# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Eduardo Peris' _publ_contact_author_email EPERIS@QIO.UJI.ES _publ_section_title ; Easy Preparation of Cp*-Functionalized N-Heterocyclic Carbenes and their Coordination to Rhodium and Iridium ; loop_ _publ_author_name 'Eduardo Peris' 'Andre Pontes da Costa' 'Beatriz Royo' 'Mercedes Sanau' # Attachment 'Compound9.txt' data_str975m/Compound9 _database_code_depnum_ccdc_archive 'CCDC 717566' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H26 I Ir N2' _chemical_formula_weight 637.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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' I I -0.4742 1.8119 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 15.0849(16) _cell_length_b 8.8037(10) _cell_length_c 16.2181(17) _cell_angle_alpha 90.00 _cell_angle_beta 98.598(2) _cell_angle_gamma 90.00 _cell_volume 2129.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 1603 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.30 _exptl_crystal_description prismatic _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 7.727 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.4264 _exptl_absorpt_correction_T_max 0.6759 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9969 _diffrn_reflns_av_R_equivalents 0.1059 _diffrn_reflns_av_sigmaI/netI 0.1214 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 23.82 _reflns_number_total 3263 _reflns_number_gt 1869 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1087P)^2^+0.0000P] 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 3263 _refine_ls_number_parameters 241 _refine_ls_number_restraints 167 _refine_ls_R_factor_all 0.1399 _refine_ls_R_factor_gt 0.0733 _refine_ls_wR_factor_ref 0.1916 _refine_ls_wR_factor_gt 0.1624 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.947 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.24782(5) 0.39393(9) 0.46809(5) 0.0345(3) Uani 1 1 d . . . N1 N 0.4092(10) 0.5410(18) 0.4004(10) 0.038(4) Uani 1 1 d . . . C1 C 0.3486(11) 0.526(2) 0.4552(11) 0.028(4) Uani 1 1 d . . . I1 I 0.30479(11) 0.11930(17) 0.42391(10) 0.0616(5) Uani 1 1 d . . . N2 N 0.3684(10) 0.6481(16) 0.5065(9) 0.033(4) Uani 1 1 d . . . C2 C 0.4117(18) 0.448(3) 0.3271(16) 0.073(8) Uani 1 1 d . . . H2A H 0.3649 0.4786 0.2836 0.109 Uiso 1 1 calc R . . H2B H 0.4031 0.3430 0.3408 0.109 Uiso 1 1 calc R . . H2C H 0.4688 0.4592 0.3084 0.109 Uiso 1 1 calc R . . C3 C 0.4602(12) 0.670(2) 0.4173(13) 0.041(5) Uani 1 1 d U . . H3 H 0.5048 0.7048 0.3881 0.049 Uiso 1 1 calc R . . C4 C 0.4336(13) 0.736(2) 0.4834(12) 0.038(5) Uani 1 1 d U . . H4 H 0.4558 0.8260 0.5088 0.046 Uiso 1 1 calc R . . C5 C 0.3155(14) 0.672(2) 0.5792(12) 0.039(4) Uani 1 1 d U . . C6 C 0.2123(13) 0.703(2) 0.5406(11) 0.040(4) Uani 1 1 d U . . H6A H 0.1790 0.7243 0.5860 0.047 Uiso 1 1 calc R . . H6B H 0.2097 0.7929 0.5059 0.047 Uiso 1 1 calc R . . C7 C 0.3491(17) 0.815(2) 0.6261(13) 0.057(6) Uani 1 1 d U . . H7A H 0.3289 0.9025 0.5933 0.086 Uiso 1 1 calc R . . H7B H 0.4135 0.8140 0.6365 0.086 Uiso 1 1 calc R . . H7C H 0.3263 0.8189 0.6782 0.086 Uiso 1 1 calc R . . C11 C 0.0988(12) 0.348(2) 0.4474(13) 0.044(4) Uani 1 1 d U . . C12 C 0.1239(13) 0.429(3) 0.3754(12) 0.048(4) Uani 1 1 d U . . C13 C 0.1583(14) 0.568(3) 0.3981(12) 0.048(4) Uani 1 1 d U . . C14 C 0.1671(12) 0.576(2) 0.4900(12) 0.036(4) Uani 1 1 d U . . C15 C 0.1207(12) 0.445(2) 0.5186(12) 0.039(4) Uani 1 1 d U . . C16 C 0.1024(14) 0.411(2) 0.6020(13) 0.052(5) Uani 1 1 d U . . H16A H 0.1303 0.3166 0.6206 0.077 Uiso 1 1 calc R . . H16B H 0.0389 0.4036 0.6014 0.077 Uiso 1 1 calc R . . H16C H 0.1261 0.4910 0.6392 0.077 Uiso 1 1 calc R . . C17 C 0.0515(16) 0.207(3) 0.4490(16) 0.075(7) Uani 1 1 d U . . H17A H 0.0707 0.1382 0.4093 0.112 Uiso 1 1 calc R . . H17B H -0.0117 0.2249 0.4349 0.112 Uiso 1 1 calc R . . H17C H 0.0638 0.1636 0.5038 0.112 Uiso 1 1 calc R . . C18 C 0.1024(16) 0.363(3) 0.2879(13) 0.067(7) Uani 1 1 d U . . H18A H 0.1434 0.2815 0.2816 0.101 Uiso 1 1 calc R . . H18B H 0.1080 0.4404 0.2476 0.101 Uiso 1 1 calc R . . H18C H 0.0421 0.3241 0.2795 0.101 Uiso 1 1 calc R . . C19 C 0.1854(15) 0.686(3) 0.3413(12) 0.054(5) Uani 1 1 d U . . H19A H 0.1391 0.7613 0.3309 0.081 Uiso 1 1 calc R . . H19B H 0.1944 0.6397 0.2896 0.081 Uiso 1 1 calc R . . H19C H 0.2401 0.7329 0.3668 0.081 Uiso 1 1 calc R . . C21 C 0.3259(13) 0.526(2) 0.6305(12) 0.036(4) Uani 1 1 d U . . C22 C 0.3093(12) 0.385(2) 0.5912(11) 0.032(4) Uani 1 1 d U . . C23 C 0.3143(13) 0.259(2) 0.6399(12) 0.044(4) Uani 1 1 d U . . H23 H 0.2961 0.1661 0.6153 0.052 Uiso 1 1 calc R . . C24 C 0.3456(15) 0.263(3) 0.7249(14) 0.062(5) Uani 1 1 d U . . H24 H 0.3557 0.1732 0.7553 0.074 Uiso 1 1 calc R . . C25 C 0.3605(14) 0.393(3) 0.7612(13) 0.056(5) Uani 1 1 d U . . H25 H 0.3775 0.3977 0.8187 0.067 Uiso 1 1 calc R . . C26 C 0.3509(14) 0.530(3) 0.7141(13) 0.053(5) Uani 1 1 d U . . H26 H 0.3619 0.6232 0.7409 0.063 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 0.0435(5) 0.0298(5) 0.0303(5) 0.0013(4) 0.0058(3) 0.0011(4) N1 0.032(9) 0.029(9) 0.051(11) 0.006(9) 0.003(8) 0.010(8) C1 0.028(11) 0.028(11) 0.028(10) 0.020(10) 0.005(8) 0.002(9) I1 0.0911(12) 0.0338(9) 0.0623(10) -0.0055(8) 0.0194(8) 0.0063(8) N2 0.046(10) 0.019(9) 0.033(9) -0.007(8) 0.004(7) 0.001(7) C2 0.09(2) 0.040(15) 0.09(2) -0.004(15) 0.021(16) 0.033(14) C3 0.032(11) 0.040(12) 0.053(12) 0.020(10) 0.011(9) -0.001(10) C4 0.041(11) 0.025(11) 0.045(11) 0.004(9) -0.004(9) -0.009(9) C5 0.061(9) 0.028(7) 0.029(9) -0.008(6) 0.010(8) 0.001(9) C6 0.058(9) 0.030(9) 0.034(9) -0.008(7) 0.018(7) 0.014(7) C7 0.099(15) 0.031(9) 0.037(12) -0.017(10) -0.005(11) 0.006(11) C11 0.023(9) 0.056(10) 0.049(7) 0.001(7) -0.005(8) 0.001(8) C12 0.039(11) 0.062(11) 0.037(7) 0.001(7) -0.009(8) -0.002(9) C13 0.052(12) 0.058(11) 0.031(7) 0.000(7) -0.002(8) 0.001(9) C14 0.041(9) 0.032(9) 0.040(7) -0.008(6) 0.019(7) 0.021(6) C15 0.021(9) 0.048(10) 0.048(7) 0.000(7) 0.003(8) 0.010(7) C16 0.055(13) 0.043(13) 0.054(8) 0.015(10) -0.001(10) 0.003(11) C17 0.057(15) 0.085(16) 0.076(16) 0.004(12) -0.009(13) -0.035(13) C18 0.070(16) 0.085(19) 0.046(9) -0.015(11) 0.008(11) -0.013(14) C19 0.072(15) 0.058(13) 0.030(10) -0.001(10) -0.001(10) -0.002(12) C21 0.049(11) 0.035(6) 0.030(8) 0.002(6) 0.018(8) 0.003(8) C22 0.034(9) 0.031(7) 0.033(8) 0.004(6) 0.009(7) 0.017(9) C23 0.045(11) 0.037(8) 0.048(9) 0.016(8) 0.002(9) 0.001(10) C24 0.065(14) 0.073(11) 0.047(9) 0.023(10) 0.007(10) 0.000(13) C25 0.047(11) 0.087(12) 0.034(9) 0.010(8) 0.010(9) 0.009(13) C26 0.057(13) 0.068(10) 0.033(8) -0.001(7) 0.007(10) 0.006(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.951(17) . ? Ir1 C14 2.073(17) . ? Ir1 C22 2.074(18) . ? Ir1 C13 2.24(2) . ? Ir1 C12 2.238(19) . ? Ir1 C15 2.239(18) . ? Ir1 C11 2.259(18) . ? Ir1 I1 2.6985(17) . ? N1 C1 1.37(2) . ? N1 C3 1.38(3) . ? N1 C2 1.45(3) . ? C1 N2 1.36(2) . ? N2 C4 1.35(2) . ? N2 C5 1.53(2) . ? C3 C4 1.33(3) . ? C5 C7 1.52(3) . ? C5 C21 1.53(3) . ? C5 C6 1.61(3) . ? C6 C14 1.49(3) . ? C11 C15 1.43(3) . ? C11 C17 1.43(3) . ? C11 C12 1.46(3) . ? C12 C13 1.36(3) . ? C12 C18 1.52(3) . ? C13 C14 1.48(3) . ? C13 C19 1.49(3) . ? C14 C15 1.46(3) . ? C15 C16 1.45(3) . ? C21 C26 1.35(3) . ? C21 C22 1.40(3) . ? C22 C23 1.36(3) . ? C23 C24 1.39(3) . ? C24 C25 1.30(3) . ? C25 C26 1.42(3) . ? 