data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Owen, Gareth' 'Tsoureas, Nikolaos' 'Hope, Rebecca' 'Kuo, Yu-Ying' 'Haddow, Mairi' _publ_contact_author_name 'Owen, Gareth' _publ_contact_author_email gareth.owen@bristol.ac.uk _publ_section_title ; Synthesis and characterisation of group nine transition metal complexes containing new mesityl and napthyl based azaindole scorpionate ligands ; # Attachment '- Ligands Li(MeCN)2[ArBai] and Complexes 4_6_9.cif' data_nt_libhmesaza2 _database_code_depnum_ccdc_archive 'CCDC 802699' #TrackingRef '- Ligands Li(MeCN)2[ArBai] and Complexes 4_6_9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Li[MesitylBai] _chemical_melting_point ? _chemical_formula_moiety 'C27 H28 B Li N6' _chemical_formula_sum 'C27 H28 B Li N6' _chemical_formula_weight 454.30 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' Li Li -0.0003 0.0001 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 14.7389(14) _cell_length_b 13.0377(11) _cell_length_c 26.415(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.055(4) _cell_angle_gamma 90.00 _cell_volume 5056.3(8) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8895 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.36 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_min 0.11 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6884 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22717 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.57 _reflns_number_total 5825 _reflns_number_gt 4731 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _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^)+(0.0472P)^2^+2.9323P] 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 5825 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0518 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1059 _refine_ls_wR_factor_gt 0.0985 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 B1 B 0.21580(9) 0.09673(10) 0.34262(5) 0.0212(3) Uani 1 1 d . . . H1 H 0.1609(9) 0.0354(11) 0.3400(5) 0.025 Uiso 1 1 d . . . C1 C 0.09064(8) 0.20925(9) 0.38133(4) 0.0216(2) Uani 1 1 d . . . C2 C 0.20670(9) 0.29535(10) 0.35671(5) 0.0275(3) Uani 1 1 d . . . H2 H 0.2632 0.3098 0.3435 0.033 Uiso 1 1 calc R . . C3 C 0.15172(9) 0.36869(10) 0.37491(5) 0.0292(3) Uani 1 1 d . . . H3 H 0.1624 0.4405 0.3764 0.035 Uiso 1 1 calc R . . C4 C 0.07525(8) 0.31515(10) 0.39108(4) 0.0249(3) Uani 1 1 d . . . C5 C -0.00438(9) 0.34089(10) 0.41265(5) 0.0280(3) Uani 1 1 d . . . H5 H -0.0184 0.4102 0.4198 0.034 Uiso 1 1 calc R . . C6 C -0.06250(8) 0.26207(11) 0.42342(5) 0.0307(3) Uani 1 1 d . . . H6 H -0.1179 0.2771 0.4377 0.037 Uiso 1 1 calc R . . C7 C -0.04008(8) 0.16078(10) 0.41338(5) 0.0280(3) Uani 1 1 d . . . H7 H -0.0814 0.1088 0.4217 0.034 Uiso 1 1 calc R . . C8 C 0.26932(7) 0.00442(9) 0.42805(4) 0.0198(2) Uani 1 1 d . . . C9 C 0.36548(8) 0.11905(9) 0.40327(5) 0.0242(3) Uani 1 1 d . . . H9 H 0.3920 0.1693 0.3831 0.029 Uiso 1 1 calc R . . C10 C 0.40224(8) 0.08882(10) 0.45018(5) 0.0253(3) Uani 1 1 d . . . H10 H 0.4571 0.1129 0.4678 0.030 Uiso 1 1 calc R . . C11 C 0.34166(7) 0.01377(9) 0.46743(4) 0.0225(2) Uani 1 1 d . . . C12 C 0.33669(8) -0.04561(10) 0.51093(5) 0.0276(3) Uani 1 1 d . . . H12 H 0.3830 -0.0426 0.5383 0.033 Uiso 1 1 calc R . . C13 C 0.26196(9) -0.10903(11) 0.51291(5) 0.0303(3) Uani 1 1 d . . . H13 H 0.2570 -0.1516 0.5417 0.036 Uiso 1 1 calc R . . C14 C 0.19389(8) -0.11082(10) 0.47286(5) 0.0269(3) Uani 1 1 d . . . H14 H 0.1433 -0.1548 0.4758 0.032 Uiso 1 1 calc R . . C15 C 0.25908(7) 0.11062(9) 0.28830(4) 0.0212(2) Uani 1 1 d . . . C16 C 0.20990(8) 0.16575(10) 0.24848(5) 0.0243(3) Uani 1 1 d . . . C17 C 0.24681(8) 0.18400(10) 0.20249(5) 0.0254(3) Uani 1 1 d . . . H17 H 0.2126 0.2225 0.1769 0.031 Uiso 1 1 calc R . . C18 C 0.33203(8) 0.14760(10) 0.19305(4) 0.0251(3) Uani 1 1 d . . . C19 C 0.37536(8) 0.08330(10) 0.22924(4) 0.0243(3) Uani 1 1 d . . . H19 H 0.4311 0.0520 0.2223 0.029 Uiso 1 1 calc R . . C20 C 0.34024(8) 0.06255(9) 0.27563(4) 0.0219(2) Uani 1 1 d . . . C21 C 0.11303(9) 0.20153(12) 0.25215(5) 0.0345(3) Uani 1 1 d . . . H21A H 0.1136 0.2681 0.2694 0.052 Uiso 1 1 calc R . . H21B H 0.0806 0.1514 0.2715 0.052 Uiso 1 1 calc R . . H21C H 0.0821 0.2083 0.2179 0.052 Uiso 1 1 calc R . . C22 C 0.37565(10) 0.17612(12) 0.14537(5) 0.0351(3) Uani 1 1 d . . . H22A H 0.4247 0.2257 0.1537 0.053 Uiso 1 1 calc R . . H22B H 0.3298 0.2067 0.1208 0.053 Uiso 1 1 calc R . . H22C H 0.4008 0.1145 0.1306 0.053 Uiso 1 1 calc R . . C23 C 0.38925(8) -0.01929(10) 0.30841(5) 0.0285(3) Uani 1 1 d . . . H23A H 0.4232 -0.0641 0.2871 0.043 Uiso 1 1 calc R . . H23B H 0.3446 -0.0600 0.3251 0.043 Uiso 1 1 calc R . . H23C H 0.4316 0.0134 0.3342 0.043 Uiso 1 1 calc R . . C24 C -0.07966(8) -0.12253(10) 0.45926(5) 0.0264(3) Uani 1 1 d . . . C25 C -0.15468(8) -0.16052(10) 0.48623(5) 0.0286(3) Uani 1 1 d . . . H25A H -0.1702 -0.1096 0.5113 0.043 Uiso 1 1 calc R . . H25B H -0.1366 -0.2248 0.5036 0.043 Uiso 1 1 calc R . . H25C H -0.2078 -0.1729 0.4620 0.043 Uiso 1 1 calc R . . C26 C -0.07098(9) -0.08802(10) 0.29691(5) 0.0271(3) Uani 1 1 d . . . C27 C -0.15099(9) -0.10249(12) 0.26149(5) 0.0378(3) Uani 1 1 d . . . H27A H -0.1637 -0.1760 0.2575 0.057 Uiso 1 1 calc R . . H27B H -0.1399 -0.0730 0.2285 0.057 Uiso 1 1 calc R . . H27C H -0.2033 -0.0683 0.2746 0.057 Uiso 1 1 calc R . . Li1 Li 0.06883(13) -0.02284(17) 0.38853(8) 0.0266(4) Uani 1 1 d . . . N1 N 0.17082(6) 0.19830(8) 0.35966(4) 0.0226(2) Uani 1 1 d . . . N2 N 0.03596(6) 0.13152(8) 0.39275(4) 0.0233(2) Uani 1 1 d . . . N3 N 0.28539(6) 0.06811(7) 0.38862(4) 0.0206(2) Uani 1 1 d . . . N4 N 0.19494(6) -0.05451(8) 0.43027(4) 0.0219(2) Uani 1 1 d . . . N5 N -0.02169(7) -0.09215(9) 0.43778(4) 0.0339(3) Uani 1 1 d . . . N6 N -0.00879(8) -0.07708(9) 0.32502(4) 0.0338(3) 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 B1 0.0206(6) 0.0231(6) 0.0204(6) 0.0002(5) 0.0052(5) 0.0025(5) C1 0.0225(5) 0.0254(6) 0.0173(5) 0.0018(5) 0.0046(4) 0.0049(5) C2 0.0301(6) 0.0255(6) 0.0283(7) 0.0028(5) 0.0105(5) 0.0003(5) C3 0.0366(7) 0.0226(6) 0.0297(7) 0.0023(5) 0.0098(5) 0.0025(5) C4 0.0299(6) 0.0251(6) 0.0201(6) 0.0018(5) 0.0043(5) 0.0064(5) C5 0.0328(6) 0.0279(6) 0.0240(6) 0.0003(5) 0.0057(5) 0.0114(5) C6 0.0260(6) 0.0372(7) 0.0301(7) 0.0003(6) 0.0100(5) 0.0103(5) C7 0.0228(6) 0.0330(7) 0.0292(7) 0.0017(5) 0.0083(5) 0.0033(5) C8 0.0198(5) 0.0211(6) 0.0191(6) -0.0025(4) 0.0055(4) 0.0047(4) C9 0.0208(5) 0.0235(6) 0.0293(6) -0.0034(5) 0.0075(5) -0.0009(5) C10 0.0201(5) 0.0276(6) 0.0282(6) -0.0065(5) 0.0026(5) 0.0032(5) C11 0.0198(5) 0.0256(6) 0.0225(6) -0.0047(5) 0.0039(4) 0.0071(5) C12 0.0243(6) 0.0355(7) 0.0229(6) 0.0004(5) 0.0011(5) 0.0102(5) C13 0.0300(6) 0.0357(7) 0.0257(7) 0.0095(5) 0.0056(5) 0.0092(6) C14 0.0256(6) 0.0275(6) 0.0285(6) 0.0057(5) 0.0072(5) 0.0027(5) C15 0.0201(5) 0.0232(6) 0.0208(6) -0.0012(5) 0.0042(4) -0.0005(5) C16 0.0215(5) 0.0280(6) 0.0236(6) -0.0007(5) 0.0029(5) 0.0009(5) C17 0.0280(6) 0.0284(6) 0.0192(6) 0.0006(5) -0.0021(5) -0.0003(5) C18 0.0277(6) 0.0307(7) 0.0171(6) -0.0040(5) 0.0034(5) -0.0065(5) C19 0.0199(5) 0.0329(7) 0.0206(6) -0.0046(5) 0.0050(4) -0.0005(5) C20 0.0206(5) 0.0249(6) 0.0204(6) -0.0019(5) 0.0029(4) -0.0003(5) C21 0.0259(6) 0.0478(8) 0.0296(7) 0.0050(6) 0.0010(5) 0.0106(6) C22 0.0400(7) 0.0454(8) 0.0210(6) -0.0006(6) 0.0083(6) -0.0064(6) C23 0.0292(6) 0.0315(7) 0.0260(6) 0.0001(5) 0.0086(5) 0.0090(5) C24 0.0273(6) 0.0271(6) 0.0246(6) -0.0013(5) 0.0018(5) 0.0019(5) C25 0.0284(6) 0.0306(7) 0.0280(7) -0.0021(5) 0.0096(5) 0.0011(5) C26 0.0306(6) 0.0263(6) 0.0247(6) 0.0015(5) 0.0045(5) -0.0043(5) C27 0.0329(7) 0.0523(9) 0.0271(7) 0.0103(6) -0.0030(5) -0.0141(7) Li1 0.0245(10) 0.0287(11) 0.0265(11) -0.0007(9) 0.0022(8) 0.0004(8) N1 0.0239(5) 0.0227(5) 0.0222(5) 0.0017(4) 0.0081(4) 0.0020(4) N2 0.0208(5) 0.0275(5) 0.0222(5) 0.0005(4) 0.0061(4) 0.0026(4) N3 0.0198(4) 0.0227(5) 0.0200(5) -0.0018(4) 0.0053(4) 0.0001(4) N4 0.0216(5) 0.0226(5) 0.0220(5) 0.0012(4) 0.0058(4) 0.0020(4) N5 0.0288(6) 0.0400(7) 0.0330(6) 0.0042(5) 0.0042(5) -0.0033(5) N6 0.0315(6) 0.0409(7) 0.0289(6) -0.0045(5) 0.0019(5) -0.0039(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 B1 N1 1.5648(16) . ? B1 N3 1.5647(16) . ? B1 C15 1.6307(17) . ? B1 H1 1.136(13) . ? C1 N2 1.3456(16) . ? C1 N1 1.3653(14) . ? C1 C4 1.4262(17) . ? C2 C3 1.3677(18) . ? C2 N1 1.3762(16) . ? C2 H2 0.9500 . ? C3 C4 1.4229(18) . ? C3 H3 0.9500 . ? C4 C5 1.3903(17) . ? C5 C6 1.3833(19) . ? C5 H5 0.9500 . ? C6 C7 1.3925(18) . ? C6 H6 0.9500 . ? C7 N2 1.3439(15) . ? C7 H7 0.9500 . ? C8 N4 1.3442(15) . ? C8 N3 1.3689(15) . ? C8 C11 1.4278(16) . ? C9 C10 1.3661(18) . ? C9 N3 1.3798(15) . ? C9 H9 0.9500 . ? C10 C11 1.4262(17) . ? C10 H10 0.9500 . ? C11 C12 1.3927(17) . ? C12 C13 1.3819(19) . ? C12 H12 0.9500 . ? C13 C14 1.3926(18) . ? C13 H13 0.9500 . ? C14 N4 1.3446(15) . ? C14 H14 0.9500 . ? C15 C20 1.4165(15) . ? C15 C16 1.4191(17) . ? C16 C17 1.3948(17) . ? C16 C21 1.5132(16) . ? C17 C18 1.3857(17) . ? C17 H17 0.9500 . ? C18 C19 1.3844(18) . ? C18 C22 1.5103(17) . ? C19 C20 1.3981(16) . ? C19 H19 0.9500 . ? C20 C23 1.5166(17) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 N5 1.1377(16) . ? C24 C25 1.4541(17) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 N6 1.1365(16) . ? C26 C27 1.4516(18) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Li1 N6 2.070(2) . ? Li1 N2 2.075(2) . ? Li1 N4 2.117(2) . ? Li1 N5 2.144(2) . ? Li1 H1 2.089(13) . ? 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 N1 B1 N3 104.11(9) . . ? N1 B1 C15 111.57(10) . . ? N3 B1 C15 115.43(9) . . ? N1 B1 H1 107.2(7) . . ? N3 B1 H1 107.1(7) . . ? C15 B1 H1 110.9(7) . . ? N2 C1 N1 124.96(11) . . ? N2 C1 C4 125.50(10) . . ? N1 C1 C4 109.52(10) . . ? C3 C2 N1 112.36(11) . . ? C3 C2 H2 123.8 . . ? N1 C2 H2 123.8 . . ? C2 C3 C4 105.78(11) . . ? C2 C3 H3 127.1 . . ? C4 C3 H3 127.1 . . ? C5 C4 C3 136.41(12) . . ? C5 C4 C1 117.45(11) . . ? C3 C4 C1 106.14(10) . . ? C6 C5 C4 117.74(12) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? C5 C6 C7 120.25(11) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? N2 C7 C6 124.53(12) . . ? N2 C7 H7 117.7 . . ? C6 C7 H7 117.7 . . ? N4 C8 N3 125.20(10) . . ? N4 C8 C11 125.21(10) . . ? N3 C8 C11 109.53(10) . . ? C10 C9 N3 112.13(11) . . ? C10 C9 H9 123.9 . . ? N3 C9 H9 123.9 . . ? C9 C10 C11 106.16(10) . . ? C9 C10 H10 126.9 . . ? C11 C10 H10 126.9 . . ? C12 C11 C10 136.46(11) . . ? C12 C11 C8 117.61(11) . . ? C10 C11 C8 105.91(10) . . ? C13 C12 C11 117.64(11) . . ? C13 C12 H12 121.2 . . ? C11 C12 H12 121.2 . . ? C12 C13 C14 120.30(12) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? N4 C14 C13 124.46(12) . . ? N4 C14 H14 117.8 . . ? C13 C14 H14 117.8 . . ? C20 C15 C16 115.83(10) . . ? C20 C15 B1 124.24(10) . . ? C16 C15 B1 119.64(10) . . ? C17 C16 C15 121.27(11) . . ? C17 C16 C21 116.47(11) . . ? C15 C16 C21 122.14(11) . . ? C18 C17 C16 121.84(11) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 C17 116.97(11) . . ? C19 C18 C22 121.37(11) . . ? C17 C18 C22 121.66(12) . . ? C18 C19 C20 122.58(11) . . ? C18 C19 H19 118.7 . . ? C20 C19 H19 118.7 . . ? C19 C20 C15 120.48(11) . . ? C19 C20 C23 116.24(10) . . ? C15 C20 C23 123.09(10) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 C25 179.17(15) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N6 C26 C27 179.32(14) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N6 Li1 N2 105.06(10) . . ? N6 Li1 N4 138.84(11) . . ? N2 Li1 N4 111.08(10) . . ? N6 Li1 N5 91.07(9) . . ? N2 Li1 N5 102.44(9) . . ? N4 Li1 N5 99.59(9) . . ? N6 Li1 H1 88.2(4) . . ? N2 Li1 H1 81.3(4) . . ? N4 Li1 H1 78.6(4) . . ? N5 Li1 H1 176.3(4) . . ? C1 N1 C2 106.18(10) . . ? C1 N1 B1 127.84(10) . . ? C2 N1 B1 125.96(9) . . ? C7 N2 C1 114.48(11) . . ? C7 N2 Li1 120.27(10) . . ? C1 N2 Li1 124.83(9) . . ? C8 N3 C9 106.24(10) . . ? C8 N3 B1 126.16(9) . . ? C9 N3 B1 126.09(10) . . ? C8 N4 C14 114.72(10) . . ? C8 N4 Li1 123.22(10) . . ? C14 N4 Li1 117.91(10) . . ? C24 N5 Li1 169.87(12) . . ? C26 N6 Li1 158.21(12) . . ? 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 N1 C2 C3 C4 0.42(15) . . . . ? C2 C3 C4 C5 -179.93(14) . . . . ? C2 C3 C4 C1 0.35(14) . . . . ? N2 C1 C4 C5 -2.28(18) . . . . ? N1 C1 C4 C5 179.21(11) . . . . ? N2 C1 C4 C3 177.50(11) . . . . ? N1 C1 C4 C3 -1.00(13) . . . . ? C3 C4 C5 C6 -179.25(14) . . . . ? C1 C4 C5 C6 0.45(17) . . . . ? C4 C5 C6 C7 0.92(19) . . . . ? C5 C6 C7 N2 -0.8(2) . . . . ? N3 C9 C10 C11 -0.50(13) . . . . ? C9 C10 C11 C12 -178.69(13) . . . . ? C9 C10 C11 C8 -0.41(12) . . . . ? N4 C8 C11 C12 2.51(17) . . . . ? N3 C8 C11 C12 179.85(10) . . . . ? N4 C8 C11 C10 -176.15(10) . . . . ? N3 C8 C11 C10 1.19(12) . . . . ? C10 C11 C12 C13 177.91(13) . . . . ? C8 C11 C12 C13 -0.22(17) . . . . ? C11 C12 C13 C14 -1.26(18) . . . . ? C12 C13 C14 N4 0.7(2) . . . . ? N1 B1 C15 C20 144.22(11) . . . . ? N3 B1 C15 C20 25.65(16) . . . . ? N1 B1 C15 C16 -42.20(15) . . . . ? N3 B1 C15 C16 -160.76(10) . . . . ? C20 C15 C16 C17 -9.41(17) . . . . ? B1 C15 C16 C17 176.47(11) . . . . ? C20 C15 C16 C21 166.45(12) . . . . ? B1 C15 C16 C21 -7.66(18) . . . . ? C15 C16 C17 C18 1.36(19) . . . . ? C21 C16 C17 C18 -174.73(12) . . . . ? C16 C17 C18 C19 6.42(18) . . . . ? C16 C17 C18 C22 -173.94(12) . . . . ? C17 C18 C19 C20 -5.91(18) . . . . ? C22 C18 C19 C20 174.43(12) . . . . ? C18 C19 C20 C15 -2.41(18) . . . . ? C18 C19 C20 C23 172.72(12) . . . . ? C16 C15 C20 C19 9.86(17) . . . . ? B1 C15 C20 C19 -176.33(11) . . . . ? C16 C15 C20 C23 -164.92(11) . . . . ? B1 C15 C20 C23 8.89(18) . . . . ? N2 C1 N1 C2 -177.28(11) . . . . ? C4 C1 N1 C2 1.24(13) . . . . ? N2 C1 N1 B1 1.21(19) . . . . ? C4 C1 N1 B1 179.73(10) . . . . ? C3 C2 N1 C1 -1.05(14) . . . . ? C3 C2 N1 B1 -179.57(11) . . . . ? N3 B1 N1 C1 -96.16(13) . . . . ? C15 B1 N1 C1 138.71(11) . . . . ? N3 B1 N1 C2 82.05(13) . . . . ? C15 B1 N1 C2 -43.08(15) . . . . ? C6 C7 N2 C1 -0.88(18) . . . . ? C6 C7 N2 Li1 172.04(12) . . . . ? N1 C1 N2 C7 -179.29(11) . . . . ? C4 C1 N2 C7 2.43(17) . . . . ? N1 C1 N2 Li1 8.17(18) . . . . ? C4 C1 N2 Li1 -170.12(11) . . . . ? N6 Li1 N2 C7 81.27(13) . . . . ? N4 Li1 N2 C7 -118.80(11) . . . . ? N5 Li1 N2 C7 -13.27(14) . . . . ? N6 Li1 N2 C1 -106.59(12) . . . . ? N4 Li1 N2 C1 53.34(15) . . . . ? N5 Li1 N2 C1 158.87(10) . . . . ? N4 C8 N3 C9 175.87(10) . . . . ? C11 C8 N3 C9 -1.47(12) . . . . ? N4 C8 N3 B1 9.24(17) . . . . ? C11 C8 N3 B1 -168.10(10) . . . . ? C10 C9 N3 C8 1.24(13) . . . . ? C10 C9 N3 B1 167.88(10) . . . . ? N1 B1 N3 C8 93.26(12) . . . . ? C15 B1 N3 C8 -144.11(11) . . . . ? N1 B1 N3 C9 -70.79(13) . . . . ? C15 B1 N3 C9 51.84(15) . . . . ? N3 C8 N4 C14 -179.91(11) . . . . ? C11 C8 N4 C14 -2.98(16) . . . . ? N3 C8 N4 Li1 -23.34(16) . . . . ? C11 C8 N4 Li1 153.59(11) . . . . ? C13 C14 N4 C8 1.33(17) . . . . ? C13 C14 N4 Li1 -156.56(12) . . . . ? N6 Li1 N4 C8 104.95(18) . . . . ? N2 Li1 N4 C8 -44.81(14) . . . . ? N5 Li1 N4 C8 -152.22(10) . . . . ? N6 Li1 N4 C14 -99.19(18) . . . . ? N2 Li1 N4 C14 111.06(12) . . . . ? N5 Li1 N4 C14 3.65(14) . . . . ? N6 Li1 N5 C24 -47.5(7) . . . . ? N2 Li1 N5 C24 58.2(7) . . . . ? N4 Li1 N5 C24 172.5(7) . . . . ? N2 Li1 N6 C26 -42.8(4) . . . . ? N4 Li1 N6 C26 166.4(3) . . . . ? N5 Li1 N6 C26 60.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.274 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.038 data_nt_libainapthyl_0m _database_code_depnum_ccdc_archive 'CCDC 802700' #TrackingRef '- Ligands Li(MeCN)2[ArBai] and Complexes 4_6_9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Li[NapthylBai] _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 B Li N6' _chemical_formula_sum 'C28 H24 B Li N6' _chemical_formula_weight 462.28 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' Li Li -0.0003 0.0001 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7576(5) _cell_length_b 8.1623(3) _cell_length_c 23.2888(8) _cell_angle_alpha 90.00 _cell_angle_beta 102.637(2) _cell_angle_gamma 90.00 _cell_volume 2551.83(16) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8186 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 27.47 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 968 _exptl_absorpt_coefficient_mu 0.073 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6723 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22182 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5858 _reflns_number_gt 4702 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _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^)+(0.0516P)^2^+0.6998P] 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 5858 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0540 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1115 _refine_ls_wR_factor_gt 0.1036 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 B1 B 0.27036(10) 0.34660(15) 0.64850(6) 0.0172(3) Uani 1 1 d . . . H1 H 0.2562(10) 0.2883(16) 0.6032(6) 0.021 Uiso 1 1 d . . . C1 C 0.45558(9) 0.26788(13) 0.64976(5) 0.0175(2) Uani 1 1 d . . . C2 C 0.43429(9) 0.39715(15) 0.72876(5) 0.0211(3) Uani 1 1 d . . . H2 H 0.4027 0.4544 0.7552 0.025 Uiso 1 1 calc R . . C3 C 0.53392(9) 0.36536(15) 0.73965(5) 0.0231(3) Uani 1 1 d . . . H3 H 0.5825 0.3946 0.7738 0.028 Uiso 1 1 calc R . . C4 C 0.55039(9) 0.27932(14) 0.68938(5) 0.0200(3) Uani 1 1 d . . . C5 C 0.63129(10) 0.20979(16) 0.67171(6) 0.0240(3) Uani 1 1 d . . . H5 H 0.6962 0.2131 0.6963 0.029 Uiso 1 1 calc R . . C6 C 0.61396(9) 0.13538(16) 0.61684(5) 0.0245(3) Uani 1 1 d . . . H6 H 0.6667 0.0809 0.6043 0.029 Uiso 1 1 calc R . . C7 C 0.51942(9) 0.14050(15) 0.58024(5) 0.0225(3) Uani 1 1 d . . . H7 H 0.5112 0.0932 0.5422 0.027 Uiso 1 1 calc R . . C8 C 0.26275(8) 0.62983(14) 0.59747(5) 0.0168(2) Uani 1 1 d . . . C9 C 0.20835(9) 0.63163(15) 0.67932(5) 0.0195(2) Uani 1 1 d . . . H9 H 0.1890 0.5938 0.7137 0.023 Uiso 1 1 calc R . . C10 C 0.20533(9) 0.79214(14) 0.66243(5) 0.0207(3) Uani 1 1 d . . . H10 H 0.1844 0.8830 0.6822 0.025 Uiso 1 1 calc R . . C11 C 0.24009(9) 0.79525(14) 0.60909(5) 0.0194(2) Uani 1 1 d . . . C12 C 0.25563(10) 0.91349(14) 0.56918(5) 0.0244(3) Uani 1 1 d . . . H12 H 0.2417 1.0257 0.5746 0.029 Uiso 1 1 calc R . . C13 C 0.29213(10) 0.86222(15) 0.52131(6) 0.0261(3) Uani 1 1 d . . . H13 H 0.3034 0.9400 0.4931 0.031 Uiso 1 1 calc R . . C14 C 0.31249(10) 0.69718(15) 0.51418(5) 0.0226(3) Uani 1 1 d . . . H14 H 0.3376 0.6670 0.4808 0.027 Uiso 1 1 calc R . . C15 C 0.20290(9) 0.25772(14) 0.68813(5) 0.0194(3) Uani 1 1 d . . . C16 C 0.24191(10) 0.18294(15) 0.74114(5) 0.0235(3) Uani 1 1 d . . . H16 H 0.3121 0.1831 0.7553 0.028 Uiso 1 1 calc R . . C17 C 0.18217(11) 0.10568(16) 0.77563(6) 0.0294(3) Uani 1 1 d . . . H17 H 0.2125 0.0564 0.8121 0.035 Uiso 1 1 calc R . . C18 C 0.08133(11) 0.10198(17) 0.75660(6) 0.0320(3) Uani 1 1 d . . . H18 H 0.0415 0.0507 0.7800 0.038 Uiso 1 1 calc R . . C19 C 0.03539(10) 0.17427(16) 0.70206(6) 0.0277(3) Uani 1 1 d . . . C20 C -0.06958(11) 0.1721(2) 0.68065(7) 0.0397(4) Uani 1 1 d . . . H20 H -0.1104 0.1211 0.7035 0.048 Uiso 1 1 calc R . . C21 C -0.11281(11) 0.2412(2) 0.62822(7) 0.0430(4) Uani 1 1 d . . . H21 H -0.1832 0.2398 0.6151 0.052 Uiso 1 1 calc R . . C22 C -0.05360(11) 0.3149(2) 0.59317(7) 0.0355(3) Uani 1 1 d . . . H22 H -0.0840 0.3618 0.5563 0.043 Uiso 1 1 calc R . . C23 C 0.04767(10) 0.31888(16) 0.61231(6) 0.0259(3) Uani 1 1 d . . . H23 H 0.0868 0.3681 0.5881 0.031 Uiso 1 1 calc R . . C24 C 0.09626(9) 0.25133(15) 0.66753(5) 0.0222(3) Uani 1 1 d . . . C25 C 0.43577(10) 0.32441(15) 0.42323(5) 0.0238(3) Uani 1 1 d . . . C26 C 0.47675(11) 0.29342(17) 0.37177(6) 0.0282(3) Uani 1 1 d . . . H26A H 0.5384 0.2301 0.3834 0.042 Uiso 1 1 calc R . . H26B H 0.4910 0.3979 0.3546 0.042 Uiso 1 1 calc R . . H26C H 0.4285 0.2314 0.3427 0.042 Uiso 1 1 calc R . . C27 C 0.12117(12) 0.21700(18) 0.45163(7) 0.0389(4) Uani 1 1 d . . . C28 C 0.02408(16) 0.1783(3) 0.41466(12) 0.0934(9) Uani 1 1 d . . . H28A H -0.0283 0.2106 0.4349 0.140 Uiso 1 1 calc R . . H28B H 0.0198 0.0602 0.4068 0.140 Uiso 1 1 calc R . . H28C H 0.0155 0.2379 0.3774 0.140 Uiso 1 1 calc R . . Li1 Li 0.32756(16) 0.3355(3) 0.53276(9) 0.0238(4) Uani 1 1 d . . . N1 N 0.38431(7) 0.33671(11) 0.67485(4) 0.0178(2) Uani 1 1 d . . . N2 N 0.43919(8) 0.20733(12) 0.59480(4) 0.0194(2) Uani 1 1 d . . . N3 N 0.24280(7) 0.53087(12) 0.64064(4) 0.0173(2) Uani 1 1 d . . . N4 N 0.29899(7) 0.57787(12) 0.55145(4) 0.0187(2) Uani 1 1 d . . . N5 N 0.40273(9) 0.34566(15) 0.46341(5) 0.0311(3) Uani 1 1 d . . . N6 N 0.19616(9) 0.24800(14) 0.48041(5) 0.0288(3) 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 B1 0.0182(7) 0.0172(6) 0.0170(6) 0.0004(5) 0.0054(5) -0.0002(5) C1 0.0185(6) 0.0153(5) 0.0196(6) 0.0029(4) 0.0063(5) -0.0010(4) C2 0.0249(7) 0.0225(6) 0.0163(6) 0.0001(4) 0.0050(5) -0.0017(5) C3 0.0224(7) 0.0282(6) 0.0178(6) 0.0015(5) 0.0024(5) -0.0035(5) C4 0.0190(6) 0.0220(6) 