# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Yu-Ying Kuo.' 'Mairi Haddow' 'Adrian Perez-Redondo' 'Gareth Owen' _publ_contact_author_name 'Gareth Owen' _publ_contact_author_email gareth.owen@bristol.ac.uk _publ_section_title ; Rhodium and Iridium Complexes Containing Diphenyl-2-(3-methyl)indolylphosphine: Synthesis, Structure and Application in the Catalytic Transfer Hydrogenation of Ketones ; # Attachment '- Complexes 1_2_3_4_8.cif' data_y004 _database_code_depnum_ccdc_archive 'CCDC 772897' #TrackingRef '- Complexes 1_2_3_4_8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H30 Cl N P Rh' _chemical_formula_sum 'C29 H30 Cl N P Rh' _chemical_formula_weight 561.87 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3430(3) _cell_length_b 15.0230(4) _cell_length_c 16.3236(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.2310(10) _cell_angle_gamma 90.00 _cell_volume 2447.32(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 33216 _cell_measurement_theta_min 2.9205 _cell_measurement_theta_max 30.5665 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9107 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details "SADABS V2008/1'" _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II kappa with CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 56256 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0154 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 30.57 _reflns_number_total 7494 _reflns_number_gt 6840 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0250P)^2^+1.7965P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7494 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0240 _refine_ls_R_factor_gt 0.0209 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0548 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.487109(9) 0.809145(6) 0.542768(6) 0.00999(3) Uani 1 1 d . . . P1 P 0.28665(3) 0.78368(2) 0.57586(2) 0.01020(6) Uani 1 1 d . . . Cl1 Cl 0.60506(3) 0.80042(2) 0.68862(2) 0.01780(7) Uani 1 1 d . . . N1 N 0.35297(11) 0.91191(7) 0.70141(7) 0.0124(2) Uani 1 1 d . . . H1 H 0.4330 0.9181 0.6928 0.015 Uiso 1 1 calc R . . C1 C 0.25504(12) 0.85266(9) 0.65891(8) 0.0117(2) Uani 1 1 d . . . C2 C 0.14147(13) 0.86263(9) 0.68791(8) 0.0144(2) Uani 1 1 d . . . C3 C 0.17292(13) 0.92995(9) 0.75237(8) 0.0147(2) Uani 1 1 d . . . C4 C 0.09960(15) 0.96945(10) 0.80430(9) 0.0198(3) Uani 1 1 d . . . H4 H 0.0106 0.9509 0.8011 0.024 Uiso 1 1 calc R . . C5 C 0.15969(17) 1.03567(11) 0.85993(9) 0.0233(3) Uani 1 1 d . . . H5 H 0.1113 1.0627 0.8954 0.028 Uiso 1 1 calc R . . C6 C 0.29147(17) 1.06388(10) 0.86511(9) 0.0229(3) Uani 1 1 d . . . H6 H 0.3301 1.1096 0.9041 0.027 Uiso 1 1 calc R . . C7 C 0.36607(15) 1.02672(10) 0.81482(9) 0.0185(3) Uani 1 1 d . . . H7 H 0.4547 1.0462 0.8181 0.022 Uiso 1 1 calc R . . C8 C 0.30498(13) 0.95915(9) 0.75889(8) 0.0136(2) Uani 1 1 d . . . C9 C 0.00947(15) 0.81617(11) 0.65784(10) 0.0230(3) Uani 1 1 d . . . H9A H 0.0053 0.7857 0.6041 0.034 Uiso 1 1 calc R . . H9B H -0.0632 0.8599 0.6493 0.034 Uiso 1 1 calc R . . H9C H -0.0001 0.7725 0.7004 0.034 Uiso 1 1 calc R . . C10 C 0.27298(13) 0.66920(9) 0.61000(8) 0.0129(2) Uani 1 1 d . . . C11 C 0.29592(14) 0.59955(9) 0.55870(9) 0.0162(2) Uani 1 1 d . . . H11 H 0.3192 0.6125 0.5074 0.019 Uiso 1 1 calc R . . C12 C 0.28497(15) 0.51152(10) 0.58223(9) 0.0191(3) Uani 1 1 d . . . H12 H 0.2995 0.4647 0.5466 0.023 Uiso 1 1 calc R . . C13 C 0.25286(14) 0.49172(10) 0.65750(9) 0.0189(3) Uani 1 1 d . . . H13 H 0.2456 0.4315 0.6736 0.023 Uiso 1 1 calc R . . C14 C 0.23136(14) 0.56043(10) 0.70923(9) 0.0183(3) Uani 1 1 d . . . H14 H 0.2093 0.5470 0.7608 0.022 Uiso 1 1 calc R . . C15 C 0.24179(13) 0.64884(9) 0.68617(8) 0.0155(2) Uani 1 1 d . . . H15 H 0.2277 0.6954 0.7223 0.019 Uiso 1 1 calc R . . C16 C 0.13530(13) 0.80268(9) 0.48950(8) 0.0125(2) Uani 1 1 d . . . C17 C 0.09692(14) 0.89119(9) 0.46997(9) 0.0159(2) Uani 1 1 d . . . H17 H 0.1444 0.9379 0.5042 0.019 Uiso 1 1 calc R . . C18 C -0.00996(14) 0.91127(10) 0.40097(9) 0.0192(3) Uani 1 1 d . . . H18 H -0.0355 0.9715 0.3886 0.023 Uiso 1 1 calc R . . C19 C -0.07965(14) 0.84366(11) 0.35002(9) 0.0194(3) Uani 1 1 d . . . H19 H -0.1520 0.8574 0.3024 0.023 Uiso 1 1 calc R . . C20 C -0.04261(14) 0.75583(10) 0.36935(9) 0.0180(3) Uani 1 1 d . . . H20 H -0.0906 0.7094 0.3350 0.022 Uiso 1 1 calc R . . C21 C 0.06428(13) 0.73492(9) 0.43865(8) 0.0153(2) Uani 1 1 d . . . H21 H 0.0887 0.6745 0.4512 0.018 Uiso 1 1 calc R . . C27 C 0.40507(13) 0.76145(9) 0.41796(8) 0.0146(2) Uani 1 1 d . . . H27 H 0.3152 0.7328 0.4092 0.017 Uiso 1 1 calc R . . C26 C 0.40101(13) 0.85522(9) 0.41664(8) 0.0144(2) Uani 1 1 d . . . H26 H 0.3088 0.8803 0.4078 0.017 Uiso 1 1 calc R . . C25 C 0.49407(14) 0.91363(10) 0.38101(9) 0.0175(3) Uani 1 1 d . . . H25A H 0.4451 0.9681 0.3564 0.021 Uiso 1 1 calc R . . H25B H 0.5188 0.8811 0.3346 0.021 Uiso 1 1 calc R . . C24 C 0.62288(13) 0.94081(9) 0.44773(9) 0.0157(2) Uani 1 1 d . . . H24A H 0.6960 0.9479 0.4194 0.019 Uiso 1 1 calc R . . H24B H 0.6084 0.9993 0.4719 0.019 Uiso 1 1 calc R . . C23 C 0.66598(13) 0.87473(9) 0.51885(8) 0.0140(2) Uani 1 1 d . . . H23 H 0.7300 0.8991 0.5709 0.017 Uiso 1 1 calc R . . C22 C 0.67832(13) 0.78429(9) 0.50756(9) 0.0145(2) Uani 1 1 d . . . H22 H 0.7495 0.7547 0.5528 0.017 Uiso 1 1 calc R . . C29 C 0.65096(14) 0.74028(10) 0.42160(9) 0.0185(3) Uani 1 1 d . . . H29A H 0.7150 0.6907 0.4243 0.022 Uiso 1 1 calc R . . H29B H 0.6658 0.7840 0.3796 0.022 Uiso 1 1 calc R . . C28 C 0.50693(15) 0.70398(10) 0.39170(10) 0.0195(3) Uani 1 1 d . . . H28A H 0.4818 0.6990 0.3290 0.023 Uiso 1 1 calc R . . H28B H 0.5044 0.6435 0.4152 0.023 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 0.01035(5) 0.01017(5) 0.00936(5) -0.00074(3) 0.00245(3) -0.00040(3) P1 0.01102(13) 0.00986(14) 0.00947(13) 0.00024(11) 0.00226(11) 0.00000(11) Cl1 0.01526(14) 0.02558(17) 0.01140(13) -0.00044(11) 0.00143(11) 0.00507(12) N1 0.0129(5) 0.0116(5) 0.0124(5) -0.0012(4) 0.0030(4) 0.0000(4) C1 0.0128(5) 0.0114(6) 0.0105(5) 0.0001(4) 0.0024(4) 0.0006(4) C2 0.0136(5) 0.0166(6) 0.0131(5) 0.0009(5) 0.0035(4) 0.0012(5) C3 0.0173(6) 0.0148(6) 0.0123(5) 0.0018(4) 0.0046(4) 0.0045(5) C4 0.0214(6) 0.0225(7) 0.0176(6) 0.0019(5) 0.0085(5) 0.0074(5) C5 0.0329(8) 0.0220(7) 0.0172(6) -0.0011(5) 0.0105(6) 0.0100(6) C6 0.0340(8) 0.0173(7) 0.0163(6) -0.0037(5) 0.0047(6) 0.0052(6) C7 0.0231(7) 0.0147(6) 0.0160(6) -0.0012(5) 0.0020(5) 0.0018(5) C8 0.0168(6) 0.0118(6) 0.0115(5) 0.0012(4) 0.0028(4) 0.0037(5) C9 0.0144(6) 0.0310(8) 0.0244(7) -0.0053(6) 0.0066(5) -0.0040(6) C10 0.0117(5) 0.0128(6) 0.0130(5) 0.0016(4) 0.0012(4) -0.0005(4) C11 0.0183(6) 0.0147(6) 0.0158(6) 0.0022(5) 0.0050(5) 0.0017(5) C12 0.0228(7) 0.0132(6) 0.0208(6) 0.0002(5) 0.0046(5) 0.0012(5) C13 0.0203(6) 0.0130(6) 0.0212(6) 0.0040(5) 0.0016(5) -0.0024(5) C14 0.0199(6) 0.0186(7) 0.0154(6) 0.0035(5) 0.0030(5) -0.0048(5) C15 0.0172(6) 0.0153(6) 0.0135(5) 0.0006(5) 0.0030(5) -0.0027(5) C16 0.0121(5) 0.0148(6) 0.0107(5) 0.0012(4) 0.0034(4) -0.0002(4) C17 0.0165(6) 0.0138(6) 0.0167(6) 0.0012(5) 0.0034(5) 0.0003(5) C18 0.0176(6) 0.0192(7) 0.0195(6) 0.0058(5) 0.0027(5) 0.0044(5) C19 0.0149(6) 0.0272(8) 0.0145(6) 0.0033(5) 0.0013(5) 0.0020(5) C20 0.0151(6) 0.0229(7) 0.0149(6) -0.0025(5) 0.0017(5) -0.0027(5) C21 0.0155(6) 0.0154(6) 0.0144(6) -0.0003(5) 0.0030(5) -0.0003(5) C27 0.0160(6) 0.0177(6) 0.0105(5) -0.0035(4) 0.0045(4) -0.0058(5) C26 0.0141(5) 0.0172(6) 0.0112(5) 0.0017(4) 0.0020(4) -0.0027(5) C25 0.0169(6) 0.0195(7) 0.0153(6) 0.0047(5) 0.0029(5) -0.0033(5) C24 0.0155(6) 0.0128(6) 0.0192(6) 0.0009(5) 0.0050(5) -0.0032(5) C23 0.0108(5) 0.0150(6) 0.0159(6) -0.0009(5) 0.0028(4) -0.0029(4) C22 0.0112(5) 0.0144(6) 0.0192(6) -0.0002(5) 0.0062(5) 0.0000(5) C29 0.0193(6) 0.0162(6) 0.0235(7) -0.0045(5) 0.0120(5) -0.0021(5) C28 0.0219(7) 0.0187(7) 0.0213(7) -0.0088(5) 0.0117(5) -0.0063(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C27 2.1156(12) . ? Rh1 C26 2.1326(13) . ? Rh1 C23 2.2193(13) . ? Rh1 C22 2.2312(13) . ? Rh1 P1 2.3077(3) . ? Rh1 Cl1 2.3766(3) . ? P1 C1 1.8032(13) . ? P1 C10 1.8247(14) . ? P1 C16 1.8330(13) . ? N1 C8 1.3695(16) . ? N1 C1 1.3893(16) . ? N1 H1 0.8800 . ? C1 C2 1.3851(17) . ? C2 C3 1.4338(19) . ? C2 C9 1.497(2) . ? C3 C4 1.4084(18) . ? C3 C8 1.4117(19) . ? C4 C5 1.380(2) . ? C4 H4 0.9500 . ? C5 C6 1.409(2) . ? C5 H5 0.9500 . ? C6 C7 1.383(2) . ? C6 H6 0.9500 . ? C7 C8 1.4000(19) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.3981(18) . ? C10 C11 1.3988(19) . ? C11 C12 1.3901(19) . ? C11 H11 0.9500 . ? C12 C13 1.387(2) . ? C12 H12 0.9500 . ? C13 C14 1.388(2) . ? C13 H13 0.9500 . ? C14 C15 1.3924(19) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.3945(18) . ? C16 C17 1.4002(19) . ? C17 C18 1.3883(19) . ? C17 H17 0.9500 . ? C18 C19 1.389(2) . ? C18 H18 0.9500 . ? C19 C20 1.387(2) . ? C19 H19 0.9500 . ? C20 C21 1.3941(19) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C27 C26 1.409(2) . ? C27 C28 1.5088(19) . ? C27 H27 1.0000 . ? C26 C25 1.5260(18) . ? C26 H26 1.0000 . ? C25 C24 1.5380(19) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C24 C23 1.5034(19) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C23 C22 1.3816(19) . ? C23 H23 1.0000 . ? C22 C29 1.5092(19) . ? C22 H22 1.0000 . ? C29 C28 1.540(2) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Rh1 C26 38.75(5) . . ? C27 Rh1 C23 97.06(5) . . ? C26 Rh1 C23 80.91(5) . . ? C27 Rh1 C22 81.59(5) . . ? C26 Rh1 C22 88.81(5) . . ? C23 Rh1 C22 36.17(5) . . ? C27 Rh1 P1 90.66(4) . . ? C26 Rh1 P1 96.13(4) . . ? C23 Rh1 P1 163.04(4) . . ? C22 Rh1 P1 160.77(4) . . ? C27 Rh1 Cl1 156.43(4) . . ? C26 Rh1 Cl1 163.61(4) . . ? C23 Rh1 Cl1 88.19(4) . . ? C22 Rh1 Cl1 89.56(4) . . ? P1 Rh1 Cl1 90.726(12) . . ? C1 P1 C10 105.56(6) . . ? C1 P1 C16 101.64(6) . . ? C10 P1 C16 105.23(6) . . ? C1 P1 Rh1 115.61(4) . . ? C10 P1 Rh1 111.98(4) . . ? C16 P1 Rh1 115.62(4) . . ? C8 N1 C1 109.04(11) . . ? C8 N1 H1 125.5 . . ? C1 N1 H1 125.5 . . ? C2 C1 N1 109.42(11) . . ? C2 C1 P1 131.05(10) . . ? N1 C1 P1 119.42(9) . . ? C1 C2 C3 106.13(12) . . ? C1 C2 C9 128.31(13) . . ? C3 C2 C9 125.53(12) . . ? C4 C3 C8 119.14(13) . . ? C4 C3 C2 133.21(13) . . ? C8 C3 C2 107.64(11) . . ? C5 C4 C3 118.63(14) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 121.19(13) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C7 C6 C5 121.65(14) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 116.94(14) . . ? C6 C7 H7 121.5 . . ? C8 C7 H7 121.5 . . ? N1 C8 C7 129.78(13) . . ? N1 C8 C3 107.75(11) . . ? C7 C8 C3 122.45(12) . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.94(12) . . ? C15 C10 P1 122.16(10) . . ? C11 C10 P1 118.90(10) . . ? C12 C11 C10 120.48(13) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.32(14) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 119.57(13) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C13 C14 C15 120.57(13) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C10 120.10(13) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C21 C16 C17 118.96(12) . . ? C21 C16 P1 123.64(10) . . ? C17 C16 P1 117.18(10) . . ? C18 C17 C16 120.58(13) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 120.29(14) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 119.39(13) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? C19 C20 C21 120.78(13) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C16 120.00(13) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? C26 C27 C28 126.00(12) . . ? C26 C27 Rh1 71.28(7) . . ? C28 C27 Rh1 109.52(9) . . ? C26 C27 H27 113.9 . . ? C28 C27 H27 113.9 . . ? Rh1 C27 H27 113.9 . . ? C27 C26 C25 124.15(12) . . ? C27 C26 Rh1 69.97(7) . . ? C25 C26 Rh1 114.17(9) . . ? C27 C26 H26 113.7 . . ? C25 C26 H26 113.7 . . ? Rh1 C26 H26 113.7 . . ? C26 C25 C24 113.49(11) . . ? C26 C25 H25A 108.9 . . ? C24 C25 H25A 108.9 . . ? C26 C25 H25B 108.9 . . ? C24 C25 H25B 108.9 . . ? H25A C25 H25B 107.7 . . ? C23 C24 C25 113.42(11) . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C22 C23 C24 124.43(12) . . ? C22 C23 Rh1 72.38(7) . . ? C24 C23 Rh1 109.71(8) . . ? C22 C23 H23 114.2 . . ? C24 C23 H23 114.2 . . ? Rh1 C23 H23 114.2 . . ? C23 C22 C29 123.61(13) . . ? C23 C22 Rh1 71.45(7) . . ? C29 C22 Rh1 110.52(9) . . ? C23 C22 H22 114.5 . . ? C29 C22 H22 114.5 . . ? Rh1 C22 H22 114.5 . . ? C22 C29 C28 112.28(11) . . ? C22 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C22 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.9 . . ? C27 C28 C29 113.37(11) . . ? C27 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? C27 C28 H28B 108.9 . . ? C29 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C27 Rh1 P1 C1 -153.58(6) . . . . ? C26 Rh1 P1 C1 -115.14(6) . . . . ? C23 Rh1 P1 C1 -36.23(13) . . . . ? C22 Rh1 P1 C1 140.70(12) . . . . ? Cl1 Rh1 P1 C1 49.95(5) . . . . ? C27 Rh1 P1 C10 85.48(6) . . . . ? C26 Rh1 P1 C10 123.92(6) . . . . ? C23 Rh1 P1 C10 -157.17(13) . . . . ? C22 Rh1 P1 C10 19.76(12) . . . . ? Cl1 Rh1 P1 C10 -70.99(5) . . . . ? C27 Rh1 P1 C16 -35.03(6) . . . . ? C26 Rh1 P1 C16 3.42(6) . . . . ? C23 Rh1 P1 C16 82.33(13) . . . . ? C22 Rh1 P1 C16 -100.75(12) . . . . ? Cl1 Rh1 P1 C16 168.50(5) . . . . ? C8 N1 C1 C2 1.11(14) . . . . ? C8 N1 C1 P1 177.66(9) . . . . ? C10 P1 C1 C2 -63.93(14) . . . . ? C16 P1 C1 C2 45.69(14) . . . . ? Rh1 P1 C1 C2 171.72(11) . . . . ? C10 P1 C1 N1 120.38(10) . . . . ? C16 P1 C1 N1 -130.00(10) . . . . ? Rh1 P1 C1 N1 -3.96(11) . . . . ? N1 C1 C2 C3 -1.19(15) . . . . ? P1 C1 C2 C3 -177.21(10) . . . . ? N1 C1 C2 C9 176.95(13) . . . . ? P1 C1 C2 C9 0.9(2) . . . . ? C1 C2 C3 C4 179.43(14) . . . . ? C9 C2 C3 C4 1.2(2) . . . . ? C1 C2 C3 C8 0.85(15) . . . . ? C9 C2 C3 C8 -177.36(13) . . . . ? C8 C3 C4 C5 0.1(2) . . . . ? C2 C3 C4 C5 -178.40(14) . . . . ? C3 C4 C5 C6 0.1(2) . . . . ? C4 C5 C6 C7 0.1(2) . . . . ? C5 C6 C7 C8 -0.5(2) . . . . ? C1 N1 C8 C7 -178.92(13) . . . . ? C1 N1 C8 C3 -0.54(14) . . . . ? C6 C7 C8 N1 178.87(13) . . . . ? C6 C7 C8 C3 0.7(2) . . . . ? C4 C3 C8 N1 -179.01(12) . . . . ? C2 C3 C8 N1 -0.20(15) . . . . ? C4 C3 C8 C7 -0.5(2) . . . . ? C2 C3 C8 C7 178.32(12) . . . . ? C1 P1 C10 C15 0.79(13) . . . . ? C16 P1 C10 C15 -106.23(11) . . . . ? Rh1 P1 C10 C15 127.39(10) . . . . ? C1 P1 C10 C11 -178.48(10) . . . . ? C16 P1 C10 C11 74.49(12) . . . . ? Rh1 P1 C10 C11 -51.89(11) . . . . ? C15 C10 C11 C12 1.4(2) . . . . ? P1 C10 C11 C12 -179.30(11) . . . . ? C10 C11 C12 C13 -0.9(2) . . . . ? C11 C12 C13 C14 0.2(2) . . . . ? C12 C13 C14 C15 0.0(2) . . . . ? C13 C14 C15 C10 0.6(2) . . . . ? C11 C10 C15 C14 -1.3(2) . . . . ? P1 C10 C15 C14 179.47(11) . . . . ? C1 P1 C16 C21 -135.75(11) . . . . ? C10 P1 C16 C21 -25.88(13) . . . . ? Rh1 P1 C16 C21 98.22(11) . . . . ? C1 P1 C16 C17 49.72(11) . . . . ? C10 P1 C16 C17 159.59(10) . . . . ? Rh1 P1 C16 C17 -76.31(11) . . . . ? C21 C16 C17 C18 -0.1(2) . . . . ? P1 C16 C17 C18 174.65(11) . . . . ? C16 C17 C18 C19 -0.4(2) . . . . ? C17 C18 C19 C20 0.8(2) . . . . ? C18 C19 C20 C21 -0.6(2) . . . . ? C19 C20 C21 C16 0.0(2) . . . . ? C17 C16 C21 C20 0.35(19) . . . . ? P1 C16 C21 C20 -174.09(10) . . . . ? C23 Rh1 C27 C26 -65.87(8) . . . . ? C22 Rh1 C27 C26 -98.67(8) . . . . ? P1 Rh1 C27 C26 99.00(7) . . . . ? Cl1 Rh1 C27 C26 -167.67(7) . . . . ? C26 Rh1 C27 C28 122.57(13) . . . . ? C23 Rh1 C27 C28 56.70(10) . . . . ? C22 Rh1 C27 C28 23.90(9) . . . . ? P1 Rh1 C27 C28 -138.43(9) . . . . ? Cl1 Rh1 C27 C28 -45.10(15) . . . . ? C28 C27 C26 C25 5.3(2) . . . . ? Rh1 C27 C26 C25 106.22(12) . . . . ? C28 C27 C26 Rh1 -100.94(13) . . . . ? C23 Rh1 C26 C27 113.47(8) . . . . ? C22 Rh1 C26 C27 78.00(8) . . . . ? P1 Rh1 C26 C27 -83.37(7) . . . . ? Cl1 Rh1 C26 C27 162.39(11) . . . . ? C27 Rh1 C26 C25 -119.43(13) . . . . ? C23 Rh1 C26 C25 -5.95(10) . . . . ? C22 Rh1 C26 C25 -41.43(10) . . . . ? P1 Rh1 C26 C25 157.20(10) . . . . ? Cl1 Rh1 C26 C25 43.0(2) . . . . ? C27 C26 C25 C24 -91.06(16) . . . . ? Rh1 C26 C25 C24 -9.64(15) . . . . ? C26 C25 C24 C23 27.92(17) . . . . ? C25 C24 C23 C22 49.94(18) . . . . ? C25 C24 C23 Rh1 -31.77(14) . . . . ? C27 Rh1 C23 C22 -65.21(9) . . . . ? C26 Rh1 C23 C22 -100.55(9) . . . . ? P1 Rh1 C23 C22 178.29(9) . . . . ? Cl1 Rh1 C23 C22 91.73(8) . . . . ? C27 Rh1 C23 C24 55.88(10) . . . . ? C26 Rh1 C23 C24 20.54(9) . . . . ? C22 Rh1 C23 C24 121.09(13) . . . . ? P1 Rh1 C23 C24 -60.62(17) . . . . ? Cl1 Rh1 C23 C24 -147.18(9) . . . . ? C24 C23 C22 C29 0.6(2) . . . . ? Rh1 C23 C22 C29 102.76(12) . . . . ? C24 C23 C22 Rh1 -102.20(12) . . . . ? C27 Rh1 C22 C23 114.39(9) . . . . ? C26 Rh1 C22 C23 76.15(8) . . . . ? P1 Rh1 C22 C23 -178.48(8) . . . . ? Cl1 Rh1 C22 C23 -87.54(8) . . . . ? C27 Rh1 C22 C29 -5.47(10) . . . . ? C26 Rh1 C22 C29 -43.70(10) . . . . ? C23 Rh1 C22 C29 -119.86(13) . . . . ? P1 Rh1 C22 C29 61.66(16) . . . . ? Cl1 Rh1 C22 C29 152.61(9) . . . . ? C23 C22 C29 C28 -94.84(16) . . . . ? Rh1 C22 C29 C28 -14.00(15) . . . . ? C26 C27 C28 C29 41.07(19) . . . . ? Rh1 C27 C28 C29 -39.52(14) . . . . ? C22 C29 C28 C27 35.56(17) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.57 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.505 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.071 #===END data_y080sad _database_code_depnum_ccdc_archive 'CCDC 772898' #TrackingRef '- Complexes 1_2_3_4_8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H30 Cl Ir N P' _chemical_formula_sum 'C29 H30 Cl Ir N P' _chemical_formula_weight 651.16 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3316(3) _cell_length_b 15.0241(5) _cell_length_c 16.3586(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.5230(10) _cell_angle_gamma 90.00 _cell_volume 2446.61(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8993 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 27.54 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.768 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 5.650 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.097 _exptl_absorpt_correction_T_max 0.138 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22523 _diffrn_reflns_av_R_equivalents 0.0333 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.56 _reflns_number_total 5635 _reflns_number_gt 4926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0153P)^2^+1.4969P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5635 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0211 _refine_ls_wR_factor_ref 0.0451 _refine_ls_wR_factor_gt 0.0432 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.487812(11) 0.807639(7) 0.543784(7) 0.01306(4) Uani 1 1 d . . . P1 P 0.28678(7) 0.78318(5) 0.57619(5) 0.01361(15) Uani 1 1 d . . . Cl1 Cl 0.60769(7) 0.79925(5) 0.68872(5) 0.02147(15) Uani 1 1 d . . . N1 N 0.3535(2) 0.91225(15) 0.70146(14) 0.0147(5) Uani 1 1 d . . . H1 H 0.4336 0.9184 0.6929 0.018 Uiso 1 1 calc R . . C1 C 0.2560(3) 0.85264(18) 0.65925(17) 0.0143(6) Uani 1 1 d . . . C2 C 0.1428(3) 0.86220(19) 0.68789(18) 0.0173(6) Uani 1 1 d . . . C3 C 0.1742(3) 0.92940(19) 0.75210(18) 0.0175(6) Uani 1 1 d . . . C4 C 0.1015(3) 0.9691(2) 0.80436(19) 0.0230(7) Uani 1 1 d . . . H4 H 0.0124 0.9506 0.8014 0.028 Uiso 1 1 calc R . . C5 C 0.1622(3) 1.0351(2) 0.8595(2) 0.0268(7) Uani 1 1 d . . . H5 H 0.1141 1.0621 0.8950 0.032 Uiso 1 1 calc R . . C6 C 0.2932(3) 1.0636(2) 0.8648(2) 0.0256(7) Uani 1 1 d . . . H6 H 0.3322 1.1090 0.9041 0.031 Uiso 1 1 calc R . . C7 C 0.3669(3) 1.02730(19) 0.81401(19) 0.0223(7) Uani 1 1 d . . . H7 H 0.4552 1.0473 0.8168 0.027 Uiso 1 1 calc R . . C8 C 0.3058(3) 0.95998(19) 0.75848(18) 0.0168(6) Uani 1 1 d . . . C9 C 0.0111(3) 0.8150(2) 0.6579(2) 0.0263(7) Uani 1 1 d . . . H9A H 0.0060 0.7857 0.6036 0.039 Uiso 1 1 calc R . . H9B H -0.0623 0.8581 0.6506 0.039 Uiso 1 1 calc R . . H9C H 0.0034 0.7703 0.7000 0.039 Uiso 1 1 calc R . . C10 C 0.2731(3) 0.66875(18) 0.61027(18) 0.0154(6) Uani 1 1 d . . . C11 C 0.2953(3) 0.59908(19) 0.55904(19) 0.0183(6) Uani 1 1 d . . . H11 H 0.3183 0.6121 0.5078 0.022 Uiso 1 1 calc R . . C12 C 0.2843(3) 0.5114(2) 0.5820(2) 0.0220(7) Uani 1 1 d . . . H12 H 0.2988 0.4646 0.5464 0.026 Uiso 1 1 calc R . . C13 C 0.2522(3) 0.4919(2) 0.6569(2) 0.0220(7) Uani 1 1 d . . . H13 H 0.2446 0.4317 0.6728 0.026 Uiso 1 1 calc R . . C14 C 0.2312(3) 0.5603(2) 0.70865(19) 0.0209(6) Uani 1 1 d . . . H14 H 0.2092 0.5468 0.7601 0.025 Uiso 1 1 calc R . . C15 C 0.2421(3) 0.64811(19) 0.68601(19) 0.0178(6) Uani 1 1 d . . . H15 H 0.2284 0.6946 0.7222 0.021 Uiso 1 1 calc R . . C16 C 0.1355(3) 0.80264(18) 0.48929(17) 0.0135(5) Uani 1 1 d . . . C17 C 0.0974(3) 0.8910(2) 0.47001(19) 0.0198(6) Uani 1 1 d . . . H17 H 0.1451 0.9375 0.5047 0.024 Uiso 1 1 calc R . . C18 C -0.0090(3) 0.9115(2) 0.40101(19) 0.0218(6) Uani 1 1 d . . . H18 H -0.0341 0.9719 0.3885 0.026 Uiso 1 1 calc R . . C19 C -0.0792(3) 0.8441(2) 0.3500(2) 0.0223(7) Uani 1 1 d . . . H19 H -0.1520 0.8580 0.3024 0.027 Uiso 1 1 calc R . . C20 C -0.0426(3) 0.7561(2) 0.36901(19) 0.0212(6) Uani 1 1 d . . . H20 H -0.0910 0.7098 0.3345 0.025 Uiso 1 1 calc R . . C21 C 0.0642(3) 0.7353(2) 0.43807(19) 0.0191(6) Uani 1 1 d . . . H21 H 0.0887 0.6749 0.4505 0.023 Uiso 1 1 calc R . . C22 C 0.6771(3) 0.78265(19) 0.50917(19) 0.0163(6) Uani 1 1 d . . . H22 H 0.7486 0.7529 0.5544 0.020 Uiso 1 1 calc R . . C23 C 0.6643(3) 0.87389(19) 0.52090(19) 0.0170(6) Uani 1 1 d . . . H23 H 0.7285 0.8982 0.5732 0.020 Uiso 1 1 calc R . . C24 C 0.6225(3) 0.94008(19) 0.44917(19) 0.0201(6) Uani 1 1 d . . . H24A H 0.6959 0.9460 0.4211 0.024 Uiso 1 1 calc R . . H24B H 0.6093 0.9989 0.4729 0.024 Uiso 1 1 calc R . . C25 C 0.4939(3) 0.9139(2) 0.38296(19) 0.0206(6) Uani 1 1 d . . . H25A H 0.5177 0.8820 0.3361 0.025 Uiso 1 1 calc R . . H25B H 0.4445 0.9686 0.3591 0.025 Uiso 1 1 calc R . . C26 C 0.4017(3) 0.85472(19) 0.41879(18) 0.0168(6) Uani 1 1 d . . . H26 H 0.3091 0.8793 0.4100 0.020 Uiso 1 1 calc R . . C27 C 0.4064(3) 0.76084(19) 0.41939(18) 0.0172(6) Uani 1 1 d . . . H27 H 0.3165 0.7320 0.4103 0.021 Uiso 1 1 calc R . . C28 C 0.5071(3) 0.70484(19) 0.3904(2) 0.0223(7) Uani 1 1 d . . . H28A H 0.4819 0.7033 0.3276 0.027 Uiso 1 1 calc R . . H28B H 0.5038 0.6431 0.4109 0.027 Uiso 1 1 calc R . . C29 C 0.6512(3) 0.7402(2) 0.4226(2) 0.0224(7) Uani 1 1 d . . . H29A H 0.7151 0.6905 0.4253 0.027 Uiso 1 1 calc R . . H29B H 0.6677 0.7846 0.3818 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ir1 0.01310(6) 0.01251(5) 0.01341(6) -0.00079(4) 0.00326(4) -0.00022(4) P1 0.0138(4) 0.0131(3) 0.0135(4) 0.0005(3) 0.0028(3) 0.0004(3) Cl1 0.0181(4) 0.0294(4) 0.0154(4) -0.0005(3) 0.0019(3) 0.0049(3) N1 0.0131(12) 0.0152(12) 0.0162(12) -0.0016(9) 0.0046(10) -0.0024(9) C1 0.0158(14) 0.0121(13) 0.0137(14) 0.0015(10) 0.0019(12) 0.0022(11) C2 0.0169(15) 0.0198(14) 0.0144(15) 0.0005(11) 0.0029(12) 0.0017(12) C3 0.0200(15) 0.0168(14) 0.0150(15) 0.0047(11) 0.0032(12) 0.0047(12) C4 0.0239(17) 0.0240(16) 0.0231(17) 0.0040(13) 0.0099(14) 0.0066(13) C5 0.037(2) 0.0258(17) 0.0203(17) 0.0015(13) 0.0121(15) 0.0115(15) C6 0.0370(19) 0.0194(16) 0.0190(16) -0.0031(12) 0.0051(14) 0.0043(14) C7 0.0262(17) 0.0142(14) 0.0241(17) 0.0001(12) 0.0028(14) 0.0030(12) C8 0.0194(15) 0.0164(14) 0.0144(14) 0.0043(11) 0.0041(12) 0.0050(12) C9 0.0174(16) 0.0338(18) 0.0277(18) -0.0043(14) 0.0062(14) -0.0037(14) C10 0.0127(14) 0.0154(14) 0.0153(15) 0.0016(11) -0.0010(12) -0.0017(11) C11 0.0203(16) 0.0161(14) 0.0182(15) 0.0032(11) 0.0049(13) 0.0018(12) C12 0.0229(17) 0.0159(14) 0.0255(17) -0.0001(12) 0.0034(14) 0.0009(12) C13 0.0229(16) 0.0141(14) 0.0273(17) 0.0031(12) 0.0036(14) -0.0031(12) C14 0.0192(16) 0.0250(16) 0.0166(15) 0.0050(12) 0.0011(13) -0.0055(12) C15 0.0152(15) 0.0191(15) 0.0179(15) -0.0011(11) 0.0023(12) -0.0026(12) C16 0.0096(13) 0.0181(14) 0.0133(14) -0.0001(11) 0.0038(11) -0.0013(11) C17 0.0176(15) 0.0187(15) 0.0233(16) 0.0011(12) 0.0059(13) -0.0001(12) C18 0.0209(16) 0.0203(15) 0.0244(17) 0.0055(12) 0.0061(13) 0.0042(13) C19 0.0176(16) 0.0317(17) 0.0160(15) 0.0048(13) 0.0017(13) 0.0032(13) C20 0.0169(15) 0.0261(16) 0.0195(16) -0.0051(12) 0.0029(13) -0.0029(12) C21 0.0171(15) 0.0201(15) 0.0203(16) 0.0016(12) 0.0055(13) 0.0016(12) C22 0.0101(14) 0.0172(14) 0.0227(16) 0.0004(11) 0.0062(12) -0.0012(11) C23 0.0103(14) 0.0179(14) 0.0222(16) -0.0019(12) 0.0031(12) -0.0031(11) C24 0.0216(16) 0.0166(15) 0.0233(16) 0.0021(12) 0.0079(13) -0.0012(12) C25 0.0203(16) 0.0209(15) 0.0200(16) 0.0056(12) 0.0042(13) -0.0034(13) C26 0.0127(14) 0.0221(15) 0.0132(14) 0.0023(11) -0.0007(12) 0.0001(12) C27 0.0162(15) 0.0218(15) 0.0145(15) -0.0046(11) 0.0056(12) -0.0062(12) C28 0.0255(17) 0.0214(16) 0.0220(16) -0.0076(12) 0.0099(14) -0.0070(13) C29 0.0240(17) 0.0191(15) 0.0273(17) -0.0041(13) 0.0126(14) -0.0012(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C27 2.104(3) . ? Ir1 C26 2.121(3) . ? Ir1 C23 2.196(3) . ? Ir1 C22 2.209(3) . ? Ir1 P1 2.3064(7) . ? Ir1 Cl1 2.3664(7) . ? P1 C1 1.808(3) . ? P1 C10 1.824(3) . ? P1 C16 1.833(3) . ? Cl1 H1 2.5521 . ? N1 C8 1.369(3) . ? N1 C1 1.386(3) . ? N1 H1 0.8800 . ? C1 C2 1.378(4) . ? C2 C3 1.430(4) . ? C2 C9 1.496(4) . ? C3 C8 1.413(4) . ? C3 C4 1.413(4) . ? C4 C5 1.374(4) . ? C4 H4 0.9500 . ? C5 C6 1.400(5) . ? C5 H5 0.9500 . ? C6 C7 1.381(4) . ? C6 H6 0.9500 . ? C7 C8 1.393(4) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.395(4) . ? C10 C11 1.398(4) . ? C11 C12 1.383(4) . ? C11 H11 0.9500 . ? C12 C13 1.384(4) . ? C12 H12 0.9500 . ? C13 C14 1.385(4) . ? C13 H13 0.9500 . ? C14 C15 1.383(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.392(4) . ? C16 C17 1.396(4) . ? C17 C18 1.383(4) . ? C17 H17 0.9500 . ? C18 C19 1.388(4) . ? C18 H18 0.9500 . ? C19 C20 1.387(4) . ? C19 H19 0.9500 . ? C20 C21 1.387(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.395(4) . ? C22 C29 1.510(4) . ? C22 H22 1.0000 . ? C23 C24 1.510(4) . ? C23 H23 1.0000 . ? C24 C25 1.524(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.530(4) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.411(4) . ? C26 H26 1.0000 . ? C27 C28 1.510(4) . ? C27 H27 1.0000 . ? C28 C29 1.535(4) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Ir1 C26 39.02(11) . . ? C27 Ir1 C23 96.99(11) . . ? C26 Ir1 C23 80.66(11) . . ? C27 Ir1 C22 81.22(11) . . ? C26 Ir1 C22 88.93(11) . . ? C23 Ir1 C22 36.93(10) . . ? C27 Ir1 P1 91.01(8) . . ? C26 Ir1 P1 95.95(8) . . ? C23 Ir1 P1 162.08(8) . . ? C22 Ir1 P1 160.98(7) . . ? C27 Ir1 Cl1 156.61(8) . . ? C26 Ir1 Cl1 162.87(8) . . ? C23 Ir1 Cl1 87.65(8) . . ? C22 Ir1 Cl1 89.19(8) . . ? P1 Ir1 Cl1 91.33(3) . . ? C1 P1 C10 105.70(13) . . ? C1 P1 C16 101.87(13) . . ? C10 P1 C16 105.51(13) . . ? C1 P1 Ir1 115.54(10) . . ? C10 P1 Ir1 111.63(9) . . ? C16 P1 Ir1 115.46(9) . . ? Ir1 Cl1 H1 78.8 . . ? C8 N1 C1 109.4(2) . . ? C8 N1 H1 125.3 . . ? C1 N1 H1 125.3 . . ? C2 C1 N1 109.4(2) . . ? C2 C1 P1 130.7(2) . . ? N1 C1 P1 119.8(2) . . ? C1 C2 C3 106.1(3) . . ? C1 C2 C9 128.3(3) . . ? C3 C2 C9 125.6(3) . . ? C8 C3 C4 118.4(3) . . ? C8 C3 C2 107.9(2) . . ? C4 C3 C2 133.6(3) . . ? C5 C4 C3 118.6(3) . . ? C5 C4 H4 120.7 . . ? C3 C4 H4 120.7 . . ? C4 C5 C6 121.7(3) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C7 C6 C5 121.5(3) . . ? C7 C6 H6 119.3 . . ? C5 C6 H6 119.3 . . ? C6 C7 C8 116.9(3) . . ? C6 C7 H7 121.5 . . ? C8 C7 H7 121.5 . . ? N1 C8 C7 129.9(3) . . ? N1 C8 C3 107.1(3) . . ? C7 C8 C3 122.9(3) . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.7(3) . . ? C15 C10 P1 122.4(2) . . ? C11 C10 P1 118.9(2) . . ? C12 C11 C10 120.8(3) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 120.5(3) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C10 120.3(3) . . ? C14 C15 H15 119.9 . . ? C10 C15 H15 119.9 . . ? C21 C16 C17 118.9(3) . . ? C21 C16 P1 123.7(2) . . ? C17 C16 P1 117.2(2) . . ? C18 C17 C16 120.7(3) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.0(3) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C20 C19 C18 119.6(3) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C21 120.5(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C16 120.3(3) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C23 C22 C29 123.0(3) . . ? C23 C22 Ir1 71.03(15) . . ? C29 C22 Ir1 111.43(19) . . ? C23 C22 H22 114.6 . . ? C29 C22 H22 114.6 . . ? Ir1 C22 H22 114.6 . . ? C22 C23 C24 123.9(3) . . ? C22 C23 Ir1 72.04(16) . . ? C24 C23 Ir1 110.65(18) . . ? C22 C23 H23 114.2 . . ? C24 C23 H23 114.2 . . ? Ir1 C23 H23 114.2 . . ? C23 C24 C25 113.3(2) . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C24 C25 C26 113.0(2) . . ? C24 C25 H25A 109.0 . . ? C26 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C26 C25 H25B 109.0 . . ? H25A C25 H25B 107.8 . . ? C27 C26 C25 124.0(3) . . ? C27 C26 Ir1 69.83(16) . . ? C25 C26 Ir1 114.83(19) . . ? C27 C26 H26 113.6 . . ? C25 C26 H26 113.6 . . ? Ir1 C26 H26 113.6 . . ? C26 C27 C28 125.5(3) . . ? C26 C27 Ir1 71.14(16) . . ? C28 C27 Ir1 111.1(2) . . ? C26 C27 H27 113.8 . . ? C28 C27 H27 113.8 . . ? Ir1 C27 H27 113.8 . . ? C27 C28 C29 112.7(2) . . ? C27 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? C27 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? C22 C29 C28 112.3(2) . . ? C22 C29 H29A 109.1 . . ? C28 C29 H29A 109.1 . . ? C22 C29 H29B 109.1 . . ? C28 C29 H29B 109.1 . . ? H29A C29 H29B 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C27 Ir1 P1 C1 -153.48(13) . . . . ? C26 Ir1 P1 C1 -114.68(13) . . . . ? C23 Ir1 P1 C1 -36.7(3) . . . . ? C22 Ir1 P1 C1 141.2(3) . . . . ? Cl1 Ir1 P1 C1 49.80(10) . . . . ? C27 Ir1 P1 C10 85.71(13) . . . . ? C26 Ir1 P1 C10 124.51(13) . . . . ? C23 Ir1 P1 C10 -157.5(3) . . . . ? C22 Ir1 P1 C10 20.4(3) . . . . ? Cl1 Ir1 P1 C10 -71.01(10) . . . . ? C27 Ir1 P1 C16 -34.78(13) . . . . ? C26 Ir1 P1 C16 4.01(13) . . . . ? C23 Ir1 P1 C16 82.0(3) . . . . ? C22 Ir1 P1 C16 -100.1(3) . . . . ? Cl1 Ir1 P1 C16 168.49(10) . . . . ? C27 Ir1 Cl1 H1 -149.8 . . . . ? C26 Ir1 Cl1 H1 61.2 . . . . ? C23 Ir1 Cl1 H1 108.0 . . . . ? C22 Ir1 Cl1 H1 144.9 . . . . ? P1 Ir1 Cl1 H1 -54.1 . . . . ? C8 N1 C1 C2 0.9(3) . . . . ? C8 N1 C1 P1 177.30(19) . . . . ? C10 P1 C1 C2 -63.7(3) . . . . ? C16 P1 C1 C2 46.4(3) . . . . ? Ir1 P1 C1 C2 172.4(2) . . . . ? C10 P1 C1 N1 120.8(2) . . . . ? C16 P1 C1 N1 -129.2(2) . . . . ? Ir1 P1 C1 N1 -3.2(2) . . . . ? N1 C1 C2 C3 -1.4(3) . . . . ? P1 C1 C2 C3 -177.3(2) . . . . ? N1 C1 C2 C9 177.0(3) . . . . ? P1 C1 C2 C9 1.1(5) . . . . ? C1 C2 C3 C8 1.5(3) . . . . ? C9 C2 C3 C8 -177.1(3) . . . . ? C1 C2 C3 C4 179.5(3) . . . . ? C9 C2 C3 C4 1.0(5) . . . . ? C8 C3 C4 C5 -0.5(4) . . . . ? C2 C3 C4 C5 -178.4(3) . . . . ? C3 C4 C5 C6 0.2(5) . . . . ? C4 C5 C6 C7 0.7(5) . . . . ? C5 C6 C7 C8 -1.1(4) . . . . ? C1 N1 C8 C7 -179.3(3) . . . . ? C1 N1 C8 C3 0.1(3) . . . . ? C6 C7 C8 N1 -180.0(3) . . . . ? C6 C7 C8 C3 0.7(4) . . . . ? C4 C3 C8 N1 -179.4(2) . . . . ? C2 C3 C8 N1 -1.0(3) . . . . ? C4 C3 C8 C7 0.1(4) . . . . ? C2 C3 C8 C7 178.5(3) . . . . ? C1 P1 C10 C15 1.0(3) . . . . ? C16 P1 C10 C15 -106.4(2) . . . . ? Ir1 P1 C10 C15 127.4(2) . . . . ? C1 P1 C10 C11 -178.5(2) . . . . ? C16 P1 C10 C11 74.0(3) . . . . ? Ir1 P1 C10 C11 -52.1(3) . . . . ? C15 C10 C11 C12 1.2(4) . . . . ? P1 C10 C11 C12 -179.2(2) . . . . ? C10 C11 C12 C13 -0.6(5) . . . . ? C11 C12 C13 C14 0.0(5) . . . . ? C12 C13 C14 C15 0.0(5) . . . . ? C13 C14 C15 C10 0.6(4) . . . . ? C11 C10 C15 C14 -1.2(4) . . . . ? P1 C10 C15 C14 179.2(2) . . . . ? C1 P1 C16 C21 -136.1(2) . . . . ? C10 P1 C16 C21 -25.9(3) . . . . ? Ir1 P1 C16 C21 97.9(2) . . . . ? C1 P1 C16 C17 49.2(2) . . . . ? C10 P1 C16 C17 159.4(2) . . . . ? Ir1 P1 C16 C17 -76.8(2) . . . . ? C21 C16 C17 C18 -0.3(4) . . . . ? P1 C16 C17 C18 174.7(2) . . . . ? C16 C17 C18 C19 0.0(4) . . . . ? C17 C18 C19 C20 0.4(4) . . . . ? C18 C19 C20 C21 -0.5(4) . . . . ? C19 C20 C21 C16 0.2(4) . . . . ? C17 C16 C21 C20 0.2(4) . . . . ? P1 C16 C21 C20 -174.4(2) . . . . ? C27 Ir1 C22 C23 114.24(19) . . . . ? C26 Ir1 C22 C23 75.80(19) . . . . ? P1 Ir1 C22 C23 -178.92(19) . . . . ? Cl1 Ir1 C22 C23 -87.17(17) . . . . ? C27 Ir1 C22 C29 -4.7(2) . . . . ? C26 Ir1 C22 C29 -43.1(2) . . . . ? C23 Ir1 C22 C29 -118.9(3) . . . . ? P1 Ir1 C22 C29 62.2(4) . . . . ? Cl1 Ir1 C22 C29 153.9(2) . . . . ? C29 C22 C23 C24 0.5(4) . . . . ? Ir1 C22 C23 C24 -103.2(3) . . . . ? C29 C22 C23 Ir1 103.7(3) . . . . ? C27 Ir1 C23 C22 -65.22(19) . . . . ? C26 Ir1 C23 C22 -100.79(19) . . . . ? P1 Ir1 C23 C22 178.9(2) . . . . ? Cl1 Ir1 C23 C22 91.77(17) . . . . ? C27 Ir1 C23 C24 55.1(2) . . . . ? C26 Ir1 C23 C24 19.5(2) . . . . ? C22 Ir1 C23 C24 120.3(3) . . . . ? P1 Ir1 C23 C24 -60.8(4) . . . . ? Cl1 Ir1 C23 C24 -147.92(19) . . . . ? C22 C23 C24 C25 51.4(4) . . . . ? Ir1 C23 C24 C25 -30.4(3) . . . . ? C23 C24 C25 C26 26.3(4) . . . . ? C24 C25 C26 C27 -90.9(3) . . . . ? C24 C25 C26 Ir1 -9.3(3) . . . . ? C23 Ir1 C26 C27 113.51(18) . . . . ? C22 Ir1 C26 C27 77.33(17) . . . . ? P1 Ir1 C26 C27 -84.25(16) . . . . ? Cl1 Ir1 C26 C27 161.1(2) . . . . ? C27 Ir1 C26 C25 -119.2(3) . . . . ? C23 Ir1 C26 C25 -5.7(2) . . . . ? C22 Ir1 C26 C25 -41.8(2) . . . . ? P1 Ir1 C26 C25 156.6(2) . . . . ? Cl1 Ir1 C26 C25 41.9(4) . . . . ? C25 C26 C27 C28 4.1(5) . . . . ? Ir1 C26 C27 C28 -102.9(3) . . . . ? C25 C26 C27 Ir1 107.0(3) . . . . ? C23 Ir1 C27 C26 -65.73(17) . . . . ? C22 Ir1 C27 C26 -99.23(17) . . . . ? P1 Ir1 C27 C26 98.20(15) . . . . ? Cl1 Ir1 C27 C26 -166.08(15) . . . . ? C26 Ir1 C27 C28 121.7(3) . . . . ? C23 Ir1 C27 C28 56.0(2) . . . . ? C22 Ir1 C27 C28 22.5(2) . . . . ? P1 Ir1 C27 C28 -140.10(19) . . . . ? Cl1 Ir1 C27 C28 -44.4(3) . . . . ? C26 C27 C28 C29 44.2(4) . . . . ? Ir1 C27 C28 C29 -37.2(3) . . . . ? C23 C22 C29 C28 -94.6(3) . . . . ? Ir1 C22 C29 C28 -13.9(3) . . . . ? C27 C28 C29 C22 33.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.638 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.109 #===END data_yc112 _database_code_depnum_ccdc_archive 'CCDC 772899' #TrackingRef '- Complexes 1_2_3_4_8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H26 Cl N P Rh' _chemical_formula_sum 'C28 H26 Cl N P Rh' _chemical_formula_weight 545.83 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3647(2) _cell_length_b 13.1993(3) _cell_length_c 17.0825(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.6650(10) _cell_angle_gamma 90.00 _cell_volume 2316.12(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9985 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 31.14 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.171 _exptl_crystal_size_mid 0.116 _exptl_crystal_size_min 0.089 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.565 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.823 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details SADABS-2008/1 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 24809 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5298 _reflns_number_gt 4563 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker ShelXTL' _computing_publication_material 'Bruker ShelXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0222P)^2^+2.0200P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5298 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0320 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0585 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.523845(14) -0.040378(12) 0.168667(9) 0.01221(5) Uani 1 1 d . . . P1 P 0.31897(5) -0.02836(4) 0.20388(3) 0.01273(11) Uani 1 1 d . . . Cl1 Cl 0.60387(5) 0.10113(4) 0.24483(3) 0.02123(12) Uani 1 1 d . . . N1 N 0.32235(15) 0.17668(13) 0.17232(10) 0.0145(3) Uani 1 1 d . . . H1 H 0.4069 0.1742 0.1710 0.017 Uiso 1 1 calc R . . C1 C 0.24498(18) 0.09522(15) 0.18841(11) 0.0142(4) Uani 1 1 d . . . C2 C 0.11696(19) 0.12684(16) 0.18404(12) 0.0156(4) Uani 1 1 d . . . C3 C 0.11647(19) 0.23250(16) 0.16475(11) 0.0154(4) Uani 1 1 d . . . C4 C 0.01758(19) 0.30652(17) 0.15108(12) 0.0192(4) Uani 1 1 d . . . H4 H -0.0706 0.2894 0.1542 0.023 Uiso 1 1 calc R . . C5 C 0.0511(2) 0.40348(17) 0.13317(12) 0.0209(5) Uani 1 1 d . . . H5 H -0.0151 0.4534 0.1231 0.025 Uiso 1 1 calc R . . C6 C 0.1812(2) 0.43056(17) 0.12942(12) 0.0193(4) Uani 1 1 d . . . H6 H 0.2014 0.4988 0.1183 0.023 Uiso 1 1 calc R . . C7 C 0.2802(2) 0.36045(16) 0.14146(12) 0.0165(4) Uani 1 1 d . . . H7 H 0.3679 0.3787 0.1381 0.020 Uiso 1 1 calc R . . C8 C 0.24608(19) 0.26148(16) 0.15877(11) 0.0144(4) Uani 1 1 d . . . C9 C 0.0002(2) 0.06426(17) 0.19548(14) 0.0214(5) Uani 1 1 d . . . H9A H -0.0330 0.0306 0.1457 0.032 Uiso 1 1 calc R . . H9B H -0.0676 0.1082 0.2119 0.032 Uiso 1 1 calc R . . H9C H 0.0250 0.0131 0.2363 0.032 Uiso 1 1 calc R . . C10 C 0.31660(18) -0.05835(16) 0.30778(12) 0.0152(4) Uani 1 1 d . . . C11 C 0.36717(19) -0.15117(17) 0.33633(13) 0.0200(4) Uani 1 1 d . . . H11 H 0.3990 -0.1978 0.3011 0.024 Uiso 1 1 calc R . . C12 C 0.3715(2) -0.17612(19) 0.41536(13) 0.0256(5) Uani 1 1 d . . . H12 H 0.4021 -0.2409 0.4335 0.031 Uiso 1 1 calc R . . C13 C 0.3315(2) -0.1068(2) 0.46796(14) 0.0301(6) Uani 1 1 d . . . H13 H 0.3369 -0.1230 0.5225 0.036 Uiso 1 1 calc R . . C14 C 0.2835(2) -0.0134(2) 0.44055(14) 0.0297(5) Uani 1 1 d . . . H14 H 0.2564 0.0345 0.4765 0.036 Uiso 1 1 calc R . . C15 C 0.2749(2) 0.01023(17) 0.36102(13) 0.0214(5) Uani 1 1 d . . . H15 H 0.2403 0.0739 0.3426 0.026 Uiso 1 1 calc R . . C16 C 0.20016(18) -0.11157(16) 0.14774(12) 0.0143(4) Uani 1 1 d . . . C17 C 0.1498(2) -0.08301(17) 0.07069(12) 0.0195(4) Uani 1 1 d . . . H17 H 0.1713 -0.0187 0.0511 0.023 Uiso 1 1 calc R . . C18 C 0.0690(2) -0.14766(18) 0.02285(13) 0.0233(5) Uani 1 1 d . . . H18 H 0.0349 -0.1271 -0.0291 0.028 Uiso 1 1 calc R . . C19 C 0.0373(2) -0.24230(18) 0.05024(13) 0.0234(5) Uani 1 1 d . . . H19 H -0.0175 -0.2869 0.0171 0.028 Uiso 1 1 calc R . . C20 C 0.0862(2) -0.27074(17) 0.12597(14) 0.0233(5) Uani 1 1 d . . . H20 H 0.0641 -0.3351 0.1452 0.028 Uiso 1 1 calc R . . C21 C 0.1673(2) -0.20651(16) 0.17469(13) 0.0192(4) Uani 1 1 d . . . H21 H 0.2006 -0.2275 0.2267 0.023 Uiso 1 1 calc R . . C22 C 0.71876(19) -0.10156(16) 0.15465(12) 0.0176(4) Uani 1 1 d . . . H22 H 0.7988 -0.0878 0.1927 0.021 Uiso 1 1 calc R . . C23 C 0.67843(18) -0.04134(17) 0.09055(12) 0.0181(4) Uani 1 1 d . . . H23 H 0.7260 0.0209 0.0773 0.022 Uiso 1 1 calc R . . C24 C 0.60170(19) -0.10993(17) 0.02787(12) 0.0191(4) Uani 1 1 d . . . H24 H 0.5885 -0.0848 -0.0279 0.023 Uiso 1 1 calc R . . C25 C 0.6668(2) -0.20849(17) 0.13413(13) 0.0200(5) Uani 1 1 d . . . H25 H 0.7082 -0.2658 0.1666 0.024 Uiso 1 1 calc R . . C26 C 0.47858(19) -0.13104(16) 0.06743(12) 0.0161(4) Uani 1 1 d . . . H26 H 0.3893 -0.1347 0.0371 0.019 Uiso 1 1 calc R . . C27 C 0.5193(2) -0.19304(16) 0.13318(12) 0.0176(4) Uani 1 1 d . . . H27 H 0.4615 -0.2447 0.1536 0.021 Uiso 1 1 calc R . . C28 C 0.6753(2) -0.21074(18) 0.04417(13) 0.0232(5) Uani 1 1 d . . . H28A H 0.7659 -0.2079 0.0319 0.028 Uiso 1 1 calc R . . H28B H 0.6288 -0.2691 0.0171 0.028 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 0.01376(8) 0.01140(9) 0.01172(8) 0.00010(6) 0.00268(5) -0.00087(6) P1 0.0150(2) 0.0128(3) 0.0107(2) 0.0004(2) 0.00248(18) -0.00079(19) Cl1 0.0191(2) 0.0150(3) 0.0279(3) -0.0054(2) -0.0030(2) 0.00026(19) N1 0.0136(8) 0.0140(9) 0.0163(9) 0.0009(7) 0.0038(6) 0.0007(6) C1 0.0183(9) 0.0136(10) 0.0111(9) 0.0004(8) 0.0037(7) -0.0010(8) C2 0.0162(9) 0.0199(11) 0.0112(10) -0.0007(8) 0.0033(7) 0.0006(8) C3 0.0183(9) 0.0193(11) 0.0087(9) -0.0016(8) 0.0021(7) 0.0017(8) C4 0.0179(10) 0.0255(12) 0.0141(10) -0.0028(9) 0.0023(8) 0.0046(9) C5 0.0247(11) 0.0220(12) 0.0157(11) -0.0014(9) 0.0015(8) 0.0101(9) C6 0.0312(11) 0.0139(11) 0.0128(10) 0.0004(8) 0.0030(8) 0.0033(9) C7 0.0203(10) 0.0149(11) 0.0149(10) -0.0011(8) 0.0043(8) 0.0003(8) C8 0.0188(9) 0.0159(11) 0.0088(9) -0.0025(8) 0.0027(7) 0.0027(8) C9 0.0166(10) 0.0247(12) 0.0236(11) 0.0017(10) 0.0058(8) -0.0009(8) C10 0.0145(9) 0.0184(11) 0.0126(10) 0.0014(8) 0.0009(7) -0.0039(8) C11 0.0168(10) 0.0234(12) 0.0195(11) 0.0025(9) 0.0013(8) -0.0006(8) C12 0.0225(11) 0.0296(13) 0.0241(12) 0.0142(10) 0.0012(9) 0.0016(9) C13 0.0307(12) 0.0442(16) 0.0158(11) 0.0080(11) 0.0040(9) -0.0061(11) C14 0.0384(13) 0.0355(15) 0.0164(11) -0.0026(11) 0.0080(10) -0.0038(11) C15 0.0274(11) 0.0193(12) 0.0183(11) 0.0006(9) 0.0066(9) -0.0008(9) C16 0.0124(9) 0.0167(11) 