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 C1 Ir1 C14 92.5(8) . . ? C1 Ir1 C22 83.2(7) . . ? C14 Ir1 C22 93.1(7) . . ? C1 Ir1 C13 87.6(8) . . ? C14 Ir1 C13 39.9(8) . . ? C22 Ir1 C13 131.6(7) . . ? C1 Ir1 C12 115.6(7) . . ? C14 Ir1 C12 63.7(8) . . ? C22 Ir1 C12 149.4(7) . . ? C13 Ir1 C12 35.4(8) . . ? C1 Ir1 C15 130.1(8) . . ? C14 Ir1 C15 39.4(7) . . ? C22 Ir1 C15 86.5(7) . . ? C13 Ir1 C15 64.2(7) . . ? C12 Ir1 C15 62.9(7) . . ? C1 Ir1 C11 149.9(7) . . ? C14 Ir1 C11 64.3(8) . . ? C22 Ir1 C11 115.4(7) . . ? C13 Ir1 C11 62.3(8) . . ? C12 Ir1 C11 38.0(7) . . ? C15 Ir1 C11 37.1(7) . . ? C1 Ir1 I1 102.8(6) . . ? C14 Ir1 I1 162.9(6) . . ? C22 Ir1 I1 96.2(5) . . ? C13 Ir1 I1 132.1(5) . . ? C12 Ir1 I1 102.2(6) . . ? C15 Ir1 I1 126.9(5) . . ? C11 Ir1 I1 98.6(6) . . ? C1 N1 C3 110.9(17) . . ? C1 N1 C2 125.4(18) . . ? C3 N1 C2 123.2(18) . . ? N2 C1 N1 102.4(15) . . ? N2 C1 Ir1 120.5(13) . . ? N1 C1 Ir1 136.9(15) . . ? C4 N2 C1 112.7(15) . . ? C4 N2 C5 128.3(16) . . ? C1 N2 C5 119.0(15) . . ? C4 C3 N1 107.0(17) . . ? C3 C4 N2 107.0(17) . . ? C7 C5 C21 115.2(15) . . ? C7 C5 N2 108.9(17) . . ? C21 C5 N2 106.4(15) . . ? C7 C5 C6 106.5(16) . . ? C21 C5 C6 111.7(16) . . ? N2 C5 C6 107.9(14) . . ? C14 C6 C5 114.9(15) . . ? C15 C11 C17 124(2) . . ? C15 C11 C12 107.4(18) . . ? C17 C11 C12 129(2) . . ? C15 C11 Ir1 70.7(10) . . ? C17 C11 Ir1 129.7(16) . . ? C12 C11 Ir1 70.2(10) . . ? C13 C12 C11 110.8(18) . . ? C13 C12 C18 128(2) . . ? C11 C12 C18 121(2) . . ? C13 C12 Ir1 72.2(12) . . ? C11 C12 Ir1 71.8(10) . . ? C18 C12 Ir1 127.9(16) . . ? C12 C13 C14 106.8(19) . . ? C12 C13 C19 126.3(19) . . ? C14 C13 C19 126.9(19) . . ? C12 C13 Ir1 72.4(13) . . ? C14 C13 Ir1 64.1(10) . . ? C19 C13 Ir1 126.3(15) . . ? C15 C14 C13 108.0(18) . . ? C15 C14 C6 128.2(17) . . ? C13 C14 C6 123.7(18) . . ? C15 C14 Ir1 76.5(11) . . ? C13 C14 Ir1 76.0(11) . . ? C6 C14 Ir1 116.2(12) . . ? C11 C15 C16 125.3(19) . . ? C11 C15 C14 106.0(18) . . ? C16 C15 C14 128.6(19) . . ? C11 C15 Ir1 72.2(11) . . ? C16 C15 Ir1 126.4(14) . . ? C14 C15 Ir1 64.2(9) . . ? C26 C21 C22 119(2) . . ? C26 C21 C5 121(2) . . ? C22 C21 C5 120.0(16) . . ? C23 C22 C21 118.1(17) . . ? C23 C22 Ir1 124.5(15) . . ? C21 C22 Ir1 115.5(13) . . ? C22 C23 C24 122(2) . . ? C25 C24 C23 119(2) . . ? C24 C25 C26 121(2) . . ? C21 C26 C25 120(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 C1 N2 -2.2(18) . . . . ? C2 N1 C1 N2 -173.8(17) . . . . ? C3 N1 C1 Ir1 172.6(15) . . . . ? C2 N1 C1 Ir1 1(3) . . . . ? C14 Ir1 C1 N2 40.6(14) . . . . ? C22 Ir1 C1 N2 -52.2(13) . . . . ? C13 Ir1 C1 N2 80.2(14) . . . . ? C12 Ir1 C1 N2 102.5(14) . . . . ? C15 Ir1 C1 N2 27.4(17) . . . . ? C11 Ir1 C1 N2 79(2) . . . . ? I1 Ir1 C1 N2 -147.1(12) . . . . ? C14 Ir1 C1 N1 -133.6(19) . . . . ? C22 Ir1 C1 N1 133.7(19) . . . . ? C13 Ir1 C1 N1 -94.0(19) . . . . ? C12 Ir1 C1 N1 -72(2) . . . . ? C15 Ir1 C1 N1 -146.7(17) . . . . ? C11 Ir1 C1 N1 -95(2) . . . . ? I1 Ir1 C1 N1 38.8(19) . . . . ? N1 C1 N2 C4 2.6(19) . . . . ? Ir1 C1 N2 C4 -173.3(13) . . . . ? N1 C1 N2 C5 -178.9(14) . . . . ? Ir1 C1 N2 C5 5(2) . . . . ? C1 N1 C3 C4 1(2) . . . . ? C2 N1 C3 C4 173.0(18) . . . . ? N1 C3 C4 N2 1(2) . . . . ? C1 N2 C4 C3 -2(2) . . . . ? C5 N2 C4 C3 179.6(17) . . . . ? C4 N2 C5 C7 -1(3) . . . . ? C1 N2 C5 C7 -179.4(16) . . . . ? C4 N2 C5 C21 -125.9(19) . . . . ? C1 N2 C5 C21 56(2) . . . . ? C4 N2 C5 C6 114(2) . . . . ? C1 N2 C5 C6 -64(2) . . . . ? C7 C5 C6 C14 178.7(17) . . . . ? C21 C5 C6 C14 -55(2) . . . . ? N2 C5 C6 C14 62(2) . . . . ? C1 Ir1 C11 C15 -81.3(19) . . . . ? C14 Ir1 C11 C15 -38.2(12) . . . . ? C22 Ir1 C11 C15 42.5(14) . . . . ? C13 Ir1 C11 C15 -83.0(13) . . . . ? C12 Ir1 C11 C15 -117.6(18) . . . . ? I1 Ir1 C11 C15 143.6(11) . . . . ? C1 Ir1 C11 C17 160.5(19) . . . . ? C14 Ir1 C11 C17 -156(2) . . . . ? C22 Ir1 C11 C17 -76(2) . . . . ? C13 Ir1 C11 C17 159(2) . . . . ? C12 Ir1 C11 C17 124(3) . . . . ? C15 Ir1 C11 C17 -118(3) . . . . ? I1 Ir1 C11 C17 25(2) . . . . ? C1 Ir1 C11 C12 36(2) . . . . ? C14 Ir1 C11 C12 79.4(13) . . . . ? C22 Ir1 C11 C12 160.0(12) . . . . ? C13 Ir1 C11 C12 34.5(12) . . . . ? C15 Ir1 C11 C12 117.6(18) . . . . ? I1 Ir1 C11 C12 -98.8(12) . . . . ? C15 C11 C12 C13 -1(2) . . . . ? C17 C11 C12 C13 172(2) . . . . ? Ir1 C11 C12 C13 -62.0(15) . . . . ? C15 C11 C12 C18 -175.0(19) . . . . ? C17 C11 C12 C18 -2(3) . . . . ? Ir1 C11 C12 C18 124(2) . . . . ? C15 C11 C12 Ir1 61.3(12) . . . . ? C17 C11 C12 Ir1 -126(2) . . . . ? C1 Ir1 C12 C13 -40.9(15) . . . . ? C14 Ir1 C12 C13 38.6(13) . . . . ? C22 Ir1 C12 C13 83(2) . . . . ? C15 Ir1 C12 C13 82.9(14) . . . . ? C11 Ir1 C12 C13 119.9(19) . . . . ? I1 Ir1 C12 C13 -151.7(12) . . . . ? C1 Ir1 C12 C11 -160.8(12) . . . . ? C14 Ir1 C12 C11 -81.3(13) . . . . ? C22 Ir1 C12 C11 -37(2) . . . . ? C13 Ir1 C12 C11 -119.9(19) . . . . ? C15 Ir1 C12 C11 -37.0(12) . . . . ? I1 Ir1 C12 C11 88.4(12) . . . . ? C1 Ir1 C12 C18 84(2) . . . . ? C14 Ir1 C12 C18 163(2) . . . . ? C22 Ir1 C12 C18 -152.6(18) . . . . ? C13 Ir1 C12 C18 125(3) . . . . ? C15 Ir1 C12 C18 -152(2) . . . . ? C11 Ir1 C12 C18 -115(3) . . . . ? I1 Ir1 C12 C18 -27(2) . . . . ? C11 C12 C13 C14 7(2) . . . . ? C18 C12 C13 C14 -180(2) . . . . ? Ir1 C12 C13 C14 -55.0(13) . . . . ? C11 C12 C13 C19 -176(2) . . . . ? C18 C12 C13 C19 -2(4) . . . . ? Ir1 C12 C13 C19 123(2) . . . . ? C11 C12 C13 Ir1 61.8(14) . . . . ? C18 C12 C13 Ir1 -125(2) . . . . ? C1 Ir1 C13 C12 143.8(14) . . . . ? C14 Ir1 C13 C12 -119.4(19) . . . . ? C22 Ir1 C13 C12 -137.5(13) . . . . ? C15 Ir1 C13 C12 -78.8(14) . . . . ? C11 Ir1 C13 C12 -37.1(13) . . . . ? I1 Ir1 C13 C12 38.6(16) . . . . ? C1 Ir1 C13 C14 -96.9(13) . . . . ? C22 Ir1 C13 C14 -18.2(16) . . . . ? C12 Ir1 C13 C14 119.4(19) . . . . ? C15 Ir1 C13 C14 40.5(12) . . . . ? C11 Ir1 C13 C14 82.3(13) . . . . ? I1 Ir1 C13 C14 158.0(9) . . . . ? C1 Ir1 C13 C19 21.3(18) . . . . ? C14 Ir1 C13 C19 118(2) . . . . ? C22 Ir1 C13 C19 100.0(18) . . . . ? C12 Ir1 C13 C19 -122(2) . . . . ? C15 Ir1 C13 C19 159(2) . . . . ? C11 Ir1 C13 C19 -160(2) . . . . ? I1 Ir1 C13 C19 -83.9(19) . . . . ? C12 C13 C14 C15 -10(2) . . . . ? C19 C13 C14 C15 172(2) . . . . ? Ir1 C13 C14 C15 -70.5(12) . . . . ? C12 C13 C14 C6 172.6(17) . . . . ? C19 C13 C14 C6 -5(3) . . . . ? Ir1 C13 C14 C6 112.4(17) . . . . ? C12 C13 C14 Ir1 60.2(15) . . . . ? C19 C13 C14 Ir1 -117(2) . . . . ? C5 C6 C14 C15 87(2) . . . . ? C5 C6 C14 C13 -97(2) . . . . ? C5 C6 C14 Ir1 -6(2) . . . . ? C1 Ir1 C14 C15 -164.0(11) . . . . ? C22 Ir1 C14 C15 -80.7(12) . . . . ? C13 Ir1 C14 C15 112.8(17) . . . . ? C12 Ir1 C14 C15 78.5(12) . . . . ? C11 Ir1 C14 C15 36.0(11) . . . . ? I1 Ir1 C14 C15 42(2) . . . . ? C1 Ir1 C14 C13 83.2(12) . . . . ? C22 Ir1 C14 C13 166.5(12) . . . . ? C12 Ir1 C14 C13 -34.3(12) . . . . ? C15 Ir1 C14 C13 -112.8(17) . . . . ? C11 Ir1 C14 C13 -76.7(13) . . . . ? I1 Ir1 C14 C13 -71(2) . . . . ? C1 Ir1 C14 C6 -37.8(15) . . . . ? C22 Ir1 C14 C6 45.5(15) . . . . ? C13 Ir1 C14 C6 -121(2) . . . . ? C12 Ir1 C14 C6 -155.3(17) . . . . ? C15 Ir1 C14 C6 126.2(19) . . . . ? C11 Ir1 C14 C6 162.3(17) . . . . ? I1 Ir1 C14 C6 168.2(11) . . . . ? C17 C11 C15 C16 3(3) . . . . ? C12 C11 C15 C16 176.6(18) . . . . ? Ir1 C11 C15 C16 -122.4(19) . . . . ? C17 C11 C15 C14 -179.2(19) . . . . ? C12 C11 C15 C14 -6(2) . . . . ? Ir1 C11 C15 C14 55.3(12) . . . . ? C17 C11 C15 Ir1 125(2) . . . . ? C12 C11 C15 Ir1 -61.0(13) . . . . ? C13 C14 C15 C11 10(2) . . . . ? C6 C14 C15 C11 -173.3(17) . . . . ? Ir1 C14 C15 C11 -60.5(13) . . . . ? C13 C14 C15 C16 -172.7(19) . . . . ? C6 C14 C15 C16 4(3) . . . . ? Ir1 C14 C15 C16 117.2(19) . . . . ? C13 C14 C15 Ir1 70.1(13) . . . . ? C6 C14 C15 Ir1 -112.9(19) . . . . ? C1 Ir1 C15 C11 139.6(12) . . . . ? C14 Ir1 C15 C11 118.5(17) . . . . ? C22 Ir1 C15 C11 -142.3(13) . . . . ? C13 Ir1 C15 C11 77.5(13) . . . . ? C12 Ir1 C15 C11 37.8(12) . . . . ? I1 Ir1 C15 C11 -47.2(13) . . . . ? C1 Ir1 C15 C16 -99.3(19) . . . . ? C14 Ir1 C15 C16 -120(2) . . . . ? C22 Ir1 C15 C16 -21.2(19) . . . . ? C13 Ir1 C15 C16 -161(2) . . . . ? C12 Ir1 C15 C16 159(2) . . . . ? C11 Ir1 