0.0190(6) 0.0052(4) 0.0041(5) -0.0015(5) C5 0.0173(6) 0.0305(7) 0.0241(6) 0.0085(5) 0.0043(5) 0.0005(5) C6 0.0215(7) 0.0275(6) 0.0272(7) 0.0052(5) 0.0110(5) 0.0042(5) C7 0.0238(7) 0.0232(6) 0.0223(6) -0.0012(5) 0.0091(5) 0.0000(5) C8 0.0146(6) 0.0174(5) 0.0175(6) 0.0001(4) 0.0015(4) -0.0015(4) C9 0.0187(6) 0.0235(6) 0.0170(6) -0.0030(4) 0.0053(5) 0.0000(5) C10 0.0207(6) 0.0200(6) 0.0217(6) -0.0044(5) 0.0051(5) 0.0014(5) C11 0.0176(6) 0.0188(6) 0.0208(6) -0.0011(4) 0.0023(5) -0.0003(4) C12 0.0284(7) 0.0162(5) 0.0283(7) 0.0004(5) 0.0059(5) -0.0003(5) C13 0.0336(8) 0.0201(6) 0.0254(7) 0.0055(5) 0.0085(6) -0.0024(5) C14 0.0264(7) 0.0233(6) 0.0194(6) 0.0008(5) 0.0077(5) -0.0019(5) C15 0.0237(7) 0.0158(5) 0.0204(6) -0.0029(4) 0.0086(5) -0.0017(5) C16 0.0274(7) 0.0213(6) 0.0228(6) 0.0002(5) 0.0078(5) -0.0020(5) C17 0.0423(9) 0.0266(6) 0.0216(6) 0.0024(5) 0.0118(6) -0.0036(6) C18 0.0416(9) 0.0317(7) 0.0291(7) -0.0018(6) 0.0211(6) -0.0107(6) C19 0.0283(7) 0.0296(7) 0.0290(7) -0.0067(5) 0.0144(6) -0.0076(5) C20 0.0293(8) 0.0533(9) 0.0420(9) -0.0064(7) 0.0201(7) -0.0132(7) C21 0.0214(8) 0.0639(11) 0.0446(9) -0.0061(8) 0.0093(7) -0.0092(7) C22 0.0243(7) 0.0475(9) 0.0337(8) -0.0009(6) 0.0040(6) -0.0023(6) C23 0.0211(7) 0.0297(7) 0.0277(7) -0.0009(5) 0.0072(5) -0.0036(5) C24 0.0238(7) 0.0210(6) 0.0239(6) -0.0045(5) 0.0102(5) -0.0035(5) C25 0.0231(7) 0.0254(6) 0.0216(6) 0.0015(5) 0.0020(5) -0.0008(5) C26 0.0319(8) 0.0342(7) 0.0199(6) -0.0005(5) 0.0085(6) -0.0038(6) C27 0.0317(9) 0.0332(8) 0.0456(9) -0.0073(6) -0.0049(7) 0.0034(6) C28 0.0432(12) 0.0850(17) 0.126(2) -0.0379(16) -0.0377(13) 0.0025(11) Li1 0.0246(11) 0.0242(10) 0.0225(10) -0.0024(8) 0.0052(9) 0.0003(8) N1 0.0194(5) 0.0179(5) 0.0165(5) -0.0008(4) 0.0047(4) -0.0002(4) N2 0.0194(5) 0.0194(5) 0.0205(5) -0.0010(4) 0.0066(4) -0.0008(4) N3 0.0176(5) 0.0181(5) 0.0167(5) -0.0007(4) 0.0052(4) -0.0002(4) N4 0.0198(5) 0.0190(5) 0.0176(5) -0.0003(4) 0.0050(4) -0.0015(4) N5 0.0321(7) 0.0379(6) 0.0246(6) -0.0006(5) 0.0091(5) 0.0032(5) N6 0.0302(7) 0.0277(6) 0.0261(6) 0.0010(5) 0.0007(5) -0.0011(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 B1 N3 1.5521(16) . ? B1 N1 1.5555(17) . ? B1 C15 1.6168(17) . ? B1 H1 1.136(13) . ? C1 N2 1.3443(15) . ? C1 N1 1.3673(15) . ? C1 C4 1.4266(17) . ? C2 C3 1.3632(18) . ? C2 N1 1.3835(15) . ? C2 H2 0.9500 . ? C3 C4 1.4252(17) . ? C3 H3 0.9500 . ? C4 C5 1.3894(18) . ? C5 C6 1.3876(18) . ? C5 H5 0.9500 . ? C6 C7 1.3910(18) . ? C6 H6 0.9500 . ? C7 N2 1.3395(15) . ? C7 H7 0.9500 . ? C8 N4 1.3457(14) . ? C8 N3 1.3635(14) . ? C8 C11 1.4249(16) . ? C9 C10 1.3660(17) . ? C9 N3 1.3781(14) . ? C9 H9 0.9500 . ? C10 C11 1.4255(17) . ? C10 H10 0.9500 . ? C11 C12 1.3885(16) . ? C12 C13 1.3838(18) . ? C12 H12 0.9500 . ? C13 C14 1.3932(17) . ? C13 H13 0.9500 . ? C14 N4 1.3441(15) . ? C14 H14 0.9500 . ? C15 C16 1.3766(17) . ? C15 C24 1.4414(18) . ? C16 C17 1.4166(17) . ? C16 H16 0.9500 . ? C17 C18 1.361(2) . ? C17 H17 0.9500 . ? C18 C19 1.418(2) . ? C18 H18 0.9500 . ? C19 C20 1.421(2) . ? C19 C24 1.4276(17) . ? C20 C21 1.358(2) . ? C20 H20 0.9500 . ? C21 C22 1.408(2) . ? C21 H21 0.9500 . ? C22 C23 1.3671(19) . ? C22 H22 0.9500 . ? C23 C24 1.4242(18) . ? C23 H23 0.9500 . ? C25 N5 1.1395(16) . ? C25 C26 1.4539(17) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 N6 1.1292(18) . ? C27 C28 1.457(2) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? Li1 N6 2.074(2) . ? Li1 N4 2.081(2) . ? Li1 N5 2.101(2) . ? Li1 N2 2.138(2) . ? Li1 H1 2.123(13) . ? 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 N3 B1 N1 107.21(9) . . ? N3 B1 C15 110.26(9) . . ? N1 B1 C15 113.97(10) . . ? N3 B1 H1 108.0(7) . . ? N1 B1 H1 107.4(7) . . ? C15 B1 H1 109.8(7) . . ? N2 C1 N1 124.86(11) . . ? N2 C1 C4 125.39(11) . . ? N1 C1 C4 109.65(10) . . ? C3 C2 N1 112.39(11) . . ? C3 C2 H2 123.8 . . ? N1 C2 H2 123.8 . . ? C2 C3 C4 105.96(11) . . ? C2 C3 H3 127.0 . . ? C4 C3 H3 127.0 . . ? C5 C4 C3 136.56(12) . . ? C5 C4 C1 117.39(11) . . ? C3 C4 C1 106.05(11) . . ? C6 C5 C4 117.65(12) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C5 C6 C7 120.02(11) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? N2 C7 C6 124.68(11) . . ? N2 C7 H7 117.7 . . ? C6 C7 H7 117.7 . . ? N4 C8 N3 124.75(10) . . ? N4 C8 C11 125.76(10) . . ? N3 C8 C11 109.49(10) . . ? C10 C9 N3 112.17(10) . . ? C10 C9 H9 123.9 . . ? N3 C9 H9 123.9 . . ? C9 C10 C11 105.85(10) . . ? C9 C10 H10 127.1 . . ? C11 C10 H10 127.1 . . ? C12 C11 C8 117.35(11) . . ? C12 C11 C10 136.53(11) . . ? C8 C11 C10 106.12(10) . . ? C13 C12 C11 117.72(11) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C12 C13 C14 120.41(11) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? N4 C14 C13 124.32(11) . . ? N4 C14 H14 117.8 . . ? C13 C14 H14 117.8 . . ? C16 C15 C24 116.81(11) . . ? C16 C15 B1 123.44(11) . . ? C24 C15 B1 119.73(10) . . ? C15 C16 C17 123.04(12) . . ? C15 C16 H16 118.5 . . ? C17 C16 H16 118.5 . . ? C18 C17 C16 120.11(12) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.35(12) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C20 121.92(12) . . ? C18 C19 C24 119.12(12) . . ? C20 C19 C24 118.96(13) . . ? C21 C20 C19 121.44(13) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C20 C21 C22 120.23(14) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C23 C22 C21 119.90(14) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 121.92(12) . . ? C22 C23 H23 119.0 . . ? C24 C23 H23 119.0 . . ? C23 C24 C19 117.51(12) . . ? C23 C24 C15 121.94(11) . . ? C19 C24 C15 120.55(12) . . ? N5 C25 C26 178.61(14) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N6 C27 C28 179.5(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N6 Li1 N4 105.68(10) . . ? N6 Li1 N5 94.24(9) . . ? N4 Li1 N5 105.70(10) . . ? N6 Li1 N2 129.32(11) . . ? N4 Li1 N2 117.68(10) . . ? N5 Li1 N2 97.88(10) . . ? N6 Li1 H1 84.3(4) . . ? N4 Li1 H1 82.6(4) . . ? N5 Li1 H1 171.7(4) . . ? N2 Li1 H1 77.0(4) . . ? C1 N1 C2 105.89(10) . . ? C1 N1 B1 127.42(10) . . ? C2 N1 B1 126.68(10) . . ? C7 N2 C1 114.51(11) . . ? C7 N2 Li1 122.56(10) . . ? C1 N2 Li1 114.17(9) . . ? C8 N3 C9 106.37(9) . . ? C8 N3 B1 125.28(9) . . ? C9 N3 B1 127.68(10) . . ? C14 N4 C8 114.43(10) . . ? C14 N4 Li1 119.64(10) . . ? C8 N4 Li1 125.87(10) . . ? C25 N5 Li1 167.68(13) . . ? C27 N6 Li1 172.71(13) . . ? 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 N1 C2 C3 C4 0.40(14) . . . . ? C2 C3 C4 C5 -178.91(14) . . . . ? C2 C3 C4 C1 1.10(13) . . . . ? N2 C1 C4 C5 -5.75(17) . . . . ? N1 C1 C4 C5 177.76(10) . . . . ? N2 C1 C4 C3 174.25(11) . . . . ? N1 C1 C4 C3 -2.24(13) . . . . ? C3 C4 C5 C6 -179.66(13) . . . . ? C1 C4 C5 C6 0.34(16) . . . . ? C4 C5 C6 C7 3.72(18) . . . . ? C5 C6 C7 N2 -3.21(19) . . . . ? N3 C9 C10 C11 0.10(14) . . . . ? N4 C8 C11 C12 0.76(18) . . . . ? N3 C8 C11 C12 -179.74(11) . . . . ? N4 C8 C11 C10 -179.21(11) . . . . ? N3 C8 C11 C10 0.29(13) . . . . ? C9 C10 C11 C12 179.81(14) . . . . ? C9 C10 C11 C8 -0.23(13) . . . . ? C8 C11 C12 C13 -0.19(18) . . . . ? C10 C11 C12 C13 179.77(14) . . . . ? C11 C12 C13 C14 -0.2(2) . . . . ? C12 C13 C14 N4 0.1(2) . . . . ? N3 B1 C15 C16 -119.20(12) . . . . ? N1 B1 C15 C16 1.42(16) . . . . ? N3 B1 C15 C24 62.16(14) . . . . ? N1 B1 C15 C24 -177.23(10) . . . . ? C24 C15 C16 C17 -1.47(17) . . . . ? B1 C15 C16 C17 179.85(11) . . . . ? C15 C16 C17 C18 0.5(2) . . . . ? C16 C17 C18 C19 0.4(2) . . . . ? C17 C18 C19 C20 179.68(13) . . . . ? C17 C18 C19 C24 -0.2(2) . . . . ? C18 C19 C20 C21 -179.75(15) . . . . ? C24 C19 C20 C21 0.1(2) . . . . ? C19 C20 C21 C22 1.1(2) . . . . ? C20 C21 C22 C23 -0.9(2) . . . . ? C21 C22 C23 C24 -0.6(2) . . . . ? C22 C23 C24 C19 1.70(19) . . . . ? C22 C23 C24 C15 -179.04(13) . . . . ? C18 C19 C24 C23 178.42(12) . . . . ? C20 C19 C24 C23 -1.47(18) . . . . ? C18 C19 C24 C15 -0.85(18) . . . . ? C20 C19 C24 C15 179.25(12) . . . . ? C16 C15 C24 C23 -177.60(11) . . . . ? B1 C15 C24 C23 1.14(17) . . . . ? C16 C15 C24 C19 1.65(17) . . . . ? B1 C15 C24 C19 -179.62(11) . . . . ? N2 C1 N1 C2 -174.07(11) . . . . ? C4 C1 N1 C2 2.44(12) . . . . ? N2 C1 N1 B1 5.63(18) . . . . ? C4 C1 N1 B1 -177.86(10) . . . . ? C3 C2 N1 C1 -1.78(13) . . . . ? C3 C2 N1 B1 178.52(10) . . . . ? N3 B1 N1 C1 -117.26(11) . . . . ? C15 B1 N1 C1 120.44(12) . . . . ? N3 B1 N1 C2 62.38(14) . . . . ? C15 B1 N1 C2 -59.93(14) . . . . ? C6 C7 N2 C1 -1.73(17) . . . . ? C6 C7 N2 Li1 143.87(12) . . . . ? N1 C1 N2 C7 -177.73(10) . . . . ? C4 C1 N2 C7 6.30(16) . . . . ? N1 C1 N2 Li1 33.72(15) . . . . ? C4 C1 N2 Li1 -142.24(12) . . . . ? N6 Li1 N2 C7 92.67(16) . . . . ? N4 Li1 N2 C7 -121.83(12) . . . . ? N5 Li1 N2 C7 -9.44(14) . . . . ? N6 Li1 N2 C1 -121.62(13) . . . . ? N4 Li1 N2 C1 23.87(15) . . . . ? N5 Li1 N2 C1 136.27(10) . . . . ? N4 C8 N3 C9 179.28(11) . . . . ? C11 C8 N3 C9 -0.23(13) . . . . ? N4 C8 N3 B1 8.02(18) . . . . ? C11 C8 N3 B1 -171.49(10) . . . . ? C10 C9 N3 C8 0.08(14) . . . . ? C10 C9 N3 B1 171.06(11) . . . . ? N1 B1 N3 C8 75.35(13) . . . . ? C15 B1 N3 C8 -160.06(10) . . . . ? N1 B1 N3 C9 -94.03(13) . . . . ? C15 B1 N3 C9 30.56(16) . . . . ? C13 C14 N4 C8 0.38(18) . . . . ? C13 C14 N4 Li1 177.51(12) . . . . ? N3 C8 N4 C14 179.74(11) . . . . ? C11 C8 N4 C14 -0.83(17) . . . . ? N3 C8 N4 Li1 2.82(18) . . . . ? C11 C8 N4 Li1 -177.75(12) . . . . ? N6 Li1 N4 C14 -87.41(13) . . . . ? N5 Li1 N4 C14 11.71(15) . . . . ? N2 Li1 N4 C14 119.66(12) . . . . ? N6 Li1 N4 C8 89.36(13) . . . . ? N5 Li1 N4 C8 -171.51(10) . . . . ? N2 Li1 N4 C8 -63.56(16) . . . . ? N6 Li1 N5 C25 -43.4(6) . . . . ? N4 Li1 N5 C25 -151.0(6) . . . . ? N2 Li1 N5 C25 87.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.284 _refine_diff_density_min -0.295 _refine_diff_density_rms 0.041 data_rh25 _database_code_depnum_ccdc_archive 'CCDC 802701' #TrackingRef '- Ligands Li(MeCN)2[ArBai] and Complexes 4_6_9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Complex_4 _chemical_melting_point ? _chemical_formula_moiety 'C31 H34 B N4 Rh' _chemical_formula_sum 'C31 H34 B N4 Rh' _chemical_formula_weight 576.34 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' 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' B B 0.0013 0.0007 '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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.102(2) _cell_length_b 16.512(3) _cell_length_c 16.633(2) _cell_angle_alpha 113.679(11) _cell_angle_beta 102.604(15) _cell_angle_gamma 97.984(12) _cell_volume 2636.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9998 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 27.61 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_max 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.452 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 0.676 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6909 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32343 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 27.63 _reflns_number_total 11921 _reflns_number_gt 9680 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _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. There are two independent molecules in the asymmetric unit and in that containing Rh(2), the cyclooctadiene ligand is disordered. This has been modelled over two positions which refined to a ratio of 0.53:0.47. Restraints were used on the thermal parameters of the disordered atoms in order to ensure a smooth refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+2.7396P] 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 11921 _refine_ls_number_parameters 701 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0447 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0692 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.011 _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 0.392347(16) 0.419881(12) 0.134701(11) 0.01182(5) Uani 1 1 d . . . N1 N 0.13899(17) 0.34354(13) -0.05187(12) 0.0149(4) Uani 1 1 d . . . N2 N 0.29472(17) 0.48319(13) 0.06051(12) 0.0134(4) Uani 1 1 d . . . N3 N 0.10216(17) 0.27638(13) 0.05215(12) 0.0143(4) Uani 1 1 d . . . N4 N 0.23369(17) 0.41446(13) 0.18496(12) 0.0131(4) Uani 1 1 d . . . B1 B 0.1801(2) 0.27454(18) -0.01601(17) 0.0147(5) Uani 1 1 d . . . H1B H 0.2730 0.2982 0.0194 0.018 Uiso 1 1 calc R . . B2 B 0.4539(2) 0.22501(18) 0.45384(17) 0.0131(5) Uani 1 1 d . . . H2B H 0.4290 0.1649 0.3977 0.016 Uiso 1 1 calc R . . C1 C 0.1901(2) 0.43548(16) -0.01309(15) 0.0140(5) Uani 1 1 d . . . C2 C 0.0300(2) 0.32538(18) -0.12245(15) 0.0193(5) Uani 1 1 d . . . H2 H -0.0263 0.2664 -0.1604 0.023 Uiso 1 1 calc R . . C3 C 0.0131(2) 0.40175(18) -0.13094(16) 0.0217(5) Uani 1 1 d . . . H3 H -0.0532 0.4053 -0.1754 0.026 Uiso 1 1 calc R . . C4 C 0.1150(2) 0.47597(17) -0.05974(16) 0.0173(5) Uani 1 1 d . . . C5 C 0.1484(2) 0.56999(18) -0.02625(17) 0.0222(5) Uani 1 1 d . . . H5 H 0.1004 0.5998 -0.0549 0.027 Uiso 1 1 calc R . . C6 C 0.2540(2) 0.61898(17) 0.05027(17) 0.0205(5) Uani 1 1 d . . . H6 H 0.2788 0.6837 0.0754 0.025 Uiso 1 1 calc R . . C7 C 0.3242(2) 0.57456(16) 0.09072(16) 0.0172(5) Uani 1 1 d . . . H7 H 0.3970 0.6105 0.1426 0.021 Uiso 1 1 calc R . . C8 C 0.1249(2) 0.34693(16) 0.13740(15) 0.0133(5) Uani 1 1 d . . . C9 C -0.0216(2) 0.22605(17) 0.02910(16) 0.0183(5) Uani 1 1 d . . . H9 H -0.0633 0.1730 -0.0275 0.022 Uiso 1 1 calc R . . C10 C -0.0763(2) 0.26145(17) 0.09679(16) 0.0187(5) Uani 1 1 d . . . H10 H -0.1594 0.2376 0.0965 0.022 Uiso 1 1 calc R . . C11 C 0.0158(2) 0.34149(16) 0.16846(15) 0.0148(5) Uani 1 1 d . . . C12 C 0.0186(2) 0.41332(17) 0.25022(16) 0.0187(5) Uani 1 1 d . . . H12 H -0.0536 0.4144 0.2722 0.022 Uiso 1 1 calc R . . C13 C 0.1286(2) 0.48283(17) 0.29853(16) 0.0190(5) Uani 1 1 d . . . H13 H 0.1332 0.5324 0.3549 0.023 Uiso 1 1 calc R . . C14 C 0.2329(2) 0.48075(16) 0.26513(15) 0.0168(5) Uani 1 1 d . . . H14 H 0.3081 0.5289 0.3009 0.020 Uiso 1 1 calc R . . C15 C 0.1574(2) 0.17344(16) -0.09808(15) 0.0160(5) Uani 1 1 d . . . C16 C 0.1620(2) 0.16065(17) -0.18693(16) 0.0193(5) Uani 1 1 d . . . C17 C 0.1147(2) 0.07402(18) -0.26143(17) 0.0249(6) Uani 1 1 d . . . H17 H 0.1136 0.0675 -0.3210 0.030 Uiso 1 1 calc R . . C18 C 0.0691(2) -0.00277(18) -0.25163(18) 0.0274(6) Uani 1 1 d . . . C19 C 0.0858(2) 0.00770(17) -0.16271(19) 0.0263(6) Uani 1 1 d . . . H19 H 0.0656 -0.0450 -0.1533 0.032 Uiso 1 1 calc R . . C20 C 0.1316(2) 0.09388(17) -0.08611(17) 0.0203(5) Uani 1 1 d . . . C21 C 0.2263(3) 0.23696(19) -0.20387(18) 0.0266(6) Uani 1 1 d . . . H21A H 0.2721 0.2125 -0.2488 0.040 Uiso 1 1 calc R . . H21B H 0.2868 0.2846 -0.1459 0.040 Uiso 1 1 calc R . . H21C H 0.1617 0.2631 -0.2278 0.040 Uiso 1 1 calc R . . C22 C 0.0062(3) -0.0943(2) -0.3341(2) 0.0419(8) Uani 1 1 d . . . H22A H -0.0760 -0.0921 -0.3686 0.063 Uiso 1 1 calc R . . H22B H -0.0077 -0.1416 -0.3133 0.063 Uiso 1 1 calc R . . H22C H 0.0614 -0.1086 -0.3738 0.063 Uiso 1 1 calc R . . C23 C 0.1580(3) 0.09518(19) 0.00795(19) 0.0286(6) Uani 1 1 d . . . H23A H 0.2185 0.1529 0.0542 0.043 Uiso 1 1 calc R . . H23B H 0.1943 0.0441 0.0068 0.043 Uiso 1 1 calc R . . H23C H 0.0781 0.0894 0.0236 0.043 Uiso 1 1 calc R . . C24 C 0.4709(2) 0.34560(16) 0.20075(15) 0.0161(5) Uani 1 1 d . . . H24 H 0.4086 0.3127 0.2197 0.019 Uiso 1 1 calc R . . C25 C 0.5187(2) 0.43952(16) 0.26059(15) 0.0151(5) Uani 1 1 d . . . H25 H 0.4831 0.4608 0.3136 0.018 Uiso 1 1 calc R . . C26 C 0.6541(2) 0.49349(18) 0.28234(17) 0.0211(5) Uani 1 1 d . . . H26A H 0.7112 0.4517 0.2744 0.025 Uiso 1 1 calc R . . H26B H 0.6841 0.5403 0.3475 0.025 Uiso 1 1 calc R . . C27 C 0.6623(2) 0.54041(18) 0.22020(17) 0.0219(5) Uani 1 1 d . . . H27A H 0.6491 0.6024 0.2500 0.026 Uiso 1 1 calc R . . H27B H 0.7488 0.5472 0.2130 0.026 Uiso 1 1 calc R . . C28 C 0.5649(2) 0.48759(17) 0.12642(16) 0.0176(5) Uani 1 1 d . . . H28 H 0.5513 0.5240 0.0910 0.021 Uiso 1 1 calc R . . C29 C 0.5389(2) 0.39316(17) 0.07064(16) 0.0178(5) Uani 1 1 d . . . H29 H 0.5106 0.3751 0.0031 0.021 Uiso 1 1 calc R . . C30 C 0.6095(2) 0.32981(18) 0.09563(17) 0.0220(5) Uani 1 1 d . . . H30A H 0.6970 0.3650 0.1362 0.026 Uiso 1 1 calc R . . H30B H 0.6162 0.2813 0.0388 0.026 Uiso 1 1 calc R . . C31 C 0.5424(2) 0.28562(17) 0.14455(17) 0.0208(5) Uani 1 1 d . . . H31A H 0.4817 0.2269 0.0980 0.025 Uiso 1 1 calc R . . H31B H 0.6066 0.2720 0.1856 0.025 Uiso 1 1 calc R . . Rh2 Rh 0.522649(17) 0.076912(12) 0.313879(12) 0.01558(5) Uani 1 1 d . . . N5 N 0.53375(17) 0.29777(13) 0.43572(12) 0.0128(4) Uani 1 1 d . A . N6 N 0.63835(17) 0.20179(13) 0.33657(12) 0.0143(4) Uani 1 1 d . A . N7 N 0.55030(17) 0.21815(13) 0.53353(13) 0.0148(4) Uani 1 1 d . A . N8 N 0.64594(17) 0.10464(13) 0.44509(13) 0.0152(4) Uani 1 1 d . A . C32 C 0.6247(2) 0.28400(16) 0.39145(15) 0.0132(4) Uani 1 1 d . . . C33 C 0.5587(2) 0.39160(16) 0.48648(15) 0.0166(5) Uani 1 1 d . . . H33 H 0.5104 0.4207 0.5249 0.020 Uiso 1 1 calc R A . C34 C 0.6604(2) 0.43757(16) 0.47512(15) 0.0165(5) Uani 1 1 d . A . H34 H 0.6936 0.5019 0.5022 0.020 Uiso 1 1 calc R . . C35 C 0.7070(2) 0.36926(16) 0.41420(15) 0.0149(5) Uani 1 1 d . A . C36 C 0.8096(2) 0.36818(17) 0.37911(16) 0.0178(5) Uani 1 1 d . . . H36 H 0.8674 0.4234 0.3927 0.021 Uiso 1 1 calc R A . C37 C 0.8249(2) 0.28394(17) 0.32359(16) 0.0199(5) Uani 1 1 d . A . H37 H 0.8945 0.2809 0.2989 0.024 Uiso 1 1 calc R . . C38 C 0.7394(2) 0.20409(17) 0.30394(16) 0.0186(5) Uani 1 1 d . . . H38 H 0.7525 0.1476 0.2652 0.022 Uiso 1 1 calc R A . C39 C 0.6398(2) 0.16896(16) 0.52503(15) 0.0146(5) Uani 1 1 d . . . C40 C 0.5838(2) 0.27842(16) 0.62603(16) 0.0184(5) Uani 1 1 d . . . H40 H 0.5383 0.3220 0.6515 0.022 Uiso 1 1 calc R A . C41 C 0.6900(2) 0.26784(17) 0.67643(16) 0.0205(5) Uani 1 1 d . A . H41 H 0.7295 0.3009 0.7411 0.025 Uiso 1 1 calc R . . C42 C 0.7293(2) 0.19750(16) 0.61277(16) 0.0181(5) Uani 1 1 d . A . C43 C 0.8306(2) 0.15635(18) 0.61685(17) 0.0223(5) Uani 1 1 d . . . H43 H 0.8925 0.1727 0.6738 0.027 Uiso 1 1 calc R A . C44 C 0.8378(2) 0.09113(17) 0.53527(17) 0.0225(5) Uani 1 1 d . A . H44 H 0.9059 0.0621 0.5356 0.027 Uiso 1 1 calc R . . C45 C 0.7456(2) 0.06756(17) 0.45231(17) 0.0200(5) Uani 1 1 d . . . H45 H 0.7538 0.0225 0.3975 0.024 Uiso 1 1 calc R A . C46 C 0.3254(2) 0.24978(15) 0.47672(15) 0.0142(5) Uani 1 1 d . . . C47 C 0.2730(2) 0.22252(15) 0.53496(15) 0.0146(5) Uani 1 1 d . . . C48 C 0.1711(2) 0.25337(16) 0.56166(15) 0.0165(5) Uani 1 1 d . . . H48 H 0.1400 0.2358 0.6027 0.020 Uiso 1 1 calc R . . C49 C 0.1132(2) 0.30901(16) 0.53037(15) 0.0162(5) Uani 1 1 d . . . C50 C 0.1538(2) 0.32599(15) 0.46412(15) 0.0146(5) Uani 1 1 d . . . H50 H 0.1113 0.3596 0.4377 0.017 Uiso 1 1 calc R . . C51 C 0.2548(2) 0.29538(15) 0.43496(15) 0.0139(5) Uani 1 1 d . . . C52 C 0.3146(2) 0.15246(17) 0.56457(17) 0.0213(5) Uani 1 1 d . . . H52A H 0.3854 0.1835 0.6220 0.032 Uiso 1 1 calc R . . H52B H 0.3424 0.1089 0.5165 0.032 Uiso 1 1 calc R . . H52C H 0.2428 0.1197 0.5743 0.032 Uiso 1 1 calc R . . C53 C 0.0065(2) 0.34445(19) 0.56399(18) 0.0244(6) Uani 1 1 d . . . H53A H -0.0050 0.3960 0.5505 0.037 Uiso 1 1 calc R . . H53B H 0.0278 0.3648 0.6306 0.037 Uiso 1 1 calc R . . H53C H -0.0727 0.2956 0.5327 0.037 Uiso 1 1 calc R . . C54 C 0.2774(2) 0.30664(17) 0.35272(16) 0.0185(5) Uani 1 1 d . . . H54A H 0.1972 0.3075 0.3145 0.028 Uiso 1 1 calc R . . H54B H 0.3084 0.2555 0.3163 0.028 Uiso 1 1 calc R . . H54C H 0.3411 0.3642 0.3744 0.028 Uiso 1 1 calc R . . C56A C 0.4919(3) 0.0305(2) 0.16974(17) 0.0339(7) Uani 0.538(14) 1 d P A 1 H56A H 0.5430 0.0781 0.1593 0.041 Uiso 0.538(14) 1 calc PR A 1 C57A C 0.5255(8) -0.0587(5) 0.1245(5) 0.0309(17) Uani 0.538(14) 1 d P A 1 H57A H 0.6183 -0.0479 0.1325 0.037 Uiso 0.538(14) 1 calc PR A 1 H57B H 0.4793 -0.0897 0.0578 0.037 Uiso 0.538(14) 1 calc PR A 1 C58A C 0.4865(4) -0.1194(2) 0.1709(3) 0.0533(10) Uani 0.538(14) 1 d P A 1 H58A H 0.3985 -0.1577 0.1353 0.064 Uiso 0.538(14) 1 calc PR A 1 H58B H 0.5436 -0.1609 0.1675 0.064 Uiso 0.538(14) 1 calc PR A 1 C56B C 0.4919(3) 0.0305(2) 0.16974(17) 0.0339(7) Uani 0.462(14) 1 d P A 2 H56B H 0.5457 0.0670 0.1488 0.041 Uiso 0.462(14) 1 calc PR A 2 C57B C 0.4614(14) -0.0765(7) 0.1186(6) 0.044(3) Uani 0.462(14) 1 d P A 2 H57C H 0.3697 -0.1001 0.0831 0.053 Uiso 0.462(14) 1 calc PR A 2 H57D H 0.5102 -0.0933 0.0738 0.053 Uiso 0.462(14) 1 calc PR A 2 C58B C 0.4865(4) -0.1194(2) 0.1709(3) 0.0533(10) Uani 0.462(14) 1 d P A 2 H58C H 0.5694 -0.1345 0.1693 0.064 Uiso 0.462(14) 1 calc PR A 2 H58D H 0.4203 -0.1777 0.1434 0.064 Uiso 0.462(14) 1 calc PR A 2 C59 C 0.4919(3) -0.06603(18) 0.2712(2) 0.0340(7) Uani 1 1 d . A . H59 H 0.5483 -0.0825 0.3149 0.041 Uiso 1 1 calc R B 1 C60 C 0.3889(3) -0.03677(18) 0.29891(19) 0.0295(6) Uani 1 1 d . A . H60 H 0.3820 -0.0371 0.3577 0.035 Uiso 1 1 calc R C 1 C55A C 0.3858(2) 0.05875(19) 0.19348(17) 0.0247(6) Uani 0.538(14) 1 d PU A 1 H55A H 0.3845 0.1191 0.1932 0.030 Uiso 0.538(14) 1 calc PR A 1 C61A C 0.2545(13) -0.0602(10) 0.2219(9) 0.023(2) Uani 0.538(14) 1 d PU A 1 H61A