# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'de Bruin, Bas' 'Erica Jellema' 'J. Reek' 'Miguel Rubio' 'Maxime A. Siegler' 'A. Spek' _publ_contact_author_name 'Bas de Bruin' _publ_contact_author_email B.DEBRUIN@UVA.NL _publ_section_title ; Supramolecular NHC ligands: On the influence of ZnII-templates on the activity of RhI(cod) complexes in Carbene Polymerization ; # Attachment '4a.cif' data_4a _database_code_depnum_ccdc_archive 'CCDC 744088' #data_s4198a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H29 Cl N3 Rh' _chemical_formula_sum 'C25 H29 Cl N3 Rh' _chemical_formula_weight 509.87 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4144(3) _cell_length_b 11.7114(4) _cell_length_c 13.4408(6) _cell_angle_alpha 93.230(2) _cell_angle_beta 104.119(2) _cell_angle_gamma 93.696(2) _cell_volume 1126.36(8) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 23176 _cell_measurement_theta_min 1.57 _cell_measurement_theta_max 27.49 _exptl_crystal_description 'irregular block' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 0.894 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.932 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31397 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0177 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5180 _reflns_number_gt 4756 _reflns_threshold_expression I>2/s(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'PEAKREF (Schreurs, 2005)' _computing_data_reduction 'EVALCCD (Duisenberg et al., 2003)' _computing_structure_solution 'DIRDIF08 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0195P)^2^+0.8550P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5180 _refine_ls_number_parameters 285 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0203 _refine_ls_wR_factor_ref 0.0479 _refine_ls_wR_factor_gt 0.0459 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.062 _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 0.223363(17) 0.226385(10) 0.312228(9) 0.01219(4) Uani 1 1 d . . . Cl1 Cl -0.00029(5) 0.07640(3) 0.22780(3) 0.01904(8) Uani 1 1 d . . . C1 C 0.4865(2) 0.30450(15) 0.39098(12) 0.0175(3) Uani 1 1 d D . . H1 H 0.566(2) 0.3104(17) 0.3453(12) 0.021 Uiso 1 1 d D . . C2 C 0.5711(2) 0.23852(17) 0.48253(14) 0.0249(4) Uani 1 1 d . . . H2A H 0.6677 0.2896 0.5320 0.030 Uiso 1 1 calc R . . H2B H 0.6332 0.1736 0.4589 0.030 Uiso 1 1 calc R . . C3 C 0.4268(3) 0.19187(18) 0.53780(14) 0.0301(4) Uani 1 1 d . . . H3A H 0.4730 0.1242 0.5740 0.036 Uiso 1 1 calc R . . H3B H 0.4122 0.2512 0.5901 0.036 Uiso 1 1 calc R . . C4 C 0.2382(3) 0.15789(16) 0.46427(13) 0.0235(4) Uani 1 1 d D . . H4 H 0.209(3) 0.0781(9) 0.4466(16) 0.028 Uiso 1 1 d D . . C5 C 0.0945(3) 0.22781(16) 0.44147(13) 0.0227(4) Uani 1 1 d D . . H5 H -0.0261(17) 0.1911(16) 0.4103(15) 0.027 Uiso 1 1 d D . . C6 C 0.0947(3) 0.35259(17) 0.47792(14) 0.0271(4) Uani 1 1 d . . . H6A H 0.0757 0.3570 0.5484 0.033 Uiso 1 1 calc R . . H6B H -0.0110 0.3867 0.4325 0.033 Uiso 1 1 calc R . . C7 C 0.2761(3) 0.42257(16) 0.47827(14) 0.0241(4) Uani 1 1 d . . . H7A H 0.2528 0.5048 0.4754 0.029 Uiso 1 1 calc R . . H7B H 0.3697 0.4138 0.5433 0.029 Uiso 1 1 calc R . . C8 C 0.3544(2) 0.38527(14) 0.38794(12) 0.0175(3) Uani 1 1 d D . . H8 H 0.350(3) 0.4403(14) 0.3384(12) 0.021 Uiso 1 1 d D . . C9 C 0.3493(2) 0.08716(13) 0.11070(12) 0.0145(3) Uani 1 1 d . . . C10 C 0.4917(2) 0.07263(14) 0.19598(13) 0.0164(3) Uani 1 1 d . . . H10 H 0.5443 0.1349 0.2450 0.020 Uiso 1 1 calc R . . C11 C 0.5553(2) -0.03591(14) 0.20767(13) 0.0190(3) Uani 1 1 d . . . H11 H 0.6526 -0.0461 0.2664 0.023 Uiso 1 1 calc R . . C12 C 0.3519(3) -0.10898(15) 0.05912(15) 0.0248(4) Uani 1 1 d . . . H12 H 0.3031 -0.1724 0.0106 0.030 Uiso 1 1 calc R . . C13 C 0.2777(2) -0.00466(15) 0.03991(13) 0.0201(3) Uani 1 1 d . . . H13 H 0.1811 0.0035 -0.0198 0.024 Uiso 1 1 calc R . . C14 C 0.2383(2) 0.26790(13) 0.16932(11) 0.0126(3) Uani 1 1 d . . . C15 C 0.2348(2) 0.24276(15) -0.00099(13) 0.0214(4) Uani 1 1 d . . . H15 H 0.2495 0.2087 -0.0641 0.026 Uiso 1 1 calc R . . C16 C 0.1676(2) 0.34395(16) 0.01357(13) 0.0216(4) Uani 1 1 d . . . H16 H 0.1254 0.3957 -0.0375 0.026 Uiso 1 1 calc R . . C17 C 0.1170(2) 0.46258(13) 0.16202(12) 0.0139(3) Uani 1 1 d . . . C18 C 0.2333(2) 0.56314(14) 0.16931(13) 0.0181(3) Uani 1 1 d . . . C19 C 0.1833(2) 0.66313(14) 0.21259(13) 0.0192(3) Uani 1 1 d . . . H19 H 0.2614 0.7319 0.2183 0.023 Uiso 1 1 calc R . . C20 C 0.0219(2) 0.66523(14) 0.24778(12) 0.0174(3) Uani 1 1 d . . . C21 C -0.0898(2) 0.56358(14) 0.23890(12) 0.0157(3) Uani 1 1 d . . . H21 H -0.1992 0.5638 0.2638 0.019 Uiso 1 1 calc R . . C22 C -0.0477(2) 0.46080(13) 0.19469(12) 0.0143(3) Uani 1 1 d . . . C23 C 0.4086(3) 0.56537(17) 0.13112(18) 0.0316(4) Uani 1 1 d . . . H23A H 0.3752 0.5569 0.0558 0.047 Uiso 1 1 calc R . . H23B H 0.4818 0.5021 0.1581 0.047 Uiso 1 1 calc R . . H23C H 0.4826 0.6386 0.1547 0.047 Uiso 1 1 calc R . . C24 C -0.0321(3) 0.77620(15) 0.29054(14) 0.0252(4) Uani 1 1 d . . . H24A H -0.1653 0.7689 0.2888 0.038 Uiso 1 1 calc R . . H24B H -0.0071 0.8386 0.2489 0.038 Uiso 1 1 calc R . . H24C H 0.0410 0.7932 0.3617 0.038 Uiso 1 1 calc R . . C25 C -0.1806(2) 0.35524(14) 0.18078(14) 0.0203(3) Uani 1 1 d . . . H25A H -0.2869 0.3723 0.2089 0.030 Uiso 0.50 1 calc PR . . H25B H -0.1162 0.2934 0.2170 0.030 Uiso 0.50 1 calc PR . . H25C H -0.2253 0.3312 0.1074 0.030 Uiso 0.50 1 calc PR . . H25D H -0.1321 0.2923 0.1466 0.030 Uiso 0.50 1 calc PR . . H25E H -0.3027 0.3712 0.1385 0.030 Uiso 0.50 1 calc PR . . H25F H -0.1936 0.3334 0.2482 0.030 Uiso 0.50 1 calc PR . . N1 N 0.4882(2) -0.12657(12) 0.14163(12) 0.0229(3) Uani 1 1 d . . . N2 N 0.27901(18) 0.19718(12) 0.09462(10) 0.0148(3) Uani 1 1 d . . . N3 N 0.17110(18) 0.35918(11) 0.11751(10) 0.0147(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01444(6) 0.01114(6) 0.01091(6) 0.00067(4) 0.00332(4) -0.00025(4) Cl1 0.01928(19) 0.01443(18) 0.0221(2) -0.00167(15) 0.00461(15) -0.00373(14) C1 0.0152(8) 0.0212(8) 0.0142(7) 0.0007(6) 0.0013(6) -0.0040(6) C2 0.0207(9) 0.0304(10) 0.0214(9) 0.0063(7) -0.0003(7) 0.0039(7) C3 0.0345(11) 0.0350(11) 0.0188(9) 0.0101(8) 0.0013(8) 0.0028(8) C4 0.0321(10) 0.0251(9) 0.0140(8) 0.0069(7) 0.0075(7) -0.0048(8) C5 0.0281(9) 0.0269(9) 0.0153(8) -0.0007(7) 0.0119(7) -0.0043(7) C6 0.0302(10) 0.0305(10) 0.0222(9) -0.0043(8) 0.0108(8) 0.0030(8) C7 0.0287(9) 0.0207(9) 0.0215(9) -0.0071(7) 0.0057(7) 0.0003(7) C8 0.0213(8) 0.0134(8) 0.0146(8) -0.0017(6) 0.0007(6) -0.0046(6) C9 0.0150(7) 0.0137(7) 0.0178(8) 0.0020(6) 0.0088(6) 0.0046(6) C10 0.0169(8) 0.0140(8) 0.0192(8) 0.0005(6) 0.0058(6) 0.0025(6) C11 0.0179(8) 0.0178(8) 0.0243(9) 0.0052(7) 0.0091(7) 0.0053(6) C12 0.0303(10) 0.0169(8) 0.0292(10) -0.0072(7) 0.0141(8) -0.0024(7) C13 0.0197(8) 0.0225(9) 0.0182(8) -0.0031(7) 0.0062(6) 0.0011(7) C14 0.0122(7) 0.0127(7) 0.0128(7) 0.0012(6) 0.0031(6) 0.0010(6) C15 0.0281(9) 0.0269(9) 0.0112(7) 0.0037(7) 0.0060(7) 0.0114(7) C16 0.0274(9) 0.0267(9) 0.0134(8) 0.0066(7) 0.0069(7) 0.0124(7) C17 0.0168(8) 0.0129(7) 0.0121(7) 0.0030(6) 0.0021(6) 0.0060(6) C18 0.0149(8) 0.0184(8) 0.0217(8) 0.0077(7) 0.0034(6) 0.0047(6) C19 0.0206(8) 0.0129(8) 0.0217(8) 0.0048(6) 0.0001(7) 0.0000(6) C20 0.0241(8) 0.0130(8) 0.0132(7) 0.0018(6) -0.0004(6) 0.0056(6) C21 0.0175(8) 0.0184(8) 0.0124(7) 0.0024(6) 0.0043(6) 0.0061(6) C22 0.0168(7) 0.0147(8) 0.0109(7) 0.0020(6) 0.0017(6) 0.0037(6) C23 0.0204(9) 0.0245(10) 0.0545(13) 0.0083(9) 0.0164(9) 0.0036(7) C24 0.0370(10) 0.0153(8) 0.0232(9) 0.0001(7) 0.0060(8) 0.0082(7) C25 0.0192(8) 0.0173(8) 0.0257(9) -0.0009(7) 0.0087(7) 0.0008(6) N1 0.0273(8) 0.0134(7) 0.0333(8) 0.0027(6) 0.0166(7) 0.0045(6) N2 0.0174(7) 0.0160(7) 0.0121(6) 0.0014(5) 0.0045(5) 0.0065(5) N3 0.0170(6) 0.0155(7) 0.0126(6) 0.0026(5) 0.0045(5) 0.0055(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 C14 2.0349(15) . ? Rh1 C1 2.1018(16) . ? Rh1 C8 2.1244(16) . ? Rh1 C5 2.1770(16) . ? Rh1 C4 2.2177(16) . ? Rh1 Cl1 2.3674(4) . ? C1 C8 1.400(2) . ? C1 C2 1.516(2) . ? C1 H1 0.951(9) . ? C2 