C15 C16 121(2) . . . . ? I1 Ir1 C15 C16 74.0(19) . . . . ? C1 Ir1 C15 C14 21.0(15) . . . . ? C22 Ir1 C15 C14 99.1(12) . . . . ? C13 Ir1 C15 C14 -41.1(12) . . . . ? C12 Ir1 C15 C14 -80.7(13) . . . . ? C11 Ir1 C15 C14 -118.5(17) . . . . ? I1 Ir1 C15 C14 -165.7(9) . . . . ? C7 C5 C21 C26 9(3) . . . . ? N2 C5 C21 C26 130.1(19) . . . . ? C6 C5 C21 C26 -112(2) . . . . ? C7 C5 C21 C22 -170.8(19) . . . . ? N2 C5 C21 C22 -50(2) . . . . ? C6 C5 C21 C22 68(2) . . . . ? C26 C21 C22 C23 4(3) . . . . ? C5 C21 C22 C23 -176.2(18) . . . . ? C26 C21 C22 Ir1 168.4(15) . . . . ? C5 C21 C22 Ir1 -11(2) . . . . ? C1 Ir1 C22 C23 -141.6(17) . . . . ? C14 Ir1 C22 C23 126.2(17) . . . . ? C13 Ir1 C22 C23 137.7(16) . . . . ? C12 Ir1 C22 C23 88(2) . . . . ? C15 Ir1 C22 C23 87.3(17) . . . . ? C11 Ir1 C22 C23 63.2(17) . . . . ? I1 Ir1 C22 C23 -39.4(16) . . . . ? C1 Ir1 C22 C21 54.7(14) . . . . ? C14 Ir1 C22 C21 -37.5(15) . . . . ? C13 Ir1 C22 C21 -26.0(18) . . . . ? C12 Ir1 C22 C21 -76(2) . . . . ? C15 Ir1 C22 C21 -76.4(14) . . . . ? C11 Ir1 C22 C21 -100.5(15) . . . . ? I1 Ir1 C22 C21 156.9(13) . . . . ? C21 C22 C23 C24 -8(3) . . . . ? Ir1 C22 C23 C24 -171.3(16) . . . . ? C22 C23 C24 C25 8(3) . . . . ? C23 C24 C25 C26 -4(3) . . . . ? C22 C21 C26 C25 0(3) . . . . ? C5 C21 C26 C25 -179.9(18) . . . . ? C24 C25 C26 C21 0(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.82 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.914 _refine_diff_density_min -1.414 _refine_diff_density_rms 0.297 data_str1000/Compound5 _database_code_depnum_ccdc_archive 'CCDC 717567' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Cl2 Ir N2' _chemical_formula_weight 492.44 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' 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 Pn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 7.9908(5) _cell_length_b 13.1311(9) _cell_length_c 8.6289(6) _cell_angle_alpha 90.00 _cell_angle_beta 116.0640(10) _cell_angle_gamma 90.00 _cell_volume 813.34(9) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3700 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 29.93 _exptl_crystal_description fiber _exptl_crystal_colour orange _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_max 0.531 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.011 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 472 _exptl_absorpt_correction_type refdelf _exptl_absorpt_coefficient_mu 8.528 _exptl_absorpt_correction_T_min 0.1050 _exptl_absorpt_correction_T_max 0.1298 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4917 _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_sigmaI/netI 0.0533 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2241 _reflns_number_gt 2119 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0073P)^2^+1.1732P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.06(3) _refine_ls_number_reflns 2241 _refine_ls_number_parameters 176 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0308 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.248 _refine_ls_restrained_S_all 1.248 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ir1 Ir 0.70824(15) 0.240136(19) 0.49534(15) 0.02978(12) Uani 1 1 d . . . Cl1 Cl 0.4234(5) 0.1914(3) 0.2525(5) 0.0638(10) Uani 1 1 d . . . C1 C 0.7894(15) 0.3277(8) 0.3449(14) 0.041(2) Uani 1 1 d . . . N1 N 0.9692(14) 0.3276(8) 0.3626(13) 0.049(2) Uani 1 1 d . . . Cl2 Cl 0.5634(6) 0.3874(3) 0.5499(5) 0.0647(9) Uani 1 1 d . . . N2 N 0.7010(15) 0.3971(8) 0.2244(14) 0.053(3) Uani 1 1 d . . . C2 C 0.501(2) 0.4254(13) 0.149(2) 0.086(6) Uani 1 1 d . . . H2A H 0.4410 0.3882 0.2069 0.129 Uiso 1 1 calc R . . H2B H 0.4426 0.4093 0.0287 0.129 Uiso 1 1 calc R . . H2C H 0.4897 0.4971 0.1645 0.129 Uiso 1 1 calc R . . C3 C 0.822(2) 0.4399(11) 0.1678(19) 0.068(4) Uani 1 1 d . . . H3A H 0.7918 0.4895 0.0828 0.081 Uiso 1 1 calc R . . C4 C 0.986(2) 0.3987(10) 0.2544(18) 0.060(3) Uani 1 1 d . . . H4A H 1.0942 0.4148 0.2443 0.073 Uiso 1 1 calc R . . C5 C 1.094(5) 0.2484(14) 0.443(3) 0.115(9) Uiso 1 1 d D . . H5A H 1.0592 0.1935 0.3594 0.138 Uiso 1 1 calc R . . H5B H 1.2148 0.2724 0.4572 0.138 Uiso 1 1 calc R . . C6 C 1.123(3) 0.204(2) 0.597(3) 0.115(7) Uiso 1 1 d D . . H6A H 1.1923 0.2526 0.6876 0.139 Uiso 1 1 calc R . . H6B H 1.2036 0.1458 0.6136 0.139 Uiso 1 1 calc R . . C11 C 0.8323(18) 0.0922(9) 0.5425(15) 0.047(3) Uani 1 1 d . . . C12 C 0.7135(17) 0.0923(8) 0.6317(14) 0.044(3) Uani 1 1 d . . . C13 C 0.7718(15) 0.1706(9) 0.7525(13) 0.042(2) Uani 1 1 d . . . C14 C 0.929(2) 0.2240(11) 0.7488(19) 0.050(3) Uani 1 1 d . . . C15 C 0.9701(17) 0.1719(11) 0.6212(18) 0.054(3) Uani 1 1 d . . . C16 C 0.827(3) 0.0145(17) 0.417(3) 0.082(6) Uani 1 1 d . . . H16A H 0.8940 -0.0448 0.4776 0.124 Uiso 1 1 calc R . . H16B H 0.8826 0.0413 0.3475 0.124 Uiso 1 1 calc R . . H16C H 0.6995 -0.0037 0.3446 0.124 Uiso 1 1 calc R . . C17 C 0.560(2) 0.0198(16) 0.5900(19) 0.056(4) Uani 1 1 d . . . H17A H 0.4931 0.0361 0.6558 0.084 Uiso 1 1 calc R . . H17B H 0.6096 -0.0480 0.6179 0.084 Uiso 1 1 calc R . . H17C H 0.4775 0.0238 0.4692 0.084 Uiso 1 1 calc R . . C18 C 0.688(2) 0.1974(12) 0.8747(18) 0.064(4) Uani 1 1 d . . . H18A H 0.5808 0.1555 0.8497 0.096 Uiso 1 1 calc R . . H18B H 0.6517 0.2678 0.8603 0.096 Uiso 1 1 calc R . . H18C H 0.7787 0.1859 0.9915 0.096 Uiso 1 1 calc R . . C19 C 1.033(3) 0.3069(16) 0.871(2) 0.096(6) Uani 1 1 d . . . H19A H 1.1189 0.2777 0.9791 0.144 Uiso 1 1 calc R . . H19B H 0.9473 0.3504 0.8898 0.144 Uiso 1 1 calc R . . H19C H 1.1011 0.3461 0.8236 0.144 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 0.02209(17) 0.03396(17) 0.03548(18) -0.0011(5) 0.01465(12) 0.0002(5) Cl1 0.0421(19) 0.059(2) 0.062(2) 0.0073(17) -0.0037(16) -0.0145(16) C1 0.029(5) 0.047(6) 0.039(6) -0.004(4) 0.008(4) -0.009(4) N1 0.042(5) 0.058(6) 0.061(6) 0.007(5) 0.035(5) 0.001(4) Cl2 0.065(2) 0.0607(19) 0.081(2) -0.0011(17) 0.0441(18) 0.0254(16) N2 0.045(6) 0.052(6) 0.058(6) 0.015(5) 0.018(5) -0.001(5) C2 0.059(10) 0.088(11) 0.092(12) 0.047(10) 0.015(9) 0.003(8) C3 0.082(11) 0.068(8) 0.062(8) 0.004(7) 0.039(8) -0.030(8) C4 0.069(10) 0.068(8) 0.061(8) 0.001(6) 0.044(7) -0.017(7) C11 0.057(8) 0.044(6) 0.054(7) 0.009(5) 0.037(6) 0.017(5) C12 0.047(7) 0.039(5) 0.044(6) 0.013(4) 0.018(5) 0.010(5) C13 0.035(6) 0.058(6) 0.034(6) 0.006(5) 0.016(5) 0.008(5) C14 0.028(7) 0.059(8) 0.053(8) 0.012(6) 0.009(6) 0.009(6) C15 0.030(6) 0.083(9) 0.055(8) 0.023(7) 0.025(6) 0.024(6) C16 0.141(18) 0.048(10) 0.095(13) 0.001(9) 0.086(13) 0.014(11) C17 0.067(9) 0.052(9) 0.057(9) 0.008(7) 0.036(7) -0.003(7) C18 0.071(10) 0.083(10) 0.045(7) -0.004(6) 0.032(7) -0.001(8) C19 0.085(14) 0.121(15) 0.050(8) -0.006(9) 0.001(8) -0.046(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 2.041(12) . ? Ir1 C15 2.089(11) . ? Ir1 C14 2.133(13) . ? Ir1 C11 2.137(11) . ? Ir1 C13 2.242(11) . ? Ir1 C12 2.261(10) . ? Ir1 Cl2 2.404(3) . ? Ir1 Cl1 2.406(4) . ? C1 N2 1.329(14) . ? C1 N1 1.376(14) . ? N1 C4 1.369(15) . ? N1 C5 1.40(3) . ? N2 C3 1.379(16) . ? N2 C2 1.485(19) . ? C3 C4 1.31(2) . ? C5 C6 1.371(18) . ? C6 C15 1.40(3) . ? C11 C15 1.453(19) . ? C11 C12 1.461(17) . ? C11 C16 1.47(2) . ? C12 C13 1.391(16) . ? C12 C17 1.47(2) . ? C13 C14 1.450(19) . ? C13 C18 1.517(17) . ? C14 C15 1.45(2) . ? C14 C19 1.49(2) . ? 