H 0.2406 -0.1210 0.1699 0.028 Uiso 0.538(14) 1 calc PR A 1 H61B H 0.1839 -0.0626 0.2490 0.028 Uiso 0.538(14) 1 calc PR A 1 C62A C 0.2539(8) 0.0105(7) 0.1871(7) 0.0314(19) Uani 0.538(14) 1 d PU A 1 H62A H 0.2139 0.0570 0.2227 0.038 Uiso 0.538(14) 1 calc PR A 1 H62B H 0.2002 -0.0191 0.1219 0.038 Uiso 0.538(14) 1 calc PR A 1 C55B C 0.3858(2) 0.05875(19) 0.19348(17) 0.0247(6) Uani 0.462(14) 1 d PU A 2 H55B H 0.3697 0.1151 0.1890 0.030 Uiso 0.462(14) 1 calc PR A 2 C61B C 0.2675(17) -0.0430(12) 0.2466(10) 0.028(3) Uani 0.462(14) 1 d PU A 2 H61C H 0.2281 0.0000 0.2872 0.033 Uiso 0.462(14) 1 calc PR A 2 H61D H 0.2136 -0.1056 0.2229 0.033 Uiso 0.462(14) 1 calc PR A 2 C62B C 0.2683(9) -0.0209(7) 0.1627(6) 0.0208(18) Uani 0.462(14) 1 d PU A 2 H62C H 0.2726 -0.0755 0.1100 0.025 Uiso 0.462(14) 1 calc PR A 2 H62D H 0.1891 -0.0036 0.1432 0.025 Uiso 0.462(14) 1 calc PR A 2 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 0.01042(8) 0.01518(10) 0.00940(9) 0.00540(7) 0.00266(7) 0.00272(7) N1 0.0155(9) 0.0164(10) 0.0099(9) 0.0040(8) 0.0022(8) 0.0034(8) N2 0.0139(9) 0.0153(10) 0.0123(9) 0.0062(8) 0.0056(8) 0.0049(8) N3 0.0127(9) 0.0150(10) 0.0124(9) 0.0045(8) 0.0030(7) 0.0017(8) N4 0.0134(9) 0.0145(10) 0.0120(9) 0.0060(8) 0.0038(7) 0.0047(8) B1 0.0116(11) 0.0165(14) 0.0121(12) 0.0045(11) 0.0012(10) 0.0016(10) B2 0.0143(12) 0.0098(13) 0.0138(12) 0.0041(10) 0.0040(10) 0.0027(10) C1 0.0143(10) 0.0177(12) 0.0109(11) 0.0058(9) 0.0059(9) 0.0051(9) C2 0.0149(11) 0.0248(14) 0.0107(11) 0.0034(10) 0.0003(9) 0.0021(10) C3 0.0165(11) 0.0327(15) 0.0171(12) 0.0126(11) 0.0028(10) 0.0089(11) C4 0.0160(11) 0.0253(14) 0.0170(12) 0.0130(10) 0.0074(9) 0.0093(10) C5 0.0229(12) 0.0289(15) 0.0267(14) 0.0198(12) 0.0111(11) 0.0134(11) C6 0.0233(12) 0.0171(13) 0.0282(14) 0.0131(11) 0.0140(11) 0.0073(10) C7 0.0176(11) 0.0169(13) 0.0161(12) 0.0055(10) 0.0077(9) 0.0030(10) C8 0.0122(10) 0.0168(12) 0.0125(11) 0.0077(9) 0.0036(9) 0.0053(9) C9 0.0146(11) 0.0176(13) 0.0195(12) 0.0078(10) 0.0024(9) 0.0005(10) C10 0.0121(11) 0.0220(13) 0.0236(13) 0.0124(11) 0.0051(10) 0.0025(10) C11 0.0133(10) 0.0197(13) 0.0170(11) 0.0121(10) 0.0064(9) 0.0058(9) C12 0.0183(11) 0.0264(14) 0.0211(12) 0.0152(11) 0.0115(10) 0.0114(10) C13 0.0236(12) 0.0212(13) 0.0147(12) 0.0074(10) 0.0092(10) 0.0097(11) C14 0.0190(11) 0.0166(12) 0.0133(11) 0.0057(10) 0.0031(9) 0.0056(10) C15 0.0113(10) 0.0187(13) 0.0132(11) 0.0035(10) 0.0022(9) 0.0031(9) C16 0.0163(11) 0.0228(14) 0.0174(12) 0.0061(10) 0.0057(10) 0.0084(10) C17 0.0189(12) 0.0287(15) 0.0157(12) -0.0009(11) 0.0031(10) 0.0084(11) C18 0.0130(11) 0.0211(14) 0.0282(14) -0.0055(11) 0.0014(10) 0.0042(10) C19 0.0173(12) 0.0140(13) 0.0425(17) 0.0075(12) 0.0095(12) 0.0036(10) C20 0.0168(11) 0.0180(13) 0.0258(13) 0.0087(11) 0.0076(10) 0.0048(10) C21 0.0312(14) 0.0318(16) 0.0220(13) 0.0118(12) 0.0161(11) 0.0119(12) C22 0.0240(14) 0.0273(17) 0.0402(18) -0.0125(14) 0.0010(13) 0.0035(13) C23 0.0342(15) 0.0243(15) 0.0340(15) 0.0175(13) 0.0120(12) 0.0110(12) C24 0.0157(11) 0.0220(13) 0.0144(11) 0.0126(10) 0.0031(9) 0.0046(10) C25 0.0150(11) 0.0202(13) 0.0103(11) 0.0090(10) 0.0017(9) 0.0020(10) C26 0.0171(11) 0.0233(14) 0.0181(12) 0.0091(11) -0.0003(10) 0.0003(10) C27 0.0154(11) 0.0264(14) 0.0211(13) 0.0109(11) 0.0029(10) 0.0001(10) C28 0.0137(11) 0.0227(13) 0.0198(12) 0.0128(11) 0.0064(9) 0.0023(10) C29 0.0139(11) 0.0264(14) 0.0167(12) 0.0106(10) 0.0094(9) 0.0048(10) C30 0.0176(11) 0.0253(14) 0.0248(13) 0.0101(11) 0.0093(10) 0.0099(11) C31 0.0219(12) 0.0192(13) 0.0221(13) 0.0098(11) 0.0053(10) 0.0080(10) Rh2 0.01695(9) 0.01160(10) 0.01386(9) 0.00403(8) -0.00002(7) 0.00321(7) N5 0.0119(9) 0.0114(10) 0.0149(9) 0.0051(8) 0.0048(7) 0.0031(8) N6 0.0150(9) 0.0162(10) 0.0126(9) 0.0073(8) 0.0035(8) 0.0051(8) N7 0.0149(9) 0.0132(10) 0.0148(10) 0.0054(8) 0.0033(8) 0.0030(8) N8 0.0144(9) 0.0127(10) 0.0176(10) 0.0076(8) 0.0019(8) 0.0027(8) C32 0.0123(10) 0.0167(12) 0.0122(11) 0.0082(9) 0.0028(9) 0.0042(9) C33 0.0189(11) 0.0152(12) 0.0151(11) 0.0056(10) 0.0050(9) 0.0063(10) C34 0.0172(11) 0.0135(12) 0.0153(11) 0.0052(10) 0.0013(9) 0.0023(9) C35 0.0152(11) 0.0152(12) 0.0134(11) 0.0077(10) 0.0007(9) 0.0026(9) C36 0.0138(11) 0.0236(14) 0.0185(12) 0.0135(11) 0.0035(9) 0.0024(10) C37 0.0159(11) 0.0298(15) 0.0197(12) 0.0144(11) 0.0081(10) 0.0082(11) C38 0.0188(11) 0.0233(14) 0.0161(12) 0.0094(10) 0.0059(10) 0.0102(10) C39 0.0129(10) 0.0143(12) 0.0178(12) 0.0093(10) 0.0036(9) 0.0018(9) C40 0.0219(12) 0.0157(13) 0.0153(12) 0.0049(10) 0.0066(10) 0.0025(10) C41 0.0205(12) 0.0220(14) 0.0145(12) 0.0063(10) 0.0025(10) 0.0016(10) C42 0.0156(11) 0.0182(13) 0.0181(12) 0.0094(10) 0.0015(9) -0.0009(10) C43 0.0178(12) 0.0271(14) 0.0213(13) 0.0137(11) 0.0003(10) 0.0032(11) C44 0.0174(12) 0.0199(14) 0.0287(14) 0.0111(11) 0.0022(10) 0.0070(10) C45 0.0194(12) 0.0175(13) 0.0225(13) 0.0086(11) 0.0048(10) 0.0067(10) C46 0.0142(10) 0.0094(11) 0.0160(11) 0.0037(9) 0.0042(9) 0.0014(9) C47 0.0152(11) 0.0130(12) 0.0118(11) 0.0038(9) 0.0019(9) 0.0009(9) C48 0.0181(11) 0.0179(13) 0.0111(11) 0.0049(10) 0.0053(9) 0.0008(10) C49 0.0128(10) 0.0144(12) 0.0132(11) 0.0002(9) 0.0023(9) -0.0004(9) C50 0.0138(10) 0.0117(12) 0.0152(11) 0.0049(9) 0.0011(9) 0.0027(9) C51 0.0139(10) 0.0119(12) 0.0117(11) 0.0036(9) 0.0019(9) -0.0007(9) C52 0.0224(12) 0.0228(14) 0.0273(14) 0.0171(11) 0.0115(11) 0.0073(11) C53 0.0234(13) 0.0307(15) 0.0245(13) 0.0131(12) 0.0124(11) 0.0121(12) C54 0.0193(12) 0.0228(13) 0.0164(12) 0.0103(10) 0.0060(10) 0.0083(10) C56A 0.0486(18) 0.0325(17) 0.0127(13) 0.0030(12) 0.0075(12) 0.0118(14) C57A 0.021(3) 0.032(4) 0.024(3) -0.001(3) 0.008(3) 0.001(3) C58A 0.058(2) 0.0213(17) 0.066(2) 0.0008(17) 0.0254(19) 0.0112(16) C56B 0.0486(18) 0.0325(17) 0.0127(13) 0.0030(12) 0.0075(12) 0.0118(14) C57B 0.056(7) 0.029(5) 0.032(4) -0.003(4) 0.011(5) 0.017(5) C58B 0.058(2) 0.0213(17) 0.066(2) 0.0008(17) 0.0254(19) 0.0112(16) C59 0.0334(15) 0.0144(14) 0.0389(17) 0.0084(12) -0.0093(13) 0.0031(12) C60 0.0402(16) 0.0199(14) 0.0238(14) 0.0115(12) 0.0042(12) -0.0025(12) C55A 0.0223(12) 0.0275(15) 0.0187(13) 0.0123(11) -0.0044(10) -0.0001(11) C61A 0.012(3) 0.027(6) 0.019(6) 0.005(4) -0.003(4) -0.004(4) C62A 0.028(3) 0.028(5) 0.025(5) 0.010(4) -0.008(3) -0.002(3) C55B 0.0223(12) 0.0275(15) 0.0187(13) 0.0123(11) -0.0044(10) -0.0001(11) C61B 0.028(5) 0.024(6) 0.012(6) -0.002(5) -0.001(5) -0.014(4) C62B 0.014(3) 0.015(4) 0.015(4) -0.006(3) -0.001(3) -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 Rh1 C24 2.106(2) . ? Rh1 N4 2.1138(18) . ? Rh1 C25 2.122(2) . ? Rh1 C29 2.134(2) . ? Rh1 N2 2.1349(18) . ? Rh1 C28 2.141(2) . ? N1 C1 1.363(3) . ? N1 C2 1.389(3) . ? N1 B1 1.560(3) . ? N2 C1 1.348(3) . ? N2 C7 1.348(3) . ? N3 C8 1.366(3) . ? N3 C9 1.386(3) . ? N3 B1 1.563(3) . ? N4 C14 1.346(3) . ? N4 C8 1.352(3) . ? B1 C15 1.618(3) . ? B1 H1B 1.0000 . ? B2 N5 1.560(3) . ? B2 N7 1.566(3) . ? B2 C46 1.619(3) . ? B2 H2B 1.0000 . ? C1 C4 1.426(3) . ? C2 C3 1.357(3) . ? C2 H2 0.9500 . ? C3 C4 1.431(3) . ? C3 H3 0.9500 . ? C4 C5 1.383(4) . ? C5 C6 1.381(4) . ? C5 H5 0.9500 . ? C6 C7 1.387(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C11 1.423(3) . ? C9 C10 1.359(3) . ? C9 H9 0.9500 . ? C10 C11 1.428(3) . ? C10 H10 0.9500 . ? C11 C12 1.390(3) . ? C12 C13 1.377(3) . ? C12 H12 0.9500 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C20 1.406(3) . ? C15 C16 1.420(3) . ? C16 C17 1.393(3) . ? C16 C21 1.516(4) . ? C17 C18 1.383(4) . ? C17 H17 0.9500 . ? C18 C19 1.385(4) . ? C18 C22 1.509(4) . ? C19 C20 1.403(3) . ? C19 H19 0.9500 . ? C20 C23 1.518(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.407(3) . ? C24 C31 1.511(3) . ? C24 H24 1.0000 . ? C25 C26 1.522(3) . ? C25 H25 1.0000 . ? C26 C27 1.530(3) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.507(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.404(3) . ? C28 H28 1.0000 . ? C29 C30 1.522(3) . ? C29 H29 1.0000 . ? C30 C31 1.530(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? Rh2 C55A 2.114(2) . ? Rh2 N6 2.115(2) . ? Rh2 C60 2.117(3) . ? Rh2 C59 2.125(3) . ? Rh2 C56A 2.132(3) . ? Rh2 N8 2.1369(19) . ? N5 C32 1.366(3) . ? N5 C33 1.385(3) . ? N6 C32 1.350(3) . ? N6 C38 1.351(3) . ? N7 C39 1.364(3) . ? N7 C40 1.383(3) . ? N8 C45 1.342(3) . ? N8 C39 1.351(3) . ? C32 C35 1.423(3) . ? C33 C34 1.362(3) . ? C33 H33 0.9500 . ? C34 C35 1.428(3) . ? C34 H34 0.9500 . ? C35 C36 1.387(3) . ? C36 C37 1.385(3) . ? C36 H36 0.9500 . ? C37 C38 1.385(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C42 1.423(3) . ? C40 C41 1.366(3) . ? C40 H40 0.9500 . ? C41 C42 1.420(3) . ? C41 H41 0.9500 . ? C42 C43 1.395(3) . ? C43 C44 1.380(4) . ? C43 H43 0.9500 . ? C44 C45 1.395(3) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.415(3) . ? C46 C51 1.418(3) . ? C47 C48 1.391(3) . ? C47 C52 1.517(3) . ? C48 C49 1.389(3) . ? C48 H48 0.9500 . ? C49 C50 1.388(3) . ? C49 C53 1.510(3) . ? C50 C51 1.394(3) . ? C50 H50 0.9500 . ? C51 C54 1.520(3) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C56A C55A 1.402(4) . ? C56A C57A 1.504(8) . ? C56A H56A 1.0000 . ? C57A C58A 1.559(9) . ? C57A H57A 0.9900 . ? C57A H57B 0.9900 . ? C58A C59 1.525(5) . ? C58A H58A 0.9900 . ? C58A H58B 0.9900 . ? C57B H57C 0.9900 . ? C57B H57D 0.9900 . ? C59 C60 1.400(4) . ? C59 H59 1.0000 . ? C60 C61B 1.401(18) . ? C60 C61A 1.619(13) . ? C60 H60 1.0000 . ? C55A C62A 1.527(10) . ? C55A H55A 1.0000 . ? C61A C62A 1.498(19) . ? C61A H61A 0.9900 . ? C61A H61B 0.9900 . ? C62A H62A 0.9900 . ? C62A H62B 0.9900 . ? C61B C62B 1.58(2) . ? C61B H61C 0.9900 . ? C61B H61D 0.9900 . ? C62B H62C 0.9900 . ? C62B H62D 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Rh1 N4 91.07(8) . . ? C24 Rh1 C25 38.86(9) . . ? N4 Rh1 C25 91.77(8) . . ? C24 Rh1 C29 82.29(9) . . ? N4 Rh1 C29 167.30(8) . . ? C25 Rh1 C29 89.82(9) . . ? C24 Rh1 N2 173.83(8) . . ? N4 Rh1 N2 85.50(7) . . ? C25 Rh1 N2 146.22(8) . . ? C29 Rh1 N2 100.08(8) . . ? C24 Rh1 C28 98.35(9) . . ? N4 Rh1 C28 154.23(8) . . ? C25 Rh1 C28 81.10(9) . . ? C29 Rh1 C28 38.34(9) . . ? N2 Rh1 C28 86.90(8) . . ? C1 N1 C2 105.68(19) . . ? C1 N1 B1 127.65(18) . . ? C2 N1 B1 126.0(2) . . ? C1 N2 C7 115.71(19) . . ? C1 N2 Rh1 121.80(15) . . ? C7 N2 Rh1 122.02(15) . . ? C8 N3 C9 105.60(18) . . ? C8 N3 B1 124.85(19) . . ? C9 N3 B1 126.39(19) . . ? C14 N4 C8 115.65(19) . . ? C14 N4 Rh1 121.70(15) . . ? C8 N4 Rh1 122.59(14) . . ? N1 B1 N3 104.69(17) . . ? N1 B1 C15 112.92(18) . . ? N3 B1 C15 113.3(2) . . ? N1 B1 H1B 108.6 . . ? N3 B1 H1B 108.6 . . ? C15 B1 H1B 108.6 . . ? N5 B2 N7 103.98(18) . . ? N5 B2 C46 113.40(18) . . ? N7 B2 C46 113.96(19) . . ? N5 B2 H2B 108.4 . . ? N7 B2 H2B 108.4 . . ? C46 B2 H2B 108.4 . . ? N2 C1 N1 125.7(2) . . ? N2 C1 C4 123.9(2) . . ? N1 C1 C4 110.4(2) . . ? C3 C2 N1 112.1(2) . . ? C3 C2 H2 123.9 . . ? N1 C2 H2 123.9 . . ? C2 C3 C4 106.6(2) . . ? C2 C3 H3 126.7 . . ? C4 C3 H3 126.7 . . ? C5 C4 C1 118.5(2) . . ? C5 C4 C3 136.2(2) . . ? C1 C4 C3 105.2(2) . . ? C6 C5 C4 117.6(2) . . ? C6 C5 H5 121.2 . . ? C4 C5 H5 121.2 . . ? C5 C6 C7 120.6(2) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? N2 C7 C6 123.7(2) . . ? N2 C7 H7 118.2 . . ? C6 C7 H7 118.2 . . ? N4 C8 N3 125.4(2) . . ? N4 C8 C11 124.2(2) . . ? N3 C8 C11 110.4(2) . . ? C10 C9 N3 112.2(2) . . ? C10 C9 H9 123.9 . . ? N3 C9 H9 123.9 . . ? C9 C10 C11 106.5(2) . . ? C9 C10 H10 126.7 . . ? C11 C10 H10 126.7 . . ? C12 C11 C8 117.6(2) . . ? C12 C11 C10 136.7(2) . . ? C8 C11 C10 105.3(2) . . ? C13 C12 C11 118.3(2) . . ? C13 C12 H12 120.9 . . ? C11 C12 H12 120.8 . . ? C12 C13 C14 120.2(2) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? N4 C14 C13 123.8(2) . . ? N4 C14 H14 118.1 . . ? C13 C14 H14 118.1 . . ? C20 C15 C16 116.4(2) . . ? C20 C15 B1 122.4(2) . . ? C16 C15 B1 121.2(2) . . ? C17 C16 C15 120.1(2) . . ? C17 C16 C21 117.3(2) . . ? C15 C16 C21 122.5(2) . . ? C18 C17 C16 122.3(2) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C19 117.1(2) . . ? C17 C18 C22 121.5(3) . . ? C19 C18 C22 121.4(3) . . ? C18 C19 C20 121.9(3) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C20 C15 120.3(2) . . ? C19 C20 C23 116.6(2) . . ? C15 C20 C23 123.0(2) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C31 125.3(2) . . ? C25 C24 Rh1 71.22(13) . . ? C31 C24 Rh1 110.22(15) . . ? C25 C24 H24 114.0 . . ? C31 C24 H24 114.0 . . ? Rh1 C24 H24 114.0 . . ? C24 C25 C26 124.1(2) . . ? C24 C25 Rh1 69.92(12) . . ? C26 C25 Rh1 114.14(15) . . ? C24 C25 H25 113.7 . . ? C26 C25 H25 113.7 . . ? Rh1 C25 H25 113.7 . . ? C25 C26 C27 111.92(19) . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26B 109.2 . . ? C27 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C28 C27 C26 112.3(2) . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.9 . . ? C29 C28 C27 125.6(2) . . ? C29 C28 Rh1 70.56(13) . . ? C27 C28 Rh1 111.07(16) . . ? C29 C28 H28 113.8 . . ? C27 C28 H28 113.8 . . ? Rh1 C28 H28 113.8 . . ? C28 C29 C30 124.2(2) . . ? C28 C29 Rh1 71.09(13) . . ? C30 C29 Rh1 112.41(16) . . ? C28 C29 H29 113.9 . . ? C30 C29 H29 113.9 . . ? Rh1 C29 H29 113.9 . . ? C29 C30 C31 112.24(19) . . ? C29 C30 H30A 109.2 . . ? C31 C30 H30A 109.2 . . ? C29 C30 H30B 109.2 . . ? C31 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? C24 C31 C30 112.8(2) . . ? C24 C31 H31A 109.0 . . ? C30 C31 H31A 109.0 . . ? C24 C31 H31B 109.0 . . ? C30 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C55A Rh2 N6 95.73(9) . . ? C55A Rh2 C60 82.45(11) . . ? N6 Rh2 C60 171.72(9) . . ? C55A Rh2 C59 92.99(11) . . ? N6 Rh2 C59 149.74(10) . . ? C60 Rh2 C59 38.54(11) . . ? C55A Rh2 C56A 38.55(11) . . ? N6 Rh2 C56A 88.56(10) . . ? C60 Rh2 C56A 94.89(12) . . ? C59 Rh2 C56A 80.42(12) . . ? C55A Rh2 N8 172.62(9) . . ? N6 Rh2 N8 84.27(7) . . ? C60 Rh2 N8 96.49(9) . . ? C59 Rh2 N8 90.64(9) . . ? C56A Rh2 N8 148.70(10) . . ? C32 N5 C33 105.59(19) . . ? C32 N5 B2 125.60(18) . . ? C33 N5 B2 125.38(19) . . ? C32 N6 C38 115.5(2) . . ? C32 N6 Rh2 122.76(15) . . ? C38 N6 Rh2 121.44(16) . . ? C39 N7 C40 105.85(18) . . ? C39 N7 B2 126.72(19) . . ? C40 N7 B2 125.45(19) . . ? C45 N8 C39 115.42(19) . . ? C45 N8 Rh2 121.38(16) . . ? C39 N8 Rh2 122.63(14) . . ? N6 C32 N5 125.5(2) . . ? N6 C32 C35 124.3(2) . . ? N5 C32 C35 110.16(19) . . ? C34 C33 N5 112.5(2) . . ? C34 C33 H33 123.8 . . ? N5 C33 H33 123.8 . . ? C33 C34 C35 106.0(2) . . ? C33 C34 H34 127.0 . . ? C35 C34 H34 127.0 . . ? C36 C35 C32 118.1(2) . . ? C36 C35 C34 136.0(2) . . ? C32 C35 C34 105.8(2) . . ? C37 C36 C35 117.8(2) . . ? C37 C36 H36 121.1 . . ? C35 C36 H36 121.1 . . ? C38 C37 C36 120.4(2) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? N6 C38 C37 123.9(2) . . ? N6 C38 H38 118.1 . . ? C37 C38 H38 118.1 . . ? N8 C39 N7 125.5(2) . . ? N8 C39 C42 124.5(2) . . ? N7 C39 C42 110.0(2) . . ? C41 C40 N7 112.1(2) . . ? C41 C40 H40 124.0 . . ? N7 C40 H40 124.0 . . ? C40 C41 C42 106.2(2) . . ? C40 C41 H41 126.9 . . ? C42 C41 H41 126.9 . . ? C43 C42 C41 136.1(2) . . ? C43 C42 C39 117.9(2) . . ? C41 C42 C39 106.0(2) . . ? C44 C43 C42 117.7(2) . . ? C44 C43 H43 121.1 . . ? C42 C43 H43 121.1 . . ? C43 C44 C45 120.4(2) . . ? C43 C44 H44 119.8 . . ? C45 C44 H44 119.8 . . ? N8 C45 C44 124.0(2) . . ? N8 C45 H45 118.0 . . ? C44 C45 H45 118.0 . . ? C47 C46 C51 116.18(19) . . ? C47 C46 B2 122.09(19) . . ? C51 C46 B2 121.6(2) . . ? C48 C47 C46 120.8(2) . . ? C48 C47 C52 116.0(2) . . ? C46 C47 C52 123.0(2) . . ? C49 C48 C47 122.2(2) . . ? C49 C48 H48 118.9 . . ? C47 C48 H48 118.9 . . ? C50 C49 C48 116.9(2) . . ? C50 C49 C53 122.3(2) . . ? C48 C49 C53 120.7(2) . . ? C49 C50 C51 122.3(2) . . ? C49 C50 H50 118.9 . . ? C51 C50 H50 118.9 . . ? C50 C51 C46 120.5(2) . . ? C50 C51 C54 116.91(19) . . ? C46 C51 C54 122.5(2) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53A 109.5 . . ? C49 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C49 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C55A C56A C57A 136.9(4) . . ? C55A C56A Rh2 70.04(14) . . ? C57A C56A Rh2 113.2(3) . . ? C55A C56A H56A 109.4 . . ? C57A C56A H56A 109.4 . . ? Rh2 C56A H56A 109.4 . . ? C56A C57A C58A 107.8(5) . . ? C56A C57A H57A 110.1 . . ? C58A C57A H57A 110.1 . . ? C56A C57A H57B 110.1 . . ? C58A C57A H57B 110.1 . . ? H57A C57A H57B 108.5 . . ? C59 C58A C57A 114.5(3) . . ? C59 C58A H58A 108.6 . . ? C57A C58A H58A 108.6 . . ? C59 C58A H58B 108.6 . . ? C57A C58A H58B 108.6 . . ? H58A C58A H58B 107.6 . . ? H57C C57B H57D 107.3 . . ? C60 C59 C58A 123.7(3) . . ? C60 C59 Rh2 70.40(15) . . ? C58A C59 Rh2 112.8(2) . . ? C60 C59 H59 114.1 . . ? C58A C59 H59 114.1 . . ? Rh2 C59 H59 114.1 . . ? C59 C60 C61B 130.5(7) . . ? C59 C60 C61A 119.6(5) . . ? C59 C60 Rh2 71.06(16) . . ? C61B C60 Rh2 110.0(8) . . ? C61A C60 Rh2 112.1(6) . . ? C59 C60 H60 115.5 . . ? C61B C60 H60 108.3 . . ? C61A C60 H60 115.5 . . ? Rh2 C60 H60 115.5 . . ? C56A C55A C62A 135.3(5) . . ? C56A C55A Rh2 71.41(14) . . ? C62A C55A Rh2 110.3(4) . . ? C56A C55A H55A 110.3 . . ? C62A C55A H55A 110.3 . . ? Rh2 C55A H55A 110.3 . . ? C62A C61A C60 110.8(10) . . ? C62A C61A H61A 109.5 . . ? C60 C61A H61A 109.5 . . ? C62A C61A H61B 109.5 . . ? C60 C61A H61B 109.5 . . ? H61A C61A H61B 108.1 . . ? C61A C62A C55A 114.3(8) . . ? C61A C62A H62A 108.7 . . ? C55A C62A H62A 108.7 . . ? C61A C62A H62B 108.7 . . ? C55A C62A H62B 108.7 . . ? H62A C62A H62B 107.6 . . ? C60 C61B C62B 113.9(13) . . ? C60 C61B H61C 108.8 . . ? C62B C61B H61C 108.8 . . ? C60 C61B H61D 108.8 . . ? C62B C61B H61D 108.8 . . ? H61C C61B H61D 107.7 . . ? C61B C62B H62C 110.0 . . ? C61B C62B H62D 110.0 . . ? H62C C62B H62D 108.4 . . ? 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 N4 Rh1 N2 C1 -72.44(17) . . . . ? C25 Rh1 N2 C1 -158.88(16) . . . . ? C29 Rh1 N2 C1 96.05(17) . . . . ? C28 Rh1 N2 C1 132.21(17) . . . . ? N4 Rh1 N2 C7 99.34(17) . . . . ? C25 Rh1 N2 C7 12.9(2) . . . . ? C29 Rh1 N2 C7 -92.18(18) . . . . ? C28 Rh1 N2 C7 -56.02(18) . . . . ? C24 Rh1 N4 C14 91.65(18) . . . . ? C25 Rh1 N4 C14 52.79(18) . . . . ? C29 Rh1 N4 C14 149.8(3) . . . . ? N2 Rh1 N4 C14 -93.49(17) . . . . ? C28 Rh1 N4 C14 -20.2(3) . . . . ? C24 Rh1 N4 C8 -91.30(17) . . . . ? C25 Rh1 N4 C8 -130.17(17) . . . . ? C29 Rh1 N4 C8 -33.1(4) . . . . ? N2 Rh1 N4 C8 83.56(17) . . . . ? C28 Rh1 N4 C8 156.83(19) . . . . ? C1 N1 B1 N3 87.2(2) . . . . ? C2 N1 B1 N3 -82.2(3) . . . . ? C1 N1 B1 C15 -149.1(2) . . . . ? C2 N1 B1 C15 41.4(3) . . . . ? C8 N3 B1 N1 -72.3(2) . . . . ? C9 N3 B1 N1 84.6(3) . . . . ? C8 N3 B1 C15 164.22(19) . . . . ? C9 N3 B1 C15 -38.8(3) . . . . ? C7 N2 C1 N1 -176.2(2) . . . . ? Rh1 N2 C1 N1 -4.0(3) . . . . ? C7 N2 C1 C4 1.8(3) . . . . ? Rh1 N2 C1 C4 174.09(16) . . . . ? C2 N1 C1 N2 177.4(2) . . . . ? B1 N1 C1 N2 6.2(4) . . . . ? C2 N1 C1 C4 -0.9(2) . . . . ? B1 N1 C1 C4 -172.1(2) . . . . ? C1 N1 C2 C3 1.8(3) . . . . ? B1 N1 C2 C3 173.2(2) . . . . ? N1 C2 C3 C4 -1.9(3) . . . . ? N2 C1 C4 C5 -2.1(3) . . . . ? N1 C1 C4 C5 176.2(2) . . . . ? N2 C1 C4 C3 -178.5(2) . . . . ? N1 C1 C4 C3 -0.2(3) . . . . ? C2 C3 C4 C5 -174.2(3) . . . . ? C2 C3 C4 C1 1.3(3) . . . . ? C1 C4 C5 C6 0.6(3) . . . . ? C3 C4 C5 C6 175.7(3) . . . . ? C4 C5 C6 C7 0.8(4) . . . . ? C1 N2 C7 C6 -0.3(3) . . . . ? Rh1 N2 C7 C6 -172.50(17) . . . . ? C5 C6 C7 N2 -1.1(4) . . . . ? C14 N4 C8 N3 175.6(2) . . . . ? Rh1 N4 C8 N3 -1.6(3) . . . . ? C14 N4 C8 C11 -2.1(3) . . . . ? Rh1 N4 C8 C11 -179.28(16) . . . . ? C9 N3 C8 N4 -178.0(2) . . . . ? B1 N3 C8 N4 -17.1(3) . . . . ? C9 N3 C8 C11 -0.1(2) . . . . ? B1 N3 C8 C11 160.83(19) . . . . ? C8 N3 C9 C10 -0.8(3) . . . . ? B1 N3 C9 C10 -161.3(2) . . . . ? N3 C9 C10 C11 1.4(3) . . . . ? N4 C8 C11 C12 4.2(3) . . . . ? N3 C8 C11 C12 -173.77(19) . . . . ? N4 C8 C11 C10 178.8(2) . . . . ? N3 C8 C11 C10 0.8(2) . . . . ? C9 C10 C11 C12 171.7(3) . . . . ? C9 C10 C11 C8 -1.3(2) . . . . ? C8 C11 C12 C13 -3.3(3) . . . . ? C10 C11 C12 C13 -175.7(3) . . . . ? C11 C12 C13 C14 0.6(3) . . . . ? C8 N4 C14 C13 -0.9(3) . . . . ? Rh1 N4 C14 C13 176.35(17) . . . . ? C12 C13 C14 N4 1.6(4) . . . . ? N1 B1 C15 C20 -150.7(2) . . . . ? N3 B1 C15 C20 -31.9(3) . . . . ? N1 B1 C15 C16 29.0(3) . . . . ? N3 B1 C15 C16 147.7(2) . . . . ? C20 C15 C16 C17 14.2(3) . . . . ? B1 C15 C16 C17 -165.5(2) . . . . ? C20 C15 C16 C21 -161.1(2) . . . . ? B1 C15 C16 C21 19.3(3) . . . . ? C15 C16 C17 C18 -4.0(3) . . . . ? C21 C16 C17 C18 171.5(2) . . . . ? C16 C17 C18 C19 -7.2(3) . . . . ? C16 C17 C18 C22 173.8(2) . . . . ? C17 C18 C19 C20 8.0(3) . . . . ? C22 C18 C19 C20 -173.1(2) . . . . ? C18 C19 C20 C15 2.5(4) . . . . ? C18 C19 C20 C23 -174.1(2) . . . . ? C16 C15 C20 C19 -13.4(3) . . . . ? B1 C15 C20 C19 166.2(2) . . . . ? C16 C15 C20 C23 163.0(2) . . . . ? B1 C15 C20 C23 -17.4(3) . . . . ? N4 Rh1 C24 C25 -91.49(14) . . . . ? C29 Rh1 C24 C25 99.38(14) . . . . ? C28 Rh1 C24 C25 64.45(15) . . . . ? N4 Rh1 C24 C31 146.79(17) . . . . ? C25 Rh1 C24 C31 -121.7(2) . . . . ? C29 Rh1 C24 C31 -22.34(17) . . . . ? C28 