C3 1.534(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.516(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.372(3) . ? C4 H4 0.949(9) . ? C5 C6 1.515(3) . ? C5 H5 0.953(9) . ? C6 C7 1.528(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.523(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8 0.949(9) . ? C9 C13 1.381(2) . ? C9 C10 1.383(2) . ? C9 N2 1.429(2) . ? C10 C11 1.388(2) . ? C10 H10 0.9500 . ? C11 N1 1.332(2) . ? C11 H11 0.9500 . ? C12 N1 1.341(2) . ? C12 C13 1.384(3) . ? C12 H12 0.9500 . ? C13 H13 0.9500 . ? C14 N3 1.3636(19) . ? C14 N2 1.3679(19) . ? C15 C16 1.337(2) . ? C15 N2 1.392(2) . ? C15 H15 0.9500 . ? C16 N3 1.392(2) . ? C16 H16 0.9500 . ? C17 C22 1.395(2) . ? C17 C18 1.398(2) . ? C17 N3 1.443(2) . ? C18 C19 1.390(2) . ? C18 C23 1.509(2) . ? C19 C20 1.390(2) . ? C19 H19 0.9500 . ? C20 C21 1.388(2) . ? C20 C24 1.508(2) . ? C21 C22 1.399(2) . ? C21 H21 0.9500 . ? C22 C25 1.504(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C25 H25D 0.9800 . ? C25 H25E 0.9800 . ? C25 H25F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Rh1 C1 96.50(6) . . ? C14 Rh1 C8 95.11(6) . . ? C1 Rh1 C8 38.69(7) . . ? C14 Rh1 C5 152.95(7) . . ? C1 Rh1 C5 97.87(7) . . ? C8 Rh1 C5 82.21(7) . . ? C14 Rh1 C4 170.25(7) . . ? C1 Rh1 C4 81.61(7) . . ? C8 Rh1 C4 89.38(7) . . ? C5 Rh1 C4 36.36(7) . . ? C14 Rh1 Cl1 86.42(4) . . ? C1 Rh1 Cl1 157.39(5) . . ? C8 Rh1 Cl1 163.61(5) . . ? C5 Rh1 Cl1 89.01(5) . . ? C4 Rh1 Cl1 91.72(5) . . ? C8 C1 C2 126.07(15) . . ? C8 C1 Rh1 71.53(9) . . ? C2 C1 Rh1 110.48(11) . . ? C8 C1 H1 118.0(12) . . ? C2 C1 H1 111.4(12) . . ? Rh1 C1 H1 110.1(12) . . ? C1 C2 C3 113.07(15) . . ? C1 C2 H2A 109.0 . . ? C3 C2 H2A 109.0 . . ? C1 C2 H2B 109.0 . . ? C3 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? C4 C3 C2 112.35(15) . . ? C4 C3 H3A 109.1 . . ? C2 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? C2 C3 H3B 109.1 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 124.92(18) . . ? C5 C4 Rh1 70.20(10) . . ? C3 C4 Rh1 110.89(12) . . ? C5 C4 H4 117.3(13) . . ? C3 C4 H4 115.9(13) . . ? Rh1 C4 H4 102.2(13) . . ? C4 C5 C6 127.86(17) . . ? C4 C5 Rh1 73.44(10) . . ? C6 C5 Rh1 106.45(11) . . ? C4 C5 H5 116.5(13) . . ? C6 C5 H5 114.4(13) . . ? Rh1 C5 H5 101.6(13) . . ? C5 C6 C7 112.67(15) . . ? C5 C6 H6A 109.1 . . ? C7 C6 H6A 109.1 . . ? C5 C6 H6B 109.1 . . ? C7 C6 H6B 109.1 . . ? H6A C6 H6B 107.8 . . ? C8 C7 C6 112.16(14) . . ? C8 C7 H7A 109.2 . . ? C6 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C6 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C1 C8 C7 124.77(15) . . ? C1 C8 Rh1 69.78(9) . . ? C7 C8 Rh1 112.37(11) . . ? C1 C8 H8 116.1(12) . . ? C7 C8 H8 114.5(12) . . ? Rh1 C8 H8 108.9(12) . . ? C13 C9 C10 119.72(15) . . ? C13 C9 N2 120.05(14) . . ? C10 C9 N2 120.22(14) . . ? C9 C10 C11 117.87(15) . . ? C9 C10 H10 121.1 . . ? C11 C10 H10 121.1 . . ? N1 C11 C10 124.03(16) . . ? N1 C11 H11 118.0 . . ? C10 C11 H11 118.0 . . ? N1 C12 C13 124.37(16) . . ? N1 C12 H12 117.8 . . ? C13 C12 H12 117.8 . . ? C9 C13 C12 117.53(16) . . ? C9 C13 H13 121.2 . . ? C12 C13 H13 121.2 . . ? N3 C14 N2 103.23(12) . . ? N3 C14 Rh1 128.57(11) . . ? N2 C14 Rh1 126.66(11) . . ? C16 C15 N2 106.41(14) . . ? C16 C15 H15 126.8 . . ? N2 C15 H15 126.8 . . ? C15 C16 N3 107.15(14) . . ? C15 C16 H16 126.4 . . ? N3 C16 H16 126.4 . . ? C22 C17 C18 121.97(15) . . ? C22 C17 N3 120.25(14) . . ? C18 C17 N3 117.77(14) . . ? C19 C18 C17 118.31(15) . . ? C19 C18 C23 119.90(16) . . ? C17 C18 C23 121.79(15) . . ? C18 C19 C20 121.81(15) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C21 C20 C19 118.05(15) . . ? C21 C20 C24 121.48(16) . . ? C19 C20 C24 120.44(16) . . ? C20 C21 C22 122.59(15) . . ? C20 C21 H21 118.7 . . ? C22 C21 H21 118.7 . . ? C17 C22 C21 117.23(15) . . ? C17 C22 C25 122.56(14) . . ? C21 C22 C25 120.18(14) . . ? C18 C23 H23A 109.5 . . ? C18 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C18 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C25 H25D 