7) _refine_ls_number_reflns 11301 _refine_ls_number_parameters 576 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1389 _refine_ls_wR_factor_gt 0.1371 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.526253(13) 0.259291(13) 0.09549(2) 0.03515(10) Uani 1 1 d . . . Rh1 Rh 0.36143(2) 0.20287(2) 0.36513(4) 0.02206(12) Uani 1 1 d . . . P1 P 0.60118(19) 0.2148(2) -0.3537(3) 0.124(2) Uani 1 1 d D . . P2 P 0.5000 0.5000 0.1799(6) 0.104(2) Uani 1 2 d SD . . P3 P 0.5000 0.0000 -0.0112(3) 0.0482(8) Uani 1 2 d SD . . F1A F 0.5929(9) 0.1968(9) -0.4548(11) 0.103(6) Uiso 0.50 1 d PD . . F1B F 0.5923(9) 0.1664(8) -0.4269(15) 0.113(7) Uiso 0.50 1 d PD . . F2A F 0.6040(7) 0.2737(5) -0.3931(12) 0.083(4) Uiso 0.50 1 d PD . . F2B F 0.6371(10) 0.2467(10) -0.2912(17) 0.133(8) Uiso 0.50 1 d PD . . F3A F 0.6597(5) 0.2160(9) -0.3432(16) 0.107(6) Uiso 0.50 1 d PD . . F3B F 0.6425(9) 0.2187(11) -0.4395(16) 0.140(9) Uiso 0.50 1 d PD . . F4A F 0.6529(6) 0.1760(8) -0.3357(15) 0.102(6) Uiso 0.50 1 d PD . . F4B F 0.5998(7) 0.2465(7) -0.2538(10) 0.088(5) Uiso 0.50 1 d PD . . F5 F 0.5784(4) 0.1708(4) -0.2960(8) 0.112(3) Uiso 1 1 d D . . F6A F 0.5395(5) 0.2289(6) -0.3457(11) 0.074(4) Uiso 0.50 1 d PD . . F6B F 0.5583(8) 0.2389(10) -0.4152(17) 0.132(8) Uiso 0.50 1 d PD . . F7 F 0.4664(6) 0.4482(6) 0.1806(11) 0.171(6) Uiso 1 1 d D . . F8 F 0.5000 0.5000 0.0676(12) 0.187(10) Uiso 1 2 d SD . . F9 F 0.4506(5) 0.5364(5) 0.1800(9) 0.139(4) Uiso 1 1 d D . . F10 F 0.5000 0.5000 0.2904(13) 0.181(9) Uiso 1 2 d SD . . F11A F 0.5029(6) -0.0599(4) -0.0144(11) 0.119(5) Uiso 0.85 1 d PD . . F12A F 0.4571(6) 0.0006(7) -0.0880(11) 0.086(4) Uiso 0.50 1 d PD . . F12B F 0.5000 0.0000 -0.1194(12) 0.175(17) Uiso 0.50 2 d SPD . . F13A F 0.5441(7) -0.0045(8) 0.0613(12) 0.098(6) Uiso 0.50 1 d PD . . F13B F 0.5000 0.0000 0.0977(12) 0.126(10) Uiso 0.50 2 d SPD . . F14B F 0.4465(7) -0.0246(10) 0.0052(19) 0.132(8) Uiso 0.50 1 d PD . . F11B F 0.4721(13) 0.0521(9) 0.007(2) 0.037(7) Uiso 0.15 1 d PD . . O2 O 0.3572(12) 0.5137(13) 0.317(2) 0.141(10) Uiso 0.55 1 d P . . O3 O 0.3632(18) 0.4637(19) 0.285(3) 0.169(16) Uiso 0.45 1 d P . . N1 N 0.4203(3) 0.2953(3) 0.1442(5) 0.0363(15) Uani 1 1 d . . . N2 N 0.4542(3) 0.2561(3) 0.1560(4) 0.0293(13) Uani 1 1 d . . . N3 N 0.4386(3) 0.2234(3) 0.2195(5) 0.0298(14) Uani 1 1 d . . . N4 N 0.3934(3) 0.2402(3) 0.2484(5) 0.0296(13) Uani 1 1 d . . . N31 N 0.5463(3) 0.2915(4) 0.2220(5) 0.0427(18) Uani 1 1 d . . . N40 N 0.5450(3) 0.1951(3) 0.1771(5) 0.0385(16) Uani 1 1 d . . . N41 N 0.3689(3) 0.1335(3) 0.2928(4) 0.0307(14) Uani 1 1 d . . . C5 C 0.3829(3) 0.2840(3) 0.2030(6) 0.0344(17) Uani 1 1 d . . . C6 C 0.3369(4) 0.3164(4) 0.2163(7) 0.046(2) Uani 1 1 d . . . H6A H 0.3280 0.3174 0.2821 0.055 Uiso 1 1 calc R . . H6B H 0.3083 0.3021 0.1810 0.055 Uiso 1 1 calc R . . H6C H 0.3441 0.3512 0.1946 0.055 Uiso 1 1 calc R . . C11 C 0.4998(4) 0.2730(4) -0.0465(6) 0.041(2) Uani 1 1 d . . . C12 C 0.5352(4) 0.2319(4) -0.0467(6) 0.040(2) Uani 1 1 d . . . C13 C 0.5840(4) 0.2519(4) -0.0129(6) 0.043(2) Uani 1 1 d . . . C14 C 0.5767(4) 0.3045(4) 0.0069(7) 0.049(2) Uani 1 1 d . . . C15 C 0.5237(4) 0.3184(4) -0.0087(6) 0.044(2) Uani 1 1 d . . . C16 C 0.4444(5) 0.2716(6) -0.0776(7) 0.064(3) Uani 1 1 d . . . H16A H 0.4238 0.2933 -0.0369 0.077 Uiso 1 1 calc R . . H16B H 0.4318 0.2364 -0.0749 0.077 Uiso 1 1 calc R . . H16C H 0.4420 0.2843 -0.1413 0.077 Uiso 1 1 calc R . . C17 C 0.5252(5) 0.1804(4) -0.0870(8) 0.062(3) Uani 1 1 d . . . H17A H 0.5490 0.1555 -0.0601 0.075 Uiso 1 1 calc R . . H17B H 0.5302 0.1817 -0.1541 0.075 Uiso 1 1 calc R . . H17C H 0.4900 0.1701 -0.0733 0.075 Uiso 1 1 calc R . . C18 C 0.6318(5) 0.2230(6) -0.0101(9) 0.071(4) Uani 1 1 d . . . H18A H 0.6245 0.1870 0.0039 0.086 Uiso 1 1 calc R . . H18B H 0.6542 0.2372 0.0378 0.086 Uiso 1 1 calc R . . H18C H 0.6489 0.2253 -0.0703 0.086 Uiso 1 1 calc R . . C19 C 0.6176(5) 0.3419(5) 0.0418(8) 0.064(3) Uani 1 1 d . . . H19A H 0.6024 0.3759 0.0494 0.076 Uiso 1 1 calc R . . H19B H 0.6456 0.3437 -0.0031 0.076 Uiso 1 1 calc R . . H19C H 0.6308 0.3299 0.1013 0.076 Uiso 1 1 calc R . . C20 C 0.5018(7) 0.3709(4) -0.0034(9) 0.074(4) Uani 1 1 d . . . H20A H 0.5213 0.3912 0.0413 0.089 Uiso 1 1 calc R . . H20B H 0.4659 0.3689 0.0163 0.089 Uiso 1 1 calc R . . H20C H 0.5037 0.3871 -0.0644 0.089 Uiso 1 1 calc R . . C21 C 0.3313(4) 0.2083(4) 0.5051(6) 0.040(2) Uani 1 1 d . . . C22 C 0.3697(3) 0.1703(4) 0.5023(6) 0.0372(19) Uani 1 1 d . . . C23 C 0.4180(3) 0.1944(4) 0.4795(6) 0.0355(19) Uani 1 1 d . . . C24 C 0.4089(4) 0.2468(4) 0.4654(6) 0.046(2) Uani 1 1 d . . . C25 C 0.3551(4) 0.2563(4) 0.4782(6) 0.045(2) Uani 1 1 d . . . C26 C 0.2779(4) 0.2031(6) 0.5379(7) 0.064(4) Uani 1 1 d . . . H26A H 0.2556 0.2259 0.5022 0.077 Uiso 1 1 calc R . . H26B H 0.2760 0.2122 0.6035 0.077 Uiso 1 1 calc R . . H26C H 0.2665 0.1676 0.5296 0.077 Uiso 1 1 calc R . . C27 C 0.3622(5) 0.1153(4) 0.5255(7) 0.053(3) Uani 1 1 d . . . H27A H 0.3320 0.1022 0.4927 0.064 Uiso 1 1 calc R . . H27B H 0.3570 0.1117 0.5923 0.064 Uiso 1 1 calc R . . H27C H 0.3924 0.0957 0.5067 0.064 Uiso 1 1 calc R . . C28 C 0.4695(4) 0.1705(5) 0.4736(7) 0.058(3) Uani 1 1 d . . . H28A H 0.4660 0.1332 0.4760 0.069 Uiso 1 1 calc R . . H28B H 0.4905 0.1822 0.5256 0.069 Uiso 1 1 calc R . . H28C H 0.4858 0.1804 0.4153 0.069 Uiso 1 1 calc R . . C29 C 0.4482(6) 0.2850(6) 0.4365(9) 0.074(4) Uani 1 1 d . . . H29A H 0.4315 0.3132 0.4034 0.088 Uiso 1 1 calc R . . H29B H 0.4732 0.2685 0.3957 0.088 Uiso 1 1 calc R . . H29C H 0.4657 0.2985 0.4912 0.088 Uiso 1 1 calc R . . C30 C 0.3312(7) 0.3077(5) 0.4808(10) 0.081(5) Uani 1 1 d . . . H30A H 0.2939 0.3042 0.4816 0.097 Uiso 1 1 calc R . . H30B H 0.3415 0.3272 0.4260 0.097 Uiso 1 1 calc R . . H30C H 0.3424 0.3258 0.5366 0.097 Uiso 1 1 calc R . . C31 C 0.5400(4) 0.3420(5) 0.2407(7) 0.053(3) Uani 1 1 d . . . H31 H 0.5268 0.3644 0.1949 0.064 Uiso 1 1 calc R . . C32 C 0.5532(5) 0.3605(5) 0.3272(8) 0.063(3) Uani 1 1 d . . . H32 H 0.5499 0.3960 0.3400 0.075 Uiso 1 1 calc R . . C33 C 0.5709(4) 0.3283(6) 0.3943(8) 0.064(3) Uani 1 1 d . . . H33 H 0.5797 0.3415 0.4535 0.077 Uiso 1 1 calc R . . C34 C 0.5760(4) 0.2774(7) 0.3766(8) 0.076(5) Uani 1 1 d . . . H34 H 0.5878 0.2547 0.4234 0.091 Uiso 1 1 calc R . . C35 C 0.5635(3) 0.2587(5) 0.2882(6) 0.046(2) Uani 1 1 d . . . C36 C 0.5628(3) 0.2057(5) 0.2643(6) 0.045(2) Uani 1 1 d . . . C37 C 0.5761(4) 0.1669(6) 0.3234(9) 0.067(4) Uani 1 1 d . . . H37 H 0.5891 0.1747 0.3831 0.081 Uiso 1 1 calc R . . C38 C 0.5704(5) 0.1160(6) 0.2959(9) 0.070(4) Uani 1 1 d . . . H38 H 0.5799 0.0886 0.3356 0.084 Uiso 1 1 calc R . . C39 C 0.5499(4) 0.1065(5) 0.2064(10) 0.062(3) Uani 1 1 d . . . H39 H 0.5444 0.0725 0.1857 0.074 Uiso 1 1 calc R . . C40 C 0.5383(4) 0.1474(4) 0.1500(7) 0.048(2) Uani 1 1 d . . . H40 H 0.5250 0.1410 0.0900 0.057 Uiso 1 1 calc R . . C41 C 0.4125(3) 0.1056(4) 0.2880(6) 0.0365(18) Uani 1 1 d . . . H41 H 0.4430 0.1196 0.3135 0.044 Uiso 1 1 calc R . . C42 C 0.4147(4) 0.0580(4) 0.2479(7) 0.047(2) Uani 1 1 d . . . H42 H 0.4457 0.0390 0.2471 0.057 Uiso 1 1 calc R . . C43 C 0.3700(5) 0.0381(4) 0.2084(7) 0.051(2) Uani 1 1 d . . . H43 H 0.3707 0.0056 0.1790 0.061 Uiso 1 1 calc R . . C44 C 0.3256(4) 0.0652(4) 0.2117(6) 0.046(2) Uani 1 1 d . . . H44 H 0.2951 0.0515 0.1858 0.055 Uiso 1 1 calc R . . C45 C 0.3252(4) 0.1149(4) 0.2547(6) 0.0376(19) Uani 1 1 d . . . C46 C 0.2829(3) 0.1489(4) 0.2589(5) 0.0337(18) Uani 1 1 d . . . C47 C 0.2337(4) 0.1374(5) 0.2232(6) 0.046(2) Uani 1 1 d . . . H47 H 0.2279 0.1053 0.1942 0.055 Uiso 1 1 calc R . . C48 C 0.1937(4) 0.1725(5) 0.2301(7) 0.055(3) Uani 1 1 d . . . H48 H 0.1608 0.1644 0.2063 0.066 Uiso 1 1 calc R . . C49 C 0.2026(4) 0.2202(5) 0.2726(7) 0.059(3) Uani 1 1 d . . . H49 H 0.1760 0.2449 0.2768 0.071 Uiso 1 1 calc R . . C50 C 0.2511(3) 0.2304(4) 0.3084(6) 0.044(2) Uani 1 1 d . . . H50 H 0.2569 0.2626 0.3372 0.053 Uiso 1 1 calc R . . C51 C 0.2909(3) 0.1957(3) 0.3038(5) 0.0318(16) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.03681(17) 0.04021(18) 0.02842(15) 0.00323(14) 0.00204(14) -0.00462(13) Rh1 0.0196(2) 0.0297(3) 0.0168(2) -0.0007(2) 0.0010(2) 0.0030(2) P1 0.125(4) 0.156(5) 0.092(3) 0.070(3) -0.060(3) -0.107(4) P2 0.083(4) 0.103(5) 0.125(6) 0.000 0.000 -0.013(4) P3 0.044(2) 0.050(2) 0.051(2) 0.000 0.000 0.0131(16) N1 0.042(4) 0.035(4) 0.032(4) 0.000(3) 0.004(3) 0.003(3) N2 0.033(3) 0.027(3) 0.028(3) 0.005(3) 0.001(2) 0.002(3) N3 0.027(3) 0.036(3) 0.026(3) 0.004(3) 0.003(3) -0.001(3) N4 0.030(3) 0.033(3) 0.026(3) 0.000(3) 0.000(3) 0.004(3) N31 0.042(4) 0.058(5) 0.029(4) -0.001(3) 0.003(3) -0.008(4) N40 0.030(3) 0.051(5) 0.035(4) 0.010(3) 0.007(3) 0.000(3) N41 0.031(3) 0.038(4) 0.024(3) 0.003(3) 0.005(3) -0.001(3) C5 0.039(4) 0.034(4) 0.030(4) 0.000(3) 0.001(3) 0.005(3) C6 0.059(6) 0.034(5) 0.045(5) 0.007(4) 0.007(4) 0.016(4) C11 0.053(5) 0.047(5) 0.023(4) 0.009(4) -0.007(4) -0.012(4) C12 0.048(5) 0.046(5) 0.027(4) 0.001(4) 0.009(4) -0.010(4) C13 0.042(5) 0.060(6) 0.027(4) 0.002(4) 0.008(4) -0.010(4) C14 0.053(6) 0.061(6) 0.033(5) 0.005(4) 0.004(4) -0.023(5) C15 0.061(6) 0.047(5) 0.022(4) 0.008(4) 0.001(4) -0.014(5) C16 0.060(7) 0.092(9) 0.040(6) 0.014(6) -0.013(5) -0.007(6) C17 0.083(8) 0.053(6) 0.051(6) -0.007(5) 0.007(6) -0.005(6) C18 0.057(7) 0.105(11) 0.053(7) 0.007(7) 0.016(6) -0.005(7) C19 0.069(8) 0.077(8) 0.045(6) -0.001(5) 0.003(5) -0.043(6) C20 0.138(13) 0.034(6) 0.051(6) 0.014(5) 0.002(7) 0.012(7) C21 0.037(4) 0.057(6) 0.025(4) 0.003(4) -0.002(3) 0.005(4) C22 0.030(4) 0.053(5) 0.029(4) -0.008(4) 0.004(3) -0.004(4) C23 0.028(4) 0.055(5) 0.023(4) -0.001(4) -0.003(3) 0.002(4) C24 0.054(6) 0.057(6) 0.028(4) -0.009(4) -0.011(4) -0.018(5) C25 0.068(7) 0.037(5) 0.031(4) -0.008(4) -0.009(4) 0.015(5) C26 0.034(5) 0.124(11) 0.033(5) 0.011(6) 0.005(4) 0.011(6) C27 0.072(7) 0.049(6) 0.038(5) 0.005(4) -0.004(5) -0.002(5) C28 0.038(5) 0.098(9) 0.037(5) -0.011(5) -0.010(4) 0.004(6) C29 0.099(10) 0.075(8) 0.047(6) -0.003(6) -0.009(6) -0.044(8) C30 0.129(14) 0.062(8) 0.052(7) -0.009(6) -0.004(8) 0.025(8) C31 0.057(6) 0.066(7) 0.038(5) -0.006(5) 0.004(4) -0.017(5) C32 0.059(7) 0.086(9) 0.043(6) -0.037(6) 0.017(5) -0.034(6) C33 0.047(6) 0.105(10) 0.040(6) -0.026(7) 0.009(5) -0.023(6) C34 0.031(5) 0.162(15) 0.034(5) -0.005(7) -0.003(4) -0.021(7) C35 0.026(4) 0.080(7) 0.032(4) 0.012(5) 0.002(3) -0.005(4) C36 0.025(4) 0.075(7) 0.035(5) 0.010(5) -0.001(3) 0.003(4) C37 0.035(5) 0.118(12) 0.049(6) 0.041(7) 0.010(5) 0.006(6) C38 0.062(7) 0.079(9) 0.068(8) 0.028(7) 0.023(6) 0.021(7) C39 0.049(6) 0.054(6) 0.083(9) 0.020(6) 0.023(6) 0.020(5) C40 0.042(5) 0.049(5) 0.052(6) 0.006(4) 0.005(4) 0.005(4) C41 0.037(4) 0.046(5) 0.026(4) -0.001(4) -0.002(3) 0.005(4) C42 0.053(6) 0.041(5) 0.047(5) 0.009(4) 0.002(4) 0.009(4) C43 0.070(7) 0.038(5) 0.044(5) -0.003(4) 0.009(5) -0.010(5) C44 0.061(6) 0.047(5) 0.030(4) -0.007(4) 0.007(4) -0.015(5) C45 0.046(5) 0.045(5) 0.021(4) 0.006(3) 0.003(3) -0.017(4) C46 0.032(4) 0.049(5) 0.021(3) 0.004(3) -0.002(3) -0.013(3) C47 0.037(5) 0.068(6) 0.033(4) 0.004(4) -0.004(4) -0.018(5) C48 0.027(5) 0.092(9) 0.046(6) 0.006(5) -0.007(4) 0.001(5) C49 0.027(4) 0.106(10) 0.045(5) 0.006(6) -0.007(4) 0.020(5) C50 0.035(5) 0.061(6) 0.036(4) -0.006(4) -0.003(4) 0.012(4) C51 0.032(4) 0.039(4) 0.024(3) -0.003(3) 0.004(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 N2 2.078(7) . ? Ir1 N31 2.082(8) . ? Ir1 N40 2.108(8) . ? Ir1 C15 2.158(9) . ? Ir1 C13 2.183(9) . ? Ir1 C14 2.185(9) . ? Ir1 C12 2.191(9) . ? Ir1 C11 2.197(8) . ? Rh1 C51 2.054(8) . ? Rh1 N41 2.102(7) . ? Rh1 N4 2.122(7) . ? Rh1 C25 2.156(9) . ? Rh1 C22 2.170(9) . ? Rh1 C21 2.176(9) . ? Rh1 C24 2.227(8) . ? Rh1 C23 2.230(8) . ? P1 F3A 1.537(13) . ? P1 F5 1.540(10) . ? P1 F2B 1.547(14) . ? P1 F1A 1.551(13) . ? P1 F6B 1.563(14) . ? P1 F2A 1.644(12) . ? P1 F3B 1.649(14) . ? P1 F6A 1.658(12) . ? P1 F1B 1.664(14) . ? P1 F4B 1.666(13) . ? P1 F4A 1.709(13) . ? P2 F10 1.598(16) . ? P2 F9 1.603(12) . ? P2 F9 1.603(12) 3_665 ? P2 F7 1.613(13) . ? P2 F7 1.613(13) 3_665 ? P2 F8 1.624(16) . ? P3 F14B 1.558(15) . ? P3 F14B 1.558(15) 3_655 ? P3 F13A 1.561(13) . ? P3 F13A 1.561(13) 3_655 ? P3 F12B 1.566(17) . ? P3 F11B 1.567(16) . ? P3 F11B 1.567(16) 3_655 ? P3 F11A 1.569(11) . ? P3 F11A 1.569(11) 3_655 ? P3 F13B 1.574(16) . ? P3 F12A 1.578(13) 3_655 ? P3 F12A 1.578(13) . ? O2 O3 1.39(5) . ? N1 C5 1.329(11) . ? N1 N2 1.364(10) . ? N2 N3 1.318(9) . ? N3 N4 1.325(9) . ? N4 C5 1.348(11) . ? N31 C31 1.355(15) . ? N31 C35 1.361(13) . ? N40 C40 1.318(13) . ? N40 C36 1.372(12) . ? N41 C41 1.353(11) . ? N41 C45 1.357(11) . ? C5 C6 1.483(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C12 1.419(15) . ? C11 C15 1.447(13) . ? C11 C16 1.514(15) . ? C12 C13 1.460(13) . ? C12 C17 1.489(14) . ? C13 C14 1.418(15) . ? C13 C18 1.461(17) . ? C14 C15 1.449(16) . ? C14 C19 1.532(14) . ? C15 C20 1.488(15) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.413(13) . ? C21 C25 1.452(15) . ? C21 C26 1.482(13) . ? C22 C23 1.448(12) . ? C22 C27 1.488(14) . ? C23 C24 1.405(14) . ? C23 C28 1.485(14) . ? C24 C25 1.438(15) . ? C24 C29 1.492(15) . ? C25 C30 1.482(16) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.386(14) . ? C31 H31 0.9500 . ? C32 C33 1.36(2) . ? C32 H32 0.9500 . ? C33 C34 1.36(2) . ? C33 H33 0.9500 . ? C34 C35 1.406(15) . ? C34 H34 0.9500 . ? C35 C36 1.430(17) . ? C36 C37 1.370(16) . ? C37 C38 1.40(2) . ? C37 H37 0.9500 . ? C38 C39 1.42(2) . ? C38 H38 0.9500 . ? C39 C40 1.377(15) . ? C39 H39 0.9500 . ? C40 H40 0.9500 . ? C41 C42 1.374(13) . ? C41 H41 0.9500 . ? C42 C43 1.400(15) . ? C42 H42 0.9500 . ? C43 C44 1.360(16) . ? C43 H43 0.9500 . ? C44 C45 1.439(13) . ? C44 H44 0.9500 . ? C45 C46 1.419(14) . ? C46 C51 1.401(12) . ? C46 C47 1.418(12) . ? C47 C48 1.394(16) . ? C47 H47 0.9500 . ? C48 C49 1.407(19) . ? C48 H48 0.9500 . ? C49 C50 1.394(14) . ? C49 H49 0.9500 . ? C50 C51 1.382(12) . ? C50 H50 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 N2 Ir1 N31 82.8(3) . . ? N2 Ir1 N40 86.7(3) . . ? N31 Ir1 N40 76.8(3) . . ? N2 Ir1 C15 107.1(3) . . ? N31 Ir1 C15 109.4(4) . . ? N40 Ir1 C15 165.3(4) . . ? N2 Ir1 C13 157.6(3) . . ? N31 Ir1 C13 119.6(3) . . ? N40 Ir1 C13 99.8(4) . . ? C15 Ir1 C13 65.4(4) . . ? N2 Ir1 C14 144.6(4) . . ? N31 Ir1 C14 98.3(4) . . ? N40 Ir1 C14 128.2(4) . . ? C15 Ir1 C14 39.0(4) . . ? C13 Ir1 C14 37.9(4) . . ? N2 Ir1 C12 118.7(3) . . ? N31 Ir1 C12 158.6(3) . . ? N40 Ir1 C12 103.9(3) . . ? C15 Ir1 C12 65.3(4) . . ? C13 Ir1 C12 39.0(3) . . ? C14 Ir1 C12 64.0(4) . . ? N2 Ir1 C11 96.6(3) . . ? N31 Ir1 C11 146.6(4) . . ? N40 Ir1 C11 136.6(3) . . ? C15 Ir1 C11 38.8(3) . . ? C13 Ir1 C11 64.0(4) . . ? C14 Ir1 C11 63.5(4) . . ? C12 Ir1 C11 37.7(4) . . ? C51 Rh1 N41 77.9(3) . . ? C51 Rh1 N4 92.9(3) . . ? N41 Rh1 N4 87.9(3) . . ? C51 Rh1 C25 108.5(4) . . ? N41 Rh1 C25 160.5(3) . . ? N4 Rh1 C25 109.7(3) . . ? C51 Rh1 C22 116.7(3) . . ? N41 Rh1 C22 96.1(3) . . ? N4 Rh1 C22 150.3(3) . . ? C25 Rh1 C22 64.4(4) . . ? C51 Rh1 C21 94.8(3) . . ? N41 Rh1 C21 123.6(3) . . ? N4 Rh1 C21 148.5(3) . . ? C25 Rh1 C21 39.2(4) . . ? C22 Rh1 C21 38.0(3) . . ? C51 Rh1 C24 145.9(4) . . ? N41 Rh1 C24 135.8(4) . . ? N4 Rh1 C24 93.6(3) . . ? C25 Rh1 C24 38.3(4) . . ? C22 Rh1 C24 63.3(4) . . ? C21 Rh1 C24 64.0(4) . . ? C51 Rh1 C23 155.0(3) . . ? N41 Rh1 C23 102.8(3) . . ? N4 Rh1 C23 112.0(3) . . ? C25 Rh1 C23 63.4(4) . . ? C22 Rh1 C23 38.4(3) . . ? C21 Rh1 C23 63.6(3) . . ? C24 Rh1 C23 36.8(4) . . ? F3A P1 F5 110.2(10) . . ? F5 P1 F2B 108.7(11) . . ? F3A P1 F1A 103.8(13) . . ? F5 P1 F1A 103.4(10) . . ? F5 P1 F6B 109.5(11) . . ? F2B P1 F6B 123.3(15) . . ? F3A P1 F2A 88.3(11) . . ? F5 P1 F2A 154.8(9) . . ? F1A P1 F2A 87.9(11) . . ? F5 P1 F3B 135.0(12) . . ? F2B P1 F3B 90.6(15) . . ? F6B P1 F3B 90.9(14) . . ? F3A P1 F6A 162.9(12) . . ? F5 P1 F6A 75.7(7) . . ? F1A P1 F6A 89.9(11) . . ? F2A P1 F6A 81.9(9) . . ? F5 P1 F1B 74.0(10) . . ? F2B P1 F1B 149.9(15) . . ? F6B P1 F1B 81.0(13) . . ? F3B P1 F1B 70.1(14) . . ? F5 P1 F4B 83.9(8) . . ? F2B P1 F4B 40.4(11) . . ? F6B P1 F4B 106.1(13) . . ? F3B P1 F4B 129.5(12) . . ? F1B P1 F4B 157.8(12) . . ? F3A P1 F4A 37.9(10) . . ? F5 P1 F4A 77.3(9) . . ? F1A P1 F4A 94.3(12) . . ? F2A P1 F4A 125.0(10) . . ? F6A P1 F4A 152.9(10) . . ? F10 P2 F9 89.9(6) . . ? F10 P2 F9 89.9(6) . 3_665 ? F9 P2 F9 179.9(12) . 3_665 ? F10 P2 F7 89.7(7) . . ? F9 P2 F7 93.4(8) . . ? F9 P2 F7 86.6(8) 3_665 . ? F10 P2 F7 89.7(7) . 3_665 ? F9 P2 F7 86.6(8) . 3_665 ? F9 P2 F7 93.4(8) 3_665 3_665 ? F7 P2 F7 179.3(14) . 3_665 ? F10 P2 F8 180.000(5) . . ? F9 P2 F8 90.1(6) . . ? F9 P2 F8 90.1(6) 3_665 . ? F7 P2 F8 90.3(7) . . ? F7 P2 F8 90.3(7) 3_665 . ? F14B P3 F14B 163(2) . 3_655 ? F13A P3 F13A 95.7(15) . 3_655 ? F14B P3 F12B 98.7(10) . . ? F14B P3 F12B 98.7(10) 3_655 . ? F14B P3 F11B 85.2(17) . . ? F14B P3 F11B 91.9(17) 3_655 . ? F12B P3 F11B 99.9(13) . . ? F14B P3 F11B 91.9(17) . 3_655 ? F14B P3 F11B 85.2(17) 3_655 3_655 ? F12B P3 F11B 99.9(13) . 3_655 ? F11B P3 F11B 160(3) . 3_655 ? F13A P3 F11A 84.8(9) . . ? F13A P3 F11A 97.6(9) 3_655 . ? F13A P3 F11A 97.6(9) . 3_655 ? F13A P3 F11A 84.8(9) 3_655 3_655 ? F11A P3 F11A 176.5(12) . 3_655 ? F14B P3 F13B 81.3(10) . . ? F14B P3 F13B 81.3(10) 3_655 . ? F12B P3 F13B 180.0 . . ? F11B P3 F13B 80.1(13) . . ? F11B P3 F13B 80.1(13) 3_655 . ? F13A P3 F12A 87.1(10) . 3_655 ? F13A P3 F12A 175.5(10) 3_655 3_655 ? F11A P3 F12A 86.2(9) . 3_655 ? F11A P3 F12A 91.3(9) 3_655 3_655 ? F13A P3 F12A 175.5(10) . . ? F13A P3 F12A 87.1(10) 3_655 . ? F11A P3 F12A 91.3(9) . . ? F11A P3 F12A 86.2(9) 3_655 . ? F12A P3 F12A 90.4(13) 3_655 . ? C5 N1 N2 103.3(7) . . ? N3 N2 N1 111.9(6) . . ? N3 N2 Ir1 126.9(5) . . ? N1 N2 Ir1 120.3(5) . . ? N2 N3 N4 106.3(6) . . ? N3 N4 C5 108.0(7) . . ? N3 N4 Rh1 116.8(5) . . ? C5 N4 Rh1 134.2(5) . . ? C31 N31 C35 120.8(9) . . ? C31 N31 Ir1 122.5(7) . . ? C35 N31 Ir1 116.6(7) . . ? C40 N40 C36 120.5(9) . . ? C40 N40 Ir1 123.7(7) . . ? C36 N40 Ir1 115.7(7) . . ? C41 N41 C45 119.6(8) . . ? C41 N41 Rh1 124.6(6) . . ? C45 N41 Rh1 115.6(6) . . ? N1 C5 N4 110.5(7) . . ? N1 C5 C6 123.5(8) . . ? N4 C5 C6 126.0(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C11 C15 109.8(9) . . ? C12 C11 C16 127.2(10) . . ? C15 C11 C16 123.0(10) . . ? C12 C11 Ir1 70.9(5) . . ? C15 C11 Ir1 69.1(5) . . ? C16 C11 Ir1 125.1(7) . . ? C11 C12 C13 107.3(8) . . ? C11 C12 C17 124.8(10) . . ? C13 C12 C17 127.4(10) . . ? C11 C12 Ir1 71.4(5) . . ? C13 C12 Ir1 70.2(5) . . ? C17 C12 Ir1 130.1(7) . . ? C14 C13 C12 107.3(9) . . ? C14 C13 C18 127.6(10) . . ? C12 C13 C18 124.8(11) . . ? C14 C13 Ir1 71.2(5) . . ? C12 C13 Ir1 70.8(5) . . ? C18 C13 Ir1 128.1(7) . . ? C13 C14 C15 109.8(9) . . ? C13 C14 C19 126.3(11) . . ? C15 C14 C19 123.9(11) . . ? C13 C14 Ir1 71.0(5) . . ? C15 C14 Ir1 69.5(5) . . ? C19 C14 Ir1 124.9(7) . . ? C11 C15 C14 105.5(9) . . ? C11 C15 C20 127.4(11) . . ? C14 C15 C20 126.2(11) . . ? C11 C15 Ir1 72.1(5) . . ? C14 C15 Ir1 71.5(5) . . ? C20 C15 Ir1 129.5(7) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 107.3(8) . . ? C22 C21 C26 127.8(10) . . ? C25 C21 C26 124.7(10) . . ? C22 C21 Rh1 70.8(5) . . ? C25 C21 Rh1 69.7(5) . . ? C26 C21 Rh1 129.2(7) . . ? C21 C22 C23 108.5(9) . . ? C21 C22 C27 125.4(9) . . ? C23 C22 C27 126.0(9) . . ? C21 C22 Rh1 71.3(5) . . ? C23 C22 Rh1 73.0(5) . . ? C27 C22 Rh1 124.9(7) . . ? C24 C23 C22 108.1(8) . . ? C24 C23 C28 123.7(10) . . ? C22 C23 C28 128.2(10) . . ? C24 C23 Rh1 71.5(5) . . ? C22 C23 Rh1 68.6(5) . . ? C28 C23 Rh1 126.8(6) . . ? C23 C24 C25 108.4(8) . . ? C23 C24 C29 125.2(11) . . ? C25 C24 C29 126.4(11) . . ? C23 C24 Rh1 71.7(5) . . ? C25 C24 Rh1 68.2(5) . . ? C29 C24 Rh1 123.0(7) . . ? C24 C25 C21 107.7(8) . . ? C24 C25 C30 124.8(12) . . ? C21 C25 C30 126.6(11) . . ? C24 C25 Rh1 73.5(5) . . ? C21 C25 Rh1 71.2(5) . . ? C30 C25 Rh1 129.7(8) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N31 C31 C32 119.2(12) . . ? N31 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? C33 C32 C31 120.8(12) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C34 C33 C32 120.1(11) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 119.1(13) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? N31 C35 C34 119.9(13) . . ? N31 C35 C36 115.8(9) . . ? C34 C35 C36 124.0(11) . . ? C37 C36 N40 120.8(12) . . ? C37 C36 C35 124.2(11) . . ? N40 C36 C35 115.0(9) . . ? C36 C37 C38 120.0(13) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C39 117.6(11) . . ? C37 C38 H38 121.2 . . ? C39 C38 H38 121.2 . . ? C40 C39 C38 119.2(12) . . ? C40 C39 H39 120.4 . . ? C38 C39 H39 120.4 . . ? N40 C40 C39 121.9(11) . . ? N40 C40 H40 119.1 . . ? C39 C40 H40 119.1 . . ? N41 C41 C42 123.0(9) . . ? N41 C41 H41 118.5 . . ? C42 C41 H41 118.5 . . ? C41 C42 C43 118.2(9) . . ? C41 C42 H42 120.9 . . ? C43 C42 H42 120.9 . . ? C44 C43 C42 120.3(9) . . ? C44 C43 H43 119.9 . . ? C42 C43 H43 119.9 . . ? C43 C44 C45 119.4(10) . . ? C43 C44 H44 120.3 . . ? C45 C44 H44 120.3 . . ? N41 C45 C46 114.5(8) . . ? N41 C45 C44 119.5(9) . . ? C46 C45 C44 126.0(9) . . ? C51 C46 C47 119.2(9) . . ? C51 C46 C45 116.8(7) . . ? C47 C46 C45 124.0(9) . . ? C48 C47 C46 121.0(10) . . ? C48 C47 H47 119.5 . . ? C46 C47 H47 119.5 . . ? C47 C48 C49 119.3(9) . . ? C47 C48 H48 120.4 . . ? C49 C48 H48 120.4 . . ? C50 C49 C48 118.9(10) . . ? C50 C49 H49 120.6 . . ? C48 C49 H49 120.6 . . ? C51 C50 C49 122.6(10) . . ? C51 C50 H50 118.7 . . ? C49 C50 H50 118.7 . . ? C50 C51 C46 119.0(8) . . ? C50 C51 Rh1 126.5(7) . . ? C46 C51 Rh1 114.4(6) . . ? 