Rh1 C24 C31 -57.28(18) . . . . ? C31 C24 C25 C26 -4.2(3) . . . . ? Rh1 C24 C25 C26 -106.2(2) . . . . ? C31 C24 C25 Rh1 101.9(2) . . . . ? N4 Rh1 C25 C24 89.51(14) . . . . ? C29 Rh1 C25 C24 -77.88(14) . . . . ? N2 Rh1 C25 C24 174.05(13) . . . . ? C28 Rh1 C25 C24 -115.38(15) . . . . ? C24 Rh1 C25 C26 119.4(2) . . . . ? N4 Rh1 C25 C26 -151.10(17) . . . . ? C29 Rh1 C25 C26 41.51(18) . . . . ? N2 Rh1 C25 C26 -66.6(2) . . . . ? C28 Rh1 C25 C26 4.01(17) . . . . ? C24 C25 C26 C27 94.4(3) . . . . ? Rh1 C25 C26 C27 13.1(3) . . . . ? C25 C26 C27 C28 -30.6(3) . . . . ? C26 C27 C28 C29 -46.9(3) . . . . ? C26 C27 C28 Rh1 33.7(2) . . . . ? C24 Rh1 C28 C29 66.18(15) . . . . ? N4 Rh1 C28 C29 176.50(16) . . . . ? C25 Rh1 C28 C29 101.13(14) . . . . ? N2 Rh1 C28 C29 -110.55(14) . . . . ? C24 Rh1 C28 C27 -55.52(18) . . . . ? N4 Rh1 C28 C27 54.8(3) . . . . ? C25 Rh1 C28 C27 -20.57(17) . . . . ? C29 Rh1 C28 C27 -121.7(2) . . . . ? N2 Rh1 C28 C27 127.76(17) . . . . ? C27 C28 C29 C30 -2.2(4) . . . . ? Rh1 C28 C29 C30 -104.7(2) . . . . ? C27 C28 C29 Rh1 102.5(2) . . . . ? C24 Rh1 C29 C28 -114.03(15) . . . . ? N4 Rh1 C29 C28 -173.1(3) . . . . ? C25 Rh1 C29 C28 -75.78(14) . . . . ? N2 Rh1 C29 C28 71.74(14) . . . . ? C24 Rh1 C29 C30 6.09(17) . . . . ? N4 Rh1 C29 C30 -52.9(4) . . . . ? C25 Rh1 C29 C30 44.33(18) . . . . ? N2 Rh1 C29 C30 -168.14(16) . . . . ? C28 Rh1 C29 C30 120.1(2) . . . . ? C28 C29 C30 C31 93.1(3) . . . . ? Rh1 C29 C30 C31 11.3(3) . . . . ? C25 C24 C31 C30 -45.6(3) . . . . ? Rh1 C24 C31 C30 35.2(2) . . . . ? C29 C30 C31 C24 -30.6(3) . . . . ? N7 B2 N5 C32 74.6(2) . . . . ? C46 B2 N5 C32 -161.10(19) . . . . ? N7 B2 N5 C33 -81.5(2) . . . . ? C46 B2 N5 C33 42.8(3) . . . . ? C55A Rh2 N6 C32 93.18(18) . . . . ? C59 Rh2 N6 C32 -160.81(19) . . . . ? C56A Rh2 N6 C32 131.11(18) . . . . ? N8 Rh2 N6 C32 -79.40(17) . . . . ? C55A Rh2 N6 C38 -93.53(18) . . . . ? C59 Rh2 N6 C38 12.5(3) . . . . ? C56A Rh2 N6 C38 -55.60(18) . . . . ? N8 Rh2 N6 C38 93.89(17) . . . . ? N5 B2 N7 C39 -81.2(3) . . . . ? C46 B2 N7 C39 154.8(2) . . . . ? N5 B2 N7 C40 80.4(3) . . . . ? C46 B2 N7 C40 -43.5(3) . . . . ? N6 Rh2 N8 C45 -96.72(19) . . . . ? C60 Rh2 N8 C45 91.6(2) . . . . ? C59 Rh2 N8 C45 53.4(2) . . . . ? C56A Rh2 N8 C45 -19.0(3) . . . . ? N6 Rh2 N8 C39 74.22(18) . . . . ? C60 Rh2 N8 C39 -97.48(19) . . . . ? C59 Rh2 N8 C39 -135.67(19) . . . . ? C56A Rh2 N8 C39 151.9(2) . . . . ? C38 N6 C32 N5 -176.4(2) . . . . ? Rh2 N6 C32 N5 -2.7(3) . . . . ? C38 N6 C32 C35 1.1(3) . . . . ? Rh2 N6 C32 C35 174.74(16) . . . . ? B2 N5 C32 N6 17.8(3) . . . . ? C33 N5 C32 C35 -0.1(2) . . . . ? B2 N5 C32 C35 -160.01(19) . . . . ? C32 N5 C33 C34 0.8(2) . . . . ? B2 N5 C33 C34 160.8(2) . . . . ? N5 C33 C34 C35 -1.2(3) . . . . ? N6 C32 C35 C36 -1.2(3) . . . . ? N5 C32 C35 C36 176.65(19) . . . . ? N6 C32 C35 C34 -178.4(2) . . . . ? N5 C32 C35 C34 -0.6(2) . . . . ? C33 C34 C35 C36 -175.5(2) . . . . ? C33 C34 C35 C32 1.1(2) . . . . ? C32 C35 C36 C37 0.4(3) . . . . ? C34 C35 C36 C37 176.6(2) . . . . ? C35 C36 C37 C38 0.4(3) . . . . ? C32 N6 C38 C37 -0.2(3) . . . . ? Rh2 N6 C38 C37 -174.00(17) . . . . ? C36 C37 C38 N6 -0.5(4) . . . . ? C45 N8 C39 N7 177.1(2) . . . . ? Rh2 N8 C39 N7 5.7(3) . . . . ? C45 N8 C39 C42 -0.5(3) . . . . ? Rh2 N8 C39 C42 -171.98(18) . . . . ? C40 N7 C39 N8 -177.2(2) . . . . ? B2 N7 C39 N8 -12.7(4) . . . . ? C40 N7 C39 C42 0.7(3) . . . . ? B2 N7 C39 C42 165.3(2) . . . . ? C39 N7 C40 C41 -1.1(3) . . . . ? B2 N7 C40 C41 -165.9(2) . . . . ? N7 C40 C41 C42 1.0(3) . . . . ? C40 C41 C42 C43 176.7(3) . . . . ? C40 C41 C42 C39 -0.5(3) . . . . ? N8 C39 C42 C43 0.0(4) . . . . ? N7 C39 C42 C43 -178.0(2) . . . . ? N8 C39 C42 C41 177.8(2) . . . . ? N7 C39 C42 C41 -0.2(3) . . . . ? C41 C42 C43 C44 -176.5(3) . . . . ? C39 C42 C43 C44 0.5(4) . . . . ? C42 C43 C44 C45 -0.4(4) . . . . ? C39 N8 C45 C44 0.6(4) . . . . ? Rh2 N8 C45 C44 172.20(19) . . . . ? C43 C44 C45 N8 -0.2(4) . . . . ? N5 B2 C46 C47 -149.5(2) . . . . ? N7 B2 C46 C47 -30.8(3) . . . . ? N5 B2 C46 C51 34.4(3) . . . . ? N7 B2 C46 C51 153.1(2) . . . . ? C51 C46 C47 C48 -10.9(3) . . . . ? B2 C46 C47 C48 172.7(2) . . . . ? C51 C46 C47 C52 163.2(2) . . . . ? B2 C46 C47 C52 -13.1(3) . . . . ? C46 C47 C48 C49 2.4(3) . . . . ? C52 C47 C48 C49 -172.2(2) . . . . ? C47 C48 C49 C50 5.8(3) . . . . ? C47 C48 C49 C53 -177.4(2) . . . . ? C48 C49 C50 C51 -5.0(3) . . . . ? C53 C49 C50 C51 178.2(2) . . . . ? C49 C50 C51 C46 -3.8(3) . . . . ? C49 C50 C51 C54 171.5(2) . . . . ? C47 C46 C51 C50 11.6(3) . . . . ? B2 C46 C51 C50 -172.0(2) . . . . ? C47 C46 C51 C54 -163.5(2) . . . . ? B2 C46 C51 C54 12.9(3) . . . . ? N6 Rh2 C56A C55A -101.05(17) . . . . ? C60 Rh2 C56A C55A 71.41(18) . . . . ? C59 Rh2 C56A C55A 107.25(19) . . . . ? N8 Rh2 C56A C55A -177.56(16) . . . . ? C55A Rh2 C56A C57A -133.6(4) . . . . ? N6 Rh2 C56A C57A 125.4(4) . . . . ? C60 Rh2 C56A C57A -62.2(4) . . . . ? C59 Rh2 C56A C57A -26.3(4) . . . . ? N8 Rh2 C56A C57A 48.9(5) . . . . ? C55A C56A C57A C58A -48.1(8) . . . . ? Rh2 C56A C57A C58A 37.0(6) . . . . ? C56A C57A C58A C59 -29.6(7) . . . . ? C57A C58A C59 C60 90.2(5) . . . . ? C57A C58A C59 Rh2 9.2(5) . . . . ? C55A Rh2 C59 C60 -73.94(17) . . . . ? N6 Rh2 C59 C60 179.34(15) . . . . ? C56A Rh2 C59 C60 -110.52(18) . . . . ? N8 Rh2 C59 C60 99.64(16) . . . . ? C55A Rh2 C59 C58A 45.4(2) . . . . ? N6 Rh2 C59 C58A -61.4(3) . . . . ? C60 Rh2 C59 C58A 119.3(3) . . . . ? C56A Rh2 C59 C58A 8.8(2) . . . . ? N8 Rh2 C59 C58A -141.1(2) . . . . ? C58A C59 C60 C61B -4.3(12) . . . . ? Rh2 C59 C60 C61B 100.6(11) . . . . ? C58A C59 C60 C61A 0.4(8) . . . . ? Rh2 C59 C60 C61A 105.3(7) . . . . ? C58A C59 C60 Rh2 -104.9(3) . . . . ? C55A Rh2 C60 C59 104.52(17) . . . . ? C56A Rh2 C60 C59 67.95(18) . . . . ? N8 Rh2 C60 C59 -82.84(16) . . . . ? C55A Rh2 C60 C61B -22.7(7) . . . . ? C59 Rh2 C60 C61B -127.2(7) . . . . ? C56A Rh2 C60 C61B -59.3(7) . . . . ? N8 Rh2 C60 C61B 149.9(7) . . . . ? C55A Rh2 C60 C61A -10.6(5) . . . . ? C59 Rh2 C60 C61A -115.1(5) . . . . ? C56A Rh2 C60 C61A -47.1(5) . . . . ? N8 Rh2 C60 C61A 162.1(5) . . . . ? C57A C56A C55A C62A 2.6(8) . . . . ? Rh2 C56A C55A C62A -100.4(5) . . . . ? C57A C56A C55A Rh2 103.0(5) . . . . ? N6 Rh2 C55A C56A 80.43(18) . . . . ? C60 Rh2 C55A C56A -107.71(19) . . . . ? C59 Rh2 C55A C56A -70.56(19) . . . . ? N6 Rh2 C55A C62A -147.1(5) . . . . ? C60 Rh2 C55A C62A 24.7(5) . . . . ? C59 Rh2 C55A C62A 61.9(5) . . . . ? C56A Rh2 C55A C62A 132.4(5) . . . . ? C59 C60 C61A C62A -85.8(10) . . . . ? C61B C60 C61A C62A 76(7) . . . . ? Rh2 C60 C61A C62A -5.7(11) . . . . ? C60 C61A C62A C55A 26.9(14) . . . . ? C56A C55A C62A C61A 47.8(12) . . . . ? Rh2 C55A C62A C61A -35.9(11) . . . . ? C59 C60 C61B C62B -41.9(17) . . . . ? C61A C60 C61B C62B -63(6) . . . . ? Rh2 C60 C61B C62B 39.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 27.63 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 0.901 _refine_diff_density_min -0.987 _refine_diff_density_rms 0.078 data_rh09_0m _database_code_depnum_ccdc_archive 'CCDC 802702' #TrackingRef '- Ligands Li(MeCN)2[ArBai] and Complexes 4_6_9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Complex_6 _chemical_melting_point ? _chemical_formula_moiety '2(C31 H34 B Ir N4), 0.5(C6 H14)' _chemical_formula_sum 'C65 H75 B2 Ir2 N8' _chemical_formula_weight 1374.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' Ir Ir -1.4442 7.9887 '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 -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7485(5) _cell_length_b 13.7294(6) _cell_length_c 19.2199(8) _cell_angle_alpha 93.257(2) _cell_angle_beta 90.316(2) _cell_angle_gamma 100.612(2) _cell_volume 2782.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9817 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 27.54 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.07 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_max 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1370 _exptl_absorpt_coefficient_mu 4.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5705 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 47551 _diffrn_reflns_av_R_equivalents 0.0324 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.55 _reflns_number_total 12785 _reflns_number_gt 11303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _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^)+(0.0164P)^2^+1.6376P] 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 12785 _refine_ls_number_parameters 701 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0249 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0458 _refine_ls_wR_factor_gt 0.0441 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 Ir1 Ir -0.086931(8) 0.764657(7) 0.389040(4) 0.01258(3) Uani 1 1 d . . . B1 B 0.1847(3) 0.7829(2) 0.39137(14) 0.0159(6) Uani 1 1 d . . . H1 H 0.1001 0.7960 0.3768 0.019 Uiso 1 1 calc R . . N1 N 0.19675(18) 0.80901(15) 0.47118(10) 0.0168(4) Uani 1 1 d . . . N2 N -0.02162(18) 0.80600(14) 0.49668(10) 0.0141(4) Uani 1 1 d . . . N3 N 0.17532(18) 0.66946(15) 0.38360(10) 0.0157(4) Uani 1 1 d . . . N4 N -0.04933(18) 0.62043(14) 0.40315(10) 0.0133(4) Uani 1 1 d . . . C1 C 0.1005(2) 0.81495(18) 0.51602(12) 0.0164(5) Uani 1 1 d . . . C2 C 0.3050(2) 0.8165(2) 0.51228(14) 0.0234(6) Uani 1 1 d . . . H2 H 0.3865 0.8130 0.4945 0.028 Uiso 1 1 calc R . . C3 C 0.2799(2) 0.8294(2) 0.58133(14) 0.0251(6) Uani 1 1 d . . . H3 H 0.3389 0.8368 0.6191 0.030 Uiso 1 1 calc R . . C4 C 0.1477(2) 0.82976(18) 0.58569(12) 0.0191(5) Uani 1 1 d . . . C5 C 0.0610(3) 0.83850(19) 0.63834(13) 0.0217(6) Uani 1 1 d . . . H5 H 0.0873 0.8485 0.6859 0.026 Uiso 1 1 calc R . . C6 C -0.0646(2) 0.83212(19) 0.61893(13) 0.0220(6) Uani 1 1 d . . . H6 H -0.1257 0.8390 0.6535 0.026 Uiso 1 1 calc R . . C7 C -0.1019(2) 0.81568(18) 0.54906(12) 0.0188(5) Uani 1 1 d . . . H7 H -0.1890 0.8110 0.5377 0.023 Uiso 1 1 calc R . . C8 C 0.0699(2) 0.60124(17) 0.39670(11) 0.0139(5) Uani 1 1 d . . . C9 C 0.2757(2) 0.61886(19) 0.38310(12) 0.0188(5) Uani 1 1 d . . . H9 H 0.3615 0.6488 0.3764 0.023 Uiso 1 1 calc R . . C10 C 0.2360(2) 0.52099(19) 0.39341(12) 0.0176(5) Uani 1 1 d . . . H10 H 0.2874 0.4716 0.3941 0.021 Uiso 1 1 calc R . . C11 C 0.1031(2) 0.50656(18) 0.40297(11) 0.0151(5) Uani 1 1 d . . . C12 C 0.0085(2) 0.42741(18) 0.41754(12) 0.0173(5) Uani 1 1 d . . . H12 H 0.0264 0.3628 0.4221 0.021 Uiso 1 1 calc R . . C13 C -0.1126(2) 0.44608(18) 0.42519(12) 0.0180(5) Uani 1 1 d . . . H13 H -0.1795 0.3937 0.4357 0.022 Uiso 1 1 calc R . . C14 C -0.1379(2) 0.54064(18) 0.41776(12) 0.0164(5) Uani 1 1 d . . . H14 H -0.2227 0.5500 0.4233 0.020 Uiso 1 1 calc R . . C15 C 0.2866(2) 0.84811(18) 0.34382(12) 0.0155(5) Uani 1 1 d . . . C16 C 0.3413(2) 0.94807(19) 0.36335(13) 0.0180(5) Uani 1 1 d . . . C17 C 0.4294(2) 1.00276(19) 0.32116(13) 0.0197(5) Uani 1 1 d . . . H17 H 0.4642 1.0696 0.3357 0.024 Uiso 1 1 calc R . . C18 C 0.4684(2) 0.96371(19) 0.25907(13) 0.0205(5) Uani 1 1 d . . . C19 C 0.4100(2) 0.8683(2) 0.23723(13) 0.0205(5) Uani 1 1 d . . . H19 H 0.4335 0.8402 0.1941 0.025 Uiso 1 1 calc R . . C20 C 0.3179(2) 0.81238(18) 0.27651(12) 0.0171(5) Uani 1 1 d . . . C21 C 0.3036(3) 1.0049(2) 0.42750(15) 0.0288(6) Uani 1 1 d . . . H21A H 0.3489 0.9889 0.4685 0.043 Uiso 1 1 calc R . . H21B H 0.2122 0.9860 0.4342 0.043 Uiso 1 1 calc R . . H21C H 0.3254 1.0763 0.4212 0.043 Uiso 1 1 calc R . . C22 C 0.5651(3) 1.0243(2) 0.21433(15) 0.0298(6) Uani 1 1 d . . . H22A H 0.5235 1.0403 0.1721 0.045 Uiso 1 1 calc R . . H22B H 0.6308 0.9860 0.2014 0.045 Uiso 1 1 calc R . . H22C H 0.6039 1.0858 0.2405 0.045 Uiso 1 1 calc R . . C23 C 0.2493(3) 0.7156(2) 0.24108(13) 0.0246(6) Uani 1 1 d . . . H23A H 0.2544 0.7196 0.1904 0.037 Uiso 1 1 calc R . . H23B H 0.1603 0.7039 0.2547 0.037 Uiso 1 1 calc R . . H23C H 0.2888 0.6608 0.2553 0.037 Uiso 1 1 calc R . . C24 C -0.1981(2) 0.71417(19) 0.30017(13) 0.0209(5) Uani 1 1 d . . . H24 H -0.1873 0.6474 0.2802 0.025 Uiso 1 1 calc R . . C25 C -0.2763(2) 0.7114(2) 0.36087(13) 0.0219(6) Uani 1 1 d . . . H25 H -0.3091 0.6427 0.3755 0.026 Uiso 1 1 calc R . . C26 C -0.3649(2) 0.7837(2) 0.37703(15) 0.0285(6) Uani 1 1 d . . . H26A H -0.4353 0.7713 0.3424 0.034 Uiso 1 1 calc R . . H26B H -0.4015 0.7719 0.4236 0.034 Uiso 1 1 calc R . . C27 C -0.2980(3) 0.8909(2) 0.37583(14) 0.0274(6) Uani 1 1 d . . . H27A H -0.3358 0.9319 0.4109 0.033 Uiso 1 1 calc R . . H27B H -0.3104 0.9158 0.3294 0.033 Uiso 1 1 calc R . . C28 C -0.1564(3) 0.90152(19) 0.39132(14) 0.0248(6) Uani 1 1 d . . . H28 H -0.1254 0.9479 0.4323 0.030 Uiso 1 1 calc R . . C29 C -0.0683(3) 0.90108(19) 0.33821(15) 0.0254(6) Uani 1 1 d . . . H29 H 0.0140 0.9473 0.3484 0.030 Uiso 1 1 calc R . . C30 C -0.1000(3) 0.8819(2) 0.26098(14) 0.0312(7) Uani 1 1 d . . . H30A H -0.0226 0.8728 0.2357 0.037 Uiso 1 1 calc R . . H30B H -0.1286 0.9406 0.2433 0.037 Uiso 1 1 calc R . . C31 C -0.2026(3) 0.7908(2) 0.24581(13) 0.0263(6) Uani 1 1 d . . . H31A H -0.1904 0.7609 0.1988 0.032 Uiso 1 1 calc R . . H31B H -0.2866 0.8106 0.2464 0.032 Uiso 1 1 calc R . . Ir2 Ir 0.685459(8) 0.596324(7) 0.865853(4) 0.01453(3) Uani 1 1 d . . . B2 B 0.8231(3) 0.7830(2) 0.92876(14) 0.0169(6) Uani 1 1 d . . . H2A H 0.7492 0.7369 0.9062 0.020 Uiso 1 1 calc R . . N5 N 0.93646(18) 0.78083(15) 0.87946(10) 0.0171(4) Uani 1 1 d . . . N6 N 0.86942(18) 0.61843(15) 0.82218(9) 0.0144(4) Uani 1 1 d . . . N7 N 0.85857(19) 0.73290(16) 0.99445(10) 0.0180(4) Uani 1 1 d . . . N8 N 0.77378(19) 0.56186(15) 0.95927(10) 0.0169(4) Uani 1 1 d . . . C32 C 0.9559(2) 0.70199(18) 0.83742(12) 0.0158(5) Uani 1 1 d . . . C33 C 1.0504(2) 0.8466(2) 0.88328(14) 0.0239(6) Uani 1 1 d . . . H33 H 1.0647 0.9076 0.9106 0.029 Uiso 1 1 calc R . . C34 C 1.1401(2) 0.8137(2) 0.84318(14) 0.0247(6) Uani 1 1 d . . . H34 H 1.2247 0.8469 0.8370 0.030 Uiso 1 1 calc R . . C35 C 1.0820(2) 0.71937(19) 0.81231(12) 0.0184(5) Uani 1 1 d . . . C36 C 1.1188(2) 0.6465(2) 0.76845(12) 0.0224(6) Uani 1 1 d . . . H36 H 1.2013 0.6553 0.7496 0.027 Uiso 1 1 calc R . . C37 C 1.0312(2) 0.5605(2) 0.75303(12) 0.0214(6) Uani 1 1 d . . . H37 H 1.0539 0.5089 0.7236 0.026 Uiso 1 1 calc R . . C38 C 0.9108(2) 0.5491(2) 0.78011(12) 0.0198(5) Uani 1 1 d . . . H38 H 0.8537 0.4888 0.7685 0.024 Uiso 1 1 calc R . . C39 C 0.8419(2) 0.63374(19) 1.00281(12) 0.0175(5) Uani 1 1 d . . . C40 C 0.9420(2) 0.7781(2) 1.04749(13) 0.0251(6) Uani 1 1 d . . . H40 H 0.9728 0.8475 1.0534 0.030 Uiso 1 1 calc R . . C41 C 0.9736(3) 0.7101(2) 1.08965(13) 0.0276(6) Uani 1 1 d . . . H41 H 1.0276 0.7233 1.1297 0.033 Uiso 1 1 calc R . . C42 C 0.9105(2) 0.6152(2) 1.06241(13) 0.0229(6) Uani 1 1 d . . . C43 C 0.9066(3) 0.5172(2) 1.07796(14) 0.0276(6) Uani 1 1 d . . . H43 H 0.9503 0.5012 1.1176 0.033 Uiso 1 1 calc R . . C44 C 0.8373(3) 0.4440(2) 1.03410(15) 0.0286(6) Uani 1 1 d . . . H44 H 0.8331 0.3763 1.0435 0.034 Uiso 1 1 calc R . . C45 C 0.7736(2) 0.4681(2) 0.97638(14) 0.0237(6) Uani 1 1 d . . . H45 H 0.7272 0.4154 0.9473 0.028 Uiso 1 1 calc R . . C46 C 0.7805(2) 0.88833(19) 0.94093(13) 0.0184(5) Uani 1 1 d . . . C47 C 0.7186(2) 0.9146(2) 1.00262(13) 0.0228(6) Uani 1 1 d . . . C48 C 0.6857(3) 1.0079(2) 1.01162(14) 0.0273(6) Uani 1 1 d . . . H48 H 0.6452 1.0239 1.0534 0.033 Uiso 1 1 calc R . . C49 C 0.7093(3) 1.0782(2) 0.96226(15) 0.0293(6) Uani 1 1 d . . . C50 C 0.7592(3) 1.0499(2) 0.89972(14) 0.0255(6) Uani 1 1 d . . . H50 H 0.7724 1.0956 0.8640 0.031 Uiso 1 1 calc R . . C51 C 0.7908(2) 0.9563(2) 0.88755(13) 0.0214(6) Uani 1 1 d . . . C52 C 0.6765(3) 0.8428(2) 1.05871(15) 0.0329(7) Uani 1 1 d . . . H52A H 0.7479 0.8414 1.0903 0.049 Uiso 1 1 calc R . . H52B H 0.6467 0.7762 1.0370 0.049 Uiso 1 1 calc R . . H52C H 0.6076 0.8644 1.0851 0.049 Uiso 1 1 calc R . . C53 C 0.6790(3) 1.1807(2) 0.97551(18) 0.0446(9) Uani 1 1 d . . . H53A H 0.7503 1.2237 1.0003 0.067 Uiso 1 1 calc R . . H53B H 0.6029 1.1765 1.0039 0.067 Uiso 1 1 calc R . . H53C H 0.6641 1.2083 0.9310 0.067 Uiso 1 1 calc R . . C54 C 0.8255(3) 0.9303(2) 0.81301(13) 0.0287(6) Uani 1 1 d . . . H54A H 0.7881 0.9705 0.7811 0.043 Uiso 1 1 calc R . . H54B H 0.7930 0.8598 0.8012 0.043 Uiso 1 1 calc R . . H54C H 0.9178 0.9438 0.8087 0.043 Uiso 1 1 calc R . . C55 C 0.6073(2) 0.6432(2) 0.77685(13) 0.0218(6) Uani 1 1 d . . . H55 H 0.6707 0.6834 0.7470 0.026 Uiso 1 1 calc R . . C56 C 0.6039(2) 0.5389(2) 0.76836(13) 0.0265(6) Uani 1 1 d . . . H56 H 0.6663 0.5199 0.7341 0.032 Uiso 1 1 calc R . . C57 C 0.4810(3) 0.4630(2) 0.77047(15) 0.0356(7) Uani 1 1 d . . . H57A H 0.4096 0.4934 0.7551 0.043 Uiso 1 1 calc R . . H57B H 0.4862 0.4056 0.7377 0.043 Uiso 1 1 calc R . . C58 C 0.4563(3) 0.4274(3) 0.84287(17) 0.0414(8) Uani 1 1 d . . . H58A H 0.4887 0.3650 0.8468 0.050 Uiso 1 1 calc R . . H58B H 0.3639 0.4130 0.8504 0.050 Uiso 1 1 calc R . . C59 C 0.5185(2) 0.5031(2) 0.89892(14) 0.0291(7) Uani 1 1 d . . . H59 H 0.5290 0.4740 0.9446 0.035 Uiso 1 1 calc R . . C60 C 0.5028(2) 0.6027(2) 0.90540(13) 0.0264(6) Uani 1 1 d . . . H60 H 0.5031 0.6308 0.9546 0.032 Uiso 1 1 calc R . . C61 C 0.4205(3) 0.6459(3) 0.85537(15) 0.0338(7) Uani 1 1 d . . . H61A H 0.3499 0.5930 0.8381 0.041 Uiso 1 1 calc R . . H61B H 0.3834 0.6982 0.8808 0.041 Uiso 1 1 calc R . . C62 C 0.4933(3) 0.6899(2) 0.79364(16) 0.0350(7) Uani 1 1 d . . . H62A H 0.4360 0.6808 0.7523 0.042 Uiso 1 1 calc R . . H62B H 0.5216 0.7621 0.8038 0.042 Uiso 1 1 calc R . . C63 C 0.4400(3) 0.2983(2) 0.40449(15) 0.0309(7) Uani 1 1 d . . . H63A H 0.4444 0.2566 0.4438 0.046 Uiso 1 1 calc R . . H63B H 0.4778 0.2703 0.3635 0.046 Uiso 1 1 calc R . . H63C H 0.3513 0.3009 0.3941 0.046 Uiso 1 1 calc R . . C64 C 0.5122(3) 0.4026(2) 0.42316(15) 0.0301(7) Uani 1 1 d . . . H64A H 0.4976 0.4466 0.3861 0.036 Uiso 1 1 calc R . . H64B H 0.6040 0.4013 0.4251 0.036 Uiso 1 1 calc R . . C65 C 0.4730(3) 0.4451(2) 0.49266(14) 0.0290(6) Uani 1 1 d . . . H65A H 0.5008 0.4075 0.5304 0.035 Uiso 1 1 calc R . . H65B H 0.3794 0.4354 0.4936 0.035 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 0.01070(5) 0.01067(5) 0.01629(5) 0.00145(3) -0.00068(3) 0.00160(3) B1 0.0096(13) 0.0148(14) 0.0229(14) -0.0001(11) -0.0008(10) 0.0016(10) N1 0.0107(10) 0.0177(11) 0.0212(11) 0.0014(8) -0.0015(8) 0.0004(8) N2 0.0139(10) 0.0083(10) 0.0198(10) 0.0001(8) -0.0008(8) 0.0013(8) N3 0.0107(10) 0.0150(11) 0.0214(10) 0.0026(8) 0.0014(8) 0.0017(8) N4 0.0139(10) 0.0104(10) 0.0153(10) 0.0000(7) -0.0007(7) 0.0019(8) C1 0.0164(12) 0.0108(12) 0.0211(12) 0.0020(9) -0.0015(9) 0.0004(10) C2 0.0137(12) 0.0253(15) 0.0307(14) 0.0008(11) -0.0059(10) 0.0024(11) C3 0.0214(14) 0.0230(15) 0.0299(15) 0.0007(11) -0.0104(11) 0.0019(11) C4 0.0242(13) 0.0129(13) 0.0193(12) 0.0011(10) -0.0049(10) 0.0011(10) C5 0.0330(15) 0.0137(13) 0.0174(12) -0.0011(10) -0.0044(10) 0.0025(11) C6 0.0259(14) 0.0193(14) 0.0203(13) -0.0007(10) 0.0032(10) 0.0035(11) C7 0.0176(13) 0.0161(13) 0.0232(13) 0.0000(10) 0.0002(10) 0.0048(10) C8 0.0154(12) 0.0127(12) 0.0136(11) 0.0005(9) 0.0008(9) 0.0022(9) C9 0.0128(12) 0.0219(14) 0.0227(13) 0.0023(10) 0.0018(9) 0.0054(10) C10 0.0180(12) 0.0187(13) 0.0184(12) 0.0016(10) 0.0002(9) 0.0090(10) C11 0.0182(12) 0.0168(13) 0.0111(11) -0.0004(9) -0.0020(9) 0.0061(10) C12 0.0247(13) 0.0122(12) 0.0157(12) 0.0023(9) 0.0008(10) 0.0042(10) C13 0.0202(13) 0.0129(13) 0.0192(12) 0.0018(9) 0.0009(10) -0.0019(10) C14 0.0134(12) 0.0159(13) 0.0185(12) -0.0003(9) 0.0016(9) -0.0005(10) C15 0.0099(11) 0.0149(13) 0.0225(12) 0.0043(10) -0.0009(9) 0.0035(9) C16 0.0119(12) 0.0171(13) 0.0255(13) 0.0020(10) 0.0017(10) 0.0034(10) C17 0.0128(12) 0.0158(13) 0.0295(14) 0.0029(10) -0.0011(10) -0.0003(10) C18 0.0163(12) 0.0191(14) 0.0260(13) 0.0079(10) -0.0012(10) 0.0008(10) C19 0.0215(13) 0.0224(14) 0.0192(12) 0.0053(10) 0.0019(10) 0.0067(11) C20 0.0166(12) 0.0142(13) 0.0205(12) 0.0050(10) -0.0050(10) 0.0019(10) C21 0.0330(16) 0.0152(14) 0.0364(16) -0.0017(11) 0.0129(12) 0.0008(12) C22 0.0293(16) 0.0254(16) 0.0328(15) 0.0061(12) 0.0092(12) -0.0015(12) C23 0.0304(15) 0.0199(14) 0.0212(13) 0.0016(10) -0.0029(11) -0.0016(11) C24 0.0249(14) 0.0158(13) 0.0219(13) -0.0016(10) -0.0077(10) 0.0043(11) C25 0.0148(12) 0.0206(14) 0.0298(14) 0.0066(11) -0.0056(10) 0.0002(10) C26 0.0178(14) 0.0406(18) 0.0294(15) 0.0116(13) 0.0013(11) 0.0089(12) C27 0.0274(15) 0.0348(17) 0.0251(14) -0.0004(12) -0.0038(11) 0.0199(13) C28 0.0304(15) 0.0154(14) 0.0307(14) -0.0041(11) -0.0131(12) 0.0118(11) C29 0.0204(14) 0.0146(14) 0.0405(16) 0.0096(11) -0.0054(12) -0.0006(11) C30 0.0263(15) 0.0381(18) 0.0321(15) 0.0192(13) 0.0056(12) 0.0078(13) C31 0.0301(15) 0.0313(16) 0.0195(13) 0.0043(11) 0.0015(11) 0.0102(12) Ir2 0.01105(5) 0.01739(5) 0.01400(5) -0.00070(4) 0.00102(3) 0.00009(4) B2 0.0158(14) 0.0177(15) 0.0152(13) -0.0014(11) -0.0028(10) -0.0017(11) N5 0.0126(10) 0.0178(11) 0.0198(10) 0.0011(8) 0.0003(8) -0.0007(8) N6 0.0121(10) 0.0191(11) 0.0119(9) 0.0007(8) -0.0020(7) 0.0022(8) N7 0.0189(11) 0.0197(12) 