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 C1 Ir1 C15 92.7(5) . . ? C1 Ir1 C14 111.0(5) . . ? C15 Ir1 C14 40.2(5) . . ? C1 Ir1 C11 112.5(5) . . ? C15 Ir1 C11 40.2(5) . . ? C14 Ir1 C11 67.0(5) . . ? C1 Ir1 C13 149.5(4) . . ? C15 Ir1 C13 64.6(4) . . ? C14 Ir1 C13 38.6(5) . . ? C11 Ir1 C13 63.7(4) . . ? C1 Ir1 C12 151.2(5) . . ? C15 Ir1 C12 64.9(5) . . ? C14 Ir1 C12 64.1(5) . . ? C11 Ir1 C12 38.7(4) . . ? C13 Ir1 C12 36.0(4) . . ? C1 Ir1 Cl2 89.2(3) . . ? C15 Ir1 Cl2 134.6(5) . . ? C14 Ir1 Cl2 97.5(5) . . ? C11 Ir1 Cl2 156.5(4) . . ? C13 Ir1 Cl2 93.0(3) . . ? C12 Ir1 Cl2 119.3(4) . . ? C1 Ir1 Cl1 92.3(3) . . ? C15 Ir1 Cl1 133.4(5) . . ? C14 Ir1 Cl1 155.0(4) . . ? C11 Ir1 Cl1 96.1(4) . . ? C13 Ir1 Cl1 118.0(3) . . ? C12 Ir1 Cl1 91.1(3) . . ? Cl2 Ir1 Cl1 91.82(16) . . ? N2 C1 N1 104.9(10) . . ? N2 C1 Ir1 132.5(9) . . ? N1 C1 Ir1 122.5(8) . . ? C4 N1 C1 109.6(11) . . ? C4 N1 C5 125.7(16) . . ? C1 N1 C5 122.6(16) . . ? C1 N2 C3 110.1(12) . . ? C1 N2 C2 127.8(11) . . ? C3 N2 C2 122.1(12) . . ? C4 C3 N2 108.2(12) . . ? C3 C4 N1 107.3(12) . . ? C6 C5 N1 125(3) . . ? C5 C6 C15 119(2) . . ? C15 C11 C12 106.7(10) . . ? C15 C11 C16 127.9(13) . . ? C12 C11 C16 124.7(13) . . ? C15 C11 Ir1 68.1(6) . . ? C12 C11 Ir1 75.2(6) . . ? C16 C11 Ir1 128.9(11) . . ? C13 C12 C11 108.3(11) . . ? C13 C12 C17 129.2(12) . . ? C11 C12 C17 122.4(12) . . ? C13 C12 Ir1 71.3(6) . . ? C11 C12 Ir1 66.1(6) . . ? C17 C12 Ir1 127.4(9) . . ? C12 C13 C14 110.4(11) . . ? C12 C13 C18 126.0(12) . . ? C14 C13 C18 123.6(12) . . ? C12 C13 Ir1 72.7(6) . . ? C14 C13 Ir1 66.6(7) . . ? C18 C13 Ir1 128.1(9) . . ? C13 C14 C15 106.0(12) . . ? C13 C14 C19 123.9(15) . . ? C15 C14 C19 129.7(16) . . ? C13 C14 Ir1 74.8(7) . . ? C15 C14 Ir1 68.3(7) . . ? C19 C14 Ir1 127.4(12) . . ? C6 C15 C14 118.5(17) . . ? C6 C15 C11 133.1(17) . . ? C14 C15 C11 108.4(11) . . ? C6 C15 Ir1 122.3(12) . . ? C14 C15 Ir1 71.5(7) . . ? C11 C15 Ir1 71.7(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C15 Ir1 C1 N2 -179.1(12) . . . . ? C14 Ir1 C1 N2 -142.3(11) . . . . ? C11 Ir1 C1 N2 144.8(11) . . . . ? C13 Ir1 C1 N2 -139.2(11) . . . . ? C12 Ir1 C1 N2 143.6(11) . . . . ? Cl2 Ir1 C1 N2 -44.5(11) . . . . ? Cl1 Ir1 C1 N2 47.3(11) . . . . ? C15 Ir1 C1 N1 -3.4(10) . . . . ? C14 Ir1 C1 N1 33.4(11) . . . . ? C11 Ir1 C1 N1 -39.5(10) . . . . ? C13 Ir1 C1 N1 36.5(15) . . . . ? C12 Ir1 C1 N1 -40.7(14) . . . . ? Cl2 Ir1 C1 N1 131.1(9) . . . . ? Cl1 Ir1 C1 N1 -137.1(9) . . . . ? N2 C1 N1 C4 1.2(13) . . . . ? Ir1 C1 N1 C4 -175.5(9) . . . . ? N2 C1 N1 C5 -163.1(15) . . . . ? Ir1 C1 N1 C5 20.2(18) . . . . ? N1 C1 N2 C3 -0.2(14) . . . . ? Ir1 C1 N2 C3 176.0(9) . . . . ? N1 C1 N2 C2 177.3(14) . . . . ? Ir1 C1 N2 C2 -6(2) . . . . ? C1 N2 C3 C4 -1.0(16) . . . . ? C2 N2 C3 C4 -178.6(14) . . . . ? N2 C3 C4 N1 1.7(16) . . . . ? C1 N1 C4 C3 -1.9(15) . . . . ? C5 N1 C4 C3 161.9(17) . . . . ? C4 N1 C5 C6 152(2) . . . . ? C1 N1 C5 C6 -46(3) . . . . ? N1 C5 C6 C15 50(4) . . . . ? C1 Ir1 C11 C15 65.7(8) . . . . ? C14 Ir1 C11 C15 -38.5(7) . . . . ? C13 Ir1 C11 C15 -81.0(7) . . . . ? C12 Ir1 C11 C15 -115.2(10) . . . . ? Cl2 Ir1 C11 C15 -90.3(11) . . . . ? Cl1 Ir1 C11 C15 160.7(7) . . . . ? C1 Ir1 C11 C12 -179.1(6) . . . . ? C15 Ir1 C11 C12 115.2(10) . . . . ? C14 Ir1 C11 C12 76.8(8) . . . . ? C13 Ir1 C11 C12 34.2(6) . . . . ? Cl2 Ir1 C11 C12 24.9(14) . . . . ? Cl1 Ir1 C11 C12 -84.1(7) . . . . ? C1 Ir1 C11 C16 -56.1(15) . . . . ? C15 Ir1 C11 C16 -121.8(17) . . . . ? C14 Ir1 C11 C16 -160.3(16) . . . . ? C13 Ir1 C11 C16 157.2(16) . . . . ? C12 Ir1 C11 C16 123.0(18) . . . . ? Cl2 Ir1 C11 C16 147.9(12) . . . . ? Cl1 Ir1 C11 C16 38.9(15) . . . . ? C15 C11 C12 C13 2.3(12) . . . . ? C16 C11 C12 C13 173.8(13) . . . . ? Ir1 C11 C12 C13 -58.9(8) . . . . ? C15 C11 C12 C17 -178.4(12) . . . . ? C16 C11 C12 C17 -7(2) . . . . ? Ir1 C11 C12 C17 120.4(12) . . . . ? C15 C11 C12 Ir1 61.2(7) . . . . ? C16 C11 C12 Ir1 -127.4(14) . . . . ? C1 Ir1 C12 C13 122.7(9) . . . . ? C15 Ir1 C12 C13 80.8(8) . . . . ? C14 Ir1 C12 C13 36.0(8) . . . . ? C11 Ir1 C12 C13 120.9(10) . . . . ? Cl2 Ir1 C12 C13 -48.0(8) . . . . ? Cl1 Ir1 C12 C13 -140.7(7) . . . . ? C1 Ir1 C12 C11 1.8(12) . . . . ? C15 Ir1 C12 C11 -40.2(8) . . . . ? C14 Ir1 C12 C11 -84.9(8) . . . . ? C13 Ir1 C12 C11 -120.9(10) . . . . ? Cl2 Ir1 C12 C11 -168.9(6) . . . . ? Cl1 Ir1 C12 C11 98.4(7) . . . . ? C1 Ir1 C12 C17 -111.8(13) . . . . ? C15 Ir1 C12 C17 -153.7(14) . . . . ? C14 Ir1 C12 C17 161.5(14) . . . . ? C11 Ir1 C12 C17 -113.5(14) . . . . ? C13 Ir1 C12 C17 125.6(15) . . . . ? Cl2 Ir1 C12 C17 77.6(12) . . . . ? Cl1 Ir1 C12 C17 -15.1(12) . . . . ? C11 C12 C13 C14 -0.3(13) . . . . ? C17 C12 C13 C14 -179.5(13) . . . . ? Ir1 C12 C13 C14 -56.0(8) . . . . ? C11 C12 C13 C18 -179.4(11) . . . . ? C17 C12 C13 C18 1(2) . . . . ? Ir1 C12 C13 C18 124.9(12) . . . . ? C11 C12 C13 Ir1 55.7(7) . . . . ? C17 C12 C13 Ir1 -123.4(13) . . . . ? C1 Ir1 C13 C12 -126.9(10) . . . . ? C15 Ir1 C13 C12 -81.6(8) . . . . ? C14 Ir1 C13 C12 -122.1(11) . . . . ? C11 Ir1 C13 C12 -36.7(7) . . . . ? Cl2 Ir1 C13 C12 139.6(7) . . . . ? Cl1 Ir1 C13 C12 45.9(8) . . . . ? C1 Ir1 C13 C14 -4.7(13) . . . . ? C15 Ir1 C13 C14 40.5(8) . . . . ? C11 Ir1 C13 C14 85.4(9) . . . . ? C12 Ir1 C13 C14 122.1(11) . . . . ? Cl2 Ir1 C13 C14 -98.3(8) . . . . ? Cl1 Ir1 C13 C14 168.0(7) . . . . ? C1 Ir1 C13 C18 110.6(13) . . . . ? C15 Ir1 C13 C18 155.8(13) . . . . ? C14 Ir1 C13 C18 115.3(15) . . . . ? C11 Ir1 C13 C18 -159.3(13) . . . . ? C12 Ir1 C13 C18 -122.5(14) . . . . ? Cl2 Ir1 C13 C18 17.0(11) . . . . ? Cl1 Ir1 C13 C18 -76.7(12) . . . . ? C12 C13 C14 C15 -1.8(13) . . . . ? C18 C13 C14 C15 177.3(11) . . . . ? Ir1 C13 C14 C15 -61.5(8) . . . . ? C12 C13 C14 C19 -175.3(14) . . . . ? C18 C13 C14 C19 4(2) . . . . ? Ir1 C13 C14 C19 125.1(16) . . . . ? C12 C13 C14 Ir1 59.6(8) . . . . ? C18 C13 C14 Ir1 -121.3(11) . . . . ? C1 Ir1 C14 C13 177.4(7) . . . . ? C15 Ir1 C14 C13 -114.6(11) . . . . ? C11 Ir1 C14 C13 -76.2(8) . . . . ? C12 Ir1 C14 C13 -33.6(7) . . . . ? Cl2 Ir1 C14 C13 85.4(7) . . . . ? Cl1 Ir1 C14 C13 -25.7(16) . . . . ? C1 Ir1 C14 C15 -67.9(9) . . . . ? C11 Ir1 C14 C15 38.5(8) . . . . ? C13 Ir1 C14 C15 114.6(11) . . . . ? C12 Ir1 C14 C15 81.0(9) . . . . ? Cl2 Ir1 C14 C15 -160.0(8) . . . . ? Cl1 Ir1 C14 C15 88.9(13) . . . . ? C1 Ir1 C14 C19 56.2(18) . . . . ? C15 Ir1 C14 C19 124(2) . . . . ? C11 Ir1 C14 C19 162.6(18) . . . . ? C13 Ir1 C14 C19 -121(2) . . . . ? C12 Ir1 C14 C19 -154.9(18) . . . . ? Cl2 Ir1 C14 C19 -35.9(17) . . . . ? Cl1 Ir1 C14 C19 -147.0(13) . . . . ? C5 C6 C15 C14 -113(2) . . . . ? C5 C6 C15 C11 67(3) . . . . ? C5 C6 C15 Ir1 -28(3) . . . . ? C13 C14 C15 C6 -176.7(14) . . . . ? C19 C14 C15 C6 -4(2) . . . . ? Ir1 C14 C15 C6 117.4(15) . . . . ? C13 C14 C15 C11 3.3(13) . . . . ? C19 C14 C15 C11 176.2(15) . . . . ? Ir1 C14 C15 C11 -62.6(8) . . . . ? C13 C14 C15 Ir1 65.9(8) . . . . ? C19 C14 C15 Ir1 -121.2(17) . . . . ? C12 C11 C15 C6 176.5(17) . . . . ? C16 C11 C15 C6 5(3) . . . . ? Ir1 C11 C15 C6 -117.5(18) . . . . ? C12 C11 C15 C14 -3.5(13) . . . . ? C16 C11 C15 C14 -174.6(14) . . . . ? Ir1 C11 C15 C14 62.5(8) . . . . ? C12 C11 C15 Ir1 -66.0(7) . . . . ? C16 C11 C15 Ir1 123.0(15) . . . . ? C1 Ir1 C15 C6 7.4(17) . . . . ? C14 Ir1 C15 C6 -113(2) . . . . ? C11 Ir1 C15 C6 130(2) . . . . ? C13 Ir1 C15 C6 -151.5(19) . . . . ? C12 Ir1 C15 C6 168.6(19) . . . . ? Cl2 Ir1 C15 C6 -84.2(17) . . . . ? Cl1 Ir1 C15 C6 103.0(17) . . . . ? C1 Ir1 C15 C14 120.0(8) . . . . ? C11 Ir1 C15 C14 -117.5(11) . . . . ? C13 Ir1 C15 C14 -38.9(8) . . . . ? C12 Ir1 C15 C14 -78.9(8) . . . . ? Cl2 Ir1 C15 C14 28.4(10) . . . . ? Cl1 Ir1 C15 C14 -144.4(7) . . . . ? C1 Ir1 C15 C11 -122.5(7) . . . . ? C14 Ir1 C15 C11 117.5(11) . . . . ? C13 Ir1 C15 C11 78.6(7) . . . . ? C12 Ir1 C15 C11 38.6(7) . . . . ? Cl2 Ir1 C15 C11 145.9(6) . . . . ? Cl1 Ir1 C15 C11 -26.9(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.107 _refine_diff_density_min -1.129 _refine_diff_density_rms 0.157 # Attachment 'Compound6.txt' data_str1011m/Compound6 _database_code_depnum_ccdc_archive 'CCDC 717568' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H25 Cl2 N2 O2 Rh, 2(H2 O1)' _chemical_formula_sum 'C15 H21 Cl2 N2 O2 Rh' _chemical_formula_weight 439.15 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' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.1280(10) _cell_length_b 10.8995(12) _cell_length_c 18.2374(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1814.