# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Gerhard Erker' _publ_contact_author_email ERKER@UNI-MUENSTER.DE _publ_section_title ; Functionalized phosphorus analogues of the beta-diketiminato ligand systems: Bis(N-arylphosphinimino)acetonitrile-derived complexes of rhodium and iridium ; loop_ _publ_author_name 'G Erker' 'Roland Frohlich' 'Gerald Kehr' 'Seda Kehr' 'Kirsten Spannhoff' # Attachment '11.cif' data_erk4173 _database_code_depnum_ccdc_archive 'CCDC 676924' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H30 N3 O2 P2 Rh' _chemical_formula_weight 749.52 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 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 9.8125(2) _cell_length_b 20.4272(5) _cell_length_c 17.5318(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.278(2) _cell_angle_gamma 90.00 _cell_volume 3433.73(12) _cell_formula_units_Z 4 _cell_measurement_temperature 198(2) _cell_measurement_reflns_used 19338 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1528 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8843 _exptl_absorpt_correction_T_max 0.9692 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 198(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22757 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 27.86 _reflns_number_total 8114 _reflns_number_gt 5740 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+2.4045P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8114 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1003 _refine_ls_wR_factor_gt 0.0891 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _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 0.07548(2) 0.689543(11) 0.200315(13) 0.02353(8) Uani 1 1 d . . . C1 C 0.3727(3) 0.69200(14) 0.17673(16) 0.0226(6) Uani 1 1 d . . . C2 C 0.4466(4) 0.69136(16) 0.1163(2) 0.0410(9) Uani 1 1 d . . . N3 N 0.5056(5) 0.69257(18) 0.0668(2) 0.0847(14) Uani 1 1 d . . . C3 C -0.0499(4) 0.62885(17) 0.1482(2) 0.0432(9) Uani 1 1 d . . . O3 O -0.1248(3) 0.59150(15) 0.11513(19) 0.0796(11) Uani 1 1 d . . . C4 C -0.0485(3) 0.75466(16) 0.15848(18) 0.0315(7) Uani 1 1 d . . . O4 O -0.1273(3) 0.79305(12) 0.13120(15) 0.0515(7) Uani 1 1 d . . . N1 N 0.2232(2) 0.75680(11) 0.26288(13) 0.0213(5) Uani 1 1 d . . . C11 C 0.1792(3) 0.80659(14) 0.31006(16) 0.0221(6) Uani 1 1 d . . . C12 C 0.1826(4) 0.79389(17) 0.38860(18) 0.0358(8) Uani 1 1 d . . . H12 H 0.2139 0.7526 0.4103 0.043 Uiso 1 1 calc R . . C13 C 0.1402(4) 0.8415(2) 0.43506(19) 0.0431(9) Uani 1 1 d . . . H13 H 0.1455 0.8329 0.4889 0.052 Uiso 1 1 calc R . . C14 C 0.0907(3) 0.90088(18) 0.4043(2) 0.0385(8) Uani 1 1 d . . . H14 H 0.0601 0.9328 0.4363 0.046 Uiso 1 1 calc R . . C15 C 0.0860(3) 0.91352(16) 0.3272(2) 0.0344(8) Uani 1 1 d . . . H15 H 0.0516 0.9545 0.3056 0.041 Uiso 1 1 calc R . . C16 C 0.1305(3) 0.86742(15) 0.28025(18) 0.0278(7) Uani 1 1 d . . . H16 H 0.1279 0.8773 0.2270 0.033 Uiso 1 1 calc R . . N2 N 0.2136(2) 0.61353(11) 0.24892(13) 0.0228(5) Uani 1 1 d . . . C21 C 0.1707(3) 0.56060(14) 0.28993(16) 0.0223(6) Uani 1 1 d . . . C22 C 0.0489(3) 0.56693(15) 0.31859(17) 0.0285(7) Uani 1 1 d . . . H22 H -0.0025 0.6066 0.3100 0.034 Uiso 1 1 calc R . . C23 C 0.0014(3) 0.51690(16) 0.35902(18) 0.0335(7) Uani 1 1 d . . . H23 H -0.0823 0.5225 0.3773 0.040 Uiso 1 1 calc R . . C24 C 0.0743(3) 0.45865(16) 0.37316(18) 0.0328(7) Uani 1 1 d . . . H24 H 0.0419 0.4243 0.4012 0.039 Uiso 1 1 calc R . . C25 C 0.1950(3) 0.45160(15) 0.34573(17) 0.0306(7) Uani 1 1 d . . . H25 H 0.2463 0.4119 0.3554 0.037 Uiso 1 1 calc R . . C26 C 0.2431(3) 0.50099(14) 0.30453(17) 0.0276(7) Uani 1 1 d . . . H26 H 0.3262 0.4946 0.2858 0.033 Uiso 1 1 calc R . . P1 P 0.35294(8) 0.76738(4) 0.22074(4) 0.02155(17) Uani 1 1 d . . . C31 C 0.5120(3) 0.79067(14) 0.28802(17) 0.0261(7) Uani 1 1 d . . . C32 C 0.6292(4) 0.80582(18) 0.2581(2) 0.0401(8) Uani 1 1 d . . . H32 H 0.6219 0.8083 0.2032 0.048 Uiso 1 1 calc R . . C33 C 0.7559(4) 0.8171(2) 0.3083(2) 0.0510(10) Uani 1 1 d . . . H33 H 0.8355 0.8275 0.2879 0.061 Uiso 1 1 calc R . . C34 C 0.7674(4) 0.81344(19) 0.3879(2) 0.0485(10) Uani 1 1 d . . . H34 H 0.8547 0.8218 0.4221 0.058 Uiso 1 1 calc R . . C35 C 0.6535(4) 0.79777(17) 0.41803(19) 0.0382(8) Uani 1 1 d . . . H35 H 0.6626 0.7947 0.4729 0.046 Uiso 1 1 calc R . . C36 C 0.5248(3) 0.78638(16) 0.36857(18) 0.0302(7) Uani 1 1 d . . . H36 H 0.4460 0.7757 0.3896 0.036 Uiso 1 1 calc R . . C41 C 0.3251(3) 0.82999(15) 0.14511(17) 0.0272(7) Uani 1 1 d . . . C42 C 0.2341(4) 0.81693(16) 0.07387(18) 0.0353(8) Uani 1 1 d . . . H42 H 0.1962 0.7743 0.0631 0.042 Uiso 1 1 calc R . . C43 C 0.1993(4) 0.86643(19) 0.01895(19) 0.0443(9) Uani 1 1 d . . . H43 H 0.1372 0.8576 -0.0294 0.053 Uiso 1 1 calc R . . C44 C 0.2543(4) 0.92826(17) 0.0341(2) 0.0426(9) Uani 1 1 d . . . H44 H 0.2308 0.9618 -0.0040 0.051 Uiso 1 1 calc R . . C45 C 0.3424(4) 0.94146(17) 0.1038(2) 0.0426(9) Uani 1 1 d . . . H45 H 0.3792 0.9843 0.1141 0.051 Uiso 1 1 calc R . . C46 C 0.3789(4) 0.89279(16) 0.15958(19) 0.0354(8) Uani 1 1 d . . . H46 H 0.4407 0.9024 0.2078 0.042 Uiso 1 1 calc R . . P2 P 0.36700(8) 0.61972(4) 0.22913(4) 0.02084(16) Uani 1 1 d . . . C51 C 0.4031(3) 0.55427(14) 0.16718(16) 0.0263(7) Uani 1 1 d . . . C52 C 0.2981(4) 0.53876(18) 0.1037(2) 0.0449(9) Uani 1 1 d . . . H52 H 0.2126 0.5623 0.0949 0.054 Uiso 1 1 calc R . . C53 C 0.3166(4) 0.4891(2) 0.0529(2) 0.0546(11) Uani 1 1 d . . . H53 H 0.2439 0.4791 0.0093 0.066 Uiso 1 1 calc R . . C54 C 0.4377(4) 0.45473(17) 0.0648(2) 0.0453(9) Uani 1 1 d . . . H54 H 0.4499 0.4209 0.0298 0.054 Uiso 1 1 calc R . . C55 C 0.5422(4) 0.46922(18) 0.1279(2) 0.0469(9) Uani 1 1 d . . . H55 H 0.6267 0.4450 0.1365 0.056 Uiso 1 1 calc R . . C56 C 0.5263(4) 0.51859(17) 0.1790(2) 0.0379(8) Uani 1 1 d . . . H56 H 0.5997 0.5282 0.2224 0.045 Uiso 1 1 calc R . . C61 C 0.5020(3) 0.62073(14) 0.31748(16) 0.0248(6) Uani 1 1 d . . . C62 C 0.6394(3) 0.63442(16) 0.31316(19) 0.0334(7) Uani 1 1 d . . . H62 H 0.6632 0.6395 0.2637 0.040 Uiso 1 1 calc R . . C63 C 0.7409(4) 0.64064(18) 0.3807(2) 0.0416(9) Uani 1 1 d . . . H63 H 0.8344 0.6501 0.3776 0.050 Uiso 1 1 calc R . . C64 C 0.7071(4) 0.63315(19) 0.4522(2) 0.0488(10) Uani 1 1 d . . . H64 H 0.7779 0.6367 0.4983 0.059 Uiso 1 1 calc R . . C65 C 0.5730(4) 0.62062(19) 0.4580(2) 0.0466(9) Uani 1 1 d . . . H65 H 0.5507 0.6158 0.5079 0.056 Uiso 1 1 calc R . . C66 C 0.4685(4) 0.61492(16) 0.39037(17) 0.0335(7) Uani 1 1 d . . . H66 H 0.3748 0.6071 0.3942 0.040 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02300(13) 0.01665(12) 0.02885(13) 0.00025(10) 0.00078(9) 0.00184(10) C1 0.0289(16) 0.0182(14) 0.0229(14) 0.0013(12) 0.0104(11) 0.0012(13) C2 0.063(2) 0.0262(18) 0.042(2) 0.0036(15) 0.0297(18) 0.0036(17) N3 0.141(4) 0.053(2) 0.089(3) 0.005(2) 0.091(3) 0.006(2) C3 0.040(2) 0.0283(19) 0.052(2) -0.0026(17) -0.0100(17) 0.0000(17) O3 0.077(2) 0.0473(19) 0.092(2) -0.0168(17) -0.0325(18) -0.0174(16) C4 0.0295(18) 0.0239(17) 0.0374(18) -0.0027(14) -0.0014(14) 0.0011(14) O4 0.0505(16) 0.0362(15) 0.0586(17) 0.0048(12) -0.0093(13) 0.0171(13) N1 0.0221(13) 0.0171(12) 0.0269(13) -0.0006(10) 0.0097(10) -0.0004(10) C11 0.0179(14) 0.0230(15) 0.0256(15) -0.0064(12) 0.0048(11) -0.0022(12) C12 0.040(2) 0.038(2) 0.0328(18) 0.0046(14) 0.0138(14) 0.0103(15) C13 0.047(2) 0.058(3) 0.0273(17) -0.0049(17) 0.0133(15) 0.0098(19) C14 0.0270(18) 0.043(2) 0.045(2) -0.0205(17) 0.0064(14) 0.0014(16) C15 0.0287(18) 0.0227(17) 0.052(2) -0.0076(15) 0.0075(14) -0.0001(14) C16 0.0262(17) 0.0213(16) 0.0356(17) 0.0010(13) 0.0057(13) 0.0000(13) N2 0.0201(13) 0.0179(13) 0.0308(13) 0.0057(10) 0.0062(10) 0.0032(10) C21 0.0245(15) 0.0193(15) 0.0230(14) -0.0008(12) 0.0047(11) -0.0013(12) C22 0.0305(17) 0.0224(16) 0.0351(17) 0.0004(13) 0.0124(13) 0.0035(13) C23 0.0304(18) 0.0322(19) 0.0413(19) -0.0002(15) 0.0155(14) -0.0046(15) C24 0.040(2) 0.0240(17) 0.0348(18) 0.0039(13) 0.0084(14) -0.0091(15) C25 0.0394(19) 0.0153(15) 0.0346(17) 0.0022(13) 0.0019(14) 0.0020(13) C26 0.0269(17) 0.0210(16) 0.0356(17) 0.0046(13) 0.0084(13) 0.0013(13) P1 0.0259(4) 0.0175(4) 0.0228(4) 0.0017(3) 0.0088(3) -0.0016(3) C31 0.0299(17) 0.0199(15) 0.0304(16) -0.0005(12) 0.0107(13) -0.0035(13) C32 0.0359(19) 0.048(2) 0.0400(19) 0.0022(16) 0.0155(15) -0.0077(17) C33 0.031(2) 0.067(3) 0.059(2) -0.003(2) 0.0170(17) -0.0184(19) C34 0.034(2) 0.056(3) 0.052(2) -0.0103(19) 0.0036(16) -0.0124(19) C35 0.039(2) 0.044(2) 0.0317(18) -0.0063(15) 0.0063(14) -0.0035(16) C36 0.0286(17) 0.0315(18) 0.0325(17) -0.0035(14) 0.0107(13) -0.0016(14) C41 0.0375(18) 0.0196(15) 0.0278(16) 0.0050(12) 0.0142(13) 0.0016(13) C42 0.048(2) 0.0251(18) 0.0330(17) 0.0040(14) 0.0079(15) 0.0024(16) C43 0.057(2) 0.045(2) 0.0315(18) 0.0057(16) 0.0118(16) 0.0114(19) C44 0.056(2) 0.033(2) 0.045(2) 0.0179(17) 0.0240(18) 0.0130(18) C45 0.056(2) 0.0205(18) 0.059(2) 0.0099(16) 0.0280(19) 0.0012(16) C46 0.049(2) 0.0231(17) 0.0361(18) 0.0021(14) 0.0136(15) -0.0025(15) P2 0.0232(4) 0.0176(4) 0.0225(4) 0.0018(3) 0.0066(3) 0.0033(3) C51 0.0365(18) 0.0193(15) 0.0239(15) -0.0007(12) 0.0086(13) 0.0029(13) C52 0.044(2) 0.043(2) 0.043(2) -0.0147(17) -0.0015(16) 0.0127(18) C53 0.061(3) 0.050(3) 0.047(2) -0.0194(19) -0.0030(19) 0.008(2) C54 0.074(3) 0.0273(19) 0.039(2) -0.0051(15) 0.0230(19) 0.0032(19) C55 0.054(2) 0.038(2) 0.052(2) -0.0011(18) 0.0181(19) 0.0189(18) C56 0.0359(19) 0.038(2) 0.0392(18) -0.0045(16) 0.0056(14) 0.0093(16) C61 0.0297(17) 0.0176(15) 0.0262(15) 0.0002(12) 0.0039(12) 0.0053(13) C62 0.0278(17) 0.0364(19) 0.0374(18) -0.0038(15) 0.0102(14) 0.0045(15) C63 0.0254(18) 0.040(2) 0.056(2) -0.0094(17) 0.0027(16) 0.0050(15) C64 0.054(3) 0.045(2) 0.037(2) -0.0042(17) -0.0145(17) 0.0037(19) C65 0.059(3) 0.049(2) 0.0294(18) 0.0052(16) 0.0029(16) -0.009(2) C66 0.0384(19) 0.0323(19) 0.0304(17) 0.0007(14) 0.0088(14) -0.0029(15) _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 C3 1.846(3) . ? Rh1 C4 1.846(3) . ? Rh1 N2 2.117(2) . ? Rh1 N1 2.125(2) . ? C1 C2 1.405(4) . ? C1 P2 1.746(3) . ? C1 P1 1.752(3) . ? C2 N3 1.140(4) . ? C3 O3 1.130(4) . ? C4 O4 1.133(4) . ? N1 C11 1.434(3) . ? N1 P1 1.617(2) . ? C11 C16 1.393(4) . ? C11 C12 1.395(4) . ? C12 C13 1.388(5) . ? C13 C14 1.374(5) . ? C14 C15 1.368(5) . ? C15 C16 1.381(4) . ? N2 C21 1.411(4) . ? N2 P2 1.620(2) . ? C21 C22 1.398(4) . ? C21 C26 1.406(4) . ? C22 C23 1.380(4) . ? C23 C24 1.384(5) . ? C24 C25 1.377(5) . ? C25 C26 1.381(4) . ? P1 C31 1.808(3) . ? P1 C41 1.821(3) . ? C31 C36 1.394(4) . ? C31 C32 1.397(4) . ? C32 C33 1.382(5) . ? C33 C34 1.378(5) . ? C34 C35 1.372(5) . ? C35 C36 1.392(4) . ? C41 C46 1.390(4) . ? C41 C42 1.398(4) . ? C42 C43 1.388(5) . ? C43 C44 1.377(5) . ? C44 C45 1.365(5) . ? C45 C46 1.387(5) . ? P2 C51 1.804(3) . ? P2 C61 1.812(3) . ? C51 C52 1.383(4) . ? C51 C56 1.389(4) . ? C52 C53 1.387(5) . ? C53 C54 1.358(5) . ? C54 C55 1.371(5) . ? C55 C56 1.380(5) . ? C61 C66 1.391(4) . ? C61 C62 1.395(4) . ? C62 C63 1.382(4) . ? C63 C64 1.371(5) . ? C64 C65 1.366(5) . ? C65 C66 