0.0148(10) -0.0033(8) -0.0030(8) 0.0030(9) N8 0.0145(10) 0.0171(11) 0.0187(10) 0.0035(8) 0.0039(8) 0.0013(8) C32 0.0162(12) 0.0192(13) 0.0127(11) 0.0033(9) -0.0014(9) 0.0042(10) C33 0.0201(13) 0.0185(14) 0.0304(14) 0.0010(11) -0.0031(11) -0.0032(11) C34 0.0140(13) 0.0265(15) 0.0309(14) 0.0059(11) 0.0010(10) -0.0045(11) C35 0.0144(12) 0.0248(14) 0.0156(12) 0.0065(10) 0.0013(9) 0.0008(10) C36 0.0138(12) 0.0393(17) 0.0151(12) 0.0048(11) 0.0011(9) 0.0069(11) C37 0.0187(13) 0.0317(16) 0.0159(12) -0.0019(10) -0.0008(10) 0.0109(11) C38 0.0180(13) 0.0231(14) 0.0173(12) -0.0041(10) -0.0036(9) 0.0029(11) C39 0.0138(12) 0.0247(14) 0.0147(12) 0.0035(10) 0.0029(9) 0.0045(10) C40 0.0224(14) 0.0294(16) 0.0218(13) -0.0077(11) -0.0063(10) 0.0033(12) C41 0.0255(15) 0.0420(18) 0.0161(13) -0.0027(12) -0.0043(11) 0.0099(13) C42 0.0173(13) 0.0377(17) 0.0167(12) 0.0061(11) 0.0035(10) 0.0111(12) C43 0.0215(14) 0.0423(18) 0.0221(14) 0.0149(12) 0.0035(11) 0.0102(13) C44 0.0249(15) 0.0253(16) 0.0379(16) 0.0175(12) 0.0046(12) 0.0057(12) C45 0.0193(13) 0.0195(14) 0.0322(15) 0.0048(11) 0.0050(11) 0.0021(11) C46 0.0161(12) 0.0167(13) 0.0209(12) -0.0031(10) -0.0030(9) 0.0005(10) C47 0.0191(13) 0.0224(15) 0.0256(14) -0.0050(11) -0.0032(10) 0.0028(11) C48 0.0233(14) 0.0316(17) 0.0271(14) -0.0123(12) -0.0067(11) 0.0099(12) C49 0.0288(15) 0.0223(15) 0.0375(16) -0.0091(12) -0.0166(12) 0.0099(12) C50 0.0273(15) 0.0163(14) 0.0323(15) 0.0031(11) -0.0109(12) 0.0022(11) C51 0.0167(13) 0.0204(14) 0.0266(14) 0.0014(11) -0.0062(10) 0.0022(11) C52 0.0321(16) 0.0390(19) 0.0297(15) 0.0009(13) 0.0090(12) 0.0118(14) C53 0.053(2) 0.0296(19) 0.055(2) -0.0113(15) -0.0172(17) 0.0216(16) C54 0.0349(16) 0.0284(16) 0.0242(14) 0.0059(11) 0.0000(12) 0.0085(13) C55 0.0125(12) 0.0363(17) 0.0174(12) 0.0061(11) -0.0001(9) 0.0050(11) C56 0.0166(13) 0.0431(18) 0.0167(13) -0.0071(11) -0.0029(10) 0.0001(12) C57 0.0229(15) 0.042(2) 0.0361(17) -0.0156(14) -0.0030(12) -0.0031(13) C58 0.0289(17) 0.038(2) 0.050(2) 0.0010(15) -0.0004(14) -0.0136(14) C59 0.0180(14) 0.0385(18) 0.0268(14) 0.0084(12) 0.0030(11) -0.0075(12) C60 0.0139(13) 0.0482(19) 0.0168(13) -0.0003(12) 0.0033(10) 0.0052(12) C61 0.0227(15) 0.049(2) 0.0316(16) 0.0010(14) 0.0037(12) 0.0126(14) C62 0.0229(15) 0.043(2) 0.0426(18) 0.0148(14) 0.0029(13) 0.0123(14) C63 0.0260(15) 0.0320(17) 0.0366(16) 0.0094(13) 0.0010(12) 0.0082(13) C64 0.0191(14) 0.0391(18) 0.0335(16) 0.0114(13) 0.0005(11) 0.0058(12) C65 0.0208(14) 0.0347(17) 0.0326(16) 0.0112(13) -0.0040(11) 0.0051(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 C24 2.089(2) . ? Ir1 C25 2.089(2) . ? Ir1 N4 2.1243(19) . ? Ir1 C29 2.139(3) . ? Ir1 C28 2.144(3) . ? Ir1 N2 2.1906(19) . ? B1 N3 1.541(3) . ? B1 N1 1.554(3) . ? B1 C15 1.605(4) . ? B1 H1 1.0000 . ? N1 C1 1.361(3) . ? N1 C2 1.387(3) . ? N2 C1 1.344(3) . ? N2 C7 1.346(3) . ? N3 C8 1.365(3) . ? N3 C9 1.387(3) . ? N4 C14 1.356(3) . ? N4 C8 1.360(3) . ? C1 C4 1.420(3) . ? C2 C3 1.364(4) . ? C2 H2 0.9500 . ? C3 C4 1.424(4) . ? C3 H3 0.9500 . ? C4 C5 1.394(4) . ? C5 C6 1.384(4) . ? C5 H5 0.9500 . ? C6 C7 1.393(3) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C11 1.421(3) . ? C9 C10 1.359(3) . ? C9 H9 0.9500 . ? C10 C11 1.420(3) . ? C10 H10 0.9500 . ? C11 C12 1.387(3) . ? C12 C13 1.379(3) . ? C12 H12 0.9500 . ? C13 C14 1.389(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.418(3) . ? C15 C20 1.422(3) . ? C16 C17 1.391(3) . ? C16 C21 1.518(3) . ? C17 C18 1.379(4) . ? C17 H17 0.9500 . ? C18 C19 1.385(4) . ? C18 C22 1.512(3) . ? C19 C20 1.390(3) . ? C19 H19 0.9500 . ? C20 C23 1.518(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.440(4) . ? C24 C31 1.531(3) . ? C24 H24 1.0000 . ? C25 C26 1.518(4) . ? C25 H25 1.0000 . ? C26 C27 1.516(4) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C28 1.529(4) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.397(4) . ? C28 H28 1.0000 . ? C29 C30 1.519(4) . ? C29 H29 1.0000 . ? C30 C31 1.520(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? Ir2 C55 2.086(2) . ? Ir2 C56 2.112(2) . ? Ir2 C60 2.124(2) . ? Ir2 C59 2.127(3) . ? Ir2 N6 2.1290(19) . ? Ir2 N8 2.143(2) . ? B2 N7 1.550(3) . ? B2 N5 1.551(3) . ? B2 C46 1.601(4) . ? B2 H2A 1.0000 . ? N5 C32 1.362(3) . ? N5 C33 1.380(3) . ? N6 C38 1.353(3) . ? N6 C32 1.354(3) . ? N7 C39 1.359(3) . ? N7 C40 1.393(3) . ? N8 C45 1.346(3) . ? N8 C39 1.358(3) . ? C32 C35 1.424(3) . ? C33 C34 1.363(4) . ? C33 H33 0.9500 . ? C34 C35 1.424(4) . ? C34 H34 0.9500 . ? C35 C36 1.386(4) . ? C36 C37 1.384(4) . ? C36 H36 0.9500 . ? C37 C38 1.382(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C42 1.419(3) . ? C40 C41 1.357(4) . ? C40 H40 0.9500 . ? C41 C42 1.423(4) . ? C41 H41 0.9500 . ? C42 C43 1.387(4) . ? C43 C44 1.377(4) . ? C43 H43 0.9500 . ? C44 C45 1.388(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C51 1.417(3) . ? C46 C47 1.424(3) . ? C47 C48 1.392(4) . ? C47 C52 1.517(4) . ? C48 C49 1.383(4) . ? C48 H48 0.9500 . ? C49 C50 1.383(4) . ? C49 C53 1.510(4) . ? C50 C51 1.396(4) . ? C50 H50 0.9500 . ? C51 C54 1.522(4) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.425(4) . ? C55 C62 1.513(4) . ? C55 H55 1.0000 . ? C56 C57 1.527(4) . ? C56 H56 1.0000 . ? C57 C58 1.509(4) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.514(4) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.408(4) . ? C59 H59 1.0000 . ? C60 C61 1.519(4) . ? C60 H60 1.0000 . ? C61 C62 1.518(4) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.520(4) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.520(4) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C65 1.521(6) 2_666 ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C24 Ir1 C25 40.32(10) . . ? C24 Ir1 N4 91.72(9) . . ? C25 Ir1 N4 93.28(9) . . ? C24 Ir1 C29 80.89(10) . . ? C25 Ir1 C29 96.61(10) . . ? N4 Ir1 C29 154.35(9) . . ? C24 Ir1 C28 89.88(10) . . ? C25 Ir1 C28 79.94(10) . . ? N4 Ir1 C28 167.43(9) . . ? C29 Ir1 C28 38.07(10) . . ? C24 Ir1 N2 163.82(9) . . ? C25 Ir1 N2 123.53(9) . . ? N4 Ir1 N2 88.12(7) . . ? C29 Ir1 N2 105.70(9) . . ? C28 Ir1 N2 86.90(9) . . ? N3 B1 N1 104.91(19) . . ? N3 B1 C15 116.7(2) . . ? N1 B1 C15 116.2(2) . . ? N3 B1 H1 106.1 . . ? N1 B1 H1 106.1 . . ? C15 B1 H1 106.1 . . ? C1 N1 C2 106.0(2) . . ? C1 N1 B1 126.80(19) . . ? C2 N1 B1 126.5(2) . . ? C1 N2 C7 115.2(2) . . ? C1 N2 Ir1 122.09(16) . . ? C7 N2 Ir1 122.48(16) . . ? C8 N3 C9 106.1(2) . . ? C8 N3 B1 125.0(2) . . ? C9 N3 B1 126.3(2) . . ? C14 N4 C8 114.3(2) . . ? C14 N4 Ir1 124.81(16) . . ? C8 N4 Ir1 120.85(15) . . ? N2 C1 N1 124.5(2) . . ? N2 C1 C4 125.3(2) . . ? N1 C1 C4 110.2(2) . . ? C3 C2 N1 111.6(2) . . ? C3 C2 H2 124.2 . . ? N1 C2 H2 124.2 . . ? C2 C3 C4 106.5(2) . . ? C2 C3 H3 126.8 . . ? C4 C3 H3 126.8 . . ? C5 C4 C1 117.5(2) . . ? C5 C4 C3 136.8(2) . . ? C1 C4 C3 105.7(2) . . ? C6 C5 C4 117.7(2) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? C5 C6 C7 120.4(2) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? N2 C7 C6 123.8(2) . . ? N2 C7 H7 118.1 . . ? C6 C7 H7 118.1 . . ? N4 C8 N3 125.4(2) . . ? N4 C8 C11 124.7(2) . . ? N3 C8 C11 109.9(2) . . ? C10 C9 N3 111.4(2) . . ? C10 C9 H9 124.3 . . ? N3 C9 H9 124.3 . . ? C9 C10 C11 106.9(2) . . ? C9 C10 H10 126.5 . . ? C11 C10 H10 126.5 . . ? C12 C11 C10 135.9(2) . . ? C12 C11 C8 118.5(2) . . ? C10 C11 C8 105.6(2) . . ? C13 C12 C11 117.4(2) . . ? C13 C12 H12 121.3 . . ? C11 C12 H12 121.3 . . ? C12 C13 C14 120.7(2) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? N4 C14 C13 124.3(2) . . ? N4 C14 H14 117.9 . . ? C13 C14 H14 117.9 . . ? C16 C15 C20 115.8(2) . . ? C16 C15 B1 122.0(2) . . ? C20 C15 B1 121.9(2) . . ? C17 C16 C15 120.8(2) . . ? C17 C16 C21 115.3(2) . . ? C15 C16 C21 123.8(2) . . ? C18 C17 C16 122.5(2) . . ? C18 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? C17 C18 C19 117.2(2) . . ? C17 C18 C22 121.6(2) . . ? C19 C18 C22 121.0(2) . . ? C18 C19 C20 122.0(2) . . ? C18 C19 H19 119.0 . . ? C20 C19 H19 119.0 . . ? C19 C20 C15 121.0(2) . . ? C19 C20 C23 115.7(2) . . ? C15 C20 C23 123.1(2) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C31 120.9(2) . . ? C25 C24 Ir1 69.85(14) . . ? C31 C24 Ir1 115.81(18) . . ? C25 C24 H24 114.3 . . ? C31 C24 H24 114.3 . . ? Ir1 C24 H24 114.3 . . ? C24 C25 C26 123.7(2) . . ? C24 C25 Ir1 69.83(14) . . ? C26 C25 Ir1 114.81(18) . . ? C24 C25 H25 113.7 . . ? C26 C25 H25 113.7 . . ? Ir1 C25 H25 113.7 . . ? C27 C26 C25 112.2(2) . . ? C27 C26 H26A 109.2 . . ? C25 C26 H26A 109.2 . . ? C27 C26 H26B 109.2 . . ? C25 C26 H26B 109.2 . . ? H26A C26 H26B 107.9 . . ? C26 C27 C28 111.3(2) . . ? C26 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? C26 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C29 C28 C27 121.9(2) . . ? C29 C28 Ir1 70.76(15) . . ? C27 C28 Ir1 115.06(18) . . ? C29 C28 H28 114.0 . . ? C27 C28 H28 114.0 . . ? Ir1 C28 H28 114.0 . . ? C28 C29 C30 125.4(2) . . ? C28 C29 Ir1 71.17(15) . . ? C30 C29 Ir1 110.89(18) . . ? C28 C29 H29 113.8 . . ? C30 C29 H29 113.8 . . ? Ir1 C29 H29 113.8 . . ? C29 C30 C31 112.6(2) . . ? C29 C30 H30A 109.1 . . ? C31 C30 H30A 109.1 . . ? C29 C30 H30B 109.1 . . ? C31 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? C30 C31 C24 110.6(2) . . ? C30 C31 H31A 109.5 . . ? C24 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C24 C31 H31B 109.5 . . ? H31A C31 H31B 108.1 . . ? C55 Ir2 C56 39.68(11) . . ? C55 Ir2 C60 82.00(10) . . ? C56 Ir2 C60 90.23(10) . . ? C55 Ir2 C59 97.12(10) . . ? C56 Ir2 C59 79.73(11) . . ? C60 Ir2 C59 38.69(11) . . ? C55 Ir2 N6 91.83(8) . . ? C56 Ir2 N6 90.66(9) . . ? C60 Ir2 N6 169.16(10) . . ? C59 Ir2 N6 151.83(10) . . ? C55 Ir2 N8 174.84(9) . . ? C56 Ir2 N8 145.13(10) . . ? C60 Ir2 N8 98.85(9) . . ? C59 Ir2 N8 86.57(9) . . ? N6 Ir2 N8 86.52(7) . . ? N7 B2 N5 104.3(2) . . ? N7 B2 C46 117.0(2) . . ? N5 B2 C46 115.7(2) . . ? N7 B2 H2A 106.4 . . ? N5 B2 H2A 106.4 . . ? C46 B2 H2A 106.4 . . ? C32 N5 C33 106.1(2) . . ? C32 N5 B2 126.1(2) . . ? C33 N5 B2 125.9(2) . . ? C38 N6 C32 115.0(2) . . ? C38 N6 Ir2 123.05(16) . . ? C32 N6 Ir2 121.87(16) . . ? C39 N7 C40 106.0(2) . . ? C39 N7 B2 126.4(2) . . ? C40 N7 B2 125.7(2) . . ? C45 N8 C39 115.3(2) . . ? C45 N8 Ir2 122.76(18) . . ? C39 N8 Ir2 121.77(17) . . ? N6 C32 N5 125.4(2) . . ? N6 C32 C35 124.5(2) . . ? N5 C32 C35 110.0(2) . . ? C34 C33 N5 112.0(2) . . ? C34 C33 H33 124.0 . . ? N5 C33 H33 124.0 . . ? C33 C34 C35 106.3(2) . . ? C33 C34 H34 126.8 . . ? C35 C34 H34 126.8 . . ? C36 C35 C32 118.0(2) . . ? C36 C35 C34 136.4(2) . . ? C32 C35 C34 105.6(2) . . ? C37 C36 C35 117.8(2) . . ? C37 C36 H36 121.1 . . ? C35 C36 H36 121.1 . . ? C38 C37 C36 120.6(2) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? N6 C38 C37 124.0(2) . . ? N6 C38 H38 118.0 . . ? C37 C38 H38 118.0 . . ? N8 C39 N7 125.4(2) . . ? N8 C39 C42 124.4(2) . . ? N7 C39 C42 110.2(2) . . ? C41 C40 N7 111.3(3) . . ? C41 C40 H40 124.4 . . ? N7 C40 H40 124.4 . . ? C40 C41 C42 106.9(2) . . ? C40 C41 H41 126.5 . . ? C42 C41 H41 126.5 . . ? C43 C42 C39 118.0(3) . . ? C43 C42 C41 136.4(3) . . ? C39 C42 C41 105.5(2) . . ? C44 C43 C42 117.9(2) . . ? C44 C43 H43 121.1 . . ? C42 C43 H43 121.1 . . ? C43 C44 C45 120.7(3) . . ? C43 C44 H44 119.6 . . ? C45 C44 H44 119.6 . . ? N8 C45 C44 123.7(3) . . ? N8 C45 H45 118.1 . . ? C44 C45 H45 118.1 . . ? C51 C46 C47 116.3(2) . . ? C51 C46 B2 121.3(2) . . ? C47 C46 B2 122.1(2) . . ? C48 C47 C46 120.2(3) . . ? C48 C47 C52 116.4(2) . . ? C46 C47 C52 123.3(2) . . ? C49 C48 C47 122.8(3) . . ? C49 C48 H48 118.6 . . ? C47 C48 H48 118.6 . . ? C48 C49 C50 117.2(3) . . ? C48 C49 C53 121.3(3) . . ? C50 C49 C53 121.5(3) . . ? C49 C50 C51 122.0(3) . . ? C49 C50 H50 119.0 . . ? C51 C50 H50 119.0 . . ? C50 C51 C46 120.8(2) . . ? C50 C51 C54 115.8(2) . . ? C46 C51 C54 123.2(2) . . ? C47 C52 H52A 109.5 . . ? C47 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C47 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53A 109.5 . . ? C49 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C49 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C56 C55 C62 124.3(2) . . ? C56 C55 Ir2 71.12(15) . . ? C62 C55 Ir2 111.85(17) . . ? C56 C55 H55 114.0 . . ? C62 C55 H55 114.0 . . ? Ir2 C55 H55 114.0 . . ? C55 C56 C57 122.5(3) . . ? C55 C56 Ir2 69.20(14) . . ? C57 C56 Ir2 116.13(18) . . ? C55 C56 H56 113.9 . . ? C57 C56 H56 113.9 . . ? Ir2 C56 H56 113.9 . . ? C58 C57 C56 111.4(2) . . ? C58 C57 H57A 109.4 . . ? C56 C57 H57A 109.4 . . ? C58 C57 H57B 109.4 . . ? C56 C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? C57 C58 C59 112.4(2) . . ? C57 C58 H58A 109.1 . . ? C59 C58 H58A 109.1 . . ? C57 C58 H58B 109.1 . . ? C59 C58 H58B 109.1 . . ? H58A C58 H58B 107.9 . . ? C60 C59 C58 124.8(3) . . ? C60 C59 Ir2 70.54(15) . . ? C58 C59 Ir2 113.67(19) . . ? C60 C59 H59 113.5 . . ? C58 C59 H59 113.5 . . ? Ir2 C59 H59 113.5 . . ? C59 C60 C61 122.6(3) . . ? C59 C60 Ir2 70.77(15) . . ? C61 C60 Ir2 112.99(17) . . ? C59 C60 H60 114.3 . . ? C61 C60 H60 114.3 . . ? Ir2 C60 H60 114.3 . . ? C62 C61 C60 112.7(2) . . ? C62 C61 H61A 109.0 . . ? C60 C61 H61A 109.0 . . ? C62 C61 H61B 109.0 . . ? C60 C61 H61B 109.0 . . ? H61A C61 H61B 107.8 . . ? C55 C62 C61 112.8(2) . . ? C55 C62 H62A 109.0 . . ? C61 C62 H62A 109.0 . . ? C55 C62 H62B 109.0 . . ? C61 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? C64 C63 H63A 109.5 . . ? C64 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C64 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C63 C64 C65 112.7(2) . . ? C63 C64 H64A 109.1 . . ? C65 C64 H64A 109.1 . . ? C63 C64 H64B 109.1 . . ? C65 C64 H64B 109.1 . . ? H64A C64 H64B 107.8 . . ? C64 C65 C65 114.0(3) . 2_666 ? C64 C65 H65A 108.8 . . ? C65 C65 H65A 108.8 2_666 . ? C64 C65 H65B 108.8 . . ? C65 C65 H65B 108.8 2_666 . ? H65A C65 H65B 107.7 . . ? 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 N3 B1 N1 C1 -91.6(3) . . . . ? C15 B1 N1 C1 137.9(2) . . . . ? N3 B1 N1 C2 78.2(3) . . . . ? C15 B1 N1 C2 -52.3(3) . . . . ? C24 Ir1 N2 C1 159.2(3) . . . . ? C25 Ir1 N2 C1 162.23(18) . . . . ? N4 Ir1 N2 C1 69.55(18) . . . . ? C29 Ir1 N2 C1 -88.52(19) . . . . ? C28 Ir1 N2 C1 -121.99(19) . . . . ? C24 Ir1 N2 C7 -14.8(4) . . . . ? C25 Ir1 N2 C7 -11.8(2) . . . . ? N4 Ir1 N2 C7 -104.50(19) . . . . ? C29 Ir1 N2 C7 97.4(2) . . . . ? C28 Ir1 N2 C7 64.0(2) . . . . ? N1 B1 N3 C8 76.2(3) . . . . ? C15 B1 N3 C8 -153.6(2) . . . . ? N1 B1 N3 C9 -83.1(3) . . . . ? C15 B1 N3 C9 47.1(3) . . . . ? C24 Ir1 N4 C14 -64.51(19) . . . . ? C25 Ir1 N4 C14 -24.18(19) . . . . ? C29 Ir1 N4 C14 -136.9(2) . . . . ? C28 Ir1 N4 C14 32.7(5) . . . . ? N2 Ir1 N4 C14 99.30(19) . . . . ? C24 Ir1 N4 C8 114.38(18) . . . . ? C25 Ir1 N4 C8 154.71(18) . . . . ? C29 Ir1 N4 C8 42.0(3) . . . . ? C28 Ir1 N4 C8 -148.4(4) . . . . ? N2 Ir1 N4 C8 -81.80(17) . . . . ? C7 N2 C1 N1 -179.1(2) . . . . ? Ir1 N2 C1 N1 6.5(3) . . . . ? C7 N2 C1 C4 2.4(3) . . . . ? Ir1 N2 C1 C4 -172.09(18) . . . . ? C2 N1 C1 N2 -176.7(2) . . . . ? B1 N1 C1 N2 -5.2(4) . . . . ? C2 N1 C1 C4 2.1(3) . . . . ? B1 N1 C1 C4 173.6(2) . . . . ? C1 N1 C2 C3 -1.5(3) . . . . ? B1 N1 C2 C3 -173.1(2) . . . . ? N1 C2 C3 C4 0.4(3) . . . . ? N2 C1 C4 C5 -1.9(4) . . . . ? N1 C1 C4 C5 179.4(2) . . . . ? N2 C1 C4 C3 176.9(2) . . . . ? N1 C1 C4 C3 -1.8(3) . . . . ? C2 C3 C4 C5 179.3(3) . . . . ? C2 C3 C4 C1 0.8(3) . . . . ? C1 C4 C5 C6 0.0(4) . . . . ? C3 C4 C5 C6 -178.3(3) . . . . ? C4 C5 C6 C7 1.1(4) . . . . ? C1 N2 C7 C6 -1.1(4) . . . . ? Ir1 N2 C7 C6 173.36(19) . . . . ? C5 C6 C7 N2 -0.6(4) . . . . ? C14 N4 C8 N3 -178.6(2) . . . . ? Ir1 N4 C8 N3 2.4(3) . . . . ? C14 N4 C8 C11 1.2(3) . . . . ? Ir1 N4 C8 C11 -177.85(17) . . . . ? C9 N3 C8 N4 178.4(2) . . . . ? B1 N3 C8 N4 15.7(4) . . . . ? C9 N3 C8 C11 -1.3(3) . . . . ? B1 N3 C8 C11 -164.1(2) . . . . ? C8 N3 C9 C10 1.8(3) . . . . ? B1 N3 C9 C10 164.2(2) . . . . ? N3 C9 C10 C11 -1.5(3) . . . . ? C9 C10 C11 C12 -177.5(3) . . . . ? C9 C10 C11 C8 0.7(3) . . . . ? N4 C8 C11 C12 -0.8(3) . . . . ? N3 C8 C11 C12 178.9(2) . . . . ? N4 C8 C11 C10 -179.3(2) . . . . ? N3 C8 C11 C10 0.4(3) . . . . ? C10 C11 C12 C13 177.8(2) . . . . ? C8 C11 C12 C13 -0.1(3) . . . . ? C11 C12 C13 C14 0.6(3) . . . . ? C8 N4 C14 C13 -0.6(3) . . . . ? Ir1 N4 C14 C13 178.35(18) . . . . ? C12 C13 C14 N4 -0.3(4) . . . . ? N3 B1 C15 C16 -154.4(2) . . . . ? N1 B1 C15 C16 -29.8(3) . . . . ? N3 B1 C15 C20 31.9(3) . . . . ? N1 B1 C15 C20 156.5(2) . . . . ? C20 C15 C16 C17 -6.1(3) . . . . ? B1 C15 C16 C17 179.9(2) . . . . ? C20 C15 C16 C21 169.9(2) . . . . ? B1 C15 C16 C21 -4.2(4) . . . . ? C15 C16 C17 C18 -0.1(4) . . . . ? C21 C16 C17 C18 -176.4(2) . . . . ? C16 C17 C18 C19 4.1(4) . . . . ? C16 C17 C18 C22 -179.5(2) . . . . ? C17 C18 C19 C20 -1.5(4) . . . . ? C22 C18 C19 C20 -178.0(2) . . . . ? C18 C19 C20 C15 -4.9(4) . . . . ? C18 C19 C20 C23 171.4(2) . . . . ? C16 C15 C20 C19 8.5(3) . . . . ? B1 C15 C20 C19 -177.4(2) . . . . ? C16 C15 C20 C23 -167.6(2) . . . . ? B1 C15 C20 C23 6.5(4) . . . . ? N4 Ir1 C24 C25 93.04(15) . . . . ? C29 Ir1 C24 C25 -111.65(16) . . . . ? C28 Ir1 C24 C25 -74.49(16) . . . . ? N2 Ir1 C24 C25 3.9(4) . . . . ? C25 Ir1 C24 C31 115.5(3) . . . . ? N4 Ir1 C24 C31 -151.45(19) . . . . ? C29 Ir1 C24 C31 3.85(19) . . . . ? C28 Ir1 C24 C31 41.0(2) . . . . ? N2 Ir1 C24 C31 119.4(3) . . . . ? C31 C24 C25 C26 -1.7(4) . . . . ? Ir1 C24 C25 C26 107.0(2) . . . . ? C31 C24 C25 Ir1 -108.7(2) . . . . ? N4 Ir1 C25 C24 -88.80(15) . . . . ? C29 Ir1 C25 C24 67.50(16) . . . . ? C28 Ir1 C25 C24 101.87(16) . . . . ? N2 Ir1 C25 C24 -178.71(13) . . . . ? C24 Ir1 C25 C26 -118.8(2) . . . . ? N4 Ir1 C25 C26 152.39(18) . . . . ? C29 Ir1 C25 C26 -51.3(2) . . . . ? C28 Ir1 C25 C26 -16.95(19) . . . . ? N2 Ir1 C25 C26 62.5(2) . . . . ? C24 C25 C26 C27 -52.8(3) . . . . ? Ir1 C25 C26 C27 28.7(3) . . . . ? C25 C26 C27 C28 -25.5(3) . . . . ? C26 C27 C28 C29 94.2(3) . . . . ? C26 C27 C28 Ir1 12.0(3) . . . . ? C24 Ir1 C28 C29 -75.29(16) . . . . ? C25 Ir1 C28 C29 -114.58(17) . . . . ? N4 Ir1 C28 C29 -172.7(3) . . . . ? N2 Ir1 C28 C29 120.57(16) . . . . ? C24 Ir1 C28 C27 41.8(2) . . . . ? C25 Ir1 C28 C27 2.5(2) . . . . ? N4 Ir1 C28 C27 -55.6(5) . . . . ? C29 Ir1 C28 C27 117.1(3) . . . . ? N2 Ir1 C28 C27 -122.4(2) . . . . ? C27 C28 C29 C30 -5.4(4) . . . . ? Ir1 C28 C29 C30 102.7(3) . . . . ? C27 C28 C29 Ir1 -108.1(2) . . . . ? C24 Ir1 C29 C28 101.60(17) . . . . ? C25 Ir1 C29 C28 64.34(17) . . . . ? N4 Ir1 C29 C28 176.32(17) . . . . ? N2 Ir1 C29 C28 -63.26(16) . . . . ? C24 Ir1 C29 C30 -20.06(18) . . . . ? C25 Ir1 C29 C30 -57.3(2) . . . . ? N4 Ir1 C29 C30 54.7(3) . . . . ? C28 Ir1 C29 C30 -121.7(3) . . . . ? N2 Ir1 C29 C30 175.08(17) . . . . ? C28 C29 C30 C31 -47.9(4) . . . . ? Ir1 C29 C30 C31 33.4(3) . . . . ? C29 C30 C31 C24 -30.1(3) . . . . ? C25 C24 C31 C30 94.1(3) . . . . ? Ir1 C24 C31 C30 13.1(3) . . . . ? N7 B2 N5 C32 80.9(3) . . . . ? C46 B2 N5 C32 -149.1(2) . . . . ? N7 B2 N5 C33 -80.7(3) . . . . ? C46 B2 N5 C33 49.3(3) . . . . ? C55 Ir2 N6 C38 -85.5(2) . . . . ? C56 Ir2 N6 C38 -45.9(2) . . . . ? C60 Ir2 N6 C38 -140.5(4) . . . . ? C59 Ir2 N6 C38 23.3(3) . . . . ? N8 Ir2 N6 C38 99.36(19) . . . . ? C55 Ir2 N6 C32 97.62(19) . . . . ? C56 Ir2 N6 C32 137.29(19) . . . . ? C60 Ir2 N6 C32 42.6(5) . . . . ? C59 Ir2 N6 C32 -153.6(2) . . . . ? N8 Ir2 N6 C32 -77.49(18) . . . . ? N5 B2 N7 C39 -82.7(3) . . . . ? C46 B2 N7 C39 148.1(2) . . . . ? N5 B2 N7 C40 79.2(3) . . . . ? C46 B2 N7 C40 -50.0(3) . . . . ? C56 Ir2 N8 C45 -12.6(3) . . . . ? C60 Ir2 N8 C45 90.7(2) . . . . ? C59 Ir2 N8 C45 53.9(2) . . . . ? N6 Ir2 N8 C45 -98.75(19) . . . . ? C56 Ir2 N8 C39 162.50(18) . . . . ? C60 Ir2 N8 C39 -94.17(19) . . . . ? C59 Ir2 N8 C39 -130.98(19) . . . . ? N6 Ir2 N8 C39 76.35(18) . . . . ? C38 N6 C32 N5 -178.9(2) . . . . ? Ir2 N6 C32 N5 -1.8(3) . . . . ? C38 N6 C32 C35 0.1(3) . . . . ? Ir2 N6 C32 C35 177.21(17) . . . . ? C33 N5 C32 N6 177.0(2) . . . . ? B2 N5 C32 N6 12.4(4) . . . . ? C33 N5 C32 C35 -2.1(3) . . . . ? B2 N5 C32 C35 -166.7(2) . . . . ? C32 N5 C33 C34 2.1(3) . . . . ? B2 N5 C33 C34 166.8(2) . . . . ? N5 C33 C34 C35 -1.3(3) . . . . ? N6 C32 C35 C36 0.9(4) . . . . ? N5 C32 C35 C36 -180.0(2) . . . . ? N6 C32 C35 C34 -177.8(2) . . . . ? N5 C32 C35 C34 1.4(3) . . . . ? C33 C34 C35 C36 -178.3(3) . . . . ? C33 C34 C35 C32 0.0(3) . . . . ? C32 C35 C36 C37 -1.3(3) . . . . ? C34 C35 C36 C37 176.8(3) . . . . ? C35 C36 C37 C38 0.8(4) . . . . ? C32 N6 C38 C37 -0.8(3) . . . . ? Ir2 N6 C38 C37 -177.80(18) . . . . ? C36 C37 C38 N6 0.3(4) . . . . ? C45 N8 C39 N7 177.8(2) . . . . ? Ir2 N8 C39 N7 2.3(3) . . . . ? C45 N8 C39 C42 0.5(3) . . . . ? Ir2 N8 C39 C42 -174.93(18) . . . . ? C40 N7 C39 N8 -175.5(2) . . . . ? B2 N7 C39 N8 -10.7(4) . . . . ? C40 N7 C39 C42 2.1(3) . . . . ? B2 N7 C39 C42 166.9(2) . . . . ? C39 N7 C40 C41 -2.2(3) . . . . ? B2 N7 C40 C41 -167.1(2) . . . . ? N7 C40 C41 C42 1.4(3) . . . . ? N8 C39 C42 C43 -0.9(4) . . . . ? N7 C39 C42 C43 -178.5(2) . . . . ? N8 C39 C42 C41 