109.5 . . ? H25A C25 H25D 141.1 . . ? H25B C25 H25D 56.3 . . ? H25C C25 H25D 56.3 . . ? C22 C25 H25E 109.5 . . ? H25A C25 H25E 56.3 . . ? H25B C25 H25E 141.1 . . ? H25C C25 H25E 56.3 . . ? H25D C25 H25E 109.5 . . ? C22 C25 H25F 109.5 . . ? H25A C25 H25F 56.3 . . ? H25B C25 H25F 56.3 . . ? H25C C25 H25F 141.1 . . ? H25D C25 H25F 109.5 . . ? H25E C25 H25F 109.5 . . ? C11 N1 C12 116.48(15) . . ? C14 N2 C15 111.76(13) . . ? C14 N2 C9 124.58(13) . . ? C15 N2 C9 123.59(13) . . ? C14 N3 C16 111.44(13) . . ? C14 N3 C17 126.13(13) . . ? C16 N3 C17 122.37(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Rh1 C1 C8 90.07(10) . . . . ? C5 Rh1 C1 C8 -66.96(11) . . . . ? C4 Rh1 C1 C8 -99.58(11) . . . . ? Cl1 Rh1 C1 C8 -173.62(9) . . . . ? C14 Rh1 C1 C2 -147.39(12) . . . . ? C8 Rh1 C1 C2 122.54(16) . . . . ? C5 Rh1 C1 C2 55.59(13) . . . . ? C4 Rh1 C1 C2 22.96(12) . . . . ? Cl1 Rh1 C1 C2 -51.08(19) . . . . ? C8 C1 C2 C3 43.8(2) . . . . ? Rh1 C1 C2 C3 -37.83(19) . . . . ? C1 C2 C3 C4 33.8(2) . . . . ? C2 C3 C4 C5 -93.4(2) . . . . ? C2 C3 C4 Rh1 -13.6(2) . . . . ? C1 Rh1 C4 C5 115.71(12) . . . . ? C8 Rh1 C4 C5 77.65(12) . . . . ? Cl1 Rh1 C4 C5 -85.99(11) . . . . ? C1 Rh1 C4 C3 -5.21(14) . . . . ? C8 Rh1 C4 C3 -43.26(14) . . . . ? C5 Rh1 C4 C3 -120.92(19) . . . . ? Cl1 Rh1 C4 C3 153.09(13) . . . . ? C3 C4 C5 C6 4.0(3) . . . . ? Rh1 C4 C5 C6 -98.22(17) . . . . ? C3 C4 C5 Rh1 102.18(16) . . . . ? C14 Rh1 C5 C4 174.40(13) . . . . ? C1 Rh1 C5 C4 -64.14(12) . . . . ? C8 Rh1 C5 C4 -99.63(12) . . . . ? Cl1 Rh1 C5 C4 94.25(11) . . . . ? C14 Rh1 C5 C6 -60.2(2) . . . . ? C1 Rh1 C5 C6 61.30(13) . . . . ? C8 Rh1 C5 C6 25.81(12) . . . . ? C4 Rh1 C5 C6 125.44(18) . . . . ? Cl1 Rh1 C5 C6 -140.32(12) . . . . ? C4 C5 C6 C7 40.7(2) . . . . ? Rh1 C5 C6 C7 -40.88(18) . . . . ? C5 C6 C7 C8 36.8(2) . . . . ? C2 C1 C8 C7 1.5(3) . . . . ? Rh1 C1 C8 C7 103.77(16) . . . . ? C2 C1 C8 Rh1 -102.30(16) . . . . ? C6 C7 C8 C1 -93.4(2) . . . . ? C6 C7 C8 Rh1 -13.14(19) . . . . ? C14 Rh1 C8 C1 -94.02(10) . . . . ? C5 Rh1 C8 C1 113.07(11) . . . . ? C4 Rh1 C8 C1 77.31(10) . . . . ? Cl1 Rh1 C8 C1 171.29(13) . . . . ? C14 Rh1 C8 C7 145.60(12) . . . . ? C1 Rh1 C8 C7 -120.38(16) . . . . ? C5 Rh1 C8 C7 -7.31(12) . . . . ? C4 Rh1 C8 C7 -43.07(13) . . . . ? Cl1 Rh1 C8 C7 50.9(2) . . . . ? C13 C9 C10 C11 -1.1(2) . . . . ? N2 C9 C10 C11 -179.74(14) . . . . ? C9 C10 C11 N1 0.3(2) . . . . ? C10 C9 C13 C12 0.9(2) . . . . ? N2 C9 C13 C12 179.60(15) . . . . ? N1 C12 C13 C9 0.0(3) . . . . ? C1 Rh1 C14 N3 -95.22(14) . . . . ? C8 Rh1 C14 N3 -56.34(14) . . . . ? C5 Rh1 C14 N3 26.5(2) . . . . ? Cl1 Rh1 C14 N3 107.30(14) . . . . ? C1 Rh1 C14 N2 101.33(14) . . . . ? C8 Rh1 C14 N2 140.20(14) . . . . ? C5 Rh1 C14 N2 -136.93(15) . . . . ? Cl1 Rh1 C14 N2 -56.16(13) . . . . ? N2 C15 C16 N3 -0.1(2) . . . . ? C22 C17 C18 C19 1.4(2) . . . . ? N3 C17 C18 C19 -179.63(14) . . . . ? C22 C17 C18 C23 -178.24(16) . . . . ? N3 C17 C18 C23 0.7(2) . . . . ? C17 C18 C19 C20 -0.3(2) . . . . ? C23 C18 C19 C20 179.32(16) . . . . ? C18 C19 C20 C21 0.2(2) . . . . ? C18 C19 C20 C24 -177.59(15) . . . . ? C19 C20 C21 C22 -1.1(2) . . . . ? C24 C20 C21 C22 176.65(15) . . . . ? C18 C17 C22 C21 -2.2(2) . . . . ? N3 C17 C22 C21 178.82(13) . . . . ? C18 C17 C22 C25 175.74(15) . . . . ? N3 C17 C22 C25 -3.2(2) . . . . ? C20 C21 C22 C17 2.1(2) . . . . ? C20 C21 C22 C25 -175.93(15) . . . . ? C10 C11 N1 C12 0.5(2) . . . . ? C13 C12 N1 C11 -0.7(3) . . . . ? N3 C14 N2 C15 -1.06(17) . . . . ? Rh1 C14 N2 C15 165.72(12) . . . . ? N3 C14 N2 C9 -178.05(14) . . . . ? Rh1 C14 N2 C9 -11.3(2) . . . . ? C16 C15 N2 C14 0.7(2) . . . . ? C16 C15 N2 C9 177.76(15) . . . . ? C13 C9 N2 C14 136.46(16) . . . . ? C10 C9 N2 C14 -44.9(2) . . . . ? C13 C9 N2 C15 -40.2(2) . . . . ? C10 C9 N2 C15 138.50(17) . . . . ? N2 C14 N3 C16 1.01(18) . . . . ? Rh1 C14 N3 C16 -165.42(12) . . . . ? N2 C14 N3 C17 -176.21(14) . . . . ? Rh1 C14 N3 C17 17.4(2) . . . . ? C15 C16 N3 C14 -0.6(2) . . . . ? C15 C16 N3 C17 176.74(15) . . . . ? C22 C17 N3 C14 -73.3(2) . . . . ? C18 C17 N3 C14 107.72(18) . . . . ? C22 C17 N3 C16 109.78(18) . . . . ? C18 C17 N3 C16 -69.2(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.535 _refine_diff_density_min -0.500 _refine_diff_density_rms 0.064 # Attachment '4b.cif' data_4b _database_code_depnum_ccdc_archive 'CCDC 744089' #data_s4078a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H31 Cl N3 Rh' _chemical_formula_sum 'C26 H31 Cl N3 Rh' _chemical_formula_weight 523.