1.398(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Rh1 C4 88.49(14) . . ? C3 Rh1 N2 90.50(13) . . ? C4 Rh1 N2 178.59(12) . . ? C3 Rh1 N1 178.03(12) . . ? C4 Rh1 N1 93.37(11) . . ? N2 Rh1 N1 87.63(9) . . ? C2 C1 P2 117.9(2) . . ? C2 C1 P1 117.6(2) . . ? P2 C1 P1 119.51(15) . . ? N3 C2 C1 178.1(4) . . ? O3 C3 Rh1 178.4(4) . . ? O4 C4 Rh1 177.6(3) . . ? C11 N1 P1 122.10(19) . . ? C11 N1 Rh1 120.05(17) . . ? P1 N1 Rh1 111.56(12) . . ? C16 C11 C12 118.1(3) . . ? C16 C11 N1 122.5(3) . . ? C12 C11 N1 119.4(3) . . ? C13 C12 C11 120.1(3) . . ? C14 C13 C12 120.9(3) . . ? C15 C14 C13 119.3(3) . . ? C14 C15 C16 120.8(3) . . ? C15 C16 C11 120.8(3) . . ? C21 N2 P2 124.05(19) . . ? C21 N2 Rh1 122.18(18) . . ? P2 N2 Rh1 113.63(12) . . ? C22 C21 C26 116.9(3) . . ? C22 C21 N2 118.8(3) . . ? C26 C21 N2 124.2(3) . . ? C23 C22 C21 121.6(3) . . ? C22 C23 C24 120.7(3) . . ? C25 C24 C23 118.5(3) . . ? C24 C25 C26 121.4(3) . . ? C25 C26 C21 120.8(3) . . ? N1 P1 C1 104.82(13) . . ? N1 P1 C31 113.04(13) . . ? C1 P1 C31 110.94(14) . . ? N1 P1 C41 114.57(13) . . ? C1 P1 C41 108.08(13) . . ? C31 P1 C41 105.39(14) . . ? C36 C31 C32 119.4(3) . . ? C36 C31 P1 121.6(2) . . ? C32 C31 P1 118.6(2) . . ? C33 C32 C31 119.9(3) . . ? C34 C33 C32 120.4(3) . . ? C35 C34 C33 120.3(3) . . ? C34 C35 C36 120.4(3) . . ? C35 C36 C31 119.7(3) . . ? C46 C41 C42 119.0(3) . . ? C46 C41 P1 121.5(2) . . ? C42 C41 P1 119.0(2) . . ? C43 C42 C41 119.8(3) . . ? C44 C43 C42 120.4(3) . . ? C45 C44 C43 120.1(3) . . ? C44 C45 C46 120.6(3) . . ? C45 C46 C41 120.1(3) . . ? N2 P2 C1 108.30(13) . . ? N2 P2 C51 112.41(14) . . ? C1 P2 C51 106.11(13) . . ? N2 P2 C61 111.20(13) . . ? C1 P2 C61 109.92(14) . . ? C51 P2 C61 108.77(14) . . ? C52 C51 C56 118.4(3) . . ? C52 C51 P2 116.5(2) . . ? C56 C51 P2 125.1(2) . . ? C51 C52 C53 120.5(3) . . ? C54 C53 C52 120.6(3) . . ? C53 C54 C55 119.5(3) . . ? C54 C55 C56 120.9(3) . . ? C55 C56 C51 120.1(3) . . ? C66 C61 C62 119.2(3) . . ? C66 C61 P2 120.8(2) . . ? C62 C61 P2 119.7(2) . . ? C63 C62 C61 120.1(3) . . ? C64 C63 C62 120.2(3) . . ? C65 C64 C63 120.9(3) . . ? C64 C65 C66 119.8(3) . . ? C61 C66 C65 119.9(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 C4 Rh1 N1 C11 49.2(2) . . . . ? N2 Rh1 N1 C11 -129.8(2) . . . . ? C4 Rh1 N1 P1 -103.53(15) . . . . ? N2 Rh1 N1 P1 77.47(13) . . . . ? P1 N1 C11 C16 62.0(3) . . . . ? Rh1 N1 C11 C16 -87.8(3) . . . . ? P1 N1 C11 C12 -119.2(3) . . . . ? Rh1 N1 C11 C12 91.1(3) . . . . ? C16 C11 C12 C13 -1.0(5) . . . . ? N1 C11 C12 C13 -179.9(3) . . . . ? C11 C12 C13 C14 1.9(5) . . . . ? C12 C13 C14 C15 -1.3(5) . . . . ? C13 C14 C15 C16 -0.1(5) . . . . ? C14 C15 C16 C11 1.0(5) . . . . ? C12 C11 C16 C15 -0.5(4) . . . . ? N1 C11 C16 C15 178.4(3) . . . . ? C3 Rh1 N2 C21 -53.2(2) . . . . ? N1 Rh1 N2 C21 126.1(2) . . . . ? C3 Rh1 N2 P2 122.71(17) . . . . ? N1 Rh1 N2 P2 -57.93(13) . . . . ? P2 N2 C21 C22 166.0(2) . . . . ? Rh1 N2 C21 C22 -18.5(3) . . . . ? P2 N2 C21 C26 -13.7(4) . . . . ? Rh1 N2 C21 C26 161.7(2) . . . . ? C26 C21 C22 C23 -0.3(4) . . . . ? N2 C21 C22 C23 179.9(3) . . . . ? C21 C22 C23 C24 0.6(5) . . . . ? C22 C23 C24 C25 -0.2(5) . . . . ? C23 C24 C25 C26 -0.4(5) . . . . ? C24 C25 C26 C21 0.7(5) . . . . ? C22 C21 C26 C25 -0.3(4) . . . . ? N2 C21 C26 C25 179.5(3) . . . . ? C11 N1 P1 C1 175.9(2) . . . . ? Rh1 N1 P1 C1 -32.00(15) . . . . ? C11 N1 P1 C31 55.0(2) . . . . ? Rh1 N1 P1 C31 -152.96(13) . . . . ? C11 N1 P1 C41 -65.8(2) . . . . ? Rh1 N1 P1 C41 86.28(16) . . . . ? C2 C1 P1 N1 160.5(3) . . . . ? P2 C1 P1 N1 -44.9(2) . . . . ? C2 C1 P1 C31 -77.2(3) . . . . ? P2 C1 P1 C31 77.4(2) . . . . ? C2 C1 P1 C41 37.9(3) . . . . ? P2 C1 P1 C41 -167.49(17) . . . . ? N1 P1 C31 C36 12.2(3) . . . . ? C1 P1 C31 C36 -105.3(3) . . . . ? C41 P1 C31 C36 138.0(3) . . . . ? N1 P1 C31 C32 -175.5(2) . . . . ? C1 P1 C31 C32 67.1(3) . . . . ? C41 P1 C31 C32 -49.7(3) . . . . ? C36 C31 C32 C33 -0.8(5) . . . . ? P1 C31 C32 C33 -173.3(3) . . . . ? C31 C32 C33 C34 0.1(6) . . . . ? C32 C33 C34 C35 0.7(6) . . . . ? C33 C34 C35 C36 -0.9(6) . . . . ? C34 C35 C36 C31 0.3(5) . . . . ? C32 C31 C36 C35 0.6(5) . . . . ? P1 C31 C36 C35 172.8(3) . . . . ? N1 P1 C41 C46 99.5(3) . . . . ? C1 P1 C41 C46 -144.1(3) . . . . ? C31 P1 C41 C46 -25.4(3) . . . . ? N1 P1 C41 C42 -72.9(3) . . . . ? C1 P1 C41 C42 43.6(3) . . . . ? C31 P1 C41 C42 162.2(3) . . . . ? C46 C41 C42 C43 0.2(5) . . . . ? P1 C41 C42 C43 172.7(3) . . . . ? C41 C42 C43 C44 0.2(5) . . . . ? C42 C43 C44 C45 -0.7(5) . . . . ? C43 C44 C45 C46 0.7(5) . . . . ? C44 C45 C46 C41 -0.3(5) . . . . ? C42 C41 C46 C45 -0.1(5) . . . . ? P1 C41 C46 C45 -172.5(3) . . . . ? C21 N2 P2 C1 179.1(2) . . . . ? Rh1 N2 P2 C1 3.31(17) . . . . ? C21 N2 P2 C51 62.2(3) . . . . ? Rh1 N2 P2 C51 -113.59(14) . . . . ? C21 N2 P2 C61 -60.0(3) . . . . ? Rh1 N2 P2 C61 124.18(13) . . . . ? C2 C1 P2 N2 -142.5(3) . . . . ? P1 C1 P2 N2 63.0(2) . . . . ? C2 C1 P2 C51 -21.6(3) . . . . ? P1 C1 P2 C51 -176.15(17) . . . . ? C2 C1 P2 C61 95.8(3) . . . . ? P1 C1 P2 C61 -58.7(2) . . . . ? N2 P2 C51 C52 45.2(3) . . . . ? C1 P2 C51 C52 -73.0(3) . . . . ? C61 P2 C51 C52 168.8(3) . . . . ? N2 P2 C51 C56 -134.1(3) . . . . ? C1 P2 C51 C56 107.7(3) . . . . ? C61 P2 C51 C56 -10.6(3) . . . . ? C56 C51 C52 C53 -0.6(6) . . . . ? P2 C51 C52 C53 180.0(3) . . . . ? C51 C52 C53 C54 0.4(6) . . . . ? C52 C53 C54 C55 0.2(6) . . . . ? C53 C54 C55 C56 -0.5(6) . . . . ? C54 C55 C56 C51 0.2(6) . . . . ? C52 C51 C56 C55 0.3(5) . . . . ? P2 C51 C56 C55 179.7(3) . . . . ? N2 P2 C61 C66 1.6(3) . . . . ? C1 P2 C61 C66 121.5(3) . . . . ? C51 P2 C61 C66 -122.8(3) . . . . ? N2 P2 C61 C62 -171.6(2) . . . . ? C1 P2 C61 C62 -51.7(3) . . . . ? C51 P2 C61 C62 64.1(3) . . . . ? C66 C61 C62 C63 1.4(5) . . . . ? P2 C61 C62 C63 174.6(3) . . . . ? C61 C62 C63 C64 0.2(5) . . . . ? C62 C63 C64 C65 -1.1(6) . . . . ? C63 C64 C65 C66 0.4(6) . . . . ? C62 C61 C66 C65 -2.1(5) . . . . ? P2 C61 C66 C65 -175.3(3) . . . . ? C64 C65 C66 C61 1.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.878 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.085 # Attachment '12.cif' data_erk4168 _database_code_depnum_ccdc_archive 'CCDC 676925' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H46 N3 P2 Rh' _chemical_formula_weight 877.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 '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 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 9.9780(1) _cell_length_b 20.7312(3) _cell_length_c 41.3429(7) _cell_angle_alpha 90.00 _cell_angle_beta 91.050(1) _cell_angle_gamma 90.00 _cell_volume 8550.6(2) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 20909 _cell_measurement_theta_min 0.88 _cell_measurement_theta_max 68.25 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3632 _exptl_absorpt_coefficient_mu 4.237 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4845 _exptl_absorpt_correction_T_max 0.9201 _exptl_absorpt_process_details 'Denzo (Otwinowski, Borek, Majewski & Minor, 2003)' _exptl_special_details ; Due to the needle shape of the crystal and the high redundancy of the data set Rmerge is quite high. ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NOnius KappaCCD APEXII' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 78803 _diffrn_reflns_av_R_equivalents 0.128 _diffrn_reflns_av_sigmaI/netI 0.0665 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -49 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 68.15 _reflns_number_total 15282 _reflns_number_gt 10879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'DEnzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to Zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on all data will be even larger. Toluene molecule B was refined with two split positions for the methyl carbon C77, using PART command, geometrical restraints (AFIX 66, SADI) and isotropic thermal parameters. ; _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^)+(0.0672P)^2^+34.0028P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15282 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0979 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1422 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1A Rh 0.29442(4) 0.76762(2) 0.140642(10) 0.03198(13) Uani 1 1 d . . . C1A C 0.0685(6) 0.8434(3) 0.20215(14) 0.0355(14) Uani 1 1 d . . . C2A C -0.0145(6) 0.8723(3) 0.22503(14) 0.0382(14) Uani 1 1 d . . . N3A N -0.0837(6) 0.8969(3) 0.24301(14) 0.0621(18) Uani 1 1 d . . . C3A C 0.4687(6) 0.7093(3) 0.13956(16) 0.0406(15) Uani 1 1 d . . . H3A H 0.4941 0.7092 0.1616 0.049 Uiso 1 1 calc R . . C4A C 0.3621(6) 0.6763(3) 0.12553(15) 0.0412(15) Uani 1 1 d . . . H4A H 0.3004 0.6496 0.1361 0.049 Uiso 1 1 calc R . . C5A C 0.3649(7) 0.6921(3) 0.08920(15) 0.0430(15) Uani 1 1 d . . . H5A H 0.3141 0.6632 0.0743 0.052 Uiso 1 1 calc R . . C6A C 0.3259(7) 0.7628(3) 0.08945(15) 0.0460(17) Uani 1 1 d . . . H6A H 0.2459 0.7807 0.0811 0.055 Uiso 1 1 calc R . . C7A C 0.4312(7) 0.7960(3) 0.10431(16) 0.0478(17) Uani 1 1 d . . . H7A H 0.4361 0.8406 0.1084 0.057 Uiso 1 1 calc R . . C8A C 0.5367(7) 0.7454(3) 0.11251(18) 0.0517(18) Uani 1 1 d . . . H8A H 0.6293 0.7608 0.1167 0.062 Uiso 1 1 calc R . . C9A C 0.5150(7) 0.6974(3) 0.08453(18) 0.0514(18) Uani 1 1 d . . . H9A1 H 0.5380 0.7155 0.0635 0.062 Uiso 1 1 calc R . . H9A2 H 0.5619 0.6564 0.0881 0.062 Uiso 1 1 calc R . . N1A N 0.1598(5) 0.8470(2) 0.13940(12) 0.0360(12) Uani 1 1 d . . . C11A C 0.1902(5) 0.9008(3) 0.11965(14) 0.0309(13) Uani 1 1 d . . . C12A C 0.2977(6) 0.9403(3) 0.12744(17) 0.0463(16) Uani 1 1 d . . . H12A H 0.3482 0.9324 0.1464 0.056 Uiso 1 1 calc R . . C13A C 0.3324(7) 0.9921(3) 0.10725(19) 0.0548(19) Uani 1 1 d . . . H13A H 0.4051 1.0190 0.1128 0.066 Uiso 1 1 calc R . . C14A C 0.2586(8) 1.0029(4) 0.0793(2) 0.065(2) Uani 1 1 d . . . H14A H 0.2817 1.0372 0.0657 0.077 Uiso 1 1 calc R . . C15A C 0.1525(7) 0.9644(4) 0.07131(17) 0.0535(18) Uani 1 1 d . . . H15A H 0.1025 0.9725 0.0522 0.064 Uiso 1 1 calc R . . C16A C 0.1183(6) 0.9137(3) 0.09110(15) 0.0410(15) Uani 1 1 d . . . H16A H 0.0451 0.8873 0.0853 0.049 Uiso 1 1 calc R . . N2A N 0.2448(5) 0.7447(2) 0.18932(11) 0.0343(11) Uani 1 1 d . . . C21A C 0.2415(6) 0.6787(3) 0.19939(13) 0.0323(13) Uani 1 1 d . . . C22A C 0.3281(7) 0.6553(3) 0.22333(16) 0.0490(17) Uani 1 1 d . . . H22A H 0.3928 0.6828 0.2328 0.059 Uiso 1 1 calc R . . C23A C 0.3194(10) 0.5915(4) 0.2333(2) 0.074(3) Uani 1 1 d . . . H23A H 0.3767 0.5764 0.2500 0.089 Uiso 1 1 calc R . . C24A C 0.2270(10) 0.5501(4) 0.2190(2) 0.076(3) Uani 1 1 d . . . H24A H 0.2212 0.5069 0.2257 0.091 Uiso 1 1 calc R . . C25A C 0.1439(9) 0.5732(3) 0.19483(19) 0.062(2) Uani 1 1 d . . . H25A H 0.0813 0.5453 0.1848 0.075 Uiso 1 1 calc R . . C26A C 0.1510(7) 0.6358(3) 0.18512(16) 0.0449(16) Uani 1 1 d . . . H26A H 0.0935 0.6503 0.1684 0.054 Uiso 1 1 calc R . . P1A P 0.02836(14) 0.84244(7) 0.16100(3) 0.0308(3) Uani 1 1 d . . . C31A C -0.0571(5) 0.7677(3) 0.15069(13) 0.0314(13) Uani 1 1 d . . . C32A C -0.0408(6) 0.7382(3) 0.12110(14) 