0.0143(10) -0.0025(8) 0.0035(7) -0.0004(7) C17 0.0214(10) 0.0215(12) 0.0158(10) 0.0003(9) 0.0030(8) -0.0003(9) C18 0.0237(11) 0.0297(13) 0.0154(11) -0.0026(10) -0.0010(8) 0.0005(9) C19 0.0187(10) 0.0255(13) 0.0254(12) -0.0111(10) 0.0014(9) -0.0029(9) C20 0.0256(11) 0.0162(12) 0.0284(13) -0.0016(10) 0.0048(9) -0.0031(9) C21 0.0215(10) 0.0181(11) 0.0179(11) 0.0005(9) 0.0022(8) -0.0008(8) C22 0.0133(9) 0.0228(12) 0.0172(10) -0.0016(9) 0.0035(8) 0.0014(8) C23 0.0140(9) 0.0232(12) 0.0183(10) 0.0013(9) 0.0068(8) -0.0021(8) C24 0.0191(10) 0.0253(12) 0.0138(10) 0.0006(9) 0.0053(8) 0.0012(9) C25 0.0232(10) 0.0173(11) 0.0190(11) -0.0002(9) 0.0013(8) 0.0054(9) C26 0.0183(10) 0.0169(11) 0.0135(10) -0.0045(8) 0.0035(8) -0.0015(8) C27 0.0231(10) 0.0125(11) 0.0179(11) -0.0032(9) 0.0056(8) -0.0020(8) C28 0.0210(10) 0.0295(13) 0.0197(11) -0.0059(10) 0.0046(8) 0.0048(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C27 2.103(2) . ? Rh1 C26 2.104(2) . ? Rh1 C23 2.2177(19) . ? Rh1 C22 2.2181(19) . ? Rh1 P1 2.2884(5) . ? Rh1 Cl1 2.3626(5) . ? P1 C1 1.807(2) . ? P1 C10 1.822(2) . ? P1 C16 1.824(2) . ? N1 C8 1.372(3) . ? N1 C1 1.391(3) . ? N1 H1 0.8800 . ? C1 C2 1.383(3) . ? C2 C3 1.433(3) . ? C2 C9 1.499(3) . ? C3 C4 1.413(3) . ? C3 C8 1.414(3) . ? C4 C5 1.371(3) . ? C4 H4 0.9500 . ? C5 C6 1.405(3) . ? C5 H5 0.9500 . ? C6 C7 1.376(3) . ? C6 H6 0.9500 . ? C7 C8 1.395(3) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.392(3) . ? C10 C11 1.395(3) . ? C11 C12 1.384(3) . ? C11 H11 0.9500 . ? C12 C13 1.385(3) . ? C12 H12 0.9500 . ? C13 C14 1.386(4) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.393(3) . ? C16 C17 1.402(3) . ? C17 C18 1.384(3) . ? C17 H17 0.9500 . ? C18 C19 1.389(3) . ? C18 H18 0.9500 . ? C19 C20 1.377(3) . ? C19 H19 0.9500 . ? C20 C21 1.390(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.372(3) . ? C22 C25 1.535(3) . ? C22 H22 1.0000 . ? C23 C24 1.540(3) . ? C23 H23 1.0000 . ? C24 C28 1.540(3) . ? C24 C26 1.547(3) . ? C24 H24 1.0000 . ? C25 C27 1.541(3) . ? C25 C28 1.551(3) . ? C25 H25 1.0000 . ? C26 C27 1.408(3) . ? C26 H26 1.0000 . ? C27 H27 1.0000 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Rh1 C26 39.11(8) . . ? C27 Rh1 C23 79.13(8) . . ? C26 Rh1 C23 66.54(8) . . ? C27 Rh1 C22 66.79(8) . . ? C26 Rh1 C22 79.08(8) . . ? C23 Rh1 C22 36.05(8) . . ? C27 Rh1 P1 98.98(6) . . ? C26 Rh1 P1 98.19(5) . . ? C23 Rh1 P1 158.24(6) . . ? C22 Rh1 P1 160.75(6) . . ? C27 Rh1 Cl1 155.38(6) . . ? C26 Rh1 Cl1 157.78(6) . . ? C23 Rh1 Cl1 96.15(6) . . ? C22 Rh1 Cl1 95.13(6) . . ? P1 Rh1 Cl1 94.034(18) . . ? C1 P1 C10 106.14(9) . . ? C1 P1 C16 102.89(9) . . ? C10 P1 C16 106.58(9) . . ? C1 P1 Rh1 114.51(6) . . ? C10 P1 Rh1 112.00(6) . . ? C16 P1 Rh1 113.90(6) . . ? C8 N1 C1 109.25(16) . . ? C8 N1 H1 125.4 . . ? C1 N1 H1 125.4 . . ? C2 C1 N1 109.28(18) . . ? C2 C1 P1 131.73(16) . . ? N1 C1 P1 118.84(14) . . ? C1 C2 C3 106.26(17) . . ? C1 C2 C9 127.71(19) . . ? C3 C2 C9 126.02(18) . . ? C4 C3 C8 118.45(19) . . ? C4 C3 C2 133.74(19) . . ? C8 C3 C2 107.80(17) . . ? C5 C4 C3 118.86(19) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.38(19) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C7 C6 C5 121.5(2) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 117.17(19) . . ? C6 C7 H7 121.4 . . ? C8 C7 H7 121.4 . . ? N1 C8 C7 130.02(18) . . ? N1 C8 C3 107.39(17) . . ? C7 C8 C3 122.59(18) . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.53(19) . . ? C15 C10 P1 122.74(16) . . ? C11 C10 P1 118.58(16) . . ? C12 C11 C10 120.8(2) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.1(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 119.6(2) . . ? C12 C13 H13 120.2 . . ? C14 C13 H13 120.2 . . ? C15 C14 C13 120.3(2) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C10 120.6(2) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C21 C16 C17 118.39(19) . . ? C21 C16 P1 123.07(16) . . ? C17 C16 P1 118.21(16) . . ? C18 C17 C16 120.6(2) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 120.5(2) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 119.2(2) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? C19 C20 C21 120.9(2) . . ? C19 C20 H20 119.5 . . ? C21 C20 H20 119.5 . . ? C20 C21 C16 120.4(2) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? C23 C22 C25 106.87(18) . . ? C23 C22 Rh1 71.96(11) . . ? C25 C22 Rh1 93.58(12) . . ? C23 C22 H22 123.5 . . ? C25 C22 H22 123.5 . . ? Rh1 C22 H22 123.5 . . ? C22 C23 C24 106.76(19) . . ? C22 C23 Rh1 71.99(11) . . ? C24 C23 Rh1 94.26(12) . . ? C22 C23 H23 123.4 . . ? C24 C23 H23 123.4 . . ? Rh1 C23 H23 123.4 . . ? C23 C24 C28 100.66(17) . . ? C23 C24 C26 100.47(15) . . ? C28 C24 C26 100.53(17) . . ? C23 C24 H24 117.4 . . ? C28 C24 H24 117.4 . . ? C26 C24 H24 117.4 . . ? C22 C25 C27 101.44(16) . . ? C22 C25 C28 100.33(17) . . ? C27 C25 C28 100.34(16) . . ? C22 C25 H25 117.2 . . ? C27 C25 H25 117.2 . . ? C28 C25 H25 117.2 . . ? C27 C26 C24 106.05(17) . . ? C27 C26 Rh1 70.41(12) . . ? C24 C26 Rh1 98.64(13) . . ? C27 C26 H26 122.9 . . ? C24 C26 H26 122.9 . . ? Rh1 C26 H26 122.9 . . ? C26 C27 C25 106.05(17) . . ? C26 C27 Rh1 70.48(12) . . ? C25 C27 Rh1 98.02(13) . . ? C26 C27 H27 123.0 . . ? C25 C27 H27 123.0 . . ? Rh1 C27 H27 123.0 . . ? C24 C28 C25 94.04(16) . . ? C24 C28 H28A 112.9 . . ? C25 C28 H28A 112.9 . . ? C24 C28 H28B 112.9 . . ? C25 C28 H28B 112.9 . . ? H28A C28 H28B 110.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C27 Rh1 P1 C1 -148.38(9) . . . . ? C26 Rh1 P1 C1 -108.81(9) . . . . ? C23 Rh1 P1 C1 -65.21(18) . . . . ? C22 Rh1 P1 C1 170.86(18) . . . . ? Cl1 Rh1 P1 C1 52.59(7) . . . . ? C27 Rh1 P1 C10 90.71(9) . . . . ? C26 Rh1 P1 C10 130.28(9) . . . . ? C23 Rh1 P1 C10 173.88(17) . . . . ? C22 Rh1 P1 C10 49.95(19) . . . . ? Cl1 Rh1 P1 C10 -68.32(8) . . . . ? C27 Rh1 P1 C16 -30.33(10) . . . . ? C26 Rh1 P1 C16 9.23(10) . . . . ? C23 Rh1 P1 C16 52.84(18) . . . . ? C22 Rh1 P1 C16 -71.09(19) . . . . ? Cl1 Rh1 P1 C16 170.64(8) . . . . ? C8 N1 C1 C2 1.0(2) . . . . ? C8 N1 C1 P1 177.00(13) . . . . ? C10 P1 C1 C2 -73.4(2) . . . . ? C16 P1 C1 C2 38.4(2) . . . . ? Rh1 P1 C1 C2 162.48(17) . . . . ? C10 P1 C1 N1 111.59(16) . . . . ? C16 P1 C1 N1 -136.63(15) . . . . ? Rh1 P1 C1 N1 -12.50(18) . . . . ? N1 C1 C2 C3 -0.3(2) . . . . ? P1 C1 C2 C3 -175.60(16) . . . . ? N1 C1 C2 C9 178.73(19) . . . . ? P1 C1 C2 C9 3.4(3) . . . . ? C1 C2 C3 C4 178.9(2) . . . . ? C9 C2 C3 C4 -0.2(4) . . . . ? C1 C2 C3 C8 -0.5(2) . . . . ? C9 C2 C3 C8 -179.53(19) . . . . ? C8 C3 C4 C5 -0.5(3) . . . . ? C2 C3 C4 C5 -179.8(2) . . . . ? C3 C4 C5 C6 -1.0(3) . . . . ? C4 C5 C6 C7 1.8(3) . . . . ? C5 C6 C7 C8 -1.0(3) . . . . ? C1 N1 C8 C7 179.1(2) . . . . ? C1 N1 C8 C3 -1.3(2) . . . . ? C6 C7 C8 N1 179.0(2) . . . . ? C6 C7 C8 C3 -0.6(3) . . . . ? C4 C3 C8 N1 -178.38(17) . . . . ? C2 C3 C8 N1 1.1(2) . . . . ? C4 C3 C8 C7 1.3(3) . . . . ? C2 C3 C8 C7 -179.24(19) . . . . ? C1 P1 C10 C15 -5.3(2) . . . . ? C16 P1 C10 C15 -114.49(18) . . . . ? Rh1 P1 C10 C15 120.33(16) . . . . ? C1 P1 C10 C11 179.34(15) . . . . ? C16 P1 C10 C11 70.16(17) . . . . ? Rh1 P1 C10 C11 -55.02(17) . . . . ? C15 C10 C11 C12 2.3(3) . . . . ? P1 C10 C11 C12 177.86(16) . . . . ? C10 C11 C12 C13 -3.2(3) . . . . ? C11 C12 C13 C14 1.9(3) . . . . ? C12 C13 C14 C15 0.3(4) . . . . ? C13 C14 C15 C10 -1.2(3) . . . . ? C11 C10 C15 C14 -0.1(3) . . . . ? P1 C10 C15 C14 -175.42(17) . . . . ? C1 P1 C16 C21 -139.50(17) . . . . ? C10 P1 C16 C21 -28.05(19) . . . . ? Rh1 P1 C16 C21 95.97(16) . . . . ? C1 P1 C16 C17 47.22(17) . . . . ? C10 P1 C16 C17 158.68(16) . . . . ? Rh1 P1 C16 C17 -77.31(16) . . . . ? C21 C16 C17 C18 0.2(3) . . . . ? P1 C16 C17 C18 173.85(16) . . . . ? C16 C17 C18 C19 -0.5(3) . . . . ? C17 C18 C19 C20 0.7(3) . . . . ? C18 C19 C20 C21 -0.6(3) . . . . ? C19 C20 C21 C16 0.4(3) . . . . ? C17 C16 C21 C20 -0.2(3) . . . . ? P1 C16 C21 C20 -173.45(16) . . . . ? C27 Rh1 C22 C23 103.92(14) . . . . ? C26 Rh1 C22 C23 64.91(13) . . . . ? P1 Rh1 C22 C23 148.48(14) . . . . ? Cl1 Rh1 C22 C23 -93.41(12) . . . . ? C27 Rh1 C22 C25 -2.66(12) . . . . ? C26 Rh1 C22 C25 -41.67(12) . . . . ? C23 Rh1 C22 C25 -106.58(18) . . . . ? P1 Rh1 C22 C25 41.9(2) . . . . ? Cl1 Rh1 C22 C25 160.00(11) . . . . ? C25 C22 C23 C24 -0.8(2) . . . . ? Rh1 C22 C23 C24 -89.06(13) . . . . ? C25 C22 C23 Rh1 88.28(13) . . . . ? C27 Rh1 C23 C22 -65.29(13) . . . . ? C26 Rh1 C23 C22 -104.21(14) . . . . ? P1 Rh1 C23 C22 -152.29(13) . . . . ? Cl1 Rh1 C23 C22 90.27(12) . . . . ? C27 Rh1 C23 C24 40.97(13) . . . . ? C26 Rh1 C23 C24 2.04(12) . . . . ? C22 Rh1 C23 C24 106.25(18) . . . . ? P1 Rh1 C23 C24 -46.0(2) . . . . ? Cl1 Rh1 C23 C24 -163.48(12) . . . . ? C22 C23 C24 C28 -33.1(2) . . . . ? Rh1 C23 C24 C28 -105.53(13) . . . . ? C22 C23 C24 C26 69.87(19) . . . . ? Rh1 C23 C24 C26 -2.59(15) . . . . ? C23 C22 C25 C27 -68.82(19) . . . . ? Rh1 C22 C25 C27 3.41(15) . . . . ? C23 C22 C25 C28 34.1(2) . . . . ? Rh1 C22 C25 C28 106.30(13) . . . . ? C23 C24 C26 C27 -69.2(2) . . . . ? C28 C24 C26 C27 33.8(2) . . . . ? C23 C24 C26 Rh1 2.75(16) . . . . ? C28 C24 C26 Rh1 105.79(14) . . . . ? C23 Rh1 C26 C27 102.01(13) . . . . ? C22 Rh1 C26 C27 66.49(12) . . . . ? P1 Rh1 C26 C27 -94.18(11) . . . . ? Cl1 Rh1 C26 C27 143.10(13) . . . . ? C27 Rh1 C26 C24 -104.05(17) . . . . ? C23 Rh1 C26 C24 -2.05(12) . . . . ? C22 Rh1 C26 C24 -37.56(13) . . . . ? P1 Rh1 C26 C24 161.77(12) . . . . ? Cl1 Rh1 C26 C24 39.1(2) . . . . ? C24 C26 C27 C25 0.6(2) . . . . ? Rh1 C26 C27 C25 -92.99(14) . . . . ? C24 C26 C27 Rh1 93.64(14) . . . . ? C22 C25 C27 C26 68.3(2) . . . . ? C28 C25 C27 C26 -34.6(2) . . . . ? C22 C25 C27 Rh1 -3.63(16) . . . . ? C28 C25 C27 Rh1 -106.50(15) . . . . ? C23 Rh1 C27 C26 -66.02(12) . . . . ? C22 Rh1 C27 C26 -101.58(13) . . . . ? P1 Rh1 C27 C26 91.97(11) . . . . ? Cl1 Rh1 C27 C26 -146.99(12) . . . . ? C26 Rh1 C27 C25 104.25(17) . . . . ? C23 Rh1 C27 C25 38.24(13) . . . . ? C22 Rh1 C27 C25 2.67(12) . . . . ? P1 Rh1 C27 C25 -163.78(11) . . . . ? Cl1 Rh1 C27 C25 -42.7(2) . . . . ? C23 C24 C28 C25 50.71(18) . . . . ? C26 C24 C28 C25 -52.18(18) . . . . ? C22 C25 C28 C24 -51.15(17) . . . . ? C27 C25 C28 C24 52.63(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.466 _refine_diff_density_min -0.398 _refine_diff_density_rms 0.073 #===END data_y019sad _database_code_depnum_ccdc_archive 'CCDC 772900' #TrackingRef '- Complexes 1_2_3_4_8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H33 N2 P Rh, C4 H8 O, B F4' _chemical_formula_sum 'C35 H41 B F4 N2 O P Rh' _chemical_formula_weight 726.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.5738(2) _cell_length_b 18.7089(4) _cell_length_c 18.5897(4) _cell_angle_alpha 90.00 _cell_angle_beta 91.677(1) _cell_angle_gamma 90.00 _cell_volume 3328.27(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3826 _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 23.60 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_min 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1496 _exptl_absorpt_coefficient_mu 0.614 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.840 _exptl_absorpt_correction_T_max 0.937 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29947 _diffrn_reflns_av_R_equivalents 0.0812 _diffrn_reflns_av_sigmaI/netI 0.0806 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.22 _diffrn_reflns_theta_max 27.51 _reflns_number_total 7630 _reflns_number_gt 5195 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker Apex II' _computing_data_reduction 'Bruker Apex II' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+3.4221P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7630 _refine_ls_number_parameters 408 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0876 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _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 0.23154(3) 0.137252(16) 0.859538(16) 0.01931(9) Uani 1 1 d . . . P1 P 0.30023(10) 0.21316(5) 0.77004(6) 0.0200(2) Uani 1 1 d . . . N1 N 0.3807(3) 0.20364(17) 0.62712(17) 0.0249(7) Uani 1 1 d . . . H1 H 0.4143 0.2474 0.6280 0.030 Uiso 1 1 calc R . . N2 N 0.4051(3) 0.07383(17) 0.84600(17) 0.0219(7) Uani 1 1 d . . . C1 C 0.3199(4) 0.1696(2) 0.6849(2) 0.0223(8) Uani 1 1 d . . . C2 C 0.2779(4) 0.1020(2) 0.6625(2) 0.0254(9) Uani 1 1 d . . . C3 C 0.3155(4) 0.0947(2) 0.5882(2) 0.0269(9) Uani 1 1 d . . . C4 C 0.3028(5) 0.0400(3) 0.5380(2) 0.0401(11) Uani 1 1 d . . . H4 H 0.2578 -0.0035 0.5498 0.048 Uiso 1 1 calc R . . C5 C 0.3568(5) 0.0499(3) 0.4706(3) 0.0460(13) Uani 1 1 d . . . H5 H 0.3493 0.0126 0.4360 0.055 Uiso 1 1 calc R . . C6 C 0.4222(5) 0.1139(2) 0.4524(2) 0.0356(11) Uani 1 1 d . . . H6 H 0.4584 0.1194 0.4057 0.043 Uiso 1 1 calc R . . C7 C 0.4352(4) 0.1692(2) 0.5009(2) 0.0301(10) Uani 1 1 d . . . H7 H 0.4798 0.2126 0.4885 0.036 Uiso 1 1 calc R . . C8 C 0.3807(4) 0.1593(2) 0.5689(2) 0.0242(9) Uani 1 1 d . . . C9 C 0.2057(5) 0.0445(2) 0.7034(2) 0.0363(11) Uani 1 1 d . . . H9A H 0.2739 0.0081 0.7187 0.054 Uiso 1 1 calc R . . H9B H 0.1332 0.0225 0.6724 0.054 Uiso 1 1 calc R . . H9C H 0.1628 0.0653 0.7458 0.054 Uiso 1 1 calc R . . C10 C 0.4693(4) 0.2552(2) 0.7915(2) 0.0213(8) Uani 1 1 d . . . C11 C 0.5209(4) 0.3101(2) 0.7488(2) 0.0276(9) Uani 1 1 d . . . H11 H 0.4667 0.3273 0.7089 0.033 Uiso 1 1 calc R . . C12 C 0.6509(4) 0.3398(2) 0.7646(2) 0.0324(10) Uani 1 1 d . . . H12 H 0.6866 0.3762 0.7346 0.039 Uiso 1 1 calc R . . C13 C 0.7286(4) 