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 11.1897(3) _cell_length_b 17.3083(6) _cell_length_c 13.4145(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.790(2) _cell_angle_gamma 90.00 _cell_volume 2339.27(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21686 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.863 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.685 _exptl_absorpt_correction_T_max 0.862 _exptl_absorpt_process_details '(SADABS; Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method '\f and \w scans ' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39101 _diffrn_reflns_av_R_equivalents 0.0230 _diffrn_reflns_av_sigmaI/netI 0.0146 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5381 _reflns_number_gt 4719 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Nonius, 1999)' _computing_cell_refinement 'PEAKREF (Schreurs, 2005)' _computing_data_reduction 'EVALCCD (Duisenberg et al., 2003)' _computing_structure_solution 'DIRDIF08 (Beurskens et al., 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2003)' _computing_publication_material 'PLATON (Spek, 2003)' _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^)+(0.0223P)^2^+1.4532P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5381 _refine_ls_number_parameters 295 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0504 _refine_ls_wR_factor_gt 0.0473 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 0.224979(11) 0.077226(7) 0.209336(9) 0.01764(4) Uani 1 1 d . . . Cl1 Cl 0.33220(4) -0.04469(2) 0.22818(3) 0.02660(9) Uani 1 1 d . . . C1 C 0.07664(17) 0.16125(10) 0.17072(15) 0.0278(4) Uani 1 1 d D . . H1 H 0.0434(19) 0.1578(12) 0.2237(15) 0.033 Uiso 1 1 d D . . C2 C -0.02736(18) 0.15304(12) 0.05271(16) 0.0360(4) Uani 1 1 d . . . H2A H -0.0729 0.2033 0.0277 0.043 Uiso 1 1 calc R . . H2B H -0.0944 0.1150 0.0507 0.043 Uiso 1 1 calc R . . C3 C 0.02699(19) 0.12754(12) -0.02793(15) 0.0380(4) Uani 1 1 d . . . H3A H -0.0433 0.0998 -0.0905 0.046 Uiso 1 1 calc R . . H3B H 0.0520 0.1737 -0.0581 0.046 Uiso 1 1 calc R . . C4 C 0.1464(2) 0.07557(12) 0.02600(14) 0.0328(4) Uani 1 1 d D . . H4 H 0.135(2) 0.0219(9) 0.0113(17) 0.039 Uiso 1 1 d D . . C5 C 0.2733(2) 0.10244(14) 0.07094(16) 0.0381(5) Uani 1 1 d D . . H5 H 0.342(2) 0.0656(11) 0.0837(19) 0.046 Uiso 1 1 d D . . C6 C 0.3127(2) 0.18534(15) 0.07670(18) 0.0510(6) Uani 1 1 d . . . H6A H 0.2923 0.2035 0.0010 0.061 Uiso 1 1 calc R . . H6B H 0.4099 0.1894 0.1215 0.061 Uiso 1 1 calc R . . C7 C 0.2438(2) 0.23872(12) 0.12659(18) 0.0459(5) Uani 1 1 d . . . H7A H 0.3054 0.2810 0.1670 0.055 Uiso 1 1 calc R . . H7B H 0.1653 0.2622 0.0658 0.055 Uiso 1 1 calc R . . C8 C 0.19964(19) 0.19782(10) 0.20537(15) 0.0312(4) Uani 1 1 d D . . H8 H 0.240(2) 0.2167(12) 0.2795(13) 0.037 Uiso 1 1 d D . . C9 C 0.63821(18) 0.32130(11) 0.5089(2) 0.0422(5) Uani 1 1 d . . . H9 H 0.6707 0.3728 0.5194 0.051 Uiso 1 1 calc R . . C10 C 0.6034(2) 0.28770(13) 0.4075(2) 0.0489(6) Uani 1 1 d . . . H10 H 0.6143 0.3148 0.3505 0.059 Uiso 1 1 calc R . . C11 C 0.55217(19) 0.21353(12) 0.38981(17) 0.0389(5) Uani 1 1 d . . . H11 H 0.5269 0.1890 0.3202 0.047 Uiso 1 1 calc R . . C12 C 0.53833(15) 0.17588(9) 0.47453(14) 0.0224(3) Uani 1 1 d . . . C13 C 0.58075(18) 0.21423(10) 0.57463(16) 0.0316(4) Uani 1 1 d . . . H13 H 0.5751 0.1877 0.6344 0.038 Uiso 1 1 calc R . . C14 C 0.49086(15) 0.09357(9) 0.46294(14) 0.0214(3) Uani 1 1 d . . . H14A H 0.4887 0.0721 0.3938 0.026 Uiso 1 1 calc R . . H14B H 0.5565 0.0633 0.5253 0.026 Uiso 1 1 calc