0.0394(14) Uani 1 1 d . . . H32A H 0.0118 0.7582 0.1054 0.047 Uiso 1 1 calc R . . C33A C -0.1012(7) 0.6790(4) 0.11428(17) 0.0486(17) Uani 1 1 d . . . H33A H -0.0902 0.6594 0.0940 0.058 Uiso 1 1 calc R . . C34A C -0.1771(7) 0.6494(3) 0.13748(18) 0.0506(18) Uani 1 1 d . . . H34A H -0.2150 0.6087 0.1333 0.061 Uiso 1 1 calc R . . C35A C -0.1978(6) 0.6788(3) 0.16662(17) 0.0473(17) Uani 1 1 d . . . H35A H -0.2522 0.6588 0.1820 0.057 Uiso 1 1 calc R . . C36A C -0.1388(6) 0.7379(3) 0.17359(16) 0.0417(15) Uani 1 1 d . . . H36A H -0.1536 0.7580 0.1936 0.050 Uiso 1 1 calc R . . C41A C -0.0904(6) 0.9068(3) 0.15363(14) 0.0346(13) Uani 1 1 d . . . C42A C -0.0664(6) 0.9671(3) 0.16747(17) 0.0456(16) Uani 1 1 d . . . H42A H 0.0111 0.9736 0.1803 0.055 Uiso 1 1 calc R . . C43A C -0.1549(8) 1.0173(4) 0.1625(2) 0.061(2) Uani 1 1 d . . . H43A H -0.1387 1.0576 0.1723 0.073 Uiso 1 1 calc R . . C44A C -0.2679(7) 1.0083(4) 0.14307(18) 0.0542(19) Uani 1 1 d . . . H44A H -0.3283 1.0424 0.1395 0.065 Uiso 1 1 calc R . . C45A C -0.2913(7) 0.9499(4) 0.12912(18) 0.057(2) Uani 1 1 d . . . H45A H -0.3677 0.9442 0.1158 0.068 Uiso 1 1 calc R . . C46A C -0.2043(6) 0.8985(4) 0.13420(16) 0.0451(16) Uani 1 1 d . . . H46A H -0.2223 0.8583 0.1245 0.054 Uiso 1 1 calc R . . P2A P 0.21561(14) 0.80290(7) 0.21355(3) 0.0304(3) Uani 1 1 d . . . C51A C 0.1997(6) 0.7770(3) 0.25515(14) 0.0349(13) Uani 1 1 d . . . C52A C 0.3012(7) 0.7877(4) 0.27820(15) 0.0492(17) Uani 1 1 d . . . H52A H 0.3764 0.8127 0.2729 0.059 Uiso 1 1 calc R . . C53A C 0.2910(8) 0.7615(4) 0.30897(16) 0.0558(19) Uani 1 1 d . . . H53A H 0.3599 0.7681 0.3244 0.067 Uiso 1 1 calc R . . C54A C 0.1802(8) 0.7259(4) 0.31684(17) 0.0571(19) Uani 1 1 d . . . H54A H 0.1733 0.7082 0.3377 0.069 Uiso 1 1 calc R . . C55A C 0.0797(8) 0.7163(4) 0.29433(16) 0.0537(18) Uani 1 1 d . . . H55A H 0.0039 0.6921 0.2999 0.064 Uiso 1 1 calc R . . C56A C 0.0885(6) 0.7415(3) 0.26384(15) 0.0404(15) Uani 1 1 d . . . H56A H 0.0186 0.7345 0.2487 0.048 Uiso 1 1 calc R . . C61A C 0.3574(6) 0.8572(3) 0.21329(14) 0.0349(14) Uani 1 1 d . . . C62A C 0.4831(6) 0.8363(4) 0.20528(16) 0.0469(17) Uani 1 1 d . . . H62A H 0.4949 0.7935 0.1983 0.056 Uiso 1 1 calc R . . C63A C 0.5922(7) 0.8769(4) 0.20731(18) 0.0557(19) Uani 1 1 d . . . H63A H 0.6774 0.8617 0.2017 0.067 Uiso 1 1 calc R . . C64A C 0.5771(7) 0.9390(4) 0.21742(17) 0.0534(19) Uani 1 1 d . . . H64A H 0.6517 0.9666 0.2192 0.064 Uiso 1 1 calc R . . C65A C 0.4526(8) 0.9606(4) 0.2249(2) 0.065(2) Uani 1 1 d . . . H65A H 0.4420 1.0036 0.2315 0.078 Uiso 1 1 calc R . . C66A C 0.3417(7) 0.9211(3) 0.22296(19) 0.0524(18) Uani 1 1 d . . . H66A H 0.2566 0.9371 0.2281 0.063 Uiso 1 1 calc R . . C71A C 0.2179(11) 0.9555(6) 0.3265(3) 0.095(3) Uani 1 1 d . . . C72A C 0.2769(11) 0.9452(6) 0.3576(2) 0.088(3) Uani 1 1 d . . . H72A H 0.2408 0.9145 0.3717 0.105 Uiso 1 1 calc R . . C73A C 0.3823(13) 0.9791(7) 0.3665(3) 0.114(4) Uani 1 1 d . . . H73A H 0.4161 0.9725 0.3876 0.137 Uiso 1 1 calc R . . C74A C 0.4527(12) 1.0266(6) 0.3464(4) 0.104(4) Uani 1 1 d . . . H74A H 0.5287 1.0503 0.3530 0.124 Uiso 1 1 calc R . . C75A C 0.3940(16) 1.0310(7) 0.3180(4) 0.135(5) Uani 1 1 d . . . H75A H 0.4332 1.0594 0.3031 0.163 Uiso 1 1 calc R . . C76A C 0.2775(11) 0.9977(5) 0.3070(2) 0.079(3) Uani 1 1 d . . . H76A H 0.2423 1.0053 0.2861 0.095 Uiso 1 1 calc R . . C77A C 0.1085(11) 0.9181(6) 0.3170(3) 0.126(5) Uani 1 1 d . . . H77A H 0.0263 0.9402 0.3225 0.189 Uiso 1 1 calc R . . H77B H 0.1124 0.8769 0.3281 0.189 Uiso 1 1 calc R . . H77C H 0.1103 0.9112 0.2938 0.189 Uiso 1 1 calc R . . Rh1B Rh 0.16944(4) 0.32002(2) 0.022584(10) 0.03184(13) Uani 1 1 d . . . C1B C 0.4030(6) 0.2388(3) 0.08347(14) 0.0364(14) Uani 1 1 d . . . C2B C 0.4858(7) 0.2044(4) 0.10482(16) 0.0469(16) Uani 1 1 d . . . N3B N 0.5560(7) 0.1757(4) 0.12255(16) 0.083(2) Uani 1 1 d . . . C3B C 0.1338(7) 0.3265(4) -0.02820(15) 0.0483(17) Uani 1 1 d . . . H3B H 0.2138 0.3089 -0.0360 0.058 Uiso 1 1 calc R . . C4B C 0.0295(7) 0.2933(3) -0.01434(16) 0.0470(17) Uani 1 1 d . . . H4B H 0.0246 0.2485 -0.0109 0.056 Uiso 1 1 calc R . . C5B C -0.0760(6) 0.3432(3) -0.00568(16) 0.0457(16) Uani 1 1 d . . . H5B H -0.1677 0.3271 -0.0017 0.055 Uiso 1 1 calc R . . C6B C -0.0054(6) 0.3792(3) 0.02201(16) 0.0424(16) Uani 1 1 d . . . H6B H -0.0286 0.3791 0.0439 0.051 Uiso 1 1 calc R . . C7B C 0.1005(6) 0.4122(3) 0.00807(16) 0.0437(16) Uani 1 1 d . . . H7B H 0.1642 0.4382 0.0189 0.052 Uiso 1 1 calc R . . C8B C 0.0930(7) 0.3978(4) -0.02831(16) 0.0504(17) Uani 1 1 d . . . H8B H 0.1415 0.4272 -0.0429 0.060 Uiso 1 1 calc R . . C9B C -0.0599(7) 0.3917(4) -0.03327(17) 0.0539(19) Uani 1 1 d . . . H9B1 H -0.1074 0.4323 -0.0295 0.065 Uiso 1 1 calc R . . H9B2 H -0.0853 0.3739 -0.0545 0.065 Uiso 1 1 calc R . . N1B N 0.2279(5) 0.3391(2) 0.07150(11) 0.0319(11) Uani 1 1 d . . . C11B C 0.2092(6) 0.4020(3) 0.08310(13) 0.0324(13) Uani 1 1 d . . . C12B C 0.3001(6) 0.4500(3) 0.07524(15) 0.0408(15) Uani 1 1 d . . . H12B H 0.3748 0.4400 0.0627 0.049 Uiso 1 1 calc R . . C13B C 0.2812(7) 0.5122(3) 0.08571(16) 0.0445(16) Uani 1 1 d . . . H13B H 0.3440 0.5441 0.0804 0.053 Uiso 1 1 calc R . . C14B C 0.1729(7) 0.5286(3) 0.10376(16) 0.0465(16) Uani 1 1 d . . . H14B H 0.1617 0.5712 0.1109 0.056 Uiso 1 1 calc R . . C15B C 0.0812(7) 0.4821(3) 0.11123(16) 0.0472(16) Uani 1 1 d . . . H15B H 0.0054 0.4930 0.1232 0.057 Uiso 1 1 calc R . . C16B C 0.0993(7) 0.4194(3) 0.10125(15) 0.0439(16) Uani 1 1 d . . . H16B H 0.0361 0.3878 0.1068 0.053 Uiso 1 1 calc R . . N2B N 0.3035(5) 0.2418(2) 0.01977(12) 0.0365(12) Uani 1 1 d . . . C21B C 0.2636(6) 0.1856(3) 0.00291(14) 0.0337(13) Uani 1 1 d . . . C22B C 0.1598(6) 0.1484(3) 0.01296(16) 0.0436(15) Uani 1 1 d . . . H22B H 0.1160 0.1590 0.0322 0.052 Uiso 1 1 calc R . . C23B C 0.1170(8) 0.0942(4) -0.0050(2) 0.062(2) Uani 1 1 d . . . H23B H 0.0448 0.0693 0.0022 0.074 Uiso 1 1 calc R . . C24B C 0.1800(9) 0.0775(4) -0.0329(2) 0.068(2) Uani 1 1 d . . . H24B H 0.1521 0.0413 -0.0450 0.081 Uiso 1 1 calc R . . C25B C 0.2842(9) 0.1148(4) -0.0429(2) 0.069(2) Uani 1 1 d . . . H25B H 0.3281 0.1039 -0.0621 0.083 Uiso 1 1 calc R . . C26B C 0.3266(7) 0.1678(3) -0.02567(16) 0.0499(17) Uani 1 1 d . . . H26B H 0.3989 0.1924 -0.0332 0.060 Uiso 1 1 calc R . . P1B P 0.25894(14) 0.27877(7) 0.09554(3) 0.0301(3) Uani 1 1 d . . . C31B C 0.2838(6) 0.3059(3) 0.13642(13) 0.0317(13) Uani 1 1 d . . . C32B C 0.1845(6) 0.2977(3) 0.15947(15) 0.0437(16) Uani 1 1 d . . . H32B H 0.1072 0.2736 0.1545 0.052 Uiso 1 1 calc R . . C33B C 0.2010(7) 0.3257(4) 0.18999(16) 0.0533(18) Uani 1 1 d . . . H33B H 0.1338 0.3207 0.2054 0.064 Uiso 1 1 calc R . . C34B C 0.3138(7) 0.3601(3) 0.19768(15) 0.0487(17) Uani 1 1 d . . . H34B H 0.3235 0.3792 0.2182 0.058 Uiso 1 1 calc R . . C35B C 0.4138(7) 0.3670(3) 0.17515(15) 0.0492(17) Uani 1 1 d . . . H35B H 0.4928 0.3894 0.1807 0.059 Uiso 1 1 calc R . . C36B C 0.3979(6) 0.3410(3) 0.14457(15) 0.0429(15) Uani 1 1 d . . . H36B H 0.4648 0.3472 0.1292 0.051 Uiso 1 1 calc R . . C41B C 0.1182(6) 0.2238(3) 0.09575(14) 0.0345(13) Uani 1 1 d . . . C42B C 0.1343(7) 0.1617(3) 0.10712(17) 0.0482(17) Uani 1 1 d . . . H42B H 0.2187 0.1480 0.1150 0.058 Uiso 1 1 calc R . . C43B C 0.0268(8) 0.1193(4) 0.1071(2) 0.065(2) Uani 1 1 d . . . H43B H 0.0388 0.0768 0.1145 0.078 Uiso 1 1 calc R . . C44B C -0.0976(8) 0.1394(4) 0.0961(2) 0.063(2) Uani 1 1 d . . . H44B H -0.1706 0.1107 0.0962 0.076 Uiso 1 1 calc R . . C45B C -0.1143(7) 0.2007(4) 0.08505(17) 0.0537(19) Uani 1 1 d . . . H45B H -0.1993 0.2143 0.0777 0.064 Uiso 1 1 calc R . . C46B C -0.0083(6) 0.2431(3) 0.08458(16) 0.0444(16) Uani 1 1 d . . . H46B H -0.0212 0.2853 0.0767 0.053 Uiso 1 1 calc R . . P2B P 0.43679(14) 0.24449(7) 0.04238(3) 0.0303(3) Uani 1 1 d . . . C51B C 0.5194(6) 0.3203(3) 0.03385(14) 0.0328(13) Uani 1 1 d . . . C52B C 0.6091(6) 0.3476(3) 0.05684(16) 0.0413(15) Uani 1 1 d . . . H52B H 0.6263 0.3263 0.0766 0.050 Uiso 1 1 calc R . . C53B C 0.6713(6) 0.4051(4) 0.05048(19) 0.0520(18) Uani 1 1 d . . . H53B H 0.7314 0.4228 0.0658 0.062 Uiso 1 1 calc R . . C54B C 0.6469(8) 0.4368(4) 0.0221(2) 0.060(2) Uani 1 1 d . . . H54B H 0.6897 0.4764 0.0181 0.071 Uiso 1 1 calc R . . C55B C 0.5598(8) 0.4113(4) -0.00066(19) 0.0556(19) Uani 1 1 d . . . H55B H 0.5433 0.4332 -0.0202 0.067 Uiso 1 1 calc R . . C56B C 0.4966(6) 0.3532(3) 0.00537(16) 0.0415(15) Uani 1 1 d . . . H56B H 0.4370 0.3360 -0.0102 0.050 Uiso 1 1 calc R . . C61B C 0.5513(6) 0.1814(3) 0.03143(14) 0.0345(13) Uani 1 1 d . . . C62B C 0.6502(7) 0.1912(4) 0.00909(17) 0.0515(18) Uani 1 1 d . . . H62B H 0.6670 0.2332 0.0017 0.062 Uiso 1 1 calc R . . C63B C 0.7244(8) 0.1409(4) -0.0025(2) 0.065(2) Uani 1 1 d . . . H63B H 0.7916 0.1487 -0.0177 0.078 Uiso 1 1 calc R . . C64B C 0.7005(9) 0.0787(4) 0.0081(2) 0.073(3) Uani 1 1 d . . . H64B H 0.7505 0.0440 0.0001 0.087 Uiso 1 1 calc R . . C65B C 0.6012(8) 0.0681(4) 0.0309(2) 0.063(2) Uani 1 1 d . . . H65B H 0.5844 0.0262 0.0384 0.075 Uiso 1 1 calc R . . C66B C 0.5284(7) 0.1191(3) 0.04230(17) 0.0471(16) Uani 1 1 d . . . H66B H 0.4620 0.1118 0.0577 0.057 Uiso 1 1 calc R . . C71B C 0.1815(16) 0.0992(8) 0.2251(4) 0.096(7) Uiso 0.468(16) 1 d PGD A 1 C72B C 0.232(2) 0.0791(9) 0.1956(4) 0.082(9) Uiso 0.468(16) 1 d PGD A 1 H72B H 0.1922 0.0440 0.1846 0.098 Uiso 0.468(16) 1 calc PR A 1 C73B C 0.340(2) 0.1110(11) 0.1823(4) 0.113(14) Uiso 0.468(16) 1 d PG A 1 H73B H 0.3741 0.0975 0.1624 0.136 Uiso 0.468(16) 1 calc PR A 1 C74B C 0.3986(19) 0.1629(10) 0.1985(5) 0.123(10) Uiso 0.468(16) 1 d PG A 1 H74B H 0.4720 0.1844 0.1896 0.148 Uiso 0.468(16) 1 calc PR A 1 C75B C 0.3484(17) 0.1829(8) 0.2280(4) 0.092(7) Uiso 0.468(16) 1 d PG A 1 H75B H 0.3879 0.2180 0.2390 0.110 Uiso 0.468(16) 1 calc PR A 1 C76B C 0.2399(17) 0.1511(8) 0.2413(3) 0.081(6) Uiso 0.468(16) 1 d PGD A 1 H76B H 0.2060 0.1646 0.2613 0.097 Uiso 0.468(16) 1 calc PR A 1 C77B C 0.064(2) 0.0700(12) 0.2374(6) 0.126(11) Uiso 0.468(16) 1 d PD A 1 H77D H 0.0405 0.0905 0.2577 0.189 Uiso 0.468(16) 1 calc PR A 1 H77E H 0.0797 0.0244 0.2411 0.189 Uiso 0.468(16) 1 calc PR A 1 H77F H -0.0097 0.0753 0.2219 0.189 Uiso 0.468(16) 1 calc PR A 1 C71C C 0.2873(13) 0.1682(6) 0.2354(3) 0.067(5) Uiso 0.532(16) 1 d PGD A 2 C72C C 0.1834(12) 0.1266(6) 0.2431(2) 0.066(5) Uiso 0.532(16) 1 d PGD A 2 H72C H 0.1379 0.1317 0.2627 0.079 Uiso 0.532(16) 1 calc PR A 2 C73C C 0.1468(13) 0.0773(6) 0.2219(3) 0.072(5) Uiso 0.532(16) 1 d PG A 2 H73C H 0.0765 0.0492 0.2271 0.086 Uiso 0.532(16) 1 calc PR A 2 C74C C 0.2141(18) 0.0697(8) 0.1930(3) 0.110(11) Uiso 0.532(16) 1 d PG A 2 H74C H 0.1893 0.0364 0.1787 0.132 Uiso 0.532(16) 1 calc PR A 2 C75C C 0.3180(18) 0.1113(9) 0.1853(3) 0.088(9) Uiso 0.532(16) 1 d PG A 2 H75C H 0.3635 0.1061 0.1658 0.105 Uiso 0.532(16) 1 calc PR A 2 C76C C 0.3546(13) 0.1605(7) 0.2065(3) 0.075(5) Uiso 0.532(16) 1 d PGD A 2 H76C H 0.4248 0.1887 0.2013 0.090 Uiso 0.532(16) 1 calc PR A 2 C77C C 0.321(2) 0.2233(10) 0.2546(5) 0.118(9) Uiso 0.532(16) 1 d PD A 2 H77G H 0.3817 0.2508 0.2428 0.176 