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 N1 N2 N3 -1.1(9) . . . . ? C5 N1 N2 Ir1 -170.6(5) . . . . ? N31 Ir1 N2 N3 -75.7(7) . . . . ? N40 Ir1 N2 N3 1.4(7) . . . . ? C15 Ir1 N2 N3 176.2(7) . . . . ? C13 Ir1 N2 N3 109.4(10) . . . . ? C14 Ir1 N2 N3 -169.9(7) . . . . ? C12 Ir1 N2 N3 105.5(7) . . . . ? C11 Ir1 N2 N3 138.0(7) . . . . ? N31 Ir1 N2 N1 92.2(6) . . . . ? N40 Ir1 N2 N1 169.3(6) . . . . ? C15 Ir1 N2 N1 -15.9(7) . . . . ? C13 Ir1 N2 N1 -82.7(11) . . . . ? C14 Ir1 N2 N1 -2.0(9) . . . . ? C12 Ir1 N2 N1 -86.6(7) . . . . ? C11 Ir1 N2 N1 -54.1(6) . . . . ? N1 N2 N3 N4 1.6(9) . . . . ? Ir1 N2 N3 N4 170.4(5) . . . . ? N2 N3 N4 C5 -1.5(8) . . . . ? N2 N3 N4 Rh1 -171.3(5) . . . . ? C51 Rh1 N4 N3 -133.1(6) . . . . ? N41 Rh1 N4 N3 -55.3(6) . . . . ? C25 Rh1 N4 N3 116.1(6) . . . . ? C22 Rh1 N4 N3 43.4(9) . . . . ? C21 Rh1 N4 N3 122.8(7) . . . . ? C24 Rh1 N4 N3 80.5(6) . . . . ? C23 Rh1 N4 N3 47.7(6) . . . . ? C51 Rh1 N4 C5 60.5(8) . . . . ? N41 Rh1 N4 C5 138.3(8) . . . . ? C25 Rh1 N4 C5 -50.3(9) . . . . ? C22 Rh1 N4 C5 -123.0(9) . . . . ? C21 Rh1 N4 C5 -43.6(11) . . . . ? C24 Rh1 N4 C5 -86.0(8) . . . . ? C23 Rh1 N4 C5 -118.7(8) . . . . ? N2 Ir1 N31 C31 -84.1(8) . . . . ? N40 Ir1 N31 C31 -172.3(8) . . . . ? C15 Ir1 N31 C31 21.6(9) . . . . ? C13 Ir1 N31 C31 93.7(9) . . . . ? C14 Ir1 N31 C31 60.2(8) . . . . ? C12 Ir1 N31 C31 93.2(12) . . . . ? C11 Ir1 N31 C31 7.0(11) . . . . ? N2 Ir1 N31 C35 92.2(7) . . . . ? N40 Ir1 N31 C35 3.9(6) . . . . ? C15 Ir1 N31 C35 -162.1(7) . . . . ? C13 Ir1 N31 C35 -90.0(7) . . . . ? C14 Ir1 N31 C35 -123.5(7) . . . . ? C12 Ir1 N31 C35 -90.6(11) . . . . ? C11 Ir1 N31 C35 -176.8(7) . . . . ? N2 Ir1 N40 C40 89.9(7) . . . . ? N31 Ir1 N40 C40 173.3(8) . . . . ? C15 Ir1 N40 C40 -70.1(16) . . . . ? C13 Ir1 N40 C40 -68.5(8) . . . . ? C14 Ir1 N40 C40 -96.5(8) . . . . ? C12 Ir1 N40 C40 -28.8(8) . . . . ? C11 Ir1 N40 C40 -6.2(10) . . . . ? N2 Ir1 N40 C36 -87.0(6) . . . . ? N31 Ir1 N40 C36 -3.7(6) . . . . ? C15 Ir1 N40 C36 112.9(14) . . . . ? C13 Ir1 N40 C36 114.6(6) . . . . ? C14 Ir1 N40 C36 86.6(7) . . . . ? C12 Ir1 N40 C36 154.2(6) . . . . ? C11 Ir1 N40 C36 176.8(6) . . . . ? C51 Rh1 N41 C41 176.2(7) . . . . ? N4 Rh1 N41 C41 82.7(7) . . . . ? C25 Rh1 N41 C41 -72.3(13) . . . . ? C22 Rh1 N41 C41 -67.8(7) . . . . ? C21 Rh1 N41 C41 -96.1(7) . . . . ? C24 Rh1 N41 C41 -10.3(9) . . . . ? C23 Rh1 N41 C41 -29.4(7) . . . . ? C51 Rh1 N41 C45 -8.6(6) . . . . ? N4 Rh1 N41 C45 -102.0(6) . . . . ? C25 Rh1 N41 C45 103.0(12) . . . . ? C22 Rh1 N41 C45 107.5(6) . . . . ? C21 Rh1 N41 C45 79.2(6) . . . . ? C24 Rh1 N41 C45 165.0(6) . . . . ? C23 Rh1 N41 C45 145.8(6) . . . . ? N2 N1 C5 N4 0.1(9) . . . . ? N2 N1 C5 C6 179.0(8) . . . . ? N3 N4 C5 N1 0.9(9) . . . . ? Rh1 N4 C5 N1 168.2(6) . . . . ? N3 N4 C5 C6 -178.0(9) . . . . ? Rh1 N4 C5 C6 -10.7(14) . . . . ? N2 Ir1 C11 C12 -129.7(5) . . . . ? N31 Ir1 C11 C12 143.4(6) . . . . ? N40 Ir1 C11 C12 -37.5(8) . . . . ? C15 Ir1 C11 C12 121.1(9) . . . . ? C13 Ir1 C11 C12 38.6(6) . . . . ? C14 Ir1 C11 C12 81.0(6) . . . . ? N2 Ir1 C11 C15 109.2(6) . . . . ? N31 Ir1 C11 C15 22.4(10) . . . . ? N40 Ir1 C11 C15 -158.6(6) . . . . ? C13 Ir1 C11 C15 -82.5(7) . . . . ? C14 Ir1 C11 C15 -40.0(6) . . . . ? C12 Ir1 C11 C15 -121.1(9) . . . . ? N2 Ir1 C11 C16 -7.2(10) . . . . ? N31 Ir1 C11 C16 -94.0(11) . . . . ? N40 Ir1 C11 C16 85.0(11) . . . . ? C15 Ir1 C11 C16 -116.4(13) . . . . ? C13 Ir1 C11 C16 161.1(11) . . . . ? C14 Ir1 C11 C16 -156.4(11) . . . . ? C12 Ir1 C11 C16 122.5(12) . . . . ? C15 C11 C12 C13 -3.1(10) . . . . ? C16 C11 C12 C13 178.6(9) . . . . ? Ir1 C11 C12 C13 -61.4(6) . . . . ? C15 C11 C12 C17 -175.3(9) . . . . ? C16 C11 C12 C17 6.4(15) . . . . ? Ir1 C11 C12 C17 126.4(9) . . . . ? C15 C11 C12 Ir1 58.3(6) . . . . ? C16 C11 C12 Ir1 -120.0(9) . . . . ? N2 Ir1 C12 C11 60.6(6) . . . . ? N31 Ir1 C12 C11 -116.3(10) . . . . ? N40 Ir1 C12 C11 154.5(5) . . . . ? C15 Ir1 C12 C11 -36.2(6) . . . . ? C13 Ir1 C12 C11 -117.1(8) . . . . ? C14 Ir1 C12 C11 -79.5(6) . . . . ? N2 Ir1 C12 C13 177.6(5) . . . . ? N31 Ir1 C12 C13 0.8(13) . . . . ? N40 Ir1 C12 C13 -88.5(6) . . . . ? C15 Ir1 C12 C13 80.8(7) . . . . ? C14 Ir1 C12 C13 37.5(6) . . . . ? C11 Ir1 C12 C13 117.1(8) . . . . ? N2 Ir1 C12 C17 -59.7(11) . . . . ? N31 Ir1 C12 C17 123.5(12) . . . . ? N40 Ir1 C12 C17 34.2(11) . . . . ? C15 Ir1 C12 C17 -156.4(12) . . . . ? C13 Ir1 C12 C17 122.7(13) . . . . ? C14 Ir1 C12 C17 160.2(12) . . . . ? C11 Ir1 C12 C17 -120.2(13) . . . . ? C11 C12 C13 C14 0.0(10) . . . . ? C17 C12 C13 C14 171.9(9) . . . . ? Ir1 C12 C13 C14 -62.1(6) . . . . ? C11 C12 C13 C18 -174.2(9) . . . . ? C17 C12 C13 C18 -2.3(16) . . . . ? Ir1 C12 C13 C18 123.6(10) . . . . ? C11 C12 C13 Ir1 62.1(6) . . . . ? C17 C12 C13 Ir1 -125.9(10) . . . . ? N2 Ir1 C13 C14 111.4(9) . . . . ? N31 Ir1 C13 C14 -62.8(7) . . . . ? N40 Ir1 C13 C14 -143.1(6) . . . . ? C15 Ir1 C13 C14 36.5(6) . . . . ? C12 Ir1 C13 C14 116.9(9) . . . . ? C11 Ir1 C13 C14 79.5(6) . . . . ? N2 Ir1 C13 C12 -5.5(12) . . . . ? N31 Ir1 C13 C12 -179.7(5) . . . . ? N40 Ir1 C13 C12 100.0(6) . . . . ? C15 Ir1 C13 C12 -80.4(6) . . . . ? C14 Ir1 C13 C12 -116.9(9) . . . . ? C11 Ir1 C13 C12 -37.4(6) . . . . ? N2 Ir1 C13 C18 -125.1(11) . . . . ? N31 Ir1 C13 C18 60.7(12) . . . . ? N40 Ir1 C13 C18 -19.6(11) . . . . ? C15 Ir1 C13 C18 159.9(12) . . . . ? C14 Ir1 C13 C18 123.4(13) . . . . ? C12 Ir1 C13 C18 -119.7(13) . . . . ? C11 Ir1 C13 C18 -157.0(12) . . . . ? C12 C13 C14 C15 3.1(10) . . . . ? C18 C13 C14 C15 177.1(10) . . . . ? Ir1 C13 C14 C15 -58.8(6) . . . . ? C12 C13 C14 C19 -178.3(9) . . . . ? C18 C13 C14 C19 -4.3(16) . . . . ? Ir1 C13 C14 C19 119.8(10) . . . . ? C12 C13 C14 Ir1 61.9(6) . . . . ? C18 C13 C14 Ir1 -124.1(10) . . . . ? N2 Ir1 C14 C13 -142.2(6) . . . . ? N31 Ir1 C14 C13 128.6(6) . . . . ? N40 Ir1 C14 C13 48.9(7) . . . . ? C15 Ir1 C14 C13 -120.8(8) . . . . ? C12 Ir1 C14 C13 -38.7(6) . . . . ? C11 Ir1 C14 C13 -80.9(6) . . . . ? N2 Ir1 C14 C15 -21.4(9) . . . . ? N31 Ir1 C14 C15 -110.6(6) . . . . ? N40 Ir1 C14 C15 169.7(5) . . . . ? C13 Ir1 C14 C15 120.8(8) . . . . ? C12 Ir1 C14 C15 82.1(6) . . . . ? C11 Ir1 C14 C15 39.8(6) . . . . ? N2 Ir1 C14 C19 96.3(12) . . . . ? N31 Ir1 C14 C19 7.1(12) . . . . ? N40 Ir1 C14 C19 -72.6(12) . . . . ? C15 Ir1 C14 C19 117.7(14) . . . . ? C13 Ir1 C14 C19 -121.5(14) . . . . ? C12 Ir1 C14 C19 -160.1(13) . . . . ? C11 Ir1 C14 C19 157.6(13) . . . . ? C12 C11 C15 C14 4.9(10) . . . . ? C16 C11 C15 C14 -176.7(8) . . . . ? Ir1 C11 C15 C14 64.2(6) . . . . ? C12 C11 C15 C20 174.2(9) . . . . ? C16 C11 C15 C20 -7.4(15) . . . . ? Ir1 C11 C15 C20 -126.4(11) . . . . ? C12 C11 C15 Ir1 -59.3(6) . . . . ? C16 C11 C15 Ir1 119.1(9) . . . . ? C13 C14 C15 C11 -4.9(10) . . . . ? C19 C14 C15 C11 176.5(9) . . . . ? Ir1 C14 C15 C11 -64.6(6) . . . . ? C13 C14 C15 C20 -174.4(9) . . . . ? C19 C14 C15 C20 7.0(15) . . . . ? Ir1 C14 C15 C20 125.9(10) . . . . ? C13 C14 C15 Ir1 59.7(7) . . . . ? C19 C14 C15 Ir1 -118.9(9) . . . . ? N2 Ir1 C15 C11 -79.0(6) . . . . ? N31 Ir1 C15 C11 -167.2(6) . . . . ? N40 Ir1 C15 C11 80.2(15) . . . . ? C13 Ir1 C15 C11 78.4(6) . . . . ? C14 Ir1 C15 C11 113.8(9) . . . . ? C12 Ir1 C15 C11 35.3(6) . . . . ? N2 Ir1 C15 C14 167.2(6) . . . . ? N31 Ir1 C15 C14 79.0(6) . . . . ? N40 Ir1 C15 C14 -33.6(16) . . . . ? C13 Ir1 C15 C14 -35.4(6) . . . . ? C12 Ir1 C15 C14 -78.6(6) . . . . ? C11 Ir1 C15 C14 -113.8(9) . . . . ? N2 Ir1 C15 C20 45.1(12) . . . . ? N31 Ir1 C15 C20 -43.1(13) . . . . ? N40 Ir1 C15 C20 -155.7(13) . . . . ? C13 Ir1 C15 C20 -157.5(13) . . . . ? C14 Ir1 C15 C20 -122.1(14) . . . . ? C12 Ir1 C15 C20 159.4(13) . . . . ? C11 Ir1 C15 C20 124.1(14) . . . . ? C51 Rh1 C21 C22 128.7(6) . . . . ? N41 Rh1 C21 C22 50.0(6) . . . . ? N4 Rh1 C21 C22 -127.7(6) . . . . ? C25 Rh1 C21 C22 -117.6(8) . . . . ? C24 Rh1 C21 C22 -79.3(6) . . . . ? C23 Rh1 C21 C22 -38.1(5) . . . . ? C51 Rh1 C21 C25 -113.7(6) . . . . ? N41 Rh1 C21 C25 167.7(5) . . . . ? N4 Rh1 C21 C25 -10.0(9) . . . . ? C22 Rh1 C21 C25 117.6(8) . . . . ? C24 Rh1 C21 C25 38.4(6) . . . . ? C23 Rh1 C21 C25 79.5(6) . . . . ? C51 Rh1 C21 C26 5.1(11) . . . . ? N41 Rh1 C21 C26 -73.6(11) . . . . ? N4 Rh1 C21 C26 108.7(11) . . . . ? C25 Rh1 C21 C26 118.8(13) . . . . ? C22 Rh1 C21 C26 -123.6(13) . . . . ? C24 Rh1 C21 C26 157.1(12) . . . . ? C23 Rh1 C21 C26 -161.7(12) . . . . ? C25 C21 C22 C23 3.5(10) . . . . ? C26 C21 C22 C23 -170.8(9) . . . . ? Rh1 C21 C22 C23 64.0(6) . . . . ? C25 C21 C22 C27 179.6(9) . . . . ? C26 C21 C22 C27 5.3(15) . . . . ? Rh1 C21 C22 C27 -120.0(9) . . . . ? C25 C21 C22 Rh1 -60.4(6) . . . . ? C26 C21 C22 Rh1 125.3(10) . . . . ? C51 Rh1 C22 C21 -60.5(6) . . . . ? N41 Rh1 C22 C21 -140.0(6) . . . . ? N4 Rh1 C22 C21 123.4(7) . . . . ? C25 Rh1 C22 C21 38.3(6) . . . . ? C24 Rh1 C22 C21 81.1(6) . . . . ? C23 Rh1 C22 C21 117.0(8) . . . . ? C51 Rh1 C22 C23 -177.6(5) . . . . ? N41 Rh1 C22 C23 102.9(5) . . . . ? N4 Rh1 C22 C23 6.4(9) . . . . ? C25 Rh1 C22 C23 -78.7(6) . . . . ? C21 Rh1 C22 C23 -117.0(8) . . . . ? C24 Rh1 C22 C23 -35.9(6) . . . . ? C51 Rh1 C22 C27 60.0(9) . . . . ? N41 Rh1 C22 C27 -19.5(9) . . . . ? N4 Rh1 C22 C27 -116.0(9) . . . . ? C25 Rh1 C22 C27 158.9(10) . . . . ? C21 Rh1 C22 C27 120.6(11) . . . . ? C24 Rh1 C22 C27 -158.3(10) . . . . ? C23 Rh1 C22 C27 -122.4(11) . . . . ? C21 C22 C23 C24 -1.9(10) . . . . ? C27 C22 C23 C24 -177.9(9) . . . . ? Rh1 C22 C23 C24 60.9(6) . . . . ? C21 C22 C23 C28 176.5(9) . . . . ? C27 C22 C23 C28 0.5(15) . . . . ? Rh1 C22 C23 C28 -120.7(9) . . . . ? C21 C22 C23 Rh1 -62.8(6) . . . . ? C27 C22 C23 Rh1 121.1(9) . . . . ? C51 Rh1 C23 C24 -113.7(9) . . . . ? N41 Rh1 C23 C24 157.5(5) . . . . ? N4 Rh1 C23 C24 64.6(6) . . . . ? C25 Rh1 C23 C24 -37.2(6) . . . . ? C22 Rh1 C23 C24 -118.8(8) . . . . ? C21 Rh1 C23 C24 -81.1(6) . . . . ? C51 Rh1 C23 C22 5.2(11) . . . . ? N41 Rh1 C23 C22 -83.7(5) . . . . ? N4 Rh1 C23 C22 -176.6(5) . . . . ? C25 Rh1 C23 C22 81.7(6) . . . . ? C21 Rh1 C23 C22 37.7(5) . . . . ? C24 Rh1 C23 C22 118.8(8) . . . . ? C51 Rh1 C23 C28 127.6(10) . . . . ? N41 Rh1 C23 C28 38.8(10) . . . . ? N4 Rh1 C23 C28 -54.2(10) . . . . ? C25 Rh1 C23 C28 -155.9(11) . . . . ? C22 Rh1 C23 C28 122.4(12) . . . . ? C21 Rh1 C23 C28 160.1(11) . . . . ? C24 Rh1 C23 C28 -118.7(12) . . . . ? C22 C23 C24 C25 -0.5(10) . . . . ? C28 C23 C24 C25 -179.0(8) . . . . ? Rh1 C23 C24 C25 58.5(6) . . . . ? C22 C23 C24 C29 -177.0(9) . . . . ? C28 C23 C24 C29 4.5(14) . . . . ? Rh1 C23 C24 C29 -118.0(9) . . . . ? C22 C23 C24 Rh1 -59.1(6) . . . . ? C28 C23 C24 Rh1 122.4(8) . . . . ? C51 Rh1 C24 C23 136.4(6) . . . . ? N41 Rh1 C24 C23 -32.3(7) . . . . ? N4 Rh1 C24 C23 -123.0(5) . . . . ? C25 Rh1 C24 C23 119.3(8) . . . . ? C22 Rh1 C24 C23 37.5(5) . . . . ? C21 Rh1 C24 C23 80.1(6) . . . . ? C51 Rh1 C24 C25 17.1(9) . . . . ? N41 Rh1 C24 C25 -151.6(5) . . . . ? N4 Rh1 C24 C25 117.7(6) . . . . ? C22 Rh1 C24 C25 -81.8(6) . . . . ? C21 Rh1 C24 C25 -39.2(6) . . . . ? C23 Rh1 C24 C25 -119.3(8) . . . . ? C51 Rh1 C24 C29 -103.0(12) . . . . ? N41 Rh1 C24 C29 88.3(12) . . . . ? N4 Rh1 C24 C29 -2.4(11) . . . . ? C25 Rh1 C24 C29 -120.1(14) . . . . ? C22 Rh1 C24 C29 158.1(12) . . . . ? C21 Rh1 C24 C29 -159.4(12) . . . . ? C23 Rh1 C24 C29 120.6(13) . . . . ? C23 C24 C25 C21 2.7(10) . . . . ? C29 C24 C25 C21 179.2(9) . . . . ? Rh1 C24 C25 C21 63.4(6) . . . . ? C23 C24 C25 C30 172.0(10) . . . . ? C29 C24 C25 C30 -11.6(16) . . . . ? Rh1 C24 C25 C30 -127.3(11) . . . . ? C23 C24 C25 Rh1 -60.7(6) . . . . ? C29 C24 C25 Rh1 115.7(10) . . . . ? C22 C21 C25 C24 -3.8(10) . . . . ? C26 C21 C25 C24 170.7(8) . . . . ? Rh1 C21 C25 C24 -65.0(6) . . . . ? C22 C21 C25 C30 -172.9(10) . . . . ? C26 C21 C25 C30 1.7(16) . . . . ? Rh1 C21 C25 C30 126.0(11) . . . . ? C22 C21 C25 Rh1 61.2(6) . . . . ? C26 C21 C25 Rh1 -124.3(9) . . . . ? C51 Rh1 C25 C24 -170.0(6) . . . . ? N41 Rh1 C25 C24 83.6(12) . . . . ? N4 Rh1 C25 C24 -69.8(6) . . . . ? C22 Rh1 C25 C24 78.6(6) . . . . ? C21 Rh1 C25 C24 115.8(8) . . . . ? C23 Rh1 C25 C24 35.7(5) . . . . ? C51 Rh1 C25 C21 74.2(6) . . . . ? N41 Rh1 C25 C21 -32.2(13) . . . . ? N4 Rh1 C25 C21 174.5(5) . . . . ? C22 Rh1 C25 C21 -37.1(5) . . . . ? C24 Rh1 C25 C21 -115.8(8) . . . . ? C23 Rh1 C25 C21 -80.1(6) . . . . ? C51 Rh1 C25 C30 -48.1(14) . . . . ? N41 Rh1 C25 C30 -154.6(12) . . . . ? N4 Rh1 C25 C30 52.1(14) . . . . ? C22 Rh1 C25 C30 -159.5(14) . . . . ? C21 Rh1 C25 C30 -122.4(15) . . . . ? C24 Rh1 C25 C30 121.9(15) . . . . ? C23 Rh1 C25 C30 157.6(14) . . . . ? C35 N31 C31 C32 2.5(15) . . . . ? Ir1 N31 C31 C32 178.6(8) . . . . ? N31 C31 C32 C33 -2.0(16) . . . . ? C31 C32 C33 C34 0.3(17) . . . . ? C32 C33 C34 C35 0.9(16) . . . . ? C31 N31 C35 C34 -1.3(14) . . . . ? Ir1 N31 C35 C34 -177.6(7) . . . . ? C31 N31 C35 C36 172.7(9) . . . . ? Ir1 N31 C35 C36 -3.6(10) . . . . ? C33 C34 C35 N31 -0.5(15) . . . . ? C33 C34 C35 C36 -174.0(10) . . . . ? C40 N40 C36 C37 2.8(13) . . . . ? Ir1 N40 C36 C37 179.9(7) . . . . ? C40 N40 C36 C35 -174.1(8) . . . . ? Ir1 N40 C36 C35 3.0(10) . . . . ? N31 C35 C36 C37 -176.4(9) . . . . ? C34 C35 C36 C37 -2.7(15) . . . . ? N31 C35 C36 N40 0.3(12) . . . . ? C34 C35 C36 N40 174.0(9) . . . . ? N40 C36 C37 C38 -1.4(15) . . . . ? C35 C36 C37 C38 175.1(10) . . . . ? C36 C37 C38 C39 -1.0(17) . . . . ? C37 C38 C39 C40 2.1(17) . . . . ? C36 N40 C40 C39 -1.6(14) . . . . ? Ir1 N40 C40 C39 -178.5(7) . . . . ? C38 C39 C40 N40 -0.8(16) . . . . ? C45 N41 C41 C42 -1.8(12) . . . . ? Rh1 N41 C41 C42 173.3(7) . . . . ? N41 C41 C42 C43 1.7(14) . . . . ? C41 C42 C43 C44 -1.4(15) . . . . ? C42 C43 C44 C45 1.2(15) . . . . ? C41 N41 C45 C46 -176.2(7) . . . . ? Rh1 N41 C45 C46 8.3(9) . . . . ? C41 N41 C45 C44 1.6(11) . . . . ? Rh1 N41 C45 C44 -174.0(6) . . . . ? C43 C44 C45 N41 -1.3(13) . . . . ? C43 C44 C45 C46 176.2(9) . . . . ? N41 C45 C46 C51 -2.0(11) . . . . ? C44 C45 C46 C51 -179.6(8) . . . . ? N41 C45 C46 C47 179.9(8) . . . . ? C44 C45 C46 C47 2.3(13) . . . . ? C51 C46 C47 C48 1.6(13) . . . . ? C45 C46 C47 C48 179.7(9) . . . . ? C46 C47 C48 C49 0.4(15) . . . . ? C47 C48 C49 C50 -1.3(16) . . . . ? C48 C49 C50 C51 0.1(16) . . . . ? C49 C50 C51 C46 1.9(14) . . . . ? C49 C50 C51 Rh1 -173.2(8) . . . . ? C47 C46 C51 C50 -2.8(12) . . . . ? C45 C46 C51 C50 179.0(8) . . . . ? C47 C46 C51 Rh1 172.9(6) . . . . ? C45 C46 C51 Rh1 -5.3(9) . . . . ? N41 Rh1 C51 C50 -177.5(8) . . . . ? N4 Rh1 C51 C50 -90.3(8) . . . . ? C25 Rh1 C51 C50 21.6(9) . . . . ? C22 Rh1 C51 C50 91.7(8) . . . . ? C21 Rh1 C51 C50 59.2(8) . . . . ? C24 Rh1 C51 C50 10.5(11) . . . . ? C23 Rh1 C51 C50 88.1(11) . . . . ? N41 Rh1 C51 C46 7.2(6) . . . . ? N4 Rh1 C51 C46 94.4(6) . . . . ? C25 Rh1 C51 C46 -153.7(6) . . . . ? C22 Rh1 C51 C46 -83.6(6) . . . . ? C21 Rh1 C51 C46 -116.1(6) . . . . ? C24 Rh1 C51 C46 -164.8(6) . . . . ? C23 Rh1 C51 C46 -87.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.938 _refine_diff_density_min -1.729 _refine_diff_density_rms 0.154 _database_code_depnum_ccdc_archive 'CCDC 945555' ####################################################################### # # 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_comp11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C43 H49 Ir N7 Ph 2+, 2(F6 P 1-)' _chemical_formula_sum 'C43 H49 F12 Ir N7 P2 Rh' _chemical_formula_weight 1248.94 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c' _symmetry_space_group_name_Hall 'P -4 2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' '-x+1/2, y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 26.0416(5) _cell_length_b 26.0416(5) _cell_length_c 14.3561(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9735.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 191(2) _cell_measurement_reflns_used 79866 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.47 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.704 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4928 _exptl_absorpt_coefficient_mu 3.220 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3986 _exptl_absorpt_correction_T_max 0.7389 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 191(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 94858 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.47 _reflns_number_total 11104 _reflns_number_gt 10584 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _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. # 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 0.500 0.500 -0.000 406 67 ' ' 2 -0.000 1.000 0.500 406 67 ' ' _platon_squeeze_details ? ; _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^)+(0.1088P)^2^+26.0825P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Hooft y Parameter Value . 