R . . C15 C 0.33971(16) 0.07362(9) 0.55538(13) 0.0220(3) Uani 1 1 d . . . H15 H 0.4048 0.0789 0.6298 0.026 Uiso 1 1 calc R . . C16 C 0.21140(16) 0.05618(10) 0.52157(13) 0.0228(3) Uani 1 1 d . . . H16 H 0.1679 0.0468 0.5674 0.027 Uiso 1 1 calc R . . C17 C 0.24526(15) 0.07014(8) 0.36752(12) 0.0167(3) Uani 1 1 d . . . C18 C 0.01963(14) 0.02854(9) 0.34134(12) 0.0187(3) Uani 1 1 d . . . C19 C -0.00070(15) -0.04890(9) 0.30899(13) 0.0205(3) Uani 1 1 d . . . C20 C -0.13033(16) -0.07289(10) 0.24446(13) 0.0249(3) Uani 1 1 d . . . H20 H -0.1462 -0.1251 0.2205 0.030 Uiso 1 1 calc R . . C21 C -0.23724(16) -0.02278(11) 0.21401(13) 0.0273(4) Uani 1 1 d . . . C22 C -0.21336(16) 0.05245(11) 0.25247(14) 0.0274(4) Uani 1 1 d . . . H22 H -0.2863 0.0867 0.2337 0.033 Uiso 1 1 calc R . . C23 C -0.08568(16) 0.07955(10) 0.31787(13) 0.0232(3) Uani 1 1 d . . . C24 C 0.11226(17) -0.10584(10) 0.34566(15) 0.0277(4) Uani 1 1 d . . . H24A H 0.0767 -0.1582 0.3255 0.042 Uiso 1 1 calc R . . H24B H 0.1643 -0.1025 0.4261 0.042 Uiso 1 1 calc R . . H24C H 0.1692 -0.0938 0.3092 0.042 Uiso 1 1 calc R . . C25 C -0.37624(18) -0.05064(15) 0.14377(16) 0.0431(5) Uani 1 1 d . . . H25A H -0.4365 -0.0291 0.1721 0.065 Uiso 1 1 calc R . . H25B H -0.3785 -0.1072 0.1464 0.065 Uiso 1 1 calc R . . H25C H -0.4043 -0.0338 0.0671 0.065 Uiso 1 1 calc R . . C26 C -0.06659(19) 0.16047(11) 0.36366(17) 0.0344(4) Uani 1 1 d . . . H26A H -0.0781 0.1608 0.4320 0.052 Uiso 1 1 calc R . . H26B H -0.1322 0.1949 0.3092 0.052 Uiso 1 1 calc R . . H26C H 0.0230 0.1784 0.3796 0.052 Uiso 1 1 calc R . . N1 N 0.62924(17) 0.28615(9) 0.59290(16) 0.0414(4) Uani 1 1 d . . . N2 N 0.35918(12) 0.08247(7) 0.46070(10) 0.0176(2) Uani 1 1 d . . . N3 N 0.15413(12) 0.05446(8) 0.40679(10) 0.0181(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01668(6) 0.02041(7) 0.01648(6) 0.00284(5) 0.00784(5) 0.00093(5) Cl1 0.0265(2) 0.0286(2) 0.02469(19) -0.00070(16) 0.01104(16) 0.00858(16) C1 0.0301(9) 0.0250(8) 0.0313(9) 0.0101(7) 0.0161(7) 0.0105(7) C2 0.0228(8) 0.0372(10) 0.0399(11) 0.0121(8) 0.0063(8) 0.0036(7) C3 0.0319(10) 0.0468(12) 0.0246(9) 0.0095(8) 0.0024(8) -0.0030(8) C4 0.0440(11) 0.0379(10) 0.0168(8) 0.0039(7) 0.0134(8) 0.0027(8) C5 0.0349(10) 0.0600(13) 0.0272(9) 0.0146(9) 0.0209(8) 0.0073(9) C6 0.0391(11) 0.0760(17) 0.0375(11) 0.0206(11) 0.0164(9) -0.0148(11) C7 0.0436(11) 0.0376(11) 0.0437(12) 0.0191(9) 0.0070(9) -0.0135(9) C8 0.0400(10) 0.0194(8) 0.0270(9) 0.0052(7) 0.0080(8) 0.0002(7) C9 0.0240(9) 0.0214(9) 0.0762(16) 0.0007(9) 0.0172(10) -0.0034(7) C10 0.0430(12) 0.0427(12) 0.0552(14) 0.0209(11) 0.0159(10) -0.0097(10) C11 0.0371(10) 0.0405(11) 0.0327(10) 0.0056(8) 0.0091(8) -0.0101(9) C12 0.0133(7) 0.0203(8) 0.0299(8) 0.0024(6) 0.0060(6) 0.0011(6) C13 0.0322(9) 0.0251(9) 0.0406(10) -0.0066(8) 0.0186(8) -0.0056(7) C14 0.0150(7) 0.0209(8) 0.0270(8) -0.0016(6) 0.0079(6) -0.0002(6) C15 0.0233(8) 0.0241(8) 0.0160(7) -0.0027(6) 0.0060(6) 0.0004(6) C16 0.0252(8) 0.0274(8) 0.0166(7) -0.0010(6) 0.0097(6) -0.0005(6) C17 0.0179(7) 0.0136(7) 0.0184(7) 0.0005(5) 0.0077(6) 0.0009(5) C18 0.0156(7) 0.0253(8) 0.0159(7) 0.0014(6) 0.0074(6) -0.0018(6) C19 0.0213(7) 0.0251(8) 0.0185(7) 0.0008(6) 0.0120(6) -0.0014(6) C20 0.0254(8) 0.0300(9) 0.0222(8) -0.0052(7) 0.0130(7) -0.0085(7) C21 0.0195(8) 0.0457(11) 0.0171(8) 0.0001(7) 0.0086(6) -0.0050(7) C22 0.0177(8) 0.0420(10) 0.0236(8) 0.0068(7) 0.0099(7) 0.0069(7) C23 0.0226(8) 0.0268(8) 0.0225(8) 0.0030(7) 0.0120(6) 0.0021(6) C24 0.0268(8) 0.0242(8) 0.0337(9) 0.0003(7) 0.0146(7) 0.0015(7) C25 0.0209(9) 0.0743(15) 0.0305(10) -0.0083(10) 0.0078(8) -0.0114(9) C26 0.0361(10) 0.0288(9) 0.0425(11) -0.0033(8) 0.0210(9) 0.0045(8) N1 0.0358(9) 0.0276(8) 0.0632(12) -0.0159(8) 0.0238(8) -0.0103(7) N2 0.0168(6) 0.0164(6) 0.0186(6) -0.0009(5) 0.0068(5) -0.0007(5) N3 0.0167(6) 0.0218(6) 0.0154(6) -0.0006(5) 0.0066(5) -0.0014(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 C17 2.0373(15) . ? Rh1 C1 2.0953(16) . ? Rh1 C8 2.1041(18) . ? Rh1 C5 2.1919(17) . ? Rh1 