Uiso 0.532(16) 1 calc PR A 2 H77H H 0.3642 0.2095 0.2746 0.176 Uiso 0.532(16) 1 calc PR A 2 H77I H 0.2401 0.2471 0.2594 0.176 Uiso 0.532(16) 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 Rh1A 0.0327(2) 0.0304(2) 0.0329(2) 0.00119(19) 0.00268(17) 0.00152(19) C1A 0.031(3) 0.042(4) 0.034(3) 0.001(3) 0.000(2) -0.001(3) C2A 0.040(4) 0.044(4) 0.030(3) 0.004(3) -0.004(3) 0.005(3) N3A 0.070(4) 0.078(5) 0.039(3) 0.002(3) 0.004(3) 0.033(4) C3A 0.042(4) 0.038(4) 0.042(4) -0.010(3) 0.002(3) 0.001(3) C4A 0.041(4) 0.043(4) 0.040(3) -0.004(3) 0.007(3) 0.001(3) C5A 0.052(4) 0.040(4) 0.036(3) -0.007(3) 0.001(3) 0.001(3) C6A 0.048(4) 0.051(4) 0.040(3) 0.002(3) 0.018(3) 0.018(3) C7A 0.056(4) 0.039(4) 0.050(4) 0.000(3) 0.017(3) 0.001(3) C8A 0.047(4) 0.042(4) 0.067(5) -0.006(3) 0.013(3) -0.009(3) C9A 0.057(4) 0.040(4) 0.058(4) -0.009(3) 0.022(3) 0.005(3) N1A 0.035(3) 0.037(3) 0.036(3) 0.009(2) 0.010(2) 0.009(2) C11A 0.028(3) 0.030(3) 0.036(3) 0.004(2) 0.007(2) 0.007(2) C12A 0.039(4) 0.045(4) 0.055(4) -0.002(3) -0.004(3) 0.001(3) C13A 0.048(4) 0.042(4) 0.075(5) -0.001(4) 0.006(4) -0.012(3) C14A 0.059(5) 0.055(5) 0.080(6) 0.029(4) 0.009(4) -0.001(4) C15A 0.058(5) 0.055(5) 0.048(4) 0.015(4) -0.005(3) -0.001(4) C16A 0.044(4) 0.038(4) 0.041(3) 0.005(3) -0.002(3) -0.005(3) N2A 0.039(3) 0.032(3) 0.032(3) 0.005(2) 0.005(2) -0.003(2) C21A 0.037(3) 0.030(3) 0.030(3) 0.003(3) 0.000(2) 0.003(3) C22A 0.056(4) 0.044(4) 0.047(4) 0.004(3) -0.012(3) 0.013(3) C23A 0.111(7) 0.047(5) 0.064(5) 0.011(4) -0.024(5) 0.024(5) C24A 0.137(8) 0.032(4) 0.060(5) 0.010(4) 0.007(5) 0.006(5) C25A 0.091(6) 0.032(4) 0.063(5) 0.002(4) 0.002(4) -0.015(4) C26A 0.049(4) 0.042(4) 0.044(4) 0.001(3) -0.007(3) 0.002(3) P1A 0.0296(8) 0.0328(8) 0.0299(7) 0.0014(6) -0.0003(6) 0.0020(6) C31A 0.030(3) 0.032(3) 0.032(3) 0.003(3) -0.007(2) 0.002(3) C32A 0.044(4) 0.043(4) 0.031(3) 0.002(3) -0.005(3) 0.001(3) C33A 0.051(4) 0.052(4) 0.042(4) -0.006(3) -0.008(3) 0.001(3) C34A 0.052(4) 0.039(4) 0.061(5) -0.005(3) -0.016(4) -0.006(3) C35A 0.038(4) 0.047(4) 0.057(4) 0.009(3) 0.000(3) -0.012(3) C36A 0.038(3) 0.048(4) 0.039(3) 0.001(3) -0.003(3) -0.005(3) C41A 0.033(3) 0.040(4) 0.031(3) 0.007(3) 0.002(2) 0.000(3) C42A 0.036(4) 0.042(4) 0.058(4) 0.008(3) -0.005(3) -0.002(3) C43A 0.067(5) 0.038(4) 0.077(5) 0.009(4) -0.003(4) 0.004(4) C44A 0.048(4) 0.056(5) 0.059(4) 0.019(4) 0.003(3) 0.012(4) C45A 0.049(4) 0.061(5) 0.059(5) -0.006(4) -0.012(3) 0.020(4) C46A 0.040(4) 0.050(4) 0.046(4) -0.003(3) -0.006(3) 0.004(3) P2A 0.0309(8) 0.0317(8) 0.0285(7) -0.0009(6) -0.0022(6) -0.0007(6) C51A 0.038(3) 0.028(3) 0.039(3) 0.002(3) -0.002(3) 0.003(3) C52A 0.046(4) 0.066(5) 0.035(3) 0.001(3) -0.007(3) -0.004(3) C53A 0.058(5) 0.074(5) 0.035(4) 0.001(4) -0.014(3) -0.006(4) C54A 0.072(5) 0.064(5) 0.035(4) 0.006(3) -0.001(3) 0.000(4) C55A 0.063(5) 0.059(5) 0.040(4) 0.006(3) 0.004(3) -0.009(4) C56A 0.038(3) 0.048(4) 0.035(3) 0.000(3) -0.003(3) -0.004(3) C61A 0.033(3) 0.040(4) 0.031(3) 0.000(3) -0.007(2) -0.005(3) C62A 0.037(4) 0.051(4) 0.053(4) -0.011(3) -0.002(3) -0.003(3) C63A 0.036(4) 0.073(6) 0.059(4) -0.012(4) 0.009(3) -0.014(4) C64A 0.053(4) 0.061(5) 0.046(4) -0.007(4) -0.005(3) -0.023(4) C65A 0.063(5) 0.041(4) 0.090(6) -0.013(4) -0.001(4) -0.011(4) C66A 0.035(4) 0.043(4) 0.080(5) -0.018(4) 0.005(3) -0.004(3) C71A 0.085(7) 0.092(8) 0.109(9) -0.019(7) 0.023(7) 0.041(6) C72A 0.088(7) 0.119(9) 0.055(5) -0.005(6) -0.006(5) 0.031(7) C73A 0.091(9) 0.136(12) 0.115(10) 0.003(9) 0.013(8) 0.039(8) C74A 0.093(8) 0.089(9) 0.129(11) -0.021(8) -0.012(8) 0.019(7) C75A 0.129(12) 0.094(10) 0.185(17) 0.002(11) 0.053(11) 0.042(9) C76A 0.097(8) 0.077(7) 0.063(6) 0.008(5) 0.013(5) 0.022(6) C77A 0.080(7) 0.151(12) 0.147(11) -0.101(10) -0.010(7) 0.035(7) Rh1B 0.0340(2) 0.0312(2) 0.0301(2) -0.00039(19) -0.00317(17) 0.00377(19) C1B 0.036(3) 0.036(3) 0.036(3) 0.006(3) -0.001(3) 0.002(3) C2B 0.044(4) 0.055(4) 0.042(4) 0.003(3) 0.005(3) 0.014(3) N3B 0.078(5) 0.118(7) 0.054(4) 0.010(4) -0.005(4) 0.054(5) C3B 0.046(4) 0.066(5) 0.032(3) 0.002(3) -0.013(3) 0.015(4) C4B 0.049(4) 0.041(4) 0.050(4) -0.006(3) -0.015(3) 0.005(3) C5B 0.036(4) 0.050(4) 0.051(4) -0.005(3) -0.001(3) 0.009(3) C6B 0.042(4) 0.045(4) 0.040(3) -0.004(3) -0.004(3) 0.016(3) C7B 0.042(4) 0.044(4) 0.045(4) 0.004(3) -0.010(3) 0.008(3) C8B 0.053(4) 0.055(5) 0.043(4) 0.007(3) 0.000(3) 0.004(3) C9B 0.053(4) 0.061(5) 0.047(4) -0.005(4) -0.012(3) 0.016(4) N1B 0.036(3) 0.030(3) 0.030(2) 0.003(2) -0.002(2) -0.003(2) C11B 0.038(3) 0.029(3) 0.030(3) -0.004(2) -0.004(2) 0.003(3) C12B 0.037(3) 0.044(4) 0.041(3) 0.003(3) 0.004(3) -0.004(3) C13B 0.051(4) 0.030(4) 0.053(4) -0.007(3) 0.002(3) -0.011(3) C14B 0.055(4) 0.037(4) 0.047(4) -0.005(3) -0.008(3) 0.006(3) C15B 0.053(4) 0.041(4) 0.048(4) -0.009(3) 0.010(3) 0.006(3) C16B 0.047(4) 0.041(4) 0.045(4) -0.002(3) 0.008(3) -0.001(3) N2B 0.040(3) 0.032(3) 0.037(3) -0.006(2) -0.007(2) 0.003(2) C21B 0.032(3) 0.037(3) 0.032(3) -0.002(3) -0.005(2) 0.004(3) C22B 0.041(4) 0.041(4) 0.049(4) 0.002(3) 0.001(3) 0.005(3) C23B 0.049(4) 0.037(4) 0.100(7) 0.001(4) -0.014(4) -0.008(3) C24B 0.078(6) 0.045(5) 0.080(6) -0.025(4) -0.034(5) 0.016(4) C25B 0.082(6) 0.069(6) 0.056(5) -0.030(4) -0.007(4) 0.013(5) C26B 0.062(4) 0.046(4) 0.042(4) -0.009(3) -0.004(3) 0.003(3) P1B 0.0316(8) 0.0313(8) 0.0273(7) 0.0018(6) 0.0011(6) 0.0005(6) C31B 0.033(3) 0.031(3) 0.031(3) 0.005(2) -0.001(2) 0.001(3) C32B 0.041(4) 0.056(4) 0.035(3) 0.000(3) 0.006(3) -0.009(3) C33B 0.055(4) 0.072(5) 0.033(3) -0.008(3) 0.005(3) -0.003(4) C34B 0.062(5) 0.055(5) 0.029(3) -0.002(3) 0.000(3) 0.006(4) C35B 0.060(4) 0.049(4) 0.038(4) -0.005(3) -0.008(3) -0.012(3) C36B 0.042(4) 0.049(4) 0.038(3) -0.003(3) 0.006(3) -0.005(3) C41B 0.035(3) 0.039(4) 0.030(3) -0.007(3) 0.009(2) -0.001(3) C42B 0.039(4) 0.041(4) 0.065(5) 0.012(3) 0.008(3) -0.002(3) C43B 0.070(5) 0.036(4) 0.088(6) 0.020(4) 0.010(4) -0.008(4) C44B 0.052(5) 0.065(6) 0.074(5) 0.005(4) 0.008(4) -0.028(4) C45B 0.043(4) 0.062(5) 0.056(4) 0.009(4) -0.003(3) -0.014(4) C46B 0.039(4) 0.042(4) 0.053(4) 0.009(3) -0.003(3) 0.001(3) P2B 0.0302(8) 0.0295(8) 0.0311(7) 0.0015(6) 0.0006(6) 0.0026(6) C51B 0.036(3) 0.029(3) 0.034(3) 0.000(3) 0.006(2) -0.001(3) C52B 0.033(3) 0.047(4) 0.045(4) -0.005(3) 0.009(3) -0.002(3) C53B 0.033(4) 0.054(5) 0.070(5) -0.016(4) 0.012(3) -0.011(3) C54B 0.057(5) 0.037(4) 0.085(6) 0.006(4) 0.023(4) -0.007(4) C55B 0.064(5) 0.044(4) 0.060(5) 0.016(4) 0.021(4) 0.010(4) C56B 0.039(3) 0.041(4) 0.045(4) 0.009(3) 0.005(3) 0.001(3) C61B 0.032(3) 0.035(3) 0.036(3) -0.003(3) 0.002(2) -0.002(3) C62B 0.050(4) 0.047(4) 0.058(4) 0.010(3) 0.014(3) 0.011(3) C63B 0.065(5) 0.060(5) 0.070(5) 0.005(4) 0.032(4) 0.027(4) C64B 0.084(6) 0.048(5) 0.087(6) 0.002(4) 0.024(5) 0.036(4) C65B 0.079(6) 0.035(4) 0.075(5) 0.005(4) 0.016(4) 0.013(4) C66B 0.050(4) 0.039(4) 0.053(4) 0.002(3) 0.010(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1A C4A 2.109(6) . ? Rh1A C3A 2.120(6) . ? Rh1A N1A 2.124(5) . ? Rh1A C7A 2.131(6) . ? Rh1A N2A 2.135(5) . ? Rh1A C6A 2.148(6) . ? C1A C2A 1.402(9) . ? C1A P1A 1.741(6) . ? C1A P2A 1.749(6) . ? C2A N3A 1.144(8) . ? C3A C4A 1.383(9) . ? C3A C8A 1.517(9) . ? C4A C5A 1.538(9) . ? C5A C6A 1.517(9) . ? C5A C9A 1.518(9) . ? C6A C7A 1.390(10) . ? C7A C8A 1.520(10) . ? C8A C9A 1.539(10) . ? N1A C11A 1.418(7) . ? N1A P1A 1.603(5) . ? C11A C12A 1.383(8) . ? C11A C16A 1.396(8) . ? C12A C13A 1.407(10) . ? C13A C14A 1.376(10) . ? C14A C15A 1.361(10) . ? C15A C16A 1.379(9) . ? N2A C21A 1.429(7) . ? N2A P2A 1.599(5) . ? C21A C22A 1.389(8) . ? C21A C26A 1.392(8) . ? C22A C23A 1.389(10) . ? C23A C24A 1.386(12) . ? C24A C25A 1.373(11) . ? C25A C26A 1.361(9) . ? P1A C41A 1.806(6) . ? P1A C31A 1.816(6) . ? C31A C32A 1.380(8) . ? C31A C36A 1.404(8) . ? C32A C33A 1.394(9) . ? C33A C34A 1.377(10) . ? C34A C35A 1.370(10) . ? C35A C36A 1.387(9) . ? C41A C46A 1.391(8) . ? C41A C42A 1.394(9) . ? C42A C43A 1.378(9) . ? C43A C44A 1.385(10) . ? C44A C45A 1.360(10) . ? C45A C46A 1.387(9) . ? P2A C61A 1.808(6) . ? P2A C51A 1.811(6) . ? C51A C56A 1.385(9) . ? C51A C52A 1.396(8) . ? C52A C53A 1.389(9) . ? C53A C54A 1.373(10) . ? C54A C55A 1.370(10) . ? C55A C56A 1.369(9) . ? C61A C62A 1.374(9) . ? C61A C66A 1.394(9) . ? C62A C63A 1.378(9) . ? C63A C64A 1.363(10) . ? C64A C65A 1.361(11) . ? C65A C66A 1.377(10) . ? C71A C76A 1.338(14) . ? C71A C77A 1.390(15) . ? C71A C72A 1.420(14) . ? C72A C73A 1.311(15) . ? C73A C74A 1.476(17) . ? C74A C75A 1.305(18) . ? C75A C76A 1.419(17) . ? Rh1B N2B 2.106(5) . ? Rh1B C7B 2.114(6) . ? Rh1B C4B 2.124(6) . ? Rh1B C3B 2.127(6) . ? Rh1B C6B 2.132(6) . ? Rh1B N1B 2.132(5) . ? C1B C2B 1.394(9) . ? C1B P1B 1.740(6) . ? C1B P2B 1.742(6) . ? C2B N3B 1.168(8) . ? C3B C4B 1.381(10) . ? C3B C8B 1.533(10) . ? C4B C5B 1.524(9) . ? C5B C6B 1.528(9) . ? C5B C9B 1.532(10) . ? C6B C7B 1.392(9) . ? C7B C8B 1.534(9) . ? C8B C9B 1.541(9) . ? N1B C11B 1.402(7) . ? N1B P1B 1.624(5) . ? C11B C16B 1.388(8) . ? C11B C12B 1.390(8) . ? C12B C13B 1.373(9) . ? C13B C14B 1.367(9) . ? C14B C15B 1.369(9) . ? C15B C16B 1.377(9) . ? N2B C21B 1.411(7) . ? N2B P2B 1.612(5) . ? C21B C22B 1.363(9) . ? C21B C26B 1.399(9) . ? C22B C23B 1.409(10) . ? C23B C24B 1.369(12) . ? C24B C25B 1.366(12) . ? C25B C26B 1.372(10) . ? P1B C31B 1.794(6) . ? P1B C41B 1.809(6) . ? C31B C36B 1.389(8) . ? C31B C32B 1.397(8) . ? C32B C33B 1.395(9) . ? C33B C34B 1.366(10) . ? C34B C35B 1.385(9) . ? C35B C36B 1.381(9) . ? C41B C42B 1.379(9) . ? C41B C46B 1.395(8) . ? C42B C43B 1.387(10) . ? C43B C44B 1.378(11) . ? C44B C45B 1.360(11) . ? C45B C46B 1.376(9) . ? P2B C61B 1.800(6) . ? P2B C51B 1.813(6) . ? C51B C56B 1.377(8) . ? C51B C52B 1.412(8) . ? C52B C53B 1.371(9) . ? C53B C54B 1.363(11) . ? C54B C55B 1.376(11) . ? C55B C56B 1.384(9) . ? C61B C62B 1.378(9) . ? C61B C66B 1.388(9) . ? C62B C63B 1.370(10) . ? C63B C64B 1.385(11) . ? C64B C65B 1.397(11) . ? C65B C66B 1.370(10) . ? C71B C72B 1.3900 . ? C71B C76B 1.3900 . ? C71B C77B 1.426(19) . ? C72B C73B 1.3900 . ? C73B C74B 1.3900 . ? C74B C75B 1.3900 . ? C75B C76B 1.3900 . ? C71C C72C 1.3900 . ? C71C C76C 1.3900 . ? C71C C77C 1.428(19) . ? C72C C73C 1.3900 . ? C73C C74C 1.3900 . ? C74C C75C 1.3900 . ? C75C C76C 1.3900 . ? 