0.3166(2) 0.8240(2) 0.0317(10) Uani 1 1 d . . . H13 H 0.8172 0.3374 0.8350 0.038 Uiso 1 1 calc R . . C14 C 0.6776(4) 0.2631(2) 0.8675(2) 0.0261(9) Uani 1 1 d . . . H14 H 0.7308 0.2475 0.9085 0.031 Uiso 1 1 calc R . . C15 C 0.5486(4) 0.2324(2) 0.8512(2) 0.0244(9) Uani 1 1 d . . . H15 H 0.5140 0.1956 0.8810 0.029 Uiso 1 1 calc R . . C16 C 0.1872(4) 0.2890(2) 0.7463(2) 0.0217(8) Uani 1 1 d . . . C17 C 0.1962(4) 0.3527(2) 0.7846(2) 0.0278(9) Uani 1 1 d . . . H17 H 0.2647 0.3578 0.8223 0.033 Uiso 1 1 calc R . . C18 C 0.1061(4) 0.4090(2) 0.7684(3) 0.0323(10) Uani 1 1 d . . . H18 H 0.1141 0.4528 0.7942 0.039 Uiso 1 1 calc R . . C19 C 0.0045(4) 0.4009(2) 0.7144(2) 0.0307(10) Uani 1 1 d . . . H19 H -0.0577 0.4392 0.7033 0.037 Uiso 1 1 calc R . . C20 C -0.0071(4) 0.3377(2) 0.6766(2) 0.0286(9) Uani 1 1 d . . . H20 H -0.0774 0.3323 0.6399 0.034 Uiso 1 1 calc R . . C21 C 0.0848(4) 0.2816(2) 0.6926(2) 0.0240(9) Uani 1 1 d . . . H21 H 0.0771 0.2381 0.6665 0.029 Uiso 1 1 calc R . . C22 C 0.2272(4) 0.0937(2) 0.9702(2) 0.0238(9) Uani 1 1 d . . . H22 H 0.3143 0.0678 0.9859 0.029 Uiso 1 1 calc R . . C23 C 0.1354(4) 0.0535(2) 0.9287(2) 0.0235(9) Uani 1 1 d . . . H23 H 0.1685 0.0038 0.9190 0.028 Uiso 1 1 calc R . . C24 C -0.0219(4) 0.0612(2) 0.9284(2) 0.0273(9) Uani 1 1 d . . . H24A H -0.0502 0.0816 0.9749 0.033 Uiso 1 1 calc R . . H24B H -0.0655 0.0134 0.9233 0.033 Uiso 1 1 calc R . . C25 C -0.0748(4) 0.1094(2) 0.8670(2) 0.0281(9) Uani 1 1 d . . . H25A H -0.0846 0.0804 0.8225 0.034 Uiso 1 1 calc R . . H25B H -0.1686 0.1275 0.8785 0.034 Uiso 1 1 calc R . . C26 C 0.0195(4) 0.1720(2) 0.8528(2) 0.0256(9) Uani 1 1 d . . . H26 H -0.0054 0.1985 0.8075 0.031 Uiso 1 1 calc R . . C27 C 0.0904(4) 0.2130(2) 0.9039(2) 0.0269(9) Uani 1 1 d . . . H27 H 0.1074 0.2632 0.8878 0.032 Uiso 1 1 calc R . . C28 C 0.0801(4) 0.2056(2) 0.9852(2) 0.0318(10) Uani 1 1 d . . . H28A H 0.0906 0.2534 1.0076 0.038 Uiso 1 1 calc R . . H28B H -0.0139 0.1873 0.9964 0.038 Uiso 1 1 calc R . . C29 C 0.1896(4) 0.1558(2) 1.0179(2) 0.0329(10) Uani 1 1 d . . . H29A H 0.2753 0.1837 1.0292 0.039 Uiso 1 1 calc R . . H29B H 0.1549 0.1368 1.0637 0.039 Uiso 1 1 calc R . . C30 C 0.4974(4) 0.0359(2) 0.8489(2) 0.0256(9) Uani 1 1 d . . . C31 C 0.6168(4) -0.0121(2) 0.8538(3) 0.0346(11) Uani 1 1 d . . . H31A H 0.6814 0.0041 0.8923 0.052 Uiso 1 1 calc R . . H31B H 0.6648 -0.0122 0.8079 0.052 Uiso 1 1 calc R . . H31C H 0.5846 -0.0606 0.8645 0.052 Uiso 1 1 calc R . . B1 B 0.3653(5) 0.8711(3) 0.9516(3) 0.0265(10) Uani 1 1 d . . . F1 F 0.2664(3) 0.82448(19) 0.9753(2) 0.0744(10) Uani 1 1 d . . . F2 F 0.3082(3) 0.90685(15) 0.89351(15) 0.0508(8) Uani 1 1 d . . . F3 F 0.4064(3) 0.9169(2) 1.00409(18) 0.0822(12) Uani 1 1 d . . . F4 F 0.4806(2) 0.83182(13) 0.92822(14) 0.0378(6) Uani 1 1 d . . . O1 O 0.1885(6) 0.5702(3) 0.8321(3) 0.1043(18) Uani 1 1 d . . . C32 C 0.2937(7) 0.6204(4) 0.8168(4) 0.082(2) Uani 1 1 d . . . H32A H 0.2941 0.6315 0.7648 0.098 Uiso 1 1 calc R . . H32B H 0.3871 0.6024 0.8323 0.098 Uiso 1 1 calc R . . C35 C 0.1103(7) 0.5918(4) 0.8952(5) 0.095(3) Uani 1 1 d . . . H35A H 0.0146 0.6073 0.8809 0.114 Uiso 1 1 calc R . . H35B H 0.1044 0.5520 0.9301 0.114 Uiso 1 1 calc R . . C33 C 0.2542(6) 0.6844(3) 0.8595(5) 0.103(3) Uani 1 1 d . . . H33A H 0.1856 0.7146 0.8327 0.123 Uiso 1 1 calc R . . H33B H 0.3372 0.7136 0.8731 0.123 Uiso 1 1 calc R . . C34 C 0.1901(7) 0.6505(4) 0.9254(5) 0.101(3) Uani 1 1 d . . . H34A H 0.2633 0.6333 0.9599 0.121 Uiso 1 1 calc R . . H34B H 0.1290 0.6848 0.9501 0.121 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 0.01900(15) 0.01876(14) 0.02040(16) 0.00479(14) 0.00485(11) 0.00276(13) P1 0.0200(5) 0.0190(5) 0.0214(5) 0.0042(4) 0.0040(4) 0.0014(4) N1 0.0310(18) 0.0188(16) 0.0252(19) 0.0039(14) 0.0064(15) -0.0007(14) N2 0.0235(17) 0.0233(17) 0.0190(17) 0.0042(14) 0.0041(14) 0.0028(14) C1 0.0198(19) 0.0214(19) 0.026(2) 0.0052(17) 0.0052(16) 0.0035(15) C2 0.026(2) 0.027(2) 0.024(2) 0.0045(17) 0.0022(17) -0.0030(17) C3 0.029(2) 0.027(2) 0.025(2) 0.0012(18) 0.0002(17) -0.0045(17) C4 0.052(3) 0.038(3) 0.031(3) -0.002(2) 0.002(2) -0.013(2) C5 0.063(3) 0.046(3) 0.029(3) -0.008(2) 0.007(2) -0.014(3) C6 0.040(3) 0.045(3) 0.023(2) -0.001(2) 0.005(2) -0.001(2) C7 0.032(2) 0.032(2) 0.027(2) 0.008(2) 0.0069(19) 0.0032(18) C8 0.023(2) 0.026(2) 0.024(2) 0.0025(17) 0.0042(17) 0.0043(16) C9 0.049(3) 0.033(2) 0.027(2) 0.004(2) 0.000(2) -0.017(2) C10 0.0200(18) 0.0194(19) 0.025(2) 0.0009(17) 0.0057(16) 0.0031(15) C11 0.025(2) 0.032(2) 0.026(2) 0.0004(19) 0.0013(17) -0.0044(17) C12 0.032(2) 0.037(2) 0.029(2) 0.003(2) 0.0088(19) -0.0106(19) C13 0.024(2) 0.040(3) 0.031(2) -0.006(2) 0.0049(18) -0.0057(18) C14 0.026(2) 0.028(2) 0.024(2) -0.0026(18) -0.0008(17) 0.0042(17) C15 0.026(2) 0.021(2) 0.026(2) 0.0009(17) 0.0056(17) 0.0019(16) C16 0.0206(19) 0.0204(19) 0.025(2) 0.0073(17) 0.0068(16) 0.0014(15) C17 0.024(2) 0.026(2) 0.034(2) 0.0035(18) 0.0027(17) -0.0022(17) C18 0.032(2) 0.021(2) 0.045(3) 0.002(2) 0.013(2) -0.0011(18) C19 0.022(2) 0.034(2) 0.037(3) 0.015(2) 0.0110(19) 0.0087(18) C20 0.026(2) 0.038(2) 0.022(2) 0.0092(19) 0.0035(17) 0.0049(18) C21 0.025(2) 0.023(2) 0.024(2) 0.0058(17) 0.0066(17) 0.0024(16) C22 0.026(2) 0.029(2) 0.016(2) 0.0078(17) 0.0032(16) 0.0046(17) C23 0.028(2) 0.0171(19) 0.026(2) 0.0113(17) 0.0079(17) 0.0018(16) C24 0.024(2) 0.024(2) 0.035(2) 0.0082(18) 0.0026(18) -0.0027(16) C25 0.020(2) 0.029(2) 0.035(2) 0.0098(19) 0.0006(18) -0.0002(17) C26 0.0189(19) 0.023(2) 0.035(2) 0.0108(18) 0.0035(17) 0.0077(16) C27 0.027(2) 0.021(2) 0.033(2) 0.0047(18) 0.0103(18) 0.0101(16) C28 0.032(2) 0.030(2) 0.034(3) -0.001(2) 0.0159(19) 0.0056(18) C29 0.034(2) 0.041(3) 0.024(2) -0.0030(19) 0.0046(19) 0.0036(19) C30 0.028(2) 0.024(2) 0.025(2) -0.0005(17) 0.0040(17) -0.0039(18) C31 0.025(2) 0.024(2) 0.055(3) -0.003(2) 0.004(2) 0.0050(17) B1 0.024(2) 0.032(3) 0.024(2) -0.001(2) -0.0004(19) 0.007(2) F1 0.056(2) 0.075(2) 0.094(3) 0.026(2) 0.0343(19) -0.0010(17) F2 0.0694(19) 0.0424(16) 0.0399(17) -0.0023(14) -0.0104(14) 0.0225(14) F3 0.0519(19) 0.112(3) 0.080(2) -0.071(2) -0.0334(17) 0.0374(19) F4 0.0310(13) 0.0387(14) 0.0438(16) -0.0126(13) 0.0038(12) 0.0097(11) O1 0.133(5) 0.070(3) 0.109(4) -0.010(3) -0.023(4) -0.045(3) C32 0.093(5) 0.078(5) 0.074(5) 0.014(4) -0.026(4) -0.040(4) C35 0.066(5) 0.062(5) 0.154(8) 0.013(5) -0.019(5) -0.011(4) C33 0.047(4) 0.037(3) 0.224(10) 0.014(5) 0.011(5) 0.002(3) C34 0.048(4) 0.095(6) 0.162(8) -0.068(6) 0.016(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N2 2.063(3) . ? Rh1 C26 2.132(4) . ? Rh1 C27 2.140(4) . ? Rh1 C22 2.214(4) . ? Rh1 C23 2.242(3) . ? Rh1 P1 2.2981(10) . ? P1 C1 1.796(4) . ? P1 C16 1.831(4) . ? P1 C10 1.833(4) . ? N1 C8 1.364(5) . ? N1 C1 1.391(5) . ? N1 H1 0.8800 . ? N2 C30 1.133(5) . ? C1 C2 1.386(5) . ? C2 C3 1.444(6) . ? C2 C9 1.498(5) . ? C3 C4 1.387(6) . ? C3 C8 1.412(5) . ? C4 C5 1.383(6) . ? C4 H4 0.9500 . ? C5 C6 1.397(6) . ? C5 H5 0.9500 . ? C6 C7 1.374(6) . ? C6 H6 0.9500 . ? C7 C8 1.393(5) . ? C7 H7 0.9500 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C15 1.394(5) . ? C10 C11 1.397(5) . ? C11 C12 1.386(5) . ? C11 H11 0.9500 . ? C12 C13 1.384(6) . ? C12 H12 0.9500 . ? C13 C14 1.384(6) . ? C13 H13 0.9500 . ? C14 C15 1.387(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.386(5) . ? C16 C17 1.391(5) . ? C17 C18 1.389(6) . ? C17 H17 0.9500 . ? C18 C19 1.386(6) . ? C18 H18 0.9500 . ? C19 C20 1.379(6) . ? C19 H19 0.9500 . ? C20 C21 1.395(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.376(5) . ? C22 C29 1.511(6) . ? C22 H22 1.0000 . ? C23 C24 1.513(5) . ? C23 H23 1.0000 . ? C24 C25 1.530(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.507(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.383(6) . ? C26 H26 1.0000 . ? C27 C28 1.524(6) . ? C27 H27 1.0000 . ? C28 C29 1.516(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.454(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? B1 F3 1.349(5) . ? B1 F2 1.371(5) . ? B1 F1 1.370(5) . ? B1 F4 1.405(5) . ? O1 C32 1.412(7) . ? O1 C35 1.467(9) . ? C32 C33 1.492(9) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C35 C34 1.443(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C33 C34 1.524(11) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Rh1 C26 159.60(15) . . ? N2 Rh1 C27 161.41(15) . . ? C26 Rh1 C27 37.77(15) . . ? N2 Rh1 C22 86.48(13) . . ? C26 Rh1 C22 97.08(15) . . ? C27 Rh1 C22 81.78(15) . . ? N2 Rh1 C23 90.78(13) . . ? C26 Rh1 C23 80.84(14) . . ? C27 Rh1 C23 88.16(14) . . ? C22 Rh1 C23 35.96(14) . . ? N2 Rh1 P1 91.06(9) . . ? C26 Rh1 P1 93.51(11) . . ? C27 Rh1 P1 93.82(11) . . ? C22 Rh1 P1 156.00(11) . . ? C23 Rh1 P1 168.03(11) . . ? C1 P1 C16 102.45(18) . . ? C1 P1 C10 105.76(17) . . ? C16 P1 C10 103.39(17) . . ? C1 P1 Rh1 113.40(13) . . ? C16 P1 Rh1 118.32(12) . . ? C10 P1 Rh1 112.18(13) . . ? C8 N1 C1 110.1(3) . . ? C8 N1 H1 125.0 . . ? C1 N1 H1 125.0 . . ? C30 N2 Rh1 169.7(3) . . ? C2 C1 N1 108.1(3) . . ? C2 C1 P1 129.9(3) . . ? N1 C1 P1 122.0(3) . . ? C1 C2 C3 107.2(3) . . ? C1 C2 C9 129.5(4) . . ? C3 C2 C9 123.3(4) . . ? C4 C3 C8 119.4(4) . . ? C4 C3 C2 133.9(4) . . ? C8 C3 C2 106.6(4) . . ? C5 C4 C3 118.8(4) . . ? C5 C4 H4 120.6 . . ? C3 C4 H4 120.6 . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 121.3(4) . . ? C7 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C6 C7 C8 117.8(4) . . ? C6 C7 H7 121.1 . . ? C8 C7 H7 121.1 . . ? N1 C8 C7 130.4(4) . . ? N1 C8 C3 108.0(3) . . ? C7 C8 C3 121.6(4) . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C15 C10 C11 118.9(4) . . ? C15 C10 P1 119.9(3) . . ? C11 C10 P1 121.2(3) . . ? C12 C11 C10 120.4(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 120.1(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.2(4) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 119.9(4) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C10 120.5(4) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? C21 C16 C17 119.2(4) . . ? C21 C16 P1 119.8(3) . . ? C17 C16 P1 120.9(3) . . ? C18 C17 C16 120.7(4) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C19 C18 C17 119.5(4) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C20 C19 C18 120.5(4) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.7(4) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C16 C21 C20 120.4(4) . . ? C16 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C23 C22 C29 126.1(4) . . ? C23 C22 Rh1 73.1(2) . . ? C29 C22 Rh1 105.9(3) . . ? C23 C22 H22 114.3 . . ? C29 C22 H22 114.3 . . ? Rh1 C22 H22 114.3 . . ? C22 C23 C24 124.7(4) . . ? C22 C23 Rh1 70.9(2) . . ? C24 C23 Rh1 110.9(2) . . ? C22 C23 H23 114.1 . . ? C24 C23 H23 114.1 . . ? Rh1 C23 H23 114.1 . . ? C23 C24 C25 111.5(3) . . ? C23 C24 H24A 109.3 . . ? C25 C24 H24A 109.3 . . ? C23 C24 H24B 109.3 . . ? C25 C24 H24B 109.3 . . ? H24A C24 H24B 108.0 . . ? C26 C25 C24 113.7(3) . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25B 108.8 . . ? C24 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C27 C26 C25 126.6(4) . . ? C27 C26 Rh1 71.4(2) . . ? C25 C26 Rh1 109.0(2) . . ? C27 C26 H26 113.8 . . ? C25 C26 H26 113.8 . . ? Rh1 C26 H26 113.8 . . ? C26 C27 C28 125.8(4) . . ? C26 C27 Rh1 70.8(2) . . ? C28 C27 Rh1 112.4(3) . . ? C26 C27 H27 113.4 . . ? C28 C27 H27 113.4 . . ? Rh1 C27 H27 113.4 . . ? C29 C28 C27 112.9(3) . . ? C29 C28 H28A 109.0 . . ? C27 C28 H28A 109.0 . . ? C29 C28 H28B 109.0 . . ? C27 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? C22 C29 C28 114.3(3) . . ? C22 C29 H29A 108.7 . . ? C28 C29 H29A 108.7 . . ? C22 C29 H29B 108.7 . . ? C28 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? N2 C30 C31 178.9(5) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? F3 B1 F2 111.2(4) . . ? F3 B1 F1 111.2(4) . . ? F2 B1 F1 107.5(4) . . ? F3 B1 F4 109.9(4) . . ? F2 B1 F4 108.1(3) . . ? F1 B1 F4 108.9(4) . . ? C32 O1 C35 111.2(5) . . ? O1 C32 C33 103.5(6) . . ? O1 C32 H32A 111.1 . . ? C33 C32 H32A 111.1 . . ? O1 C32 H32B 111.1 . . ? C33 C32 H32B 111.1 . . ? H32A C32 H32B 109.0 . . ? C34 C35 O1 104.2(6) . . ? C34 C35 H35A 110.9 . . ? O1 C35 H35A 110.9 . . ? C34 C35 H35B 110.9 . . ? O1 C35 H35B 110.9 . . ? H35A C35 H35B 108.9 . . ? C32 C33 C34 102.0(5) . . ? C32 C33 H33A 111.4 . . ? C34 C33 H33A 111.4 . . ? C32 C33 H33B 111.4 . . ? C34 C33 H33B 111.4 . . ? H33A C33 H33B 109.2 . . ? C35 C34 C33 103.0(7) . . ? C35 C34 H34A 111.2 . . ? C33 C34 H34A 111.2 . . ? C35 C34 H34B 111.2 . . ? C33 C34 H34B 111.2 . . ? H34A C34 H34B 109.