C4 2.2228(17) . ? Rh1 Cl1 2.3858(4) . ? C1 C8 1.398(3) . ? C1 C2 1.509(3) . ? C1 H1 0.936(15) . ? C2 C3 1.519(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.509(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.361(3) . ? C4 H4 0.947(15) . ? C5 C6 1.493(3) . ? C5 H5 0.956(15) . ? C6 C7 1.531(3) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C8 1.522(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8 0.954(15) . ? C9 N1 1.323(3) . ? C9 C10 1.370(3) . ? C9 H9 0.9500 . ? C10 C11 1.384(3) . ? C10 H10 0.9500 . ? C11 C12 1.376(3) . ? C11 H11 0.9500 . ? C12 C13 1.384(2) . ? C12 C14 1.505(2) . ? C13 N1 1.337(2) . ? C13 H13 0.9500 . ? C14 N2 1.4731(19) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.339(2) . ? C15 N2 1.387(2) . ? C15 H15 0.9500 . ? C16 N3 1.387(2) . ? C16 H16 0.9500 . ? C17 N2 1.3588(19) . ? C17 N3 1.3632(19) . ? C18 C23 1.394(2) . ? C18 C19 1.397(2) . ? C18 N3 1.4447(19) . ? C19 C20 1.390(2) . ? C19 C24 1.507(2) . ? C20 C21 1.388(2) . ? C20 H20 0.9500 . ? C21 C22 1.383(3) . ? C21 C25 1.505(2) . ? C22 C23 1.393(2) . ? C22 H22 0.9500 . ? C23 C26 1.507(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C17 Rh1 C1 90.95(6) . . ? C17 Rh1 C8 92.22(6) . . ? C1 Rh1 C8 38.89(7) . . ? C17 Rh1 C5 159.65(7) . . ? C1 Rh1 C5 96.51(7) . . ? C8 Rh1 C5 82.03(8) . . ? C17 Rh1 C4 164.34(7) . . ? C1 Rh1 C4 81.14(7) . . ? C8 Rh1 C4 90.04(7) . . ? C5 Rh1 C4 35.90(8) . . ? C17 Rh1 Cl1 90.77(4) . . ? C1 Rh1 Cl1 161.41(5) . . ? C8 Rh1 Cl1 159.41(5) . . ? C5 Rh1 Cl1 88.15(6) . . ? C4 Rh1 Cl1 92.55(5) . . ? C8 C1 C2 126.14(16) . . ? C8 C1 Rh1 70.90(10) . . ? C2 C1 Rh1 111.13(12) . . ? C8 C1 H1 115.8(12) . . ? C2 C1 H1 114.2(12) . . ? Rh1 C1 H1 107.6(12) . . ? C1 C2 C3 114.17(15) . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C1 C2 H2B 108.7 . . ? C3 C2 H2B 108.7 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 112.16(15) . . ? C4 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C4 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C3 122.99(19) . . ? C5 C4 Rh1 70.81(11) . . ? C3 C4 Rh1 111.36(13) . . ? C5 C4 H4 116.8(13) . . ? C3 C4 H4 118.2(13) . . ? Rh1 C4 H4 101.2(13) . . ? C4 C5 C6 125.4(2) . . ? C4 C5 Rh1 73.29(10) . . ? C6 C5 Rh1 108.88(14) . . ? C4 C5 H5 117.1(14) . . ? C6 C5 H5 115.8(14) . . ? Rh1 C5 H5 101.1(14) . . ? C5 C6 C7 114.15(16) . . ? C5 C6 H6A 108.7 . . ? C7 C6 H6A 108.7 . . ? C5 C6 H6B 108.7 . . ? C7 C6 H6B 108.7 . . ? H6A C6 H6B 107.6 . . ? C8 C7 C6 113.60(17) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C1 C8 C7 123.36(17) . . ? C1 C8 Rh1 70.22(10) . . ? C7 C8 Rh1 113.45(14) . . ? C1 C8 H8 116.7(13) . . ? C7 C8 H8 114.7(13) . . ? Rh1 C8 H8 108.5(13) . . ? N1 C9 C10 123.80(18) . . ? N1 C9 H9 118.1 . . ? C10 C9 H9 118.1 . . ? C9 C10 C11 118.8(2) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 119.0(2) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 117.38(16) . . ? C11 C12 C14 121.64(16) . . ? C13 C12 C14 120.74(15) . . ? N1 C13 C12 124.40(18) . . ? N1 C13 H13 117.8 . . ? C12 C13 H13 117.8 . . ? N2 C14 C12 115.51(13) . . ? N2 C14 H14A 108.4 . . ? C12 C14 H14A 108.4 . . ? N2 C14 H14B 108.4 . . ? C12 C14 H14B 108.4 . . ? H14A C14 H14B 107.5 . . ? C16 C15 N2 106.69(14) . . ? C16 C15 H15 126.7 . . ? N2 C15 H15 126.7 . . ? C15 C16 N3 106.88(14) . . ? C15 C16 H16 126.6 . . ? N3 C16 H16 126.6 . . ? N2 C17 N3 103.65(12) . . ? N2 C17 Rh1 125.69(11) . . ? N3 C17 Rh1 130.65(11) . . ? C23 C18 C19 122.01(14) . . ? C23 C18 N3 119.68(14) . . ? C19 C18 N3 118.20(13) . . ? C20 C19 C18 117.70(15) . . ? C20 C19 C24 120.51(15) . . ? C18 C19 C24 121.75(14) . . ? C21 C20 C19 121.93(16) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C22 C21 C20 118.48(15) . . ? C22 C21 C25 120.97(17) . . ? C20 C21 C25 120.52(18) . . ? C21 C22 C23 122.06(16) . . ? C21 C22 H22 119.0 . . ? C23 C22 H22 119.0 . . ? C22 C23 C18 117.61(15) . . ? C22 C23 C26 119.64(15) . . ? C18 C23 C26 122.71(15) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C9 N1 C13 