176.3(2) . . . . ? N7 C39 C42 C41 -1.3(3) . . . . ? C40 C41 C42 C43 176.4(3) . . . . ? C40 C41 C42 C39 0.0(3) . . . . ? C39 C42 C43 C44 0.7(4) . . . . ? C41 C42 C43 C44 -175.4(3) . . . . ? C42 C43 C44 C45 -0.1(4) . . . . ? C39 N8 C45 C44 0.1(4) . . . . ? Ir2 N8 C45 C44 175.5(2) . . . . ? C43 C44 C45 N8 -0.3(4) . . . . ? N7 B2 C46 C51 156.6(2) . . . . ? N5 B2 C46 C51 33.0(3) . . . . ? N7 B2 C46 C47 -30.1(3) . . . . ? N5 B2 C46 C47 -153.7(2) . . . . ? C51 C46 C47 C48 -7.7(4) . . . . ? B2 C46 C47 C48 178.6(2) . . . . ? C51 C46 C47 C52 167.7(2) . . . . ? B2 C46 C47 C52 -6.0(4) . . . . ? C46 C47 C48 C49 0.6(4) . . . . ? C52 C47 C48 C49 -175.1(3) . . . . ? C47 C48 C49 C50 4.9(4) . . . . ? C47 C48 C49 C53 -176.5(3) . . . . ? C48 C49 C50 C51 -3.2(4) . . . . ? C53 C49 C50 C51 178.3(3) . . . . ? C49 C50 C51 C46 -4.2(4) . . . . ? C49 C50 C51 C54 171.0(3) . . . . ? C47 C46 C51 C50 9.4(4) . . . . ? B2 C46 C51 C50 -176.8(2) . . . . ? C47 C46 C51 C54 -165.4(2) . . . . ? B2 C46 C51 C54 8.3(4) . . . . ? C60 Ir2 C55 C56 -100.12(17) . . . . ? C59 Ir2 C55 C56 -64.41(17) . . . . ? N6 Ir2 C55 C56 88.82(15) . . . . ? C56 Ir2 C55 C62 120.3(3) . . . . ? C60 Ir2 C55 C62 20.1(2) . . . . ? C59 Ir2 C55 C62 55.9(2) . . . . ? N6 Ir2 C55 C62 -150.9(2) . . . . ? C62 C55 C56 C57 4.4(4) . . . . ? Ir2 C55 C56 C57 108.5(2) . . . . ? C62 C55 C56 Ir2 -104.1(2) . . . . ? C60 Ir2 C56 C55 77.12(16) . . . . ? C59 Ir2 C56 C55 114.57(17) . . . . ? N6 Ir2 C56 C55 -92.07(15) . . . . ? N8 Ir2 C56 C55 -176.93(14) . . . . ? C55 Ir2 C56 C57 -117.0(3) . . . . ? C60 Ir2 C56 C57 -39.9(2) . . . . ? C59 Ir2 C56 C57 -2.4(2) . . . . ? N6 Ir2 C56 C57 150.9(2) . . . . ? N8 Ir2 C56 C57 66.1(3) . . . . ? C55 C56 C57 C58 -93.2(3) . . . . ? Ir2 C56 C57 C58 -12.2(4) . . . . ? C56 C57 C58 C59 25.9(4) . . . . ? C57 C58 C59 C60 53.4(4) . . . . ? C57 C58 C59 Ir2 -28.7(4) . . . . ? C55 Ir2 C59 C60 -67.63(17) . . . . ? C56 Ir2 C59 C60 -103.45(17) . . . . ? N6 Ir2 C59 C60 -175.19(16) . . . . ? N8 Ir2 C59 C60 108.75(16) . . . . ? C55 Ir2 C59 C58 52.7(2) . . . . ? C56 Ir2 C59 C58 16.9(2) . . . . ? C60 Ir2 C59 C58 120.4(3) . . . . ? N6 Ir2 C59 C58 -54.8(3) . . . . ? N8 Ir2 C59 C58 -130.9(2) . . . . ? C58 C59 C60 C61 -0.3(4) . . . . ? Ir2 C59 C60 C61 105.6(2) . . . . ? C58 C59 C60 Ir2 -105.8(3) . . . . ? C55 Ir2 C60 C59 112.08(17) . . . . ? C56 Ir2 C60 C59 73.13(17) . . . . ? N6 Ir2 C60 C59 167.8(4) . . . . ? N8 Ir2 C60 C59 -73.07(16) . . . . ? C55 Ir2 C60 C61 -6.0(2) . . . . ? C56 Ir2 C60 C61 -45.0(2) . . . . ? C59 Ir2 C60 C61 -118.1(3) . . . . ? N6 Ir2 C60 C61 49.7(6) . . . . ? N8 Ir2 C60 C61 168.8(2) . . . . ? C59 C60 C61 C62 -90.4(3) . . . . ? Ir2 C60 C61 C62 -9.2(3) . . . . ? C56 C55 C62 C61 50.4(4) . . . . ? Ir2 C55 C62 C61 -31.1(3) . . . . ? C60 C61 C62 C55 26.1(4) . . . . ? C63 C64 C65 C65 -170.4(3) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.176 _refine_diff_density_min -0.598 _refine_diff_density_rms 0.090 data_rh19_0m _database_code_depnum_ccdc_archive 'CCDC 802703' #TrackingRef '- Ligands Li(MeCN)2[ArBai] and Complexes 4_6_9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Complex_9 _chemical_melting_point ? _chemical_formula_moiety 'C31 H26 B N4 Rh' _chemical_formula_sum 'C31 H26 B N4 Rh' _chemical_formula_weight 568.28 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' 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 triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1069(3) _cell_length_b 19.9356(8) _cell_length_c 21.0333(8) _cell_angle_alpha 98.628(2) _cell_angle_beta 92.235(2) _cell_angle_gamma 101.699(2) _cell_volume 3687.5(2) _cell_formula_units_Z 6 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9898 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 27.49 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1740 _exptl_absorpt_coefficient_mu 0.724 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6743 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 60488 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 27.57 _reflns_number_total 16964 _reflns_number_gt 13980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _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. Theh structure contains three independent molecules in the asymmetric unit. In that containing Rh(3), the naphthyl unit is disordered over two positions. Some restraints on the thermal parameters were necessary in order to ensure a smooth refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.2632P] 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 16964 _refine_ls_number_parameters 1091 _refine_ls_number_restraints 326 _refine_ls_R_factor_all 0.0604 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.154 _refine_ls_restrained_S_all 1.143 _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 0.34637(3) 0.220928(14) 0.285848(13) 0.01490(6) Uani 1 1 d . . . N1 N 0.1299(3) 0.20617(15) 0.14916(14) 0.0153(6) Uani 1 1 d . . . N2 N 0.1071(3) 0.19042(15) 0.26005(14) 0.0177(6) Uani 1 1 d . . . N3 N 0.3743(3) 0.16825(14) 0.13058(13) 0.0147(6) Uani 1 1 d . . . N4 N 0.3734(3) 0.12590(14) 0.23213(14) 0.0151(6) Uani 1 1 d . . . B1 B 0.3025(4) 0.2323(2) 0.15000(19) 0.0163(8) Uani 1 1 d . . . H1B H 0.3396 0.2524 0.1956 0.020 Uiso 1 1 calc R . . C1 C 0.0490(4) 0.18797(18) 0.19982(17) 0.0163(7) Uani 1 1 d . . . C2 C 0.0261(4) 0.19068(18) 0.09600(17) 0.0184(8) Uani 1 1 d . . . H2 H 0.0511 0.1965 0.0535 0.022 Uiso 1 1 calc R . . C3 C -0.1158(4) 0.16610(19) 0.11242(18) 0.0208(8) Uani 1 1 d . . . H3 H -0.2046 0.1531 0.0843 0.025 Uiso 1 1 calc R . . C4 C -0.1056(4) 0.16370(17) 0.17893(18) 0.0174(7) Uani 1 1 d . . . C5 C -0.2047(4) 0.14352(19) 0.22452(19) 0.0235(8) Uani 1 1 d . . . H5 H -0.3095 0.1281 0.2133 0.028 Uiso 1 1 calc R . . C6 C -0.1455(4) 0.14671(19) 0.28688(19) 0.0238(8) Uani 1 1 d . . . H6 H -0.2104 0.1337 0.3192 0.029 Uiso 1 1 calc R . . C7 C 0.0077(4) 0.1688(2) 0.30231(19) 0.0233(8) Uani 1 1 d . . . H7 H 0.0448 0.1686 0.3451 0.028 Uiso 1 1 calc R . . C8 C 0.3910(4) 0.11988(17) 0.16849(16) 0.0150(7) Uani 1 1 d . . . C9 C 0.4067(4) 0.14179(19) 0.06963(17) 0.0181(7) Uani 1 1 d . . . H9 H 0.4030 0.1648 0.0334 0.022 Uiso 1 1 calc R . . C10 C 0.4447(4) 0.07839(19) 0.06733(17) 0.0195(8) Uani 1 1 d . . . H10 H 0.4728 0.0509 0.0308 0.023 Uiso 1 1 calc R . . C11 C 0.4333(4) 0.06203(18) 0.13088(17) 0.0168(7) Uani 1 1 d . . . C12 C 0.4512(4) 0.00682(19) 0.16160(18) 0.0205(8) Uani 1 1 d . . . H12 H 0.4794 -0.0329 0.1388 0.025 Uiso 1 1 calc R . . C13 C 0.4267(4) 0.01160(19) 0.22607(19) 0.0217(8) Uani 1 1 d . . . H13 H 0.4346 -0.0261 0.2479 0.026 Uiso 1 1 calc R . . C14 C 0.3905(4) 0.07102(18) 0.25986(18) 0.0199(8) Uani 1 1 d . . . H14 H 0.3771 0.0729 0.3046 0.024 Uiso 1 1 calc R . . C15 C 0.3504(4) 0.29281(17) 0.10694(16) 0.0146(7) Uani 1 1 d . . . C16 C 0.2462(4) 0.32666(18) 0.08416(17) 0.0181(7) Uani 1 1 d . . . H16 H 0.1449 0.3137 0.0947 0.022 Uiso 1 1 calc R . . C17 C 0.2818(4) 0.37945(19) 0.04611(18) 0.0220(8) Uani 1 1 d . . . H17 H 0.2053 0.4007 0.0314 0.026 Uiso 1 1 calc R . . C18 C 0.4254(4) 0.39998(19) 0.03044(18) 0.0228(8) Uani 1 1 d . . . H18 H 0.4480 0.4342 0.0033 0.027 Uiso 1 1 calc R . . C19 C 0.5423(4) 0.37063(18) 0.05435(17) 0.0181(7) Uani 1 1 d . . . C20 C 0.6924(4) 0.3938(2) 0.04093(17) 0.0234(8) Uani 1 1 d . . . H20 H 0.7157 0.4283 0.0142 0.028 Uiso 1 1 calc R . . C21 C 0.8053(4) 0.3675(2) 0.06577(19) 0.0247(9) Uani 1 1 d . . . H21 H 0.9061 0.3830 0.0558 0.030 Uiso 1 1 calc R . . C22 C 0.7711(4) 0.31737(19) 0.10610(18) 0.0219(8) Uani 1 1 d . . . H22 H 0.8501 0.3001 0.1244 0.026 Uiso 1 1 calc R . . C23 C 0.6264(4) 0.29285(18) 0.11962(17) 0.0172(7) Uani 1 1 d . . . H23 H 0.6067 0.2587 0.1469 0.021 Uiso 1 1 calc R . . C24 C 0.5038(4) 0.31756(17) 0.09352(16) 0.0144(7) Uani 1 1 d . . . C25 C 0.4001(5) 0.32912(19) 0.32587(18) 0.0246(9) Uani 1 1 d . . . H25 H 0.3665 0.3657 0.3048 0.029 Uiso 1 1 calc R . . C26 C 0.3152(4) 0.2927(2) 0.36794(18) 0.0266(9) Uani 1 1 d . . . H26 H 0.2141 0.3005 0.3798 0.032 Uiso 1 1 calc R . . C27 C 0.4279(4) 0.2742(2) 0.41540(17) 0.0248(9) Uani 1 1 d . . . H27 H 0.3904 0.2611 0.4569 0.030 Uiso 1 1 calc R . . C28 C 0.4805(4) 0.2189(2) 0.36875(17) 0.0222(8) Uani 1 1 d . . . H28 H 0.4987 0.1747 0.3815 0.027 Uiso 1 1 calc R . . C29 C 0.5667(4) 0.2534(2) 0.32411(18) 0.0219(8) Uani 1 1 d . . . H29 H 0.6532 0.2372 0.3036 0.026 Uiso 1 1 calc R . . C30 C 0.5642(4) 0.33146(19) 0.34606(18) 0.0221(8) Uani 1 1 d . . . H30 H 0.6421 0.3665 0.3297 0.027 Uiso 1 1 calc R . . C31 C 0.5593(4) 0.3367(2) 0.41946(18) 0.0256(9) Uani 1 1 d . . . H31A H 0.6526 0.3294 0.4406 0.031 Uiso 1 1 calc R . . H31B H 0.5346 0.3806 0.4402 0.031 Uiso 1 1 calc R . . Rh2 Rh -0.01032(3) 0.867617(14) 0.141765(13) 0.01403(6) Uani 1 1 d . . . B2 B 0.1205(5) 0.8661(2) 0.26858(19) 0.0195(9) Uani 1 1 d . . . H2B H 0.0797 0.8874 0.2334 0.023 Uiso 1 1 calc R . . N5 N 0.2608(3) 0.84147(15) 0.24315(14) 0.0181(6) Uani 1 1 d . . . N6 N 0.2013(3) 0.83515(14) 0.12893(14) 0.0156(6) Uani 1 1 d . . . N7 N -0.0009(3) 0.80100(15) 0.27521(14) 0.0193(7) Uani 1 1 d . . . N8 N -0.1061(3) 0.76997(15) 0.16531(14) 0.0165(6) Uani 1 1 d . . . C32 C 0.2879(4) 0.82650(17) 0.17928(17) 0.0151(7) Uani 1 1 d . . . C33 C 0.3708(4) 0.81898(19) 0.27671(19) 0.0241(9) Uani 1 1 d . . . H33 H 0.3774 0.8212 0.3222 0.029 Uiso 1 1 calc R . . C34 C 0.4681(4) 0.79340(19) 0.2373(2) 0.0266(9) Uani 1 1 d . . . H34 H 0.5539 0.7769 0.2499 0.032 Uiso 1 1 calc R . . C35 C 0.4159(4) 0.79628(18) 0.17316(19) 0.0202(8) Uani 1 1 d . . . C36 C 0.4555(4) 0.77493(19) 0.1116(2) 0.0238(8) Uani 1 1 d . . . H36 H 0.5405 0.7545 0.1052 0.029 Uiso 1 1 calc R . . C37 C 0.3678(4) 0.78427(18) 0.05971(19) 0.0219(8) Uani 1 1 d . . . H37 H 0.3921 0.7701 0.0169 0.026 Uiso 1 1 calc R . . C38 C 0.2440(4) 0.81441(18) 0.07027(17) 0.0194(8) Uani 1 1 d . . . H38 H 0.1865 0.8206 0.0338 0.023 Uiso 1 1 calc R . . C39 C -0.0925(4) 0.75827(18) 0.22682(17) 0.0183(8) Uani 1 1 d . . . C40 C -0.0205(5) 0.7690(2) 0.32910(19) 0.0263(9) Uani 1 1 d . . . H40 H 0.0301 0.7877 0.3702 0.032 Uiso 1 1 calc R . . C41 C -0.1215(5) 0.7071(2) 0.31586(19) 0.0274(9) Uani 1 1 d . . . H41 H -0.1524 0.6760 0.3452 0.033 Uiso 1 1 calc R . . C42 C -0.1716(4) 0.69828(19) 0.24967(19) 0.0210(8) Uani 1 1 d . . . C43 C -0.2663(4) 0.6480(2) 0.2061(2) 0.0257(9) Uani 1 1 d . . . H43 H -0.3216 0.6072 0.2193 0.031 Uiso 1 1 calc R . . C44 C -0.2786(4) 0.65847(19) 0.1426(2) 0.0253(9) Uani 1 1 d . . . H44 H -0.3424 0.6245 0.1115 0.030 Uiso 1 1 calc R . . C45 C -0.1977(4) 0.71870(18) 0.12430(19) 0.0200(8) Uani 1 1 d . . . H45 H -0.2076 0.7240 0.0803 0.024 Uiso 1 1 calc R . . C46 C 0.1455(5) 0.92442(19) 0.33215(17) 0.0241(9) Uani 1 1 d . . . C47 C 0.2814(5) 0.9508(2) 0.36644(18) 0.0302(10) Uani 1 1 d . . . H47 H 0.3653 0.9315 0.3542 0.036 Uiso 1 1 calc R . . C48 C 0.3012(6) 1.0057(2) 0.4194(2) 0.0406(12) Uani 1 1 d . . . H48 H 0.3974 1.0223 0.4419 0.049 Uiso 1 1 calc R . . C49 C 0.1855(7) 1.0345(2) 0.4384(2) 0.0481(14) Uani 1 1 d . . . H49 H 0.2009 1.0714 0.4738 0.058 Uiso 1 1 calc R . . C50 C 0.0414(6) 1.0105(2) 0.40606(19) 0.0371(11) Uani 1 1 d . . . C51 C -0.0843(7) 1.0392(3) 0.4256(2) 0.0517(15) Uani 1 1 d . . . H51 H -0.0717 1.0748 0.4620 0.062 Uiso 1 1 calc R . . C52 C -0.2214(7) 1.0164(3) 0.3933(2) 0.0512(14) Uani 1 1 d . . . H52 H -0.3033 1.0365 0.4070 0.061 Uiso 1 1 calc R . . C53 C -0.2426(6) 0.9639(2) 0.3400(2) 0.0428(12) Uani 1 1 d . . . H53 H -0.3387 0.9484 0.3173 0.051 Uiso 1 1 calc R . . C54 C -0.1248(5) 0.9341(2) 0.3202(2) 0.0352(11) Uani 1 1 d . . . H54 H -0.1414 0.8983 0.2837 0.042 Uiso 1 1 calc R . . C55 C 0.0202(5) 0.9553(2) 0.35230(19) 0.0311(10) Uani 1 1 d . . . C56 C -0.2112(4) 0.90064(18) 0.13838(17) 0.0176(7) Uani 1 1 d . . . H56 H -0.3000 0.8810 0.1614 0.021 Uiso 1 1 calc R . . C57 C -0.1831(4) 0.87108(18) 0.07530(17) 0.0179(7) Uani 1 1 d . . . H57 H -0.2498 0.8284 0.0503 0.022 Uiso 1 1 calc R . . C58 C -0.1037(4) 0.93173(18) 0.04340(17) 0.0180(7) Uani 1 1 d . . . H58 H -0.1018 0.9237 -0.0046 0.022 Uiso 1 1 calc R . . C59 C 0.0481(4) 0.94795(18) 0.08351(17) 0.0197(8) Uani 1 1 d . . . H59 H 0.1473 0.9585 0.0644 0.024 Uiso 1 1 calc R . . C60 C 0.0218(4) 0.97797(18) 0.14519(18) 0.0196(8) Uani 1 1 d . . . H60 H 0.1000 1.0124 0.1745 0.023 Uiso 1 1 calc R . . C61 C -0.1469(4) 0.97902(18) 0.14392(17) 0.0199(8) Uani 1 1 d . . . H61 H -0.1809 1.0105 0.1793 0.024 Uiso 1 1 calc R . . C62 C -0.1766(4) 0.99068(18) 0.07419(18) 0.0208(8) Uani 1 1 d . . . H62A H -0.2851 0.9828 0.0610 0.025 Uiso 1 1 calc R . . H62B H -0.1239 1.0369 0.0663 0.025 Uiso 1 1 calc R . . Rh3 Rh 0.23719(3) 0.532324(14) 0.226004(13) 0.01262(6) Uani 1 1 d . . . N9 N 0.4680(3) 0.56795(15) 0.36045(14) 0.0187(6) Uani 1 1 d . A . N10 N 0.4474(3) 0.50882(14) 0.25038(14) 0.0147(6) Uani 1 1 d . A . N11 N 0.2028(3) 0.52084(18) 0.38187(14) 0.0241(7) Uani 1 1 d . A . N12 N 0.1270(3) 0.45362(15) 0.27653(14) 0.0181(6) Uani 1 1 d . A . B3 B 0.3087(5) 0.5852(2) 0.3633(2) 0.0209(9) Uani 1 1 d . . . H3B H 0.2750 0.5891 0.3185 0.025 Uiso 1 1 calc R A 1 C63 C 0.5196(4) 0.53130(18) 0.30926(17) 0.0166(7) Uani 1 1 d . . . C64 C 0.5744(4) 0.5764(2) 0.41162(18) 0.0245(9) Uani 1 1 d . . . H64 H 0.5654 0.5991 0.4539 0.029 Uiso 1 1 calc R A . C65 C 0.6932(4) 0.5480(2) 0.39369(18) 0.0283(10) Uani 1 1 d . A . H65 H 0.7798 0.5479 0.4203 0.034 Uiso 1 1 calc R . . C66 C 0.6630(4) 0.51846(19) 0.32756(18) 0.0215(8) Uani 1 1 d . A . C67 C 0.7336(4) 0.48218(19) 0.28124(19) 0.0228(8) Uani 1 1 d . . . H67 H 0.8305 0.4738 0.2907 0.027 Uiso 1 1 calc R A . C68 C 0.6604(4) 0.45851(18) 0.22097(19) 0.0212(8) Uani 1 1 d . A . H68 H 0.7061 0.4330 0.1885 0.025 Uiso 1 1 calc R . . C69 C 0.5193(4) 0.47214(18) 0.20785(17) 0.0177(7) Uani 1 1 d . . . H69 H 0.4707 0.4544 0.1662 0.021 Uiso 1 1 calc R A . C70 C 0.1271(4) 0.4633(2) 0.34114(17) 0.0203(8) Uani 1 1 d . . . C71 C 0.1782(5) 0.5065(3) 0.44359(19) 0.0406(12) Uani 1 1 d . . . H71 H 0.2203 0.5371 0.4819 0.049 Uiso 1 1 calc R A . C72 C 0.0867(5) 0.4434(3) 0.4426(2) 0.0469(14) Uani 1 1 d . A . H72 H 0.0533 0.4231 0.4790 0.056 Uiso 1 1 calc R . . C73 C 0.0506(4) 0.4138(2) 0.3772(2) 0.0289(10) Uani 1 1 d . A . C74 C -0.0342(4) 0.3520(2) 0.3438(2) 0.0333(10) Uani 1 1 d . . . H74 H -0.0890 0.3179 0.3659 0.040 Uiso 1 1 calc R A . C75 C -0.0363(5) 0.3416(2) 0.2775(2) 0.0289(9) Uani 1 1 d . A . H75 H -0.0938 0.3000 0.2531 0.035 Uiso 1 1 calc R . . C76 C 0.0459(4) 0.39223(19) 0.24616(19) 0.0238(8) Uani 1 1 d . . . H76 H 0.0446 0.3828 0.2005 0.029 Uiso 1 1 calc R A . C77A C 0.2736(7) 0.6514(3) 0.4106(3) 0.0163(12) Uani 0.669(5) 1 d PU B 1 C78A C 0.1356(8) 0.6489(4) 0.4367(3) 0.0186(14) Uani 0.669(5) 1 d PU B 1 H78A H 0.0640 0.6061 0.4283 0.022 Uiso 0.669(5) 1 calc PR B 1 C79A C 0.0950(8) 0.7052(3) 0.4749(3) 0.0240(13) Uani 0.669(5) 1 d PU B 1 H79A H -0.0014 0.7003 0.4916 0.029 Uiso 0.669(5) 1 calc PR B 1 C80A C 0.1967(8) 0.7680(4) 0.4879(3) 0.0255(14) Uani 0.669(5) 1 d PU B 1 H80A H 0.1733 0.8055 0.5162 0.031 Uiso 0.669(5) 1 calc PR B 1 C81A C 0.3362(13) 0.7766(8) 0.4590(10) 0.020(2) Uani 0.669(5) 1 d PU B 1 C82A C 0.4347(9) 0.8417(4) 0.4681(4) 0.0241(15) Uani 0.669(5) 1 d PU B 1 H82A H 0.4087 0.8797 0.4948 0.029 Uiso 0.669(5) 1 calc PR B 1 C83A C 0.5658(7) 0.8512(3) 0.4395(3) 0.0256(14) Uani 0.669(5) 1 d PU B 1 H83A H 0.6305 0.8959 0.4459 0.031 Uiso 0.669(5) 1 calc PR B 1 C84A C 0.6069(7) 0.7951(3) 0.4002(3) 0.0226(13) Uani 0.669(5) 1 d PU B 1 H84A H 0.6992 0.8021 0.3801 0.027 Uiso 0.669(5) 1 calc PR B 1 C85A C 0.5145(15) 0.7310(5) 0.3912(8) 0.020(2) Uani 0.669(5) 1 d PU B 1 H85A H 0.5439 0.6937 0.3648 0.024 Uiso 0.669(5) 1 calc PR B 1 C86A C 0.3744(6) 0.7184(3) 0.4204(3) 0.0171(12) Uani 0.669(5) 1 d PU B 1 C77B C 0.3599(14) 0.6700(6) 0.4004(5) 0.013(2) Uani 0.331(5) 1 d PU B 2 C78B C 0.501(3) 0.7117(10) 0.3963(15) 0.018(4) Uani 0.331(5) 1 d PU B 2 H78B H 0.5720 0.6916 0.3724 0.022 Uiso 0.331(5) 1 calc PR B 2 C79B C 0.5441(14) 0.7816(6) 0.4254(6) 0.018(2) Uani 0.331(5) 1 d PU B 2 H79B H 0.6422 0.8076 0.4218 0.022 Uiso 0.331(5) 1 calc PR B 2 C80B C 0.4402(18) 0.8120(7) 0.4597(8) 0.022(3) Uani 0.331(5) 1 d PU B 2 H80B H 0.4671 0.8591 0.4803 0.026 Uiso 0.331(5) 1 calc PR B 2 C81B C 0.295(3) 0.7728(16) 0.464(2) 0.016(3) Uani 0.331(5) 1 d PU B 2 C82B C 0.1874(15) 0.8050(7) 0.4978(6) 0.025(3) Uani 0.331(5) 1 d PU B 2 H82B H 0.2176 0.8515 0.5197 0.030 Uiso 0.331(5) 1 calc PR B 2 C83B C 0.0446(14) 0.7708(6) 0.4995(5) 0.025(3) Uani 0.331(5) 1 d PU B 2 H83B H -0.0236 0.7929 0.5234 0.030 Uiso 0.331(5) 1 calc PR B 2 C84B C -0.0057(15) 0.7021(6) 0.4660(6) 0.023(3) Uani 0.331(5) 1 d PU B 2 H84B H -0.1073 0.6784 0.4660 0.028 Uiso 0.331(5) 1 calc PR B 2 C85B C 0.0974(16) 0.6708(8) 0.4335(8) 0.020(3) Uani 0.331(5) 1 d PU B 2 H85B H 0.0632 0.6249 0.4109 0.024 Uiso 0.331(5) 1 calc PR B 2 C86B C 0.2509(12) 0.7024(5) 0.4314(5) 0.014(2) Uani 0.331(5) 1 d PU B 2 C87 C 0.3102(4) 0.61896(18) 0.18099(17) 0.0186(8) Uani 1 1 d . A . H87 H 0.4098 0.6516 0.1924 0.022 Uiso 1 1 calc R . . C88 C 0.2888(4) 0.55846(18) 0.13454(16) 0.0169(7) Uani 1 1 d . A . H88 H 0.3722 0.5437 0.1103 0.020 Uiso 1 1 calc R . . C89 C 0.1268(4) 0.54679(19) 0.10460(17) 0.0188(8) Uani 1 1 d . . . H89 H 0.1008 0.5154 0.0622 0.023 Uiso 1 1 calc R A . C90 C 0.0443(4) 0.52447(19) 0.16260(16) 0.0180(7) Uani 1 1 d . A . H90 H -0.0452 0.4852 0.1584 0.022 Uiso 1 1 calc R . . C91 C 0.0620(4) 0.58442(19) 0.20955(17) 0.0186(8) Uani 1 1 d . A . H91 H -0.0141 0.5924 0.2413 0.022 Uiso 1 1 calc R . . C92 C 0.1599(4) 0.64282(19) 0.18015(17) 0.0192(8) Uani 1 1 d . . . H92 H 0.1613 0.6916 0.2005 0.023 Uiso 1 1 calc R A . C93 C 0.1056(4) 0.62198(19) 0.10832(17) 0.0215(8) Uani 1 1 d . A . H93A H 0.1708 0.6485 0.0801 0.026 Uiso 1 1 calc R . . H93B H -0.0005 0.6247 0.0997 0.026 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 0.01390(14) 0.01706(14) 0.01420(14) 0.00306(11) -0.00017(10) 0.00418(11) N1 0.0144(15) 0.0141(15) 0.0174(15) 0.0015(12) -0.0022(12) 0.0041(12) N2 0.0145(15) 0.0194(16) 0.0202(16) 0.0048(13) 0.0012(12) 0.0044(12) N3 0.0136(15) 0.0135(15) 0.0165(15) 0.0023(12) -0.0010(11) 0.0021(11) N4 0.0153(15) 0.0135(15) 0.0172(15) 0.0055(12) -0.0003(12) 0.0026(11) B1 0.016(2) 0.018(2) 0.0120(19) -0.0018(16) -0.0010(15) 0.0009(16) C1 0.0125(17) 0.0140(17) 0.0223(19) 0.0028(15) 0.0011(14) 0.0030(13) C2 0.0210(19) 0.0159(18) 0.0183(18) 0.0013(15) -0.0035(14) 0.0058(15) C3 0.0188(19) 0.0203(19) 0.0220(19) 0.0010(15) -0.0082(15) 0.0048(15) C4 0.0130(18) 0.0104(17) 0.028(2) -0.0002(15) -0.0017(14) 0.0037(13) C5 0.0133(18) 0.021(2) 0.036(2) 0.0033(17) 0.0022(16) 0.0023(15) C6 0.0176(19) 0.021(2) 0.032(2) 0.0041(17) 0.0079(16) 0.0027(15) C7 0.023(2) 0.026(2) 0.023(2) 0.0068(16) 0.0025(16) 0.0061(16) C8 0.0108(17) 0.0139(17) 0.0182(18) 0.0012(14) -0.0029(13) -0.0005(13) C9 0.0191(19) 0.0216(19) 0.0127(17) 0.0012(14) -0.0011(14) 0.0040(15) C10 0.0207(19) 0.0201(19) 0.0169(18) -0.0022(15) -0.0008(14) 0.0063(15) C11 0.0118(17) 0.0145(18) 0.0212(19) -0.0020(14) -0.0040(14) 0.0004(13) C12 0.0191(19) 0.0138(18) 0.028(2) 0.0030(15) -0.0037(15) 0.0038(14) C13 0.0173(19) 0.0167(19) 0.032(2) 0.0118(16) -0.0037(16) 0.0020(15) C14 0.0198(19) 0.0197(19) 0.0201(19) 0.0068(15) -0.0013(15) 0.0018(15) C15 0.0181(18) 0.0131(17) 0.0119(16) -0.0003(13) -0.0002(13) 0.0032(14) C16 0.0156(18) 0.0180(19) 0.0200(18) 0.0015(15) -0.0011(14) 0.0040(14) C17 0.025(2) 0.0188(19) 0.023(2) 0.0024(16) -0.0063(16) 0.0086(16) C18 0.029(2) 0.020(2) 0.0198(19) 0.0087(16) -0.0014(16) 0.0014(16) C19 0.023(2) 0.0158(18) 0.0140(17) 0.0008(14) 0.0022(14) 0.0003(15) C20 0.029(2) 0.021(2) 0.0165(19) 0.0006(15) 0.0066(16) -0.0018(16) C21 0.020(2) 0.022(2) 0.028(2) -0.0030(17) 0.0077(16) -0.0022(16) C22 0.022(2) 0.0176(19) 0.024(2) -0.0044(16) -0.0008(15) 0.0059(15) C23 0.0204(19) 0.0119(17) 0.0178(18) -0.0016(14) 0.0023(14) 0.0030(14) C24 0.0198(18) 0.0104(16) 0.0112(16) -0.0012(13) 0.0001(13) 0.0014(13) C25 0.042(2) 0.0129(18) 0.0181(19) -0.0075(15) -0.0097(17) 0.0127(17) C26 0.024(2) 0.036(2) 0.021(2) -0.0073(17) 0.0017(16) 0.0156(18) C27 0.029(2) 0.030(2) 0.0124(18) 0.0031(16) -0.0009(15) -0.0004(17) C28 0.027(2) 0.021(2) 0.0184(19) 0.0046(16) -0.0085(15) 0.0056(16) C29 0.0098(18) 0.029(2) 0.026(2) 0.0100(17) -0.0049(14) 0.0006(15) C30 0.021(2) 0.021(2) 0.0211(19) 0.0045(16) -0.0025(15) -0.0039(15) C31 0.028(2) 0.030(2) 0.0184(19) 0.0007(17) -0.0036(16) 0.0063(17) Rh2 0.01574(14) 0.01202(14) 0.01493(14) 0.00433(11) -0.00012(10) 0.00296(10) B2 0.032(2) 0.014(2) 0.014(2) 0.0038(16) 0.0007(17) 0.0060(17) N5 0.0229(17) 0.0136(15) 0.0162(15) 0.0022(12) -0.0072(12) 0.0019(12) N6 0.0192(16) 0.0121(15) 0.0158(15) 0.0041(12) -0.0007(12) 0.0030(12) N7 0.0265(17) 0.0176(16) 0.0153(15) 0.0049(13) 0.0040(13) 0.0059(13) N8 0.0150(15) 0.0150(15) 0.0202(16) 0.0052(12) 0.0019(12) 0.0029(12) C32 0.0152(18) 0.0084(16) 0.0193(18) 0.0008(14) -0.0050(14) -0.0011(13) C33 0.030(2) 0.0162(19) 