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Rh1 P1 C1 58.34(16) . . . . ? C26 Rh1 P1 C1 -101.77(18) . . . . ? C27 Rh1 P1 C1 -139.62(18) . . . . ? C22 Rh1 P1 C1 142.1(3) . . . . ? C23 Rh1 P1 C1 -40.4(5) . . . . ? N2 Rh1 P1 C16 178.34(18) . . . . ? C26 Rh1 P1 C16 18.23(19) . . . . ? C27 Rh1 P1 C16 -19.62(19) . . . . ? C22 Rh1 P1 C16 -97.9(3) . . . . ? C23 Rh1 P1 C16 79.6(5) . . . . ? N2 Rh1 P1 C10 -61.41(16) . . . . ? C26 Rh1 P1 C10 138.49(17) . . . . ? C27 Rh1 P1 C10 100.64(17) . . . . ? C22 Rh1 P1 C10 22.3(3) . . . . ? C23 Rh1 P1 C10 -160.2(5) . . . . ? C26 Rh1 N2 C30 -100.4(19) . . . . ? C27 Rh1 N2 C30 51(2) . . . . ? C22 Rh1 N2 C30 0.5(18) . . . . ? C23 Rh1 N2 C30 -35.3(18) . . . . ? P1 Rh1 N2 C30 156.6(18) . . . . ? C8 N1 C1 C2 -1.0(4) . . . . ? C8 N1 C1 P1 -179.0(3) . . . . ? C16 P1 C1 C2 -116.3(4) . . . . ? C10 P1 C1 C2 135.7(4) . . . . ? Rh1 P1 C1 C2 12.4(4) . . . . ? C16 P1 C1 N1 61.3(3) . . . . ? C10 P1 C1 N1 -46.7(3) . . . . ? Rh1 P1 C1 N1 -170.1(3) . . . . ? N1 C1 C2 C3 0.3(4) . . . . ? P1 C1 C2 C3 178.2(3) . . . . ? N1 C1 C2 C9 -179.2(4) . . . . ? P1 C1 C2 C9 -1.4(6) . . . . ? C1 C2 C3 C4 178.8(5) . . . . ? C9 C2 C3 C4 -1.7(7) . . . . ? C1 C2 C3 C8 0.4(4) . . . . ? C9 C2 C3 C8 179.9(4) . . . . ? C8 C3 C4 C5 1.1(7) . . . . ? C2 C3 C4 C5 -177.1(5) . . . . ? C3 C4 C5 C6 -0.5(7) . . . . ? C4 C5 C6 C7 0.0(7) . . . . ? C5 C6 C7 C8 -0.1(7) . . . . ? C1 N1 C8 C7 -177.0(4) . . . . ? C1 N1 C8 C3 1.2(4) . . . . ? C6 C7 C8 N1 178.7(4) . . . . ? C6 C7 C8 C3 0.7(6) . . . . ? C4 C3 C8 N1 -179.6(4) . . . . ? C2 C3 C8 N1 -1.0(4) . . . . ? C4 C3 C8 C7 -1.2(6) . . . . ? C2 C3 C8 C7 177.5(4) . . . . ? C1 P1 C10 C15 -115.6(3) . . . . ? C16 P1 C10 C15 137.1(3) . . . . ? Rh1 P1 C10 C15 8.6(3) . . . . ? C1 P1 C10 C11 64.5(3) . . . . ? C16 P1 C10 C11 -42.8(4) . . . . ? Rh1 P1 C10 C11 -171.4(3) . . . . ? C15 C10 C11 C12 2.0(6) . . . . ? P1 C10 C11 C12 -178.0(3) . . . . ? C10 C11 C12 C13 -1.9(6) . . . . ? C11 C12 C13 C14 0.7(6) . . . . ? C12 C13 C14 C15 0.4(6) . . . . ? C13 C14 C15 C10 -0.3(6) . . . . ? C11 C10 C15 C14 -1.0(6) . . . . ? P1 C10 C15 C14 179.1(3) . . . . ? C1 P1 C16 C21 34.6(3) . . . . ? C10 P1 C16 C21 144.4(3) . . . . ? Rh1 P1 C16 C21 -90.9(3) . . . . ? C1 P1 C16 C17 -149.8(3) . . . . ? C10 P1 C16 C17 -40.1(3) . . . . ? Rh1 P1 C16 C17 84.6(3) . . . . ? C21 C16 C17 C18 -1.6(6) . . . . ? P1 C16 C17 C18 -177.1(3) . . . . ? C16 C17 C18 C19 1.3(6) . . . . ? C17 C18 C19 C20 -0.3(6) . . . . ? C18 C19 C20 C21 -0.4(6) . . . . ? C17 C16 C21 C20 0.8(6) . . . . ? P1 C16 C21 C20 176.4(3) . . . . ? C19 C20 C21 C16 0.2(6) . . . . ? N2 Rh1 C22 C23 -96.2(2) . . . . ? C26 Rh1 C22 C23 63.6(2) . . . . ? C27 Rh1 C22 C23 98.3(2) . . . . ? P1 Rh1 C22 C23 179.12(19) . . . . ? N2 Rh1 C22 C29 140.2(3) . . . . ? C26 Rh1 C22 C29 -60.0(3) . . . . ? C27 Rh1 C22 C29 -25.4(3) . . . . ? C23 Rh1 C22 C29 -123.7(4) . . . . ? P1 Rh1 C22 C29 55.5(4) . . . . ? C29 C22 C23 C24 -5.1(6) . . . . ? Rh1 C22 C23 C24 -102.7(3) . . . . ? C29 C22 C23 Rh1 97.6(4) . . . . ? N2 Rh1 C23 C22 82.9(2) . . . . ? C26 Rh1 C23 C22 -115.8(3) . . . . ? C27 Rh1 C23 C22 -78.5(2) . . . . ? P1 Rh1 C23 C22 -178.3(4) . . . . ? N2 Rh1 C23 C24 -156.2(3) . . . . ? C26 Rh1 C23 C24 5.1(3) . . . . ? C27 Rh1 C23 C24 42.4(3) . . . . ? C22 Rh1 C23 C24 120.9(4) . . . . ? P1 Rh1 C23 C24 -57.4(6) . . . . ? C22 C23 C24 C25 96.0(4) . . . . ? Rh1 C23 C24 C25 15.2(4) . . . . ? C23 C24 C25 C26 -37.7(5) . . . . ? C24 C25 C26 C27 -39.1(5) . . . . ? C24 C25 C26 Rh1 41.5(4) . . . . ? N2 Rh1 C26 C27 165.7(3) . . . . ? C22 Rh1 C26 C27 66.7(2) . . . . ? C23 Rh1 C26 C27 98.9(2) . . . . ? P1 Rh1 C26 C27 -91.7(2) . . . . ? N2 Rh1 C26 C25 42.4(6) . . . . ? C27 Rh1 C26 C25 -123.3(4) . . . . ? C22 Rh1 C26 C25 -56.6(3) . . . . ? C23 Rh1 C26 C25 -24.4(3) . . . . ? P1 Rh1 C26 C25 145.0(3) . . . . ? C25 C26 C27 C28 -3.9(6) . . . . ? Rh1 C26 C27 C28 -104.3(4) . . . . ? C25 C26 C27 Rh1 100.3(4) . . . . ? N2 Rh1 C27 C26 -164.3(4) . . . . ? C22 Rh1 C27 C26 -112.9(2) . . . . ? C23 Rh1 C27 C26 -77.4(2) . . . . ? P1 Rh1 C27 C26 90.8(2) . . . . ? N2 Rh1 C27 C28 -42.6(6) . . . . ? C26 Rh1 C27 C28 121.8(4) . . . . ? C22 Rh1 C27 C28 8.8(3) . . . . ? C23 Rh1 C27 C28 44.4(3) . . . . ? P1 Rh1 C27 C28 -147.4(3) . . . . ? C26 C27 C28 C29 92.0(5) . . . . ? Rh1 C27 C28 C29 10.1(5) . . . . ? C23 C22 C29 C28 -41.2(6) . . . . ? Rh1 C22 C29 C28 39.2(4) . . . . ? C27 C28 C29 C22 -34.1(5) . . . . ? Rh1 N2 C30 C31 -53(27) . . . . ? C35 O1 C32 C33 -15.3(8) . . . . ? C32 O1 C35 C34 -10.4(9) . . . . ? O1 C32 C33 C34 33.5(7) . . . . ? O1 C35 C34 C33 31.0(7) . . . . ? C32 C33 C34 C35 -40.4(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.814 _refine_diff_density_min -0.799 _refine_diff_density_rms 0.105 #===END data_y051_0m _database_code_depnum_ccdc_archive 'CCDC 772901' #TrackingRef '- Complexes 1_2_3_4_8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H51 N2 P Rh2, 2(B F4), 1.5(C H2 Cl2)' _chemical_formula_sum 'C46.50 H54 B2 Cl3 F8 N2 P Rh2' _chemical_formula_weight 1157.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall -P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.0623(4) _cell_length_b 11.2983(4) _cell_length_c 19.1151(7) _cell_angle_alpha 92.954(2) _cell_angle_beta 98.481(2) _cell_angle_gamma 99.342(2) _cell_volume 2324.66(15) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9918 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1170 _exptl_absorpt_coefficient_mu 0.986 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.715295 _exptl_absorpt_correction_T_max 0.797792 _exptl_absorpt_process_details 'SADABS V2008/1' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Apex II with CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32973 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0383 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.51 _reflns_number_total 10602 _reflns_number_gt 8222 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex II (Bruker-AXS, 2007)' _computing_cell_refinement 'Apex II (Bruker-AXS, 2007)' _computing_data_reduction ; SAINT v7.34A (Bruker-AXS, 2007) & XPREP v2005/4 (Bruker-AXS, 2005) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+7.5634P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10602 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0675 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1302 _refine_ls_wR_factor_gt 0.1171 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _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 0.56899(3) 0.56186(3) 0.208324(17) 0.02474(10) Uani 1 1 d . . . Rh2 Rh 0.15097(3) 0.08918(3) 0.222732(16) 0.02160(9) Uani 1 1 d . . . P1 P 0.31169(10) 0.16036(9) 0.31490(5) 0.0205(2) Uani 1 1 d . . . N2 N 0.0726(4) 0.2453(3) 0.23475(19) 0.0279(8) Uani 1 1 d . . . N1 N 0.4314(3) 0.2673(3) 0.21025(17) 0.0238(7) Uani 1 1 d . . . H1 H 0.3723 0.2298 0.1768 0.029 Uiso 1 1 calc R . . C1 C 0.4367(4) 0.2541(4) 0.2823(2) 0.0218(8) Uani 1 1 d . . . C2 C 0.5416(4) 0.3268(4) 0.3191(2) 0.0228(8) Uani 1 1 d . . . C3 C 0.6046(4) 0.3850(4) 0.2669(2) 0.0233(8) Uani 1 1 d . . . C4 C 0.7152(4) 0.4721(4) 0.2706(2) 0.0262(9) Uani 1 1 d . . . H4 H 0.7613 0.5097 0.3175 0.031 Uiso 1 1 calc R . . C5 C 0.7583(4) 0.5048(4) 0.2068(3) 0.0321(10) Uani 1 1 d . . . H5 H 0.8339 0.5677 0.2088 0.039 Uiso 1 1 calc R . . C6 C 0.6831(4) 0.4666(4) 0.1414(2) 0.0315(10) Uani 1 1 d . . . H6 H 0.7068 0.5037 0.0979 0.038 Uiso 1 1 calc R . . C7 C 0.5667(5) 0.3963(4) 0.1369(2) 0.0294(9) Uani 1 1 d . . . H7 H 0.5093 0.3799 0.0906 0.035 Uiso 1 1 calc R . . C8 C 0.5313(4) 0.3468(4) 0.1995(2) 0.0256(9) Uani 1 1 d . . . C9 C 0.5855(4) 0.3455(4) 0.3974(2) 0.0265(9) Uani 1 1 d . . . H9A H 0.5735 0.4252 0.4148 0.040 Uiso 1 1 calc R . . H9B H 0.6737 0.3398 0.4073 0.040 Uiso 1 1 calc R . . H9C H 0.5379 0.2836 0.4214 0.040 Uiso 1 1 calc R . . C10 C 0.2786(4) 0.2623(4) 0.3844(2) 0.0230(8) Uani 1 1 d . . . C11 C 0.2723(4) 0.3804(4) 0.3698(2) 0.0289(9) Uani 1 1 d . . . H11 H 0.2928 0.4076 0.3261 0.035 Uiso 1 1 calc R . . C12 C 0.2366(4) 0.4601(4) 0.4177(3) 0.0338(10) Uani 1 1 d . . . H12 H 0.2326 0.5407 0.4069 0.041 Uiso 1 1 calc R . . C13 C 0.2070(4) 0.4202(4) 0.4814(3) 0.0341(11) Uani 1 1 d . . . H13 H 0.1816 0.4733 0.5143 0.041 Uiso 1 1 calc R . . C14 C 0.2145(4) 0.3033(4) 0.4973(2) 0.0306(10) Uani 1 1 d . . . H14 H 0.1955 0.2769 0.5414 0.037 Uiso 1 1 calc R . . C15 C 0.2492(4) 0.2245(4) 0.4493(2) 0.0258(9) Uani 1 1 d . . . H15 H 0.2532 0.1441 0.4606 0.031 Uiso 1 1 calc R . . C16 C 0.3867(4) 0.0472(4) 0.3613(2) 0.0218(8) Uani 1 1 d . . . C17 C 0.5123(4) 0.0410(4) 0.3624(2) 0.0256(9) Uani 1 1 d . . . H17 H 0.5620 0.0965 0.3382 0.031 Uiso 1 1 calc R . . C18 C 0.5637(4) -0.0463(4) 0.3988(2) 0.0284(9) Uani 1 1 d . . . H18 H 0.6489 -0.0505 0.3992 0.034 Uiso 1 1 calc R . . C19 C 0.4929(4) -0.1275(4) 0.4344(2) 0.0294(9) Uani 1 1 d . . . H19 H 0.5297 -0.1859 0.4600 0.035 Uiso 1 1 calc R . . C20 C 0.3679(4) -0.1232(4) 0.4328(2) 0.0282(9) Uani 1 1 d . . . H20 H 0.3188 -0.1788 0.4572 0.034 Uiso 1 1 calc R . . C21 C 0.3149(4) -0.0374(4) 0.3953(2) 0.0259(9) Uani 1 1 d . . . H21 H 0.2287 -0.0365 0.3929 0.031 Uiso 1 1 calc R . . C22 C 0.3935(5) 0.5925(5) 0.1577(2) 0.0342(10) Uani 1 1 d . . . H22 H 0.3475 0.5259 0.1225 0.041 Uiso 1 1 calc R . . C23 C 0.4859(5) 0.6695(5) 0.1322(3) 0.0410(12) Uani 1 1 d . . . H23 H 0.4951 0.6482 0.0821 0.049 Uiso 1 1 calc R . . C24 C 0.5185(7) 0.8033(5) 0.1548(3) 0.0568(16) Uani 1 1 d . . . H24A H 0.5463 0.8465 0.1147 0.068 Uiso 1 1 calc R . . H24B H 0.4428 0.8322 0.1653 0.068 Uiso 1 1 calc R . . C25 C 0.6162(6) 0.8340(5) 0.2176(4) 0.0530(15) Uani 1 1 d . . . H25A H 0.6006 0.9056 0.2446 0.064 Uiso 1 1 calc R . . H25B H 0.6973 0.8558 0.2014 0.064 Uiso 1 1 calc R . . C26 C 0.6236(5) 0.7334(4) 0.2665(3) 0.0355(11) Uani 1 1 d . . . H26 H 0.7044 0.7420 0.2992 0.043 Uiso 1 1 calc R . . C27 C 0.5235(5) 0.6693(4) 0.2930(2) 0.0334(10) Uani 1 1 d . . . H27 H 0.5453 0.6409 0.3412 0.040 Uiso 1 1 calc R . . C28 C 0.3934(5) 0.6980(5) 0.2773(3) 0.0414(12) Uani 1 1 d . . . H28A H 0.3498 0.6771 0.3179 0.050 Uiso 1 1 calc R . . H28B H 0.3992 0.7857 0.2734 0.050 Uiso 1 1 calc R . . C29 C 0.3179(5) 0.6335(5) 0.2113(3) 0.0436(13) Uani 1 1 d . . . H29A H 0.2640 0.6872 0.1887 0.052 Uiso 1 1 calc R . . H29B H 0.2634 0.5623 0.2242 0.052 Uiso 1 1 calc R . . C30 C -0.0256(4) -0.0013(5) 0.1552(2) 0.0316(10) Uani 1 1 d . . . H30 H -0.0975 0.0411 0.1581 0.038 Uiso 1 1 calc R . . C31 C 0.0530(4) 0.0474(5) 0.1103(2) 0.0326(10) Uani 1 1 d . . . H31 H 0.0276 0.1190 0.0874 0.039 Uiso 1 1 calc R . . C32 C 0.1249(4) -0.0234(5) 0.0667(2) 0.0329(10) Uani 1 1 d . . . H32A H 0.1311 0.0140 0.0214 0.039 Uiso 1 1 calc R . . H32B H 0.0782 -0.1063 0.0554 0.039 Uiso 1 1 calc R . . C33 C 0.2566(4) -0.0292(5) 0.1047(2) 0.0313(10) Uani 1 1 d . . . H33A H 0.2822 -0.1036 0.0867 0.038 Uiso 1 1 calc R . . H33B H 0.3150 0.0400 0.0927 0.038 Uiso 1 1 calc R . . C34 C 0.2668(4) -0.0277(4) 0.1849(2) 0.0262(9) Uani 1 1 d . . . H34 H 0.3540 -0.0131 0.2107 0.031 Uiso 1 1 calc R . . C35 C 0.1819(4) -0.0946(4) 0.2202(2) 0.0264(9) Uani 1 1 d . . . H35 H 0.2195 -0.1184 0.2671 0.032 Uiso 1 1 calc R . . C36 C 0.0697(4) -0.1849(4) 0.1835(2) 0.0320(10) Uani 1 1 d . . . H36A H 0.0864 -0.2142 0.1367 0.038 Uiso 1 1 calc R . . H36B H 0.0571 -0.2549 0.2123 0.038 Uiso 1 1 calc R . . C37 C -0.0480(4) -0.1303(5) 0.1729(3) 0.0360(11) Uani 1 1 d . . . H37A H -0.1081 -0.1781 0.1341 0.043 Uiso 1 1 calc R . . H37B H -0.0856 -0.1352 0.2168 0.043 Uiso 1 1 calc R . . C38 C 0.0989(6) 0.3372(5) 0.1846(3) 0.0434(13) Uani 1 1 d . . . H38A H 0.0550 0.3074 0.1371 0.065 Uiso 1 1 calc R . . H38B H 0.1884 0.3542 0.1837 0.065 Uiso 1 1 calc R . . H38C H 0.0709 0.4110 0.1997 0.065 Uiso 1 1 calc R . . C39 C 0.0068(4) 0.2735(4) 0.2807(2) 0.0286(9) Uani 1 1 d . . . H39 H -0.0184 0.3499 0.2783 0.034 Uiso 1 1 calc R . . C40 C -0.0337(4) 0.2004(4) 0.3365(2) 0.0256(9) Uani 1 1 d . . . C41 C -0.0725(4) 0.2610(4) 0.3927(3) 0.0314(10) Uani 1 1 d . . . H41 H -0.0759 0.3443 0.3917 0.038 Uiso 1 1 calc R . . C42 C -0.1060(4) 0.1991(5) 0.4499(3) 0.0357(11) Uani 1 1 d . . . H42 H -0.1303 0.2406 0.4886 0.043 Uiso 1 1 calc R . . C43 C -0.1039(4) 0.0770(5) 0.4503(3) 0.0360(11) Uani 1 1 d . . . H43 H -0.1272 0.0349 0.4893 0.043 Uiso 1 1 calc R . . C44 C -0.0677(4) 0.0148(4) 0.3937(2) 0.0315(10) Uani 1 1 d . . . H44 H -0.0678 -0.0693 0.3939 0.038 Uiso 1 1 calc R . . C45 C -0.0323(4) 0.0768(4) 0.3383(2) 0.0264(9) Uani 1 1 d . . . H45 H -0.0063 0.0351 0.3003 0.032 Uiso 1 1 calc R . . B1 B 0.2630(7) 0.2741(6) 0.0081(3) 0.0469(15) Uani 1 1 d . . . F1 F 0.3338(4) 0.3823(3) -0.00190(18) 0.0668(11) Uani 1 1 d . . . F2 F 0.1362(4) 0.2779(4) -0.0098(2) 0.0854(14) Uani 1 1 d . . . F3 F 0.2837(3) 0.2577(3) 0.07956(15) 0.0548(9) Uani 1 1 d . . . F4 F 0.2895(4) 0.1821(4) -0.0323(2) 0.0681(11) Uani 1 1 d . . . B2 B 0.0113(5) 0.6471(5) 0.3501(3) 0.0328(11) Uani 1 1 d . . . F5 F -0.0762(3) 0.7189(3) 0.32653(17) 0.0460(7) Uani 1 1 d . . . F6 F 0.1189(3) 0.7207(3) 0.38212(18) 0.0505(8) Uani 1 1 d . . . F7 F -0.0369(3) 0.5709(3) 0.39690(17) 0.0471(8) Uani 1 1 d . . . F8 F 0.0354(3) 0.5794(3) 0.29235(15) 0.0404(7) Uani 1 1 d . . . C46A C 0.6891(6) 0.1058(7) 0.0829(4) 0.0617(17) Uani 0.50 1 d P A 1 H46A H 0.7553 0.1601 0.0650 0.074 Uiso 0.50 1 calc PR A 1 H46B H 0.7027 0.0223 0.0739 0.074 Uiso 0.50 1 calc PR A 1 Cl1A Cl 0.70225(18) 0.13855(16) 0.17576(9) 0.0638(4) Uani 0.50 1 d P A 1 Cl2A Cl 0.5530(3) 0.1205(3) 0.03802(14) 0.0478(6) Uani 0.50 1 d P A 1 C46B C 0.6891(6) 0.1058(7) 0.0829(4) 0.0617(17) Uani 0.50 1 d P B 2 H46C H 0.6016 0.0964 0.0597 0.074 Uiso 0.50 1 calc PR B 2 H46D H 0.7213 0.0311 0.0724 0.074 Uiso 0.50 1 calc PR B 2 Cl1B Cl 0.70225(18) 0.13855(16) 0.17576(9) 0.0638(4) Uani 0.50 1 d P B 2 Cl2B Cl 0.7842(4) 0.2370(3) 0.0525(2) 0.0703(10) Uani 0.50 1 d P B 2 C47 C 0.9625(16) 0.4728(14) -0.0135(7) 0.072(5) Uani 0.50 1 d P C 1 H47A H 1.0167 0.4388 -0.0431 0.086 Uiso 0.50 1 calc PR C 1 H47B H 0.9256 0.5343 -0.0403 0.086 Uiso 0.50 1 calc PR C 1 Cl3 Cl 0.8399(4) 0.3551(3) -0.0012(2) 0.0743(10) Uani 0.50 1 d P C 1 Cl4 Cl 1.0496(7) 0.5400(4) 0.0602(3) 0.136(3) Uani 0.50 1 d P C 1 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 0.02397(18) 0.02913(18) 0.02326(17) 0.00193(13) 0.00830(13) 0.00674(14) Rh2 