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 C4A Rh1A C3A 38.2(2) . . ? C4A Rh1A N1A 153.4(2) . . ? C3A Rh1A N1A 163.8(2) . . ? C4A Rh1A C7A 80.0(3) . . ? C3A Rh1A C7A 66.8(3) . . ? N1A Rh1A C7A 100.5(2) . . ? C4A Rh1A N2A 99.2(2) . . ? C3A Rh1A N2A 95.6(2) . . ? N1A Rh1A N2A 92.20(18) . . ? C7A Rh1A N2A 152.7(2) . . ? C4A Rh1A C6A 67.2(2) . . ? C3A Rh1A C6A 79.5(2) . . ? N1A Rh1A C6A 96.7(2) . . ? C7A Rh1A C6A 37.9(3) . . ? N2A Rh1A C6A 163.6(2) . . ? C2A C1A P1A 122.4(4) . . ? C2A C1A P2A 121.8(4) . . ? P1A C1A P2A 115.8(3) . . ? N3A C2A C1A 178.0(7) . . ? C4A C3A C8A 106.6(6) . . ? C4A C3A Rh1A 70.5(4) . . ? C8A C3A Rh1A 96.4(4) . . ? C3A C4A C5A 106.1(6) . . ? C3A C4A Rh1A 71.3(4) . . ? C5A C4A Rh1A 96.3(4) . . ? C6A C5A C9A 100.6(5) . . ? C6A C5A C4A 101.0(5) . . ? C9A C5A C4A 100.1(5) . . ? C7A C6A C5A 106.9(6) . . ? C7A C6A Rh1A 70.4(4) . . ? C5A C6A Rh1A 95.4(4) . . ? C6A C7A C8A 105.7(6) . . ? C6A C7A Rh1A 71.7(4) . . ? C8A C7A Rh1A 95.8(4) . . ? C3A C8A C7A 100.9(5) . . ? C3A C8A C9A 100.1(5) . . ? C7A C8A C9A 101.1(6) . . ? C5A C9A C8A 94.4(5) . . ? C11A N1A P1A 123.5(4) . . ? C11A N1A Rh1A 118.8(3) . . ? P1A N1A Rh1A 117.7(3) . . ? C12A C11A C16A 117.9(6) . . ? C12A C11A N1A 120.3(5) . . ? C16A C11A N1A 121.7(5) . . ? C11A C12A C13A 120.8(6) . . ? C14A C13A C12A 119.2(7) . . ? C15A C14A C13A 120.8(7) . . ? C14A C15A C16A 120.1(7) . . ? C15A C16A C11A 121.2(6) . . ? C21A N2A P2A 122.3(4) . . ? C21A N2A Rh1A 119.7(4) . . ? P2A N2A Rh1A 118.0(3) . . ? C22A C21A C26A 118.0(6) . . ? C22A C21A N2A 121.6(6) . . ? C26A C21A N2A 120.4(5) . . ? C23A C22A C21A 120.2(7) . . ? C24A C23A C22A 120.5(7) . . ? C25A C24A C23A 118.9(7) . . ? C26A C25A C24A 120.9(7) . . ? C25A C26A C21A 121.5(6) . . ? N1A P1A C1A 111.6(3) . . ? N1A P1A C41A 113.8(3) . . ? C1A P1A C41A 107.1(3) . . ? N1A P1A C31A 107.7(3) . . ? C1A P1A C31A 109.8(3) . . ? C41A P1A C31A 106.7(3) . . ? C32A C31A C36A 118.8(6) . . ? C32A C31A P1A 121.6(5) . . ? C36A C31A P1A 119.5(5) . . ? C31A C32A C33A 120.8(6) . . ? C34A C33A C32A 119.5(6) . . ? C35A C34A C33A 120.5(7) . . ? C34A C35A C36A 120.4(7) . . ? C35A C36A C31A 119.8(6) . . ? C46A C41A C42A 118.7(6) . . ? C46A C41A P1A 122.2(5) . . ? C42A C41A P1A 119.1(4) . . ? C43A C42A C41A 120.8(6) . . ? C42A C43A C44A 119.8(7) . . ? C45A C44A C43A 119.9(7) . . ? C44A C45A C46A 121.2(7) . . ? C45A C46A C41A 119.7(7) . . ? N2A P2A C1A 110.9(3) . . ? N2A P2A C61A 108.3(3) . . ? C1A P2A C61A 110.6(3) . . ? N2A P2A C51A 113.0(3) . . ? C1A P2A C51A 108.1(3) . . ? C61A P2A C51A 105.8(3) . . ? C56A C51A C52A 118.8(6) . . ? C56A C51A P2A 119.3(4) . . ? C52A C51A P2A 121.7(5) . . ? C53A C52A C51A 119.9(7) . . ? C54A C53A C52A 120.0(6) . . ? C55A C54A C53A 120.0(7) . . ? C56A C55A C54A 120.8(7) . . ? C55A C56A C51A 120.5(6) . . ? C62A C61A C66A 118.5(6) . . ? C62A C61A P2A 121.5(5) . . ? C66A C61A P2A 119.9(5) . . ? C61A C62A C63A 121.1(7) . . ? C64A C63A C62A 120.3(7) . . ? C65A C64A C63A 119.1(7) . . ? C64A C65A C66A 121.9(7) . . ? C65A C66A C61A 119.1(7) . . ? C76A C71A C77A 123.4(13) . . ? C76A C71A C72A 117.5(12) . . ? C77A C71A C72A 118.9(13) . . ? C73A C72A C71A 119.3(13) . . ? C72A C73A C74A 126.0(13) . . ? C75A C74A C73A 110.1(13) . . ? C74A C75A C76A 127.2(15) . . ? C71A C76A C75A 119.8(12) . . ? N2B Rh1B C7B 152.1(2) . . ? N2B Rh1B C4B 99.7(2) . . ? C7B Rh1B C4B 80.0(3) . . ? N2B Rh1B C3B 95.1(2) . . ? C7B Rh1B C3B 67.4(3) . . ? C4B Rh1B C3B 37.9(3) . . ? N2B Rh1B C6B 164.3(2) . . ? C7B Rh1B C6B 38.3(3) . . ? C4B Rh1B C6B 67.4(3) . . ? C3B Rh1B C6B 80.3(3) . . ? N2B Rh1B N1B 91.85(18) . . ? C7B Rh1B N1B 100.6(2) . . ? C4B Rh1B N1B 153.6(2) . . ? C3B Rh1B N1B 164.3(2) . . ? C6B Rh1B N1B 96.5(2) . . ? C2B C1B P1B 123.0(5) . . ? C2B C1B P2B 121.9(5) . . ? P1B C1B P2B 115.0(3) . . ? N3B C2B C1B 179.4(9) . . ? C4B C3B C8B 106.3(6) . . ? C4B C3B Rh1B 70.9(4) . . ? C8B C3B Rh1B 95.9(4) . . ? C3B C4B C5B 106.7(6) . . ? C3B C4B Rh1B 71.2(4) . . ? C5B C4B Rh1B 95.8(4) . . ? C4B C5B C6B 101.4(5) . . ? C4B C5B C9B 100.9(6) . . ? C6B C5B C9B 100.6(6) . . ? C7B C6B C5B 105.9(6) . . ? C7B C6B Rh1B 70.1(4) . . ? C5B C6B Rh1B 95.3(4) . . ? C6B C7B C8B 106.6(6) . . ? C6B C7B Rh1B 71.6(4) . . ? C8B C7B Rh1B 96.4(4) . . ? C3B C8B C7B 100.2(5) . . ? C3B C8B C9B 100.6(6) . . ? C7B C8B C9B 100.2(5) . . ? C5B C9B C8B 94.1(5) . . ? C11B N1B P1B 122.1(4) . . ? C11B N1B Rh1B 117.5(3) . . ? P1B N1B Rh1B 118.9(3) . . ? C16B C11B C12B 117.7(6) . . ? C16B C11B N1B 122.6(6) . . ? C12B C11B N1B 119.7(5) . . ? C13B C12B C11B 120.3(6) . . ? C14B C13B C12B 121.3(6) . . ? C13B C14B C15B 119.1(6) . . ? C14B C15B C16B 120.3(6) . . ? C15B C16B C11B 121.1(6) . . ? C21B N2B P2B 122.5(4) . . ? C21B N2B Rh1B 119.2(4) . . ? P2B N2B Rh1B 117.4(3) . . ? C22B C21B C26B 117.6(6) . . ? C22B C21B N2B 121.8(6) . . ? C26B C21B N2B 120.5(6) . . ? C21B C22B C23B 121.0(7) . . ? C24B C23B C22B 120.5(7) . . ? C25B C24B C23B 118.4(7) . . ? C24B C25B C26B 121.7(8) . . ? C25B C26B C21B 120.8(7) . . ? N1B P1B C1B 109.9(3) . . ? N1B P1B C31B 110.9(3) . . ? C1B P1B C31B 108.6(3) . . ? N1B P1B C41B 110.4(3) . . ? C1B P1B C41B 110.3(3) . . ? C31B P1B C41B 106.7(3) . . ? C36B C31B C32B 119.1(6) . . ? C36B C31B P1B 119.4(4) . . ? C32B C31B P1B 121.2(5) . . ? C33B C32B C31B 119.6(6) . . ? C34B C33B C32B 120.7(6) . . ? C33B C34B C35B 119.9(6) . . ? C36B C35B C34B 120.3(6) . . ? C35B C36B C31B 120.4(6) . . ? C42B C41B C46B 118.7(6) . . ? C42B C41B P1B 120.3(5) . . ? C46B C41B P1B 121.0(5) . . ? C41B C42B C43B 120.4(6) . . ? C44B C43B C42B 120.0(7) . . ? C45B C44B C43B 119.8(7) . . ? C44B C45B C46B 120.9(7) . . ? C45B C46B C41B 120.2(6) . . ? N2B P2B C1B 113.0(3) . . ? N2B P2B C61B 110.5(3) . . ? C1B P2B C61B 109.3(3) . . ? N2B P2B C51B 106.9(3) . . ? C1B P2B C51B 110.2(3) . . ? C61B P2B C51B 106.7(3) . . ? C56B C51B C52B 118.0(6) . . ? C56B C51B P2B 121.8(5) . . ? C52B C51B P2B 120.1(5) . . ? C53B C52B C51B 120.2(6) . . ? C54B C53B C52B 120.7(7) . . ? C53B C54B C55B 120.2(7) . . ? C54B C55B C56B 119.7(7) . . ? C51B C56B C55B 121.1(7) . . ? C62B C61B C66B 118.5(6) . . ? C62B C61B P2B 121.8(5) . . ? C66B C61B P2B 119.1(5) . . ? C63B C62B C61B 121.4(7) . . ? C62B C63B C64B 120.0(7) . . ? C63B C64B C65B 119.2(7) . . ? C66B C65B C64B 119.8(7) . . ? C65B C66B C61B 121.0(7) . . ? C72B C71B C76B 120.0 . . ? C72B C71B C77B 120.0(8) . . ? C76B C71B C77B 119.8(8) . . ? C73B C72B C71B 120.0 . . ? C72B C73B C74B 120.0 . . ? C75B C74B C73B 120.0 . . ? C74B C75B C76B 120.0 . . ? C75B C76B C71B 120.0 . . ? C72C C71C C76C 120.0 . . ? C72C C71C C77C 122.6(7) . . ? C76C C71C C77C 117.1(7) . . ? C73C C72C C71C 120.0 . . ? C72C C73C C74C 120.0 . . ? C75C C74C C73C 120.0 . . ? C76C C75C C74C 120.0 . . ? C75C C76C C71C 120.0 . . ? 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 N1A Rh1A C3A C4A -143.9(7) . . . . ? C7A Rh1A C3A C4A -103.9(4) . . . . ? N2A Rh1A C3A C4A 97.8(4) . . . . ? C6A Rh1A C3A C4A -66.4(4) . . . . ? C4A Rh1A C3A C8A 105.4(6) . . . . ? N1A Rh1A C3A C8A -38.5(10) . . . . ? C7A Rh1A C3A C8A 1.6(4) . . . . ? N2A Rh1A C3A C8A -156.8(4) . . . . ? C6A Rh1A C3A C8A 39.1(4) . . . . ? C8A C3A C4A C5A 0.3(7) . . . . ? Rh1A C3A C4A C5A 91.3(4) . . . . ? C8A C3A C4A Rh1A -91.0(5) . . . . ? N1A Rh1A C4A C3A 158.5(4) . . . . ? C7A Rh1A C4A C3A 65.0(4) . . . . ? N2A Rh1A C4A C3A -87.3(4) . . . . ? C6A Rh1A C4A C3A 102.4(4) . . . . ? C3A Rh1A C4A C5A -104.9(6) . . . . ? N1A Rh1A C4A C5A 53.6(7) . . . . ? C7A Rh1A C4A C5A -39.9(4) . . . . ? N2A Rh1A C4A C5A 167.8(4) . . . . ? C6A Rh1A C4A C5A -2.5(4) . . . . ? C3A C4A C5A C6A -69.0(6) . . . . ? Rh1A C4A C5A C6A 3.3(5) . . . . ? C3A C4A C5A C9A 34.0(6) . . . . ? Rh1A C4A C5A C9A 106.4(4) . . . . ? C9A C5A C6A C7A -34.7(6) . . . . ? C4A C5A C6A C7A 67.8(6) . . . . ? C9A C5A C6A Rh1A -105.9(4) . . . . ? C4A C5A C6A Rh1A -3.3(5) . . . . ? C4A Rh1A C6A C7A -103.5(4) . . . . ? C3A Rh1A C6A C7A -65.6(4) . . . . ? N1A Rh1A C6A C7A 98.5(4) . . . . ? N2A Rh1A C6A C7A -139.3(7) . . . . ? C4A Rh1A C6A C5A 2.5(4) . . . . ? C3A Rh1A C6A C5A 40.4(4) . . . . ? N1A Rh1A C6A C5A -155.5(4) . . . . ? C7A Rh1A C6A C5A 106.1(6) . . . . ? N2A Rh1A C6A C5A -33.3(10) . . . . ? C5A C6A C7A C8A 1.3(7) . . . . ? Rh1A C6A C7A C8A 91.0(5) . . . . ? C5A C6A C7A Rh1A -89.8(4) . . . . ? C4A Rh1A C7A C6A 65.5(4) . . . . ? C3A Rh1A C7A C6A 103.1(4) . . . . ? N1A Rh1A C7A C6A -87.4(4) . . . . ? N2A Rh1A C7A C6A 156.3(5) . . . . ? C4A Rh1A C7A C8A -39.1(4) . . . . ? C3A Rh1A C7A C8A -1.6(4) . . . . ? N1A Rh1A C7A C8A 167.9(4) . . . . ? N2A Rh1A C7A C8A 51.7(7) . . . . ? C6A Rh1A C7A C8A -104.7(6) . . . . ? C4A C3A C8A C7A 69.4(6) . . . . ? Rh1A C3A C8A C7A -2.1(5) . . . . ? C4A C3A C8A C9A -34.0(7) . . . . ? Rh1A C3A C8A C9A -105.5(5) . . . . ? C6A C7A C8A C3A -70.5(6) . . . . ? Rh1A C7A C8A C3A 2.1(5) . . . . ? C6A C7A C8A C9A 32.1(7) . . . . ? Rh1A C7A C8A C9A 104.7(5) . . . . ? C6A C5A C9A C8A 51.3(6) . . . . ? C4A C5A C9A C8A -52.0(6) . . . . ? C3A C8A C9A C5A 52.4(6) . . . . ? C7A C8A C9A C5A -50.9(6) . . . . ? C4A Rh1A N1A C11A -94.7(6) . . . . ? C3A Rh1A N1A C11A 30.9(10) . . . . ? C7A Rh1A N1A C11A -6.1(5) . . . . ? N2A Rh1A N1A C11A 149.6(4) . . . . ? C6A Rh1A N1A C11A -44.3(5) . . . . ? C4A Rh1A N1A P1A 85.2(6) . . . . ? C3A Rh1A N1A P1A -149.2(7) . . . . ? C7A Rh1A N1A P1A 173.8(3) . . . . ? N2A Rh1A N1A P1A -30.5(3) . . . . ? C6A Rh1A N1A P1A 135.6(3) . . . . ? P1A N1A C11A C12A 111.6(6) . . . . ? Rh1A N1A C11A C12A -68.5(7) . . . . ? P1A N1A C11A C16A -71.8(7) . . . . ? Rh1A N1A C11A C16A 108.1(6) . . . . ? C16A C11A C12A C13A 0.4(9) . . . . ? N1A C11A C12A C13A 177.2(6) . . . . ? C11A C12A C13A C14A -0.5(11) . . . . ? C12A C13A C14A C15A 0.5(12) . . . . ? C13A C14A C15A C16A -0.4(12) . . . . ? C14A C15A C16A C11A 0.3(11) . . . . ? C12A C11A C16A C15A -0.3(10) . . . . ? N1A C11A C16A C15A -177.0(6) . . . . ? C4A Rh1A N2A C21A -10.9(4) . . . . ? C3A Rh1A N2A C21A -49.3(4) . . . . ? N1A Rh1A N2A C21A 144.9(4) . . . . ? C7A Rh1A N2A C21A -97.0(6) . . . . ? C6A Rh1A N2A C21A 22.2(10) . . . . ? C4A Rh1A N2A P2A 167.8(3) . . . . ? C3A Rh1A N2A P2A 129.4(3) . . . . ? N1A Rh1A N2A P2A -36.3(3) . . . . ? C7A Rh1A N2A P2A 81.7(6) . . . . ? C6A Rh1A N2A P2A -159.1(7) . . . . ? P2A N2A C21A C22A -61.5(7) . . . . ? Rh1A N2A C21A C22A 117.2(6) . . . . ? P2A N2A C21A C26A 119.0(6) . . . . ? Rh1A N2A C21A C26A -62.3(7) . . . . ? C26A C21A C22A C23A -2.6(10) . . . . ? N2A C21A C22A C23A 177.8(7) . . . . ? C21A C22A C23A C24A 1.8(13) . . . . ? C22A C23A C24A C25A -0.2(14) . . . . ? C23A C24A C25A C26A -0.5(14) . . . . ? C24A C25A C26A C21A -0.5(12) . . . . ? C22A C21A C26A C25A 2.0(10) . . . . ? N2A C21A C26A C25A -178.5(6) . . . . ? C11A N1A P1A C1A -113.0(5) . . . . ? Rh1A N1A P1A C1A 67.2(4) . . . . ? C11A N1A P1A C41A 8.4(6) . . . . ? Rh1A N1A P1A C41A -171.4(3) . . . . ? C11A N1A P1A C31A 126.5(5) . . . . ? Rh1A N1A P1A C31A -53.4(3) . . . . ? C2A C1A P1A N1A 146.3(5) . . . . ? P2A C1A P1A N1A -36.5(5) . . . . ? C2A C1A P1A C41A 21.1(6) . . . . ? P2A C1A P1A C41A -161.7(3) . . . . ? C2A C1A P1A C31A -94.3(6) . . . . ? P2A C1A P1A C31A 82.8(4) . . . . ? N1A P1A C31A C32A -24.4(5) . . . . ? C1A P1A C31A C32A -146.1(5) . . . . ? C41A P1A C31A C32A 98.1(5) . . . . ? N1A P1A C31A C36A 153.7(5) . . . . ? C1A P1A C31A C36A 32.0(5) . . . . ? C41A P1A C31A C36A -83.8(5) . . . . ? C36A C31A C32A C33A -1.7(9) . . . . ? P1A C31A C32A C33A 176.4(5) . . . . ? C31A C32A C33A C34A -0.6(10) . . . . ? C32A C33A C34A C35A 2.5(10) . . . . ? C33A C34A C35A C36A -2.1(10) . . . . ? C34A C35A C36A C31A -0.2(10) . . . . ? C32A C31A C36A C35A 2.1(9) . . . . ? P1A C31A C36A C35A -176.0(5) . . . . ? N1A P1A C41A C46A 100.3(6) . . . . ? C1A P1A C41A C46A -135.9(5) . . . . ? C31A P1A C41A C46A -18.4(6) . . . . ? N1A