0.024(2) 0.0046(16) -0.0117(16) 0.0021(16) C34 0.027(2) 0.019(2) 0.034(2) 0.0028(17) -0.0130(17) 0.0069(16) C35 0.0142(18) 0.0107(17) 0.033(2) 0.0030(16) -0.0047(15) -0.0017(14) C36 0.0150(19) 0.018(2) 0.037(2) 0.0048(17) 0.0003(16) 0.0019(15) C37 0.022(2) 0.0169(19) 0.025(2) 0.0017(16) 0.0085(16) 0.0007(15) C38 0.024(2) 0.0184(19) 0.0152(18) 0.0026(15) 0.0010(14) 0.0021(15) C39 0.0203(19) 0.0182(19) 0.0198(19) 0.0074(15) 0.0059(15) 0.0080(15) C40 0.043(3) 0.024(2) 0.0180(19) 0.0085(16) 0.0091(17) 0.0152(18) C41 0.040(2) 0.022(2) 0.030(2) 0.0171(18) 0.0169(18) 0.0147(18) C42 0.0188(19) 0.0185(19) 0.031(2) 0.0123(16) 0.0114(16) 0.0093(15) C43 0.018(2) 0.018(2) 0.046(3) 0.0140(18) 0.0076(17) 0.0056(15) C44 0.0150(19) 0.0135(19) 0.047(3) 0.0056(17) -0.0035(17) 0.0020(14) C45 0.0182(19) 0.0166(19) 0.027(2) 0.0061(16) -0.0010(15) 0.0054(15) C46 0.045(3) 0.0149(19) 0.0134(18) 0.0042(15) -0.0011(16) 0.0070(17) C47 0.052(3) 0.018(2) 0.018(2) 0.0039(16) -0.0023(18) 0.0045(19) C48 0.069(4) 0.023(2) 0.021(2) -0.0027(18) -0.010(2) -0.003(2) C49 0.096(5) 0.025(2) 0.020(2) -0.0060(19) 0.010(3) 0.012(3) C50 0.077(4) 0.020(2) 0.016(2) 0.0025(17) 0.005(2) 0.014(2) C51 0.106(5) 0.031(3) 0.028(3) 0.006(2) 0.029(3) 0.033(3) C52 0.087(4) 0.045(3) 0.037(3) 0.012(2) 0.020(3) 0.040(3) C53 0.063(3) 0.042(3) 0.034(3) 0.011(2) 0.013(2) 0.032(3) C54 0.057(3) 0.032(2) 0.025(2) 0.0086(19) 0.007(2) 0.024(2) C55 0.062(3) 0.019(2) 0.0161(19) 0.0054(16) 0.0036(19) 0.016(2) C56 0.0167(18) 0.0166(18) 0.0212(19) 0.0055(15) -0.0005(14) 0.0061(14) C57 0.0207(19) 0.0149(18) 0.0190(18) 0.0060(15) -0.0020(14) 0.0040(14) C58 0.0202(19) 0.0158(18) 0.0184(18) 0.0047(15) -0.0014(14) 0.0038(14) C59 0.026(2) 0.0146(18) 0.0217(19) 0.0115(15) 0.0019(15) 0.0049(15) C60 0.022(2) 0.0090(17) 0.026(2) 0.0053(15) -0.0067(15) -0.0010(14) C61 0.027(2) 0.0126(18) 0.0190(19) -0.0006(14) -0.0021(15) 0.0063(15) C62 0.023(2) 0.0137(18) 0.026(2) 0.0066(15) -0.0046(15) 0.0033(15) Rh3 0.01399(14) 0.01246(13) 0.01136(13) 0.00197(10) -0.00025(10) 0.00283(10) N9 0.0221(17) 0.0172(16) 0.0150(15) 0.0041(12) -0.0023(12) -0.0006(13) N10 0.0139(15) 0.0114(14) 0.0177(15) 0.0022(12) -0.0006(12) 0.0001(11) N11 0.0203(17) 0.043(2) 0.0132(15) 0.0087(15) 0.0027(12) 0.0120(15) N12 0.0213(16) 0.0164(16) 0.0196(16) 0.0058(13) 0.0059(12) 0.0083(13) B3 0.031(2) 0.019(2) 0.015(2) -0.0010(17) -0.0031(17) 0.0127(18) C63 0.0144(18) 0.0125(17) 0.0215(19) 0.0076(14) -0.0027(14) -0.0034(13) C64 0.023(2) 0.029(2) 0.0177(19) 0.0100(16) -0.0073(15) -0.0060(16) C65 0.020(2) 0.040(3) 0.021(2) 0.0151(18) -0.0105(16) -0.0080(18) C66 0.0182(19) 0.023(2) 0.025(2) 0.0139(16) -0.0035(15) 0.0011(15) C67 0.0149(19) 0.023(2) 0.034(2) 0.0166(17) 0.0017(16) 0.0029(15) C68 0.0182(19) 0.0153(18) 0.033(2) 0.0069(16) 0.0054(16) 0.0060(15) C69 0.0183(19) 0.0127(17) 0.0206(19) 0.0016(14) 0.0012(14) 0.0006(14) C70 0.0162(18) 0.032(2) 0.0190(19) 0.0120(17) 0.0050(14) 0.0141(16) C71 0.024(2) 0.087(4) 0.0117(19) 0.012(2) 0.0029(16) 0.010(2) C72 0.022(2) 0.098(4) 0.026(2) 0.033(3) 0.0070(18) 0.005(2) C73 0.017(2) 0.049(3) 0.030(2) 0.027(2) 0.0086(16) 0.0120(18) C74 0.021(2) 0.040(3) 0.048(3) 0.031(2) 0.0091(19) 0.0091(19) C75 0.027(2) 0.020(2) 0.045(3) 0.0138(19) 0.0121(19) 0.0075(17) C76 0.030(2) 0.0163(19) 0.028(2) 0.0061(16) 0.0100(17) 0.0073(16) C77A 0.019(3) 0.017(3) 0.012(3) 0.003(2) -0.001(2) 0.002(2) C78A 0.017(3) 0.023(4) 0.017(3) 0.003(3) 0.002(2) 0.005(2) C79A 0.025(4) 0.029(3) 0.021(3) 0.004(3) 0.010(3) 0.012(3) C80A 0.041(4) 0.024(3) 0.014(3) -0.001(3) 0.001(3) 0.015(3) C81A 0.032(6) 0.014(4) 0.014(4) 0.001(3) -0.002(5) 0.006(4) C82A 0.039(4) 0.013(4) 0.018(3) 0.000(3) -0.005(3) 0.004(3) C83A 0.033(3) 0.015(3) 0.025(3) 0.008(2) -0.011(2) -0.004(2) C84A 0.025(3) 0.020(3) 0.022(3) 0.010(2) -0.005(3) -0.001(2) C85A 0.020(4) 0.018(5) 0.021(4) 0.003(4) -0.004(3) 0.004(4) C86A 0.023(3) 0.015(3) 0.013(3) 0.001(2) -0.004(2) 0.005(2) C77B 0.018(5) 0.015(6) 0.008(5) 0.003(4) -0.001(4) 0.007(4) C78B 0.030(7) 0.012(8) 0.011(7) -0.004(8) 0.003(6) 0.006(6) C79B 0.022(6) 0.014(5) 0.018(6) 0.010(5) -0.005(4) 0.001(4) C80B 0.032(6) 0.005(6) 0.026(7) -0.005(6) -0.005(5) 0.004(5) C81B 0.027(8) 0.013(6) 0.005(7) -0.002(5) -0.001(8) 0.002(6) C82B 0.036(6) 0.016(6) 0.026(7) -0.005(5) 0.000(5) 0.016(5) C83B 0.032(5) 0.030(6) 0.020(6) 0.004(5) 0.004(5) 0.020(5) C84B 0.019(6) 0.026(6) 0.027(6) 0.005(5) 0.010(5) 0.005(5) C85B 0.019(6) 0.014(7) 0.029(7) 0.003(5) 0.004(5) 0.006(4) C86B 0.019(5) 0.015(5) 0.008(5) -0.002(4) -0.003(4) 0.006(4) C87 0.0158(18) 0.0168(18) 0.0240(19) 0.0099(15) 0.0020(14) 0.0002(14) C88 0.0180(18) 0.0191(19) 0.0165(18) 0.0083(15) 0.0040(14) 0.0061(14) C89 0.022(2) 0.023(2) 0.0116(17) 0.0042(15) -0.0029(14) 0.0055(15) C90 0.0148(18) 0.024(2) 0.0141(17) 0.0058(15) -0.0049(14) 0.0000(14) C91 0.0153(18) 0.027(2) 0.0181(18) 0.0058(16) 0.0018(14) 0.0128(15) C92 0.0209(19) 0.0177(19) 0.0215(19) 0.0053(15) 0.0050(15) 0.0076(15) C93 0.021(2) 0.025(2) 0.0221(19) 0.0126(16) 0.0024(15) 0.0074(16) _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 H1B 2.0891 . ? Rh1 C29 2.069(3) . ? Rh1 C28 2.100(3) . ? Rh1 N4 2.120(3) . ? Rh1 C26 2.137(4) . ? Rh1 C25 2.144(4) . ? Rh1 N2 2.164(3) . ? N1 C1 1.370(4) . ? N1 C2 1.391(4) . ? N1 B1 1.551(5) . ? N2 C1 1.344(4) . ? N2 C7 1.348(5) . ? N3 C8 1.367(4) . ? N3 C9 1.377(4) . ? N3 B1 1.558(5) . ? N4 C8 1.345(4) . ? N4 C14 1.347(4) . ? B1 C15 1.617(5) . ? B1 H1B 1.0000 . ? C1 C4 1.422(5) . ? C2 C3 1.363(5) . ? C2 H2 0.9500 . ? C3 C4 1.407(5) . ? C3 H3 0.9500 . ? C4 C5 1.390(5) . ? C5 C6 1.386(5) . ? C5 H5 0.9500 . ? C6 C7 1.385(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C11 1.427(5) . ? C9 C10 1.371(5) . ? C9 H9 0.9500 . ? C10 C11 1.425(5) . ? C10 H10 0.9500 . ? C11 C12 1.390(5) . ? C12 C13 1.375(5) . ? C12 H12 0.9500 . ? C13 C14 1.394(5) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.382(5) . ? C15 C24 1.438(5) . ? C16 C17 1.410(5) . ? C16 H16 0.9500 . ? C17 C18 1.357(5) . ? C17 H17 0.9500 . ? C18 C19 1.424(5) . ? C18 H18 0.9500 . ? C19 C20 1.405(5) . ? C19 C24 1.433(5) . ? C20 C21 1.366(5) . ? C20 H20 0.9500 . ? C21 C22 1.401(5) . ? C21 H21 0.9500 . ? C22 C23 1.366(5) . ? C22 H22 0.9500 . ? C23 C24 1.431(5) . ? C23 H23 0.9500 . ? C25 C26 1.388(6) . ? C25 C30 1.527(5) . ? C25 H25 1.0000 . ? C26 C27 1.539(5) . ? C26 H26 1.0000 . ? C27 C28 1.528(5) . ? C27 C31 1.532(5) . ? C27 H27 1.0000 . ? C28 C29 1.416(5) . ? C28 H28 1.0000 . ? C29 C30 1.560(5) . ? C29 H29 1.0000 . ? C30 C31 1.535(5) . ? C30 H30 1.0000 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? Rh2 H2B 2.0156 . ? Rh2 C56 2.068(3) . ? Rh2 C57 2.083(3) . ? Rh2 N8 2.105(3) . ? Rh2 C60 2.149(3) . ? Rh2 C59 2.155(3) . ? Rh2 N6 2.168(3) . ? B2 N5 1.545(5) . ? B2 N7 1.553(5) . ? B2 C46 1.610(5) . ? B2 H2B 1.0000 . ? N5 C32 1.375(4) . ? N5 C33 1.388(4) . ? N6 C38 1.340(4) . ? N6 C32 1.348(4) . ? N7 C39 1.357(5) . ? N7 C40 1.382(4) . ? N8 C45 1.349(5) . ? N8 C39 1.354(4) . ? C32 C35 1.418(5) . ? C33 C34 1.359(6) . ? C33 H33 0.9500 . ? C34 C35 1.426(5) . ? C34 H34 0.9500 . ? C35 C36 1.386(5) . ? C36 C37 1.385(5) . ? C36 H36 0.9500 . ? C37 C38 1.391(5) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 C42 1.425(5) . ? C40 C41 1.365(6) . ? C40 H40 0.9500 . ? C41 C42 1.422(5) . ? C41 H41 0.9500 . ? C42 C43 1.379(5) . ? C43 C44 1.388(6) . ? C43 H43 0.9500 . ? C44 C45 1.390(5) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.371(6) . ? C46 C55 1.451(6) . ? C47 C48 1.418(6) . ? C47 H47 0.9500 . ? C48 C49 1.345(7) . ? C48 H48 0.9500 . ? C49 C50 1.411(7) . ? C49 H49 0.9500 . ? C50 C51 1.428(7) . ? C50 C55 1.431(5) . ? C51 C52 1.356(8) . ? C51 H51 0.9500 . ? C52 C53 1.392(7) . ? C52 H52 0.9500 . ? C53 C54 1.376(6) . ? C53 H53 0.9500 . ? C54 C55 1.413(6) . ? C54 H54 0.9500 . ? C56 C57 1.423(5) . ? C56 C61 1.539(5) . ? C56 H56 1.0000 . ? C57 C58 1.537(5) . ? C57 H57 1.0000 . ? C58 C62 1.537(5) . ? C58 C59 1.540(5) . ? C58 H58 1.0000 . ? C59 C60 1.396(5) . ? C59 H59 1.0000 . ? C60 C61 1.540(5) . ? C60 H60 1.0000 . ? C61 C62 1.541(5) . ? C61 H61 1.0000 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? Rh3 H3B 2.0762 . ? Rh3 C87 2.097(3) . ? Rh3 C88 2.113(3) . ? Rh3 C91 2.117(3) . ? Rh3 N10 2.123(3) . ? Rh3 C90 2.129(3) . ? Rh3 N12 2.132(3) . ? N9 C63 1.362(5) . ? N9 C64 1.387(4) . ? N9 B3 1.559(5) . ? N10 C69 1.344(4) . ? N10 C63 1.348(4) . ? N11 C70 1.365(5) . ? N11 C71 1.388(5) . ? N11 B3 1.551(5) . ? N12 C70 1.344(4) . ? N12 C76 1.347(5) . ? B3 C77A 1.623(7) . ? B3 C77B 1.714(13) . ? B3 H3B 1.0000 . ? C63 C66 1.430(5) . ? C64 C65 1.360(6) . ? C64 H64 0.9500 . ? C65 C66 1.420(5) . ? C65 H65 0.9500 . ? C66 C67 1.383(5) . ? C67 C68 1.379(5) . ? C67 H67 0.9500 . ? C68 C69 1.392(5) . ? C68 H68 0.9500 . ? C69 H69 0.9500 . ? C70 C73 1.422(5) . ? C71 C72 1.358(7) . ? C71 H71 0.9500 . ? C72 C73 1.411(6) . ? C72 H72 0.9500 . ? C73 C74 1.385(6) . ? C74 C75 1.378(6) . ? C74 H74 0.9500 . ? C75 C76 1.394(5) . ? C75 H75 0.9500 . ? C76 H76 0.9500 . ? C77A C78A 1.386(9) . ? C77A C86A 1.439(8) . ? C78A C79A 1.401(9) . ? C78A H78A 0.9500 . ? C79A C80A 1.381(9) . ? C79A H79A 0.9500 . ? C80A C81A 1.420(11) . ? C80A H80A 0.9500 . ? C81A C82A 1.401(13) . ? C81A C86A 1.426(14) . ? C82A C83A 1.348(10) . ? C82A H82A 0.9500 . ? C83A C84A 1.411(9) . ? C83A H83A 0.9500 . ? C84A C85A 1.363(10) . ? C84A H84A 0.9500 . ? C85A C86A 1.430(14) . ? C85A H85A 0.9500 . ? C77B C78B 1.39(3) . ? C77B C86B 1.418(15) . ? C78B C79B 1.41(2) . ? C78B H78B 0.9500 . ? C79B C80B 1.39(2) . ? C79B H79B 0.9500 . ? C80B C81B 1.40(2) . ? C80B H80B 0.9500 . ? C81B C86B 1.43(3) . ? C81B C82B 1.44(3) . ? C82B C83B 1.345(18) . ? C82B H82B 0.9500 . ? C83B C84B 1.419(17) . ? C83B H83B 0.9500 . ? C84B C85B 1.377(18) . ? C84B H84B 0.9500 . ? C85B C86B 1.418(18) . ? C85B H85B 0.9500 . ? C87 C88 1.408(5) . ? C87 C92 1.538(5) . ? C87 H87 1.0000 . ? C88 C89 1.540(5) . ? C88 H88 1.0000 . ? C89 C90 1.533(5) . ? C89 C93 1.541(5) . ? C89 H89 1.0000 . ? C90 C91 1.409(5) . ? C90 H90 1.0000 . ? C91 C92 1.540(5) . ? C91 H91 1.0000 . ? C92 C93 1.539(5) . ? C92 H92 1.0000 . ? C93 H93A 0.9900 . ? C93 H93B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag H1B Rh1 C29 106.6 . . ? H1B Rh1 C28 146.3 . . ? C29 Rh1 C28 39.69(14) . . ? H1B Rh1 N4 83.9 . . ? C29 Rh1 N4 96.35(14) . . ? C28 Rh1 N4 97.68(13) . . ? H1B Rh1 C26 117.8 . . ? C29 Rh1 C26 80.43(16) . . ? C28 Rh1 C26 66.04(15) . . ? N4 Rh1 C26 158.16(13) . . ? H1B Rh1 C25 86.6 . . ? C29 Rh1 C25 67.59(15) . . ? C28 Rh1 C25 79.58(14) . . ? N4 Rh1 C25 158.15(14) . . ? C26 Rh1 C25 37.85(15) . . ? H1B Rh1 N2 80.2 . . ? C29 Rh1 N2 171.68(14) . . ? C28 Rh1 N2 133.37(13) . . ? N4 Rh1 N2 89.07(11) . . ? C26 Rh1 N2 92.20(13) . . ? C25 Rh1 N2 108.70(13) . . ? C1 N1 C2 105.3(3) . . ? C1 N1 B1 127.1(3) . . ? C2 N1 B1 127.4(3) . . ? C1 N2 C7 115.6(3) . . ? C1 N2 Rh1 122.1(2) . . ? C7 N2 Rh1 122.2(2) . . ? C8 N3 C9 106.0(3) . . ? C8 N3 B1 125.8(3) . . ? C9 N3 B1 127.1(3) . . ? C8 N4 C14 115.9(3) . . ? C8 N4 Rh1 120.9(2) . . ? C14 N4 Rh1 122.8(2) . . ? N1 B1 N3 108.2(3) . . ? N1 B1 C15 113.3(3) . . ? N3 B1 C15 113.4(3) . . ? N1 B1 H1B 107.2 . . ? N3 B1 H1B 107.2 . . ? C15 B1 H1B 107.2 . . ? N2 C1 N1 125.3(3) . . ? N2 C1 C4 124.6(3) . . ? N1 C1 C4 110.0(3) . . ? C3 C2 N1 111.7(3) . . ? C3 C2 H2 124.1 . . ? N1 C2 H2 124.1 . . ? C2 C3 C4 106.9(3) . . ? C2 C3 H3 126.5 . . ? C4 C3 H3 126.5 . . ? C5 C4 C3 136.2(3) . . ? C5 C4 C1 117.8(3) . . ? C3 C4 C1 106.0(3) . . ? C6 C5 C4 117.7(3) . . ? C6 C5 H5 121.1 . . ? C4 C5 H5 121.1 . . ? C7 C6 C5 120.4(4) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? N2 C7 C6 123.7(4) . . ? N2 C7 H7 118.1 . . ? C6 C7 H7 118.1 . . ? N4 C8 N3 125.5(3) . . ? N4 C8 C11 124.4(3) . . ? N3 C8 C11 110.0(3) . . ? C10 C9 N3 112.2(3) . . ? C10 C9 H9 123.9 . . ? N3 C9 H9 123.9 . . ? C9 C10 C11 106.1(3) . . ? C9 C10 H10 127.0 . . ? C11 C10 H10 127.0 . . ? C12 C11 C10 136.6(3) . . ? C12 C11 C8 117.7(3) . . ? C10 C11 C8 105.7(3) . . ? C13 C12 C11 117.9(3) . . ? C13 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C12 C13 C14 120.9(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? N4 C14 C13 123.2(3) . . ? N4 C14 H14 118.4 . . ? C13 C14 H14 118.4 . . ? C16 C15 C24 116.1(3) . . ? C16 C15 B1 121.3(3) . . ? C24 C15 B1 122.5(3) . . ? C15 C16 C17 123.5(3) . . ? C15 C16 H16 118.2 . . ? C17 C16 H16 118.2 . . ? C18 C17 C16 120.1(3) . . ? C18 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? C17 C18 C19 120.5(3) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 121.0(3) . . ? C20 C19 C24 120.6(3) . . ? C18 C19 C24 118.4(3) . . ? C21 C20 C19 121.0(4) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C20 C21 C22 119.4(3) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 121.3(4) . . ? C23 C22 H22 119.4 . . ? C21 C22 H22 119.4 . . ? C22 C23 C24 121.4(3) . . ? C22 C23 H23 119.3 . . ? C24 C23 H23 119.3 . . ? C23 C24 C19 116.2(3) . . ? C23 C24 C15 122.7(3) . . ? C19 C24 C15 121.1(3) . . ? C26 C25 C30 106.0(3) . . ? C26 C25 Rh1 70.8(2) . . ? C30 C25 Rh1 95.8(2) . . ? C26 C25 H25 123.5 . . ? C30 C25 H25 123.5 . . ? Rh1 C25 H25 123.5 . . ? C25 C26 C27 106.4(3) . . ? C25 C26 Rh1 71.3(2) . . ? C27 C26 Rh1 97.2(2) . . ? C25 C26 H26 123.0 . . ? C27 C26 H26 123.0 . . ? Rh1 C26 H26 123.0 . . ? C28 C27 C31 102.2(3) . . ? C28 C27 C26 97.7(3) . . ? C31 C27 C26 101.1(3) . . ? C28 C27 H27 117.5 . . ? C31 C27 H27 117.5 . . ? C26 C27 H27 117.5 . . ? C29 C28 C27 107.2(3) . . ? C29 C28 Rh1 69.0(2) . . ? C27 C28 Rh1 99.1(2) . . ? C29 C28 H28 122.7 . . ? C27 C28 H28 122.7 . . ? Rh1 C28 H28 122.7 . . ? C28 C29 C30 104.0(3) . . ? C28 C29 Rh1 71.3(2) . . ? C30 C29 Rh1 97.8(2) . . ? C28 C29 H29 123.5 . . ? C30 C29 H29 123.5 . . ? Rh1 C29 H29 123.5 . . ? C25 C30 C31 101.2(3) . . ? C25 C30 C29 98.8(3) . . ? C31 C30 C29 102.6(3) . . ? C25 C30 H30 117.1 . . ? C31 C30 H30 117.1 . . ? C29 C30 H30 117.1 . . ? C27 C31 C30 94.1(3) . . ? C27 C31 H31A 112.9 . . ? C30 C31 H31A 112.9 . . ? C27 C31 H31B 112.9 . . ? C30 C31 H31B 112.9 . . ? H31A C31 H31B 110.3 . . ? H2B Rh2 C56 109.4 . . ? H2B Rh2 C57 149.5 . . ? C56 Rh2 C57 40.11(14) . . ? H2B Rh2 N8 83.9 . . ? C56 Rh2 N8 94.78(13) . . ? C57 Rh2 N8 96.46(12) . . ? H2B Rh2 C60 87.5 . . ? C56 Rh2 C60 67.41(14) . . ? C57 Rh2 C60 80.09(14) . . ? N8 Rh2 C60 156.31(13) . . ? H2B Rh2 C59 117.4 . . ? C56 Rh2 C59 80.39(14) . . ? C57 Rh2 C59 66.45(14) . . ? N8 Rh2 C59 158.64(13) . . ? C60 Rh2 C59 37.84(14) . . ? H2B Rh2 N6 79.1 . . ? C56 Rh2 N6 170.64(12) . . ? C57 Rh2 N6 131.27(13) . . ? N8 Rh2 N6 89.82(11) . . ? C60 Rh2 N6 110.18(12) . . ? C59 Rh2 N6 92.38(12) . . ? N5 B2 N7 108.1(3) . . ? N5 B2 C46 117.4(3) . . ? N7 B2 C46 112.6(3) . . ? N5 B2 H2B 106.0 . . ? N7 B2 H2B 106.0 . . ? C46 B2 H2B 106.0 . . ? C32 N5 C33 105.1(3) . . ? C32 N5 B2 125.4(3) . . ? C33 N5 B2 128.7(3) . . ? C38 N6 C32 116.0(3) . . ? C38 N6 Rh2 121.7(2) . . ? C32 N6 Rh2 121.8(2) . . ? C39 N7 C40 106.2(3) . . ? C39 N7 B2 126.6(3) . . ? C40 N7 B2 126.5(3) . . ? C45 N8 C39 115.3(3) . . ? C45 N8 Rh2 124.1(2) . . ? C39 N8 Rh2 120.1(2) . . ? N6 C32 N5 125.5(3) . . ? N6 C32 C35 124.1(3) . . ? N5 C32 C35 110.3(3) . . ? C34 C33 N5 112.5(3) . . ? C34 C33 H33 123.7 . . ? N5 C33 H33 123.7 . . ? C33 C34 C35 106.3(3) . . ? C33 C34 H34 126.9 . . ? C35 C34 H34 126.9 . . ? C36 C35 C32 118.1(3) . . ? C36 C35 C34 136.1(4) . . ? C32 C35 C34 105.8(3) . . ? C37 C36 C35 118.1(4) . . ? C37 C36 H36 120.9 . . ? C35 C36 H36 120.9 . . ? C36 C37 C38 119.9(4) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? N6 C38 C37 123.8(3) . . ? N6 C38 H38 118.1 . . ? C37 C38 H38 118.1 . . ? N8 C39 N7 125.3(3) . . ? N8 C39 C42 124.4(3) . . ? N7 C39 C42 110.2(3) . . ? C41 C40 N7 111.6(4) . . ? C41 C40 H40 124.2 . . ? N7 C40 H40 124.2 . . ? C40 C41 C42 106.7(3) . . ? C40 C41 H41 126.7 . . ? C42 C41 H41 126.7 . . ? C43 C42 C41 136.6(4) . . ? C43 C42 C39 118.0(3) . . ? C41 C42 C39 105.3(3) . . ? C42 C43 C44 118.2(3) . . ? C42 C43 H43 120.9 . . ? C44 C43 H43 120.9 . . ? C43 C44 C45 120.1(4) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? N8 C45 C44 123.9(4) . . ? N8 C45 H45 118.0 . . ? C44 C45 H45 118.0 . . ? C47 C46 C55 117.0(4) . . ? C47 C46 B2 124.1(4) . . ? C55 C46 B2 118.7(4) . . ? C46 C47 C48 122.4(4) . . ? C46 C47 H47 118.8 . . ? C48 C47 H47 118.8 . . ? C49 C48 C47 120.8(5) . . ? C49 C48 H48 119.6 . . ? C47 C48 H48 119.6 . . ? C48 C49 C50 120.6(4) . . ? C48 C49 H49 119.7 . . ? C50 C49 H49 119.7 . . ? C49 C50 C51 122.0(4) . . ? C49 C50 C55 119.1(4) . . ? C51 C50 C55 118.9(5) . . ? C52 C51 C50 121.3(5) . . ? C52 C51 H51 119.4 . . ? C50 C51 H51 119.3 . . ? C51 C52 C53 120.3(5) . . ? C51 C52 H52 119.9 . . ? C53 C52 H52 119.9 . . ? C54 C53 C52 120.2(5) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 122.0(4) . . ? C53 C54 H54 119.0 . . ? C55 C54 H54 119.0 . . ? C54 C55 C50 117.3(4) . . ? C54 C55 C46 122.7(4) . . ? C50 C55 C46 120.0(4) . . ? C57 C56 C61 105.5(3) . . ? C57 C56 Rh2 70.5(2) . . ? C61 C56 Rh2 98.4(2) . . ? C57 C56 H56 123.1 . . ? C61 C56 H56 123.1 . . ? Rh2 C56 H56 123.1 . . ? C56 C57 C58 106.3(3) . . ? C56 C57 Rh2 69.4(2) . . ? C58 C57 Rh2 99.3(2) . . ? C56 C57 H57 122.8 . . ? C58 C57 H57 122.8 . . ? Rh2 C57 H57 122.8 . . ? C57 C58 C62 101.3(3) . . ? C57 C58 C59 98.0(3) . . ? C62 C58 C59 101.5(3) . . ? C57 C58 H58 117.6 . . ? C62 C58 H58 117.6 . . ? C59 C58 H58 117.6 . . ? C60 C59 C58 106.3(3) . . ? C60 C59 Rh2 70.9(2) . . ? C58 C59 Rh2 96.2(2) . . ? C60 C59 H59 123.3 . . ? C58 C59 H59 123.3 . . ? Rh2 C59 H59 123.3 . . ? C59 C60 C61 106.5(3) . . ? C59 C60 Rh2 71.3(2) . . ? C61 C60 Rh2 95.1(2) . . ? C59 C60 H60 123.4 . . ? C61 C60 H60 123.4 . . ? Rh2 C60 H60 123.4 . . ? C56 C61 C60 99.0(3) . . ? C56 C61 C62 101.4(3) . . ? C60 C61 C62 100.9(3) . . ? C56 C61 H61 117.4 . . ? C60 C61 H61 117.4 . . ? C62 C61 H61 117.4 . . ? C58 C62 C61 94.8(3) . . ? C58 C62 H62A 112.8 . . ? C61 C62 H62A 112.8 . . ? C58 C62 H62B 112.8 . . ? C61 C62 H62B 112.8 . . ? H62A C62 H62B 110.2 . . ? H3B Rh3 C87 94.1 . . ? H3B Rh3 C88 132.6 . . ? C87 Rh3 C88 39.09(14) . . ? H3B Rh3 C91 88.3 . . ? C87 Rh3 C91 67.94(14) . . ? C88 Rh3 C91 80.47(14) . . ? H3B Rh3 N10 82.0 . . ? C87 Rh3 N10 99.98(12) . . ? C88 Rh3 N10 96.78(12) . . ? C91 Rh3 N10 164.01(13) . . ? H3B Rh3 C90 125.0 . . ? C87 Rh3 C90 80.28(14) . . ? C88 Rh3 C90 66.26(13) . . ? C91 Rh3 C90 38.76(14) . . ? N10 Rh3 C90 152.99(13) . . ? H3B Rh3 N12 81.9 . . ? C87 Rh3 N12 168.77(13) . . ? C88 Rh3 N12 145.43(13) . . ? C91 Rh3 N12 101.33(13) . . ? N10 Rh3 N12 89.89(11) . . ? C90 Rh3 N12 93.39(13) . . ? C63 N9 C64 106.4(3) . . ? C63 N9 B3 125.9(3) . . ? C64 N9 B3 126.9(3) . . ? C69 N10 C63 115.5(3) . . ? C69 N10 Rh3 122.4(2) . . ? C63 N10 Rh3 122.1(2) . . ? C70 N11 C71 105.5(3) . . ? C70 N11 B3 127.2(3) . . ? C71 N11 B3 127.0(4) . . ? C70 N12 C76 115.1(3) . . ? C70 N12 Rh3 122.1(3) . . ? C76 N12 Rh3 122.7(2) . . ? N11 B3 N9 106.5(3) . . ? N11 B3 C77A 105.4(4) . . ? N9 B3 C77A 123.1(4) . . ? N11 B3 C77B 132.3(5) . . ? N9 B3 C77B 98.7(5) . . ? N11 B3 H3B 107.0 . . ? N9 B3 H3B 107.0 . . ? C77A B3 H3B 107.0 . . ? C77B B3 H3B 103.3 . . ? N10 C63 N9 126.2(3) . . ? N10 C63 C66 124.2(3) . . ? N9 C63 C66 109.6(3) . . ? C65 C64 N9 111.5(4) . . ? C65 C64 H64 124.3 . . ? N9 C64 H64 124.3 . . ? C64 C65 C66 106.9(3) . . ? C64 C65 H65 126.6 . . ? C66 C65 H65 126.6 . . ? C67 C66 C65 136.6(4) . . ? C67 C66 C63 117.7(3) . . ? C65 C66 C63 105.6(3) . . ? C68 C67 C66 118.5(3) . . ? C68 C67 H67 120.7 . . ? C66 C67 H67 120.7 . . ? C67 C68 C69 119.8(4) . . ? C67 C68 H68 120.1 . . ? C69 C68 H68 120.1 . . ? N10 C69 C68 124.2(3) . . ? N10 C69 H69 117.9 . . ? C68 C69 H69 117.9 . . ? N12 C70 N11 125.4(3) . . ? N12 C70 C73 124.6(4) . . ? N11 C70 C73 110.0(3) . . ? C72 C71 N11 111.9(4) . . ? C72 C71 H71 124.1 . . ? N11 C71 H71 124.1 . . ? C71 C72 C73 106.8(4) . . ? C71 C72 H72 126.6 . . ? C73 C72 H72 126.6 . . ? C74 C73 C72 136.0(4) . . ? C74 C73 C70 118.2(4) . . ? C72 C73 C70 105.8(4) . . ? C75 C74 C73 117.8(4) . . ? C75 C74 H74 121.1 . . ? C73 C74 H74 121.1 . . ? C74 C75 C76 120.1(4) . . ? C74 C75 H75 120.0 . . ? C76 C75 H75 120.0 . . ? N12 C76 C75 124.1(4) . . ? N12 C76 H76 117.9 . . ? C75 C76 H76 117.9 . . ? C78A C77A C86A 116.1(6) . . ? C78A C77A B3 121.3(5) . . ? C86A C77A B3 122.1(5) . . ? C77A C78A C79A 124.2(6) . . ? C77A C78A H78A 117.9 . . ? C79A C78A H78A 117.9 . . ? C80A C79A C78A 119.2(6) . . ? C80A C79A H79A 120.4 . . ? C78A C79A H79A 120.4 . . ? C79A C80A C81A 120.2(8) . . ? C79A C80A H80A 119.9 . . ? C81A C80A H80A 119.9 . . ? C82A C81A C80A 120.4(10) . . ? C82A C81A C86A 120.5(8) . . ? C80A C81A C86A 119.1(10) . . ? C83A C82A C81A 121.2(8) . . ? C83A C82A H82A 119.4 . . ? C81A C82A H82A 119.4 . . ? C82A C83A C84A 120.2(6) . . ? C82A C83A H83A 119.9 . . ? C84A C83A H83A 119.9 . . ? C85A C84A C83A 120.0(8) . . ? C85A C84A H84A 120.0 . . ? C83A C84A H84A 120.0 . . ? C84A C85A C86A 121.8(11) . . ? C84A C85A H85A 119.1 . . ? C86A C85A H85A 119.1 . . ? C81A C86A C85A 116.3(7) . . ? C81A C86A C77A 120.8(6) . . ? C85A C86A C77A 122.8(7) . . ? C78B C77B C86B 117.1(14) . . ? C78B C77B B3 123.1(13) . . ? C86B C77B B3 119.5(10) . . ? C77B C78B C79B 124(2) . . ? C77B C78B H78B 118.0 . . ? C79B C78B H78B 118.0 . . ? C80B C79B C78B 118.6(16) . . ? C80B C79B H79B 120.7 . . ? C78B C79B H79B 120.7 . . ? C79B C80B C81B 119.5(16) . . ? C79B C80B H80B 120.2 . . ? C81B C80B H80B 120.2 . . ? C80B C81B C86B 121.1(19) . . ? C80B C81B C82B 119(2) . . ? C86B C81B C82B 119.5(17) . . ? C83B C82B C81B 121.3(16) . . ? C83B C82B H82B 119.3 . . ? C81B C82B H82B 119.3 . . ? C82B C83B C84B 121.0(12) . . ? C82B C83B H83B 119.5 . . ? C84B C83B H83B 119.5 . . ? C85B C84B C83B 117.9(13) . . ? C85B C84B H84B 121.0 . . ? C83B C84B H84B 121.0 . . ? C84B C85B C86B 124.5(13) . . ? C84B C85B H85B 117.7 . . ? C86B C85B H85B 117.7 . . ? C85B C86B C77B 125.2(11) . . ? C85B C86B C81B 115.6(13) . . ? C77B C86B C81B 119.1(13) . . ? C88 C87 C92 105.8(3) . . ? C88 C87 Rh3 71.09(19) . . ? C92 C87 Rh3 96.5(2) . . ? C88 C87 H87 123.3 . . ? C92 C87 H87 123.3 . . ? Rh3 C87 H87 123.3 . . ? C87 C88 C89 106.2(3) . . ? C87 C88 Rh3 69.82(19) . . ? C89 C88 Rh3 98.1(2) . . ? C87 C88 H88 123.1 . . ? C89 C88 H88 123.1 . . ? Rh3 C88 H88 123.1 . . ? C90 C89 C88 98.0(3) . . ? C90 C89 C93 101.5(3) . . ? C88 C89 C93 101.5(3) . . ? C90 C89 H89 117.5 . . ? C88 C89 H89 117.5 . . ? C93 C89 H89 117.5 . . ? C91 C90 C89 106.6(3) . . ? C91 C90 Rh3 70.17(19) . . ? C89 C90 Rh3 97.7(2) . . ? C91 C90 H90 123.0 . . ? C89 C90 H90 123.0 . . ? Rh3 C90 H90 123.0 . . ? C90 C91 C92 105.5(3) . . ? C90 C91 Rh3 71.1(2) . . ? C92 C91 Rh3 95.6(2) . . ? C90 C91 H91 123.6 . . ? C92 C91 H91 123.6 . . ? Rh3 C91 H91 123.6 . . ? C87 C92 C93 101.3(3) . . ? C87 C92 C91 99.8(3) . . ? C93 C92 C91 101.4(3) . . ? C87 C92 H92 117.1 . . ? C93 C92 H92 117.1 . . ? C91 C92 H92 117.1 . . ? C92 C93 C89 94.3(3) . . ? C92 C93 H93A 112.9 . . ? C89 C93 H93A 112.9 . . ? C92 C93 H93B 112.9 . . ? C89 C93 H93B 112.9 . . ? H93A C93 H93B 110.3 . . ? 