0.01960(17) 0.02863(17) 0.01483(15) -0.00241(12) 0.00010(12) 0.00263(13) P1 0.0191(5) 0.0263(5) 0.0146(4) -0.0020(4) 0.0023(4) 0.0009(4) N2 0.029(2) 0.0323(19) 0.0202(17) 0.0028(14) 0.0005(15) 0.0032(16) N1 0.0218(18) 0.0324(19) 0.0156(16) -0.0018(14) 0.0039(13) -0.0002(15) C1 0.020(2) 0.028(2) 0.0167(18) -0.0027(15) 0.0031(15) 0.0034(16) C2 0.021(2) 0.027(2) 0.0201(19) -0.0001(15) 0.0046(16) 0.0035(16) C3 0.020(2) 0.028(2) 0.023(2) 0.0008(16) 0.0048(16) 0.0050(16) C4 0.021(2) 0.028(2) 0.030(2) 0.0000(17) 0.0055(17) 0.0047(17) C5 0.026(2) 0.034(2) 0.041(3) 0.008(2) 0.014(2) 0.0077(19) C6 0.035(3) 0.036(2) 0.029(2) 0.0032(19) 0.0134(19) 0.015(2) C7 0.040(3) 0.032(2) 0.022(2) 0.0045(17) 0.0150(19) 0.013(2) C8 0.026(2) 0.030(2) 0.023(2) -0.0021(16) 0.0062(17) 0.0081(17) C9 0.024(2) 0.035(2) 0.0176(19) -0.0011(16) 0.0008(16) -0.0013(18) C10 0.0166(19) 0.033(2) 0.0177(18) -0.0037(16) 0.0031(15) 0.0004(16) C11 0.023(2) 0.035(2) 0.026(2) -0.0051(18) 0.0032(17) -0.0012(18) C12 0.026(2) 0.030(2) 0.042(3) -0.009(2) 0.004(2) -0.0007(18) C13 0.025(2) 0.041(3) 0.034(2) -0.016(2) 0.0069(19) 0.001(2) C14 0.023(2) 0.046(3) 0.021(2) -0.0078(18) 0.0064(17) 0.0009(19) C15 0.019(2) 0.037(2) 0.0201(19) -0.0017(17) 0.0024(16) 0.0019(17) C16 0.022(2) 0.028(2) 0.0131(17) -0.0030(15) -0.0010(15) 0.0034(16) C17 0.023(2) 0.031(2) 0.0205(19) -0.0046(16) 0.0018(16) 0.0004(17) C18 0.021(2) 0.033(2) 0.029(2) -0.0027(18) -0.0028(17) 0.0052(18) C19 0.028(2) 0.035(2) 0.022(2) -0.0009(17) -0.0064(17) 0.0059(19) C20 0.030(2) 0.034(2) 0.0177(19) 0.0021(17) 0.0017(17) 0.0002(18) C21 0.024(2) 0.033(2) 0.0181(19) -0.0035(16) 0.0018(16) 0.0003(17) C22 0.034(3) 0.044(3) 0.026(2) -0.0021(19) 0.0007(19) 0.017(2) C23 0.053(3) 0.047(3) 0.027(2) 0.010(2) 0.008(2) 0.019(3) C24 0.078(5) 0.046(3) 0.053(4) 0.020(3) 0.019(3) 0.016(3) C25 0.058(4) 0.035(3) 0.068(4) 0.005(3) 0.018(3) 0.008(3) C26 0.033(3) 0.033(2) 0.040(3) -0.005(2) 0.004(2) 0.008(2) C27 0.035(3) 0.039(3) 0.027(2) -0.0042(19) 0.0045(19) 0.012(2) C28 0.034(3) 0.059(3) 0.036(3) -0.003(2) 0.013(2) 0.016(2) C29 0.031(3) 0.052(3) 0.047(3) -0.011(2) 0.004(2) 0.012(2) C30 0.020(2) 0.049(3) 0.022(2) -0.0108(19) -0.0057(17) 0.0056(19) C31 0.032(2) 0.045(3) 0.0176(19) -0.0087(18) -0.0085(17) 0.011(2) C32 0.034(3) 0.046(3) 0.0171(19) -0.0034(18) -0.0007(18) 0.009(2) C33 0.029(2) 0.045(3) 0.020(2) -0.0030(18) 0.0057(18) 0.009(2) C34 0.026(2) 0.033(2) 0.0194(19) -0.0062(16) -0.0001(16) 0.0088(18) C35 0.031(2) 0.029(2) 0.0188(19) -0.0020(16) 0.0010(17) 0.0072(18) C36 0.035(3) 0.034(2) 0.025(2) -0.0060(18) 0.0051(19) 0.002(2) C37 0.028(2) 0.045(3) 0.029(2) -0.012(2) 0.0030(19) -0.003(2) C38 0.063(4) 0.036(3) 0.034(3) 0.006(2) 0.012(2) 0.011(2) C39 0.025(2) 0.029(2) 0.030(2) -0.0010(18) -0.0025(18) 0.0080(18) C40 0.0159(19) 0.031(2) 0.028(2) -0.0043(17) 0.0012(16) 0.0040(17) C41 0.020(2) 0.035(2) 0.038(3) -0.003(2) 0.0050(19) 0.0049(18) C42 0.024(2) 0.050(3) 0.033(2) -0.006(2) 0.0099(19) 0.007(2) C43 0.024(2) 0.047(3) 0.036(3) 0.002(2) 0.010(2) -0.002(2) C44 0.026(2) 0.033(2) 0.033(2) 0.0001(19) 0.0041(19) -0.0006(19) C45 0.017(2) 0.033(2) 0.028(2) -0.0045(17) 0.0043(16) 0.0017(17) B1 0.063(4) 0.047(4) 0.027(3) 0.001(2) 0.003(3) 0.003(3) F1 0.104(3) 0.057(2) 0.0411(19) 0.0148(16) 0.021(2) 0.008(2) F2 0.075(3) 0.100(3) 0.075(3) -0.028(2) -0.020(2) 0.036(3) F3 0.058(2) 0.076(2) 0.0217(14) 0.0062(14) 0.0025(14) -0.0108(17) F4 0.087(3) 0.071(2) 0.050(2) -0.0097(18) 0.016(2) 0.024(2) B2 0.030(3) 0.031(3) 0.036(3) -0.003(2) 0.007(2) 0.002(2) F5 0.0453(18) 0.0383(16) 0.0546(19) -0.0024(14) 0.0020(15) 0.0145(14) F6 0.0369(17) 0.0540(19) 0.0528(19) -0.0104(15) 0.0041(14) -0.0081(14) F7 0.0493(19) 0.0446(17) 0.0513(19) 0.0075(14) 0.0231(15) 0.0049(14) F8 0.0466(17) 0.0410(16) 0.0361(15) -0.0029(12) 0.0117(13) 0.0121(13) C46A 0.054(4) 0.068(4) 0.061(4) -0.012(3) 0.011(3) 0.008(3) Cl1A 0.0740(11) 0.0658(10) 0.0642(10) 0.0090(8) 0.0195(8) 0.0402(9) Cl2A 0.0385(14) 0.0665(18) 0.0391(13) -0.0061(12) 0.0017(11) 0.0187(13) C46B 0.054(4) 0.068(4) 0.061(4) -0.012(3) 0.011(3) 0.008(3) Cl1B 0.0740(11) 0.0658(10) 0.0642(10) 0.0090(8) 0.0195(8) 0.0402(9) Cl2B 0.096(3) 0.0538(18) 0.067(2) -0.0120(16) 0.036(2) 0.0161(18) C47 0.095(13) 0.076(11) 0.031(7) -0.011(6) -0.031(7) 0.016(8) Cl3 0.090(3) 0.061(2) 0.077(2) -0.0123(17) 0.036(2) 0.0134(19) Cl4 0.214(7) 0.048(2) 0.110(4) -0.006(2) -0.084(4) 0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C22 2.127(5) . ? Rh1 C26 2.134(5) . ? Rh1 C27 2.140(5) . ? Rh1 C23 2.142(5) . ? Rh1 C7 2.252(4) . ? Rh1 C4 2.270(4) . ? Rh1 C6 2.273(4) . ? Rh1 C5 2.293(5) . ? Rh1 C8 2.391(4) . ? Rh1 C3 2.399(4) . ? Rh2 N2 2.105(4) . ? Rh2 C34 2.153(4) . ? Rh2 C35 2.158(4) . ? Rh2 C30 2.236(4) . ? Rh2 C31 2.249(4) . ? Rh2 P1 2.3190(10) . ? P1 C1 1.808(4) . ? P1 C10 1.830(4) . ? P1 C16 1.831(4) . ? N2 C39 1.280(6) . ? N2 C38 1.472(6) . ? N1 C8 1.354(6) . ? N1 C1 1.387(5) . ? N1 H1 0.8800 . ? C1 C2 1.381(6) . ? C2 C3 1.428(6) . ? C2 C9 1.497(5) . ? C3 C8 1.423(6) . ? C3 C4 1.431(6) . ? C4 C5 1.419(6) . ? C4 H4 1.0000 . ? C5 C6 1.401(7) . ? C5 H5 1.0000 . ? C6 C7 1.387(7) . ? C6 H6 1.0000 . ? C7 C8 1.426(6) . ? C7 H7 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.389(6) . ? C10 C15 1.399(6) . ? C11 C12 1.395(6) . ? C11 H11 0.9500 . ? C12 C13 1.385(7) . ? C12 H12 0.9500 . ? C13 C14 1.383(7) . ? C13 H13 0.9500 . ? C14 C15 1.382(6) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C21 1.392(6) . ? C16 C17 1.399(6) . ? C17 C18 1.385(6) . ? C17 H17 0.9500 . ? C18 C19 1.381(7) . ? C18 H18 0.9500 . ? C19 C20 1.387(6) . ? C19 H19 0.9500 . ? C20 C21 1.389(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.393(7) . ? C22 C29 1.514(7) . ? C22 H22 1.0000 . ? C23 C24 1.520(8) . ? C23 H23 1.0000 . ? C24 C25 1.476(9) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.513(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.397(7) . ? C26 H26 1.0000 . ? C27 C28 1.517(7) . ? C27 H27 1.0000 . ? C28 C29 1.489(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.381(7) . ? C30 C37 1.503(7) . ? C30 H30 1.0000 . ? C31 C32 1.516(6) . ? C31 H31 1.0000 . ? C32 C33 1.543(6) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.520(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.385(6) . ? C34 H34 1.0000 . ? C35 C36 1.528(6) . ? C35 H35 1.0000 . ? C36 C37 1.521(7) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.459(6) . ? C39 H39 0.9500 . ? C40 C41 1.400(6) . ? C40 C45 1.402(6) . ? C41 C42 1.391(7) . ? C41 H41 0.9500 . ? C42 C43 1.384(7) . ? C42 H42 0.9500 . ? C43 C44 1.401(7) . ? C43 H43 0.9500 . ? C44 C45 1.370(6) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? B1 F4 1.358(7) . ? B1 F3 1.379(7) . ? B1 F1 1.379(8) . ? B1 F2 1.402(8) . ? B2 F6 1.376(6) . ? B2 F7 1.378(6) . ? B2 F8 1.392(6) . ? B2 F5 1.400(6) . ? C46A Cl2A 1.657(7) . ? C46A Cl1A 1.774(7) . ? C46A H46A 0.9900 . ? C46A H46B 0.9900 . ? C47 Cl4 1.656(15) . ? C47 Cl3 1.789(18) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Rh1 C26 96.56(19) . . ? C22 Rh1 C27 81.59(18) . . ? C26 Rh1 C27 38.14(19) . . ? C22 Rh1 C23 38.1(2) . . ? C26 Rh1 C23 81.0(2) . . ? C27 Rh1 C23 90.40(19) . . ? C22 Rh1 C7 93.94(18) . . ? C26 Rh1 C7 162.94(18) . . ? C27 Rh1 C7 157.96(18) . . ? C23 Rh1 C7 99.36(19) . . ? C22 Rh1 C4 160.64(18) . . ? C26 Rh1 C4 96.01(18) . . ? C27 Rh1 C4 99.58(17) . . ? C23 Rh1 C4 159.83(19) . . ? C7 Rh1 C4 77.68(16) . . ? C22 Rh1 C6 117.24(18) . . ? C26 Rh1 C6 127.31(19) . . ? C27 Rh1 C6 160.15(19) . . ? C23 Rh1 C6 100.92(18) . . ? C7 Rh1 C6 35.70(17) . . ? C4 Rh1 C6 64.95(16) . . ? C22 Rh1 C5 152.42(18) . . ? C26 Rh1 C5 100.74(19) . . ? C27 Rh1 C5 124.73(18) . . ? C23 Rh1 C5 124.42(19) . . ? C7 Rh1 C5 64.80(18) . . ? C4 Rh1 C5 36.24(16) . . ? C6 Rh1 C5 35.73(17) . . ? C22 Rh1 C8 99.47(18) . . ? C26 Rh1 C8 152.85(17) . . ? C27 Rh1 C8 123.58(17) . . ? C23 Rh1 C8 124.35(19) . . ? C7 Rh1 C8 35.62(14) . . ? C4 Rh1 C8 63.61(15) . . ? C6 Rh1 C8 62.44(16) . . ? C5 Rh1 C8 73.90(16) . . ? C22 Rh1 C3 125.11(17) . . ? C26 Rh1 C3 118.96(17) . . ? C27 Rh1 C3 100.86(17) . . ? C23 Rh1 C3 158.41(19) . . ? C7 Rh1 C3 64.11(15) . . ? C4 Rh1 C3 35.55(14) . . ? C6 Rh1 C3 74.15(15) . . ? C5 Rh1 C3 63.10(15) . . ? C8 Rh1 C3 34.57(14) . . ? N2 Rh2 C34 158.47(16) . . ? N2 Rh2 C35 163.28(16) . . ? C34 Rh2 C35 37.48(17) . . ? N2 Rh2 C30 89.51(16) . . ? C34 Rh2 C30 96.14(17) . . ? C35 Rh2 C30 80.16(18) . . ? N2 Rh2 C31 92.17(16) . . ? C34 Rh2 C31 80.71(16) . . ? C35 Rh2 C31 87.14(17) . . ? C30 Rh2 C31 35.87(18) . . ? N2 Rh2 P1 91.40(10) . . ? C34 Rh2 P1 88.13(12) . . ? C35 Rh2 P1 95.47(12) . . ? C30 Rh2 P1 165.85(13) . . ? C31 Rh2 P1 158.06(13) . . ? C1 P1 C10 101.32(19) . . ? C1 P1 C16 104.14(19) . . ? C10 P1 C16 105.73(18) . . ? C1 P1 Rh2 110.40(13) . . ? C10 P1 Rh2 116.88(14) . . ? C16 P1 Rh2 116.59(13) . . ? C39 N2 C38 114.7(4) . . ? C39 N2 Rh2 129.2(3) . . ? C38 N2 Rh2 116.1(3) . . ? C8 N1 C1 109.4(3) . . ? C8 N1 H1 125.3 . . ? C1 N1 H1 125.3 . . ? C2 C1 N1 109.5(4) . . ? C2 C1 P1 130.0(3) . . ? N1 C1 P1 120.3(3) . . ? C1 C2 C3 106.1(4) . . ? C1 C2 C9 129.2(4) . . ? C3 C2 C9 124.7(4) . . ? C8 C3 C2 107.4(4) . . ? C8 C3 C4 119.0(4) . . ? C2 C3 C4 133.5(4) . . ? C8 C3 Rh1 72.4(2) . . ? C2 C3 Rh1 129.4(3) . . ? C4 C3 Rh1 67.3(2) . . ? C5 C4 C3 119.1(4) . . ? C5 C4 Rh1 72.8(3) . . ? C3 C4 Rh1 77.1(2) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? Rh1 C4 H4 120.5 . . ? C6 C5 C4 119.8(4) . . ? C6 C5 Rh1 71.4(3) . . ? C4 C5 Rh1 71.0(2) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? Rh1 C5 H5 119.6 . . ? C7 C6 C5 121.8(4) . . ? C7 C6 Rh1 71.3(3) . . ? C5 C6 Rh1 72.9(3) . . ? C7 C6 H6 118.6 . . ? C5 C6 H6 118.6 . . ? Rh1 C6 H6 118.6 . . ? C6 C7 C8 118.6(4) . . ? C6 C7 Rh1 73.0(3) . . ? C8 C7 Rh1 77.5(3) . . ? C6 C7 H7 120.7 . . ? C8 C7 H7 120.7 . . ? Rh1 C7 H7 120.7 . . ? N1 C8 C3 107.6(4) . . ? N1 C8 C7 132.0(4) . . ? C3 C8 C7 120.3(4) . . ? N1 C8 Rh1 130.8(3) . . ? C3 C8 Rh1 73.0(2) . . ? C7 C8 Rh1 66.9(2) . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C15 118.3(4) . . ? C11 C10 P1 118.3(3) . . ? C15 C10 P1 123.1(3) . . ? C10 C11 C12 121.5(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 119.1(5) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.5(4) . . ? C15 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? C14 C15 C10 120.4(4) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? C21 C16 C17 119.0(4) . . ? C21 C16 P1 118.5(3) . . ? C17 C16 P1 122.5(3) . . ? C18 C17 C16 119.8(4) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 120.9(4) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 119.7(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C21 119.8(4) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C20 C21 C16 120.8(4) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? C23 C22 C29 123.3(5) . . ? C23 C22 Rh1 71.6(3) . . ? C29 C22 Rh1 111.2(3) . . ? C23 C22 H22 114.4 . . ? C29 C22 H22 114.4 . . ? Rh1 C22 H22 114.4 . . ? C22 C23 C24 122.9(5) . . ? C22 C23 Rh1 70.4(3) . . ? C24 C23 Rh1 112.7(4) . . ? C22 C23 H23 114.4 . . ? C24 C23 H23 114.4 . . ? Rh1 C23 H23 114.4 . . ? C25 C24 C23 114.0(5) . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24B 108.8 . . ? C23 C24 H24B 108.8 . . ? H24A C24 H24B 107.6 . . ? C24 C25 C26 113.7(5) . . ? C24 C25 H25A 108.8 . . ? C26 C25 H25A 108.8 . . ? C24 C25 H25B 108.8 . . ? C26 C25 H25B 108.8 . . ? H25A C25 H25B 107.7 . . ? C27 C26 C25 125.3(5) . . ? C27 C26 Rh1 71.1(3) . . ? C25 C26 Rh1 110.9(4) . . ? C27 C26 H26 113.9 . . ? C25 C26 H26 113.9 . . ? Rh1 C26 H26 113.9 . . ? C26 C27 C28 122.4(5) . . ? C26 C27 Rh1 70.7(3) . . ? C28 C27 Rh1 112.8(3) . . ? C26 C27 H27 114.5 . . ? C28 C27 H27 114.5 . . ? Rh1 C27 H27 114.5 . . ? C29 C28 C27 114.1(4) . . ? C29 C28 H28A 108.7 . . ? C27 C28 H28A 108.7 . . ? C29 C28 H28B 108.7 . . ? C27 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C28 C29 C22 114.4(4) . . ? C28 C29 H29A 108.7 . . ? C22 C29 H29A 108.7 . . ? C28 C29 H29B 108.7 . . ? C22 C29 H29B 108.7 . . ? H29A C29 H29B 107.6 . . ? C31 C30 C37 126.3(4) . . ? C31 C30 Rh2 72.6(3) . . ? C37 C30 Rh2 107.4(3) . . ? C31 C30 H30 114.0 . . ? C37 C30 H30 114.0 . . ? Rh2 C30 H30 114.0 . . ? C30 C31 C32 125.1(5) . . ? C30 C31 Rh2 71.6(2) . . ? C32 C31 Rh2 111.3(3) . . ? C30 C31 H31 113.8 . . ? C32 C31 H31 113.8 . . ? Rh2 C31 H31 113.8 . . ? C31 C32 C33 113.3(4) . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.7 . . ? C34 C33 C32 113.5(4) . . ? C34 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? C34 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C35 C34 C33 124.5(4) . . ? C35 C34 Rh2 71.5(2) . . ? C33 C34 Rh2 110.4(3) . . ? C35 C34 H34 114.2 . . ? C33 C34 H34 114.2 . . ? Rh2 C34 H34 114.2 . . ? C34 C35 C36 124.2(4) . . ? C34 C35 Rh2 71.0(3) . . ? C36 C35 Rh2 113.5(3) . . ? C34 C35 H35 113.6 . . ? C36 C35 H35 113.6 . . ? Rh2 C35 H35 113.6 . . ? C37 C36 C35 112.2(4) . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C30 C37 C36 113.1(4) . . ? C30 C37 H37A 109.0 . . ? C36 C37 H37A 109.0 . . ? C30 C37 H37B 109.0 . . ? C36 C37 H37B 109.0 . . ? H37A C37 H37B 107.8 . . ? N2 C38 H38A 109.5 . . ? N2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N2 C39 C40 126.8(4) . . ? N2 C39 H39 116.6 . . ? C40 C39 H39 116.6 . . ? C41 C40 C45 118.9(4) . . ? C41 C40 C39 116.5(4) . . ? C45 C40 C39 124.6(4) . . ? C42 C41 C40 120.1(4) . . ? C42 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C43 C42 C41 119.8(4) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C42 C43 C44 120.7(5) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C45 C44 C43 119.1(4) . . ? C45 C44 H44 120.4 . . ? C43 C44 H44 120.4 . . ? C44 C45 C40 121.3(4) . . ? C44 C45 H45 119.3 . . ? C40 C45 H45 119.3 . . ? F4 B1 F3 112.5(5) . . ? F4 B1 F1 111.4(6) . . ? F3 B1 F1 107.4(5) . . ? F4 B1 F2 108.1(5) . . ? F3 B1 F2 106.5(5) . . ? F1 B1 F2 110.8(6) . . ? F6 B2 F7 111.1(4) . . ? F6 B2 F8 109.6(4) . . ? F7 B2 F8 109.4(4) . . ? F6 B2 F5 108.7(4) . . ? F7 B2 F5 108.6(4) . . ? F8 B2 F5 109.4(4) . . ? Cl2A C46A Cl1A 113.7(4) . . ? Cl2A C46A H46A 108.8 . . ? Cl1A C46A H46A 108.8 . . ? Cl2A C46A H46B 108.8 . . ? Cl1A C46A H46B 108.8 . . ? H46A C46A H46B 107.7 . . ? Cl4 C47 Cl3 115.5(9) . . ? Cl4 C47 H47A 108.4 . . ? Cl3 C47 H47A 108.4 . . ? Cl4 C47 H47B 108.4 . . ? Cl3 C47 H47B 108.4 . . ? H47A C47 H47B 107.5 . . ? 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 N2 Rh2 P1 C1 -86.31(18) . . . . ? C34 Rh2 P1 C1 72.15(19) . . . . ? C35 Rh2 P1 C1 108.96(19) . . . . ? C30 Rh2 P1 C1 -179.9(5) . . . . ? C31 Rh2 P1 C1 13.0(4) . . . . ? N2 Rh2 P1 C10 28.74(19) . . . . ? C34 Rh2 P1 C10 -172.8(2) . . . . ? C35 Rh2 P1 C10 -136.0(2) . . . . ? C30 Rh2 P1 C10 -64.8(6) . . . . ? C31 Rh2 P1 C10 128.1(4) . . . . ? N2 Rh2 P1 C16 155.16(18) . . . . ? C34 Rh2 P1 C16 -46.38(19) . . . . ? C35 Rh2 P1 C16 -9.58(19) . . . . ? C30 Rh2 P1 C16 61.6(6) . . . . ? C31 Rh2 P1 C16 -105.5(4) . . . . ? C34 Rh2 N2 C39 -167.1(4) . . . . ? C35 Rh2 N2 C39 35.7(7) . . . . ? C30 Rh2 N2 C39 87.2(4) . . . . ? C31 Rh2 N2 C39 123.0(4) . . . . ? P1 Rh2 N2 C39 -78.7(4) . . . . ? C34 Rh2 N2 C38 11.2(6) . . . . ? C35 Rh2 N2 C38 -145.9(5) . . . . ? C30 Rh2 N2 C38 -94.4(4) . . . . ? C31 Rh2 N2 C38 -58.7(4) . . . . ? P1 Rh2 N2 C38 99.7(3) . . . . ? C8 N1 C1 C2 0.3(5) . . . . ? C8 N1 C1 P1 176.4(3) . . . . ? C10 P1 C1 C2 46.0(4) . . . . ? C16 P1 C1 C2 -63.6(4) . . . . ? Rh2 P1 C1 C2 170.5(4) . . . . ? C10 P1 C1 N1 -129.2(3) . . . . ? C16 P1 C1 N1 121.2(3) . . . . ? Rh2 P1 C1 N1 -4.7(4) . . . . ? N1 C1 C2 C3 -1.3(5) . . . . ? P1 C1 C2 C3 -176.9(3) . . . . ? N1 C1 C2 C9 178.4(4) . . . . ? P1 C1 C2 C9 2.8(7) . . . . ? C1 C2 C3 C8 1.7(5) . . . . ? C9 C2 C3 C8 -178.0(4) . . . . ? C1 C2 C3 C4 178.2(5) . . . . ? C9 C2 C3 C4 -1.5(8) . . . . ? C1 C2 C3 Rh1 83.0(4) . . . . ? C9 C2 C3 Rh1 -96.7(5) . . . . ? C22 Rh1 C3 C8 48.3(3) . . . . ? C26 Rh1 C3 C8 171.6(3) . . . . ? C27 Rh1 C3 C8 135.6(3) . . . . ? C23 Rh1 C3 C8 15.3(6) . . . . ? C7 Rh1 C3 C8 -27.4(2) . . . . ? C4 Rh1 C3 C8 -133.1(4) . . . . ? C6 Rh1 C3 C8 -64.2(3) . . . . ? C5 Rh1 C3 C8 -100.8(3) . . . . ? C22 Rh1 C3 C2 -50.1(4) . . . . ? C26 Rh1 C3 C2 73.2(4) . . . . ? C27 Rh1 C3 C2 37.2(4) . . . . ? C23 Rh1 C3 C2 -83.1(6) . . . . ? C7 Rh1 C3 C2 -125.8(4) . . . . ? C4 Rh1 C3 C2 128.5(5) . . . . ? C6 Rh1 C3 C2 -162.6(4) . . . . ? C5 Rh1 C3 C2 160.8(4) . . . . ? C8 Rh1 C3 C2 -98.4(4) . . . . ? C22 Rh1 C3 C4 -178.6(3) . . . . ? C26 Rh1 C3 C4 -55.3(3) . . . . ? C27 Rh1 C3 C4 -91.3(3) . . . . ? C23 Rh1 C3 C4 148.4(5) . . . . ? C7 Rh1 C3 C4 105.7(3) . . . . ? C6 Rh1 C3 C4 68.9(3) . . . . ? C5 Rh1 C3 C4 32.3(3) . . . . ? C8 Rh1 C3 C4 133.1(4) . . . . ? C8 C3 C4 C5 -9.0(6) . . . . ? C2 C3 C4 C5 174.9(4) . . . . ? Rh1 C3 C4 C5 -61.7(4) . . . . ? C8 C3 C4 Rh1 52.7(4) . . . . ? C2 C3 C4 Rh1 -123.4(5) . . . . ? C22 Rh1 C4 C5 129.8(5) . . . . ? C26 Rh1 C4 C5 -100.0(3) . . . . ? C27 Rh1 C4 C5 -138.3(3) . . . . ? C23 Rh1 C4 C5 -19.6(7) . . . . ? C7 Rh1 C4 C5 63.9(3) . . . . ? C6 Rh1 C4 C5 28.6(3) . . . . ? C8 Rh1 C4 C5 98.8(3) . . . . ? C3 Rh1 C4 C5 126.4(4) . . . . ? C22 Rh1 C4 C3 3.4(6) . . . . ? C26 Rh1 C4 C3 133.6(3) . . . . ? C27 Rh1 C4 C3 95.3(3) . . . . ? C23 Rh1 C4 C3 -146.0(5) . . . . ? C7 Rh1 C4 C3 -62.4(3) . . . . ? C6 Rh1 C4 C3 -97.8(3) . . . . ? C5 Rh1 C4 C3 -126.4(4) . . . . ? C8 Rh1 C4 C3 -27.6(2) . . . . ? C3 C4 C5 C6 9.8(6) . . . . ? Rh1 C4 C5 C6 -54.1(4) . . . . ? C3 C4 C5 Rh1 64.0(4) . . . . ? C22 Rh1 C5 C6 -14.5(5) . . . . ? C26 Rh1 C5 C6 -142.4(3) . . . . ? C27 Rh1 C5 C6 -175.0(3) . . . . ? C23 Rh1 C5 C6 -56.0(4) . . . . ? C7 Rh1 C5 C6 28.0(3) . . . . ? C4 Rh1 C5 C6 132.1(4) . . . . ? C8 Rh1 C5 C6 64.9(3) . . . . ? C3 Rh1 C5 C6 100.4(3) . . . . ? C22 Rh1 C5 C4 -146.6(4) . . . . ? C26 Rh1 C5 C4 85.5(3) . . . . ? C27 Rh1 C5 C4 52.9(3) . . . . ? C23 Rh1 C5 C4 171.9(3) . . . . ? C7 Rh1 C5 C4 -104.1(3) . . . . ? C6 Rh1 C5 C4 -132.1(4) . . . . ? C8 Rh1 C5 C4 -67.1(3) . . . . ? C3 Rh1 C5 C4 -31.7(2) . . . . ? C4 C5 C6 C7 -0.3(7) . . . . ? Rh1 C5 C6 C7 -54.2(4) . . . . ? C4 C5 C6 Rh1 53.9(4) . . . . ? C22 Rh1 C6 C7 -54.2(3) . . . . ? C26 Rh1 C6 C7 -177.9(3) . . . . ? C27 Rh1 C6 C7 145.4(5) . . . . ? C23 Rh1 C6 C7 -90.9(3) . . . . ? C4 Rh1 C6 C7 104.3(3) . . . . ? C5 Rh1 C6 C7 133.3(4) . . . . ? C8 Rh1 C6 C7 32.3(3) . . . . ? C3 Rh1 C6 C7 67.5(3) . . . . ? C22 Rh1 C6 C5 172.5(3) . . . . ? C26 Rh1 C6 C5 48.9(4) . . . . ? C27 Rh1 C6 C5 12.1(7) . . . . ? C23 Rh1 C6 C5 135.9(3) . . . . ? C7 Rh1 C6 C5 -133.3(4) . . . . ? C4 Rh1 C6 C5 -29.0(3) . . . . ? C8 Rh1 C6 C5 -100.9(3) . . . . ? C3 Rh1 C6 C5 -65.8(3) . . . . ? C5 C6 C7 C8 -9.9(7) . . . . ? Rh1 C6 C7 C8 -64.8(4) . . . . ? C5 C6 C7 Rh1 55.0(4) . . . . ? C22 Rh1 C7 C6 133.7(3) . . . . ? C26 Rh1 C7 C6 5.7(7) . . . . ? C27 Rh1 C7 C6 -149.1(4) . . . . ? C23 Rh1 C7 C6 95.7(3) . . . . ? C4 Rh1 C7 C6 -64.0(3) . . . . ? C5 Rh1 C7 C6 -28.0(3) . . . . ? C8 Rh1 C7 C6 -125.5(4) . . . . ? C3 Rh1 C7 C6 -98.9(3) . . . . ? C22 Rh1 C7 C8 -100.8(3) . . . . ? C26 Rh1 C7 C8 131.3(6) . . . . ? C27 Rh1 C7 C8 -23.5(6) . . . . ? C23 Rh1 C7 C8 -138.8(3) . . . . ? C4 Rh1 C7 C8 61.6(3) . . . . ? C6 Rh1 C7 C8 125.5(4) . . . . ? C5 Rh1 C7 C8 97.5(3) . . . . ? C3 Rh1 C7 C8 26.6(2) . . . . ? C1 N1 C8 C3 0.8(5) . . . . ? C1 N1 C8 C7 -176.2(4) . . . . ? C1 N1 C8 Rh1 -81.7(4) . . . . ? C2 C3 C8 N1 -1.6(5) . . . . ? C4 C3 C8 N1 -178.6(4) . . . . ? Rh1 C3 C8 N1 -128.3(3) . . . . ? C2 C3 C8 C7 175.9(4) . . . . ? C4 C3 C8 C7 -1.2(6) . . . . ? Rh1 C3 C8 C7 49.2(4) . . . . ? C2 C3 C8 Rh1 126.7(3) . . . . ? C4 C3 C8 Rh1 -50.3(3) . . . . ? C6 C7 C8 N1 -172.7(4) . . . . ? Rh1 C7 C8 N1 124.9(5) . . . . ? C6 C7 C8 C3 10.5(6) . . . . ? Rh1 C7 C8 C3 -51.9(4) . . . . ? C6 C7 C8 Rh1 62.4(4) . . . . ? C22 Rh1 C8 N1 -42.9(4) . . . . ? C26 Rh1 C8 N1 82.5(5) . . . . ? C27 Rh1 C8 N1 43.2(4) . . . . ? C23 Rh1 C8 N1 -74.4(4) . . . . ? C7 Rh1 C8 N1 -126.4(5) . . . . ? C4 Rh1 C8 N1 127.1(4) . . . . ? C6 Rh1 C8 N1 -158.8(4) . . . . ? C5 Rh1 C8 N1 164.6(4) . . . . ? C3 Rh1 C8 N1 98.8(5) . . . . ? C22 Rh1 C8 C3 -141.8(3) . . . . ? C26 Rh1 C8 C3 -16.3(5) . . . . ? C27 Rh1 C8 C3 -55.6(3) . . . . ? C23 Rh1 C8 C3 -173.3(3) . . . . ? C7 Rh1 C8 C3 134.8(4) . . . . ? C4 Rh1 C8 C3 28.3(2) . . . . ? C6 Rh1 C8 C3 102.4(3) . . . . ? C5 Rh1 C8 C3 65.7(3) . . . . ? C22 Rh1 C8 C7 83.5(3) . . . . ? C26 Rh1 C8 C7 -151.1(4) . . . . ? C27 Rh1 C8 C7 169.6(3) . . . . ? C23 Rh1 C8 C7 52.0(3) . . . . ? C4 Rh1 C8 C7 -106.5(3) . . . . ? C6 Rh1 C8 C7 -32.4(3) . . . . ? C5 Rh1 C8 C7 -69.0(3) . . . . ? C3 Rh1 C8 C7 -134.8(4) . . . . ? C1 P1 C10 C11 44.4(4) . . . . ? C16 P1 C10 C11 152.8(3) . . . . ? Rh2 P1 C10 C11 -75.6(3) . . . . ? C1 P1 C10 C15 -141.1(4) . . . . ? C16 P1 C10 C15 -32.7(4) . . . . ? Rh2 P1 C10 C15 98.9(3) . . . . ? C15 C10 C11 C12 -0.6(6) . . . . ? P1 C10 C11 C12 174.2(3) . . . . ? C10 C11 C12 C13 0.1(7) . . . . ? C11 C12 C13 C14 0.8(7) . . . . ? C12 C13 C14 C15 -1.2(7) . . . . ? C13 C14 C15 C10 0.6(7) . . . . ? C11 C10 C15 C14 0.2(6) . . . . ? P1 C10 C15 C14 -174.3(3) . . . . ? C1 P1 C16 C21 177.6(3) . . . . ? C10 P1 C16 C21 71.2(3) . . . . ? Rh2 P1 C16 C21 -60.5(3) . . . . ? C1 P1 C16 C17 -3.9(4) . . . . ? C10 P1 C16 C17 -110.3(3) . . . . ? Rh2 P1 C16 C17 117.9(3) . . . . ? C21 C16 C17 C18 -1.9(6) . . . . ? P1 C16 C17 C18 179.6(3) . . . . ? C16 C17 C18 C19 -0.3(6) . . . . ? C17 C18 C19 C20 1.2(7) . . . . ? C18 C19 C20 C21 0.0(6) . . . . ? C19 C20 C21 C16 -2.2(6) . . . . ? C17 C16 C21 C20 3.1(6) . . . . ? P1 C16 C21 C20 -178.3(3) . . . . ? C26 Rh1 C22 C23 66.4(3) . . . . ? C27 Rh1 C22 C23 101.6(3) . . . . ? C7 Rh1 C22 C23 -100.2(3) . . . . ? C4 Rh1 C22 C23 -163.5(5) . . . . ? C6 Rh1 C22 C23 -71.8(3) . . . . ? C5 Rh1 C22 C23 -62.3(5) . . . . ? C8 Rh1 C22 C23 -135.6(3) . . . . ? C3 Rh1 C22 C23 -161.0(3) . . . . ? C26 Rh1 C22 C29 -53.1(4) . . . . ? C27 Rh1 C22 C29 -17.9(4) . . . . ? C23 Rh1 C22 C29 -119.4(5) . . . . ? C7 Rh1 C22 C29 140.4(4) . . . . ? C4 Rh1 C22 C29 77.1(6) . . . . ? C6 Rh1 C22 C29 168.7(3) . . . . ? C5 Rh1 C22 C29 178.2(4) . . . . ? C8 Rh1 C22 C29 104.9(4) . . . . ? C3 Rh1 C22 C29 79.5(4) . . . . ? C29 C22 C23 C24 -1.2(8) . . . . ? Rh1 C22 C23 C24 -104.9(5) . . . . ? C29 C22 C23 Rh1 103.7(5) . . . . ? C26 Rh1 C23 C22 -112.9(3) . . . . ? C27 Rh1 C23 C22 -75.7(3) . . . . ? C7 Rh1 C23 C22 84.4(3) . . . . ? C4 Rh1 C23 C22 164.1(4) . . . . ? C6 Rh1 C23 C22 120.7(3) . . . . ? C5 Rh1 C23 C22 150.2(3) . . . . ? C8 Rh1 C23 C22 56.7(3) . . . . ? C3 Rh1 C23 C22 46.2(6) . . . . ? C22 Rh1 C23 C24 118.4(5) . . . . ? C26 Rh1 C23 C24 5.6(4) . . . . ? C27 Rh1 C23 C24 42.7(4) . . . . ? C7 Rh1 C23 C24 -157.2(4) . . . . ? C4 Rh1 C23 C24 -77.4(7) . . . . ? C6 Rh1 C23 C24 -120.9(4) . . . . ? C5 Rh1 C23 C24 -91.4(4) . . . . ? C8 Rh1 C23 C24 175.1(4) . . . . ? C3 Rh1 C23 C24 164.7(4) . . . . ? C22 C23 C24 C25 90.4(7) . . . . ? Rh1 C23 C24 C25 9.8(7) . . . . ? C23 C24 C25 C26 -26.7(8) . . . . ? C24 C25 C26 C27 -50.4(8) . . . . ? C24 C25 C26 Rh1 30.8(6) . . . . ? C22 Rh1 C26 C27 67.4(3) . . . . ? C23 Rh1 C26 C27 102.3(3) . . . . ? C7 Rh1 C26 C27 -165.0(5) . . . . ? C4 Rh1 C26 C27 -97.9(3) . . . . ? C6 Rh1 C26 C27 -160.8(3) . . . . ? C5 Rh1 C26 C27 -134.2(3) . . . . ? C8 Rh1 C26 C27 -58.6(5) . . . . ? C3 Rh1 C26 C27 -69.1(3) . . . . ? C22 Rh1 C26 C25 -54.2(4) . . . . ? C27 Rh1 C26 C25 -121.6(5) . . . . ? C23 Rh1 C26 C25 -19.3(4) . . . . ? C7 Rh1 C26 C25 73.4(7) . . . . ? C4 Rh1 C26 C25 140.5(4) . . . . ? C6 Rh1 C26 C25 77.6(4) . . . . ? C5 Rh1 C26 C25 104.2(4) . . . . ? C8 Rh1 C26 C25 179.8(3) . . . . ? C3 Rh1 C26 C25 169.3(3) . . . . ? C25 C26 C27 C28 -2.6(8) . . . . ? Rh1 C26 C27 C28 -105.3(4) . . . . ? C25 C26 C27 Rh1 102.8(5) . . . . ? C22 Rh1 C27 C26 -112.0(3) . . . . ? C23 Rh1 C27 C26 -74.9(3) . . . . ? C7 Rh1 C27 C26 168.3(4) . . . . ? C4 Rh1 C27 C26 87.5(3) . . . . ? C6 Rh1 C27 C26 50.4(6) . . . . ? C5 Rh1 C27 C26 59.0(3) . . . . ? C8 Rh1 C27 C26 152.1(3) . . . . ? C3 Rh1 C27 C26 123.7(3) . . . . ? C22 Rh1 C27 C28 5.9(4) . . . . ? C26 Rh1 C27 C28 118.0(5) . . . . ? C23 Rh1 C27 C28 43.1(4) . . . . ? C7 Rh1 C27 C28 -73.7(6) . . . . ? C4 Rh1 C27 C28 -154.5(4) . . . . ? C6 Rh1 C27 C28 168.4(4) . . . . ? C5 Rh1 C27 C28 177.0(3) . . . . ? C8 Rh1 C27 C28 -89.9(4) . . . . ? C3 Rh1 C27 C28 -118.4(4) . . . . ? C26 C27 C28 C29 88.5(6) . . . . ? Rh1 C27 C28 C29 7.5(6) . . . . ? C27 C28 C29 C22 -23.2(7) . . . . ? C23 C22 C29 C28 -53.7(7) . . . . ? Rh1 C22 C29 C28 27.6(6) . . . . ? N2 Rh2 C30 C31 94.4(3) . . . . ? C34 Rh2 C30 C31 -64.8(3) . . . . ? C35 Rh2 C30 C31 -98.8(3) . . . . ? P1 Rh2 C30 C31 -171.8(4) . . . . ? N2 Rh2 C30 C37 -142.1(3) . . . . ? C34 Rh2 C30 C37 58.7(3) . . . . ? C35 Rh2 C30 C37 24.7(3) . . . . ? C31 Rh2 C30 C37 123.5(5) . . . . ? P1 Rh2 C30 C37 -48.3(7) . . . . ? C37 C30 C31 C32 4.4(7) . . . . ? Rh2 C30 C31 C32 103.5(4) . . . . ? C37 C30 C31 Rh2 -99.1(4) . . . . ? N2 Rh2 C31 C30 -86.2(3) . . . . ? C34 Rh2 C31 C30 114.3(3) . . . . ? C35 Rh2 C31 C30 77.1(3) . . . . ? P1 Rh2 C31 C30 174.7(3) . . . . ? N2 Rh2 C31 C32 152.5(4) . . . . ? C34 Rh2 C31 C32 -7.1(3) . . . . ? C35 Rh2 C31 C32 -44.2(4) . . . . ? C30 Rh2 C31 C32 -121.3(5) . . . . ? P1 Rh2 C31 C32 53.3(6) . . . . ? C30 C31 C32 C33 -92.6(5) . . . . ? Rh2 C31 C32 C33 -10.7(5) . . . . ? C31 C32 C33 C34 31.4(6) . . . . ? C32 C33 C34 C35 44.2(6) . . . . ? C32 C33 C34 Rh2 -36.9(5) . . . . ? N2 Rh2 C34 C35 -169.4(4) . . . . ? C30 Rh2 C34 C35 -65.0(3) . . . . ? C31 Rh2 C34 C35 -97.5(3) . . . . ? P1 Rh2 C34 C35 101.5(2) . . . . ? N2 Rh2 C34 C33 -48.5(6) . . . . ? C35 Rh2 C34 C33 120.9(4) . . . . ? C30 Rh2 C34 C33 55.9(3) . . . . ? C31 Rh2 C34 C33 23.4(3) . . . . ? P1 Rh2 C34 C33 -137.6(3) . . . . ? C33 C34 C35 C36 3.6(7) . . . . ? Rh2 C34 C35 C36 106.0(4) . . . . ? C33 C34 C35 Rh2 -102.4(4) . . . . ? N2 Rh2 C35 C34 166.5(4) . . . . ? C30 Rh2 C35 C34 113.9(3) . . . . ? C31 Rh2 C35 C34 78.4(3) . . . . ? P1 Rh2 C35 C34 -79.7(2) . . . . ? N2 Rh2 C35 C36 46.6(7) . . . . ? C34 Rh2 C35 C36 -119.9(4) . . . . ? C30 Rh2 C35 C36 -6.0(3) . . . . ? C31 Rh2 C35 C36 -41.5(3) . . . . ? P1 Rh2 C35 C36 160.4(3) . . . . ? C34 C35 C36 C37 -96.4(5) . . . . ? Rh2 C35 C36 C37 -14.0(5) . . . . ? C31 C30 C37 C36 40.5(6) . . . . ? Rh2 C30 C37 C36 -40.3(4) . . . . ? C35 C36 C37 C30 36.9(5) . . . . ? C38 N2 C39 C40 179.9(4) . . . . ? Rh2 N2 C39 C40 -1.7(7) . . . . ? N2 C39 C40 C41 161.8(4) . . . . ? N2 C39 C40 C45 -16.2(7) . . . . ? C45 C40 C41 C42 1.6(6) . . . . ? C39 C40 C41 C42 -176.5(4) . . . . ? C40 C41 C42 C43 -1.6(7) . . . . ? C41 C42 C43 C44 0.3(7) . . . . ? C42 C43 C44 C45 1.1(7) . . . . ? C43 C44 C45 C40 -1.1(7) . . . . ? C41 C40 C45 C44 -0.2(6) . . . . ? C39 C40 C45 C44 177.7(4) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 27.51 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.613 _refine_diff_density_min -1.560 _refine_diff_density_rms 0.121 #===END