P1A C41A C42A -78.7(6) . . . . ? C1A P1A C41A C42A 45.1(6) . . . . ? C31A P1A C41A C42A 162.6(5) . . . . ? C46A C41A C42A C43A 1.2(10) . . . . ? P1A C41A C42A C43A -179.7(6) . . . . ? C41A C42A C43A C44A -1.3(11) . . . . ? C42A C43A C44A C45A 0.3(12) . . . . ? C43A C44A C45A C46A 0.6(12) . . . . ? C44A C45A C46A C41A -0.6(11) . . . . ? C42A C41A C46A C45A -0.3(10) . . . . ? P1A C41A C46A C45A -179.3(5) . . . . ? C21A N2A P2A C1A -114.2(5) . . . . ? Rh1A N2A P2A C1A 67.1(4) . . . . ? C21A N2A P2A C61A 124.2(5) . . . . ? Rh1A N2A P2A C61A -54.4(3) . . . . ? C21A N2A P2A C51A 7.3(5) . . . . ? Rh1A N2A P2A C51A -171.4(3) . . . . ? C2A C1A P2A N2A 147.9(5) . . . . ? P1A C1A P2A N2A -29.2(4) . . . . ? C2A C1A P2A C61A -91.8(6) . . . . ? P1A C1A P2A C61A 91.0(4) . . . . ? C2A C1A P2A C51A 23.5(6) . . . . ? P1A C1A P2A C51A -153.6(3) . . . . ? N2A P2A C51A C56A -70.0(6) . . . . ? C1A P2A C51A C56A 53.1(6) . . . . ? C61A P2A C51A C56A 171.6(5) . . . . ? N2A P2A C51A C52A 105.1(6) . . . . ? C1A P2A C51A C52A -131.9(6) . . . . ? C61A P2A C51A C52A -13.4(6) . . . . ? C56A C51A C52A C53A 1.6(10) . . . . ? P2A C51A C52A C53A -173.5(6) . . . . ? C51A C52A C53A C54A -1.0(12) . . . . ? C52A C53A C54A C55A 0.0(12) . . . . ? C53A C54A C55A C56A 0.4(12) . . . . ? C54A C55A C56A C51A 0.2(11) . . . . ? C52A C51A C56A C55A -1.2(10) . . . . ? P2A C51A C56A C55A 174.0(5) . . . . ? N2A P2A C61A C62A -25.2(6) . . . . ? C1A P2A C61A C62A -146.9(5) . . . . ? C51A P2A C61A C62A 96.3(5) . . . . ? N2A P2A C61A C66A 158.1(5) . . . . ? C1A P2A C61A C66A 36.4(6) . . . . ? C51A P2A C61A C66A -80.4(6) . . . . ? C66A C61A C62A C63A 1.3(10) . . . . ? P2A C61A C62A C63A -175.5(5) . . . . ? C61A C62A C63A C64A 0.1(11) . . . . ? C62A C63A C64A C65A -1.2(12) . . . . ? C63A C64A C65A C66A 1.1(12) . . . . ? C64A C65A C66A C61A 0.3(13) . . . . ? C62A C61A C66A C65A -1.4(11) . . . . ? P2A C61A C66A C65A 175.3(6) . . . . ? C76A C71A C72A C73A 3.1(15) . . . . ? C77A C71A C72A C73A 178.2(10) . . . . ? C71A C72A C73A C74A -2.9(18) . . . . ? C72A C73A C74A C75A 0.6(18) . . . . ? C73A C74A C75A C76A 1.7(18) . . . . ? C77A C71A C76A C75A -176.0(10) . . . . ? C72A C71A C76A C75A -1.1(14) . . . . ? C74A C75A C76A C71A -1.4(19) . . . . ? N2B Rh1B C3B C4B 99.3(4) . . . . ? C7B Rh1B C3B C4B -103.2(5) . . . . ? C6B Rh1B C3B C4B -65.5(4) . . . . ? N1B Rh1B C3B C4B -144.8(7) . . . . ? N2B Rh1B C3B C8B -155.5(4) . . . . ? C7B Rh1B C3B C8B 2.0(4) . . . . ? C4B Rh1B C3B C8B 105.2(6) . . . . ? C6B Rh1B C3B C8B 39.7(4) . . . . ? N1B Rh1B C3B C8B -39.6(11) . . . . ? C8B C3B C4B C5B -0.2(7) . . . . ? Rh1B C3B C4B C5B 90.6(4) . . . . ? C8B C3B C4B Rh1B -90.7(4) . . . . ? N2B Rh1B C4B C3B -85.8(4) . . . . ? C7B Rh1B C4B C3B 65.9(4) . . . . ? C6B Rh1B C4B C3B 103.7(5) . . . . ? N1B Rh1B C4B C3B 159.5(5) . . . . ? N2B Rh1B C4B C5B 168.5(4) . . . . ? C7B Rh1B C4B C5B -39.8(4) . . . . ? C3B Rh1B C4B C5B -105.7(6) . . . . ? C6B Rh1B C4B C5B -2.0(4) . . . . ? N1B Rh1B C4B C5B 53.7(7) . . . . ? C3B C4B C5B C6B -69.4(6) . . . . ? Rh1B C4B C5B C6B 2.7(5) . . . . ? C3B C4B C5B C9B 33.9(6) . . . . ? Rh1B C4B C5B C9B 105.9(5) . . . . ? C4B C5B C6B C7B 68.2(6) . . . . ? C9B C5B C6B C7B -35.3(6) . . . . ? C4B C5B C6B Rh1B -2.7(5) . . . . ? C9B C5B C6B Rh1B -106.1(4) . . . . ? N2B Rh1B C6B C7B -139.6(8) . . . . ? C4B Rh1B C6B C7B -102.9(4) . . . . ? C3B Rh1B C6B C7B -65.6(4) . . . . ? N1B Rh1B C6B C7B 98.8(4) . . . . ? N2B Rh1B C6B C5B -34.6(11) . . . . ? C7B Rh1B C6B C5B 104.9(6) . . . . ? C4B Rh1B C6B C5B 2.0(4) . . . . ? C3B Rh1B C6B C5B 39.3(4) . . . . ? N1B Rh1B C6B C5B -156.2(4) . . . . ? C5B C6B C7B C8B 1.3(7) . . . . ? Rh1B C6B C7B C8B 91.4(5) . . . . ? C5B C6B C7B Rh1B -90.0(4) . . . . ? N2B Rh1B C7B C6B 157.9(4) . . . . ? C4B Rh1B C7B C6B 66.0(4) . . . . ? C3B Rh1B C7B C6B 103.4(4) . . . . ? N1B Rh1B C7B C6B -87.1(4) . . . . ? N2B Rh1B C7B C8B 52.5(7) . . . . ? C4B Rh1B C7B C8B -39.4(4) . . . . ? C3B Rh1B C7B C8B -2.0(4) . . . . ? C6B Rh1B C7B C8B -105.4(6) . . . . ? N1B Rh1B C7B C8B 167.4(4) . . . . ? C4B C3B C8B C7B 69.2(6) . . . . ? Rh1B C3B C8B C7B -2.6(5) . . . . ? C4B C3B C8B C9B -33.3(6) . . . . ? Rh1B C3B C8B C9B -105.1(5) . . . . ? C6B C7B C8B C3B -70.0(6) . . . . ? Rh1B C7B C8B C3B 2.6(5) . . . . ? C6B C7B C8B C9B 32.8(7) . . . . ? Rh1B C7B C8B C9B 105.4(5) . . . . ? C4B C5B C9B C8B -51.2(6) . . . . ? C6B C5B C9B C8B 52.6(6) . . . . ? C3B C8B C9B C5B 51.0(6) . . . . ? C7B C8B C9B C5B -51.5(6) . . . . ? N2B Rh1B N1B C11B 155.7(4) . . . . ? C7B Rh1B N1B C11B 0.8(5) . . . . ? C4B Rh1B N1B C11B -87.9(6) . . . . ? C3B Rh1B N1B C11B 39.4(10) . . . . ? C6B Rh1B N1B C11B -37.7(4) . . . . ? N2B Rh1B N1B P1B -38.1(3) . . . . ? C7B Rh1B N1B P1B 167.0(3) . . . . ? C4B Rh1B N1B P1B 78.4(6) . . . . ? C3B Rh1B N1B P1B -154.4(7) . . . . ? C6B Rh1B N1B P1B 128.5(3) . . . . ? P1B N1B C11B C16B -67.5(7) . . . . ? Rh1B N1B C11B C16B 98.3(6) . . . . ? P1B N1B C11B C12B 115.3(5) . . . . ? Rh1B N1B C11B C12B -78.9(6) . . . . ? C16B C11B C12B C13B 1.0(9) . . . . ? N1B C11B C12B C13B 178.3(6) . . . . ? C11B C12B C13B C14B -0.6(10) . . . . ? C12B C13B C14B C15B -0.6(10) . . . . ? C13B C14B C15B C16B 1.3(10) . . . . ? C14B C15B C16B C11B -0.9(10) . . . . ? C12B C11B C16B C15B -0.3(9) . . . . ? N1B C11B C16B C15B -177.5(6) . . . . ? C7B Rh1B N2B C21B -102.3(6) . . . . ? C4B Rh1B N2B C21B -15.3(5) . . . . ? C3B Rh1B N2B C21B -53.3(5) . . . . ? C6B Rh1B N2B C21B 18.7(11) . . . . ? N1B Rh1B N2B C21B 140.8(4) . . . . ? C7B Rh1B N2B P2B 88.3(5) . . . . ? C4B Rh1B N2B P2B 175.3(3) . . . . ? C3B Rh1B N2B P2B 137.3(3) . . . . ? C6B Rh1B N2B P2B -150.7(7) . . . . ? N1B Rh1B N2B P2B -28.5(3) . . . . ? P2B N2B C21B C22B 104.8(6) . . . . ? Rh1B N2B C21B C22B -64.0(7) . . . . ? P2B N2B C21B C26B -77.8(7) . . . . ? Rh1B N2B C21B C26B 113.3(6) . . . . ? C26B C21B C22B C23B -0.5(9) . . . . ? N2B C21B C22B C23B 176.9(6) . . . . ? C21B C22B C23B C24B 0.5(11) . . . . ? C22B C23B C24B C25B -0.3(12) . . . . ? C23B C24B C25B C26B 0.1(12) . . . . ? C24B C25B C26B C21B -0.2(12) . . . . ? C22B C21B C26B C25B 0.4(10) . . . . ? N2B C21B C26B C25B -177.1(6) . . . . ? C11B N1B P1B C1B -126.7(5) . . . . ? Rh1B N1B P1B C1B 67.7(3) . . . . ? C11B N1B P1B C31B -6.6(5) . . . . ? Rh1B N1B P1B C31B -172.2(3) . . . . ? C11B N1B P1B C41B 111.4(5) . . . . ? Rh1B N1B P1B C41B -54.2(3) . . . . ? C2B C1B P1B N1B 152.6(6) . . . . ? P2B C1B P1B N1B -27.6(4) . . . . ? C2B C1B P1B C31B 31.1(7) . . . . ? P2B C1B P1B C31B -149.1(3) . . . . ? C2B C1B P1B C41B -85.4(6) . . . . ? P2B C1B P1B C41B 94.4(4) . . . . ? N1B P1B C31B C36B -69.5(5) . . . . ? C1B P1B C31B C36B 51.4(6) . . . . ? C41B P1B C31B C36B 170.2(5) . . . . ? N1B P1B C31B C32B 104.2(5) . . . . ? C1B P1B C31B C32B -134.9(5) . . . . ? C41B P1B C31B C32B -16.1(6) . . . . ? C36B C31B C32B C33B 0.8(10) . . . . ? P1B C31B C32B C33B -172.9(5) . . . . ? C31B C32B C33B C34B -0.9(11) . . . . ? C32B C33B C34B C35B -0.7(11) . . . . ? C33B C34B C35B C36B 2.3(11) . . . . ? C34B C35B C36B C31B -2.3(11) . . . . ? C32B C31B C36B C35B 0.7(10) . . . . ? P1B C31B C36B C35B 174.6(5) . . . . ? N1B P1B C41B C42B 162.4(5) . . . . ? C1B P1B C41B C42B 40.7(6) . . . . ? C31B P1B C41B C42B -77.0(6) . . . . ? N1B P1B C41B C46B -17.7(6) . . . . ? C1B P1B C41B C46B -139.4(5) . . . . ? C31B P1B C41B C46B 102.9(5) . . . . ? C46B C41B C42B C43B 0.7(10) . . . . ? P1B C41B C42B C43B -179.5(6) . . . . ? C41B C42B C43B C44B -1.0(12) . . . . ? C42B C43B C44B C45B 0.5(13) . . . . ? C43B C44B C45B C46B 0.3(12) . . . . ? C44B C45B C46B C41B -0.6(11) . . . . ? C42B C41B C46B C45B 0.1(10) . . . . ? P1B C41B C46B C45B -179.7(5) . . . . ? C21B N2B P2B C1B -101.7(5) . . . . ? Rh1B N2B P2B C1B 67.3(4) . . . . ? C21B N2B P2B C61B 21.1(6) . . . . ? Rh1B N2B P2B C61B -169.9(3) . . . . ? C21B N2B P2B C51B 136.9(5) . . . . ? Rh1B N2B P2B C51B -54.1(4) . . . . ? C2B C1B P2B N2B 142.0(6) . . . . ? P1B C1B P2B N2B -37.8(5) . . . . ? C2B C1B P2B C61B 18.5(7) . . . . ? P1B C1B P2B C61B -161.3(3) . . . . ? C2B C1B P2B C51B -98.5(6) . . . . ? P1B C1B P2B C51B 81.7(4) . . . . ? N2B P2B C51B C56B -21.9(6) . . . . ? C1B P2B C51B C56B -145.1(5) . . . . ? C61B P2B C51B C56B 96.3(5) . . . . ? N2B P2B C51B C52B 157.4(5) . . . . ? C1B P2B C51B C52B 34.3(6) . . . . ? C61B P2B C51B C52B -84.4(5) . . . . ? C56B C51B C52B C53B -0.4(9) . . . . ? P2B C51B C52B C53B -179.7(5) . . . . ? C51B C52B C53B C54B 0.5(10) . . . . ? C52B C53B C54B C55B -0.4(11) . . . . ? C53B C54B C55B C56B 0.2(11) . . . . ? C52B C51B C56B C55B 0.2(9) . . . . ? P2B C51B C56B C55B 179.5(5) . . . . ? C54B C55B C56B C51B -0.1(10) . . . . ? N2B P2B C61B C62B 91.8(6) . . . . ? C1B P2B C61B C62B -143.3(6) . . . . ? C51B P2B C61B C62B -24.1(6) . . . . ? N2B P2B C61B C66B -79.2(6) . . . . ? C1B P2B C61B C66B 45.7(6) . . . . ? C51B P2B C61B C66B 164.9(5) . . . . ? C66B C61B C62B C63B 0.4(11) . . . . ? P2B C61B C62B C63B -170.7(6) . . . . ? C61B C62B C63B C64B 0.3(13) . . . . ? C62B C63B C64B C65B -0.7(14) . . . . ? C63B C64B C65B C66B 0.4(13) . . . . ? C64B C65B C66B C61B 0.3(12) . . . . ? C62B C61B C66B C65B -0.7(10) . . . . ? P2B C61B C66B C65B 170.6(6) . . . . ? C76B C71B C72B C73B 0.0 . . . . ? C77B C71B C72B C73B 174.8(19) . . . . ? C71B C72B C73B C74B 0.0 . . . . ? C72B C73B C74B C75B 0.0 . . . . ? C73B C74B C75B C76B 0.0 . . . . ? C74B C75B C76B C71B 0.0 . . . . ? C72B C71B C76B C75B 0.0 . . . . ? C77B C71B C76B C75B -174.9(19) . . . . ? C76C C71C C72C C73C 0.0 . . . . ? C77C C71C C72C C73C 173.8(17) . . . . ? C71C C72C C73C C74C 0.0 . . . . ? C72C C73C C74C C75C 0.0 . . . . ? C73C C74C C75C C76C 0.0 . . . . ? C74C C75C C76C C71C 0.0 . . . . ? C72C C71C C76C C75C 0.0 . . . . ? C77C C71C C76C C75C -174.1(16) . . . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 68.15 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 0.937 _refine_diff_density_min -0.908 _refine_diff_density_rms 0.101 # Attachment '13.cif' data_erk4289 _database_code_depnum_ccdc_archive 'CCDC 676926' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53 H50 Ir N3 P2' _chemical_formula_weight 983.10 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' P P 0.1023 0.0942 '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 monoclinic _symmetry_space_group_name_H-M P21/c 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 19.7081(2) _cell_length_b 11.3012(1) _cell_length_c 21.4893(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.446(1) _cell_angle_gamma 90.00 _cell_volume 4454.82(7) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 10670 _cell_measurement_theta_min 0.41 _cell_measurement_theta_max 27.88 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 3.108 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4092 _exptl_absorpt_correction_T_max 0.7463 _exptl_absorpt_process_details 'SORTAV (Blessing, 1995 & 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode Nonius FR591' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41726 _diffrn_reflns_av_R_equivalents 0.0530 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 27.90 _reflns_number_total 10575 _reflns_number_gt 8671 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius B.V., 1998)' _computing_cell_refinement 'Collect (Nonius B.V., 1998)' _computing_data_reduction 'Denzo-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SCHAKAL (Keller, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0387P)^2^+0.4542P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10575 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0412 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0721 _refine_ls_wR_factor_gt 0.0670 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Ir Ir 0.825885(5) 1.164391(9) 0.496890(5) 0.02744(4) Uani 1 1 d . . . P1 P 0.67748(4) 1.07689(6) 0.37847(3) 0.02807(15) Uani 1 1 d . . . P2 P 0.66313(4) 1.14164(6) 0.50616(3) 0.02660(15) Uani 1 1 d . . . N1 N 0.76126(12) 1.04318(19) 0.42384(11) 0.0310(5) Uani 1 1 d . . . N2 N 0.73067(12) 1.22760(19) 0.51152(11) 0.0297(5) Uani 1 1 d . . . C1 C 0.62199(14) 1.0863(2) 0.42560(12) 0.0292(6) Uani 1 1 d . . . C2 C 0.54793(16) 1.0585(2) 0.39639(13) 0.0313(6) Uani 1 1 d . . . N3 N 0.48652(14) 1.0370(2) 0.37059(13) 0.0442(6) Uani 1 1 d . . . C3 C 0.88757(17) 1.3191(3) 0.53713(17) 0.0412(7) Uani 1 1 d . . . H3 H 0.8440 1.3601 0.5147 0.049 Uiso 1 1 calc R . . C4 C 0.89018(16) 1.2418(3) 0.58955(14) 0.0391(7) Uani 1 1 d . . . H4 H 0.8490 1.2378 0.6016 0.047 Uiso 1 1 calc R . . C5 C 0.95485(19) 1.1649(3) 0.62753(16) 0.0502(9) Uani 1 1 d . . . H5A H 0.9406 1.1092 0.6555 0.060 Uiso 1 1 calc R . . H5B H 0.9939 1.2150 0.6572 0.060 Uiso 1 1 calc R . . C6 C 0.98356(16) 1.0962(3) 0.58198(15) 0.0448(8) Uani 1 1 d . . . H6A H 1.0226 1.1416 0.5751 0.054 Uiso 1 1 calc R . . H6B H 1.0044 1.0213 0.6036 0.054 Uiso 1 1 calc R . . C7 C 0.92467(15) 1.0705(3) 0.51486(14) 0.0364(6) Uani 1 1 d . . . H7 H 0.8960 1.0023 0.5107 0.044 Uiso 1 1 calc R . . C8 C 0.91044(16) 1.1427(3) 0.45854(16) 0.0408(7) Uani 1 1 d . . . H8 H 0.8745 1.1174 0.4183 0.049 Uiso 1 1 calc R . . C9 C 0.94860(19) 1.2581(3) 0.45779(17) 0.0555(9) Uani 1 1 d . . . H9A H 0.9230 1.2988 0.4154 0.067 Uiso 1 1 calc R . . H9B H 0.9984 1.2416 0.4604 0.067 Uiso 1 1 calc R . . C10 C 0.9517(2) 1.3392(3) 0.5152(2) 0.0540(9) Uani 1 1 d . . . H10A H 0.9972 1.3251 0.5531 0.065 Uiso 1 1 calc R . . H10B H 0.9516 1.4217 0.5012 0.065 Uiso 1 1 calc R . . C11 C 0.78975(15) 0.9331(3) 0.41151(14) 0.0369(7) Uani 1 1 d . . . C12 C 0.8042(2) 0.8432(3) 0.4582(2) 0.0573(10) Uani 1 1 d . . . H12 H 0.7957 0.8550 0.4980 0.069 Uiso 1 1 calc R . . C13 C 0.8315(2) 0.7346(4) 0.4464(3) 0.0882(16) Uani 1 1 d . . . H13 H 0.8424 0.6742 0.4787 0.106 Uiso 1 1 calc R . . C14 C 0.8424(2) 0.7164(5) 0.3874(4) 0.109(2) Uani 1 1 d . . . H14 H 0.8594 0.6427 0.3788 0.131 Uiso 1 1 calc R . . C15 C 0.8285(2) 0.8046(5) 0.3416(3) 0.0848(17) Uani 1 1 d . . . H15 H 0.8365 0.7917 0.3016 0.102 Uiso 1 1 calc R . . C16 C 0.80265(17) 0.9143(3) 0.35301(17) 0.0525(9) Uani 1 1 d . . . H16 H 0.7940 0.9751 0.3212 0.063 Uiso 1 1 calc R . . C21 C 0.72322(16) 1.3523(2) 0.52104(16) 0.0362(7) Uani 1 1 d . . . C22 C 0.71161(17) 1.4294(3) 0.46728(17) 0.0461(8) Uani 1 1 d . . . H22 H 0.7071 1.3987 0.4253 0.055 Uiso 1 1 calc R . . C23 C 0.7067(2) 1.5499(3) 0.4749(2) 0.0641(10) Uani 1 1 d . . . H23 H 0.7001 1.6010 0.4386 0.077 Uiso 1 1 calc R . . C24 C 0.7114(2) 1.5945(4) 0.5350(3) 0.0758(13) Uani 1 1 d . . . H24 H 0.7070 1.6765 0.5398 0.091 Uiso 1 1 calc R . . C25 C 0.7225(2) 1.5215(4) 0.5890(2) 0.0706(12) Uani 1 1 d . . . H25 H 0.7264 1.5536 0.6305 0.085 Uiso 1 1 calc R . . C26 C 0.72815(18) 1.3977(3) 0.58190(17) 0.0505(8) Uani 1 1 d . . . H26 H 0.7352 1.3471 0.6184 0.061 Uiso 1 1 calc R . . C31 C 0.67412(15) 1.2153(3) 0.33426(13) 0.0320(6) Uani 1 1 d . . . C32 C 0.73475(17) 1.2605(3) 0.32478(15) 0.0444(7) Uani 1 1 d . . . H32 H 0.7794 1.2198 0.3415 0.053 Uiso 1 1 calc R . . C33 C 0.7295(2) 1.3665(3) 0.29043(19) 0.0604(10) Uani 1 1 d . . . H33 H 0.7709 1.3983 0.2847 0.072 Uiso 1 1 calc R . . C34 C 0.6635(2) 1.4252(3) 0.26467(17) 0.0571(9) Uani 1 1 d . . . H34 H 0.6601 1.4966 0.2413 0.068 Uiso 1 1 calc R . . C35 C 0.6028(2) 1.3796(3) 0.27313(16) 0.0514(8) Uani 1 1 d . . . H35 H 0.5579 1.4193 0.2553 0.062 Uiso 1 1 calc R . . C36 C 0.60804(16) 1.2744(3) 0.30818(14) 0.0395(7) Uani 1 1 d . . . H36 H 0.5666 1.2433 0.3142 0.047 Uiso 1 1 calc R . . C41 C 0.63687(15) 0.9656(3) 0.31561(13) 0.0355(6) Uani 1 1 d . . . C42 C 0.62319(18) 0.9858(3) 0.24804(15) 0.0498(8) Uani 1 1 d . . . H42 H 0.6312 1.0610 0.2333 0.060 Uiso 1 1 calc R . . C43 C 0.5976(2) 0.8937(4) 0.20293(18) 0.0671(11) Uani 1 1 d . . . H43 H 0.5883 0.9068 0.1573 0.081 Uiso 1 1 calc R . . C44 C 0.5858(2) 0.7835(4) 0.2241(2) 0.0674(12) Uani 1 1 d . . . H44 H 0.5692 0.7213 0.1932 0.081 Uiso 1 1 calc R . . C45 C 0.59808(19) 0.7646(3) 0.2897(2) 0.0579(10) Uani 1 1 d . . . H45 H 0.5894 0.6893 0.3039 0.070 Uiso 1 1 calc R . . C46 C 0.62315(18) 0.8545(3) 0.33567(18) 0.0442(8) Uani 1 1 d . . . H46 H 0.6310 0.8405 0.3809 0.053 Uiso 1 1 calc R . . C51 C 0.69351(15) 1.0218(2) 0.56568(13) 0.0301(6) Uani 1 1 d . . . C52 C 0.76048(16) 1.0255(3) 0.61876(14) 0.0400(7) Uani 1 1 d . . . H52 H 0.7932 1.0879 0.6222 0.048 Uiso 1 1 calc R . . C53 C 0.77842(19) 0.9363(3) 0.66647(15) 0.0499(8) Uani 1 1 d . . . H53 H 0.8239 0.9374 0.7018 0.060 Uiso 1 1 calc R . . C54 C 0.7299(2) 0.8462(3) 0.66222(17) 0.0489(9) Uani 1 1 d . . . H54 H 0.7419 0.7870 0.6952 0.059 Uiso 1 1 calc R . . C55 C 0.6640(2) 0.8425(2) 0.60989(17) 0.0441(8) Uani 1 1 d . . . H55 H 0.6313 0.7805 0.6071 0.053 Uiso 1 1 calc R . . C56 C 0.64560(17) 0.9292(3) 0.56142(14) 0.0379(7) Uani 1 1 d . . . H56 H 0.6006 0.9258 0.5255 0.046 Uiso 1 1 calc R . . C61 C 0.59289(15) 1.2162(2) 0.52727(12) 0.0291(6) Uani 1 1 d . . . C62 C 0.58710(18) 1.2002(3) 0.58921(15) 0.0405(7) Uani 1 1 d . . . H62 H 0.6189 1.1481 0.6206 0.049 Uiso 1 1 calc R . . C63 C 0.53430(19) 1.2612(3) 0.60465(17) 0.0503(8) Uani 1 1 d . . . H63 H 0.5308 1.2512 0.6468 0.060 Uiso 1 1 calc R . . C64 C 0.4870(2) 1.3361(3) 0.55872(18) 0.0489(8) Uani 1 1 d . . . H64 H 0.4511 1.3769 0.5693 0.059 Uiso 1 1 calc R . . C65 C 0.49245(19) 1.3513(3) 0.49681(17) 0.0437(8) Uani 1 1 d . . . H65 H 0.4599 1.4022 0.4653 0.052 Uiso 1 1 calc R . . C66 C 0.54499(17) 1.2926(3) 0.48100(14) 0.0370(6) Uani 1 1 d . . . H66 H 0.5486 1.3040 0.4390 0.044 Uiso 1 1 calc R . . C71 C 0.9444(4) 1.3584(6) 0.2959(3) 0.102(2) Uani 1 1 d . . . H71 H 0.8957 1.3835 0.2769 0.122 Uiso 1 1 calc R . . C72 C 0.9998(5) 1.4415(6) 0.3261(3) 0.117(2) Uani 1 1 d . . . H72 H 0.9882 1.5220 0.3273 0.141 Uiso 1 1 calc R . . C73 C 1.0697(4) 1.4052(6) 0.3535(3) 0.112(2) Uani 1 1 d . . . H73 H 1.1066 1.4607 0.3740 0.134 Uiso 1 1 calc R . . C74 C 1.0872(3) 1.2907(6) 0.3517(3) 0.0978(16) Uani 1 1 d . . . H74 H 1.1362 1.2669 0.3703 0.117 Uiso 1 1 calc R . . C75 C 1.0340(3) 1.2090(5) 0.3229(2) 0.0819(13) Uani 1 1 d . . . H75 H 1.0472 1.1291 0.3228 0.098 Uiso 1 1 calc R . . C76 C 0.9611(3) 1.2401(5) 0.2938(2) 0.0766(13) Uani 1 1 d . . . C77 C 0.9047(3) 1.1498(6) 0.2645(3) 0.119(2) Uani 1 1 d . . . H77A H 0.8943 1.1095 0.2999 0.178 Uiso 1 1 calc R . . H77B H 0.9220 1.0930 0.2398 0.178 Uiso 1 1 calc R . . H77C H 0.8607 1.1875 0.2345 0.178 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 Ir 0.02224(7) 0.03236(7) 0.02794(7) -0.00377(4) 0.00942(5) -0.00245(4) P1 0.0251(4) 0.0324(4) 0.0261(3) -0.0029(3) 0.0087(3) -0.0008(3) P2 0.0240(4) 0.0302(4) 0.0262(3) -0.0013(3) 0.0098(3) -0.0008(3) N1 0.0254(12) 0.0318(12) 0.0334(11) -0.0084(9) 0.0078(9) -0.0011(10) N2 0.0269(12) 0.0270(12) 0.0376(12) -0.0030(10) 0.0149(10) -0.0007(10) C1 0.0255(14) 0.0335(14) 0.0289(13) -0.0026(11) 0.0100(11) -0.0024(11) C2 0.0328(16) 0.0282(14) 0.0337(14) -0.0005(11) 0.0131(12) 0.0015(12) N3 0.0324(15) 0.0525(16) 0.0467(15) -0.0094(12) 0.0133(12) -0.0058(12) C3 0.0278(16) 0.0390(17) 0.0554(19) -0.0150(14) 0.0134(14) -0.0125(13) C4 0.0259(15) 0.0527(19) 0.0374(15) -0.0168(14) 0.0098(12) -0.0061(14) C5 0.0327(18) 0.074(3) 0.0351(17) -0.0101(15) 0.0020(14) 0.0018(16) C6 0.0285(17) 0.055(2) 0.0440(17) -0.0045(15) 0.0045(13) 0.0038(15) C7 0.0214(15) 0.0434(17) 0.0436(16) -0.0070(13) 0.0112(12) 0.0007(12) C8 0.0225(15) 0.060(2) 0.0426(17) -0.0100(14) 0.0154(13) -0.0040(14) C9 0.042(2) 0.076(3) 0.057(2) 0.0000(18) 0.0282(17) -0.0172(19) C10 0.042(2) 0.050(2) 0.075(3) -0.0051(17) 0.0271(19) -0.0133(16) C11 0.0235(15) 0.0357(15) 0.0465(16) -0.0135(13) 0.0069(12) -0.0016(12) C12 0.036(2) 0.0378(19) 0.083(3) 0.0052(17) 0.0044(18) -0.0024(15) C13 0.041(2) 0.036(2) 0.159(5) 0.006(3) 0.002(3) -0.0014(18) C14 0.038(3) 0.065(3) 0.194(7) -0.075(4) 0.007(3) 0.002(2) C15 0.031(2) 0.099(3) 0.109(4) -0.072(3) 0.008(2) 0.004(2) C16 0.0288(17) 0.066(2) 0.058(2) -0.0283(18) 0.0102(15) 0.0015(16) C21 0.0231(15) 0.0358(16) 0.0512(18) -0.0095(13) 0.0152(13) -0.0023(12) C22 0.0382(19) 0.0349(16) 0.064(2) -0.0003(15) 0.0175(16) -0.0012(14) C23 0.053(2) 0.0372(19) 0.099(3) 0.003(2) 0.025(2) 0.0006(17) C24 0.060(3) 0.047(2) 0.125(4) -0.022(3) 0.040(3) -0.003(2) C25 0.060(3) 0.070(3) 0.094(3) -0.046(2) 0.042(2) -0.013(2) C26 0.042(2) 0.055(2) 0.059(2) -0.0229(17) 0.0248(16) -0.0106(16) C31 0.0303(15) 0.0383(15) 0.0259(13) 0.0012(12) 0.0086(11) 0.0007(13) C32 0.0375(18) 0.053(2) 0.0463(17) 0.0101(15) 0.0196(14) 0.0045(15) C33 0.054(2) 0.068(2) 0.068(2) 0.023(2) 0.032(2) -0.0030(19) C34 0.065(3) 0.052(2) 0.055(2) 0.0176(17) 0.0223(18) 0.0021(19) C35 0.049(2) 0.054(2) 0.0479(19) 0.0145(16) 0.0126(16) 0.0098(17) C36 0.0314(16) 0.0445(18) 0.0400(16) 0.0059(14) 0.0099(13) -0.0008(14) C41 0.0235(14) 0.0454(17) 0.0348(14) -0.0109(12) 0.0074(12) 0.0001(12) C42 0.046(2) 0.067(2) 0.0338(16) -0.0100(15) 0.0117(14) 0.0011(17) C43 0.056(2) 0.098(3) 0.0415(19) -0.031(2) 0.0115(17) -0.003(2) C44 0.039(2) 0.079(3) 0.083(3) -0.051(2) 0.0209(19) -0.014(2) C45 0.042(2) 0.052(2) 0.082(3) -0.0291(19) 0.0253(19) -0.0106(17) C46 0.0358(19) 0.0456(19) 0.0500(19) -0.0117(14) 0.0144(15) -0.0053(14) C51 0.0302(15) 0.0308(14) 0.0310(13) -0.0011(11) 0.0133(11) 0.0034(12) C52 0.0323(16) 0.0438(17) 0.0388(15) 0.0034(13) 0.0069(13) -0.0024(13) C53 0.047(2) 0.056(2) 0.0381(16) 0.0099(15) 0.0051(14) 0.0122(17) C54 0.067(3) 0.0388(18) 0.0437(18) 0.0128(14) 0.0231(18) 0.0133(16) C55 0.050(2) 0.0341(16) 0.0525(19) 0.0027(13) 0.0239(17) -0.0004(14) C56 0.0338(16) 0.0358(16) 0.0428(16) 0.0015(13) 0.0123(13) 0.0001(13) C61 0.0264(14) 0.0309(14) 0.0310(13) -0.0031(11) 0.0118(11) -0.0025(12) C62 0.0407(18) 0.0476(17) 0.0393(16) 0.0052(14) 0.0218(14) 0.0101(14) C63 0.052(2) 0.059(2) 0.0505(19) 0.0039(16) 0.0313(17) 0.0138(18) C64 0.040(2) 0.053(2) 0.059(2) -0.0068(16) 0.0244(17) 0.0078(15) C65 0.0388(19) 0.0390(17) 0.0464(18) -0.0038(13) 0.0075(15) 0.0099(13) C66 0.0365(17) 0.0367(15) 0.0342(15) -0.0002(13) 0.0088(12) 0.0014(13) C71 0.124(5) 0.123(5) 0.088(4) 0.059(4) 0.073(4) 0.064(4) C72 0.184(8) 0.085(4) 0.124(5) 0.026(4) 0.105(6) 0.031(5) C73 