0.150( 1)' _refine_ls_abs_structure_Flack 0.166(7) _refine_ls_number_reflns 11104 _refine_ls_number_parameters 567 _refine_ls_number_restraints 48 _refine_ls_R_factor_all 0.0516 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1507 _refine_ls_wR_factor_gt 0.1485 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.357131(10) 0.204693(11) 0.13465(2) 0.03377(10) Uani 1 1 d . . . Rh1 Rh 0.527197(19) 0.26061(2) 0.40004(3) 0.02523(12) Uani 1 1 d . . . P1 P 0.0000 0.0000 0.1859(11) 0.159(4) Uani 1 2 d SD . . P2 P 0.5000 0.0000 0.5051(3) 0.0529(8) Uani 1 2 d SD . . P3A P 0.1967(3) 0.3881(3) 0.1373(7) 0.093(3) Uani 0.50 1 d PD . . P3B P 0.2312(4) 0.4146(3) 0.1683(4) 0.106(4) Uani 0.50 1 d PD . . F1 F 0.0000 0.0000 0.3031(17) 0.261(16) Uiso 1 2 d SD . . F2 F 0.0511(7) 0.0403(8) 0.1938(16) 0.218(8) Uiso 1 1 d D . . F3 F 0.0000 0.0000 0.0791 0.231 Uiso 1 2 d S . . F4 F -0.0381(8) 0.0522(7) 0.1857(16) 0.215(8) Uiso 1 1 d D . . F5 F 0.5065(6) -0.0601(4) 0.5087(11) 0.140(5) Uiso 1 1 d D . . F6A F 0.4448(7) -0.0275(11) 0.501(2) 0.142(9) Uiso 0.50 1 d PD . . F6B F 0.5442(9) -0.0023(12) 0.5820(19) 0.152(10) Uiso 0.50 1 d PD . . F7A F 0.5000 0.0000 0.6157(12) 0.105(7) Uiso 0.50 2 d SPD . . F8A F 0.5000 0.0000 0.3942(11) 0.084(6) Uiso 0.50 2 d SPD . . F9 F 0.1761(5) 0.4219(5) 0.2125(9) 0.130(4) Uiso 1 1 d D . . F10 F 0.2349(6) 0.3584(5) 0.1922(12) 0.176(6) Uiso 1 1 d D . . F11A F 0.1664(8) 0.3408(7) 0.1704(15) 0.107(6) Uiso 0.50 1 d PD . . F11B F 0.2481(8) 0.4023(8) 0.2670(11) 0.102(6) Uiso 0.50 1 d PD . . F12A F 0.2266(15) 0.4371(12) 0.111(4) 0.210(16) Uiso 0.50 1 d PD . . F12B F 0.2172(17) 0.4045(19) 0.0635(15) 0.200(15) Uiso 0.50 1 d PD . . F13A F 0.1487(8) 0.4055(10) 0.0846(18) 0.133(8) Uiso 0.50 1 d PD . . F13B F 0.2483(10) 0.4713(8) 0.144(2) 0.140(8) Uiso 0.50 1 d PD . . F14A F 0.2177(15) 0.3482(14) 0.071(3) 0.196(16) Uiso 0.50 1 d PD . . F14B F 0.2849(6) 0.4016(7) 0.1302(15) 0.102(5) Uiso 0.50 1 d PD . . F78B F 0.4582(10) -0.0026(12) 0.4232(18) 0.157(10) Uiso 0.50 1 d PD . . N1 N 0.3910(3) 0.2411(3) 0.2492(4) 0.0317(13) Uani 1 1 d . . . N2 N 0.4364(3) 0.2238(3) 0.2800(4) 0.0336(13) Uani 1 1 d . . . N3 N 0.4530(2) 0.2579(3) 0.3424(4) 0.0350(13) Uani 1 1 d . . . N4 N 0.4197(3) 0.2965(3) 0.3523(5) 0.0392(14) Uani 1 1 d . . . N31 N 0.3673(3) 0.1360(2) 0.2054(4) 0.0328(12) Uani 1 1 d . . . N42 N 0.5452(3) 0.1972(3) 0.3162(5) 0.0425(16) Uani 1 1 d . . . N51 N 0.5459(3) 0.2954(3) 0.2739(5) 0.0441(16) Uani 1 1 d . . . C5 C 0.3811(3) 0.2857(3) 0.2943(5) 0.0358(15) Uani 1 1 d . . . C6 C 0.3372(4) 0.3202(4) 0.2796(6) 0.0456(19) Uani 1 1 d . . . H6A H 0.3495 0.3534 0.2565 0.055 Uiso 1 1 calc R . . H6B H 0.3190 0.3252 0.3387 0.055 Uiso 1 1 calc R . . H6C H 0.3137 0.3050 0.2339 0.055 Uiso 1 1 calc R . . C11 C 0.3459(5) 0.2574(4) 0.0215(6) 0.056(3) Uani 1 1 d . . . C12 C 0.4011(5) 0.2522(4) 0.0329(7) 0.059(3) Uani 1 1 d . . . C13 C 0.4147(3) 0.2002(4) 0.0193(6) 0.0453(19) Uani 1 1 d . . . C14 C 0.3675(3) 0.1737(3) -0.0038(5) 0.0356(16) Uani 1 1 d . . . C15 C 0.3260(4) 0.2089(4) -0.0057(6) 0.047(2) Uani 1 1 d . . . C16 C 0.3173(9) 0.3090(6) 0.0176(8) 0.110(7) Uani 1 1 d . . . H16A H 0.3302 0.3292 -0.0349 0.132 Uiso 1 1 calc R . . H16B H 0.3230 0.3278 0.0758 0.132 Uiso 1 1 calc R . . H16C H 0.2805 0.3027 0.0096 0.132 Uiso 1 1 calc R . . C17 C 0.4339(8) 0.2969(6) 0.0579(11) 0.106(7) Uani 1 1 d . . . H17A H 0.4231 0.3106 0.1184 0.128 Uiso 1 1 calc R . . H17B H 0.4304 0.3236 0.0103 0.128 Uiso 1 1 calc R . . H17C H 0.4698 0.2859 0.0616 0.128 Uiso 1 1 calc R . . C18 C 0.4665(4) 0.1780(6) 0.0237(8) 0.071(4) Uani 1 1 d . . . H18A H 0.4810 0.1838 0.0858 0.085 Uiso 1 1 calc R . . H18B H 0.4884 0.1944 -0.0231 0.085 Uiso 1 1 calc R . . H18C H 0.4647 0.1410 0.0115 0.085 Uiso 1 1 calc R . . C19 C 0.3648(5) 0.1178(4) -0.0267(6) 0.054(2) Uani 1 1 d . . . H19A H 0.3534 0.1135 -0.0913 0.064 Uiso 1 1 calc R . . H19B H 0.3405 0.1008 0.0153 0.064 Uiso 1 1 calc R . . H19C H 0.3989 0.1024 -0.0192 0.064 Uiso 1 1 calc R . . C20 C 0.2720(4) 0.1966(6) -0.0356(7) 0.065(3) Uani 1 1 d . . . H20A H 0.2670 0.2076 -0.1003 0.078 Uiso 1 1 calc R . . H20B H 0.2477 0.2148 0.0048 0.078 Uiso 1 1 calc R . . H20C H 0.2662 0.1596 -0.0308 0.078 Uiso 1 1 calc R . . C21 C 0.5252(4) 0.3197(4) 0.5071(6) 0.048(2) Uani 1 1 d . . . C22 C 0.5779(4) 0.3053(4) 0.4873(6) 0.0446(19) Uani 1 1 d . . . C23 C 0.5833(4) 0.2520(4) 0.5087(6) 0.048(2) Uani 1 1 d . . . C24 C 0.5359(4) 0.2327(4) 0.5412(5) 0.046(2) Uani 1 1 d . . . C25 C 0.5002(4) 0.2736(4) 0.5437(5) 0.048(2) Uani 1 1 d . . . C26 C 0.6194(5) 0.3413(5) 0.4554(8) 0.065(3) Uani 1 1 d . . . H26A H 0.6339 0.3289 0.3966 0.078 Uiso 1 1 calc R . . H26B H 0.6465 0.3429 0.5027 0.078 Uiso 1 1 calc R . . H26C H 0.6049 0.3756 0.4462 0.078 Uiso 1 1 calc R . . C27 C 0.6321(4) 0.2233(5) 0.5020(9) 0.067(3) Uani 1 1 d . . . H27A H 0.6277 0.1939 0.4599 0.080 Uiso 1 1 calc R . . H27B H 0.6420 0.2109 0.5639 0.080 Uiso 1 1 calc R . . H27C H 0.6590 0.2459 0.4777 0.080 Uiso 1 1 calc R . . C28 C 0.5271(6) 0.1803(5) 0.5794(7) 0.068(3) Uani 1 1 d . . . H28A H 0.5489 0.1751 0.6342 0.082 Uiso 1 1 calc R . . H28B H 0.5356 0.1546 0.5319 0.082 Uiso 1 1 calc R . . H28C H 0.4910 0.1766 0.5973 0.082 Uiso 1 1 calc R . . C29 C 0.4467(5) 0.2712(5) 0.5780(7) 0.064(3) Uani 1 1 d . . . H29A H 0.4467 0.2607 0.6436 0.076 Uiso 1 1 calc R . . H29B H 0.4274 0.2461 0.5411 0.076 Uiso 1 1 calc R . . H29C H 0.4307 0.3050 0.5720 0.076 Uiso 1 1 calc R . . C30 C 0.5016(6) 0.3729(5) 0.5000(9) 0.074(3) Uani 1 1 d . . . H30A H 0.5048 0.3854 0.4359 0.089 Uiso 1 1 calc R . . H30B H 0.5197 0.3963 0.5423 0.089 Uiso 1 1 calc R . . H30C H 0.4653 0.3712 0.5174 0.089 Uiso 1 1 calc R . . C31 C 0.4113(3) 0.1099(3) 0.2071(6) 0.0408(17) Uani 1 1 d . . . H31 H 0.4409 0.1247 0.1794 0.049 Uiso 1 1 calc R . . C32 C 0.4154(4) 0.0609(4) 0.2486(7) 0.050(2) Uani 1 1 d . . . H32 H 0.4473 0.0432 0.2503 0.060 Uiso 1 1 calc R . . C33 C 0.3732(5) 0.0402(3) 0.2855(7) 0.053(2) Uani 1 1 d . . . H33 H 0.3748 0.0067 0.3118 0.063 Uiso 1 1 calc R . . C34 C 0.3255(4) 0.0676(4) 0.2858(6) 0.048(2) Uani 1 1 d . . . H34 H 0.2956 0.0533 0.3132 0.057 Uiso 1 1 calc R . . C35 C 0.3247(3) 0.1153(3) 0.2452(5) 0.0343(16) Uani 1 1 d . . . C36 C 0.2794(3) 0.1493(4) 0.2425(5) 0.0388(18) Uani 1 1 d . . . C37 C 0.2313(3) 0.1358(4) 0.2769(6) 0.045(2) Uani 1 1 d . . . H37 H 0.2261 0.1029 0.3039 0.054 Uiso 1 1 calc R . . C38 C 0.1905(4) 0.1707(5) 0.2717(7) 0.057(3) Uani 1 1 d . . . H38 H 0.1574 0.1616 0.2943 0.069 Uiso 1 1 calc R . . C39 C 0.1986(4) 0.2164(5) 0.2351(7) 0.053(2) Uani 1 1 d . . . H39 H 0.1714 0.2407 0.2339 0.063 Uiso 1 1 calc R . . C40 C 0.2459(4) 0.2298(4) 0.1984(7) 0.051(2) Uani 1 1 d . . . H40 H 0.2500 0.2628 0.1712 0.061 Uiso 1 1 calc R . . C41 C 0.2875(3) 0.1965(3) 0.2001(4) 0.0331(15) Uani 1 1 d . . . C42 C 0.5393(4) 0.1476(4) 0.3427(8) 0.055(2) Uani 1 1 d . . . H42 H 0.5271 0.1393 0.4032 0.066 Uiso 1 1 calc R . . C43 C 0.5519(5) 0.1083(5) 0.2780(11) 0.071(4) Uani 1 1 d . . . H43 H 0.5478 0.0735 0.2960 0.085 Uiso 1 1 calc R . . C44 C 0.5696(5) 0.1189(6) 0.1917(11) 0.077(4) Uani 1 1 d . . . H44 H 0.5777 0.0922 0.1491 0.092 Uiso 1 1 calc R . . C45 C 0.5755(4) 0.1691(5) 0.1677(9) 0.064(3) Uani 1 1 d . . . H45 H 0.5893 0.1773 0.1083 0.077 Uiso 1 1 calc R . . C46 C 0.5620(3) 0.2084(4) 0.2274(6) 0.0418(18) Uani 1 1 d . . . C47 C 0.5611(3) 0.2627(4) 0.2046(5) 0.045(2) Uani 1 1 d . . . C48 C 0.5724(4) 0.2809(6) 0.1151(7) 0.065(3) Uani 1 1 d . . . H48 H 0.5845 0.2586 0.0676 0.077 Uiso 1 1 calc R . . C49 C 0.5650(4) 0.3353(6) 0.0980(8) 0.069(3) Uani 1 1 d . . . H49 H 0.5728 0.3492 0.0385 0.083 Uiso 1 1 calc R . . C50 C 0.5466(5) 0.3671(5) 0.1679(8) 0.067(3) Uani 1 1 d . . . H50 H 0.5409 0.4026 0.1563 0.081 Uiso 1 1 calc R . . C51 C 0.5366(4) 0.3461(4) 0.2555(7) 0.054(2) Uani 1 1 d . . . H51 H 0.5230 0.3674 0.3033 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.03443(15) 0.04232(16) 0.02457(14) 0.00119(12) -0.00104(11) 0.00111(11) Rh1 0.0268(2) 0.0319(2) 0.0170(2) -0.00136(18) -0.00344(18) -0.00192(19) P1 0.174(10) 0.111(7) 0.191(11) 0.000 0.000 -0.003(7) P2 0.0517(19) 0.0503(19) 0.057(2) 0.000 0.000 0.0159(15) P3A 0.103(6) 0.084(5) 0.092(6) 0.048(5) 0.038(5) 0.041(4) P3B 0.172(10) 0.105(6) 0.040(3) 0.005(4) 0.007(4) 0.107(7) N1 0.034(3) 0.037(3) 0.024(3) 0.003(2) -0.004(2) 0.004(3) N2 0.035(3) 0.041(3) 0.025(3) -0.002(2) -0.003(2) 0.002(3) N3 0.037(3) 0.039(3) 0.029(3) -0.001(3) -0.002(2) 0.001(3) N4 0.043(3) 0.038(3) 0.036(4) -0.007(3) -0.005(3) 0.007(3) N31 0.040(3) 0.036(3) 0.022(3) 0.002(2) 0.001(2) -0.004(2) N42 0.031(3) 0.051(4) 0.045(4) -0.011(3) -0.008(3) 0.003(3) N51 0.040(3) 0.059(4) 0.033(4) 0.005(3) 0.002(3) -0.003(3) C5 0.042(4) 0.036(4) 0.029(3) -0.002(3) 0.002(3) 0.004(3) C6 0.056(5) 0.042(4) 0.040(4) 0.000(4) -0.006(4) 0.014(4) C11 0.092(8) 0.057(6) 0.020(3) 0.008(4) 0.008(4) 0.019(5) C12 0.095(8) 0.054(5) 0.028(4) -0.001(4) 0.013(5) -0.030(6) C13 0.039(4) 0.064(5) 0.033(4) -0.002(4) 0.005(3) -0.011(4) C14 0.035(4) 0.050(4) 0.023(3) 0.003(3) -0.002(3) -0.002(3) C15 0.044(4) 0.073(6) 0.023(3) 0.004(4) 0.002(3) 0.014(4) C16 0.21(2) 0.090(10) 0.032(5) 0.016(6) 0.012(8) 0.079(12) C17 0.161(17) 0.089(10) 0.068(9) 0.002(8) 0.028(10) -0.072(11) C18 0.036(5) 0.137(12) 0.041(5) 0.004(6) 0.002(4) 0.005(6) C19 0.076(7) 0.056(5) 0.029(4) -0.006(4) 0.009(4) -0.016(5) C20 0.040(5) 0.125(10) 0.031(4) 0.002(6) -0.004(4) 0.017(6) C21 0.074(6) 0.048(4) 0.022(4) -0.014(3) -0.002(4) -0.010(4) C22 0.044(4) 0.054(5) 0.036(4) -0.008(4) -0.007(3) -0.016(4) C23 0.047(5) 0.064(6) 0.031(4) -0.005(4) -0.019(4) -0.003(4) C24 0.060(5) 0.057(5) 0.021(3) 0.005(3) -0.013(3) -0.011(4) C25 0.063(5) 0.066(6) 0.016(3) -0.001(3) -0.001(3) -0.017(4) C26 0.066(6) 0.070(7) 0.058(6) -0.012(5) 0.016(5) -0.029(5) C27 0.048(5) 0.093(9) 0.059(6) 0.011(6) -0.018(5) 0.003(5) C28 0.104(9) 0.069(7) 0.033(5) 0.014(4) -0.003(5) -0.018(6) C29 0.065(6) 0.089(8) 0.037(5) -0.010(5) 0.005(4) -0.016(6) C30 0.105(10) 0.061(7) 0.056(6) -0.017(6) 0.011(7) -0.003(7) C31 0.041(4) 0.045(4) 0.037(4) 0.003(3) 0.002(3) 0.009(3) C32 0.063(6) 0.040(4) 0.045(5) 0.003(4) -0.009(4) 0.014(4) C33 0.085(7) 0.030(4) 0.042(5) 0.005(3) -0.011(5) -0.006(4) C34 0.058(5) 0.050(5) 0.035(4) 0.004(4) -0.007(4) -0.013(4) C35 0.040(4) 0.043(4) 0.020(3) -0.006(3) -0.003(3) -0.007(3) C36 0.039(4) 0.055(5) 0.023(3) -0.011(3) -0.005(3) -0.010(3) C37 0.032(4) 0.068(6) 0.036(4) -0.004(4) 0.003(3) -0.011(4) C38 0.039(5) 0.090(8) 0.043(5) -0.002(5) -0.001(4) -0.005(5) C39 0.036(4) 0.079(7) 0.042(5) -0.009(5) 0.000(4) 0.008(4) C40 0.044(5) 0.070(6) 0.039(4) -0.002(4) -0.001(4) 0.005(4) C41 0.031(3) 0.053(4) 0.016(3) -0.005(3) -0.001(2) 0.000(3) C42 0.050(5) 0.048(5) 0.069(7) -0.002(4) -0.016(4) 0.009(4) C43 0.052(6) 0.060(6) 0.101(11) -0.017(7) -0.016(6) 0.007(5) C44 0.067(7) 0.083(9) 0.080(9) -0.032(7) -0.017(6) 0.030(7) C45 0.045(5) 0.089(8) 0.059(6) -0.024(6) -0.001(4) 0.018(5) C46 0.031(4) 0.061(5) 0.033(4) -0.012(4) -0.002(3) 0.001(3) C47 0.029(4) 0.081(6) 0.025(4) -0.005(4) 0.002(3) -0.006(4) C48 0.042(4) 0.119(10) 0.033(5) 0.004(5) 0.008(4) -0.013(5) C49 0.054(6) 0.112(10) 0.041(5) 0.014(6) 0.001(5) -0.021(6) C50 0.074(7) 0.073(7) 0.055(6) 0.032(6) -0.008(5) -0.005(6) C51 0.063(6) 0.059(6) 0.038(5) 0.009(4) -0.006(4) -0.011(5) _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 C41 2.054(7) . ? Ir1 N31 2.074(6) . ? Ir1 N1 2.094(7) . ? Ir1 C11 2.146(9) . ? Ir1 C14 2.162(8) . ? Ir1 C15 2.174(8) . ? Ir1 C12 2.230(9) . ? Ir1 C13 2.237(9) . ? Rh1 N51 2.082(8) . ? Rh1 N42 2.098(7) . ? Rh1 N3 2.104(6) . ? Rh1 C23 2.149(8) . ? Rh1 C22 2.159(8) . ? Rh1 C24 2.165(8) . ? Rh1 C21 2.176(8) . ? Rh1 C25 2.205(8) . ? P1 F3 1.533(15) . ? P1 F4 1.683(16) . ? P1 F4 1.683(16) 3 ? P1 F1 1.68(2) . ? P1 F2 1.698(16) 3 ? P1 F2 1.698(16) . ? P2 F5 1.575(12) . ? P2 F5 1.576(12) 3_655 ? P2 F7A 1.587(16) . ? P2 F8A 1.593(15) . ? P2 F6B 1.596(16) . ? P2 F6B 1.596(16) 3_655 ? P2 F78B 1.604(16) 3_655 ? P2 F78B 1.604(16) . ? P2 F6A 1.606(16) 3_655 ? P2 F6A 1.606(16) . ? P3A F10 1.488(14) . ? P3A F9 1.490(13) . ? P3A F14A 1.513(17) . ? P3A F13A 1.527(16) . ? P3A F11A 1.540(15) . ? P3A F12A 1.541(18) . ? P3B F10 1.507(14) . ? P3B F11B 1.519(15) . ? P3B F14B 1.539(14) . ? P3B F12B 1.570(17) . ? P3B F9 1.580(12) . ? P3B F13B 1.583(16) . ? N1 N2 1.340(9) . ? N1 C5 1.354(10) . ? N2 N3 1.333(9) . ? N3 N4 1.333(9) . ? N4 C5 1.335(11) . ? N31 C31 1.333(11) . ? N31 C35 1.360(10) . ? N42 C42 1.355(13) . ? N42 C46 1.379(12) . ? N51 C51 1.368(14) . ? N51 C47 1.369(12) . ? C5 C6 1.471(12) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C15 1.420(16) . ? C11 C12 1.452(18) . ? C11 C16 1.537(16) . ? C12 C13 1.414(15) . ? C12 C17 1.487(17) . ? C13 C14 1.448(12) . ? C13 C18 1.469(14) . ? C14 C15 1.417(13) . ? C14 C19 1.494(13) . ? C15 C20 1.505(14) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.452(14) . ? C21 C25 1.463(13) . ? C21 C30 1.517(17) . ? C22 C23 1.427(14) . ? C22 C26 1.502(13) . ? C23 C24 1.411(14) . ? C23 C27 1.480(16) . ? C24 C25 1.417(16) . ? C24 C28 1.488(14) . ? C25 C29 1.477(15) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.412(12) . ? C31 H31 0.9500 . ? C32 C33 1.334(16) . ? C32 H32 0.9500 . ? C33 C34 1.432(15) . ? C33 H33 0.9500 . ? C34 C35 1.372(12) . ? C34 H34 0.9500 . ? C35 C36 1.474(12) . ? C36 C41 1.388(12) . ? C36 C37 1.392(11) . ? C37 C38 1.400(15) . ? C37 H37 0.9500 . ? C38 C39 1.319(17) . ? C38 H38 0.9500 . ? C39 C40 1.383(14) . ? C39 H39 0.9500 . ? C40 C41 1.388(12) . ? C40 H40 0.9500 . ? C42 C43 1.421(17) . ? C42 H42 0.9500 . ? C43 C44 1.35(2) . ? C43 H43 0.9500 . ? C44 C45 1.36(2) . ? C44 H44 0.9500 . ? C45 C46 1.380(14) . ? C45 H45 0.9500 . ? C46 C47 1.451(15) . ? C47 C48 1.401(13) . ? C48 C49 1.45(2) . ? C48 H48 0.9500 . ? C49 C50 1.39(2) . ? C49 H49 0.9500 . ? C50 C51 1.397(14) . ? C50 H50 0.9500 . ? C51 H51 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 C41 Ir1 N31 78.4(3) . . ? C41 Ir1 N1 93.4(3) . . ? N31 Ir1 N1 87.3(2) . . ? C41 Ir1 C11 107.0(4) . . ? N31 Ir1 C11 159.9(3) . . ? N1 Ir1 C11 111.2(4) . . ? C41 Ir1 C14 119.5(3) . . ? N31 Ir1 C14 96.4(3) . . ? N1 Ir1 C14 147.0(3) . . ? C11 Ir1 C14 63.9(3) . . ? C41 Ir1 C15 95.7(3) . . ? N31 Ir1 C15 123.0(3) . . ? N1 Ir1 C15 149.6(3) . . ? C11 Ir1 C15 38.4(4) . . ? C14 Ir1 C15 38.2(3) . . ? C41 Ir1 C12 144.1(4) . . ? N31 Ir1 C12 137.2(4) . . ? N1 Ir1 C12 92.7(3) . . ? C11 Ir1 C12 38.7(5) . . ? C14 Ir1 C12 62.7(3) . . ? C15 Ir1 C12 63.7(4) . . ? C41 Ir1 C13 157.7(3) . . ? N31 Ir1 C13 103.4(3) . . ? N1 Ir1 C13 108.8(3) . . ? C11 Ir1 C13 64.2(4) . . ? C14 Ir1 C13 38.4(3) . . ? C15 Ir1 C13 64.3(3) . . ? C12 Ir1 C13 36.9(4) . . ? N51 Rh1 N42 77.9(3) . . ? N51 Rh1 N3 83.5(3) . . ? N42 Rh1 N3 87.3(3) . . ? N51 Rh1 C23 121.2(3) . . ? N42 Rh1 C23 100.5(3) . . ? N3 Rh1 C23 155.0(3) . . ? N51 Rh1 C22 97.3(3) . . ? N42 Rh1 C22 128.3(3) . . ? N3 Rh1 C22 143.9(3) . . ? C23 Rh1 C22 38.7(4) . . ? N51 Rh1 C24 159.3(3) . . ? N42 Rh1 C24 104.4(3) . . ? N3 Rh1 C24 117.0(3) . . ? C23 Rh1 C24 38.2(4) . . ? C22 Rh1 C24 64.8(4) . . ? N51 Rh1 C21 108.2(3) . . ? N42 Rh1 C21 165.5(4) . . ? N3 Rh1 C21 106.2(3) . . ? C23 Rh1 C21 65.0(4) . . ? C22 Rh1 C21 39.1(4) . . ? C24 Rh1 C21 65.1(4) . . ? N51 Rh1 C25 145.2(4) . . ? N42 Rh1 C25 136.8(4) . . ? N3 Rh1 C25 94.6(3) . . ? C23 Rh1 C25 63.5(4) . . ? C22 Rh1 C25 64.6(4) . . ? C24 Rh1 C25 37.8(4) . . ? C21 Rh1 C25 39.0(4) . . ? F3 P1 F4 89.9(9) . . ? F3 P1 F4 89.9(9) . 3 ? F4 P1 F4 179.8(19) . 3 ? F3 P1 F1 180.000(2) . . ? F4 P1 F1 90.1(9) . . ? F4 P1 F1 90.1(9) 3 . ? F3 P1 F2 93.8(10) . 3 ? F4 P1 F2 92.1(11) . 3 ? F4 P1 F2 87.9(11) 3 3 ? F1 P1 F2 86.2(10) . 3 ? F3 P1 F2 93.8(10) . . ? F4 P1 F2 87.9(11) . . ? F4 P1 F2 92.1(11) 3 . ? F1 P1 F2 86.2(10) . . ? F2 P1 F2 172.4(19) 3 . ? F5 P2 F5 176.3(12) . 3_655 ? F5 P2 F7A 88.1(6) . . ? F5 P2 F7A 88.1(6) 3_655 . ? F5 P2 F8A 91.9(6) . . ? F5 P2 F8A 91.9(6) 3_655 . ? F7A P2 F8A 180.000(2) . . ? F5 P2 F6B 82.1(12) . . ? F5 P2 F6B 95.3(12) 3_655 . ? F5 P2 F6B 95.3(12) . 3_655 ? F5 P2 F6B 82.1(12) 3_655 3_655 ? F6B P2 F6B 92(2) . 3_655 ? F5 P2 F78B 89.6(12) . 3_655 ? F5 P2 F78B 93.1(12) 3_655 3_655 ? F6B P2 F78B 91.1(16) . 3_655 ? F6B P2 F78B 174.3(16) 3_655 3_655 ? F5 P2 F78B 93.1(12) . . ? F5 P2 F78B 89.6(12) 3_655 . ? F6B P2 F78B 174.3(16) . . ? F6B P2 F78B 91.1(16) 3_655 . ? F78B P2 F78B 86(2) 3_655 . ? F5 P2 F6A 110.3(12) . 3_655 ? F5 P2 F6A 69.8(12) 3_655 3_655 ? F7A P2 F6A 91.9(11) . 3_655 ? F8A P2 F6A 88.1(11) . 3_655 ? F5 P2 F6A 69.8(12) . . ? F5 P2 F6A 110.3(12) 3_655 . ? F7A P2 F6A 91.9(11) . . ? F8A P2 F6A 88.1(11) . . ? F6A P2 F6A 176(2) 3_655 . ? F10 P3A F9 99.4(11) . . ? F10 P3A F14A 74.5(18) . . ? F9 P3A F14A 172.2(19) . . ? F10 P3A F13A 164.4(14) . . ? F9 P3A F13A 83.8(12) . . ? F14A P3A F13A 101(2) . . ? F10 P3A F11A 76.3(11) . . ? F9 P3A F11A 93.7(10) . . ? F14A P3A F11A 80.2(18) . . ? F13A P3A F11A 88.3(14) . . ? F10 P3A F12A 103(2) . . ? F9 P3A F12A 83(2) . . ? F14A P3A F12A 103(2) . . ? F13A P3A F12A 93(2) . . ? F11A P3A F12A 176(2) . . ? F10 P3B F11B 64.1(10) . . ? F10 P3B F14B 78.9(10) . . ? F11B P3B F14B 91.2(12) . . ? F10 P3B F12B 94(2) . . ? F11B P3B F12B 158(2) . . ? F14B P3B F12B 80.4(18) . . ? F10 P3B F9 94.8(10) . . ? F11B P3B F9 85.1(10) . . ? F14B P3B F9 173.6(11) . . ? F12B P3B F9 101.2(18) . . ? F10 P3B F13B 159.9(14) . . ? F11B P3B F13B 108.8(16) . . ? F14B P3B F13B 82.6(14) . . ? F12B P3B F13B 90(2) . . ? F9 P3B F13B 103.5(12) . . ? N2 N1 C5 107.5(7) . . ? N2 N1 Ir1 118.5(5) . . ? C5 N1 Ir1 133.1(5) . . ? N3 N2 N1 106.3(6) . . ? N2 N3 N4 111.3(6) . . ? N2 N3 Rh1 125.7(5) . . ? N4 N3 Rh1 122.0(5) . . ? N3 N4 C5 105.3(6) . . ? C31 N31 C35 119.4(7) . . ? C31 N31 Ir1 124.0(5) . . ? C35 N31 Ir1 116.4(5) . . ? C42 N42 C46 119.9(8) . . ? C42 N42 Rh1 124.3(7) . . ? C46 N42 Rh1 115.8(6) . . ? C51 N51 C47 120.8(9) . . ? C51 N51 Rh1 123.1(7) . . ? C47 N51 Rh1 115.4(7) . . ? N4 C5 N1 109.5(7) . . ? N4 C5 C6 123.1(7) . . ? N1 C5 C6 127.2(8) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C15 C11 C12 108.0(9) . . ? C15 C11 C16 126.2(13) . . ? C12 C11 C16 124.4(14) . . ? C15 C11 Ir1 71.9(5) . . ? C12 C11 Ir1 73.8(5) . . ? C16 C11 Ir1 130.7(7) . . ? C13 C12 C11 108.8(9) . . ? C13 C12 C17 129.7(14) . . ? C11 C12 C17 121.5(13) . . ? C13 C12 Ir1 71.8(5) . . ? C11 C12 Ir1 67.5(5) . . ? C17 C12 Ir1 124.8(8) . . ? C12 C13 C14 106.0(9) . . ? C12 C13 C18 126.9(10) . . ? C14 C13 C18 127.0(10) . . ? C12 C13 Ir1 71.3(5) . . ? C14 C13 Ir1 68.0(4) . . ? C18 C13 Ir1 127.2(7) . . ? C15 C14 C13 110.1(8) . . ? C15 C14 C19 126.2(8) . . ? C13 C14 C19 123.6(9) . . ? C15 C14 Ir1 71.4(5) . . ? C13 C14 Ir1 73.6(5) . . ? C19 C14 Ir1 124.1(6) . . ? C14 C15 C11 107.0(8) . . ? C14 C15 C20 125.5(10) . . ? C11 C15 C20 127.5(10) . . ? C14 C15 Ir1 70.4(4) . . ? C11 C15 Ir1 69.7(5) . . ? C20 C15 Ir1 127.0(6) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 106.2(9) . . ? C22 C21 C30 127.3(10) . . ? C25 C21 C30 126.3(11) . . ? C22 C21 Rh1 69.8(5) . . ? C25 C21 Rh1 71.6(5) . . ? C30 C21 Rh1 127.4(7) . . ? C23 C22 C21 107.6(8) . . ? C23 C22 C26 127.0(10) . . ? C21 C22 C26 125.3(10) . . ? C23 C22 Rh1 70.3(5) . . ? C21 C22 Rh1 71.1(4) . . ? C26 C22 Rh1 126.9(7) . . ? C24 C23 C22 109.4(9) . . ? C24 C23 C27 126.3(10) . . ? C22 C23 C27 124.2(10) . . ? C24 C23 Rh1 71.5(5) . . ? C22 C23 Rh1 71.1(5) . . ? C27 C23 Rh1 126.1(7) . . ? C23 C24 C25 108.3(8) . . ? C23 C24 C28 125.7(10) . . ? C25 C24 C28 125.4(10) . . ? C23 C24 Rh1 70.3(5) . . ? C25 C24 Rh1 72.6(5) . . ? C28 C24 Rh1 129.6(7) . . ? C24 C25 C21 108.4(9) . . ? C24 C25 C29 126.5(10) . . ? C21 C25 C29 125.1(11) . . ? C24 C25 Rh1 69.5(5) . . ? C21 C25 Rh1 69.4(4) . . ? C29 C25 Rh1 127.3(6) . . ? C22 C26 H26A 109.5 . . ? C22 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C22 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C21 C30 H30A 109.5 . . ? C21 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C21 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N31 C31 C32 122.3(8) . . ? N31 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C33 C32 C31 118.0(9) . . ? C33 C32 H32 121.0 . . ? C31 C32 H32 121.0 . . ? C32 C33 C34 120.9(8) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C35 C34 C33 117.7(9) . . ? C35 C34 H34 121.2 . . ? C33 C34 H34 121.2 . . ? N31 C35 C34 121.6(8) . . ? N31 C35 C36 113.8(7) . . ? C34 C35 C36 124.6(8) . . ? C41 C36 C37 121.0(9) . . ? C41 C36 C35 115.0(7) . . ? C37 C36 C35 124.0(9) . . ? C36 C37 C38 