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(8) _cell_measurement_reflns_used 3173 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 25.43 _exptl_crystal_description prismatic _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.593 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 1.242 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.6384 _exptl_absorpt_correction_T_max 0.7772 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(8) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9499 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0735 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.37 _reflns_number_total 3706 _reflns_number_gt 3075 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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. PLAT306 ALERT 2 A Isolated Oxygen Atom (H-atoms Missing ?) ....... O1 No hydrogen atoms are found at geometrically idealized position PLAT306 ALERT 2 A Isolated Oxygen Atom (H-atoms Missing ?) ....... O2 No hydrogen atoms are found at geometrically idealized position ; _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^)+(0.0324P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(5) _refine_ls_number_reflns 3706 _refine_ls_number_parameters 204 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.0859 _refine_ls_wR_factor_gt 0.0786 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.65439(4) 0.29416(3) 0.84530(2) 0.02570(11) Uani 1 1 d . . . Cl1 Cl 0.86777(17) 0.42400(13) 0.86310(9) 0.0464(4) Uani 1 1 d . . . C1 C 0.7876(5) 0.1449(4) 0.8409(3) 0.0266(10) Uani 1 1 d . . . N1 N 0.9055(5) 0.1208(4) 0.7974(2) 0.0323(11) Uani 1 1 d . . . O1 O 0.9315(5) 0.6832(4) 0.9484(2) 0.0565(12) Uani 1 1 d . . . Cl2 Cl 0.6448(2) 0.32435(13) 0.71245(7) 0.0500(4) Uani 1 1 d . . . C2 C 0.9642(6) 0.1939(6) 0.7394(3) 0.0456(14) Uani 1 1 d . . . H2A H 0.8869 0.2170 0.7065 0.068 Uiso 1 1 calc R . . H2B H 1.0366 0.1475 0.7132 0.068 Uiso 1 1 calc R . . H2C H 1.0085 0.2663 0.7596 0.068 Uiso 1 1 calc R . . N2 N 0.7776(5) 0.0437(4) 0.8845(3) 0.0349(11) Uani 1 1 d . . . O2 O 0.7719(6) 0.2533(5) 0.5543(2) 0.0768(16) Uani 1 1 d . . . C3 C 0.9647(6) 0.0076(5) 0.8132(3) 0.0373(13) Uani 1 1 d . . . H3A H 1.0443 -0.0287 0.7899 0.045 Uiso 1 1 calc R . . C4 C 0.8877(6) -0.0400(5) 0.8675(3) 0.0396(15) Uani 1 1 d . . . H4A H 0.9039 -0.1153 0.8901 0.048 Uiso 1 1 calc R . . C5 C 0.6814(7) 0.0294(6) 0.9492(4) 0.0541(18) Uani 1 1 d . . . H5A H 0.7212 0.0774 0.9893 0.065 Uiso 1 1 calc R . . H5B H 0.6821 -0.0560 0.9642 0.065 Uiso 1 1 calc R . . C6 C 0.5249(7) 0.0685(5) 0.9361(4) 0.0470(17) Uani 1 1 d . . . H6A H 0.4836 0.0174 0.8978 0.056 Uiso 1 1 calc R . . H6B H 0.4689 0.0538 0.9805 0.056 Uiso 1 1 calc R . . C11 C 0.4291(6) 0.3753(5) 0.8535(3) 0.0349(13) Uani 1 1 d . . . C12 C 0.5091(6) 0.4138(5) 0.9131(3) 0.0346(14) Uani 1 1 d . . . C13 C 0.5619(6) 0.3069(6) 0.9516(3) 0.0379(13) Uani 1 1 d . . . C14 C 0.5071(5) 0.2007(6) 0.9145(3) 0.0331(12) Uani 1 1 d . . . C15 C 0.4300(5) 0.2421(5) 0.8510(3) 0.0368(13) Uani 1 1 d . . . C16 C 0.3471(8) 0.1663(6) 0.7974(4) 0.0600(18) Uani 1 1 d . . . H16A H 0.4055 0.0972 0.7830 0.090 Uiso 1 1 calc R . . H16B H 0.3242 0.2149 0.7550 0.090 Uiso 1 1 calc R . . H16C H 0.2580 0.1379 0.8196 0.090 Uiso 1 1 calc R . . C17 C 0.3484(8) 0.4537(5) 0.7991(3) 0.0546(16) Uani 1 1 d . . . H17A H 0.3813 0.5371 0.8032 0.082 Uiso 1 1 calc R . . H17B H 0.2452 0.4499 0.8089 0.082 Uiso 1 1 calc R . . H17C H 0.3672 0.4243 0.7504 0.082 Uiso 1 1 calc R . . C18 C 0.5374(8) 0.5429(5) 0.9338(4) 0.0516(17) Uani 1 1 d . . . H18A H 0.5717 0.5874 0.8918 0.077 Uiso 1 1 calc R . . H18B H 0.6103 0.5456 0.9717 0.077 Uiso 1 1 calc R . . H18C H 0.4484 0.5795 0.9514 0.077 Uiso 1 1 calc R . . C19 C 0.6351(7) 0.3100(7) 1.0255(3) 0.0597(18) Uani 1 1 d . . . H19A H 0.5864 0.2540 1.0580 0.089 Uiso 1 1 calc R . . H19B H 0.6297 0.3916 1.0452 0.089 Uiso 1 1 calc R . . H19C H 0.7359 0.2865 1.0204 0.089 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 0.02788(17) 0.02334(17) 0.02588(18) 0.00202(17) 0.00172(18) 0.0009(2) Cl1 0.0447(9) 0.0405(8) 0.0540(10) -0.0126(6) 0.0117(7) -0.0161(7) C1 0.026(2) 0.027(3) 0.027(3) -0.001(2) -0.006(2) -0.003(2) N1 0.035(2) 0.030(2) 0.032(3) -0.004(2) -0.002(2) 0.006(2) O1 0.067(3) 0.045(3) 0.057(3) -0.004(2) 0.012(2) -0.006(2) Cl2 0.0657(9) 0.0542(9) 0.0302(7) 0.0072(6) 0.0042(8) 0.0193(9) C2 0.045(3) 0.048(4) 0.043(3) 0.006(3) 0.011(3) 0.007(4) N2 0.036(3) 0.029(3) 0.040(3) 0.008(2) 0.003(2) 0.004(2) O2 0.076(3) 0.116(4) 0.038(3) 0.006(3) -0.002(2) 0.008(3) C3 0.035(3) 0.032(3) 0.045(3) -0.010(3) -0.006(3) 0.008(3) C4 0.041(4) 0.033(3) 0.045(4) 0.009(3) -0.004(3) 0.010(3) C5 0.057(5) 0.043(4) 0.062(4) 0.026(3) 0.016(3) 0.006(3) C6 0.045(4) 0.039(4) 0.057(4) 0.015(3) 0.017(3) -0.002(3) C11 0.030(3) 0.030(3) 0.045(4) 0.005(3) 0.008(3) 0.007(2) C12 0.030(3) 0.038(3) 0.036(3) -0.007(3) 0.002(2) 0.008(3) C13 0.034(3) 0.048(4) 0.032(3) 0.004(3) 0.003(2) 0.002(3) C14 0.029(3) 0.033(3) 0.037(3) 0.005(3) 0.008(2) 0.000(3) C15 0.024(2) 0.044(3) 0.043(3) 0.002(3) -0.001(3) -0.002(2) C16 0.055(4) 0.059(4) 0.066(4) -0.004(3) -0.022(4) -0.018(4) C17 0.049(4) 0.053(4) 0.061(4) 0.014(3) -0.003(4) 0.015(4) C18 0.048(4) 0.048(4) 0.059(4) -0.016(3) 0.002(3) 0.003(3) C19 0.057(4) 0.092(5) 0.029(3) -0.008(3) -0.006(3) 0.006(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 C1 2.033(5) . ? Rh1 C14 2.106(5) . ? Rh1 C13 2.119(5) . ? Rh1 C15 2.127(5) . ? Rh1 C12 2.233(5) . ? Rh1 C11 2.244(5) . ? Rh1 Cl1 2.4294(15) . ? Rh1 Cl2 2.4467(13) . ? C1 N2 1.363(6) . ? C1 N1 1.363(6) . ? N1 C3 1.377(7) . ? N1 C2 1.428(7) . ? N2 C4 1.392(7) . ? N2 C5 1.480(7) . ? C3 C4 1.320(8) . ? C5 C6 1.510(9) . ? C6 C14 1.503(8) . ? C11 C12 1.375(8) . ? C11 C15 1.453(7) . ? C11 C17 1.502(8) . ? C12 C13 1.443(8) . ? C12 C18 1.481(8) . ? C13 C14 1.431(8) . ? C13 C19 1.504(8) . ? C14 C15 1.428(8) . ? C15 C16 1.487(8) . ? 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 C1 Rh1 C14 91.0(2) . . ? C1 Rh1 C13 109.1(2) . . ? C14 Rh1 C13 39.6(2) . . ? C1 Rh1 C15 111.37(19) . . ? C14 Rh1 C15 39.4(2) . . ? C13 Rh1 C15 65.7(2) . . ? C1 Rh1 C12 147.6(2) . . ? C14 Rh1 C12 64.6(2) . . ? C13 Rh1 C12 38.6(2) . . ? C15 Rh1 C12 63.7(2) . . ? C1 Rh1 C11 150.06(19) . . ? C14 Rh1 C11 64.3(2) . . ? C13 Rh1 C11 63.1(2) . . ? C15 Rh1 C11 38.70(19) . . ? C12 Rh1 C11 35.8(2) . . ? C1 Rh1 Cl1 89.53(14) . . ? C14 Rh1 Cl1 135.51(15) . . ? C13 Rh1 Cl1 99.15(16) . . ? C15 Rh1 Cl1 157.00(15) . . ? C12 Rh1 Cl1 93.57(15) . . ? C11 Rh1 Cl1 119.75(15) . . ? C1 Rh1 Cl2 95.18(16) . . ? C14 Rh1 Cl2 129.46(15) . . ? C13 Rh1 Cl2 152.00(15) . . ? C15 Rh1 Cl2 92.87(17) . . ? C12 Rh1 Cl2 116.64(15) . . ? C11 Rh1 Cl2 88.85(16) . . ? Cl1 Rh1 Cl2 94.73(6) . . ? N2 C1 N1 103.7(4) . . ? N2 C1 Rh1 125.8(4) . . ? N1 C1 Rh1 130.5(4) . . ? C1 N1 C3 111.1(5) . . ? C1 N1 C2 128.3(5) . . ? C3 N1 C2 120.5(5) . . ? C1 N2 C4 110.6(4) . . ? C1 N2 C5 126.2(5) . . ? C4 N2 C5 122.6(5) . . ? C4 C3 N1 107.4(5) . . ? C3 C4 N2 107.1(5) . . ? N2 C5 C6 114.0(5) . . ? C14 C6 C5 114.5(5) . . ? C12 C11 C15 109.0(5) . . ? C12 C11 C17 127.5(5) . . ? C15 C11 C17 123.4(6) . . ? C12 C11 Rh1 71.7(3) . . ? C15 C11 Rh1 66.3(3) . . ? C17 C11 Rh1 129.0(4) . . ? C11 C12 C13 108.5(5) . . ? C11 C12 C18 125.8(5) . . ? C13 C12 C18 125.8(5) . . ? C11 C12 Rh1 