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 H1B Rh1 N2 C1 13.1 . . . . ? C28 Rh1 N2 C1 -170.6(3) . . . . ? N4 Rh1 N2 C1 -70.9(3) . . . . ? C26 Rh1 N2 C1 130.9(3) . . . . ? C25 Rh1 N2 C1 96.1(3) . . . . ? H1B Rh1 N2 C7 -170.9 . . . . ? C28 Rh1 N2 C7 5.4(4) . . . . ? N4 Rh1 N2 C7 105.1(3) . . . . ? C26 Rh1 N2 C7 -53.1(3) . . . . ? C25 Rh1 N2 C7 -87.9(3) . . . . ? H1B Rh1 N4 C8 6.3 . . . . ? C29 Rh1 N4 C8 -99.8(3) . . . . ? C28 Rh1 N4 C8 -139.8(3) . . . . ? C26 Rh1 N4 C8 -179.9(3) . . . . ? C25 Rh1 N4 C8 -58.6(5) . . . . ? N2 Rh1 N4 C8 86.6(3) . . . . ? H1B Rh1 N4 C14 178.8 . . . . ? C29 Rh1 N4 C14 72.8(3) . . . . ? C28 Rh1 N4 C14 32.8(3) . . . . ? C26 Rh1 N4 C14 -7.3(5) . . . . ? C25 Rh1 N4 C14 113.9(4) . . . . ? N2 Rh1 N4 C14 -100.9(3) . . . . ? C1 N1 B1 N3 91.8(4) . . . . ? C2 N1 B1 N3 -82.2(4) . . . . ? C1 N1 B1 C15 -141.5(3) . . . . ? C2 N1 B1 C15 44.4(5) . . . . ? C8 N3 B1 N1 -73.8(4) . . . . ? C9 N3 B1 N1 92.8(4) . . . . ? C8 N3 B1 C15 159.6(3) . . . . ? C9 N3 B1 C15 -33.8(5) . . . . ? C7 N2 C1 N1 -178.7(3) . . . . ? Rh1 N2 C1 N1 -2.4(5) . . . . ? C7 N2 C1 C4 -0.9(5) . . . . ? Rh1 N2 C1 C4 175.3(3) . . . . ? C2 N1 C1 N2 175.8(3) . . . . ? B1 N1 C1 N2 0.7(6) . . . . ? C2 N1 C1 C4 -2.2(4) . . . . ? B1 N1 C1 C4 -177.3(3) . . . . ? C1 N1 C2 C3 2.2(4) . . . . ? B1 N1 C2 C3 177.3(3) . . . . ? N1 C2 C3 C4 -1.3(4) . . . . ? C2 C3 C4 C5 -179.0(4) . . . . ? C2 C3 C4 C1 -0.1(4) . . . . ? N2 C1 C4 C5 2.6(5) . . . . ? N1 C1 C4 C5 -179.4(3) . . . . ? N2 C1 C4 C3 -176.6(3) . . . . ? N1 C1 C4 C3 1.5(4) . . . . ? C3 C4 C5 C6 177.1(4) . . . . ? C1 C4 C5 C6 -1.7(5) . . . . ? C4 C5 C6 C7 -0.6(6) . . . . ? C1 N2 C7 C6 -1.5(5) . . . . ? Rh1 N2 C7 C6 -177.8(3) . . . . ? C5 C6 C7 N2 2.3(6) . . . . ? C14 N4 C8 N3 178.0(3) . . . . ? Rh1 N4 C8 N3 -9.0(5) . . . . ? C14 N4 C8 C11 -3.5(5) . . . . ? C9 N3 C8 N4 178.4(3) . . . . ? B1 N3 C8 N4 -12.7(5) . . . . ? C9 N3 C8 C11 -0.4(4) . . . . ? B1 N3 C8 C11 168.6(3) . . . . ? C8 N3 C9 C10 -0.5(4) . . . . ? B1 N3 C9 C10 -169.3(3) . . . . ? N3 C9 C10 C11 1.2(4) . . . . ? C9 C10 C11 C12 177.9(4) . . . . ? C9 C10 C11 C8 -1.3(4) . . . . ? N4 C8 C11 C12 2.9(5) . . . . ? N3 C8 C11 C12 -178.3(3) . . . . ? N4 C8 C11 C10 -177.7(3) . . . . ? N3 C8 C11 C10 1.1(4) . . . . ? C10 C11 C12 C13 -179.1(4) . . . . ? C8 C11 C12 C13 0.1(5) . . . . ? C11 C12 C13 C14 -2.2(5) . . . . ? C8 N4 C14 C13 1.1(5) . . . . ? Rh1 N4 C14 C13 -171.8(3) . . . . ? C12 C13 C14 N4 1.7(6) . . . . ? N1 B1 C15 C16 13.0(5) . . . . ? N3 B1 C15 C16 136.8(3) . . . . ? N1 B1 C15 C24 -171.0(3) . . . . ? N3 B1 C15 C24 -47.1(4) . . . . ? C24 C15 C16 C17 4.2(5) . . . . ? B1 C15 C16 C17 -179.6(3) . . . . ? C15 C16 C17 C18 -0.6(6) . . . . ? C16 C17 C18 C19 -2.6(6) . . . . ? C17 C18 C19 C20 -177.0(3) . . . . ? C17 C18 C19 C24 1.9(5) . . . . ? C18 C19 C20 C21 177.6(4) . . . . ? C24 C19 C20 C21 -1.3(5) . . . . ? C19 C20 C21 C22 -1.0(6) . . . . ? C20 C21 C22 C23 1.9(6) . . . . ? C21 C22 C23 C24 -0.4(5) . . . . ? C22 C23 C24 C19 -1.9(5) . . . . ? C22 C23 C24 C15 -179.9(3) . . . . ? C20 C19 C24 C23 2.7(5) . . . . ? C18 C19 C24 C23 -176.2(3) . . . . ? C20 C19 C24 C15 -179.2(3) . . . . ? C18 C19 C24 C15 1.9(5) . . . . ? C16 C15 C24 C23 173.2(3) . . . . ? B1 C15 C24 C23 -3.0(5) . . . . ? C16 C15 C24 C19 -4.7(5) . . . . ? B1 C15 C24 C19 179.1(3) . . . . ? H1B Rh1 C25 C26 146.8 . . . . ? C29 Rh1 C25 C26 -103.7(3) . . . . ? C28 Rh1 C25 C26 -64.1(2) . . . . ? N4 Rh1 C25 C26 -148.8(3) . . . . ? N2 Rh1 C25 C26 68.3(2) . . . . ? H1B Rh1 C25 C30 -108.3 . . . . ? C29 Rh1 C25 C30 1.2(2) . . . . ? C28 Rh1 C25 C30 40.8(2) . . . . ? N4 Rh1 C25 C30 -43.8(4) . . . . ? C26 Rh1 C25 C30 105.0(3) . . . . ? N2 Rh1 C25 C30 173.3(2) . . . . ? C30 C25 C26 C27 1.5(4) . . . . ? Rh1 C25 C26 C27 92.1(3) . . . . ? C30 C25 C26 Rh1 -90.7(3) . . . . ? H1B Rh1 C26 C25 -38.2 . . . . ? C29 Rh1 C26 C25 65.6(2) . . . . ? C28 Rh1 C26 C25 104.4(3) . . . . ? N4 Rh1 C26 C25 148.8(3) . . . . ? N2 Rh1 C26 C25 -118.3(2) . . . . ? H1B Rh1 C26 C27 -143.1 . . . . ? C29 Rh1 C26 C27 -39.4(2) . . . . ? C28 Rh1 C26 C27 -0.5(2) . . . . ? N4 Rh1 C26 C27 43.8(5) . . . . ? C25 Rh1 C26 C27 -105.0(3) . . . . ? N2 Rh1 C26 C27 136.8(2) . . . . ? C25 C26 C27 C28 -71.9(4) . . . . ? Rh1 C26 C27 C28 0.7(3) . . . . ? C25 C26 C27 C31 32.2(4) . . . . ? Rh1 C26 C27 C31 104.8(3) . . . . ? C31 C27 C28 C29 -33.1(4) . . . . ? C26 C27 C28 C29 70.0(4) . . . . ? C31 C27 C28 Rh1 -103.8(3) . . . . ? C26 C27 C28 Rh1 -0.7(3) . . . . ? H1B Rh1 C28 C29 0.1 . . . . ? N4 Rh1 C28 C29 90.7(2) . . . . ? C26 Rh1 C28 C29 -104.5(3) . . . . ? C25 Rh1 C28 C29 -67.3(2) . . . . ? N2 Rh1 C28 C29 -173.3(2) . . . . ? H1B Rh1 C28 C27 105.2 . . . . ? C29 Rh1 C28 C27 105.1(3) . . . . ? N4 Rh1 C28 C27 -164.2(2) . . . . ? C26 Rh1 C28 C27 0.5(2) . . . . ? C25 Rh1 C28 C27 37.7(2) . . . . ? N2 Rh1 C28 C27 -68.2(3) . . . . ? C27 C28 C29 C30 0.3(4) . . . . ? Rh1 C28 C29 C30 93.6(2) . . . . ? C27 C28 C29 Rh1 -93.3(3) . . . . ? H1B Rh1 C29 C28 -179.9 . . . . ? N4 Rh1 C29 C28 -94.4(2) . . . . ? C26 Rh1 C29 C28 63.8(2) . . . . ? C25 Rh1 C29 C28 101.0(3) . . . . ? H1B Rh1 C29 C30 77.9 . . . . ? C28 Rh1 C29 C30 -102.2(3) . . . . ? N4 Rh1 C29 C30 163.4(2) . . . . ? C26 Rh1 C29 C30 -38.4(2) . . . . ? C25 Rh1 C29 C30 -1.2(2) . . . . ? C26 C25 C30 C31 -34.7(4) . . . . ? Rh1 C25 C30 C31 -106.4(3) . . . . ? C26 C25 C30 C29 70.2(3) . . . . ? Rh1 C25 C30 C29 -1.5(3) . . . . ? C28 C29 C30 C25 -71.0(3) . . . . ? Rh1 C29 C30 C25 1.6(3) . . . . ? C28 C29 C30 C31 32.7(4) . . . . ? Rh1 C29 C30 C31 105.3(3) . . . . ? C28 C27 C31 C30 50.1(3) . . . . ? C26 C27 C31 C30 -50.4(3) . . . . ? C25 C30 C31 C27 51.6(3) . . . . ? C29 C30 C31 C27 -50.2(3) . . . . ? N7 B2 N5 C32 90.2(4) . . . . ? C46 B2 N5 C32 -141.2(3) . . . . ? N7 B2 N5 C33 -78.2(4) . . . . ? C46 B2 N5 C33 50.5(5) . . . . ? H2B Rh2 N6 C38 -175.4 . . . . ? C57 Rh2 N6 C38 2.3(3) . . . . ? N8 Rh2 N6 C38 100.8(3) . . . . ? C60 Rh2 N6 C38 -92.2(3) . . . . ? C59 Rh2 N6 C38 -58.0(3) . . . . ? H2B Rh2 N6 C32 13.0 . . . . ? C57 Rh2 N6 C32 -169.3(2) . . . . ? N8 Rh2 N6 C32 -70.9(3) . . . . ? C60 Rh2 N6 C32 96.2(3) . . . . ? C59 Rh2 N6 C32 130.4(3) . . . . ? C46 B2 N7 C39 150.0(3) . . . . ? N5 B2 N7 C40 90.2(4) . . . . ? C46 B2 N7 C40 -41.1(5) . . . . ? H2B Rh2 N8 C45 179.1 . . . . ? C56 Rh2 N8 C45 70.0(3) . . . . ? C57 Rh2 N8 C45 29.7(3) . . . . ? C60 Rh2 N8 C45 109.8(4) . . . . ? C59 Rh2 N8 C45 -5.8(5) . . . . ? N6 Rh2 N8 C45 -101.9(3) . . . . ? H2B Rh2 N8 C39 7.2 . . . . ? C56 Rh2 N8 C39 -101.9(3) . . . . ? C57 Rh2 N8 C39 -142.2(3) . . . . ? C60 Rh2 N8 C39 -62.1(4) . . . . ? C59 Rh2 N8 C39 -177.6(3) . . . . ? N6 Rh2 N8 C39 86.3(3) . . . . ? C38 N6 C32 N5 -177.1(3) . . . . ? Rh2 N6 C32 N5 -5.0(5) . . . . ? C38 N6 C32 C35 -1.3(5) . . . . ? Rh2 N6 C32 C35 170.8(2) . . . . ? C33 N5 C32 N6 175.1(3) . . . . ? B2 N5 C32 N6 4.5(5) . . . . ? C33 N5 C32 C35 -1.3(4) . . . . ? B2 N5 C32 C35 -171.9(3) . . . . ? C32 N5 C33 C34 2.4(4) . . . . ? B2 N5 C33 C34 172.6(3) . . . . ? N5 C33 C34 C35 -2.6(4) . . . . ? N6 C32 C35 C36 0.7(5) . . . . ? N5 C32 C35 C36 177.1(3) . . . . ? N6 C32 C35 C34 -176.6(3) . . . . ? N5 C32 C35 C34 -0.2(4) . . . . ? C33 C34 C35 C36 -174.9(4) . . . . ? C33 C34 C35 C32 1.7(4) . . . . ? C32 C35 C36 C37 -0.1(5) . . . . ? C34 C35 C36 C37 176.2(4) . . . . ? C35 C36 C37 C38 0.0(5) . . . . ? C32 N6 C38 C37 1.2(5) . . . . ? Rh2 N6 C38 C37 -170.9(3) . . . . ? C36 C37 C38 N6 -0.7(6) . . . . ? C45 N8 C39 N7 176.5(3) . . . . ? Rh2 N8 C39 N7 -10.9(5) . . . . ? C45 N8 C39 C42 -2.6(5) . . . . ? Rh2 N8 C39 C42 170.0(3) . . . . ? C40 N7 C39 N8 -179.2(3) . . . . ? B2 N7 C39 N8 -8.5(6) . . . . ? C40 N7 C39 C42 0.0(4) . . . . ? B2 N7 C39 C42 170.7(3) . . . . ? C39 N7 C40 C41 0.2(4) . . . . ? B2 N7 C40 C41 -170.5(3) . . . . ? N7 C40 C41 C42 -0.3(5) . . . . ? C40 C41 C42 C43 177.3(4) . . . . ? C40 C41 C42 C39 0.3(4) . . . . ? N8 C39 C42 C43 1.3(5) . . . . ? N7 C39 C42 C43 -177.8(3) . . . . ? N8 C39 C42 C41 179.0(3) . . . . ? N7 C39 C42 C41 -0.2(4) . . . . ? C41 C42 C43 C44 -176.5(4) . . . . ? C39 C42 C43 C44 0.3(5) . . . . ? C42 C43 C44 C45 -0.5(5) . . . . ? C39 N8 C45 C44 2.3(5) . . . . ? Rh2 N8 C45 C44 -169.9(3) . . . . ? C43 C44 C45 N8 -0.8(6) . . . . ? N5 B2 C46 C47 -3.2(5) . . . . ? N7 B2 C46 C47 123.3(4) . . . . ? N5 B2 C46 C55 171.9(3) . . . . ? N7 B2 C46 C55 -61.6(4) . . . . ? C55 C46 C47 C48 0.1(6) . . . . ? B2 C46 C47 C48 175.3(4) . . . . ? C46 C47 C48 C49 -0.1(6) . . . . ? C47 C48 C49 C50 0.4(7) . . . . ? C48 C49 C50 C51 178.9(4) . . . . ? C48 C49 C50 C55 -0.7(7) . . . . ? C49 C50 C51 C52 178.6(5) . . . . ? C55 C50 C51 C52 -1.8(7) . . . . ? C50 C51 C52 C53 0.4(7) . . . . ? C51 C52 C53 C54 0.5(7) . . . . ? C52 C53 C54 C55 0.0(7) . . . . ? C53 C54 C55 C50 -1.4(6) . . . . ? C53 C54 C55 C46 179.8(4) . . . . ? C49 C50 C55 C54 -178.2(4) . . . . ? C51 C50 C55 C54 2.2(6) . . . . ? C49 C50 C55 C46 0.6(6) . . . . ? C51 C50 C55 C46 -178.9(4) . . . . ? C47 C46 C55 C54 178.4(4) . . . . ? B2 C46 C55 C54 2.9(6) . . . . ? C47 C46 C55 C50 -0.3(5) . . . . ? B2 C46 C55 C50 -175.9(3) . . . . ? H2B Rh2 C56 C57 -179.6 . . . . ? N8 Rh2 C56 C57 -94.4(2) . . . . ? C60 Rh2 C56 C57 101.8(2) . . . . ? C59 Rh2 C56 C57 64.7(2) . . . . ? H2B Rh2 C56 C61 76.9 . . . . ? C57 Rh2 C56 C61 -103.6(3) . . . . ? N8 Rh2 C56 C61 162.1(2) . . . . ? C60 Rh2 C56 C61 -1.8(2) . . . . ? C59 Rh2 C56 C61 -38.9(2) . . . . ? C61 C56 C57 C58 -0.4(4) . . . . ? Rh2 C56 C57 C58 -94.0(2) . . . . ? C61 C56 C57 Rh2 93.6(2) . . . . ? H2B Rh2 C57 C56 0.8 . . . . ? N8 Rh2 C57 C56 89.8(2) . . . . ? C60 Rh2 C57 C56 -66.6(2) . . . . ? C59 Rh2 C57 C56 -103.6(2) . . . . ? N6 Rh2 C57 C56 -174.78(18) . . . . ? H2B Rh2 C57 C58 104.8 . . . . ? C56 Rh2 C57 C58 104.0(3) . . . . ? N8 Rh2 C57 C58 -166.3(2) . . . . ? C60 Rh2 C57 C58 37.4(2) . . . . ? C59 Rh2 C57 C58 0.4(2) . . . . ? N6 Rh2 C57 C58 -70.8(3) . . . . ? C56 C57 C58 C62 -32.8(3) . . . . ? Rh2 C57 C58 C62 -104.0(2) . . . . ? C56 C57 C58 C59 70.6(3) . . . . ? Rh2 C57 C58 C59 -0.5(3) . . . . ? C57 C58 C59 C60 -71.4(3) . . . . ? C62 C58 C59 C60 31.9(3) . . . . ? C57 C58 C59 Rh2 0.5(3) . . . . ? C62 C58 C59 Rh2 103.8(2) . . . . ? H2B Rh2 C59 C60 -41.7 . . . . ? C56 Rh2 C59 C60 65.4(2) . . . . ? C57 Rh2 C59 C60 104.8(2) . . . . ? N8 Rh2 C59 C60 143.8(3) . . . . ? N6 Rh2 C59 C60 -120.6(2) . . . . ? H2B Rh2 C59 C58 -146.8 . . . . ? C56 Rh2 C59 C58 -39.8(2) . . . . ? C57 Rh2 C59 C58 -0.4(2) . . . . ? N8 Rh2 C59 C58 38.6(5) . . . . ? C60 Rh2 C59 C58 -105.2(3) . . . . ? N6 Rh2 C59 C58 134.2(2) . . . . ? C58 C59 C60 C61 1.2(4) . . . . ? Rh2 C59 C60 C61 -89.8(2) . . . . ? C58 C59 C60 Rh2 91.0(2) . . . . ? H2B Rh2 C60 C59 143.8 . . . . ? C56 Rh2 C60 C59 -103.9(2) . . . . ? C57 Rh2 C60 C59 -64.1(2) . . . . ? N8 Rh2 C60 C59 -147.6(3) . . . . ? N6 Rh2 C60 C59 66.4(2) . . . . ? H2B Rh2 C60 C61 -110.5 . . . . ? C56 Rh2 C60 C61 1.7(2) . . . . ? C57 Rh2 C60 C61 41.5(2) . . . . ? N8 Rh2 C60 C61 -41.9(4) . . . . ? C59 Rh2 C60 C61 105.7(3) . . . . ? N6 Rh2 C60 C61 172.03(19) . . . . ? C57 C56 C61 C60 -69.7(3) . . . . ? Rh2 C56 C61 C60 2.3(3) . . . . ? C57 C56 C61 C62 33.5(4) . . . . ? Rh2 C56 C61 C62 105.5(2) . . . . ? C59 C60 C61 C56 69.8(3) . . . . ? Rh2 C60 C61 C56 -2.2(3) . . . . ? C59 C60 C61 C62 -33.7(3) . . . . ? Rh2 C60 C61 C62 -105.7(2) . . . . ? C57 C58 C62 C61 50.8(3) . . . . ? C59 C58 C62 C61 -49.9(3) . . . . ? C56 C61 C62 C58 -51.2(3) . . . . ? C60 C61 C62 C58 50.5(3) . . . . ? H3B Rh3 N10 C69 -174.8 . . . . ? C87 Rh3 N10 C69 -82.0(3) . . . . ? C88 Rh3 N10 C69 -42.6(3) . . . . ? C91 Rh3 N10 C69 -121.7(5) . . . . ? C90 Rh3 N10 C69 6.1(4) . . . . ? N12 Rh3 N10 C69 103.4(3) . . . . ? H3B Rh3 N10 C63 3.5 . . . . ? C87 Rh3 N10 C63 96.3(3) . . . . ? C88 Rh3 N10 C63 135.7(3) . . . . ? C91 Rh3 N10 C63 56.6(6) . . . . ? C90 Rh3 N10 C63 -175.6(3) . . . . ? N12 Rh3 N10 C63 -78.3(3) . . . . ? H3B Rh3 N12 C70 -4.1 . . . . ? C87 Rh3 N12 C70 -73.8(8) . . . . ? C88 Rh3 N12 C70 179.7(3) . . . . ? C91 Rh3 N12 C70 -90.7(3) . . . . ? N10 Rh3 N12 C70 77.8(3) . . . . ? C90 Rh3 N12 C70 -129.0(3) . . . . ? H3B Rh3 N12 C76 172.3 . . . . ? C87 Rh3 N12 C76 102.6(7) . . . . ? C88 Rh3 N12 C76 -3.9(4) . . . . ? C91 Rh3 N12 C76 85.7(3) . . . . ? N10 Rh3 N12 C76 -105.8(3) . . . . ? C90 Rh3 N12 C76 47.4(3) . . . . ? C70 N11 B3 N9 -86.7(4) . . . . ? C71 N11 B3 N9 85.7(4) . . . . ? C70 N11 B3 C77A 141.0(4) . . . . ? C71 N11 B3 C77A -46.5(5) . . . . ? C70 N11 B3 C77B 154.4(6) . . . . ? C71 N11 B3 C77B -33.1(8) . . . . ? C63 N9 B3 N11 83.6(4) . . . . ? C64 N9 B3 N11 -85.0(4) . . . . ? C63 N9 B3 C77A -154.9(4) . . . . ? C64 N9 B3 C77A 36.6(6) . . . . ? C63 N9 B3 C77B -137.4(5) . . . . ? C64 N9 B3 C77B 54.1(5) . . . . ? C69 N10 C63 N9 -178.5(3) . . . . ? Rh3 N10 C63 N9 3.1(5) . . . . ? C69 N10 C63 C66 0.1(5) . . . . ? Rh3 N10 C63 C66 -178.3(3) . . . . ? C64 N9 C63 N10 176.7(3) . . . . ? B3 N9 C63 N10 6.2(5) . . . . ? C64 N9 C63 C66 -2.1(4) . . . . ? B3 N9 C63 C66 -172.5(3) . . . . ? C63 N9 C64 C65 1.8(4) . . . . ? B3 N9 C64 C65 172.1(3) . . . . ? N9 C64 C65 C66 -0.8(4) . . . . ? C64 C65 C66 C67 -179.1(4) . . . . ? C64 C65 C66 C63 -0.5(4) . . . . ? N10 C63 C66 C67 1.8(5) . . . . ? N9 C63 C66 C67 -179.4(3) . . . . ? N10 C63 C66 C65 -177.2(3) . . . . ? N9 C63 C66 C65 1.6(4) . . . . ? C65 C66 C67 C68 176.4(4) . . . . ? C63 C66 C67 C68 -2.1(5) . . . . ? C66 C67 C68 C69 0.8(5) . . . . ? C63 N10 C69 C68 -1.6(5) . . . . ? Rh3 N10 C69 C68 176.8(3) . . . . ? C67 C68 C69 N10 1.2(5) . . . . ? C76 N12 C70 N11 179.0(3) . . . . ? Rh3 N12 C70 N11 -4.4(5) . . . . ? C76 N12 C70 C73 0.7(5) . . . . ? Rh3 N12 C70 C73 177.4(3) . . . . ? C71 N11 C70 N12 -176.5(3) . . . . ? B3 N11 C70 N12 -2.7(6) . . . . ? C71 N11 C70 C73 2.0(4) . . . . ? B3 N11 C70 C73 175.8(3) . . . . ? C70 N11 C71 C72 -1.9(5) . . . . ? B3 N11 C71 C72 -175.7(4) . . . . ? N11 C71 C72 C73 1.0(5) . . . . ? C71 C72 C73 C74 179.2(5) . . . . ? C71 C72 C73 C70 0.3(5) . . . . ? N12 C70 C73 C74 -2.1(6) . . . . ? N11 C70 C73 C74 179.4(3) . . . . ? N12 C70 C73 C72 177.0(4) . . . . ? N11 C70 C73 C72 -1.5(4) . . . . ? C72 C73 C74 C75 -177.4(5) . . . . ? C70 C73 C74 C75 1.4(6) . . . . ? C73 C74 C75 C76 0.4(6) . . . . ? C70 N12 C76 C75 1.4(5) . . . . ? Rh3 N12 C76 C75 -175.2(3) . . . . ? C74 C75 C76 N12 -2.0(6) . . . . ? N11 B3 C77A C78A -25.5(6) . . . . ? N9 B3 C77A C78A -147.5(5) . . . . ? C77B B3 C77A C78A 175.1(11) . . . . ? N11 B3 C77A C86A 163.4(4) . . . . ? N9 B3 C77A C86A 41.3(6) . . . . ? C77B B3 C77A C86A 3.9(7) . . . . ? C86A C77A C78A C79A -4.6(9) . . . . ? B3 C77A C78A C79A -176.3(5) . . . . ? C77A C78A C79A C80A 0.1(10) . . . . ? C78A C79A C80A C81A 4.7(15) . . . . ? C79A C80A C81A C82A 175.1(13) . . . . ? C79A C80A C81A C86A -5(2) . . . . ? C80A C81A C82A C83A -178.2(13) . . . . ? C86A C81A C82A C83A 2(2) . . . . ? C81A C82A C83A C84A -0.7(15) . . . . ? C82A C83A C84A C85A -0.2(11) . . . . ? C83A C84A C85A C86A 0.3(17) . . . . ? C82A C81A C86A C85A -1(2) . . . . ? C80A C81A C86A C85A 178.3(15) . . . . ? C82A C81A C86A C77A -179.7(12) . . . . ? C80A C81A C86A C77A 0(2) . . . . ? C84A C85A C86A C81A 0.5(19) . . . . ? C84A C85A C86A C77A 178.8(9) . . . . ? C78A C77A C86A C81A 4.5(14) . . . . ? B3 C77A C86A C81A 176.1(12) . . . . ? C78A C77A C86A C85A -173.8(9) . . . . ? B3 C77A C86A C85A -2.1(11) . . . . ? N11 B3 C77B C78B 147.9(17) . . . . ? N9 B3 C77B C78B 26.0(18) . . . . ? C77A B3 C77B C78B 175(2) . . . . ? N11 B3 C77B C86B -38.8(11) . . . . ? N9 B3 C77B C86B -160.7(8) . . . . ? C77A B3 C77B C86B -11.7(6) . . . . ? C86B C77B C78B C79B 5(3) . . . . ? B3 C77B C78B C79B 178.9(18) . . . . ? C77B C78B C79B C80B -1(4) . . . . ? C78B C79B C80B C81B -1(3) . . . . ? C79B C80B C81B C86B -2(5) . . . . ? C79B C80B C81B C82B -178(2) . . . . ? C80B C81B C82B C83B 176(2) . . . . ? C86B C81B C82B C83B -1(5) . . . . ? C81B C82B C83B C84B -2(3) . . . . ? C82B C83B C84B C85B 2.0(18) . . . . ? C83B C84B C85B C86B 0(2) . . . . ? C84B C85B C86B C77B 177.2(12) . . . . ? C84B C85B C86B C81B -3(3) . . . . ? C78B C77B C86B C85B 172.1(18) . . . . ? B3 C77B C86B C85B -1.6(15) . . . . ? C78B C77B C86B C81B -8(3) . . . . ? B3 C77B C86B C81B 178(2) . . . . ? C80B C81B C86B C85B -174(3) . . . . ? C82B C81B C86B C85B 3(4) . . . . ? C80B C81B C86B C77B 6(5) . . . . ? C82B C81B C86B C77B -177(2) . . . . ? H3B Rh3 C87 C88 171.0 . . . . ? C91 Rh3 C87 C88 -102.4(2) . . . . ? N10 Rh3 C87 C88 88.5(2) . . . . ? C90 Rh3 C87 C88 -64.1(2) . . . . ? N12 Rh3 C87 C88 -120.4(6) . . . . ? H3B Rh3 C87 C92 -84.4 . . . . ? C88 Rh3 C87 C92 104.6(3) . . . . ? C91 Rh3 C87 C92 2.1(2) . . . . ? N10 Rh3 C87 C92 -167.0(2) . . . . ? C90 Rh3 C87 C92 40.5(2) . . . . ? N12 Rh3 C87 C92 -15.8(8) . . . . ? C92 C87 C88 C89 1.3(3) . . . . ? Rh3 C87 C88 C89 92.8(2) . . . . ? C92 C87 C88 Rh3 -91.6(2) . . . . ? H3B Rh3 C88 C87 -12.2 . . . . ? C91 Rh3 C88 C87 66.6(2) . . . . ? N10 Rh3 C88 C87 -97.5(2) . . . . ? C90 Rh3 C88 C87 104.4(2) . . . . ? N12 Rh3 C88 C87 162.8(2) . . . . ? H3B Rh3 C88 C89 -116.5 . . . . ? C87 Rh3 C88 C89 -104.3(3) . . . . ? C91 Rh3 C88 C89 -37.8(2) . . . . ? N10 Rh3 C88 C89 158.2(2) . . . . ? C90 Rh3 C88 C89 0.1(2) . . . . ? N12 Rh3 C88 C89 58.4(3) . . . . ? C87 C88 C89 C90 -71.3(3) . . . . ? Rh3 C88 C89 C90 -0.1(3) . . . . ? C87 C88 C89 C93 32.2(3) . . . . ? Rh3 C88 C89 C93 103.5(2) . . . . ? C88 C89 C90 C91 71.6(3) . . . . ? C93 C89 C90 C91 -31.9(3) . . . . ? C88 C89 C90 Rh3 0.1(3) . . . . ? C93 C89 C90 Rh3 -103.4(2) . . . . ? H3B Rh3 C90 C91 21.5 . . . . ? C87 Rh3 C90 C91 -66.7(2) . . . . ? C88 Rh3 C90 C91 -105.0(2) . . . . ? N10 Rh3 C90 C91 -159.6(2) . . . . ? N12 Rh3 C90 C91 103.9(2) . . . . ? H3B Rh3 C90 C89 126.4 . . . . ? C87 Rh3 C90 C89 38.2(2) . . . . ? C88 Rh3 C90 C89 -0.1(2) . . . . ? C91 Rh3 C90 C89 104.9(3) . . . . ? N10 Rh3 C90 C89 -54.7(4) . . . . ? N12 Rh3 C90 C89 -151.1(2) . . . . ? C89 C90 C91 C92 -1.6(4) . . . . ? Rh3 C90 C91 C92 90.7(2) . . . . ? C89 C90 C91 Rh3 -92.3(2) . . . . ? H3B Rh3 C91 C90 -162.6 . . . . ? C87 Rh3 C91 C90 102.3(2) . . . . ? C88 Rh3 C91 C90 63.7(2) . . . . ? N10 Rh3 C91 C90 145.0(4) . . . . ? N12 Rh3 C91 C90 -81.2(2) . . . . ? H3B Rh3 C91 C92 93.0 . . . . ? C87 Rh3 C91 C92 -2.1(2) . . . . ? C88 Rh3 C91 C92 -40.7(2) . . . . ? N10 Rh3 C91 C92 40.6(6) . . . . ? C90 Rh3 C91 C92 -104.4(3) . . . . ? N12 Rh3 C91 C92 174.4(2) . . . . ? C88 C87 C92 C93 -34.4(3) . . . . ? Rh3 C87 C92 C93 -106.5(2) . . . . ? C88 C87 C92 C91 69.4(3) . . . . ? Rh3 C87 C92 C91 -2.7(3) . . . . ? C90 C91 C92 C87 -69.2(3) . . . . ? Rh3 C91 C92 C87 2.7(3) . . . . ? C90 C91 C92 C93 34.6(3) . . . . ? Rh3 C91 C92 C93 106.5(2) . . . . ? C87 C92 C93 C89 51.3(3) . . . . ? C91 C92 C93 C89 -51.3(3) . . . . ? C90 C89 C93 C92 50.2(3) . . . . ? C88 C89 C93 C92 -50.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.630 _refine_diff_density_min -1.041 _refine_diff_density_rms 0.099