120.1(10) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C39 C38 C37 119.0(9) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C38 C39 C40 121.5(10) . . ? C38 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C39 C40 C41 122.0(10) . . ? C39 C40 H40 119.0 . . ? C41 C40 H40 119.0 . . ? C40 C41 C36 116.3(8) . . ? C40 C41 Ir1 128.0(7) . . ? C36 C41 Ir1 115.2(6) . . ? N42 C42 C43 118.4(11) . . ? N42 C42 H42 120.8 . . ? C43 C42 H42 120.8 . . ? C44 C43 C42 122.2(13) . . ? C44 C43 H43 118.9 . . ? C42 C43 H43 118.9 . . ? C43 C44 C45 117.8(11) . . ? C43 C44 H44 121.1 . . ? C45 C44 H44 121.1 . . ? C44 C45 C46 121.8(12) . . ? C44 C45 H45 119.1 . . ? C46 C45 H45 119.1 . . ? N42 C46 C45 119.8(10) . . ? N42 C46 C47 114.2(7) . . ? C45 C46 C47 125.9(9) . . ? N51 C47 C48 121.1(11) . . ? N51 C47 C46 116.5(8) . . ? C48 C47 C46 122.3(10) . . ? C47 C48 C49 117.2(11) . . ? C47 C48 H48 121.4 . . ? C49 C48 H48 121.4 . . ? C50 C49 C48 120.5(10) . . ? C50 C49 H49 119.7 . . ? C48 C49 H49 119.7 . . ? C49 C50 C51 118.8(12) . . ? C49 C50 H50 120.6 . . ? C51 C50 H50 120.6 . . ? N51 C51 C50 121.3(11) . . ? N51 C51 H51 119.4 . . ? C50 C51 H51 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 C41 Ir1 N1 N2 130.1(6) . . . . ? N31 Ir1 N1 N2 51.9(6) . . . . ? C11 Ir1 N1 N2 -120.2(6) . . . . ? C14 Ir1 N1 N2 -45.7(8) . . . . ? C15 Ir1 N1 N2 -122.5(7) . . . . ? C12 Ir1 N1 N2 -85.3(6) . . . . ? C13 Ir1 N1 N2 -51.4(6) . . . . ? C41 Ir1 N1 C5 -62.3(8) . . . . ? N31 Ir1 N1 C5 -140.5(8) . . . . ? C11 Ir1 N1 C5 47.4(8) . . . . ? C14 Ir1 N1 C5 121.9(8) . . . . ? C15 Ir1 N1 C5 45.1(11) . . . . ? C12 Ir1 N1 C5 82.3(8) . . . . ? C13 Ir1 N1 C5 116.3(8) . . . . ? C5 N1 N2 N3 -0.1(8) . . . . ? Ir1 N1 N2 N3 170.5(5) . . . . ? N1 N2 N3 N4 -0.1(8) . . . . ? N1 N2 N3 Rh1 -168.8(5) . . . . ? N51 Rh1 N3 N2 79.1(6) . . . . ? N42 Rh1 N3 N2 0.9(6) . . . . ? C23 Rh1 N3 N2 -108.6(9) . . . . ? C22 Rh1 N3 N2 172.6(6) . . . . ? C24 Rh1 N3 N2 -103.9(6) . . . . ? C21 Rh1 N3 N2 -173.8(6) . . . . ? C25 Rh1 N3 N2 -135.9(6) . . . . ? N51 Rh1 N3 N4 -88.5(6) . . . . ? N42 Rh1 N3 N4 -166.6(6) . . . . ? C23 Rh1 N3 N4 83.9(10) . . . . ? C22 Rh1 N3 N4 5.1(9) . . . . ? C24 Rh1 N3 N4 88.6(6) . . . . ? C21 Rh1 N3 N4 18.7(6) . . . . ? C25 Rh1 N3 N4 56.6(6) . . . . ? N2 N3 N4 C5 0.2(8) . . . . ? Rh1 N3 N4 C5 169.4(5) . . . . ? C41 Ir1 N31 C31 -175.8(7) . . . . ? N1 Ir1 N31 C31 -81.7(7) . . . . ? C11 Ir1 N31 C31 76.2(13) . . . . ? C14 Ir1 N31 C31 65.4(7) . . . . ? C15 Ir1 N31 C31 94.9(7) . . . . ? C12 Ir1 N31 C31 9.3(9) . . . . ? C13 Ir1 N31 C31 27.0(7) . . . . ? C41 Ir1 N31 C35 9.8(5) . . . . ? N1 Ir1 N31 C35 103.8(5) . . . . ? C11 Ir1 N31 C35 -98.2(12) . . . . ? C14 Ir1 N31 C35 -109.1(5) . . . . ? C15 Ir1 N31 C35 -79.6(6) . . . . ? C12 Ir1 N31 C35 -165.2(6) . . . . ? C13 Ir1 N31 C35 -147.4(5) . . . . ? N51 Rh1 N42 C42 -174.0(7) . . . . ? N3 Rh1 N42 C42 -90.1(7) . . . . ? C23 Rh1 N42 C42 66.1(7) . . . . ? C22 Rh1 N42 C42 96.2(7) . . . . ? C24 Rh1 N42 C42 27.1(7) . . . . ? C21 Rh1 N42 C42 69.3(15) . . . . ? C25 Rh1 N42 C42 3.8(9) . . . . ? N51 Rh1 N42 C46 3.2(6) . . . . ? N3 Rh1 N42 C46 87.2(6) . . . . ? C23 Rh1 N42 C46 -116.7(6) . . . . ? C22 Rh1 N42 C46 -86.6(7) . . . . ? C24 Rh1 N42 C46 -155.7(6) . . . . ? C21 Rh1 N42 C46 -113.4(14) . . . . ? C25 Rh1 N42 C46 -179.0(6) . . . . ? N42 Rh1 N51 C51 168.7(8) . . . . ? N3 Rh1 N51 C51 80.0(8) . . . . ? C23 Rh1 N51 C51 -96.2(8) . . . . ? C22 Rh1 N51 C51 -63.6(8) . . . . ? C24 Rh1 N51 C51 -92.4(12) . . . . ? C21 Rh1 N51 C51 -25.0(8) . . . . ? C25 Rh1 N51 C51 -8.6(11) . . . . ? N42 Rh1 N51 C47 -1.8(6) . . . . ? N3 Rh1 N51 C47 -90.5(6) . . . . ? C23 Rh1 N51 C47 93.3(7) . . . . ? C22 Rh1 N51 C47 125.9(6) . . . . ? C24 Rh1 N51 C47 97.1(11) . . . . ? C21 Rh1 N51 C47 164.5(6) . . . . ? C25 Rh1 N51 C47 -179.1(6) . . . . ? N3 N4 C5 N1 -0.2(9) . . . . ? N3 N4 C5 C6 -176.5(8) . . . . ? N2 N1 C5 N4 0.2(9) . . . . ? Ir1 N1 C5 N4 -168.4(6) . . . . ? N2 N1 C5 C6 176.3(8) . . . . ? Ir1 N1 C5 C6 7.7(13) . . . . ? C41 Ir1 C11 C15 -77.4(6) . . . . ? N31 Ir1 C11 C15 25.6(14) . . . . ? N1 Ir1 C11 C15 -178.1(5) . . . . ? C14 Ir1 C11 C15 37.6(5) . . . . ? C12 Ir1 C11 C15 115.8(8) . . . . ? C13 Ir1 C11 C15 80.5(6) . . . . ? C41 Ir1 C11 C12 166.8(5) . . . . ? N31 Ir1 C11 C12 -90.2(12) . . . . ? N1 Ir1 C11 C12 66.1(6) . . . . ? C14 Ir1 C11 C12 -78.1(6) . . . . ? C15 Ir1 C11 C12 -115.8(8) . . . . ? C13 Ir1 C11 C12 -35.2(5) . . . . ? C41 Ir1 C11 C16 45.1(16) . . . . ? N31 Ir1 C11 C16 148.1(14) . . . . ? N1 Ir1 C11 C16 -55.6(16) . . . . ? C14 Ir1 C11 C16 160.1(17) . . . . ? C15 Ir1 C11 C16 122.5(18) . . . . ? C12 Ir1 C11 C16 -121.7(18) . . . . ? C13 Ir1 C11 C16 -157.0(17) . . . . ? C15 C11 C12 C13 -4.1(10) . . . . ? C16 C11 C12 C13 -171.2(8) . . . . ? Ir1 C11 C12 C13 60.2(7) . . . . ? C15 C11 C12 C17 177.7(10) . . . . ? C16 C11 C12 C17 10.5(15) . . . . ? Ir1 C11 C12 C17 -118.1(10) . . . . ? C15 C11 C12 Ir1 -64.2(6) . . . . ? C16 C11 C12 Ir1 128.6(9) . . . . ? C41 Ir1 C12 C13 -142.0(6) . . . . ? N31 Ir1 C12 C13 29.5(8) . . . . ? N1 Ir1 C12 C13 118.4(6) . . . . ? C11 Ir1 C12 C13 -120.2(9) . . . . ? C14 Ir1 C12 C13 -38.6(5) . . . . ? C15 Ir1 C12 C13 -81.6(6) . . . . ? C41 Ir1 C12 C11 -21.8(9) . . . . ? N31 Ir1 C12 C11 149.7(6) . . . . ? N1 Ir1 C12 C11 -121.4(6) . . . . ? C14 Ir1 C12 C11 81.5(6) . . . . ? C15 Ir1 C12 C11 38.6(6) . . . . ? C13 Ir1 C12 C11 120.2(9) . . . . ? C41 Ir1 C12 C17 91.9(15) . . . . ? N31 Ir1 C12 C17 -96.6(14) . . . . ? N1 Ir1 C12 C17 -7.7(14) . . . . ? C11 Ir1 C12 C17 113.7(16) . . . . ? C14 Ir1 C12 C17 -164.8(16) . . . . ? C15 Ir1 C12 C17 152.3(15) . . . . ? C13 Ir1 C12 C17 -126.1(17) . . . . ? C11 C12 C13 C14 1.9(10) . . . . ? C17 C12 C13 C14 180.0(11) . . . . ? Ir1 C12 C13 C14 59.4(6) . . . . ? C11 C12 C13 C18 179.5(9) . . . . ? C17 C12 C13 C18 -2.4(17) . . . . ? Ir1 C12 C13 C18 -122.9(10) . . . . ? C11 C12 C13 Ir1 -57.5(6) . . . . ? C17 C12 C13 Ir1 120.5(12) . . . . ? C41 Ir1 C13 C12 108.1(10) . . . . ? N31 Ir1 C13 C12 -159.9(6) . . . . ? N1 Ir1 C13 C12 -68.2(7) . . . . ? C11 Ir1 C13 C12 36.9(7) . . . . ? C14 Ir1 C13 C12 116.8(8) . . . . ? C15 Ir1 C13 C12 79.7(7) . . . . ? C41 Ir1 C13 C14 -8.7(12) . . . . ? N31 Ir1 C13 C14 83.4(5) . . . . ? N1 Ir1 C13 C14 175.1(5) . . . . ? C11 Ir1 C13 C14 -79.9(6) . . . . ? C15 Ir1 C13 C14 -37.1(5) . . . . ? C12 Ir1 C13 C14 -116.8(8) . . . . ? C41 Ir1 C13 C18 -129.3(11) . . . . ? N31 Ir1 C13 C18 -37.2(11) . . . . ? N1 Ir1 C13 C18 54.5(11) . . . . ? C11 Ir1 C13 C18 159.5(12) . . . . ? C14 Ir1 C13 C18 -120.6(13) . . . . ? C15 Ir1 C13 C18 -157.7(12) . . . . ? C12 Ir1 C13 C18 122.6(13) . . . . ? C12 C13 C14 C15 0.9(9) . . . . ? C18 C13 C14 C15 -176.7(9) . . . . ? Ir1 C13 C14 C15 62.5(6) . . . . ? C12 C13 C14 C19 178.0(8) . . . . ? C18 C13 C14 C19 0.3(14) . . . . ? Ir1 C13 C14 C19 -120.4(8) . . . . ? C12 C13 C14 Ir1 -61.6(6) . . . . ? C18 C13 C14 Ir1 120.8(10) . . . . ? C41 Ir1 C14 C15 57.8(6) . . . . ? N31 Ir1 C14 C15 138.0(6) . . . . ? N1 Ir1 C14 C15 -127.0(6) . . . . ? C11 Ir1 C14 C15 -37.8(6) . . . . ? C12 Ir1 C14 C15 -81.3(7) . . . . ? C13 Ir1 C14 C15 -118.4(8) . . . . ? C41 Ir1 C14 C13 176.2(5) . . . . ? N31 Ir1 C14 C13 -103.5(5) . . . . ? N1 Ir1 C14 C13 -8.6(8) . . . . ? C11 Ir1 C14 C13 80.6(7) . . . . ? C15 Ir1 C14 C13 118.4(8) . . . . ? C12 Ir1 C14 C13 37.1(6) . . . . ? C41 Ir1 C14 C19 -63.9(9) . . . . ? N31 Ir1 C14 C19 16.4(8) . . . . ? N1 Ir1 C14 C19 111.3(8) . . . . ? C11 Ir1 C14 C19 -159.5(9) . . . . ? C15 Ir1 C14 C19 -121.7(10) . . . . ? C12 Ir1 C14 C19 157.0(9) . . . . ? C13 Ir1 C14 C19 119.9(10) . . . . ? C13 C14 C15 C11 -3.4(9) . . . . ? C19 C14 C15 C11 179.6(8) . . . . ? Ir1 C14 C15 C11 60.5(5) . . . . ? C13 C14 C15 C20 174.0(8) . . . . ? C19 C14 C15 C20 -3.0(13) . . . . ? Ir1 C14 C15 C20 -122.1(8) . . . . ? C13 C14 C15 Ir1 -63.9(6) . . . . ? C19 C14 C15 Ir1 119.2(8) . . . . ? C12 C11 C15 C14 4.5(9) . . . . ? C16 C11 C15 C14 171.4(9) . . . . ? Ir1 C11 C15 C14 -60.9(5) . . . . ? C12 C11 C15 C20 -172.8(8) . . . . ? C16 C11 C15 C20 -5.9(15) . . . . ? Ir1 C11 C15 C20 121.7(9) . . . . ? C12 C11 C15 Ir1 65.5(6) . . . . ? C16 C11 C15 Ir1 -127.7(10) . . . . ? C41 Ir1 C15 C14 -132.2(5) . . . . ? N31 Ir1 C15 C14 -52.4(6) . . . . ? N1 Ir1 C15 C14 120.9(6) . . . . ? C11 Ir1 C15 C14 117.5(8) . . . . ? C12 Ir1 C15 C14 78.6(6) . . . . ? C13 Ir1 C15 C14 37.3(5) . . . . ? C41 Ir1 C15 C11 110.3(6) . . . . ? N31 Ir1 C15 C11 -169.8(6) . . . . ? N1 Ir1 C15 C11 3.4(9) . . . . ? C14 Ir1 C15 C11 -117.5(8) . . . . ? C12 Ir1 C15 C11 -38.9(6) . . . . ? C13 Ir1 C15 C11 -80.2(7) . . . . ? C41 Ir1 C15 C20 -12.0(10) . . . . ? N31 Ir1 C15 C20 67.9(10) . . . . ? N1 Ir1 C15 C20 -118.8(10) . . . . ? C11 Ir1 C15 C20 -122.3(12) . . . . ? C14 Ir1 C15 C20 120.3(12) . . . . ? C12 Ir1 C15 C20 -161.2(11) . . . . ? C13 Ir1 C15 C20 157.6(11) . . . . ? N51 Rh1 C21 C22 -78.9(6) . . . . ? N42 Rh1 C21 C22 34.1(16) . . . . ? N3 Rh1 C21 C22 -167.3(5) . . . . ? C23 Rh1 C21 C22 37.7(6) . . . . ? C24 Rh1 C21 C22 80.0(6) . . . . ? C25 Rh1 C21 C22 115.9(8) . . . . ? N51 Rh1 C21 C25 165.2(6) . . . . ? N42 Rh1 C21 C25 -81.7(15) . . . . ? N3 Rh1 C21 C25 76.8(6) . . . . ? C23 Rh1 C21 C25 -78.2(6) . . . . ? C22 Rh1 C21 C25 -115.9(8) . . . . ? C24 Rh1 C21 C25 -35.8(6) . . . . ? N51 Rh1 C21 C30 43.2(11) . . . . ? N42 Rh1 C21 C30 156.3(12) . . . . ? N3 Rh1 C21 C30 -45.2(11) . . . . ? C23 Rh1 C21 C30 159.8(12) . . . . ? C22 Rh1 C21 C30 122.1(13) . . . . ? C24 Rh1 C21 C30 -157.9(12) . . . . ? C25 Rh1 C21 C30 -122.0(13) . . . . ? C25 C21 C22 C23 1.7(9) . . . . ? C30 C21 C22 C23 176.7(9) . . . . ? Rh1 C21 C22 C23 -61.1(6) . . . . ? C25 C21 C22 C26 -175.0(9) . . . . ? C30 C21 C22 C26 0.1(15) . . . . ? Rh1 C21 C22 C26 122.3(9) . . . . ? C25 C21 C22 Rh1 62.8(5) . . . . ? C30 C21 C22 Rh1 -122.2(10) . . . . ? N51 Rh1 C22 C23 -132.5(6) . . . . ? N42 Rh1 C22 C23 -52.1(7) . . . . ? N3 Rh1 C22 C23 138.5(6) . . . . ? C24 Rh1 C22 C23 36.7(6) . . . . ? C21 Rh1 C22 C23 117.6(8) . . . . ? C25 Rh1 C22 C23 78.7(6) . . . . ? N51 Rh1 C22 C21 110.0(6) . . . . ? N42 Rh1 C22 C21 -169.7(5) . . . . ? N3 Rh1 C22 C21 21.0(8) . . . . ? C23 Rh1 C22 C21 -117.6(8) . . . . ? C24 Rh1 C22 C21 -80.9(6) . . . . ? C25 Rh1 C22 C21 -38.8(6) . . . . ? N51 Rh1 C22 C26 -10.4(10) . . . . ? N42 Rh1 C22 C26 69.9(11) . . . . ? N3 Rh1 C22 C26 -99.4(10) . . . . ? C23 Rh1 C22 C26 122.1(12) . . . . ? C24 Rh1 C22 C26 158.7(11) . . . . ? C21 Rh1 C22 C26 -120.4(12) . . . . ? C25 Rh1 C22 C26 -159.2(11) . . . . ? C21 C22 C23 C24 0.1(9) . . . . ? C26 C22 C23 C24 176.6(9) . . . . ? Rh1 C22 C23 C24 -61.5(6) . . . . ? C21 C22 C23 C27 -177.0(9) . . . . ? C26 C22 C23 C27 -0.5(15) . . . . ? Rh1 C22 C23 C27 121.4(10) . . . . ? C21 C22 C23 Rh1 61.6(6) . . . . ? C26 C22 C23 Rh1 -121.8(10) . . . . ? N51 Rh1 C23 C24 177.8(6) . . . . ? N42 Rh1 C23 C24 -100.0(6) . . . . ? N3 Rh1 C23 C24 6.7(11) . . . . ? C22 Rh1 C23 C24 119.1(9) . . . . ? C21 Rh1 C23 C24 80.9(6) . . . . ? C25 Rh1 C23 C24 37.4(6) . . . . ? N51 Rh1 C23 C22 58.8(7) . . . . ? N42 Rh1 C23 C22 141.0(5) . . . . ? N3 Rh1 C23 C22 -112.3(8) . . . . ? C24 Rh1 C23 C22 -119.1(9) . . . . ? C21 Rh1 C23 C22 -38.1(6) . . . . ? C25 Rh1 C23 C22 -81.6(6) . . . . ? N51 Rh1 C23 C27 -60.3(11) . . . . ? N42 Rh1 C23 C27 21.9(10) . . . . ? N3 Rh1 C23 C27 128.6(10) . . . . ? C22 Rh1 C23 C27 -119.0(12) . . . . ? C24 Rh1 C23 C27 121.9(12) . . . . ? C21 Rh1 C23 C27 -157.2(11) . . . . ? C25 Rh1 C23 C27 159.4(11) . . . . ? C22 C23 C24 C25 -1.9(9) . . . . ? C27 C23 C24 C25 175.2(9) . . . . ? Rh1 C23 C24 C25 -63.1(6) . . . . ? C22 C23 C24 C28 -173.6(8) . . . . ? C27 C23 C24 C28 3.5(15) . . . . ? Rh1 C23 C24 C28 125.2(9) . . . . ? C22 C23 C24 Rh1 61.3(6) . . . . ? C27 C23 C24 Rh1 -121.7(10) . . . . ? N51 Rh1 C24 C23 -5.2(14) . . . . ? N42 Rh1 C24 C23 88.8(6) . . . . ? N3 Rh1 C24 C23 -176.8(5) . . . . ? C22 Rh1 C24 C23 -37.1(6) . . . . ? C21 Rh1 C24 C23 -80.5(7) . . . . ? C25 Rh1 C24 C23 -117.5(8) . . . . ? N51 Rh1 C24 C25 112.2(11) . . . . ? N42 Rh1 C24 C25 -153.8(5) . . . . ? N3 Rh1 C24 C25 -59.4(6) . . . . ? C23 Rh1 C24 C25 117.5(8) . . . . ? C22 Rh1 C24 C25 80.3(6) . . . . ? C21 Rh1 C24 C25 36.9(6) . . . . ? N51 Rh1 C24 C28 -125.8(12) . . . . ? N42 Rh1 C24 C28 -31.8(11) . . . . ? N3 Rh1 C24 C28 62.6(12) . . . . ? C23 Rh1 C24 C28 -120.6(13) . . . . ? C22 Rh1 C24 C28 -157.7(12) . . . . ? C21 Rh1 C24 C28 158.9(12) . . . . ? C25 Rh1 C24 C28 122.0(13) . . . . ? C23 C24 C25 C21 2.9(9) . . . . ? C28 C24 C25 C21 174.6(8) . . . . ? Rh1 C24 C25 C21 -58.7(5) . . . . ? C23 C24 C25 C29 -176.5(8) . . . . ? C28 C24 C25 C29 -4.8(14) . . . . ? Rh1 C24 C25 C29 121.9(9) . . . . ? C23 C24 C25 Rh1 61.6(6) . . . . ? C28 C24 C25 Rh1 -126.7(9) . . . . ? C22 C21 C25 C24 -2.8(9) . . . . ? C30 C21 C25 C24 -177.9(9) . . . . ? Rh1 C21 C25 C24 58.8(6) . . . . ? C22 C21 C25 C29 176.6(8) . . . . ? C30 C21 C25 C29 1.5(14) . . . . ? Rh1 C21 C25 C29 -121.8(8) . . . . ? C22 C21 C25 Rh1 -61.6(5) . . . . ? C30 C21 C25 Rh1 123.3(10) . . . . ? N51 Rh1 C25 C24 -145.1(6) . . . . ? N42 Rh1 C25 C24 38.7(7) . . . . ? N3 Rh1 C25 C24 129.7(5) . . . . ? C23 Rh1 C25 C24 -37.8(6) . . . . ? C22 Rh1 C25 C24 -81.0(6) . . . . ? C21 Rh1 C25 C24 -120.0(8) . . . . ? N51 Rh1 C25 C21 -25.1(9) . . . . ? N42 Rh1 C25 C21 158.7(6) . . . . ? N3 Rh1 C25 C21 -110.3(6) . . . . ? C23 Rh1 C25 C21 82.2(7) . . . . ? C22 Rh1 C25 C21 39.0(6) . . . . ? C24 Rh1 C25 C21 120.0(8) . . . . ? N51 Rh1 C25 C29 94.0(11) . . . . ? N42 Rh1 C25 C29 -82.2(11) . . . . ? N3 Rh1 C25 C29 8.8(11) . . . . ? C23 Rh1 C25 C29 -158.7(12) . . . . ? C22 Rh1 C25 C29 158.1(12) . . . . ? C24 Rh1 C25 C29 -120.9(12) . . . . ? C21 Rh1 C25 C29 119.1(13) . . . . ? C35 N31 C31 C32 0.4(12) . . . . ? Ir1 N31 C31 C32 -173.9(7) . . . . ? N31 C31 C32 C33 1.3(14) . . . . ? C31 C32 C33 C34 -2.2(15) . . . . ? C32 C33 C34 C35 1.4(14) . . . . ? C31 N31 C35 C34 -1.3(11) . . . . ? Ir1 N31 C35 C34 173.5(6) . . . . ? C31 N31 C35 C36 177.1(7) . . . . ? Ir1 N31 C35 C36 -8.2(8) . . . . ? C33 C34 C35 N31 0.4(12) . . . . ? C33 C34 C35 C36 -177.7(8) . . . . ? N31 C35 C36 C41 0.0(9) . . . . ? C34 C35 C36 C41 178.3(8) . . . . ? N31 C35 C36 C37 178.3(7) . . . . ? C34 C35 C36 C37 -3.4(12) . . . . ? C41 C36 C37 C38 -2.1(12) . . . . ? C35 C36 C37 C38 179.7(8) . . . . ? C36 C37 C38 C39 -0.9(14) . . . . ? C37 C38 C39 C40 2.7(16) . . . . ? C38 C39 C40 C41 -1.6(15) . . . . ? C39 C40 C41 C36 -1.3(13) . . . . ? C39 C40 C41 Ir1 170.9(7) . . . . ? C37 C36 C41 C40 3.1(11) . . . . ? C35 C36 C41 C40 -178.6(7) . . . . ? C37 C36 C41 Ir1 -170.2(6) . . . . ? C35 C36 C41 Ir1 8.2(8) . . . . ? N31 Ir1 C41 C40 178.2(8) . . . . ? N1 Ir1 C41 C40 91.6(7) . . . . ? C11 Ir1 C41 C40 -21.8(8) . . . . ? C14 Ir1 C41 C40 -91.0(8) . . . . ? C15 Ir1 C41 C40 -59.3(8) . . . . ? C12 Ir1 C41 C40 -7.7(10) . . . . ? C13 Ir1 C41 C40 -84.8(12) . . . . ? N31 Ir1 C41 C36 -9.5(5) . . . . ? N1 Ir1 C41 C36 -96.0(5) . . . . ? C11 Ir1 C41 C36 150.5(6) . . . . ? C14 Ir1 C41 C36 81.3(6) . . . . ? C15 Ir1 C41 C36 113.0(6) . . . . ? C12 Ir1 C41 C36 164.6(6) . . . . ? C13 Ir1 C41 C36 87.5(10) . . . . ? C46 N42 C42 C43 1.4(13) . . . . ? Rh1 N42 C42 C43 178.5(7) . . . . ? N42 C42 C43 C44 0.2(16) . . . . ? C42 C43 C44 C45 0.4(18) . . . . ? C43 C44 C45 C46 -2.7(17) . . . . ? C42 N42 C46 C45 -3.6(12) . . . . ? Rh1 N42 C46 C45 179.0(7) . . . . ? C42 N42 C46 C47 173.3(7) . . . . ? Rh1 N42 C46 C47 -4.0(9) . . . . ? C44 C45 C46 N42 4.3(15) . . . . ? C44 C45 C46 C47 -172.2(10) . . . . ? C51 N51 C47 C48 6.3(13) . . . . ? Rh1 N51 C47 C48 177.1(7) . . . . ? C51 N51 C47 C46 -170.5(8) . . . . ? Rh1 N51 C47 C46 0.3(9) . . . . ? N42 C46 C47 N51 2.5(11) . . . . ? C45 C46 C47 N51 179.2(9) . . . . ? N42 C46 C47 C48 -174.3(8) . . . . ? C45 C46 C47 C48 2.4(14) . . . . ? N51 C47 C48 C49 -2.9(13) . . . . ? C46 C47 C48 C49 173.7(8) . . . . ? C47 C48 C49 C50 -1.0(15) . . . . ? C48 C49 C50 C51 1.6(17) . . . . ? C47 N51 C51 C50 -5.7(15) . . . . ? Rh1 N51 C51 C50 -175.8(8) . . . . ? C49 C50 C51 N51 1.8(17) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.895 _refine_diff_density_min -1.771 _refine_diff_density_rms 0.181 _database_code_depnum_ccdc_archive 'CCDC 945556' ####################################################################### # # 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_comp12b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H49 N6 Rh2 1+, B F4 1-, 0.5(C2 H3 N), 0.25(H2 O)' _chemical_formula_sum 'C45 H51 B F4 Ir N6.50 O0.25 Rh' _chemical_formula_weight 1068.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6443(9) _cell_length_b 14.1518(8) _cell_length_c 14.4628(8) _cell_angle_alpha 99.082(2) _cell_angle_beta 111.484(3) _cell_angle_gamma 96.501(4) _cell_volume 2151.6(2) _cell_formula_units_Z 2 _cell_measurement_temperature 192(2) _cell_measurement_reflns_used 17236 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.57 _exptl_crystal_description platelet _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1063 _exptl_absorpt_coefficient_mu 3.531 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3324 _exptl_absorpt_correction_T_max 0.7191 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 192(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21169 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 9779 _reflns_number_gt 8380 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0489P)^2^+9.5763P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9779 _refine_ls_number_parameters 515 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0555 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1241 _refine_ls_wR_factor_gt 0.1179 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir -0.16468(2) 0.303678(17) 0.242260(17) 0.03225(9) Uani 1 1 d . . . Rh1 Rh 0.17173(4) 0.01309(3) 0.26677(3) 0.02307(10) Uani 1 1 d . . . F1 F 0.6267(11) 0.4191(8) 0.6042(8) 0.078(3) Uiso 0.50 1 d PD . . F2 F 0.7774(11) 0.3970(8) 0.7228(9) 0.124(3) Uiso 0.75 1 d PD . . F3 F 0.6087(6) 0.3185(5) 0.7179(5) 0.0840(16) Uiso 1 1 d D . . F4 F 0.6457(11) 0.4739(8) 0.7857(8) 0.119(3) Uiso 0.75 1 d PD . . F5 F 0.5431(12) 0.4235(10) 0.6313(10) 0.094(4) Uiso 0.50 1 d PD . . F6 F 0.7253(15) 0.4866(10) 0.7670(11) 0.116(5) Uiso 0.50 1 d PD . . O1 O -0.5000 -0.5000 0.0000 0.132(10) Uiso 0.50 2 d SP . . N1 N -0.1234(5) 0.1651(3) 0.2136(3) 0.0280(10) Uani 1 1 d . . . N2 N -0.0033(4) 0.1594(3) 0.2316(4) 0.0277(10) Uani 1 1 d . . . N3 N 0.0041(5) 0.0678(4) 0.2282(4) 0.0295(10) Uani 1 1 d . . . N4 N -0.1069(5) 0.0121(4) 0.2079(4) 0.0352(11) Uani 1 1 d . . . N5 N -0.7627(19) -0.5899(15) -0.0811(15) 0.097(6) Uiso 0.50 1 d PD . . N31 N -0.1043(5) 0.3320(4) 0.1280(4) 0.0342(11) Uani 1 1 d . . . N42 N 0.2658(5) 0.1546(4) 0.2908(4) 0.0390(12) Uani 1 1 d . . . C1 C -0.557(3) -0.510(2) 0.070(2) 0.139(12) Uiso 0.50 1 d PD . . C2 C -0.6771(18) -0.5533(15) -0.0238(15) 0.071(5) Uiso 0.50 1 d PD . . C5 C -0.1847(6) 0.0752(4) 0.2001(4) 0.0310(12) Uani 1 1 d . . . C6 C -0.3192(7) 0.0451(5) 0.1797(6) 0.0478(17) Uani 1 1 d . . . H6A H -0.3327 -0.0192 0.1952 0.057 Uiso 1 1 calc R . . H6B H -0.3700 0.0420 0.1079 0.057 Uiso 1 1 calc R . . H6C H -0.3438 0.0926 0.2226 0.057 Uiso 1 1 calc R . . C11 C -0.2169(6) 0.3247(5) 0.3734(4) 0.0346(13) Uani 1 1 d . . . C12 C -0.2211(6) 0.4110(4) 0.3320(5) 0.0350(14) Uani 1 1 d . . . C13 C -0.0982(7) 0.4487(5) 0.3415(5) 0.0374(14) Uani 1 1 d . . . C14 C -0.0140(6) 0.3870(5) 0.3904(4) 0.0352(14) Uani 1 1 d . . . C15 C -0.0876(6) 0.3118(5) 0.4089(4) 0.0348(14) Uani 1 1 d . . . C16 C -0.3192(7) 0.2691(6) 0.3931(5) 0.0462(17) Uani 1 1 d . . . H16A H -0.3056 0.2021 0.3946 0.055 Uiso 1 1 calc R . . H16B H -0.4004 0.2682 0.3389 0.055 Uiso 1 1 calc R . . H16C H -0.3187 0.3003 0.4588 0.055 Uiso 1 1 calc R . . C17 C -0.3344(7) 0.4576(5) 0.2954(6) 0.0483(18) Uani 1 1 d . . . H17A H -0.4081 0.4073 0.2525 0.058 Uiso 1 1 calc R . . H17B H -0.3207 0.5046 0.2558 0.058 Uiso 1 1 calc R . . H17C H -0.3482 0.4912 0.3540 0.058 Uiso 1 1 calc R . . C18 C -0.0579(8) 0.5402(5) 0.3132(6) 0.0539(19) Uani 1 1 d . . . H18A H 0.0172 0.5353 0.2985 0.065 Uiso 1 1 calc R . . H18B H -0.0389 0.5958 0.3697 0.065 Uiso 1 1 calc R . . H18C H -0.1257 0.5496 0.2527 0.065 Uiso 1 1 calc R . . C19 C 0.1262(7) 0.4050(6) 0.4248(6) 0.054(2) Uani 1 1 d . . . H19A H 0.1520 0.4538 0.3916 0.065 Uiso 1 1 calc R . . H19B H 0.1531 0.3441 0.4066 0.065 Uiso 1 1 calc R . . H19C H 0.1650 0.4289 0.4988 0.065 Uiso 1 1 calc R . . C20 C -0.0396(7) 0.2299(5) 0.4578(5) 0.0441(16) Uani 1 1 d . . . H20A H -0.1057 0.1716 0.4298 0.053 Uiso 1 1 calc R . . H20B H -0.0157 0.2489 0.5314 0.053 Uiso 1 1 calc R . . H20C H 0.0337 0.2160 0.4438 0.053 Uiso 1 1 calc R . . C21 C 0.2395(8) -0.1207(5) 0.2964(5) 0.0445(17) Uani 1 1 d . . . C22 C 0.3106(7) -0.0695(5) 0.2520(5) 0.0429(16) Uani 1 1 d . . . C23 C 0.2298(7) -0.0686(5) 0.1493(5) 0.0397(15) Uani 1 1 d . . . C24 C 0.1079(7) -0.1131(4) 0.1332(5) 0.0384(15) Uani 1 1 d . . . C25 C 0.1113(7) -0.1437(4) 0.2261(5) 0.0409(15) Uani 1 1 d . . . C26 C 0.2905(10) -0.1481(7) 0.3979(6) 0.068(3) Uani 1 1 d . . . H26A H 0.2227 -0.1601 0.4218 0.082 Uiso 1 1 calc R . . H26B H 0.3564 -0.0949 0.4469 0.082 Uiso 1 1 calc R . . H26C H 0.3258 -0.2073 0.3912 0.082 Uiso 1 1 calc R . . C27 C 0.4508(8) -0.0336(7) 0.3001(8) 0.071(3) Uani 1 1 d . . . H27A H 0.4720 0.0242 0.2759 0.085 Uiso 1 1 calc R . . H27B H 0.4933 -0.0849 0.2814 0.085 Uiso 1 1 calc R . . H27C H 0.4783 -0.0169 0.3743 0.085 Uiso 1 1 calc R . . C28 C 0.2709(9) -0.0326(6) 0.0728(7) 0.059(2) Uani 1 1 d . . . H28A H 0.3332 0.0278 0.1058 0.071 Uiso 1 1 calc R . . H28B H 0.1982 -0.0200 0.0182 0.071 Uiso 1 1 calc R . . H28C H 0.3085 -0.0819 0.0441 0.071 Uiso 1 1 calc R . . C29 C -0.0087(8) -0.1288(5) 0.0385(6) 0.054(2) Uani 1 1 d . . . H29A H -0.0803 -0.1197 0.0570 0.064 Uiso 1 1 calc R . . H29B H -0.0239 -0.1951 -0.0012 0.064 Uiso 1 1 calc R . . H29C H 0.0017 -0.0819 -0.0022 0.064 Uiso 1 1 calc R . . C30 C 0.0041(9) -0.2005(6) 0.2382(7) 0.061(2) Uani 1 1 d . . . H30A H -0.0749 -0.1951 0.1849 0.073 Uiso 1 1 calc R . . H30B H 0.0039 -0.1747 0.3052 0.073 Uiso 1 1 calc R . . H30C H 0.0126 -0.2690 0.2326 0.073 Uiso 1 1 calc R . . C31 C 0.0147(7) 0.3670(5) 0.1454(5) 0.0398(15) Uani 1 1 d . . . H31 H 0.0770 0.3754 0.2121 0.048 Uiso 1 1 calc R . . C32 C 0.0507(8) 0.3917(5) 0.0698(6) 0.0450(16) Uani 1 1 d . . . H32 H 0.1357 0.4185 0.0848 0.054 Uiso 1 1 calc R . . C33 C -0.0388(9) 0.3766(5) -0.0275(6) 0.052(2) Uani 1 1 d . . . H33 H -0.0159 0.3929 -0.0805 0.062 Uiso 1 1 calc R . . C34 C -0.1618(8) 0.3379(5) -0.0480(5) 0.0465(17) Uani 1 1 d . . . H34 H -0.2239 0.3263 -0.1152 0.056 Uiso 1 1 calc R . . C35 C -0.1944(7) 0.3158(4) 0.0318(4) 0.0362(14) Uani 1 1 d . . . C36 C -0.3204(7) 0.2797(5) 0.0230(5) 0.0392(15) Uani 1 1 d . . . C37 C -0.4276(8) 0.2592(5) -0.0684(5) 0.0515(19) Uani 1 1 d . . . H37 H -0.4194 0.2678 -0.1297 0.062 Uiso 1 1 calc R . . C38 C -0.5433(8) 0.2272(6) -0.0697(6) 0.060(2) Uani 1 1 d . . . H38 H -0.6156 0.2135 -0.1315 0.072 Uiso 1 1 calc R . . C39 C -0.5544(7) 0.2148(6) 0.0196(6) 0.0523(19) Uani 1 1 d . . . H39 H -0.6347 0.1924 0.0192 0.063 Uiso 1 1 calc R . . C40 C -0.4489(7) 0.2350(5) 0.1100(5) 0.0455(16) Uani 1 1 d . . . H40 H -0.4589 0.2265 0.1707 0.055 Uiso 1 1 calc R . . C41 C -0.3298(6) 0.2669(4) 0.1146(5) 0.0356(14) Uani 1 1 d . . . C42 C 0.2749(6) 0.1961(5) 0.2149(6) 0.0451(16) Uani 1 1 d . . . H42 H 0.2404 0.1595 0.1467 0.054 Uiso 1 1 calc R . . C43 C 0.3349(7) 0.2924(5) 0.2370(8) 0.058(2) Uani 1 1 d . . . H43 H 0.3405 0.3215 0.1836 0.070 Uiso 1 1 calc R . . C44 C 0.3858(7) 0.3455(6) 0.3346(8) 0.063(2) Uani 1 1 d . . . H44 H 0.4275 0.4111 0.3495 0.075 Uiso 1 1 calc R . . C45 C 0.3760(7) 0.3030(6) 0.4109(8) 0.061(2) Uani 1 1 d . . . H45 H 0.4127 0.3389 0.4793 0.073 Uiso 1 1 calc R . . C46 C 0.3124(6) 0.2073(5) 0.3884(6) 0.0420(16) Uani 1 1 d . . . C47 C 0.2794(7) 0.1591(6) 0.4595(5) 0.0473(18) Uani 1 1 d . . . C48 C 0.3100(7) 0.2004(7) 0.5613(6) 0.059(2) Uani 1 1 d . . . H48 H 0.3656 0.2614 0.5915 0.071 Uiso 1 1 calc R . . C49 C 0.2605(9) 0.1536(8) 0.6188(6) 0.069(3) Uani 1 1 d . . . H49 H 0.2809 0.1830 0.6879 0.082 Uiso 1 1 calc R . . C50 C 0.1823(9) 0.0652(8) 0.5765(6) 0.065(3) Uani 1 1 d . . . H50 H 0.1482 0.0333 0.6164 0.078 Uiso 1 1 calc R . . C51 C 0.1516(8) 0.0209(6) 0.4741(5) 0.0489(18) Uani 1 1 d . . . H51 H 0.0968 -0.0406 0.4452 0.059 Uiso 1 1 calc R . . C52 C 0.2013(6) 0.0669(5) 0.4151(5) 0.0369(14) Uani 1 1 d . . . B1 B 0.6531(11) 0.4061(6) 0.7029(6) 0.120(7) Uani 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 0.03798(15) 0.02939(13) 0.02579(13) 0.00396(9) 0.00776(10) 0.01137(10) Rh1 0.0294(2) 0.0191(2) 0.01914(19) 0.00352(16) 0.00665(17) 0.00942(16) N1 0.035(3) 0.023(2) 0.023(2) 0.0021(19) 0.008(2) 0.008(2) N2 0.029(3) 0.024(2) 0.026(2) 0.0050(19) 0.007(2) 0.0092(19) N3 0.034(3) 0.028(2) 0.026(2) 0.006(2) 0.010(2) 0.009(2) N4 0.038(3) 0.027(2) 0.040(3) 0.005(2) 0.015(2) 0.006(2) N31 0.049(3) 0.024(2) 0.028(2) 0.007(2) 0.013(2) 0.010(2) N42 0.033(3) 0.033(3) 0.047(3) 0.006(2) 0.011(2) 0.010(2) C5 0.038(3) 0.026(3) 0.028(3) 0.003(2) 0.013(3) 0.007(2) C6 0.044(4) 0.032(3) 0.068(5) 0.008(3) 0.024(4) 0.004(3) C11 0.041(3) 0.042(3) 0.021(3) 0.004(3) 0.011(2) 0.016(3) C12 0.042(4) 0.027(3) 0.027(3) -0.004(2) 0.007(3) 0.011(3) C13 0.051(4) 0.030(3) 0.028(3) -0.002(2) 0.014(3) 0.011(3) C14 0.035(3) 0.038(3) 0.026(3) -0.005(3) 0.008(2) 0.012(3) C15 0.039(3) 0.043(3) 0.019(3) 0.001(2) 0.008(2) 0.018(3) C16 0.047(4) 0.057(4) 0.036(3) 0.012(3) 0.017(3) 0.016(3) C17 0.047(4) 0.044(4) 0.051(4) 0.008(3) 0.012(3) 0.023(3) C18 0.069(5) 0.029(3) 0.058(5) -0.004(3) 0.026(4) 0.002(3) C19 0.038(4) 0.071(5) 0.039(4) -0.007(4) 0.009(3) 0.006(4) C20 0.056(4) 0.050(4) 0.027(3) 0.014(3) 0.011(3) 0.025(3) C21 0.074(5) 0.033(3) 0.036(3) 0.013(3) 0.023(3) 0.031(3) C22 0.047(4) 0.038(3) 0.045(4) 0.005(3) 0.016(3) 0.024(3) C23 0.061(4) 0.029(3) 0.037(3) 0.007(3) 0.023(3) 0.023(3) C24 0.054(4) 0.026(3) 0.033(3) 0.001(3) 0.013(3) 0.019(3) C25 0.059(4) 0.021(3) 0.048(4) 0.005(3) 0.026(3) 0.012(3) C26 0.102(7) 0.067(6) 0.042(4) 0.024(4) 0.020(4) 0.052(5) C27 0.056(5) 0.074(6) 0.080(6) 0.006(5) 0.023(5) 0.030(5) C28 0.092(7) 0.049(4) 0.065(5) 0.020(4) 0.053(5) 0.036(4) C29 0.061(5) 0.039(4) 0.043(4) -0.001(3) 0.002(3) 0.018(3) C30 0.080(6) 0.039(4) 0.073(6) 0.011(4) 0.042(5) 0.006(4) C31 0.058(4) 0.031(3) 0.033(3) 0.005(3) 0.021(3) 0.012(3) C32 0.062(5) 0.030(3) 0.050(4) 0.009(3) 0.030(4) 0.009(3) C33 0.095(6) 0.030(3) 0.044(4) 0.012(3) 0.039(4) 0.017(4) C34 0.075(5) 0.033(3) 0.033(3) 0.008(3) 0.019(3) 0.018(3) C35 0.058(4) 0.026(3) 0.024(3) 0.006(2) 0.013(3) 0.018(3) C36 0.054(4) 0.027(3) 0.028(3) 0.004(3) 0.006(3) 0.015(3) C37 0.073(6) 0.040(4) 0.027(3) 0.006(3) 0.003(3) 0.013(4) C38 0.056(5) 0.053(5) 0.042(4) 0.007(4) -0.010(4) 0.007(4) C39 0.045(4) 0.046(4) 0.045(4) 0.003(3) -0.004(3) 0.004(3) C40 0.047(4) 0.039(4) 0.041(4) 0.008(3) 0.006(3) 0.013(3) C41 0.043(4) 0.027(3) 0.028(3) 0.003(2) 0.002(3) 0.015(3) C42 0.032(4) 0.038(4) 0.066(5) 0.017(3) 0.017(3) 0.011(3) C43 0.040(4) 0.038(4) 0.105(7) 0.025(5) 0.033(5) 0.012(3) C44 0.039(4) 0.035(4) 0.112(8) 0.002(5) 0.034(5) 0.003(3) C45 0.031(4) 0.047(4) 0.086(6) -0.018(4) 0.014(4) 0.006(3) C46 0.025(3) 0.034(3) 0.056(4) -0.003(3) 0.008(3) 0.008(3) C47 0.035(4) 0.053(4) 0.037(3) -0.006(3) -0.002(3) 0.018(3) C48 0.044(4) 0.069(5) 0.040(4) -0.012(4) -0.004(3) 0.023(4) C49 0.074(6) 0.094(7) 0.025(3) 0.001(4) 0.002(4) 0.045(6) C50 0.085(7) 0.095(7) 0.033(4) 0.028(4) 0.026(4) 0.055(6) C51 0.059(5) 0.060(5) 0.034(3) 0.012(3) 0.018(3) 0.031(4) C52 0.038(3) 0.043(4) 0.030(3) 0.007(3) 0.009(3) 0.022(3) B1 0.203(18) 0.051(6) 0.041(6) -0.010(5) -0.029(8) 0.059(9) _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 C41 2.061(6) . ? Ir1 N1 2.086(4) . ? Ir1 N31 2.094(5) . ? Ir1 C12 2.157(6) . ? Ir1 C11 2.183(6) . ? Ir1 C13 2.184(6) . ? Ir1 C15 2.220(6) . ? Ir1 C14 2.245(6) . ? Rh1 C52 2.046(6) . ? Rh1 N42 2.082(6) . ? Rh1 N3 2.098(5) . ? Rh1 C22 2.152(6) . ? Rh1 C25 2.166(6) . ? Rh1 C21 2.176(6) . ? Rh1 C24 2.243(6) . ? Rh1 C23 2.254(6) . ? F1 B1 1.394(11) . ? F2 B1 1.394(11) . ? F3 B1 1.369(10) . ? F4 B1 1.446(11) . ? F5 B1 1.398(12) . ? F6 B1 1.320(12) . ? O1 C1 1.42(4) . ? N1 C5 1.335(7) . ? N1 N2 1.340(7) . ? N2 N3 1.302(6) . ? N3 N4 1.341(7) . ? N4 C5 1.332(8) . ? N5 C2 1.045(15) . ? N31 C31 1.334(9) . ? N31 C35 1.365(8) . ? N42 C42 1.356(9) . ? N42 C46 1.362(9) . ? C1 C2 1.523(17) . ? C5 C6 1.480(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C11 C12 1.440(9) . ? C11 C15 1.445(9) . ? C11 C16 1.492(10) . ? C12 C13 1.418(10) . ? C12 C17 1.500(9) . ? C13 C14 1.452(9) . ? C13 C18 1.495(10) . ? C14 C15 1.411(10) . ? C14 C19 1.498(9) . ? C15 C20 1.507(9) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.422(11) . ? C21 C25 1.429(11) . ? C21 C26 1.501(10) . ? C22 C23 1.441(9) . ? C22 C27 1.508(11) . ? C23 C24 1.404(10) . ? C23 C28 1.492(10) . ? C24 C25 1.464(9) . ? C24 C29 1.497(10) . ? C25 C30 1.488(11) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.385(9) . ? C31 H31 0.9500 . ? C32 C33 1.376(11) . ? C32 H32 0.9500 . ? C33 C34 1.378(12) . ? C33 H33 0.9500 . ? C34 C35 1.407(9) . ? C34 H34 0.9500 . ? C35 C36 1.450(10) . ? C36 C41 1.406(9) . ? C36 C37 1.407(9) . ? C37 C38 1.365(12) . ? C37 H37 0.9500 . ? C38 C39 1.380(12) . ? C38 H38 0.9500 . ? C39 C40 1.388(10) . ? C39 H39 0.9500 . ? C40 C41 1.384(10) . ? C40 H40 0.9500 . ? C42 C43 1.389(10) . ? C42 H42 0.9500 . ? C43 C44 1.364(13) . ? C43 H43 0.9500 . ? C44 C45 1.370(13) . ? C44 H44 0.9500 . ? C45 C46 1.396(11) . ? C45 H45 0.9500 . ? C46 C47 1.457(11) . ? C47 C48 1.389(10) . ? C47 C52 1.408(10) . ? C48 C49 1.379(14) . ? C48 H48 0.9500 . ? C49 C50 1.365(14) . ? C49 H49 0.9500 . ? C50 C51 1.408(10) . ? C50 H50 0.9500 . ? C51 C52 1.392(10) . ? C51 H51 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 C41 Ir1 N1 91.4(2) . . ? C41 Ir1 N31 77.8(2) . . ? N1 Ir1 N31 86.28(19) . . ? C41 Ir1 C12 97.9(2) . . ? N1 Ir1 C12 149.8(2) . . ? N31 Ir1 C12 123.7(2) . . ? C41 Ir1 C11 106.7(3) . . ? N1 Ir1 C11 111.0(2) . . ? N31 Ir1 C11 161.7(2) . . ? C12 Ir1 C11 38.8(2) . . ? C41 Ir1 C13 123.2(2) . . ? N1 Ir1 C13 145.3(2) . . ? N31 Ir1 C13 98.3(2) . . ? C12 Ir1 C13 38.1(2) . . ? C11 Ir1 C13 64.2(3) . . ? C41 Ir1 C15 142.3(3) . . ? N1 Ir1 C15 91.7(2) . . ? N31 Ir1 C15 139.9(2) . . ? C12 Ir1 C15 63.7(2) . . ? C11 Ir1 C15 38.3(2) . . ? C13 Ir1 C15 62.9(2) . . ? C41 Ir1 C14 160.8(2) . . ? N1 Ir1 C14 107.4(2) . . ? N31 Ir1 C14 106.4(2) . . ? C12 Ir1 C14 63.9(2) . . ? C11 Ir1 C14 63.7(2) . . ? C13 Ir1 C14 38.2(2) . . ? C15 Ir1 C14 36.8(2) . . ? C52 Rh1 N42 78.5(3) . . ? C52 Rh1 N3 86.4(2) . . ? N42 Rh1 N3 87.7(2) . . ? C52 Rh1 C22 112.8(3) . . ? N42 Rh1 C22 101.0(3) . . ? N3 Rh1 C22 160.0(2) . . ? C52 Rh1 C25 111.1(3) . . ? N42 Rh1 C25 164.6(2) . . ? N3 Rh1 C25 104.5(2) . . ? C22 Rh1 C25 64.5(3) . . ? C52 Rh1 C21 94.3(2) . . ? N42 Rh1 C21 131.9(3) . . ? N3 Rh1 C21 139.8(3) . . ? C22 Rh1 C21 38.4(3) . . ? C25 Rh1 C21 38.4(3) . . ? C52 Rh1 C24 149.7(3) . . ? N42 Rh1 C24 131.5(2) . . ? N3 Rh1 C24 97.8(2) . . ? C22 Rh1 C24 62.9(3) . . ? C25 Rh1 C24 38.7(2) . . ? C21 Rh1 C24 63.4(2) . . ? C52 Rh1 C23 150.9(2) . . ? N42 Rh1 C23 102.1(2) . . ? N3 Rh1 C23 122.7(2) . . ? C22 Rh1 C23 38.1(2) . . ? C25 Rh1 C23 63.6(3) . . ? C21 Rh1 C23 63.4(2) . . ? C24 Rh1 C23 36.4(3) . . ? C5 N1 N2 107.3(5) . . ? C5 N1 Ir1 133.8(4) . . ? N2 N1 Ir1 117.3(4) . . ? N3 N2 N1 106.3(5) . . ? N2 N3 N4 112.3(5) . . ? N2 N3 Rh1 124.9(4) . . ? N4 N3 Rh1 122.4(4) . . ? C5 N4 N3 103.8(5) . . ? C31 N31 C35 119.7(6) . . ? C31 N31 Ir1 123.5(4) . . ? C35 N31 Ir1 116.7(5) . . ? C42 N42 C46 120.5(6) . . ? C42 N42 Rh1 123.4(5) . . ? C46 N42 Rh1 115.9(5) . . ? O1 C1 C2 85.4(17) . . ? N5 C2 C1 171(3) . . ? N4 C5 N1 110.3(5) . . ? N4 C5 C6 122.5(6) . . ? N1 C5 C6 127.2(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C12 C11 C15 106.4(6) . . ? C12 C11 C16 127.2(6) . . ? C15 C11 C16 125.6(6) . . ? C12 C11 Ir1 69.6(3) . . ? C15 C11 Ir1 72.3(3) . . ? C16 C11 Ir1 130.8(5) . . ? C13 C12 C11 108.4(5) . . ? C13 C12 C17 126.3(6) . . ? C11 C12 C17 125.0(6) . . ? C13 C12 Ir1 72.0(3) . . ? C11 C12 Ir1 71.6(3) . . ? C17 C12 Ir1 127.0(4) . . ? C12 C13 C14 108.6(6) . . ? C12 C13 C18 126.7(6) . . ? C14 C13 C18 124.7(7) . . ? C12 C13 Ir1 69.9(3) . . ? C14 C13 Ir1 73.2(3) . . ? C18 C13 Ir1 126.0(5) . . ? C15 C14 C13 106.8(6) . . ? C15 C14 C19 126.2(6) . . ? C13 C14 C19 126.7(7) . . ? C15 C14 Ir1 70.6(3) . . ? C13 C14 Ir1 68.6(3) . . ? C19 C14 Ir1 130.5(4) . . ? C14 C15 C11 109.7(6) . . ? C14 C15 C20 125.4(6) . . ? C11 C15 C20 124.8(6) . . ? C14 C15 Ir1 72.5(3) . . ? C11 C15 Ir1 69.4(3) . . ? C20 C15 Ir1 124.3(4) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 107.9(6) . . ? C22 C21 C26 126.1(8) . . ? C25 C21 C26 126.0(8) . . ? C22 C21 Rh1 69.9(4) . . ? C25 C21 Rh1 70.4(4) . . ? C26 C21 Rh1 126.5(5) . . ? C21 C22 C23 108.7(6) . . ? C21 C22 C27 125.1(7) . . ? C23 C22 C27 125.7(7) . . ? C21 C22 Rh1 71.7(4) . . ? C23 C22 Rh1 74.8(4) . . ? C27 C22 Rh1 125.4(5) . . ? C24 C23 C22 107.6(6) . . ? C24 C23 C28 126.7(7) . . ? C22 C23 C28 125.6(7) . . ? C24 C23 Rh1 71.4(3) . . ? C22 C23 Rh1 67.1(3) . . ? C28 C23 Rh1 129.6(5) . . ? C23 C24 C25 108.6(6) . . ? C23 C24 C29 127.6(7) . . ? C25 C24 C29 123.8(7) . . ? C23 C24 Rh1 72.2(4) . . ? C25 C24 Rh1 67.8(3) . . ? C29 C24 Rh1 125.9(4) . . ? C21 C25 C24 106.9(6) . . ? C21 C25 C30 126.9(7) . . ? C24 C25 C30 125.7(7) . . ? C21 C25 Rh1 71.2(4) . . ? C24 C25 Rh1 73.5(3) . . ? C30 C25 Rh1 127.1(5) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N31 C31 C32 122.3(7) . . ? N31 C31 H31 118.8 . . ? C32 C31 H31 118.8 . . ? C33 C32 C31 118.8(7) . . ? C33 C32 H32 120.6 . . ? C31 C32 H32 120.6 . . ? C32 C33 C34 119.8(7) . . ? C32 C33 H33 120.1 . . ? C34 C33 H33 120.1 . . ? C33 C34 C35 119.3(7) . . ? C33 C34 H34 120.3 . . ? C35 C34 H34 120.3 . . ? N31 C35 C34 119.9(7) . . ? N31 C35 C36 114.5(5) . . ? C34 C35 C36 125.5(6) . . ? C41 C36 C37 120.9(7) . . ? C41 C36 C35 114.9(6) . . ? C37 C36 C35 124.2(6) . . ? C38 C37 C36 120.5(7) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 119.4(7) . . ? C37 C38 H38 120.3 . . ? C39 C38 H38 120.3 . . ? C38 C39 C40 120.4(8) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 122.1(7) . . ? C41 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? C40 C41 C36 116.7(6) . . ? C40 C41 Ir1 127.2(5) . . ? C36 C41 Ir1 116.0(5) . . ? N42 C42 C43 119.7(8) . . ? N42 C42 H42 120.1 . . ? C43 C42 H42 120.1 . . ? C44 C43 C42 120.7(9) . . ? C44 C43 H43 119.6 . . ? C42 C43 H43 119.6 . . ? C43 C44 C45 119.1(8) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C44 C45 C46 120.2(8) . . ? C44 C45 H45 119.9 . . ? C46 C45 H45 119.9 . . ? N42 C46 C45 119.6(8) . . ? N42 C46 C47 114.8(6) . . ? C45 C46 C47 125.3(7) . . ? C48 C47 C52 120.2(8) . . ? C48 C47 C46 125.2(8) . . ? C52 C47 C46 114.4(6) . . ? C49 C48 C47 120.6(9) . . ? C49 C48 H48 119.7 . . ? C47 C48 H48 119.7 . . ? C50 C49 C48 120.1(7) . . ? C50 C49 H49 120.0 . . ? C48 C49 H49 120.0 . . ? C49 C50 C51 120.4(9) . . ? C49 C50 H50 119.8 . . ? C51 C50 H50 119.8 . . ? C52 C51 C50 120.2(8) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C47 118.5(6) . . ? C51 C52 Rh1 126.0(5) . . ? C47 C52 Rh1 115.5(5) . . ? F6 B1 F2 72.7(10) . . ? F6 B1 F1 108.3(11) . . ? F2 B1 F1 94.7(10) . . ? F6 B1 F3 132.0(10) . . ? F2 B1 F3 100.0(8) . . ? F1 B1 F3 119.6(8) . . ? F6 B1 F5 112.6(11) . . ? F2 B1 F5 144.7(11) . . ? F1 B1 F5 50.0(7) . . ? F3 B1 F5 100.2(10) . . ? F6 B1 F4 44.8(8) . . ? F2 B1 F4 110.6(9) . . ? F1 B1 F4 126.6(9) . . ? F3 B1 F4 101.8(9) . . ? F5 B1 F4 93.2(10) . . ? 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 C41 Ir1 N1 C5 -55.7(6) . . . . ? N31 Ir1 N1 C5 -133.4(6) . . . . ? C12 Ir1 N1 C5 52.8(7) . . . . ? C11 Ir1 N1 C5 52.8(6) . . . . ? C13 Ir1 N1 C5 127.4(6) . . . . ? C15 Ir1 N1 C5 86.7(6) . . . . ? C14 Ir1 N1 C5 120.6(5) . . . . ? C41 Ir1 N1 N2 140.9(4) . . . . ? N31 Ir1 N1 N2 63.2(4) . . . . ? C12 Ir1 N1 N2 -110.6(5) . . . . ? C11 Ir1 N1 N2 -110.6(4) . . . . ? C13 Ir1 N1 N2 -36.0(6) . . . . ? C15 Ir1 N1 N2 -76.7(4) . . . . ? C14 Ir1 N1 N2 -42.8(4) . . . . ? C5 N1 N2 N3 0.2(6) . . . . ? Ir1 N1 N2 N3 167.7(3) . . . . ? N1 N2 N3 N4 0.4(6) . . . . ? N1 N2 N3 Rh1 -172.6(3) . . . . ? C52 Rh1 N3 N2 75.6(5) . . . . ? N42 Rh1 N3 N2 -3.0(5) . . . . ? C22 Rh1 N3 N2 -119.6(8) . . . . ? C25 Rh1 N3 N2 -173.5(4) . . . . ? C21 Rh1 N3 N2 168.0(4) . . . . ? C24 Rh1 N3 N2 -134.5(5) . . . . ? C23 Rh1 N3 N2 -105.9(5) . . . . ? C52 Rh1 N3 N4 -96.7(5) . . . . ? N42 Rh1 N3 N4 -175.3(4) . . . . ? C22 Rh1 N3 N4 68.1(9) . . . . ? C25 Rh1 N3 N4 14.2(5) . . . . ? C21 Rh1 N3 N4 -4.3(6) . . . . ? C24 Rh1 N3 N4 53.1(5) . . . . ? C23 Rh1 N3 N4 81.8(5) . . . . ? N2 N3 N4 C5 -0.8(6) . . . . ? Rh1 N3 N4 C5 172.4(4) . . . . ? C41 Ir1 N31 C31 178.9(5) . . . . ? N1 Ir1 N31 C31 -88.9(5) . . . . ? C12 Ir1 N31 C31 87.4(5) . . . . ? C11 Ir1 N31 C31 72.5(9) . . . . ? C13 Ir1 N31 C31 56.5(5) . . . . ? C15 Ir1 N31 C31 -0.7(6) . . . . ? C14 Ir1 N31 C31 18.2(5) . . . . ? C41 Ir1 N31 C35 0.9(4) . . . . ? N1 Ir1 N31 C35 93.2(4) . . . . ? C12 Ir1 N31 C35 -90.6(5) . . . . ? C11 Ir1 N31 C35 -105.5(8) . . . . ? C13 Ir1 N31 C35 -121.4(4) . . . . ? C15 Ir1 N31 C35 -178.7(4) . . . . ? C14 Ir1 N31 C35 -159.8(4) . . . . ? C52 Rh1 N42 C42 -168.6(5) . . . . ? N3 Rh1 N42 C42 -81.8(5) . . . . ? C22 Rh1 N42 C42 80.1(5) . . . . ? C25 Rh1 N42 C42 61.2(11) . . . . ? C21 Rh1 N42 C42 106.1(5) . . . . ? C24 Rh1 N42 C42 16.6(6) . . . . ? C23 Rh1 N42 C42 41.2(5) . . . . ? C52 Rh1 N42 C46 7.5(4) . . . . ? N3 Rh1 N42 C46 94.3(4) . . . . ? C22 Rh1 N42 C46 -103.9(5) . . . . ? C25 Rh1 N42 C46 -122.8(9) . . . . ? C21 Rh1 N42 C46 -77.9(5) . . . . ? C24 Rh1 N42 C46 -167.3(4) . . . . ? C23 Rh1 N42 C46 -142.8(4) . . . . ? N3 N4 C5 N1 0.9(6) . . . . ? N3 N4 C5 C6 -178.8(6) . . . . ? N2 N1 C5 N4 -0.7(6) . . . . ? Ir1 N1 C5 N4 -165.3(4) . . . . ? N2 N1 C5 C6 179.0(6) . . . . ? Ir1 N1 C5 C6 14.4(10) . . . . ? C41 Ir1 C11 C12 -81.8(4) . . . . ? N1 Ir1 C11 C12 180.0(3) . . . . ? N31 Ir1 C11 C12 20.0(9) . . . . ? C13 Ir1 C11 C12 37.6(4) . . . . ? C15 Ir1 C11 C12 115.8(5) . . . . ? C14 Ir1 C11 C12 80.3(4) . . . . ? C41 Ir1 C11 C15 162.4(4) . . . . ? N1 Ir1 C11 C15 64.2(4) . . . . ? N31 Ir1 C11 C15 -95.9(8) . . . . ? C12 Ir1 C11 C15 -115.8(5) . . . . ? C13 Ir1 C11 C15 -78.3(4) . . . . ? C14 Ir1 C11 C15 -35.5(4) . . . . ? C41 Ir1 C11 C16 40.3(7) . . . . ? N1 Ir1 C11 C16 -57.9(6) . . . . ? N31 Ir1 C11 C16 142.1(7) . . . . ? C12 Ir1 C11 C16 122.1(8) . . . . ? C13 Ir1 C11 C16 159.7(7) . . . . ? C15 Ir1 C11 C16 -122.1(8) . . . . ? C14 Ir1 C11 C16 -157.6(7) . . . . ? C15 C11 C12 C13 0.4(6) . . . . ? C16 C11 C12 C13 170.6(6) . . . . ? Ir1 C11 C12 C13 -63.0(4) . . . . ? C15 C11 C12 C17 -173.9(6) . . . . ? C16 C11 C12 C17 -3.7(10) . . . . ? Ir1 C11 C12 C17 122.8(6) . . . . ? C15 C11 C12 Ir1 63.4(4) . . . . ? C16 C11 C12 Ir1 -126.4(6) . . . . ? C41 Ir1 C12 C13 -135.9(4) . . . . ? N1 Ir1 C12 C13 117.3(5) . . . . ? N31 Ir1 C12 C13 -55.3(4) . . . . ? C11 Ir1 C12 C13 117.3(5) . . . . ? C15 Ir1 C12 C13 78.8(4) . . . . ? C14 Ir1 C12 C13 37.6(4) . . . . ? C41 Ir1 C12 C11 106.8(4) . . . . ? N1 