72.5(3) . . ? C13 C12 Rh1 66.4(3) . . ? C18 C12 Rh1 126.4(4) . . ? C14 C13 C12 107.8(5) . . ? C14 C13 C19 126.6(6) . . ? C12 C13 C19 124.5(6) . . ? C14 C13 Rh1 69.7(3) . . ? C12 C13 Rh1 75.0(3) . . ? C19 C13 Rh1 130.1(4) . . ? C15 C14 C13 107.4(5) . . ? C15 C14 C6 124.7(6) . . ? C13 C14 C6 127.9(5) . . ? C15 C14 Rh1 71.1(3) . . ? C13 C14 Rh1 70.7(3) . . ? C6 C14 Rh1 123.5(4) . . ? C14 C15 C11 107.1(6) . . ? C14 C15 C16 127.4(5) . . ? C11 C15 C16 124.9(6) . . ? C14 C15 Rh1 69.5(3) . . ? C11 C15 Rh1 75.0(3) . . ? C16 C15 Rh1 127.3(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 C14 Rh1 C1 N2 -11.6(5) . . . . ? C13 Rh1 C1 N2 24.4(5) . . . . ? C15 Rh1 C1 N2 -46.3(5) . . . . ? C12 Rh1 C1 N2 28.0(7) . . . . ? C11 Rh1 C1 N2 -44.7(7) . . . . ? Cl1 Rh1 C1 N2 123.9(4) . . . . ? Cl2 Rh1 C1 N2 -141.4(4) . . . . ? C14 Rh1 C1 N1 169.6(5) . . . . ? C13 Rh1 C1 N1 -154.4(4) . . . . ? C15 Rh1 C1 N1 135.0(4) . . . . ? C12 Rh1 C1 N1 -150.8(4) . . . . ? C11 Rh1 C1 N1 136.5(5) . . . . ? Cl1 Rh1 C1 N1 -54.9(4) . . . . ? Cl2 Rh1 C1 N1 39.8(5) . . . . ? N2 C1 N1 C3 0.8(6) . . . . ? Rh1 C1 N1 C3 179.7(4) . . . . ? N2 C1 N1 C2 177.9(5) . . . . ? Rh1 C1 N1 C2 -3.2(8) . . . . ? N1 C1 N2 C4 0.0(6) . . . . ? Rh1 C1 N2 C4 -179.0(4) . . . . ? N1 C1 N2 C5 170.6(5) . . . . ? Rh1 C1 N2 C5 -8.5(8) . . . . ? C1 N1 C3 C4 -1.3(6) . . . . ? C2 N1 C3 C4 -178.6(5) . . . . ? N1 C3 C4 N2 1.2(6) . . . . ? C1 N2 C4 C3 -0.8(6) . . . . ? C5 N2 C4 C3 -171.7(6) . . . . ? C1 N2 C5 C6 47.6(8) . . . . ? C4 N2 C5 C6 -142.8(6) . . . . ? N2 C5 C6 C14 -60.1(8) . . . . ? C1 Rh1 C11 C12 118.9(5) . . . . ? C14 Rh1 C11 C12 81.7(4) . . . . ? C13 Rh1 C11 C12 37.3(3) . . . . ? C15 Rh1 C11 C12 121.3(5) . . . . ? Cl1 Rh1 C11 C12 -47.9(4) . . . . ? Cl2 Rh1 C11 C12 -142.7(3) . . . . ? C1 Rh1 C11 C15 -2.4(7) . . . . ? C14 Rh1 C11 C15 -39.6(4) . . . . ? C13 Rh1 C11 C15 -84.0(4) . . . . ? C12 Rh1 C11 C15 -121.3(5) . . . . ? Cl1 Rh1 C11 C15 -169.2(3) . . . . ? Cl2 Rh1 C11 C15 96.0(4) . . . . ? C1 Rh1 C11 C17 -117.2(6) . . . . ? C14 Rh1 C11 C17 -154.4(6) . . . . ? C13 Rh1 C11 C17 161.2(6) . . . . ? C15 Rh1 C11 C17 -114.8(7) . . . . ? C12 Rh1 C11 C17 123.9(7) . . . . ? Cl1 Rh1 C11 C17 76.0(6) . . . . ? Cl2 Rh1 C11 C17 -18.8(5) . . . . ? C15 C11 C12 C13 -1.0(6) . . . . ? C17 C11 C12 C13 177.6(6) . . . . ? Rh1 C11 C12 C13 -56.8(4) . . . . ? C15 C11 C12 C18 178.5(6) . . . . ? C17 C11 C12 C18 -2.9(9) . . . . ? Rh1 C11 C12 C18 122.7(6) . . . . ? C15 C11 C12 Rh1 55.8(4) . . . . ? C17 C11 C12 Rh1 -125.6(6) . . . . ? C1 Rh1 C12 C11 -125.4(4) . . . . ? C14 Rh1 C12 C11 -80.6(4) . . . . ? C13 Rh1 C12 C11 -120.0(5) . . . . ? C15 Rh1 C12 C11 -36.6(3) . . . . ? Cl1 Rh1 C12 C11 139.8(3) . . . . ? Cl2 Rh1 C12 C11 42.7(4) . . . . ? C1 Rh1 C12 C13 -5.4(5) . . . . ? C14 Rh1 C12 C13 39.4(3) . . . . ? C15 Rh1 C12 C13 83.4(4) . . . . ? C11 Rh1 C12 C13 120.0(5) . . . . ? Cl1 Rh1 C12 C13 -100.2(3) . . . . ? Cl2 Rh1 C12 C13 162.7(3) . . . . ? C1 Rh1 C12 C18 112.6(6) . . . . ? C14 Rh1 C12 C18 157.5(6) . . . . ? C13 Rh1 C12 C18 118.1(7) . . . . ? C15 Rh1 C12 C18 -158.5(6) . . . . ? C11 Rh1 C12 C18 -122.0(7) . . . . ? Cl1 Rh1 C12 C18 17.9(5) . . . . ? Cl2 Rh1 C12 C18 -79.2(5) . . . . ? C11 C12 C13 C14 -1.8(6) . . . . ? C18 C12 C13 C14 178.7(6) . . . . ? Rh1 C12 C13 C14 -62.4(3) . . . . ? C11 C12 C13 C19 -170.7(5) . . . . ? C18 C12 C13 C19 9.8(9) . . . . ? Rh1 C12 C13 C19 128.6(6) . . . . ? C11 C12 C13 Rh1 60.6(4) . . . . ? C18 C12 C13 Rh1 -118.9(6) . . . . ? C1 Rh1 C13 C14 -67.2(3) . . . . ? C15 Rh1 C13 C14 38.3(3) . . . . ? C12 Rh1 C13 C14 115.9(4) . . . . ? C11 Rh1 C13 C14 81.3(3) . . . . ? Cl1 Rh1 C13 C14 -159.9(3) . . . . ? Cl2 Rh1 C13 C14 81.4(5) . . . . ? C1 Rh1 C13 C12 176.9(3) . . . . ? C14 Rh1 C13 C12 -115.9(4) . . . . ? C15 Rh1 C13 C12 -77.6(3) . . . . ? C11 Rh1 C13 C12 -34.6(3) . . . . ? Cl1 Rh1 C13 C12 84.2(3) . . . . ? Cl2 Rh1 C13 C12 -34.5(6) . . . . ? C1 Rh1 C13 C19 54.2(7) . . . . ? C14 Rh1 C13 C19 121.4(8) . . . . ? C15 Rh1 C13 C19 159.7(7) . . . . ? C12 Rh1 C13 C19 -122.7(8) . . . . ? C11 Rh1 C13 C19 -157.3(7) . . . . ? Cl1 Rh1 C13 C19 -38.5(6) . . . . ? Cl2 Rh1 C13 C19 -157.2(4) . . . . ? C12 C13 C14 C15 3.9(6) . . . . ? C19 C13 C14 C15 172.5(5) . . . . ? Rh1 C13 C14 C15 -61.9(3) . . . . ? C12 C13 C14 C6 -176.2(6) . . . . ? C19 C13 C14 C6 -7.6(9) . . . . ? Rh1 C13 C14 C6 117.9(5) . . . . ? C12 C13 C14 Rh1 65.9(4) . . . . ? C19 C13 C14 Rh1 -125.5(6) . . . . ? C5 C6 C14 C15 126.8(6) . . . . ? C5 C6 C14 C13 -53.0(8) . . . . ? C5 C6 C14 Rh1 37.6(8) . . . . ? C1 Rh1 C14 C15 -123.5(3) . . . . ? C13 Rh1 C14 C15 117.1(5) . . . . ? C12 Rh1 C14 C15 78.7(3) . . . . ? C11 Rh1 C14 C15 38.9(3) . . . . ? Cl1 Rh1 C14 C15 146.1(3) . . . . ? Cl2 Rh1 C14 C15 -25.9(4) . . . . ? C1 Rh1 C14 C13 119.4(3) . . . . ? C15 Rh1 C14 C13 -117.1(5) . . . . ? C12 Rh1 C14 C13 -38.4(3) . . . . ? C11 Rh1 C14 C13 -78.2(3) . . . . ? Cl1 Rh1 C14 C13 29.0(4) . . . . ? Cl2 Rh1 C14 C13 -143.0(3) . . . . ? C1 Rh1 C14 C6 -3.9(5) . . . . ? C13 Rh1 C14 C6 -123.3(6) . . . . ? C15 Rh1 C14 C6 119.6(7) . . . . ? C12 Rh1 C14 C6 -161.7(6) . . . . ? C11 Rh1 C14 C6 158.5(6) . . . . ? Cl1 Rh1 C14 C6 -94.3(5) . . . . ? Cl2 Rh1 C14 C6 93.7(5) . . . . ? C13 C14 C15 C11 -4.5(6) . . . . ? C6 C14 C15 C11 175.7(5) . . . . ? Rh1 C14 C15 C11 -66.1(4) . . . . ? C13 C14 C15 C16 -176.4(6) . . . . ? C6 C14 C15 C16 3.8(9) . . . . ? Rh1 C14 C15 C16 121.9(6) . . . . ? C13 C14 C15 Rh1 61.7(3) . . . . ? C6 C14 C15 Rh1 -118.2(5) . . . . ? C12 C11 C15 C14 3.4(7) . . . . ? C17 C11 C15 C14 -175.2(5) . . . . ? Rh1 C11 C15 C14 62.5(3) . . . . ? C12 C11 C15 C16 175.6(5) . . . . ? C17 C11 C15 C16 -3.0(10) . . . . ? Rh1 C11 C15 C16 -125.3(6) . . . . ? C12 C11 C15 Rh1 -59.1(4) . . . . ? C17 C11 C15 Rh1 122.3(6) . . . . ? C1 Rh1 C15 C14 63.6(4) . . . . ? C13 Rh1 C15 C14 -38.5(3) . . . . ? C12 Rh1 C15 C14 -81.3(4) . . . . ? C11 Rh1 C15 C14 -115.2(5) . . . . ? Cl1 Rh1 C15 C14 -90.5(5) . . . . ? Cl2 Rh1 C15 C14 160.3(3) . . . . ? C1 Rh1 C15 C11 178.7(4) . . . . ? C14 Rh1 C15 C11 115.2(5) . . . . ? C13 Rh1 C15 C11 76.7(4) . . . . ? C12 Rh1 C15 C11 33.8(4) . . . . ? Cl1 Rh1 C15 C11 24.6(7) . . . . ? Cl2 Rh1 C15 C11 -84.6(4) . . . . ? C1 Rh1 C15 C16 -58.5(6) . . . . ? C14 Rh1 C15 C16 -122.1(6) . . . . ? C13 Rh1 C15 C16 -160.6(6) . . . . ? C12 Rh1 C15 C16 156.6(6) . . . . ? C11 Rh1 C15 C16 122.8(7) . . . . ? Cl1 Rh1 C15 C16 147.4(4) . . . . ? Cl2 Rh1 C15 C16 38.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.414 _refine_diff_density_min -0.513 _refine_diff_density_rms 0.090 # Attachment 'Compound8.txt' data_str1012m/Compound8 _database_code_depnum_ccdc_archive 'CCDC 717569' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H29 Cl2 I2 N2 Rh' _chemical_formula_weight 761.