116.56(18) . . ? C17 N2 C15 111.51(13) . . ? C17 N2 C14 124.68(13) . . ? C15 N2 C14 123.35(13) . . ? C17 N3 C16 111.26(13) . . ? C17 N3 C18 125.71(12) . . ? C16 N3 C18 122.50(13) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Rh1 C1 C8 92.36(11) . . . . ? C5 Rh1 C1 C8 -68.67(12) . . . . ? C4 Rh1 C1 C8 -101.22(12) . . . . ? Cl1 Rh1 C1 C8 -172.40(12) . . . . ? C17 Rh1 C1 C2 -145.28(13) . . . . ? C8 Rh1 C1 C2 122.36(17) . . . . ? C5 Rh1 C1 C2 53.70(14) . . . . ? C4 Rh1 C1 C2 21.14(13) . . . . ? Cl1 Rh1 C1 C2 -50.0(2) . . . . ? C8 C1 C2 C3 45.7(3) . . . . ? Rh1 C1 C2 C3 -35.5(2) . . . . ? C1 C2 C3 C4 31.7(2) . . . . ? C2 C3 C4 C5 -93.2(2) . . . . ? C2 C3 C4 Rh1 -12.8(2) . . . . ? C17 Rh1 C4 C5 174.7(2) . . . . ? C1 Rh1 C4 C5 114.27(14) . . . . ? C8 Rh1 C4 C5 76.26(14) . . . . ? Cl1 Rh1 C4 C5 -83.31(13) . . . . ? C17 Rh1 C4 C3 55.8(3) . . . . ? C1 Rh1 C4 C3 -4.61(14) . . . . ? C8 Rh1 C4 C3 -42.62(14) . . . . ? C5 Rh1 C4 C3 -118.9(2) . . . . ? Cl1 Rh1 C4 C3 157.81(13) . . . . ? C3 C4 C5 C6 1.9(3) . . . . ? Rh1 C4 C5 C6 -101.6(2) . . . . ? C3 C4 C5 Rh1 103.53(17) . . . . ? C17 Rh1 C5 C4 -175.86(16) . . . . ? C1 Rh1 C5 C4 -65.04(14) . . . . ? C8 Rh1 C5 C4 -101.23(13) . . . . ? Cl1 Rh1 C5 C4 96.91(12) . . . . ? C17 Rh1 C5 C6 -53.4(3) . . . . ? C1 Rh1 C5 C6 57.39(15) . . . . ? C8 Rh1 C5 C6 21.20(14) . . . . ? C4 Rh1 C5 C6 122.4(2) . . . . ? Cl1 Rh1 C5 C6 -140.66(14) . . . . ? C4 C5 C6 C7 51.4(3) . . . . ? Rh1 C5 C6 C7 -31.1(2) . . . . ? C5 C6 C7 C8 25.9(3) . . . . ? C2 C1 C8 C7 3.0(3) . . . . ? Rh1 C1 C8 C7 105.63(19) . . . . ? C2 C1 C8 Rh1 -102.67(18) . . . . ? C6 C7 C8 C1 -87.9(2) . . . . ? C6 C7 C8 Rh1 -6.8(2) . . . . ? C17 Rh1 C8 C1 -88.76(11) . . . . ? C5 Rh1 C8 C1 110.85(12) . . . . ? C4 Rh1 C8 C1 75.74(11) . . . . ? Cl1 Rh1 C8 C1 173.11(11) . . . . ? C17 Rh1 C8 C7 152.49(14) . . . . ? C1 Rh1 C8 C7 -118.75(18) . . . . ? C5 Rh1 C8 C7 -7.90(14) . . . . ? C4 Rh1 C8 C7 -43.01(14) . . . . ? Cl1 Rh1 C8 C7 54.4(2) . . . . ? N1 C9 C10 C11 1.9(3) . . . . ? C9 C10 C11 C12 -0.2(3) . . . . ? C10 C11 C12 C13 -1.9(3) . . . . ? C10 C11 C12 C14 -176.36(17) . . . . ? C11 C12 C13 N1 2.7(3) . . . . ? C14 C12 C13 N1 177.22(16) . . . . ? C11 C12 C14 N2 -112.18(18) . . . . ? C13 C12 C14 N2 73.53(19) . . . . ? N2 C15 C16 N3 0.09(18) . . . . ? C1 Rh1 C17 N2 -122.31(13) . . . . ? C8 Rh1 C17 N2 -83.42(13) . . . . ? C5 Rh1 C17 N2 -10.6(3) . . . . ? C4 Rh1 C17 N2 178.5(2) . . . . ? Cl1 Rh1 C17 N2 76.20(12) . . . . ? C1 Rh1 C17 N3 56.17(14) . . . . ? C8 Rh1 C17 N3 95.05(14) . . . . ? C5 Rh1 C17 N3 167.92(19) . . . . ? C4 Rh1 C17 N3 -3.1(3) . . . . ? Cl1 Rh1 C17 N3 -105.32(13) . . . . ? C23 C18 C19 C20 4.8(2) . . . . ? N3 C18 C19 C20 -178.93(13) . . . . ? C23 C18 C19 C24 -172.87(14) . . . . ? N3 C18 C19 C24 3.3(2) . . . . ? C18 C19 C20 C21 -1.1(2) . . . . ? C24 C19 C20 C21 176.68(15) . . . . ? C19 C20 C21 C22 -2.1(2) . . . . ? C19 C20 C21 C25 179.80(16) . . . . ? C20 C21 C22 C23 1.7(2) . . . . ? C25 C21 C22 C23 179.80(16) . . . . ? C21 C22 C23 C18 1.8(2) . . . . ? C21 C22 C23 C26 -175.91(16) . . . . ? C19 C18 C23 C22 -5.2(2) . . . . ? N3 C18 C23 C22 178.63(14) . . . . ? C19 C18 C23 C26 172.45(15) . . . . ? N3 C18 C23 C26 -3.7(2) . . . . ? C10 C9 N1 C13 -1.3(3) . . . . ? C12 C13 N1 C9 -1.1(3) . . . . ? N3 C17 N2 C15 0.82(16) . . . . ? Rh1 C17 N2 C15 179.63(10) . . . . ? N3 C17 N2 C14 173.18(13) . . . . ? Rh1 C17 N2 C14 -8.0(2) . . . . ? C16 C15 N2 C17 -0.58(18) . . . . ? C16 C15 N2 C14 -173.07(14) . . . . ? C12 C14 N2 C17 101.38(17) . . . . ? C12 C14 N2 C15 -87.13(18) . . . . ? N2 C17 N3 C16 -0.76(16) . . . . ? Rh1 C17 N3 C16 -179.48(11) . . . . ? N2 C17 N3 C18 -172.50(13) . . . . ? Rh1 C17 N3 C18 8.8(2) . . . . ? C15 C16 N3 C17 0.43(18) . . . . ? C15 C16 N3 C18 172.48(14) . . . . ? C23 C18 N3 C17 -106.34(17) . . . . ? C19 C18 N3 C17 77.35(19) . . . . ? C23 C18 N3 C16 82.79(19) . . . . ? C19 C18 N3 C16 -93.52(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.345 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.053