Ir1 C12 C11 0.0(6) . . . . ? N31 Ir1 C12 C11 -172.6(3) . . . . ? C13 Ir1 C12 C11 -117.3(5) . . . . ? C15 Ir1 C12 C11 -38.5(4) . . . . ? C14 Ir1 C12 C11 -79.7(4) . . . . ? C41 Ir1 C12 C17 -13.5(7) . . . . ? N1 Ir1 C12 C17 -120.4(6) . . . . ? N31 Ir1 C12 C17 67.0(7) . . . . ? C11 Ir1 C12 C17 -120.4(8) . . . . ? C13 Ir1 C12 C17 122.3(8) . . . . ? C15 Ir1 C12 C17 -158.9(7) . . . . ? C14 Ir1 C12 C17 159.9(7) . . . . ? C11 C12 C13 C14 -0.6(6) . . . . ? C17 C12 C13 C14 173.5(6) . . . . ? Ir1 C12 C13 C14 -63.3(4) . . . . ? C11 C12 C13 C18 -176.8(6) . . . . ? C17 C12 C13 C18 -2.6(10) . . . . ? Ir1 C12 C13 C18 120.5(6) . . . . ? C11 C12 C13 Ir1 62.7(4) . . . . ? C17 C12 C13 Ir1 -123.1(6) . . . . ? C41 Ir1 C13 C12 55.5(5) . . . . ? N1 Ir1 C13 C12 -128.2(4) . . . . ? N31 Ir1 C13 C12 136.3(4) . . . . ? C11 Ir1 C13 C12 -38.2(4) . . . . ? C15 Ir1 C13 C12 -81.2(4) . . . . ? C14 Ir1 C13 C12 -117.7(5) . . . . ? C41 Ir1 C13 C14 173.2(4) . . . . ? N1 Ir1 C13 C14 -10.5(6) . . . . ? N31 Ir1 C13 C14 -106.0(4) . . . . ? C12 Ir1 C13 C14 117.7(5) . . . . ? C11 Ir1 C13 C14 79.5(4) . . . . ? C15 Ir1 C13 C14 36.5(4) . . . . ? C41 Ir1 C13 C18 -65.8(7) . . . . ? N1 Ir1 C13 C18 110.5(6) . . . . ? N31 Ir1 C13 C18 15.0(7) . . . . ? C12 Ir1 C13 C18 -121.3(8) . . . . ? C11 Ir1 C13 C18 -159.5(7) . . . . ? C15 Ir1 C13 C18 157.5(7) . . . . ? C14 Ir1 C13 C18 121.0(8) . . . . ? C12 C13 C14 C15 0.6(6) . . . . ? C18 C13 C14 C15 176.9(6) . . . . ? Ir1 C13 C14 C15 -60.6(4) . . . . ? C12 C13 C14 C19 -173.5(6) . . . . ? C18 C13 C14 C19 2.8(10) . . . . ? Ir1 C13 C14 C19 125.3(6) . . . . ? C12 C13 C14 Ir1 61.3(4) . . . . ? C18 C13 C14 Ir1 -122.5(6) . . . . ? C41 Ir1 C14 C15 100.4(8) . . . . ? N1 Ir1 C14 C15 -68.4(4) . . . . ? N31 Ir1 C14 C15 -159.6(3) . . . . ? C12 Ir1 C14 C15 80.3(4) . . . . ? C11 Ir1 C14 C15 36.9(3) . . . . ? C13 Ir1 C14 C15 117.8(5) . . . . ? C41 Ir1 C14 C13 -17.5(10) . . . . ? N1 Ir1 C14 C13 173.8(4) . . . . ? N31 Ir1 C14 C13 82.5(4) . . . . ? C12 Ir1 C14 C13 -37.5(4) . . . . ? C11 Ir1 C14 C13 -80.9(4) . . . . ? C15 Ir1 C14 C13 -117.8(5) . . . . ? C41 Ir1 C14 C19 -138.1(8) . . . . ? N1 Ir1 C14 C19 53.1(7) . . . . ? N31 Ir1 C14 C19 -38.1(7) . . . . ? C12 Ir1 C14 C19 -158.2(8) . . . . ? C11 Ir1 C14 C19 158.4(8) . . . . ? C13 Ir1 C14 C19 -120.7(9) . . . . ? C15 Ir1 C14 C19 121.5(8) . . . . ? C13 C14 C15 C11 -0.4(6) . . . . ? C19 C14 C15 C11 173.8(6) . . . . ? Ir1 C14 C15 C11 -59.7(4) . . . . ? C13 C14 C15 C20 179.4(5) . . . . ? C19 C14 C15 C20 -6.5(10) . . . . ? Ir1 C14 C15 C20 120.1(6) . . . . ? C13 C14 C15 Ir1 59.3(4) . . . . ? C19 C14 C15 Ir1 -126.5(6) . . . . ? C12 C11 C15 C14 0.0(6) . . . . ? C16 C11 C15 C14 -170.4(6) . . . . ? Ir1 C11 C15 C14 61.6(4) . . . . ? C12 C11 C15 C20 -179.8(5) . . . . ? C16 C11 C15 C20 9.8(9) . . . . ? Ir1 C11 C15 C20 -118.2(6) . . . . ? C12 C11 C15 Ir1 -61.6(4) . . . . ? C16 C11 C15 Ir1 128.0(6) . . . . ? C41 Ir1 C15 C14 -148.0(4) . . . . ? N1 Ir1 C15 C14 117.4(4) . . . . ? N31 Ir1 C15 C14 31.2(5) . . . . ? C12 Ir1 C15 C14 -80.8(4) . . . . ? C11 Ir1 C15 C14 -119.8(5) . . . . ? C13 Ir1 C15 C14 -37.9(4) . . . . ? C41 Ir1 C15 C11 -28.3(6) . . . . ? N1 Ir1 C15 C11 -122.8(4) . . . . ? N31 Ir1 C15 C11 151.0(4) . . . . ? C12 Ir1 C15 C11 38.9(4) . . . . ? C13 Ir1 C15 C11 81.8(4) . . . . ? C14 Ir1 C15 C11 119.8(5) . . . . ? C41 Ir1 C15 C20 90.5(6) . . . . ? N1 Ir1 C15 C20 -4.0(6) . . . . ? N31 Ir1 C15 C20 -90.2(7) . . . . ? C12 Ir1 C15 C20 157.8(7) . . . . ? C11 Ir1 C15 C20 118.8(8) . . . . ? C13 Ir1 C15 C20 -159.3(7) . . . . ? C14 Ir1 C15 C20 -121.4(7) . . . . ? C52 Rh1 C21 C22 -122.2(4) . . . . ? N42 Rh1 C21 C22 -43.9(5) . . . . ? N3 Rh1 C21 C22 148.3(4) . . . . ? C25 Rh1 C21 C22 118.6(6) . . . . ? C24 Rh1 C21 C22 79.2(4) . . . . ? C23 Rh1 C21 C22 38.3(4) . . . . ? C52 Rh1 C21 C25 119.2(4) . . . . ? N42 Rh1 C21 C25 -162.5(4) . . . . ? N3 Rh1 C21 C25 29.7(5) . . . . ? C22 Rh1 C21 C25 -118.6(6) . . . . ? C24 Rh1 C21 C25 -39.4(4) . . . . ? C23 Rh1 C21 C25 -80.3(4) . . . . ? C52 Rh1 C21 C26 -1.6(8) . . . . ? N42 Rh1 C21 C26 76.7(8) . . . . ? N3 Rh1 C21 C26 -91.1(8) . . . . ? C22 Rh1 C21 C26 120.6(10) . . . . ? C25 Rh1 C21 C26 -120.8(9) . . . . ? C24 Rh1 C21 C26 -160.2(9) . . . . ? C23 Rh1 C21 C26 158.9(9) . . . . ? C25 C21 C22 C23 -5.7(7) . . . . ? C26 C21 C22 C23 172.7(6) . . . . ? Rh1 C21 C22 C23 -66.2(4) . . . . ? C25 C21 C22 C27 -178.6(6) . . . . ? C26 C21 C22 C27 -0.2(11) . . . . ? Rh1 C21 C22 C27 120.9(7) . . . . ? C25 C21 C22 Rh1 60.4(4) . . . . ? C26 C21 C22 Rh1 -121.1(7) . . . . ? C52 Rh1 C22 C21 66.3(5) . . . . ? N42 Rh1 C22 C21 148.3(4) . . . . ? N3 Rh1 C22 C21 -97.2(8) . . . . ? C25 Rh1 C22 C21 -37.2(4) . . . . ? C24 Rh1 C22 C21 -80.6(4) . . . . ? C23 Rh1 C22 C21 -116.1(6) . . . . ? C52 Rh1 C22 C23 -177.6(4) . . . . ? N42 Rh1 C22 C23 -95.6(4) . . . . ? N3 Rh1 C22 C23 18.9(10) . . . . ? C25 Rh1 C22 C23 79.0(4) . . . . ? C21 Rh1 C22 C23 116.1(6) . . . . ? C24 Rh1 C22 C23 35.6(4) . . . . ? C52 Rh1 C22 C27 -54.3(8) . . . . ? N42 Rh1 C22 C27 27.7(8) . . . . ? N3 Rh1 C22 C27 142.2(7) . . . . ? C25 Rh1 C22 C27 -157.8(8) . . . . ? C21 Rh1 C22 C27 -120.6(9) . . . . ? C24 Rh1 C22 C27 158.8(8) . . . . ? C23 Rh1 C22 C27 123.3(9) . . . . ? C21 C22 C23 C24 4.0(7) . . . . ? C27 C22 C23 C24 176.8(6) . . . . ? Rh1 C22 C23 C24 -60.2(4) . . . . ? C21 C22 C23 C28 -172.5(6) . . . . ? C27 C22 C23 C28 0.4(11) . . . . ? Rh1 C22 C23 C28 123.3(6) . . . . ? C21 C22 C23 Rh1 64.2(4) . . . . ? C27 C22 C23 Rh1 -123.0(7) . . . . ? C52 Rh1 C23 C24 123.7(6) . . . . ? N42 Rh1 C23 C24 -148.4(4) . . . . ? N3 Rh1 C23 C24 -53.3(4) . . . . ? C22 Rh1 C23 C24 119.2(6) . . . . ? C25 Rh1 C23 C24 37.5(4) . . . . ? C21 Rh1 C23 C24 80.6(4) . . . . ? C52 Rh1 C23 C22 4.6(8) . . . . ? N42 Rh1 C23 C22 92.5(4) . . . . ? N3 Rh1 C23 C22 -172.4(4) . . . . ? C25 Rh1 C23 C22 -81.7(5) . . . . ? C21 Rh1 C23 C22 -38.6(4) . . . . ? C24 Rh1 C23 C22 -119.2(6) . . . . ? C52 Rh1 C23 C28 -113.6(8) . . . . ? N42 Rh1 C23 C28 -25.7(8) . . . . ? N3 Rh1 C23 C28 69.4(8) . . . . ? C22 Rh1 C23 C28 -118.1(9) . . . . ? C25 Rh1 C23 C28 160.1(8) . . . . ? C21 Rh1 C23 C28 -156.7(8) . . . . ? C24 Rh1 C23 C28 122.7(9) . . . . ? C22 C23 C24 C25 -0.7(7) . . . . ? C28 C23 C24 C25 175.7(6) . . . . ? Rh1 C23 C24 C25 -58.2(4) . . . . ? C22 C23 C24 C29 179.6(6) . . . . ? C28 C23 C24 C29 -4.0(10) . . . . ? Rh1 C23 C24 C29 122.1(6) . . . . ? C22 C23 C24 Rh1 57.6(4) . . . . ? C28 C23 C24 Rh1 -126.1(6) . . . . ? C52 Rh1 C24 C23 -126.6(5) . . . . ? N42 Rh1 C24 C23 43.2(5) . . . . ? N3 Rh1 C24 C23 137.1(4) . . . . ? C22 Rh1 C24 C23 -37.2(4) . . . . ? C25 Rh1 C24 C23 -119.5(6) . . . . ? C21 Rh1 C24 C23 -80.4(4) . . . . ? C52 Rh1 C24 C25 -7.1(7) . . . . ? N42 Rh1 C24 C25 162.7(4) . . . . ? N3 Rh1 C24 C25 -103.4(4) . . . . ? C22 Rh1 C24 C25 82.3(4) . . . . ? C21 Rh1 C24 C25 39.1(4) . . . . ? C23 Rh1 C24 C25 119.5(6) . . . . ? C52 Rh1 C24 C29 109.4(7) . . . . ? N42 Rh1 C24 C29 -80.7(7) . . . . ? N3 Rh1 C24 C29 13.1(7) . . . . ? C22 Rh1 C24 C29 -161.2(8) . . . . ? C25 Rh1 C24 C29 116.5(8) . . . . ? C21 Rh1 C24 C29 155.6(8) . . . . ? C23 Rh1 C24 C29 -124.0(8) . . . . ? C22 C21 C25 C24 5.2(7) . . . . ? C26 C21 C25 C24 -173.3(6) . . . . ? Rh1 C21 C25 C24 65.3(4) . . . . ? C22 C21 C25 C30 177.2(6) . . . . ? C26 C21 C25 C30 -1.3(11) . . . . ? Rh1 C21 C25 C30 -122.7(7) . . . . ? C22 C21 C25 Rh1 -60.1(4) . . . . ? C26 C21 C25 Rh1 121.4(7) . . . . ? C23 C24 C25 C21 -2.8(7) . . . . ? C29 C24 C25 C21 176.9(6) . . . . ? Rh1 C24 C25 C21 -63.8(4) . . . . ? C23 C24 C25 C30 -174.9(6) . . . . ? C29 C24 C25 C30 4.8(10) . . . . ? Rh1 C24 C25 C30 124.1(7) . . . . ? C23 C24 C25 Rh1 61.0(4) . . . . ? C29 C24 C25 Rh1 -119.3(6) . . . . ? C52 Rh1 C25 C21 -68.9(4) . . . . ? N42 Rh1 C25 C21 57.8(11) . . . . ? N3 Rh1 C25 C21 -160.7(4) . . . . ? C22 Rh1 C25 C21 37.1(4) . . . . ? C24 Rh1 C25 C21 114.9(6) . . . . ? C23 Rh1 C25 C21 79.7(4) . . . . ? C52 Rh1 C25 C24 176.2(4) . . . . ? N42 Rh1 C25 C24 -57.2(11) . . . . ? N3 Rh1 C25 C24 84.4(4) . . . . ? C22 Rh1 C25 C24 -77.8(4) . . . . ? C21 Rh1 C25 C24 -114.9(6) . . . . ? C23 Rh1 C25 C24 -35.2(4) . . . . ? C52 Rh1 C25 C30 53.6(8) . . . . ? N42 Rh1 C25 C30 -179.7(8) . . . . ? N3 Rh1 C25 C30 -38.2(7) . . . . ? C22 Rh1 C25 C30 159.6(8) . . . . ? C21 Rh1 C25 C30 122.5(9) . . . . ? C24 Rh1 C25 C30 -122.6(9) . . . . ? C23 Rh1 C25 C30 -157.8(8) . . . . ? C35 N31 C31 C32 2.6(9) . . . . ? Ir1 N31 C31 C32 -175.3(5) . . . . ? N31 C31 C32 C33 -2.1(10) . . . . ? C31 C32 C33 C34 0.2(10) . . . . ? C32 C33 C34 C35 1.1(10) . . . . ? C31 N31 C35 C34 -1.3(9) . . . . ? Ir1 N31 C35 C34 176.7(4) . . . . ? C31 N31 C35 C36 -178.7(5) . . . . ? Ir1 N31 C35 C36 -0.7(7) . . . . ? C33 C34 C35 N31 -0.5(9) . . . . ? C33 C34 C35 C36 176.6(6) . . . . ? N31 C35 C36 C41 -0.2(8) . . . . ? C34 C35 C36 C41 -177.4(6) . . . . ? N31 C35 C36 C37 179.1(6) . . . . ? C34 C35 C36 C37 1.9(10) . . . . ? C41 C36 C37 C38 0.5(10) . . . . ? C35 C36 C37 C38 -178.7(7) . . . . ? C36 C37 C38 C39 0.0(12) . . . . ? C37 C38 C39 C40 0.1(12) . . . . ? C38 C39 C40 C41 -0.6(11) . . . . ? C39 C40 C41 C36 1.0(10) . . . . ? C39 C40 C41 Ir1 178.1(5) . . . . ? C37 C36 C41 C40 -0.9(9) . . . . ? C35 C36 C41 C40 178.4(5) . . . . ? C37 C36 C41 Ir1 -178.4(5) . . . . ? C35 C36 C41 Ir1 0.9(7) . . . . ? N1 Ir1 C41 C40 96.0(6) . . . . ? N31 Ir1 C41 C40 -178.1(6) . . . . ? C12 Ir1 C41 C40 -55.2(6) . . . . ? C11 Ir1 C41 C40 -16.4(6) . . . . ? C13 Ir1 C41 C40 -86.1(6) . . . . ? C15 Ir1 C41 C40 1.4(8) . . . . ? C14 Ir1 C41 C40 -73.3(10) . . . . ? N1 Ir1 C41 C36 -86.8(5) . . . . ? N31 Ir1 C41 C36 -1.0(4) . . . . ? C12 Ir1 C41 C36 122.0(5) . . . . ? C11 Ir1 C41 C36 160.7(4) . . . . ? C13 Ir1 C41 C36 91.1(5) . . . . ? C15 Ir1 C41 C36 178.6(4) . . . . ? C14 Ir1 C41 C36 103.9(8) . . . . ? C46 N42 C42 C43 1.5(9) . . . . ? Rh1 N42 C42 C43 177.3(5) . . . . ? N42 C42 C43 C44 0.6(10) . . . . ? C42 C43 C44 C45 -0.6(11) . . . . ? C43 C44 C45 C46 -1.3(11) . . . . ? C42 N42 C46 C45 -3.4(9) . . . . ? Rh1 N42 C46 C45 -179.6(5) . . . . ? C42 N42 C46 C47 170.9(6) . . . . ? Rh1 N42 C46 C47 -5.3(7) . . . . ? C44 C45 C46 N42 3.4(10) . . . . ? C44 C45 C46 C47 -170.3(7) . . . . ? N42 C46 C47 C48 -176.2(6) . . . . ? C45 C46 C47 C48 -2.2(11) . . . . ? N42 C46 C47 C52 -1.8(8) . . . . ? C45 C46 C47 C52 172.1(6) . . . . ? C52 C47 C48 C49 -2.6(11) . . . . ? C46 C47 C48 C49 171.4(7) . . . . ? C47 C48 C49 C50 1.1(12) . . . . ? C48 C49 C50 C51 0.1(12) . . . . ? C49 C50 C51 C52 0.2(12) . . . . ? C50 C51 C52 C47 -1.6(10) . . . . ? C50 C51 C52 Rh1 178.4(5) . . . . ? C48 C47 C52 C51 2.8(10) . . . . ? C46 C47 C52 C51 -171.8(6) . . . . ? C48 C47 C52 Rh1 -177.2(5) . . . . ? C46 C47 C52 Rh1 8.2(7) . . . . ? N42 Rh1 C52 C51 171.6(6) . . . . ? N3 Rh1 C52 C51 83.2(6) . . . . ? C22 Rh1 C52 C51 -91.2(6) . . . . ? C25 Rh1 C52 C51 -20.9(6) . . . . ? C21 Rh1 C52 C51 -56.4(6) . . . . ? C24 Rh1 C52 C51 -16.1(9) . . . . ? C23 Rh1 C52 C51 -94.2(7) . . . . ? N42 Rh1 C52 C47 -8.4(5) . . . . ? N3 Rh1 C52 C47 -96.8(5) . . . . ? C22 Rh1 C52 C47 88.8(5) . . . . ? C25 Rh1 C52 C47 159.1(5) . . . . ? C21 Rh1 C52 C47 123.6(5) . . . . ? C24 Rh1 C52 C47 163.9(5) . . . . ? C23 Rh1 C52 C47 85.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.527 _refine_diff_density_min -1.424 _refine_diff_density_rms 0.158 _database_code_depnum_ccdc_archive 'CCDC 945557' ####################################################################### # # 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_comp12bp _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H49 Ir N6 Ph 1+, C24 H20 B 1-, C H2 Cl2, 2(C4 H10 O)' _chemical_formula_sum 'C77 H91 B Cl2 Ir N6 O2 Rh' _chemical_formula_weight 1509.38 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.7305(4) _cell_length_b 15.6553(9) _cell_length_c 18.2761(8) _cell_angle_alpha 67.466(3) _cell_angle_beta 76.436(2) _cell_angle_gamma 82.757(2) _cell_volume 3524.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 192(2) _cell_measurement_reflns_used 27637 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.57 _exptl_crystal_description platelet _exptl_crystal_colour orange _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.422 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 2.246 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5070 _exptl_absorpt_correction_T_max 0.8960 _exptl_absorpt_process_details 'NUMABS (Rigaku, 1999)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 192(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku R-axis rapid' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34982 _diffrn_reflns_av_R_equivalents 0.0383 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _reflns_number_total 16053 _reflns_number_gt 13131 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'Process auto' _computing_cell_refinement 'Process auto' _computing_data_reduction CrystalStructure _computing_structure_solution SIR2004 _computing_structure_refinement SHELXL-97 _computing_molecular_graphics 'ortep-3 for win' _computing_publication_material SHELXL-97 _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. Electron density synthesis with coefficients Fo-Fc Highest peak 4.07 at 0.2163 0.0722 0.1139 [ 0.30 A from RH1 ] Deepest hole -1.60 at 0.2974 0.6761 0.1751 [ 0.59 A from IR1 ] ; _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^)+(0.0828P)^2^+17.9338P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16053 _refine_ls_number_parameters 811 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0704 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1664 _refine_ls_wR_factor_gt 0.1554 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.271818(18) 0.676278(16) 0.153057(14) 0.02819(9) Uani 1 1 d . . . Rh1 Rh 0.20461(3) 1.07011(3) 0.13045(2) 0.01492(10) Uani 1 1 d . . . Cl1 Cl 0.5462(8) 0.3462(8) 0.1880(4) 0.278(6) Uani 1 1 d D . . Cl2 Cl 0.3928(5) 0.2843(5) 0.3255(5) 0.186(3) Uani 1 1 d D . . O1 O 0.5349(12) 0.9685(9) 0.2732(8) 0.153(5) Uani 1 1 d D . . O2 O 0.8230(18) 0.0788(14) 0.3579(14) 0.209(9) Uani 1 1 d D . . N1 N 0.2896(4) 0.8197(3) 0.0984(3) 0.0232(10) Uani 1 1 d . . . N2 N 0.2597(4) 0.8697(3) 0.1456(3) 0.0257(10) Uani 1 1 d . . . N3 N 0.2568(4) 0.9570(3) 0.0969(3) 0.0260(10) Uani 1 1 d . . . N4 N 0.2828(4) 0.9667(4) 0.0182(3) 0.0288(11) Uani 1 1 d . . . N41 N 0.3554(4) 0.6739(3) 0.2359(3) 0.0280(11) Uani 1 1 d . . . N52 N 0.1797(4) 0.9772(4) 0.2506(3) 0.0323(12) Uani 1 1 d . . . C1 C 0.5143(12) 0.8898(8) 0.1959(7) 0.097(5) Uani 1 1 d . . . H1A H 0.5529 0.9334 0.1464 0.117 Uiso 1 1 calc R . . H1B H 0.4427 0.9076 0.1997 0.117 Uiso 1 1 calc R . . H1C H 0.5255 0.8272 0.1947 0.117 Uiso 1 1 calc R . . C2 C 0.5451(12) 0.8913(9) 0.2629(12) 0.114(6) Uani 1 1 d D . . H2A H 0.5071 0.8449 0.3120 0.137 Uiso 1 1 calc R . . H2B H 0.6167 0.8710 0.2588 0.137 Uiso 1 1 calc R . . C3 C 0.578(3) 0.9731(15) 0.330(2) 0.227(17) Uani 1 1 d D . . H3A H 0.6511 0.9763 0.3096 0.272 Uiso 1 1 calc R . . H3B H 0.5641 0.9164 0.3786 0.272 Uiso 1 1 calc R . . C4 C 0.541(3) 1.051(3) 0.349(2) 0.31(2) Uani 1 1 d . . . H4A H 0.4679 1.0487 0.3679 0.369 Uiso 1 1 calc R . . H4B H 0.5575 1.1074 0.3015 0.369 Uiso 1 1 calc R . . H4C H 0.5715 1.0516 0.3925 0.369 Uiso 1 1 calc R . . C5 C 0.3014(4) 0.8807(4) 0.0202(4) 0.0259(12) Uani 1 1 d . . . C6 C 0.3319(5) 0.8578(5) -0.0538(4) 0.0324(14) Uani 1 1 d . . . H6A H 0.3947 0.8877 -0.0860 0.039 Uiso 1 1 calc R . . H6B H 0.2794 0.8801 -0.0857 0.039 Uiso 1 1 calc R . . H6C H 0.3418 0.7906 -0.0384 0.039 Uiso 1 1 calc R . . C7 C 0.792(4) -0.041(3) 0.493(3) 0.45(5) Uani 1 1 d D . . H7A H 0.7954 -0.0895 0.4703 0.543 Uiso 1 1 calc R . . H7B H 0.7226 -0.0184 0.5036 0.543 Uiso 1 1 calc R . . H7C H 0.8174 -0.0668 0.5431 0.543 Uiso 1 1 calc R . . C8 C 0.856(3) 0.038(3) 0.432(3) 0.36(4) Uani 1 1 d D . . H8A H 0.8545 0.0858 0.4556 0.430 Uiso 1 1 calc R . . H8B H 0.9266 0.0148 0.4217 0.430 Uiso 1 1 calc R . . C9 C 0.8430(19) 0.1565(15) 0.2804(16) 0.147(8) Uani 1 1 d D . . H9A H 0.9050 0.1402 0.2471 0.177 Uiso 1 1 calc R . . H9B H 0.8573 0.2105 0.2912 0.177 Uiso 1 1 calc R . . C10 C 0.765(3) 0.1860(19) 0.2312(17) 0.250(18) Uani 1 1 d . . . H10A H 0.7039 0.2056 0.2617 0.300 Uiso 1 1 calc R . . H10B H 0.7513 0.1343 0.2180 0.300 Uiso 1 1 calc R . . H10C H 0.7889 0.2379 0.1811 0.300 Uiso 1 1 calc R . . C11 C 0.1088(5) 0.6913(4) 0.1497(4) 0.0311(13) Uani 1 1 d . . . C12 C 0.1182(5) 0.6393(5) 0.2306(4) 0.0335(14) Uani 1 1 d . . . C13 C 0.1820(5) 0.5583(5) 0.2303(4) 0.0369(15) Uani 1 1 d . . . C14 C 0.2064(5) 0.5604(5) 0.1501(5) 0.0383(16) Uani 1 1 d . . . C15 C 0.1651(5) 0.6445(5) 0.0979(4) 0.0319(14) Uani 1 1 d . . . C16 C 0.0505(6) 0.7820(6) 0.1224(6) 0.050(2) Uani 1 1 d . . . H16A H 0.0782 0.8277 0.1358 0.061 Uiso 1 1 calc R . . H16B H -0.0200 0.7735 0.1500 0.061 Uiso 1 1 calc R . . H16C H 0.0554 0.8041 0.0638 0.061 Uiso 1 1 calc R . . C17 C 0.0653(6) 0.6583(7) 0.3051(5) 0.056(2) Uani 1 1 d . . . H17A H 0.0982 0.6216 0.3502 0.067 Uiso 1 1 calc R . . H17B H -0.0048 0.6415 0.3188 0.067 Uiso 1 1 calc R . . H17C H 0.0681 0.7242 0.2948 0.067 Uiso 1 1 calc R . . C18 C 0.2065(7) 0.4812(6) 0.3048(5) 0.059(2) Uani 1 1 d . . . H18A H 0.2793 0.4704 0.2982 0.071 Uiso 1 1 calc R . . H18B H 0.1754 0.4245 0.3125 0.071 Uiso 1 1 calc R . . H18C H 0.1806 0.4985 0.3522 0.071 Uiso 1 1 calc R . . C19 C 0.2598(7) 0.4832(5) 0.1237(6) 0.054(2) Uani 1 1 d . . . H19A H 0.2208 0.4274 0.1514 0.065 Uiso 1 1 calc R . . H19B H 0.3263 0.4704 0.1375 0.065 Uiso 1 1 calc R . . H19C H 0.2670 0.5019 0.0651 0.065 Uiso 1 1 calc R . . C20 C 0.1635(6) 0.6718(6) 0.0102(5) 0.049(2) Uani 1 1 d . . . H20A H 0.1871 0.7348 -0.0197 0.059 Uiso 1 1 calc R . . H20B H 0.0949 0.6696 0.0042 0.059 Uiso 1 1 calc R . . H20C H 0.2075 0.6289 -0.0114 0.059 Uiso 1 1 calc R . . C21 C 0.1675(5) 1.2187(4) 0.0771(5) 0.0366(15) Uani 1 1 d . . . C22 C 0.2089(6) 1.1995(4) 0.1469(4) 0.0363(15) Uani 1 1 d . . . C23 C 0.3110(5) 1.1670(4) 0.1296(4) 0.0328(14) Uani 1 1 d . . . C24 C 0.3295(5) 1.1619(4) 0.0527(4) 0.0302(13) Uani 1 1 d . . . C25 C 0.2406(5) 1.1923(4) 0.0188(4) 0.0338(14) Uani 1 1 d . . . C26 C 0.0677(6) 1.2635(6) 0.0635(6) 0.058(2) Uani 1 1 d . . . H26A H 0.0636 1.3257 0.0652 0.070 Uiso 1 1 calc R . . H26B H 0.0149 1.2263 0.1058 0.070 Uiso 1 1 calc R . . H26C H 0.0588 1.2680 0.0104 0.070 Uiso 1 1 calc R . . C27 C 0.1608(8) 1.2187(6) 0.2216(6) 0.058(2) Uani 1 1 d . . . H27A H 0.0988 1.1850 0.2472 0.070 Uiso 1 1 calc R . . H27B H 0.1454 1.2852 0.2072 0.070 Uiso 1 1 calc R . . H27C H 0.2068 1.1984 0.2593 0.070 Uiso 1 1 calc R . . C28 C 0.3869(7) 1.1517(6) 0.1814(5) 0.050(2) Uani 1 1 d . . . H28A H 0.4395 1.1967 0.1526 0.060 Uiso 1 1 calc R . . H28B H 0.4169 1.0889 0.1930 0.060 Uiso 1 1 calc R . . H28C H 0.3539 1.1594 0.2322 0.060 Uiso 1 1 calc R . . C29 C 0.4259(5) 1.1305(5) 0.0100(5) 0.0428(17) Uani 1 1 d . . . H29A H 0.4431 1.0665 0.0423 0.051 Uiso 1 1 calc R . . H29B H 0.4795 1.1706 0.0028 0.051 Uiso 1 1 calc R . . H29C H 0.4182 1.1340 -0.0431 0.051 Uiso 1 1 calc R . . C30 C 0.2320(7) 1.2031(6) -0.0647(5) 0.052(2) Uani 1 1 d . . . H30A H 0.2471 1.1432 -0.0713 0.063 Uiso 1 1 calc R . . H30B H 0.2796 1.2482 -0.1049 0.063 Uiso 1 1 calc R . . H30C H 0.1636 1.2247 -0.0724 0.063 Uiso 1 1 calc R . . C31 C 0.4134(4) 0.6487(4) 0.0982(4) 0.0250(12) Uani 1 1 d . . . C32 C 0.4427(5) 0.6384(5) 0.0246(4) 0.0328(14) Uani 1 1 d . . . H32 H 0.3939 0.6458 -0.0069 0.039 Uiso 1 1 calc R . . C33 C 0.5425(5) 0.6174(5) -0.0050(4) 0.0387(16) Uani 1 1 d . . . H33 H 0.5613 0.6125 -0.0568 0.046 Uiso 1 1 calc R . . C34 C 0.6129(5) 0.6038(5) 0.0406(5) 0.0417(17) Uani 