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.702(10) _cell_length_b 12.165(12) _cell_length_c 12.351(12) _cell_angle_alpha 71.958(19) _cell_angle_beta 67.00(2) _cell_angle_gamma 73.90(2) _cell_volume 1255(2) _cell_formula_units_Z 2 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 971 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 30.61 _exptl_crystal_description prismatic _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.013 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_correction_type refdelf _exptl_absorpt_coefficient_mu 3.366 _exptl_absorpt_correction_T_min 0.3894 _exptl_absorpt_correction_T_max 0.5249 _exptl_absorpt_process_details ; Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56 Cubic fit to sin(theta)/lambda - 24 parameters ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8108 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0448 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 28.28 _reflns_number_total 5801 _reflns_number_gt 4596 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.1063P)^2^+3.6145P] 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 ? _refine_ls_extinction_coef ? _refine_ls_number_reflns 5801 _refine_ls_number_parameters 277 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1534 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 Rh Rh 0.75332(5) 0.23272(4) 0.62154(4) 0.03026(15) Uani 1 1 d . . . I1 I 0.51408(5) 0.32240(5) 0.79532(4) 0.04851(18) Uani 1 1 d . . . C1 C 0.7952(7) 0.0864(5) 0.7493(5) 0.0311(12) Uani 1 1 d . . . N1 N 0.7047(7) 0.0071(5) 0.8246(5) 0.0373(12) Uani 1 1 d . . . Cl1 Cl 0.5603(5) 0.7161(4) 0.7397(4) 0.1084(13) Uani 1 1 d . . . I2 I 0.59609(7) 0.14315(6) 0.53986(5) 0.05617(19) Uani 1 1 d . . . N2 N 0.9251(6) 0.0491(5) 0.7803(5) 0.0319(11) Uani 1 1 d . . . C2 C 0.5539(9) 0.0018(8) 0.8312(7) 0.0505(19) Uani 1 1 d . . . H2A H 0.5000 0.0801 0.8108 0.076 Uiso 1 1 calc R . . H2B H 0.4994 -0.0360 0.9118 0.076 Uiso 1 1 calc R . . H2C H 0.5627 -0.0421 0.7756 0.076 Uiso 1 1 calc R . . Cl2 Cl 0.7797(4) 0.6297(3) 0.8659(3) 0.0931(10) Uani 1 1 d . . . C3 C 0.7752(9) -0.0760(7) 0.9005(6) 0.0422(16) Uani 1 1 d . . . H3 H 0.7352 -0.1389 0.9594 0.051 Uiso 1 1 calc R . . C4 C 0.9104(9) -0.0501(7) 0.8744(6) 0.0420(16) Uani 1 1 d . . . H4 H 0.9821 -0.0909 0.9121 0.050 Uiso 1 1 calc R . . C5 C 1.0516(7) 0.1110(6) 0.7470(6) 0.0322(12) Uani 1 1 d . . . C6 C 1.0976(7) 0.1771(6) 0.6129(6) 0.0362(14) Uani 1 1 d . . . H6A H 1.1714 0.2237 0.6005 0.043 Uiso 1 1 calc R . . H6B H 1.1506 0.1184 0.5652 0.043 Uiso 1 1 calc R . . C7 C 1.1934(8) 0.0196(7) 0.7603(7) 0.0458(17) Uani 1 1 d . . . H7A H 1.1802 -0.0125 0.8445 0.069 Uiso 1 1 calc R . . H7B H 1.2813 0.0567 0.7225 0.069 Uiso 1 1 calc R . . H7C H 1.2070 -0.0423 0.7222 0.069 Uiso 1 1 calc R . . C11 C 0.8426(8) 0.3360(7) 0.4274(6) 0.0383(14) Uani 1 1 d . . . C12 C 0.7998(8) 0.4121(6) 0.5047(6) 0.0377(14) Uani 1 1 d . . . C13 C 0.8858(7) 0.3659(6) 0.5871(6) 0.0325(12) Uani 1 1 d . . . C14 C 0.9804(7) 0.2566(6) 0.5599(5) 0.0319(13) Uani 1 1 d . . . C15 C 0.9510(8) 0.2370(6) 0.4626(5) 0.0344(13) Uani 1 1 d . . . C16 C 1.0341(10) 0.1422(7) 0.3952(6) 0.0481(18) Uani 1 1 d . . . H16A H 1.1001 0.1748 0.3169 0.072 Uiso 1 1 calc R . . H16B H 0.9621 0.1082 0.3861 0.072 Uiso 1 1 calc R . . H16C H 1.0935 0.0826 0.4392 0.072 Uiso 1 1 calc R . . C17 C 0.7954(11) 0.3583(8) 0.3198(7) 0.053(2) Uani 1 1 d . . . H17A H 0.6895 0.3931 0.3388 0.080 Uiso 1 1 calc R . . H17B H 0.8116 0.2854 0.2980 0.080 Uiso 1 1 calc R . . H17C H 0.8547 0.4107 0.2534 0.080 Uiso 1 1 calc R . . C18 C 0.6933(10) 0.5264(7) 0.4970(7) 0.0481(18) Uani 1 1 d . . . H18A H 0.7501 0.5895 0.4636 0.072 Uiso 1 1 calc R . . H18B H 0.6238 0.5326 0.5763 0.072 Uiso 1 1 calc R . . H18C H 0.6374 0.5311 0.4460 0.072 Uiso 1 1 calc R . . C19 C 0.8871(9) 0.4339(7) 0.6664(7) 0.0433(16) Uani 1 1 d . . . H19A H 0.8030 0.4228 0.7404 0.065 Uiso 1 1 calc R . . H19B H 0.8785 0.5158 0.6268 0.065 Uiso 1 1 calc R . . H19C H 0.9807 0.4076 0.6838 0.065 Uiso 1 1 calc R . . C20 C 0.6070(16) 0.6283(15) 0.8696(11) 0.096(4) Uani 1 1 d . . . H20A H 0.5325 0.6553 0.9400 0.115 Uiso 1 1 calc R . . H20B H 0.5989 0.5479 0.8793 0.115 Uiso 1 1 calc R . . C21 C 1.0098(8) 0.1921(6) 0.8326(6) 0.0369(14) Uani 1 1 d . . . C22 C 0.8653(8) 0.2089(7) 0.9182(6) 0.0421(16) Uani 1 1 d . . . H22 H 0.7911 0.1704 0.9244 0.050 Uiso 1 1 calc R . . C23 C 0.8324(10) 0.2827(8) 0.9937(7) 0.0512(19) Uani 1 1 d . . . H23 H 0.7359 0.2933 1.0509 0.061 Uiso 1 1 calc R . . C24 C 0.9397(12) 0.3404(8) 0.9854(8) 0.057(2) Uani 1 1 d . . . H24 H 0.9162 0.3909 1.0358 0.068 Uiso 1 1 calc R . . C25 C 1.0838(11) 0.3229(8) 0.9012(7) 0.0506(19) Uani 1 1 d . . . H25 H 1.1576 0.3616 0.8953 0.061 Uiso 1 1 calc R . . C26 C 1.1182(9) 0.2495(7) 0.8267(7) 0.0441(16) Uani 1 1 d . . . H26 H 1.2159 0.2378 0.7713 0.053 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 Rh 0.0276(3) 0.0359(3) 0.0232(2) -0.00573(18) -0.00881(18) -0.00001(19) I1 0.0335(3) 0.0591(3) 0.0425(3) -0.0181(2) -0.0041(2) 0.0024(2) C1 0.033(3) 0.030(3) 0.024(3) -0.004(2) -0.006(2) -0.004(2) N1 0.034(3) 0.044(3) 0.029(3) -0.005(2) -0.009(2) -0.003(2) Cl1 0.110(3) 0.128(3) 0.095(2) -0.045(2) -0.047(2) 0.010(2) I2 0.0572(4) 0.0759(4) 0.0450(3) -0.0112(3) -0.0235(2) -0.0198(3) N2 0.033(3) 0.034(3) 0.028(2) -0.004(2) -0.013(2) -0.004(2) C2 0.043(4) 0.064(5) 0.041(4) -0.003(3) -0.012(3) -0.017(4) Cl2 0.095(2) 0.096(2) 0.096(2) -0.0310(18) -0.0416(19) -0.0031(19) C3 0.051(4) 0.039(4) 0.032(3) 0.002(3) -0.015(3) -0.009(3) C4 0.044(4) 0.042(4) 0.034(3) 0.002(3) -0.018(3) -0.006(3) C5 0.025(3) 0.038(3) 0.031(3) -0.006(2) -0.010(2) -0.004(2) C6 0.027(3) 0.046(4) 0.028(3) -0.008(3) -0.006(2) 0.000(3) C7 0.035(3) 0.051(4) 0.044(4) -0.008(3) -0.018(3) 0.008(3) C11 0.039(3) 0.046(4) 0.024(3) 0.000(2) -0.010(2) -0.007(3) C12 0.036(3) 0.039(3) 0.030(3) -0.004(2) -0.009(3) -0.001(3) C13 0.029(3) 0.031(3) 0.032(3) -0.002(2) -0.004(2) -0.011(2) C14 0.027(3) 0.038(3) 0.023(3) -0.005(2) -0.005(2) -0.001(2) C15 0.035(3) 0.040(3) 0.024(3) -0.006(2) -0.006(2) -0.007(3) C16 0.055(5) 0.050(4) 0.032(3) -0.016(3) -0.007(3) -0.003(4) C17 0.061(5) 0.063(5) 0.031(3) -0.003(3) -0.021(3) -0.003(4) C18 0.049(4) 0.038(4) 0.049(4) -0.001(3) -0.020(3) 0.001(3) C19 0.048(4) 0.038(4) 0.043(4) -0.015(3) -0.014(3) -0.001(3) C20 0.093(9) 0.116(11) 0.062(7) -0.027(7) -0.007(6) -0.012(8) C21 0.034(3) 0.045(4) 0.029(3) -0.003(3) -0.015(2) -0.001(3) C22 0.033(3) 0.054(4) 0.034(3) -0.009(3) -0.013(3) 0.002(3) C23 0.045(4) 0.064(5) 0.041(4) -0.018(4) -0.013(3) 0.001(4) C24 0.074(6) 0.055(5) 0.043(4) -0.019(4) -0.029(4) 0.006(4) C25 0.057(5) 0.057(5) 0.045(4) -0.009(3) -0.027(4) -0.011(4) C26 0.040(4) 0.055(4) 0.039(3) -0.009(3) -0.016(3) -0.007(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh C1 2.045(6) . ? Rh C14 2.104(7) . ? Rh C15 2.141(7) . ? Rh C13 2.181(7) . ? Rh C12 2.266(7) . ? Rh C11 2.279(6) . ? Rh I1 2.7088(19) . ? Rh I2 2.7088(18) . ? C1 N1 1.357(9) . ? C1 N2 1.376(8) . ? N1 C3 1.378(9) . ? N1 C2 1.451(10) . ? Cl1 C20 1.776(14) . ? N2 C4 1.388(8) . ? N2 C5 1.472(9) . ? Cl2 C20 1.663(16) . ? C3 C4 1.327(11) . ? C5 C21 1.530(10) . ? C5 C7 1.540(9) . ? C5 C6 1.544(9) . ? C6 C14 1.496(9) . ? C11 C12 1.402(10) . ? C11 C15 1.441(9) . ? C11 C17 1.494(10) . ? C12 C13 1.448(9) . ? C12 C18 1.487(10) . ? C13 C14 1.442(9) . ? C13 C19 1.471(10) . ? C14 C15 1.437(9) . ? C15 C16 1.493(10) . ? C21 C26 1.385(11) . ? C21 C22 1.393(10) . ? C22 C23 1.380(12) . ? C23 C24 1.365(14) . ? C24 C25 1.385(13) . ? C25 C26 1.363(12) . ? 