0.142(6) 0.099(5) 0.103(4) -0.009(3) 0.056(4) 0.007(4) C74 0.085(4) 0.106(4) 0.102(4) -0.011(4) 0.035(3) 0.000(4) C75 0.096(4) 0.082(3) 0.076(3) 0.007(3) 0.042(3) 0.015(3) C76 0.079(3) 0.111(4) 0.048(2) 0.018(2) 0.033(2) 0.003(3) C77 0.107(5) 0.191(7) 0.060(3) 0.004(3) 0.034(3) -0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir C4 2.119(3) . ? Ir N1 2.122(2) . ? Ir C3 2.124(3) . ? Ir C7 2.125(3) . ? Ir C8 2.126(3) . ? Ir N2 2.136(2) . ? P1 N1 1.626(2) . ? P1 C1 1.744(3) . ? P1 C41 1.805(3) . ? P1 C31 1.819(3) . ? P2 N2 1.618(2) . ? P2 C1 1.738(3) . ? P2 C51 1.808(3) . ? P2 C61 1.814(3) . ? N1 C11 1.429(3) . ? N2 C21 1.439(3) . ? C1 C2 1.398(4) . ? C2 N3 1.158(4) . ? C3 C4 1.411(4) . ? C3 C10 1.518(5) . ? C4 C5 1.511(4) . ? C5 C6 1.512(4) . ? C6 C7 1.513(4) . ? C7 C8 1.400(4) . ? C8 C9 1.509(4) . ? C9 C10 1.519(5) . ? C11 C12 1.383(5) . ? C11 C16 1.387(4) . ? C12 C13 1.400(6) . ? C13 C14 1.376(8) . ? C14 C15 1.357(8) . ? C15 C16 1.396(6) . ? C21 C26 1.375(4) . ? C21 C22 1.398(4) . ? C22 C23 1.380(5) . ? C23 C24 1.358(6) . ? C24 C25 1.374(6) . ? C25 C26 1.416(5) . ? C31 C32 1.381(4) . ? C31 C36 1.387(4) . ? C32 C33 1.391(5) . ? C33 C34 1.383(5) . ? C34 C35 1.374(5) . ? C35 C36 1.390(4) . ? C41 C46 1.386(4) . ? C41 C42 1.396(4) . ? C42 C43 1.386(5) . ? C43 C44 1.375(6) . ? C44 C45 1.358(6) . ? C45 C46 1.376(4) . ? C51 C56 1.390(4) . ? C51 C52 1.394(4) . ? C52 C53 1.388(4) . ? C53 C54 1.377(5) . ? C54 C55 1.373(5) . ? C55 C56 1.379(4) . ? C61 C62 1.389(4) . ? C61 C66 1.392(4) . ? C62 C63 1.386(4) . ? C63 C64 1.373(5) . ? C64 C65 1.384(5) . ? C65 C66 1.373(4) . ? C71 C76 1.381(7) . ? C71 C72 1.406(9) . ? C72 C73 1.348(9) . ? C73 C74 1.343(8) . ? C74 C75 1.364(7) . ? C75 C76 1.386(7) . ? C76 C77 1.469(7) . ? 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 C4 Ir N1 162.31(11) . . ? C4 Ir C3 38.86(12) . . ? N1 Ir C3 158.74(11) . . ? C4 Ir C7 80.92(11) . . ? N1 Ir C7 94.25(10) . . ? C3 Ir C7 89.26(12) . . ? C4 Ir C8 97.34(12) . . ? N1 Ir C8 88.98(10) . . ? C3 Ir C8 80.78(12) . . ? C7 Ir C8 38.47(11) . . ? C4 Ir N2 88.82(10) . . ? N1 Ir N2 90.16(8) . . ? C3 Ir N2 93.89(10) . . ? C7 Ir N2 159.41(10) . . ? C8 Ir N2 161.98(11) . . ? N1 P1 C1 112.39(12) . . ? N1 P1 C41 111.13(12) . . ? C1 P1 C41 106.06(13) . . ? N1 P1 C31 110.47(13) . . ? C1 P1 C31 109.87(13) . . ? C41 P1 C31 106.68(13) . . ? N2 P2 C1 111.03(12) . . ? N2 P2 C51 110.39(12) . . ? C1 P2 C51 110.40(12) . . ? N2 P2 C61 112.74(12) . . ? C1 P2 C61 107.19(13) . . ? C51 P2 C61 104.88(12) . . ? C11 N1 P1 118.32(18) . . ? C11 N1 Ir 121.94(17) . . ? P1 N1 Ir 119.71(12) . . ? C21 N2 P2 118.30(19) . . ? C21 N2 Ir 119.28(17) . . ? P2 N2 Ir 122.21(12) . . ? C2 C1 P2 123.96(19) . . ? C2 C1 P1 119.93(19) . . ? P2 C1 P1 115.94(15) . . ? N3 C2 C1 178.1(3) . . ? C4 C3 C10 123.3(3) . . ? C4 C3 Ir 70.37(16) . . ? C10 C3 Ir 114.5(2) . . ? C3 C4 C5 124.3(3) . . ? C3 C4 Ir 70.77(16) . . ? C5 C4 Ir 111.5(2) . . ? C4 C5 C6 112.8(3) . . ? C7 C6 C5 112.2(3) . . ? C8 C7 C6 123.6(3) . . ? C8 C7 Ir 70.80(17) . . ? C6 C7 Ir 114.20(19) . . ? C7 C8 C9 124.7(3) . . ? C7 C8 Ir 70.73(16) . . ? C9 C8 Ir 111.6(2) . . ? C8 C9 C10 112.6(3) . . ? C3 C10 C9 111.8(3) . . ? C12 C11 C16 119.1(3) . . ? C12 C11 N1 119.8(3) . . ? C16 C11 N1 121.1(3) . . ? C11 C12 C13 120.3(4) . . ? C14 C13 C12 119.8(5) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C16 120.9(5) . . ? C11 C16 C15 119.7(4) . . ? C26 C21 C22 119.1(3) . . ? C26 C21 N2 121.7(3) . . ? C22 C21 N2 119.2(3) . . ? C23 C22 C21 121.0(3) . . ? C24 C23 C22 119.7(4) . . ? C23 C24 C25 121.0(4) . . ? C24 C25 C26 119.8(4) . . ? C21 C26 C25 119.4(4) . . ? C32 C31 C36 119.8(3) . . ? C32 C31 P1 121.8(2) . . ? C36 C31 P1 118.4(2) . . ? C31 C32 C33 119.7(3) . . ? C34 C33 C32 120.2(3) . . ? C35 C34 C33 120.3(3) . . ? C34 C35 C36 119.7(3) . . ? C31 C36 C35 120.3(3) . . ? C46 C41 C42 119.1(3) . . ? C46 C41 P1 118.8(2) . . ? C42 C41 P1 121.9(2) . . ? C43 C42 C41 119.1(4) . . ? C44 C43 C42 120.8(4) . . ? C45 C44 C43 119.9(3) . . ? C44 C45 C46 120.6(4) . . ? C45 C46 C41 120.4(3) . . ? C56 C51 C52 119.6(3) . . ? C56 C51 P2 118.4(2) . . ? C52 C51 P2 121.7(2) . . ? C53 C52 C51 119.4(3) . . ? C54 C53 C52 120.3(3) . . ? C55 C54 C53 120.2(3) . . ? C54 C55 C56 120.4(3) . . ? C55 C56 C51 120.0(3) . . ? C62 C61 C66 119.6(3) . . ? C62 C61 P2 121.1(2) . . ? C66 C61 P2 119.3(2) . . ? C63 C62 C61 119.8(3) . . ? C64 C63 C62 120.4(3) . . ? C63 C64 C65 119.8(3) . . ? C66 C65 C64 120.5(3) . . ? C65 C66 C61 119.9(3) . . ? C76 C71 C72 120.5(6) . . ? C73 C72 C71 119.6(6) . . ? C74 C73 C72 120.9(7) . . ? C73 C74 C75 120.1(6) . . ? C74 C75 C76 122.1(5) . . ? C71 C76 C75 116.7(6) . . ? C71 C76 C77 122.3(6) . . ? C75 C76 C77 120.9(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 P1 N1 C11 115.7(2) . . . . ? C41 P1 N1 C11 -3.0(3) . . . . ? C31 P1 N1 C11 -121.2(2) . . . . ? C1 P1 N1 Ir -66.24(17) . . . . ? C41 P1 N1 Ir 175.07(13) . . . . ? C31 P1 N1 Ir 56.86(16) . . . . ? C4 Ir N1 C11 -64.5(4) . . . . ? C3 Ir N1 C11 107.7(3) . . . . ? C7 Ir N1 C11 8.8(2) . . . . ? C8 Ir N1 C11 46.9(2) . . . . ? N2 Ir N1 C11 -151.1(2) . . . . ? C4 Ir N1 P1 117.5(3) . . . . ? C3 Ir N1 P1 -70.3(3) . . . . ? C7 Ir N1 P1 -169.27(15) . . . . ? C8 Ir N1 P1 -131.14(16) . . . . ? N2 Ir N1 P1 30.86(14) . . . . ? C1 P2 N2 C21 110.6(2) . . . . ? C51 P2 N2 C21 -126.6(2) . . . . ? C61 P2 N2 C21 -9.7(2) . . . . ? C1 P2 N2 Ir -64.23(17) . . . . ? C51 P2 N2 Ir 58.55(16) . . . . ? C61 P2 N2 Ir 175.48(12) . . . . ? C4 Ir N2 C21 57.3(2) . . . . ? N1 Ir N2 C21 -140.3(2) . . . . ? C3 Ir N2 C21 18.8(2) . . . . ? C7 Ir N2 C21 117.1(3) . . . . ? C8 Ir N2 C21 -53.1(4) . . . . ? C4 Ir N2 P2 -127.89(16) . . . . ? N1 Ir N2 P2 34.45(14) . . . . ? C3 Ir N2 P2 -166.44(16) . . . . ? C7 Ir N2 P2 -68.1(3) . . . . ? C8 Ir N2 P2 121.6(3) . . . . ? N2 P2 C1 C2 -149.0(2) . . . . ? C51 P2 C1 C2 88.2(3) . . . . ? C61 P2 C1 C2 -25.5(3) . . . . ? N2 P2 C1 P1 26.2(2) . . . . ? C51 P2 C1 P1 -96.58(17) . . . . ? C61 P2 C1 P1 149.72(15) . . . . ? N1 P1 C1 C2 -149.6(2) . . . . ? C41 P1 C1 C2 -27.9(3) . . . . ? C31 P1 C1 C2 87.0(2) . . . . ? N1 P1 C1 P2 35.0(2) . . . . ? C41 P1 C1 P2 156.62(16) . . . . ? C31 P1 C1 P2 -88.44(18) . . . . ? N1 Ir C3 C4 -176.2(2) . . . . ? C7 Ir C3 C4 -76.37(18) . . . . ? C8 Ir C3 C4 -114.07(19) . . . . ? N2 Ir C3 C4 83.26(18) . . . . ? C4 Ir C3 C10 118.6(3) . . . . ? N1 Ir C3 C10 -57.7(4) . . . . ? C7 Ir C3 C10 42.2(3) . . . . ? C8 Ir C3 C10 4.5(3) . . . . ? N2 Ir C3 C10 -158.2(3) . . . . ? C10 C3 C4 C5 -3.5(4) . . . . ? Ir C3 C4 C5 103.4(3) . . . . ? C10 C3 C4 Ir -107.0(3) . . . . ? N1 Ir C4 C3 175.5(3) . . . . ? C7 Ir C4 C3 100.24(19) . . . . ? C8 Ir C4 C3 65.3(2) . . . . ? N2 Ir C4 C3 -97.68(18) . . . . ? N1 Ir C4 C5 55.2(4) . . . . ? C3 Ir C4 C5 -120.3(3) . . . . ? C7 Ir C4 C5 -20.1(2) . . . . ? C8 Ir C4 C5 -55.0(2) . . . . ? N2 Ir C4 C5 142.0(2) . . . . ? C3 C4 C5 C6 -48.6(4) . . . . ? Ir C4 C5 C6 32.2(4) . . . . ? C4 C5 C6 C7 -28.2(4) . . . . ? C5 C6 C7 C8 93.5(4) . . . . ? C5 C6 C7 Ir 11.2(4) . . . . ? C4 Ir C7 C8 -114.16(19) . . . . ? N1 Ir C7 C8 82.98(18) . . . . ? C3 Ir C7 C8 -76.03(19) . . . . ? N2 Ir C7 C8 -175.1(2) . . . . ? C4 Ir C7 C6 4.9(2) . . . . ? N1 Ir C7 C6 -157.9(2) . . . . ? C3 Ir C7 C6 43.1(2) . . . . ? C8 Ir C7 C6 119.1(3) . . . . ? N2 Ir C7 C6 -56.1(4) . . . . ? C6 C7 C8 C9 -3.4(5) . . . . ? Ir C7 C8 C9 103.4(3) . . . . ? C6 C7 C8 Ir -106.8(3) . . . . ? C4 Ir C8 C7 65.28(19) . . . . ? N1 Ir C8 C7 -98.14(17) . . . . ? C3 Ir C8 C7 100.57(19) . . . . ? N2 Ir C8 C7 174.5(3) . . . . ? C4 Ir C8 C9 -55.4(2) . . . . ? N1 Ir C8 C9 141.1(2) . . . . ? C3 Ir C8 C9 -20.2(2) . . . . ? C7 Ir C8 C9 -120.7(3) . . . . ? N2 Ir C8 C9 53.8(4) . . . . ? C7 C8 C9 C10 -48.2(4) . . . . ? Ir C8 C9 C10 32.7(4) . . . . ? C4 C3 C10 C9 93.7(4) . . . . ? Ir C3 C10 C9 11.9(4) . . . . ? C8 C9 C10 C3 -29.0(4) . . . . ? P1 N1 C11 C12 -110.4(3) . . . . ? Ir N1 C11 C12 71.5(3) . . . . ? P1 N1 C11 C16 69.0(3) . . . . ? Ir N1 C11 C16 -109.0(3) . . . . ? C16 C11 C12 C13 0.0(5) . . . . ? N1 C11 C12 C13 179.4(3) . . . . ? C11 C12 C13 C14 -1.5(6) . . . . ? C12 C13 C14 C15 1.8(7) . . . . ? C13 C14 C15 C16 -0.6(7) . . . . ? C12 C11 C16 C15 1.3(5) . . . . ? N1 C11 C16 C15 -178.2(3) . . . . ? C14 C15 C16 C11 -1.0(6) . . . . ? P2 N2 C21 C26 75.5(3) . . . . ? Ir N2 C21 C26 -109.5(3) . . . . ? P2 N2 C21 C22 -105.3(3) . . . . ? Ir N2 C21 C22 69.7(3) . . . . ? C26 C21 C22 C23 1.5(5) . . . . ? N2 C21 C22 C23 -177.7(3) . . . . ? C21 C22 C23 C24 -1.6(5) . . . . ? C22 C23 C24 C25 1.4(6) . . . . ? C23 C24 C25 C26 -0.9(6) . . . . ? C22 C21 C26 C25 -1.0(5) . . . . ? N2 C21 C26 C25 178.2(3) . . . . ? C24 C25 C26 C21 0.8(6) . . . . ? N1 P1 C31 C32 19.1(3) . . . . ? C1 P1 C31 C32 143.6(2) . . . . ? C41 P1 C31 C32 -101.8(3) . . . . ? N1 P1 C31 C36 -162.6(2) . . . . ? C1 P1 C31 C36 -38.1(3) . . . . ? C41 P1 C31 C36 76.5(2) . . . . ? C36 C31 C32 C33 1.5(5) . . . . ? P1 C31 C32 C33 179.8(3) . . . . ? C31 C32 C33 C34 -1.3(6) . . . . ? C32 C33 C34 C35 0.4(6) . . . . ? C33 C34 C35 C36 0.5(6) . . . . ? C32 C31 C36 C35 -0.7(5) . . . . ? P1 C31 C36 C35 -179.0(2) . . . . ? C34 C35 C36 C31 -0.3(5) . . . . ? N1 P1 C41 C46 68.3(3) . . . . ? C1 P1 C41 C46 -54.1(3) . . . . ? C31 P1 C41 C46 -171.2(2) . . . . ? N1 P1 C41 C42 -107.6(3) . . . . ? C1 P1 C41 C42 130.0(3) . . . . ? C31 P1 C41 C42 12.9(3) . . . . ? C46 C41 C42 C43 -1.3(5) . . . . ? P1 C41 C42 C43 174.6(3) . . . . ? C41 C42 C43 C44 0.0(5) . . . . ? C42 C43 C44 C45 1.1(6) . . . . ? C43 C44 C45 C46 -0.7(6) . . . . ? C44 C45 C46 C41 -0.6(5) . . . . ? C42 C41 C46 C45 1.6(5) . . . . ? P1 C41 C46 C45 -174.4(3) . . . . ? N2 P2 C51 C56 -170.3(2) . . . . ? C1 P2 C51 C56 -47.2(2) . . . . ? C61 P2 C51 C56 68.0(2) . . . . ? N2 P2 C51 C52 15.7(3) . . . . ? C1 P2 C51 C52 138.8(2) . . . . ? C61 P2 C51 C52 -106.0(2) . . . . ? C56 C51 C52 C53 0.3(4) . . . . ? P2 C51 C52 C53 174.2(2) . . . . ? C51 C52 C53 C54 -1.4(5) . . . . ? C52 C53 C54 C55 1.5(5) . . . . ? C53 C54 C55 C56 -0.5(5) . . . . ? C54 C55 C56 C51 -0.6(5) . . . . ? C52 C51 C56 C55 0.7(4) . . . . ? P2 C51 C56 C55 -173.4(2) . . . . ? N2 P2 C61 C62 -102.0(3) . . . . ? C1 P2 C61 C62 135.5(2) . . . . ? C51 P2 C61 C62 18.1(3) . . . . ? N2 P2 C61 C66 76.7(2) . . . . ? C1 P2 C61 C66 -45.8(3) . . . . ? C51 P2 C61 C66 -163.2(2) . . . . ? C66 C61 C62 C63 -0.7(5) . . . . ? P2 C61 C62 C63 178.0(3) . . . . ? C61 C62 C63 C64 0.9(5) . . . . ? C62 C63 C64 C65 -0.4(5) . . . . ? C63 C64 C65 C66 -0.4(5) . . . . ? C64 C65 C66 C61 0.6(5) . . . . ? C62 C61 C66 C65 -0.1(4) . . . . ? P2 C61 C66 C65 -178.8(2) . . . . ? C76 C71 C72 C73 -0.2(8) . . . . ? C71 C72 C73 C74 0.6(9) . . . . ? C72 C73 C74 C75 -1.0(9) . . . . ? C73 C74 C75 C76 1.1(8) . . . . ? C72 C71 C76 C75 0.2(6) . . . . ? C72 C71 C76 C77 178.2(4) . . . . ? C74 C75 C76 C71 -0.6(7) . . . . ? C74 C75 C76 C77 -178.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.90 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.225 _refine_diff_density_min -1.115 _refine_diff_density_rms 0.092