1 1 d . . . H34 H 0.6805 0.5886 0.0207 0.050 Uiso 1 1 calc R . . C35 C 0.5867(5) 0.6121(5) 0.1153(5) 0.0379(15) Uani 1 1 d . . . H35 H 0.6360 0.6025 0.1468 0.046 Uiso 1 1 calc R . . C36 C 0.4878(5) 0.6345(4) 0.1441(4) 0.0301(13) Uani 1 1 d . . . C37 C 0.4543(5) 0.6471(4) 0.2209(4) 0.0311(13) Uani 1 1 d . . . C38 C 0.5131(6) 0.6347(5) 0.2773(5) 0.0412(16) Uani 1 1 d . . . H38 H 0.5818 0.6158 0.2669 0.049 Uiso 1 1 calc R . . C39 C 0.4719(7) 0.6495(6) 0.3482(5) 0.050(2) Uani 1 1 d . . . H39 H 0.5115 0.6399 0.3871 0.061 Uiso 1 1 calc R . . C40 C 0.3721(6) 0.6787(5) 0.3616(4) 0.0425(17) Uani 1 1 d . . . H40 H 0.3419 0.6899 0.4097 0.051 Uiso 1 1 calc R . . C41 C 0.3182(5) 0.6911(5) 0.3037(4) 0.0339(14) Uani 1 1 d . . . H41 H 0.2504 0.7132 0.3121 0.041 Uiso 1 1 calc R . . C42 C 0.0646(4) 1.0258(4) 0.1437(4) 0.0256(12) Uani 1 1 d . . . C43 C 0.0127(5) 1.0480(5) 0.0828(4) 0.0336(14) Uani 1 1 d . . . H43 H 0.0427 1.0855 0.0294 0.040 Uiso 1 1 calc R . . C44 C -0.0824(6) 1.0170(5) 0.0975(5) 0.0425(17) Uani 1 1 d . . . H44 H -0.1177 1.0336 0.0548 0.051 Uiso 1 1 calc R . . C45 C -0.1259(5) 0.9610(5) 0.1759(5) 0.0438(18) Uani 1 1 d . . . H45 H -0.1924 0.9415 0.1871 0.053 Uiso 1 1 calc R . . C46 C -0.0728(5) 0.9338(5) 0.2371(5) 0.0420(17) Uani 1 1 d . . . H46 H -0.1016 0.8937 0.2900 0.050 Uiso 1 1 calc R . . C47 C 0.0237(5) 0.9656(4) 0.2211(4) 0.0304(13) Uani 1 1 d . . . C48 C 0.0893(5) 0.9376(4) 0.2793(4) 0.0299(13) Uani 1 1 d . . . C49 C 0.0685(6) 0.8706(5) 0.3573(4) 0.0397(16) Uani 1 1 d . . . H49 H 0.0053 0.8427 0.3771 0.048 Uiso 1 1 calc R . . C50 C 0.1388(6) 0.8444(5) 0.4058(4) 0.0457(18) Uani 1 1 d . . . H50 H 0.1244 0.7986 0.4587 0.055 Uiso 1 1 calc R . . C51 C 0.2288(6) 0.8852(6) 0.3767(4) 0.0457(18) Uani 1 1 d . . . H51 H 0.2776 0.8688 0.4096 0.055 Uiso 1 1 calc R . . C52 C 0.2496(5) 0.9519(5) 0.2978(4) 0.0353(15) Uani 1 1 d . . . H52 H 0.3130 0.9795 0.2773 0.042 Uiso 1 1 calc R . . C55 C 0.5014(15) 0.328(3) 0.2816(10) 0.249(18) Uani 1 1 d D . . H55A H 0.4992 0.3881 0.2883 0.298 Uiso 1 1 calc R . . H55B H 0.5506 0.2871 0.3124 0.298 Uiso 1 1 calc R . . C56 C 0.8425(5) 0.4536(4) 0.2634(4) 0.0291(13) Uani 1 1 d . . . C57 C 0.7751(5) 0.4369(5) 0.2242(4) 0.0351(14) Uani 1 1 d . . . H57 H 0.7104 0.4165 0.2543 0.042 Uiso 1 1 calc R . . C58 C 0.7998(6) 0.4494(5) 0.1422(4) 0.0411(16) Uani 1 1 d . . . H58 H 0.7517 0.4374 0.1179 0.049 Uiso 1 1 calc R . . C59 C 0.8910(6) 0.4783(5) 0.0970(4) 0.0412(17) Uani 1 1 d . . . H59 H 0.9072 0.4866 0.0413 0.049 Uiso 1 1 calc R . . C60 C 0.9606(6) 0.4956(6) 0.1334(4) 0.0476(19) Uani 1 1 d . . . H60 H 1.0253 0.5155 0.1027 0.057 Uiso 1 1 calc R . . C61 C 0.9352(6) 0.4838(6) 0.2143(4) 0.0430(17) Uani 1 1 d . . . H61 H 0.9836 0.4969 0.2377 0.052 Uiso 1 1 calc R . . C62 C 0.7927(5) 0.5442(5) 0.3656(4) 0.0298(13) Uani 1 1 d . . . C63 C 0.8014(6) 0.6275(5) 0.2993(5) 0.0419(16) Uani 1 1 d . . . H63 H 0.8242 0.6250 0.2469 0.050 Uiso 1 1 calc R . . C64 C 0.7787(7) 0.7140(6) 0.3050(7) 0.058(2) Uani 1 1 d . . . H64 H 0.7837 0.7684 0.2576 0.069 Uiso 1 1 calc R . . C65 C 0.7489(6) 0.7199(6) 0.3799(7) 0.060(3) Uani 1 1 d . . . H65 H 0.7364 0.7786 0.3849 0.072 Uiso 1 1 calc R . . C66 C 0.7371(5) 0.6390(6) 0.4488(6) 0.0463(19) Uani 1 1 d . . . H66 H 0.7147 0.6428 0.5008 0.056 Uiso 1 1 calc R . . C67 C 0.7576(5) 0.5539(5) 0.4418(5) 0.0380(15) Uani 1 1 d . . . H67 H 0.7480 0.4998 0.4895 0.046 Uiso 1 1 calc R . . C68 C 0.9132(4) 0.3870(4) 0.4001(3) 0.0258(12) Uani 1 1 d . . . C69 C 0.9475(5) 0.4064(4) 0.4576(4) 0.0283(12) Uani 1 1 d . . . H69 H 0.9135 0.4537 0.4756 0.034 Uiso 1 1 calc R . . C70 C 1.0304(5) 0.3587(5) 0.4903(4) 0.0309(13) Uani 1 1 d . . . H70 H 1.0524 0.3755 0.5283 0.037 Uiso 1 1 calc R . . C71 C 1.0802(5) 0.2875(5) 0.4674(4) 0.0329(14) Uani 1 1 d . . . H71 H 1.1357 0.2541 0.4898 0.040 Uiso 1 1 calc R . . C72 C 1.0461(5) 0.2668(5) 0.4103(4) 0.0359(15) Uani 1 1 d . . . H72 H 1.0787 0.2181 0.3936 0.043 Uiso 1 1 calc R . . C73 C 0.9661(5) 0.3155(5) 0.3778(4) 0.0314(13) Uani 1 1 d . . . H73 H 0.9459 0.2999 0.3384 0.038 Uiso 1 1 calc R . . C74 C 0.7161(5) 0.3794(5) 0.4045(3) 0.0286(13) Uani 1 1 d . . . C75 C 0.7174(5) 0.2832(5) 0.4258(4) 0.0365(15) Uani 1 1 d . . . H75 H 0.7802 0.2515 0.4174 0.044 Uiso 1 1 calc R . . C76 C 0.6324(6) 0.2320(6) 0.4583(5) 0.0471(19) Uani 1 1 d . . . H76 H 0.6378 0.1670 0.4715 0.057 Uiso 1 1 calc R . . C77 C 0.5394(6) 0.2752(7) 0.4717(5) 0.055(2) Uani 1 1 d . . . H77 H 0.4805 0.2404 0.4950 0.066 Uiso 1 1 calc R . . C78 C 0.5341(6) 0.3697(7) 0.4505(5) 0.051(2) Uani 1 1 d . . . H78 H 0.4707 0.4007 0.4582 0.061 Uiso 1 1 calc R . . C79 C 0.6197(5) 0.4198(5) 0.4182(4) 0.0371(15) Uani 1 1 d . . . H79 H 0.6131 0.4850 0.4045 0.045 Uiso 1 1 calc R . . B1 B 0.8159(5) 0.4417(5) 0.3589(4) 0.0263(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.02952(14) 0.02623(14) 0.02714(14) -0.00967(10) -0.00290(9) -0.00094(9) Rh1 0.01697(19) 0.01016(18) 0.01443(19) -0.00069(14) -0.00244(15) -0.00302(14) Cl1 0.312(10) 0.398(13) 0.136(5) -0.045(7) -0.044(6) -0.236(10) Cl2 0.157(5) 0.203(7) 0.240(7) -0.113(6) -0.085(5) 0.028(5) O1 0.228(15) 0.111(9) 0.161(11) -0.053(8) -0.124(11) 0.021(9) O2 0.32(3) 0.158(15) 0.203(19) -0.146(16) -0.075(18) 0.083(16) N1 0.024(2) 0.021(2) 0.022(2) -0.0066(19) -0.0004(19) -0.0013(19) N2 0.031(3) 0.017(2) 0.026(3) -0.007(2) -0.004(2) 0.001(2) N3 0.025(2) 0.024(2) 0.026(2) -0.005(2) -0.005(2) -0.004(2) N4 0.032(3) 0.027(3) 0.025(3) -0.008(2) 0.000(2) -0.006(2) N41 0.032(3) 0.023(2) 0.027(3) -0.007(2) -0.007(2) 0.004(2) N52 0.039(3) 0.025(3) 0.030(3) -0.009(2) -0.002(2) -0.002(2) C1 0.151(13) 0.058(7) 0.061(7) -0.019(6) 0.008(8) 0.006(8) C2 0.095(10) 0.056(7) 0.188(18) -0.030(10) -0.054(11) 0.009(7) C3 0.32(4) 0.092(15) 0.31(4) -0.025(19) -0.23(4) -0.002(19) C4 0.44(6) 0.34(5) 0.30(4) -0.19(4) -0.26(4) 0.06(5) C5 0.023(3) 0.026(3) 0.025(3) -0.005(2) -0.004(2) -0.002(2) C6 0.034(3) 0.034(3) 0.025(3) -0.009(3) -0.002(3) -0.003(3) C7 0.83(12) 0.32(5) 0.44(7) -0.31(5) -0.51(8) 0.43(7) C8 0.42(6) 0.38(7) 0.49(10) -0.36(8) -0.29(7) 0.28(6) C9 0.20(2) 0.106(15) 0.151(19) -0.082(15) -0.012(17) 0.007(15) C10 0.45(6) 0.15(2) 0.16(2) -0.032(19) -0.09(3) -0.08(3) C11 0.028(3) 0.025(3) 0.043(4) -0.013(3) -0.014(3) 0.001(2) C12 0.025(3) 0.043(4) 0.033(3) -0.018(3) 0.001(3) -0.005(3) C13 0.032(3) 0.031(3) 0.039(4) -0.005(3) -0.003(3) -0.007(3) C14 0.034(3) 0.031(3) 0.052(4) -0.022(3) 0.002(3) -0.007(3) C15 0.034(3) 0.033(3) 0.036(3) -0.017(3) -0.010(3) -0.007(3) C16 0.042(4) 0.046(4) 0.073(6) -0.028(4) -0.029(4) 0.015(4) C17 0.038(4) 0.089(7) 0.050(5) -0.045(5) 0.008(4) -0.009(4) C18 0.060(5) 0.042(4) 0.049(5) 0.010(4) -0.006(4) -0.010(4) C19 0.055(5) 0.032(4) 0.078(6) -0.033(4) 0.004(4) -0.003(3) C20 0.052(4) 0.065(5) 0.041(4) -0.024(4) -0.006(3) -0.025(4) C21 0.034(3) 0.016(3) 0.051(4) -0.004(3) -0.005(3) -0.004(2) C22 0.049(4) 0.017(3) 0.041(4) -0.010(3) -0.002(3) -0.008(3) C23 0.045(4) 0.019(3) 0.034(3) -0.004(2) -0.011(3) -0.012(3) C24 0.032(3) 0.022(3) 0.030(3) -0.002(2) -0.001(3) -0.014(2) C25 0.038(3) 0.021(3) 0.032(3) 0.004(2) -0.007(3) -0.015(3) C26 0.050(5) 0.029(4) 0.085(7) -0.011(4) -0.014(5) 0.009(3) C27 0.076(6) 0.041(4) 0.058(5) -0.028(4) 0.008(5) -0.015(4) C28 0.062(5) 0.046(4) 0.043(4) -0.007(4) -0.021(4) -0.017(4) C29 0.036(4) 0.040(4) 0.042(4) -0.006(3) 0.001(3) -0.014(3) C30 0.070(5) 0.045(4) 0.037(4) 0.001(3) -0.019(4) -0.020(4) C31 0.022(3) 0.021(3) 0.027(3) -0.005(2) -0.004(2) -0.001(2) C32 0.031(3) 0.030(3) 0.036(3) -0.013(3) -0.006(3) 0.003(3) C33 0.042(4) 0.036(4) 0.031(3) -0.013(3) 0.007(3) 0.000(3) C34 0.029(3) 0.038(4) 0.050(4) -0.018(3) 0.007(3) 0.004(3) C35 0.029(3) 0.035(4) 0.049(4) -0.015(3) -0.009(3) 0.005(3) C36 0.035(3) 0.020(3) 0.031(3) -0.007(2) -0.002(3) 0.000(2) C37 0.032(3) 0.023(3) 0.035(3) -0.006(3) -0.011(3) 0.004(3) C38 0.037(4) 0.043(4) 0.045(4) -0.015(3) -0.021(3) 0.010(3) C39 0.061(5) 0.054(5) 0.042(4) -0.017(4) -0.033(4) 0.017(4) C40 0.061(5) 0.040(4) 0.029(3) -0.016(3) -0.011(3) 0.002(4) C41 0.036(3) 0.037(4) 0.028(3) -0.014(3) -0.006(3) 0.003(3) C42 0.026(3) 0.020(3) 0.032(3) -0.009(2) -0.011(2) 0.002(2) C43 0.032(3) 0.027(3) 0.041(4) -0.009(3) -0.013(3) 0.002(3) C44 0.038(4) 0.036(4) 0.057(5) -0.015(3) -0.020(3) 0.001(3) C45 0.026(3) 0.035(4) 0.069(5) -0.015(4) -0.010(3) -0.009(3) C46 0.034(4) 0.036(4) 0.049(4) -0.011(3) 0.000(3) -0.009(3) C47 0.030(3) 0.024(3) 0.034(3) -0.011(3) 0.003(3) -0.005(2) C48 0.038(3) 0.026(3) 0.024(3) -0.010(2) 0.000(3) -0.002(3) C49 0.048(4) 0.035(4) 0.030(3) -0.010(3) 0.005(3) -0.011(3) C50 0.066(5) 0.037(4) 0.022(3) -0.002(3) 0.001(3) -0.004(4) C51 0.058(5) 0.045(4) 0.030(4) -0.008(3) -0.015(3) 0.006(4) C52 0.041(4) 0.034(3) 0.028(3) -0.007(3) -0.011(3) 0.002(3) C55 0.141(19) 0.50(6) 0.118(17) -0.10(3) 0.009(14) -0.14(3) C56 0.032(3) 0.027(3) 0.029(3) -0.010(2) -0.006(3) 0.000(2) C57 0.035(3) 0.043(4) 0.030(3) -0.014(3) -0.009(3) -0.003(3) C58 0.047(4) 0.050(4) 0.030(3) -0.015(3) -0.012(3) -0.005(3) C59 0.055(4) 0.047(4) 0.022(3) -0.014(3) -0.003(3) -0.008(3) C60 0.047(4) 0.059(5) 0.030(4) -0.007(3) 0.003(3) -0.026(4) C61 0.042(4) 0.054(5) 0.031(3) -0.010(3) -0.005(3) -0.017(3) C62 0.024(3) 0.032(3) 0.036(3) -0.013(3) -0.010(3) 0.000(2) C63 0.045(4) 0.032(4) 0.047(4) -0.010(3) -0.012(3) -0.004(3) C64 0.053(5) 0.032(4) 0.082(7) -0.013(4) -0.019(5) 0.001(4) C65 0.041(4) 0.041(5) 0.115(8) -0.044(5) -0.028(5) 0.009(4) C66 0.030(3) 0.053(5) 0.073(5) -0.042(4) -0.014(4) 0.004(3) C67 0.036(3) 0.038(4) 0.043(4) -0.018(3) -0.009(3) 0.001(3) C68 0.027(3) 0.026(3) 0.020(3) -0.004(2) -0.001(2) -0.007(2) C69 0.030(3) 0.032(3) 0.023(3) -0.012(2) -0.003(2) -0.002(3) C70 0.026(3) 0.038(4) 0.028(3) -0.008(3) -0.005(2) -0.011(3) C71 0.028(3) 0.033(3) 0.031(3) -0.004(3) -0.005(3) 0.001(3) C72 0.037(3) 0.034(3) 0.035(3) -0.015(3) -0.002(3) 0.001(3) C73 0.037(3) 0.031(3) 0.026(3) -0.012(3) -0.003(3) 0.000(3) C74 0.031(3) 0.035(3) 0.018(3) -0.005(2) -0.007(2) -0.006(3) C75 0.037(4) 0.038(4) 0.033(3) -0.010(3) -0.008(3) -0.006(3) C76 0.056(5) 0.038(4) 0.044(4) -0.004(3) -0.015(4) -0.019(4) C77 0.047(5) 0.062(5) 0.047(5) -0.004(4) -0.007(4) -0.024(4) C78 0.034(4) 0.064(5) 0.047(4) -0.011(4) -0.006(3) -0.008(4) C79 0.027(3) 0.043(4) 0.035(4) -0.009(3) -0.004(3) -0.001(3) B1 0.031(3) 0.027(3) 0.019(3) -0.005(3) -0.004(3) -0.007(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 C31 2.043(6) . ? Ir1 N41 2.090(5) . ? Ir1 N1 2.099(5) . ? Ir1 C14 2.148(7) . ? Ir1 C15 2.161(6) . ? Ir1 C13 2.164(7) . ? Ir1 C11 2.233(6) . ? Ir1 C12 2.251(6) . ? Rh1 C42 2.055(6) . ? Rh1 N3 2.082(5) . ? Rh1 N52 2.093(5) . ? Rh1 C22 2.168(6) . ? Rh1 C21 2.195(6) . ? Rh1 C25 2.200(6) . ? Rh1 C24 2.222(6) . ? Rh1 C23 2.228(6) . ? Cl1 C55 1.600(15) . ? Cl2 C55 1.617(15) . ? O1 C2 1.279(15) . ? O1 C3 1.327(18) . ? O2 C8 1.42(3) . ? O2 C9 1.46(2) . ? N1 N2 1.340(7) . ? N1 C5 1.365(7) . ? N2 N3 1.316(7) . ? N3 N4 1.350(7) . ? N4 C5 1.325(8) . ? N41 C41 1.339(8) . ? N41 C37 1.366(8) . ? N52 C48 1.356(8) . ? N52 C52 1.362(9) . ? C1 C2 1.40(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.41(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.484(9) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.52(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.47(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.416(9) . ? C11 C15 1.440(9) . ? C11 C16 1.505(9) . ? C12 C13 1.448(10) . ? C12 C17 1.504(9) . ? C13 C14 1.415(10) . ? C13 C18 1.509(10) . ? C14 C15 1.438(10) . ? C14 C19 1.512(10) . ? C15 C20 1.497(10) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.429(11) . ? C21 C25 1.430(10) . ? C21 C26 1.489(10) . ? C22 C23 1.435(10) . ? C22 C27 1.494(11) . ? C23 C24 1.400(9) . ? C23 C28 1.505(10) . ? C24 C25 1.443(9) . ? C24 C29 1.499(10) . ? C25 C30 1.501(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.377(9) . ? C31 C36 1.413(9) . ? C32 C33 1.398(9) . ? C32 H32 0.9500 . ? C33 C34 1.366(11) . ? C33 H33 0.9500 . ? C34 C35 1.380(11) . ? C34 H34 0.9500 . ? C35 C36 1.390(9) . ? C35 H35 0.9500 . ? C36 C37 1.452(9) . ? C37 C38 1.396(9) . ? C38 C39 1.380(11) . ? C38 H38 0.9500 . ? C39 C40 1.384(11) . ? C39 H39 0.9500 . ? C40 C41 1.373(10) . ? C40 H40 0.9500 . ? C41 H41 0.9500 . ? C42 C43 1.372(9) . ? C42 C47 1.394(9) . ? C43 C44 1.381(10) . ? C43 H43 0.9500 . ? C44 C45 1.394(11) . ? C44 H44 0.9500 . ? C45 C46 1.381(11) . ? C45 H45 0.9500 . ? C46 C47 1.401(9) . ? C46 H46 0.9500 . ? C47 C48 1.459(9) . ? C48 C49 1.397(9) . ? C49 C50 1.382(11) . ? C49 H49 0.9500 . ? C50 C51 1.361(12) . ? C50 H50 0.9500 . ? C51 C52 1.406(10) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 C61 1.393(9) . ? C56 C57 1.398(9) . ? C56 B1 1.639(9) . ? C57 C58 1.397(9) . ? C57 H57 0.9500 . ? C58 C59 1.351(11) . ? C58 H58 0.9500 . ? C59 C60 1.389(11) . ? C59 H59 0.9500 . ? C60 C61 1.381(10) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C63 1.394(10) . ? C62 C67 1.423(10) . ? C62 B1 1.641(10) . ? C63 C64 1.388(11) . ? C63 H63 0.9500 . ? C64 C65 1.368(14) . ? C64 H64 0.9500 . ? C65 C66 1.396(13) . ? C65 H65 0.9500 . ? C66 C67 1.374(10) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? C68 C69 1.391(8) . ? C68 C73 1.396(9) . ? C68 B1 1.664(9) . ? C69 C70 1.403(9) . ? C69 H69 0.9500 . ? C70 C71 1.384(10) . ? C70 H70 0.9500 . ? C71 C72 1.393(10) . ? C71 H71 0.9500 . ? C72 C73 1.374(10) . ? C72 H72 0.9500 . ? C73 H73 0.9500 . ? C74 C75 1.403(10) . ? C74 C79 1.404(9) . ? C74 B1 1.644(9) . ? C75 C76 1.379(10) . ? C75 H75 0.9500 . ? C76 C77 1.381(12) . ? C76 H76 0.9500 . ? C77 C78 1.375(13) . ? C77 H77 0.9500 . ? C78 C79 1.377(10) . ? C78 H78 0.9500 . ? C79 H79 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 C31 Ir1 N41 78.6(2) . . ? C31 Ir1 N1 92.3(2) . . ? N41 Ir1 N1 88.15(19) . . ? C31 Ir1 C14 95.4(2) . . ? N41 Ir1 C14 126.8(3) . . ? N1 Ir1 C14 145.0(3) . . ? C31 Ir1 C15 108.8(3) . . ? N41 Ir1 C15 162.9(2) . . ? N1 Ir1 C15 106.5(2) . . ? C14 Ir1 C15 39.0(3) . . ? C31 Ir1 C13 116.8(3) . . ? N41 Ir1 C13 97.9(2) . . ? N1 Ir1 C13 151.0(2) . . ? C14 Ir1 C13 38.3(3) . . ? C15 Ir1 C13 65.1(3) . . ? C31 Ir1 C11 146.2(2) . . ? N41 Ir1 C11 135.0(2) . . ? N1 Ir1 C11 92.5(2) . . ? C14 Ir1 C11 63.3(3) . . ? C15 Ir1 C11 38.2(2) . . ? C13 Ir1 C11 63.3(2) . . ? C31 Ir1 C12 154.9(2) . . ? N41 Ir1 C12 102.9(2) . . ? N1 Ir1 C12 112.8(2) . . ? C14 Ir1 C12 63.3(3) . . ? C15 Ir1 C12 63.7(3) . . ? C13 Ir1 C12 38.2(3) . . ? C11 Ir1 C12 36.8(2) . . ? C42 Rh1 N3 84.9(2) . . ? C42 Rh1 N52 78.5(2) . . ? N3 Rh1 N52 87.4(2) . . ? C42 Rh1 C22 116.2(3) . . ? N3 Rh1 C22 158.4(2) . . ? N52 Rh1 C22 100.9(2) . . ? C42 Rh1 C21 96.4(2) . . ? N3 Rh1 C21 140.8(2) . . ? N52 Rh1 C21 131.4(3) . . ? C22 Rh1 C21 38.2(3) . . ? C42 Rh1 C25 110.9(2) . . ? N3 Rh1 C25 105.2(2) . . ? N52 Rh1 C25 164.6(2) . . ? C22 Rh1 C25 64.2(3) . . ? C21 Rh1 C25 38.0(3) . . ? C42 Rh1 C24 148.3(2) . . ? N3 Rh1 C24 96.9(2) . . ? N52 Rh1 C24 133.1(2) . . ? C22 Rh1 C24 62.9(3) . . ? C21 Rh1 C24 62.7(2) . . ? C25 Rh1 C24 38.1(2) . . ? C42 Rh1 C23 154.2(3) . . ? N3 Rh1 C23 120.8(2) . . ? N52 Rh1 C23 102.8(2) . . ? C22 Rh1 C23 38.1(3) . . ? C21 Rh1 C23 63.0(3) . . ? C25 Rh1 C23 63.3(2) . . ? C24 Rh1 C23 36.7(2) . . ? C2 O1 C3 116.6(16) . . ? C8 O2 C9 141(3) . . ? N2 N1 C5 106.7(5) . . ? N2 N1 Ir1 117.4(4) . . ? C5 N1 Ir1 133.5(4) . . ? N3 N2 N1 106.6(5) . . ? N2 N3 N4 112.1(5) . . ? N2 N3 Rh1 126.5(4) . . ? N4 N3 Rh1 121.1(4) . . ? C5 N4 N3 104.2(5) . . ? C41 N41 C37 118.5(6) . . ? C41 N41 Ir1 125.1(4) . . ? C37 N41 Ir1 116.2(4) . . ? C48 N52 C52 120.0(6) . . ? C48 N52 Rh1 115.9(4) . . ? C52 N52 Rh1 124.0(5) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C1 117.0(13) . . ? O1 C2 H2A 108.0 . . ? C1 C2 H2A 108.0 . . ? O1 C2 H2B 108.0 . . ? C1 C2 H2B 108.0 . . ? H2A C2 H2B 107.3 . . ? O1 C3 C4 111(2) . . ? O1 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? O1 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N4 C5 N1 110.3(5) . . ? N4 C5 C6 123.0(5) . . ? N1 C5 C6 126.7(6) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O2 C8 C7 112(4) . . ? O2 C8 H8A 109.2 . . ? C7 C8 H8A 109.2 . . ? O2 C8 H8B 109.2 . . ? C7 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? O2 C9 C10 118(2) . . ? O2 C9 H9A 107.7 . . ? C10 C9 H9A 107.7 . . ? O2 C9 H9B 107.7 . . ? C10 C9 H9B 107.7 . . ? H9A C9 H9B 107.1 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C15 109.3(6) . . ? C12 C11 C16 125.0(7) . . ? C15 C11 C16 125.7(7) . . ? C12 C11 Ir1 72.3(4) . . ? C15 C11 Ir1 68.2(3) . . ? C16 C11 Ir1 124.9(5) . . ? C11 C12 C13 107.4(6) . . ? C11 C12 C17 127.3(7) . . ? C13 C12 C17 125.1(7) . . ? C11 C12 Ir1 70.9(4) . . ? C13 C12 Ir1 67.6(4) . . ? C17 C12 Ir1 130.7(5) . . ? C14 C13 C12 107.6(6) . . ? C14 C13 C18 127.0(7) . . ? C12 C13 C18 125.0(7) . . ? C14 C13 Ir1 70.2(4) . . ? C12 C13 Ir1 74.1(4) . . ? C18 C13 Ir1 126.6(5) . . ? C13 C14 C15 109.3(6) . . ? C13 C14 C19 125.7(7) . . ? C15 C14 C19 124.8(7) . . ? C13 C14 Ir1 71.5(4) . . ? C15 C14 Ir1 71.0(4) . . ? C19 C14 Ir1 127.6(5) . . ? C14 C15 C11 106.2(6) . . ? C14 C15 C20 127.9(7) . . ? C11 C15 C20 125.1(7) . . ? C14 C15 Ir1 70.0(4) . . ? C11 C15 Ir1 73.6(4) . . ? C20 C15 Ir1 129.4(5) . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C12 C17 H17A 109.5 . . ? C12 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C12 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C25 108.6(6) . . ? C22 C21 C26 127.0(7) . . ? C25 C21 C26 124.3(8) . . ? C22 C21 Rh1 69.9(4) . . ? C25 C21 Rh1 71.2(3) . . ? C26 C21 Rh1 127.4(5) . . ? C21 C22 C23 107.7(6) . . ? C21 C22 C27 127.3(7) . . ? C23 C22 C27 124.7(7) . . ? C21 C22 Rh1 71.9(4) . . ? C23 C22 Rh1 73.2(4) . . ? C27 C22 Rh1 125.5(5) . . ? C24 C23 C22 107.8(6) . . ? C24 C23 C28 126.4(7) . . ? C22 C23 C28 125.5(7) . . ? C24 C23 Rh1 71.4(4) . . ? C22 C23 Rh1 68.7(4) . . ? C28 C23 Rh1 130.4(5) . . ? C23 C24 C25 109.6(6) . . ? C23 C24 C29 126.5(6) . . ? C25 C24 C29 123.9(6) . . ? C23 C24 Rh1 71.9(4) . . ? C25 C24 Rh1 70.2(3) . . ? C29 C24 Rh1 124.6(5) . . ? C21 C25 C24 106.2(6) . . ? C21 C25 C30 127.6(7) . . ? C24 C25 C30 125.9(7) . . ? C21 C25 Rh1 70.8(4) . . ? C24 C25 Rh1 71.8(3) . . ? C30 C25 Rh1 127.0(5) . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C24 C29 H29A 109.5 . . ? C24 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C24 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 C36 117.3(5) . . ? C32 C31 Ir1 127.6(5) . . ? C36 C31 Ir1 115.0(4) . . ? C31 C32 C33 121.5(6) . . ? C31 C32 H32 119.2 . . ? C33 C32 H32 119.2 . . ? C34 C33 C32 119.9(6) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.5(6) . . ? C33 C34 H34 119.7 . . ? C35 C34 H34 119.7 . . ? C34 C35 C36 119.5(7) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C31 121.1(6) . . ? C35 C36 C37 123.1(6) . . ? C31 C36 C37 115.7(6) . . ? N41 C37 C38 119.9(6) . . ? N41 C37 C36 113.9(6) . . ? C38 C37 C36 126.2(6) . . ? C39 C38 C37 120.4(7) . . ? C39 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? C38 C39 C40 119.0(7) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C41 C40 C39 118.1(7) . . ? C41 C40 H40 120.9 . . ? C39 C40 H40 120.9 . . ? N41 C41 C40 123.9(6) . . ? N41 C41 H41 118.0 . . ? C40 C41 H41 118.0 . . ? C43 C42 C47 119.5(6) . . ? C43 C42 Rh1 125.2(5) . . ? C47 C42 Rh1 115.2(4) . . ? C42 C43 C44 121.4(7) . . ? C42 C43 H43 119.3 . . ? C44 C43 H43 119.3 . . ? C43 C44 C45 119.2(7) . . ? C43 C44 H44 120.4 . . ? C45 C44 H44 120.4 . . ? C46 C45 C44 120.3(6) . . ? C46 C45 H45 119.9 . . ? C44 C45 H45 119.9 . . ? C45 C46 C47 119.8(7) . . ? C45 C46 H46 120.1 . . ? C47 C46 H46 120.1 . . ? C42 C47 C46 119.6(6) . . ? C42 C47 C48 115.4(6) . . ? C46 C47 C48 124.9(6) . . ? N52 C48 C49 119.8(6) . . ? N52 C48 C47 114.8(5) . . ? C49 C48 C47 125.3(6) . . ? C50 C49 C48 120.8(7) . . ? C50 C49 H49 119.6 . . ? C48 C49 H49 119.6 . . ? C51 C50 C49 119.0(6) . . ? C51 C50 H50 120.5 . . ? C49 C50 H50 120.5 . . ? C50 C51 C52 119.9(7) . . ? C50 C51 H51 120.1 . . ? C52 C51 H51 120.1 . . ? N52 C52 C51 120.6(7) . . ? N52 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? Cl1 C55 Cl2 121.2(15) . . ? Cl1 C55 H55A 107.0 . . ? Cl2 C55 H55A 107.0 . . ? Cl1 C55 H55B 107.0 . . ? Cl2 C55 H55B 107.0 . . ? H55A C55 H55B 106.8 . . ? C61 C56 C57 114.8(6) . . ? C61 C56 B1 121.5(6) . . ? C57 C56 B1 123.7(6) . . ? C56 C57 C58 122.1(7) . . ? C56 C57 H57 118.9 . . ? C58 C57 H57 118.9 . . ? C59 C58 C57 121.1(7) . . ? C59 C58 H58 119.4 . . ? C57 C58 H58 119.4 . . ? C58 C59 C60 118.8(6) . . ? C58 C59 H59 120.6 . . ? C60 C59 H59 120.6 . . ? C61 C60 C59 119.7(7) . . ? C61 C60 H60 120.2 . . ? C59 C60 H60 120.2 . . ? C60 C61 C56 123.5(7) . . ? C60 C61 H61 118.2 . . ? C56 C61 H61 118.2 . . ? C63 C62 C67 114.4(6) . . ? C63 C62 B1 124.3(6) . . ? C67 C62 B1 121.2(6) . . ? C64 C63 C62 124.2(8) . . ? C64 C63 H63 117.9 . . ? C62 C63 H63 117.9 . . ? C65 C64 C63 119.1(8) . . ? C65 C64 H64 120.4 . . ? C63 C64 H64 120.4 . . ? C64 C65 C66 119.6(8) . . ? C64 C65 H65 120.2 . . ? C66 C65 H65 120.2 . . ? C67 C66 C65 120.4(8) . . ? C67 C66 H66 119.8 . . ? C65 C66 H66 119.8 . . ? C66 C67 C62 122.2(7) . . ? C66 C67 H67 118.9 . . ? C62 C67 H67 118.9 . . ? C69 C68 C73 115.2(6) . . ? C69 C68 B1 124.6(6) . . ? C73 C68 B1 120.2(5) . . ? C68 C69 C70 122.6(6) . . ? C68 C69 H69 118.7 . . ? C70 C69 H69 118.7 . . ? C71 C70 C69 120.5(6) . . ? C71 C70 H70 119.7 . . ? C69 C70 H70 119.7 . . ? C70 C71 C72 117.5(6) . . ? C70 C71 H71 121.2 . . ? C72 C71 H71 121.2 . . ? C73 C72 C71 121.1(6) . . ? C73 C72 H72 119.5 . . ? C71 C72 H72 119.5 . . ? C72 C73 C68 123.1(6) . . ? C72 C73 H73 118.5 . . ? C68 C73 H73 118.5 . . ? C75 C74 C79 113.9(6) . . ? C75 C74 B1 123.7(6) . . ? C79 C74 B1 122.2(6) . . ? C76 C75 C74 123.6(7) . . ? C76 C75 H75 118.2 . . ? C74 C75 H75 118.2 . . ? C75 C76 C77 120.2(8) . . ? C75 C76 H76 119.9 . . ? C77 C76 H76 119.9 . . ? C78 C77 C76 118.4(7) . . ? C78 C77 H77 120.8 . . ? C76 C77 H77 120.8 . . ? C77 C78 C79 120.8(8) . . ? C77 C78 H78 119.6 . . ? C79 C78 H78 119.6 . . ? C78 C79 C74 123.2(7) . . ? C78 C79 H79 118.4 . . ? C74 C79 H79 118.4 . . ? C56 B1 C62 109.3(5) . . ? C56 B1 C74 108.8(5) . . ? C62 B1 C74 109.4(5) . . ? C56 B1 C68 108.1(5) . . ? C62 B1 C68 111.5(5) . . ? C74 B1 C68 109.7(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 C31 Ir1 N1 N2 -134.1(4) . . . . ? N41 Ir1 N1 N2 -55.5(4) . . . . ? C14 Ir1 N1 N2 123.2(5) . . . . ? C15 Ir1 N1 N2 115.6(4) . . . . ? C13 Ir1 N1 N2 47.4(7) . . . . ? C11 Ir1 N1 N2 79.4(4) . . . . ? C12 Ir1 N1 N2 47.7(5) . . . . ? C31 Ir1 N1 C5 66.3(5) . . . . ? N41 Ir1 N1 C5 144.8(5) . . . . ? C14 Ir1 N1 C5 -36.4(7) . . . . ? C15 Ir1 N1 C5 -44.1(6) . . . . ? C13 Ir1 N1 C5 -112.3(6) . . . . ? C11 Ir1 N1 C5 -80.3(6) . . . . ? C12 Ir1 N1 C5 -112.0(5) . . . . ? C5 N1 N2 N3 -1.7(6) . . . . ? Ir1 N1 N2 N3 -166.4(4) . . . . ? N1 N2 N3 N4 0.9(6) . . . . ? N1 N2 N3 Rh1 174.3(4) . . . . ? C42 Rh1 N3 N2 -76.4(5) . . . . ? N52 Rh1 N3 N2 2.4(5) . . . . ? C22 Rh1 N3 N2 116.0(7) . . . . ? C21 Rh1 N3 N2 -170.2(5) . . . . ? C25 Rh1 N3 N2 173.4(5) . . . . ? C24 Rh1 N3 N2 135.4(5) . . . . ? C23 Rh1 N3 N2 105.8(5) . . . . ? C42 Rh1 N3 N4 96.5(5) . . . . ? N52 Rh1 N3 N4 175.3(4) . . . . ? C22 Rh1 N3 N4 -71.1(8) . . . . ? C21 Rh1 N3 N4 2.7(6) . . . . ? C25 Rh1 N3 N4 -13.7(5) . . . . ? C24 Rh1 N3 N4 -51.6(5) . . . . ? C23 Rh1 N3 N4 -81.3(5) . . . . ? N2 N3 N4 C5 0.4(7) . . . . ? Rh1 N3 N4 C5 -173.5(4) . . . . ? C31 Ir1 N41 C41 177.5(6) . . . . ? N1 Ir1 N41 C41 84.8(5) . . . . ? C14 Ir1 N41 C41 -94.3(6) . . . . ? C15 Ir1 N41 C41 -64.9(10) . . . . ? C13 Ir1 N41 C41 -66.7(6) . . . . ? C11 Ir1 N41 C41 -6.9(7) . . . . ? C12 Ir1 N41 C41 -28.1(6) . . . . ? C31 Ir1 N41 C37 -6.6(4) . . . . ? N1 Ir1 N41 C37 -99.3(4) . . . . ? C14 Ir1 N41 C37 81.6(5) . . . . ? C15 Ir1 N41 C37 111.0(8) . . . . ? C13 Ir1 N41 C37 109.2(5) . . . . ? C11 Ir1 N41 C37 169.0(4) . . . . ? C12 Ir1 N41 C37 147.8(5) . . . . ? C42 Rh1 N52 C48 -2.3(5) . . . . ? N3 Rh1 N52 C48 -87.5(5) . . . . ? C22 Rh1 N52 C48 112.5(5) . . . . ? C21 Rh1 N52 C48 86.2(5) . . . . ? C25 Rh1 N52 C48 127.0(9) . . . . ? C24 Rh1 N52 C48 175.5(4) . . . . ? C23 Rh1 N52 C48 151.4(5) . . . . ? C42 Rh1 N52 C52 174.0(6) . . . . ? N3 Rh1 N52 C52 88.7(5) . . . . ? C22 Rh1 N52 C52 -71.2(6) . . . . ? C21 Rh1 N52 C52 -97.5(6) . . . . ? C25 Rh1 N52 C52 -56.8(11) . . . . ? C24 Rh1 N52 C52 -8.3(7) . . . . ? C23 Rh1 N52 C52 -32.4(6) . . . . ? C3 O1 C2 C1 -170(2) . . . . ? C2 O1 C3 C4 -165(3) . . . . ? N3 N4 C5 N1 -1.5(6) . . . . ? N3 N4 C5 C6 179.3(5) . . . . ? N2 N1 C5 N4 2.0(7) . . . . ? Ir1 N1 C5 N4 163.2(4) . . . . ? N2 N1 C5 C6 -178.8(6) . . . . ? Ir1 N1 C5 C6 -17.6(9) . . . . ? C9 O2 C8 C7 175(3) . . . . ? C8 O2 C9 C10 -161(3) . . . . ? C31 Ir1 C11 C12 136.2(5) . . . . ? N41 Ir1 C11 C12 -36.1(5) . . . . ? N1 Ir1 C11 C12 -126.0(4) . . . . ? C14 Ir1 C11 C12 80.4(4) . . . . ? C15 Ir1 C11 C12 120.2(6) . . . . ? C13 Ir1 C11 C12 37.3(4) . . . . ? C31 Ir1 C11 C15 16.0(6) . . . . ? N41 Ir1 C11 C15 -156.3(4) . . . . ? N1 Ir1 C11 C15 113.8(4) . . . . ? C14 Ir1 C11 C15 -39.8(4) . . . . ? C13 Ir1 C11 C15 -82.9(4) . . . . ? C12 Ir1 C11 C15 -120.2(6) . . . . ? C31 Ir1 C11 C16 -103.1(7) . . . . ? N41 Ir1 C11 C16 84.6(7) . . . . ? N1 Ir1 C11 C16 -5.3(6) . . . . ? C14 Ir1 C11 C16 -158.9(7) . . . . ? C15 Ir1 C11 C16 -119.1(8) . . . . ? C13 Ir1 C11 C16 158.0(7) . . . . ? C12 Ir1 C11 C16 120.7(8) . . . . ? C15 C11 C12 C13 0.3(7) . . . . ? C16 C11 C12 C13 -178.6(6) . . . . ? Ir1 C11 C12 C13 -58.0(5) . . . . ? C15 C11 C12 C17 -174.6(7) . . . . ? C16 C11 C12 C17 6.5(11) . . . . ? Ir1 C11 C12 C17 127.1(7) . . . . ? C15 C11 C12 Ir1 58.3(4) . . . . ? C16 C11 C12 Ir1 -120.7(7) . . . . ? C31 Ir1 C12 C11 -114.6(6) . . . . ? N41 Ir1 C12 C11 154.7(4) . . . . ? N1 Ir1 C12 C11 61.2(4) . . . . ? C14 Ir1 C12 C11 -80.4(4) . . . . ? C15 Ir1 C12 C11 -36.6(4) . . . . ? C13 Ir1 C12 C11 -119.0(6) . . . . ? C31 Ir1 C12 C13 4.4(8) . . . . ? N41 Ir1 C12 C13 -86.3(4) . . . . ? N1 Ir1 C12 C13 -179.8(4) . . . . ? C14 Ir1 C12 C13 38.6(4) . . . . ? C15 Ir1 C12 C13 82.4(4) . . . . ? C11 Ir1 C12 C13 119.0(6) . . . . ? C31 Ir1 C12 C17 122.1(8) . . . . ? N41 Ir1 C12 C17 31.4(8) . . . . ? N1 Ir1 C12 C17 -62.0(8) . . . . ? C14 Ir1 C12 C17 156.3(8) . . . . ? C15 Ir1 C12 C17 -159.9(8) . . . . ? C13 Ir1 C12 C17 117.7(9) . . . . ? C11 Ir1 C12 C17 -123.3(9) . . . . ? C11 C12 C13 C14 -2.6(8) . . . . ? C17 C12 C13 C14 172.4(7) . . . . ? Ir1 C12 C13 C14 -62.7(5) . . . . ? C11 C12 C13 C18 -176.0(7) . . . . ? C17 C12 C13 C18 -1.0(12) . . . . ? Ir1 C12 C13 C18 123.9(8) . . . . ? C11 C12 C13 Ir1 60.0(5) . . . . ? C17 C12 C13 Ir1 -124.9(7) . . . . ? C31 Ir1 C13 C14 -62.0(5) . . . . ? N41 Ir1 C13 C14 -143.2(4) . . . . ? N1 Ir1 C13 C14 116.3(5) . . . . ? C15 Ir1 C13 C14 37.4(4) . . . . ? C11 Ir1 C13 C14 80.0(4) . . . . ? C12 Ir1 C13 C14 115.9(6) . . . . ? C31 Ir1 C13 C12 -177.9(4) . . . . ? N41 Ir1 C13 C12 100.9(4) . . . . ? N1 Ir1 C13 C12 0.4(7) . . . . ? C14 Ir1 C13 C12 -115.9(6) . . . . ? C15 Ir1 C13 C12 -78.5(4) . . . . ? C11 Ir1 C13 C12 -35.9(4) . . . . ? C31 Ir1 C13 C18 60.0(8) . . . . ? N41 Ir1 C13 C18 -21.2(7) . . . . ? N1 Ir1 C13 C18 -121.6(7) . . . . ? C14 Ir1 C13 C18 122.0(9) . . . . ? C15 Ir1 C13 C18 159.4(8) . . . . ? C11 Ir1 C13 C18 -158.0(8) . . . . ? C12 Ir1 C13 C18 -122.1(9) . . . . ? C12 C13 C14 C15 4.0(8) . . . . ? C18 C13 C14 C15 177.2(7) . . . . ? Ir1 C13 C14 C15 -61.3(5) . . . . ? C12 C13 C14 C19 -171.3(7) . . . . ? C18 C13 C14 C19 1.9(12) . . . . ? Ir1 C13 C14 C19 123.4(7) . . . . ? C12 C13 C14 Ir1 65.2(5) . . . . ? C18 C13 C14 Ir1 -121.5(8) . . . . ? C31 Ir1 C14 C13 127.6(4) . . . . ? N41 Ir1 C14 C13 47.8(5) . . . . ? N1 Ir1 C14 C13 -130.6(4) . . . . ? C15 Ir1 C14 C13 -118.9(6) . . . . ? C11 Ir1 C14 C13 -79.9(4) . . . . ? C12 Ir1 C14 C13 -38.5(4) . . . . ? C31 Ir1 C14 C15 -113.4(4) . . . . ? N41 Ir1 C14 C15 166.8(4) . . . . ? N1 Ir1 C14 C15 -11.7(6) . . . . ? C13 Ir1 C14 C15 118.9(6) . . . . ? C11 Ir1 C14 C15 39.0(4) . . . . ? C12 Ir1 C14 C15 80.4(4) . . . . ? C31 Ir1 C14 C19 6.3(8) . . . . ? N41 Ir1 C14 C19 -73.5(8) . . . . ? N1 Ir1 C14 C19 108.1(8) . . . . ? C15 Ir1 C14 C19 119.8(9) . . . . ? C13 Ir1 C14 C19 -121.3(9) . . . . ? C11 Ir1 C14 C19 158.8(8) . . . . ? C12 Ir1 C14 C19 -159.8(8) . . . . ? C13 C14 C15 C11 -3.7(7) . . . . ? C19 C14 C15 C11 171.6(7) . . . . ? Ir1 C14 C15 C11 -65.3(4) . . . . ? C13 C14 C15 C20 -173.5(7) . . . . ? C19 C14 C15 C20 1.8(11) . . . . ? Ir1 C14 C15 C20 124.9(7) . . . . ? C13 C14 C15 Ir1 61.5(5) . . . . ? C19 C14 C15 Ir1 -123.1(7) . . . . ? C12 C11 C15 C14 2.1(7) . . . . ? C16 C11 C15 C14 -179.0(7) . . . . ? Ir1 C11 C15 C14 62.8(4) . . . . ? C12 C11 C15 C20 172.2(6) . . . . ? C16 C11 C15 C20 -8.8(11) . . . . ? Ir1 C11 C15 C20 -127.0(7) . . . . ? C12 C11 C15 Ir1 -60.8(5) . . . . ? C16 C11 C15 Ir1 118.2(7) . . . . ? C31 Ir1 C15 C14 74.8(4) . . . . ? N41 Ir1 C15 C14 -38.7(10) . . . . ? N1 Ir1 C15 C14 173.0(4) . . . . ? C13 Ir1 C15 C14 -36.7(4) . . . . ? C11 Ir1 C15 C14 -114.6(6) . . . . ? C12 Ir1 C15 C14 -79.3(4) . . . . ? C31 Ir1 C15 C11 -170.7(4) . . . . ? N41 Ir1 C15 C11 75.9(9) . . . . ? N1 Ir1 C15 C11 -72.4(4) . . . . ? C14 Ir1 C15 C11 114.6(6) . . . . ? C13 Ir1 C15 C11 77.8(4) . . . . ? C12 Ir1 C15 C11 35.3(4) . . . . ? C31 Ir1 C15 C20 -48.4(7) . . . . ? N41 Ir1 C15 C20 -161.9(7) . . . . ? N1 Ir1 C15 C20 49.9(7) . . . . ? C14 Ir1 C15 C20 -123.2(9) . . . . ? C13 Ir1 C15 C20 -159.9(8) . . . . ? C11 Ir1 C15 C20 122.3(9) . . . . ? C12 Ir1 C15 C20 157.5(8) . . . . ? C42 Rh1 C21 C22 125.1(4) . . . . ? N3 Rh1 C21 C22 -145.2(4) . . . . ? N52 Rh1 C21 C22 44.7(5) . . . . ? C25 Rh1 C21 C22 -119.0(6) . . . . ? C24 Rh1 C21 C22 -80.0(4) . . . . ? C23 Rh1 C21 C22 -38.6(4) . . . . ? C42 Rh1 C21 C25 -116.0(4) . . . . ? N3 Rh1 C21 C25 -26.2(6) . . . . ? N52 Rh1 C21 C25 163.6(4) . . . . ? C22 Rh1 C21 C25 119.0(6) . . . . ? C24 Rh1 C21 C25 38.9(4) . . . . ? C23 Rh1 C21 C25 80.4(4) . . . . ? C42 Rh1 C21 C26 3.3(8) . . . . ? N3 Rh1 C21 C26 93.1(8) . . . . ? N52 Rh1 C21 C26 -77.0(9) . . . . ? C22 Rh1 C21 C26 -121.7(9) . . . . ? C25 Rh1 C21 C26 119.3(9) . . . . ? C24 Rh1 C21 C26 158.2(9) . . . . ? C23 Rh1 C21 C26 -160.3(9) . . . . ? C25 C21 C22 C23 4.1(7) . . . . ? C26 C21 C22 C23 -172.8(7) . . . . ? Rh1 C21 C22 C23 65.0(4) . . . . ? C25 C21 C22 C27 177.8(7) . . . . ? C26 C21 C22 C27 0.9(11) . . . . ? Rh1 C21 C22 C27 -121.3(7) . . . . ? C25 C21 C22 Rh1 -60.9(4) . . . . ? C26 C21 C22 Rh1 122.2(7) . . . . ? C42 Rh1 C22 C21 -65.0(4) . . . . ? N3 Rh1 C22 C21 101.2(7) . . . . ? N52 Rh1 C22 C21 -147.5(4) . . . . ? C25 Rh1 C22 C21 36.7(4) . . . . ? C24 Rh1 C22 C21 79.4(4) . . . . ? C23 Rh1 C22 C21 115.6(6) . . . . ? C42 Rh1 C22 C23 179.4(4) . . . . ? N3 Rh1 C22 C23 -14.3(9) . . . . ? N52 Rh1 C22 C23 96.9(4) . . . . ? C21 Rh1 C22 C23 -115.6(6) . . . . ? C25 Rh1 C22 C23 -78.9(4) . . . . ? C24 Rh1 C22 C23 -36.1(4) . . . . ? C42 Rh1 C22 C27 58.4(8) . . . . ? N3 Rh1 C22 C27 -135.4(7) . . . . ? N52 Rh1 C22 C27 -24.1(8) . . . . ? C21 Rh1 C22 C27 123.4(9) . . . . ? C25 Rh1 C22 C27 160.1(8) . . . . ? C24 Rh1 C22 C27 -157.2(8) . . . . ? C23 Rh1 C22 C27 -121.0(9) . . . . ? C21 C22 C23 C24 -3.1(7) . . . . ? C27 C22 C23 C24 -177.0(6) . . . . ? Rh1 C22 C23 C24 61.0(4) . . . . ? C21 C22 C23 C28 170.7(6) . . . . ? C27 C22 C23 C28 -3.2(10) . . . . ? Rh1 C22 C23 C28 -125.1(6) . . . . ? C21 C22 C23 Rh1 -64.1(4) . . . . ? C27 C22 C23 Rh1 122.0(7) . . . . ? C42 Rh1 C23 C24 -119.7(6) . . . . ? N3 Rh1 C23 C24 55.4(4) . . . . ? N52 Rh1 C23 C24 150.1(4) . . . . ? C22 Rh1 C23 C24 -118.5(6) . . . . ? C21 Rh1 C23 C24 -79.7(4) . . . . ? C25 Rh1 C23 C24 -36.9(4) . . . . ? C42 Rh1 C23 C22 -1.2(7) . . . . ? N3 Rh1 C23 C22 173.9(4) . . . . ? N52 Rh1 C23 C22 -91.4(4) . . . . ? C21 Rh1 C23 C22 38.8(4) . . . . ? C25 Rh1 C23 C22 81.6(4) . . . . ? C24 Rh1 C23 C22 118.5(6) . . . . ? C42 Rh1 C23 C28 117.8(8) . . . . ? N3 Rh1 C23 C28 -67.0(8) . . . . ? N52 Rh1 C23 C28 27.7(8) . . . . ? C22 Rh1 C23 C28 119.1(9) . . . . ? C21 Rh1 C23 C28 157.8(8) . . . . ? C25 Rh1 C23 C28 -159.4(8) . . . . ? C24 Rh1 C23 C28 -122.5(9) . . . . ? C22 C23 C24 C25 1.0(7) . . . . ? C28 C23 C24 C25 -172.8(6) . . . . ? Rh1 C23 C24 C25 60.3(4) . . . . ? C22 C23 C24 C29 -179.4(6) . . . . ? C28 C23 C24 C29 6.8(10) . . . . ? Rh1 C23 C24 C29 -120.1(6) . . . . ? C22 C23 C24 Rh1 -59.3(4) . . . . ? C28 C23 C24 Rh1 126.9(7) . . . . ? C42 Rh1 C24 C23 134.1(5) . . . . ? N3 Rh1 C24 C23 -134.6(4) . . . . ? N52 Rh1 C24 C23 -41.7(5) . . . . ? C22 Rh1 C24 C23 37.5(4) . . . . ? C21 Rh1 C24 C23 80.7(4) . . . . ? C25 Rh1 C24 C23 119.5(6) . . . . ? C42 Rh1 C24 C25 14.5(7) . . . . ? N3 Rh1 C24 C25 105.9(4) . . . . ? N52 Rh1 C24 C25 -161.2(4) . . . . ? C22 Rh1 C24 C25 -82.0(5) . . . . ? C21 Rh1 C24 C25 -38.8(4) . . . . ? C23 Rh1 C24 C25 -119.5(6) . . . . ? C42 Rh1 C24 C29 -103.6(7) . . . . ? N3 Rh1 C24 C29 -12.3(6) . . . . ? N52 Rh1 C24 C29 80.6(7) . . . . ? C22 Rh1 C24 C29 159.8(7) . . . . ? C21 Rh1 C24 C29 -157.0(7) . . . . ? C25 Rh1 C24 C29 -118.1(8) . . . . ? C23 Rh1 C24 C29 122.3(8) . . . . ? C22 C21 C25 C24 -3.4(7) . . . . ? C26 C21 C25 C24 173.5(6) . . . . ? Rh1 C21 C25 C24 -63.5(4) . . . . ? C22 C21 C25 C30 -177.5(6) . . . . ? C26 C21 C25 C30 -0.5(11) . . . . ? Rh1 C21 C25 C30 122.4(7) . . . . ? C22 C21 C25 Rh1 60.1(4) . . . . ? C26 C21 C25 Rh1 -123.0(7) . . . . ? C23 C24 C25 C21 1.5(7) . . . . ? C29 C24 C25 C21 -178.1(6) . . . . ? Rh1 C24 C25 C21 62.9(4) . . . . ? C23 C24 C25 C30 175.7(6) . . . . ? C29 C24 C25 C30 -4.0(10) . . . . ? Rh1 C24 C25 C30 -122.9(7) . . . . ? C23 C24 C25 Rh1 -61.4(4) . . . . ? C29 C24 C25 Rh1 119.0(6) . . . . ? C42 Rh1 C25 C21 72.9(4) . . . . ? N3 Rh1 C25 C21 163.2(4) . . . . ? N52 Rh1 C25 C21 -52.8(11) . . . . ? C22 Rh1 C25 C21 -37.0(4) . . . . ? C24 Rh1 C25 C21 -115.2(6) . . . . ? C23 Rh1 C25 C21 -79.6(4) . . . . ? C42 Rh1 C25 C24 -171.9(4) . . . . ? N3 Rh1 C25 C24 -81.7(4) . . . . ? N52 Rh1 C25 C24 62.4(11) . . . . ? C22 Rh1 C25 C24 78.2(4) . . . . ? C21 Rh1 C25 C24 115.2(6) . . . . ? C23 Rh1 C25 C24 35.6(4) . . . . ? C42 Rh1 C25 C30 -50.2(7) . . . . ? N3 Rh1 C25 C30 40.0(7) . . . . ? N52 Rh1 C25 C30 -175.9(8) . . . . ? C22 Rh1 C25 C30 -160.1(8) . . . . ? C21 Rh1 C25 C30 -123.2(9) . . . . ? C24 Rh1 C25 C30 121.7(9) . . . . ? C23 Rh1 C25 C30 157.2(8) . . . . ? N41 Ir1 C31 C32 -177.9(6) . . . . ? N1 Ir1 C31 C32 -90.2(6) . . . . ? C14 Ir1 C31 C32 55.6(6) . . . . ? C15 Ir1 C31 C32 18.1(6) . . . . ? C13 Ir1 C31 C32 89.0(6) . . . . ? C11 Ir1 C31 C32 7.7(8) . . . . ? C12 Ir1 C31 C32 86.0(8) . . . . ? N41 Ir1 C31 C36 5.3(4) . . . . ? N1 Ir1 C31 C36 93.0(5) . . . . ? C14 Ir1 C31 C36 -121.2(5) . . . . ? C15 Ir1 C31 C36 -158.7(4) . . . . ? C13 Ir1 C31 C36 -87.8(5) . . . . ? C11 Ir1 C31 C36 -169.1(4) . . . . ? C12 Ir1 C31 C36 -90.8(7) . . . . ? C36 C31 C32 C33 -1.8(9) . . . . ? Ir1 C31 C32 C33 -178.5(5) . . . . ? C31 C32 C33 C34 2.0(11) . . . . ? C32 C33 C34 C35 -1.0(11) . . . . ? C33 C34 C35 C36 -0.1(11) . . . . ? C34 C35 C36 C31 0.3(10) . . . . ? C34 C35 C36 C37 -178.2(6) . . . . ? C32 C31 C36 C35 0.6(9) . . . . ? Ir1 C31 C36 C35 177.8(5) . . . . ? C32 C31 C36 C37 179.2(6) . . . . ? Ir1 C31 C36 C37 -3.6(7) . . . . ? C41 N41 C37 C38 2.6(9) . . . . ? Ir1 N41 C37 C38 -173.6(5) . . . . ? C41 N41 C37 C36 -177.3(6) . . . . ? Ir1 N41 C37 C36 6.5(7) . . . . ? C35 C36 C37 N41 176.6(6) . . . . ? C31 C36 C37 N41 -1.9(8) . . . . ? C35 C36 C37 C38 -3.3(11) . . . . ? C31 C36 C37 C38 178.2(7) . . . . ? N41 C37 C38 C39 -0.3(11) . . . . ? C36 C37 C38 C39 179.6(7) . . . . ? C37 C38 C39 C40 -1.2(12) . . . . ? C38 C39 C40 C41 0.4(12) . . . . ? C37 N41 C41 C40 -3.7(10) . . . . ? Ir1 N41 C41 C40 172.2(6) . . . . ? C39 C40 C41 N41 2.1(12) . . . . ? N3 Rh1 C42 C43 -85.3(6) . . . . ? N52 Rh1 C42 C43 -173.7(6) . . . . ? C22 Rh1 C42 C43 89.6(6) . . . . ? C21 Rh1 C42 C43 55.3(6) . . . . ? C25 Rh1 C42 C43 19.0(6) . . . . ? C24 Rh1 C42 C43 9.4(8) . . . . ? C23 Rh1 C42 C43 90.5(8) . . . . ? N3 Rh1 C42 C47 92.1(5) . . . . ? N52 Rh1 C42 C47 3.7(4) . . . . ? C22 Rh1 C42 C47 -93.0(5) . . . . ? C21 Rh1 C42 C47 -127.4(5) . . . . ? C25 Rh1 C42 C47 -163.7(5) . . . . ? C24 Rh1 C42 C47 -173.2(4) . . . . ? C23 Rh1 C42 C47 -92.1(7) . . . . ? C47 C42 C43 C44 4.4(10) . . . . ? Rh1 C42 C43 C44 -178.4(5) . . . . ? C42 C43 C44 C45 -0.7(11) . . . . ? C43 C44 C45 C46 -2.7(12) . . . . ? C44 C45 C46 C47 2.5(11) . . . . ? C43 C42 C47 C46 -4.5(9) . . . . ? Rh1 C42 C47 C46 177.9(5) . . . . ? C43 C42 C47 C48 173.0(6) . . . . ? Rh1 C42 C47 C48 -4.5(7) . . . . ? C45 C46 C47 C42 1.1(11) . . . . ? C45 C46 C47 C48 -176.2(7) . . . . ? C52 N52 C48 C49 -0.3(9) . . . . ? Rh1 N52 C48 C49 176.1(5) . . . . ? C52 N52 C48 C47 -175.9(6) . . . . ? Rh1 N52 C48 C47 0.5(7) . . . . ? C42 C47 C48 N52 2.6(8) . . . . ? C46 C47 C48 N52 180.0(6) . . . . ? C42 C47 C48 C49 -172.7(6) . . . . ? C46 C47 C48 C49 4.6(11) . . . . ? N52 C48 C49 C50 0.4(10) . . . . ? C47 C48 C49 C50 175.5(7) . . . . ? C48 C49 C50 C51 0.3(11) . . . . ? C49 C50 C51 C52 -1.0(12) . . . . ? C48 N52 C52 C51 -0.5(10) . . . . ? Rh1 N52 C52 C51 -176.6(5) . . . . ? C50 C51 C52 N52 1.1(11) . . . . ? C61 C56 C57 C58 0.3(10) . . . . ? B1 C56 C57 C58 178.8(6) . . . . ? C56 C57 C58 C59 0.1(12) . . . . ? C57 C58 C59 C60 0.0(12) . . . . ? C58 C59 C60 C61 -0.5(13) . . . . ? C59 C60 C61 C56 0.9(13) . . . . ? C57 C56 C61 C60 -0.8(11) . . . . ? B1 C56 C61 C60 -179.4(7) . . . . ? C67 C62 C63 C64 0.2(11) . . . . ? B1 C62 C63 C64 177.9(7) . . . . ? C62 C63 C64 C65 2.3(13) . . . . ? C63 C64 C65 C66 -3.2(13) . . . . ? C64 C65 C66 C67 1.7(12) . . . . ? C65 C66 C67 C62 1.0(11) . . . . ? C63 C62 C67 C66 -1.9(10) . . . . ? B1 C62 C67 C66 -179.6(6) . . . . ? C73 C68 C69 C70 1.0(9) . . . . ? B1 C68 C69 C70 -179.6(6) . . . . ? C68 C69 C70 C71 -1.8(10) . . . . ? C69 C70 C71 C72 1.1(9) . . . . ? C70 C71 C72 C73 0.2(10) . . . . ? C71 C72 C73 C68 -1.1(11) . . . . ? C69 C68 C73 C72 0.4(9) . . . . ? B1 C68 C73 C72 -179.0(6) . . . . ? C79 C74 C75 C76 -0.8(10) . . . . ? B1 C74 C75 C76 -174.8(6) . . . . ? C74 C75 C76 C77 -0.1(12) . . . . ? C75 C76 C77 C78 1.2(12) . . . . ? C76 C77 C78 C79 -1.3(13) . . . . ? C77 C78 C79 C74 0.3(12) . . . . ? C75 C74 C79 C78 0.7(10) . . . . ? B1 C74 C79 C78 174.8(7) . . . . ? C61 C56 B1 C62 75.9(8) . . . . ? C57 C56 B1 C62 -102.6(7) . . . . ? C61 C56 B1 C74 -164.7(6) . . . . ? C57 C56 B1 C74 16.8(8) . . . . ? C61 C56 B1 C68 -45.6(8) . . . . ? C57 C56 B1 C68 135.9(6) . . . . ? C63 C62 B1 C56 -3.9(9) . . . . ? C67 C62 B1 C56 173.6(6) . . . . ? C63 C62 B1 C74 -123.0(7) . . . . ? C67 C62 B1 C74 54.6(7) . . . . ? C63 C62 B1 C68 115.5(7) . . . . ? C67 C62 B1 C68 -67.0(7) . . . . ? C75 C74 B1 C56 75.6(7) . . . . ? C79 C74 B1 C56 -97.8(7) . . . . ? C75 C74 B1 C62 -165.0(6) . . . . ? C79 C74 B1 C62 21.5(8) . . . . ? C75 C74 B1 C68 -42.4(8) . . . . ? C79 C74 B1 C68 144.1(6) . . . . ? C69 C68 B1 C56 142.4(6) . . . . ? C73 C68 B1 C56 -38.2(7) . . . . ? C69 C68 B1 C62 22.2(8) . . . . ? C73 C68 B1 C62 -158.3(6) . . . . ? C69 C68 B1 C74 -99.2(7) . . . . ? C73 C68 B1 C74 80.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 4.069 _refine_diff_density_min -1.604 _refine_diff_density_rms 0.176 #==END _database_code_depnum_ccdc_archive 'CCDC 945558'