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 C1 Rh C14 91.0(3) . . ? C1 Rh C15 108.3(3) . . ? C14 Rh C15 39.6(2) . . ? C1 Rh C13 112.9(3) . . ? C14 Rh C13 39.3(2) . . ? C15 Rh C13 65.1(3) . . ? C1 Rh C12 150.7(3) . . ? C14 Rh C12 64.2(2) . . ? C15 Rh C12 63.0(3) . . ? C13 Rh C12 37.9(2) . . ? C1 Rh C11 146.0(3) . . ? C14 Rh C11 64.0(2) . . ? C15 Rh C11 37.9(2) . . ? C13 Rh C11 62.6(3) . . ? C12 Rh C11 35.9(3) . . ? C1 Rh I1 89.69(18) . . ? C14 Rh I1 127.60(18) . . ? C15 Rh I1 156.07(19) . . ? C13 Rh I1 93.76(18) . . ? C12 Rh I1 93.57(18) . . ? C11 Rh I1 123.50(19) . . ? C1 Rh I2 97.5(2) . . ? C14 Rh I2 133.84(18) . . ? C15 Rh I2 95.4(2) . . ? C13 Rh I2 147.54(17) . . ? C12 Rh I2 110.82(19) . . ? C11 Rh I2 85.9(2) . . ? I1 Rh I2 97.86(8) . . ? N1 C1 N2 104.2(5) . . ? N1 C1 Rh 129.7(5) . . ? N2 C1 Rh 126.0(5) . . ? C1 N1 C3 110.9(6) . . ? C1 N1 C2 128.5(6) . . ? C3 N1 C2 120.6(7) . . ? C1 N2 C4 110.0(6) . . ? C1 N2 C5 129.3(5) . . ? C4 N2 C5 119.2(5) . . ? C4 C3 N1 107.7(6) . . ? C3 C4 N2 107.2(6) . . ? N2 C5 C21 109.5(5) . . ? N2 C5 C7 108.8(6) . . ? C21 C5 C7 108.6(5) . . ? N2 C5 C6 111.9(5) . . ? C21 C5 C6 112.5(6) . . ? C7 C5 C6 105.4(5) . . ? C14 C6 C5 120.8(5) . . ? C12 C11 C15 108.4(6) . . ? C12 C11 C17 126.1(7) . . ? C15 C11 C17 125.4(7) . . ? C12 C11 Rh 71.5(4) . . ? C15 C11 Rh 65.9(3) . . ? C17 C11 Rh 132.4(6) . . ? C11 C12 C13 108.9(6) . . ? C11 C12 C18 125.6(6) . . ? C13 C12 C18 125.3(7) . . ? C11 C12 Rh 72.5(4) . . ? C13 C12 Rh 67.9(4) . . ? C18 C12 Rh 129.4(5) . . ? C14 C13 C12 107.2(6) . . ? C14 C13 C19 129.5(6) . . ? C12 C13 C19 122.6(6) . . ? C14 C13 Rh 67.5(4) . . ? C12 C13 Rh 74.2(4) . . ? C19 C13 Rh 131.2(5) . . ? C15 C14 C13 107.7(5) . . ? C15 C14 C6 123.1(6) . . ? C13 C14 C6 129.1(6) . . ? C15 C14 Rh 71.6(4) . . ? C13 C14 Rh 73.2(4) . . ? C6 C14 Rh 123.5(5) . . ? C14 C15 C11 107.9(6) . . ? C14 C15 C16 126.9(6) . . ? C11 C15 C16 124.5(6) . . ? C14 C15 Rh 68.8(4) . . ? C11 C15 Rh 76.2(4) . . ? C16 C15 Rh 127.9(6) . . ? Cl2 C20 Cl1 114.8(8) . . ? C26 C21 C22 118.5(7) . . ? C26 C21 C5 119.6(6) . . ? C22 C21 C5 121.9(7) . . ? C23 C22 C21 120.0(8) . . ? C24 C23 C22 120.9(8) . . ? C23 C24 C25 119.3(8) . . ? C26 C25 C24 120.5(9) . . ? C25 C26 C21 120.9(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C14 Rh C1 N1 -172.5(6) . . . . ? C15 Rh C1 N1 -136.2(6) . . . . ? C13 Rh C1 N1 153.9(6) . . . . ? C12 Rh C1 N1 156.7(5) . . . . ? C11 Rh C1 N1 -131.7(6) . . . . ? I1 Rh C1 N1 59.9(6) . . . . ? I2 Rh C1 N1 -38.0(6) . . . . ? C14 Rh C1 N2 9.9(6) . . . . ? C15 Rh C1 N2 46.2(6) . . . . ? C13 Rh C1 N2 -23.7(6) . . . . ? C12 Rh C1 N2 -20.9(9) . . . . ? C11 Rh C1 N2 50.7(8) . . . . ? I1 Rh C1 N2 -117.7(5) . . . . ? I2 Rh C1 N2 144.5(5) . . . . ? N2 C1 N1 C3 0.5(7) . . . . ? Rh C1 N1 C3 -177.5(5) . . . . ? N2 C1 N1 C2 -179.0(7) . . . . ? Rh C1 N1 C2 3.0(11) . . . . ? N1 C1 N2 C4 -1.0(7) . . . . ? Rh C1 N2 C4 177.1(5) . . . . ? N1 C1 N2 C5 -167.1(6) . . . . ? Rh C1 N2 C5 11.0(9) . . . . ? C1 N1 C3 C4 0.2(9) . . . . ? C2 N1 C3 C4 179.7(7) . . . . ? N1 C3 C4 N2 -0.8(9) . . . . ? C1 N2 C4 C3 1.1(8) . . . . ? C5 N2 C4 C3 168.8(6) . . . . ? C1 N2 C5 C21 83.4(7) . . . . ? C4 N2 C5 C21 -81.6(7) . . . . ? C1 N2 C5 C7 -158.1(6) . . . . ? C4 N2 C5 C7 37.0(8) . . . . ? C1 N2 C5 C6 -42.0(9) . . . . ? C4 N2 C5 C6 153.0(6) . . . . ? N2 C5 C6 C14 49.8(9) . . . . ? C21 C5 C6 C14 -74.0(8) . . . . ? C7 C5 C6 C14 167.9(7) . . . . ? C1 Rh C11 C12 -127.8(5) . . . . ? C14 Rh C11 C12 -81.2(5) . . . . ? C15 Rh C11 C12 -120.9(6) . . . . ? C13 Rh C11 C12 -37.0(4) . . . . ? I1 Rh C11 C12 38.2(5) . . . . ? I2 Rh C11 C12 134.9(4) . . . . ? C1 Rh C11 C15 -6.9(7) . . . . ? C14 Rh C11 C15 39.7(4) . . . . ? C13 Rh C11 C15 83.9(5) . . . . ? C12 Rh C11 C15 120.9(6) . . . . ? I1 Rh C11 C15 159.1(3) . . . . ? I2 Rh C11 C15 -104.2(4) . . . . ? C1 Rh C11 C17 109.8(8) . . . . ? C14 Rh C11 C17 156.4(8) . . . . ? C15 Rh C11 C17 116.7(9) . . . . ? C13 Rh C11 C17 -159.4(8) . . . . ? C12 Rh C11 C17 -122.4(9) . . . . ? I1 Rh C11 C17 -84.2(8) . . . . ? I2 Rh C11 C17 12.5(7) . . . . ? C15 C11 C12 C13 2.8(8) . . . . ? C17 C11 C12 C13 -172.1(7) . . . . ? Rh C11 C12 C13 58.4(5) . . . . ? C15 C11 C12 C18 178.1(7) . . . . ? C17 C11 C12 C18 3.2(13) . . . . ? Rh C11 C12 C18 -126.3(8) . . . . ? C15 C11 C12 Rh -55.6(5) . . . . ? C17 C11 C12 Rh 129.6(8) . . . . ? C1 Rh C12 C11 115.4(6) . . . . ? C14 Rh C12 C11 80.6(4) . . . . ? C15 Rh C12 C11 36.3(4) . . . . ? C13 Rh C12 C11 119.6(6) . . . . ? I1 Rh C12 C11 -148.9(4) . . . . ? I2 Rh C12 C11 -49.1(4) . . . . ? C1 Rh C12 C13 -4.2(7) . . . . ? C14 Rh C12 C13 -38.9(4) . . . . ? C15 Rh C12 C13 -83.3(4) . . . . ? C11 Rh C12 C13 -119.6(6) . . . . ? I1 Rh C12 C13 91.5(4) . . . . ? I2 Rh C12 C13 -168.7(3) . . . . ? C1 Rh C12 C18 -122.5(7) . . . . ? C14 Rh C12 C18 -157.2(8) . . . . ? C15 Rh C12 C18 158.4(8) . . . . ? C13 Rh C12 C18 -118.3(8) . . . . ? C11 Rh C12 C18 122.1(9) . . . . ? I1 Rh C12 C18 -26.8(7) . . . . ? I2 Rh C12 C18 73.0(7) . . . . ? C11 C12 C13 C14 -1.5(8) . . . . ? C18 C12 C13 C14 -176.9(7) . . . . ? Rh C12 C13 C14 59.7(4) . . . . ? C11 C12 C13 C19 169.6(7) . . . . ? C18 C12 C13 C19 -5.7(11) . . . . ? Rh C12 C13 C19 -129.2(7) . . . . ? C11 C12 C13 Rh -61.2(5) . . . . ? C18 C12 C13 Rh 123.4(7) . . . . ? C1 Rh C13 C14 61.1(4) . . . . ? C15 Rh C13 C14 -39.3(4) . . . . ? C12 Rh C13 C14 -116.7(5) . . . . ? C11 Rh C13 C14 -81.6(4) . . . . ? I1 Rh C13 C14 152.3(3) . . . . ? I2 Rh C13 C14 -96.7(4) . . . . ? C1 Rh C13 C12 177.8(4) . . . . ? C14 Rh C13 C12 116.7(5) . . . . ? C15 Rh C13 C12 77.4(4) . . . . ? C11 Rh C13 C12 35.1(4) . . . . ? I1 Rh C13 C12 -91.0(4) . . . . ? I2 Rh C13 C12 20.0(5) . . . . ? C1 Rh C13 C19 -62.5(7) . . . . ? C14 Rh C13 C19 -123.6(8) . . . . ? C15 Rh C13 C19 -162.8(7) . . . . ? C12 Rh C13 C19 119.7(8) . . . . ? C11 Rh C13 C19 154.8(7) . . . . ? I1 Rh C13 C19 28.7(6) . . . . ? I2 Rh C13 C19 139.7(5) . . . . ? C12 C13 C14 C15 -0.3(7) . . . . ? C19 C13 C14 C15 -170.6(7) . . . . ? Rh C13 C14 C15 63.8(5) . . . . ? C12 C13 C14 C6 176.0(7) . . . . ? C19 C13 C14 C6 5.7(12) . . . . ? Rh C13 C14 C6 -119.9(7) . . . . ? C12 C13 C14 Rh -64.1(5) . . . . ? C19 C13 C14 Rh 125.6(7) . . . . ? C5 C6 C14 C15 -118.2(7) . . . . ? C5 C6 C14 C13 66.1(10) . . . . ? C5 C6 C14 Rh -29.3(9) . . . . ? C1 Rh C14 C15 118.0(4) . . . . ? C13 Rh C14 C15 -115.7(5) . . . . ? C12 Rh C14 C15 -78.1(4) . . . . ? C11 Rh C14 C15 -38.0(4) . . . . ? I1 Rh C14 C15 -151.5(3) . . . . ? I2 Rh C14 C15 16.6(5) . . . . ? C1 Rh C14 C13 -126.2(4) . . . . ? C15 Rh C14 C13 115.7(5) . . . . ? C12 Rh C14 C13 37.6(4) . . . . ? C11 Rh C14 C13 77.7(4) . . . . ? I1 Rh C14 C13 -35.8(4) . . . . ? I2 Rh C14 C13 132.4(3) . . . . ? C1 Rh C14 C6 0.0(6) . . . . ? C15 Rh C14 C6 -118.1(7) . . . . ? C13 Rh C14 C6 126.2(7) . . . . ? C12 Rh C14 C6 163.8(6) . . . . ? C11 Rh C14 C6 -156.1(6) . . . . ? I1 Rh C14 C6 90.4(6) . . . . ? I2 Rh C14 C6 -101.4(5) . . . . ? C13 C14 C15 C11 2.0(8) . . . . ? C6 C14 C15 C11 -174.6(6) . . . . ? Rh C14 C15 C11 66.8(5) . . . . ? C13 C14 C15 C16 172.9(7) . . . . ? C6 C14 C15 C16 -3.6(11) . . . . ? Rh C14 C15 C16 -122.2(8) . . . . ? C13 C14 C15 Rh -64.9(4) . . . . ? C6 C14 C15 Rh 118.6(7) . . . . ? C12 C11 C15 C14 -2.9(8) . . . . ? C17 C11 C15 C14 172.0(7) . . . . ? Rh C11 C15 C14 -62.0(5) . . . . ? C12 C11 C15 C16 -174.1(7) . . . . ? C17 C11 C15 C16 0.7(12) . . . . ? Rh C11 C15 C16 126.8(8) . . . . ? C12 C11 C15 Rh 59.0(5) . . . . ? C17 C11 C15 Rh -126.1(8) . . . . ? C1 Rh C15 C14 -68.3(4) . . . . ? C13 Rh C15 C14 39.0(4) . . . . ? C12 Rh C15 C14 81.3(4) . . . . ? C11 Rh C15 C14 115.7(6) . . . . ? I1 Rh C15 C14 68.6(6) . . . . ? I2 Rh C15 C14 -168.0(3) . . . . ? C1 Rh C15 C11 175.9(4) . . . . ? C14 Rh C15 C11 -115.7(6) . . . . ? C13 Rh C15 C11 -76.7(5) . . . . ? C12 Rh C15 C11 -34.4(4) . . . . ? I1 Rh C15 C11 -47.2(7) . . . . ? I2 Rh C15 C11 76.2(4) . . . . ? C1 Rh C15 C16 52.7(7) . . . . ? C14 Rh C15 C16 121.0(8) . . . . ? C13 Rh C15 C16 160.0(7) . . . . ? C12 Rh C15 C16 -157.7(7) . . . . ? C11 Rh C15 C16 -123.3(8) . . . . ? I1 Rh C15 C16 -170.4(4) . . . . ? I2 Rh C15 C16 -47.0(6) . . . . ? N2 C5 C21 C26 172.9(6) . . . . ? C7 C5 C21 C26 54.3(8) . . . . ? C6 C5 C21 C26 -62.0(8) . . . . ? N2 C5 C21 C22 -6.2(8) . . . . ? C7 C5 C21 C22 -124.8(7) . . . . ? C6 C5 C21 C22 118.9(7) . . . . ? C26 C21 C22 C23 0.8(10) . . . . ? C5 C21 C22 C23 179.9(6) . . . . ? C21 C22 C23 C24 0.3(12) . . . . ? C22 C23 C24 C25 -0.9(13) . . . . ? C23 C24 C25 C26 0.4(12) . . . . ? C24 C25 C26 C21 0.8(12) . . . . ? C22 C21 C26 C25 -1.4(11) . . . . ? C5 C21 C26 C25 179.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 28.28 _diffrn_measured_fraction_theta_full 0.930 _refine_diff_density_max 1.563 _refine_diff_density_min -2.389 _refine_diff_density_rms 0.190