Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Neil Connelly' _publ_contact_author_address ; School of Chemistry University of Bristol BRISTOL BS8 1TS UNITED KINGDOM ; _publ_contact_author_email NEIL.CONNELLY@BRIS.AC.UK _publ_section_title ; Iodination reactions of triazenide-bridged rhodium and iridium complexes: oxidative addition vs. one-electron oxidation ; loop_ _publ_author_name N.Connelly C.Adams R.A.Baber P.Harding O.D.Hayward M.Kandiah ; A.Orpen ; data_4 _database_code_depnum_ccdc_archive 'CCDC 633932' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 I2 Ir N6 O4 Rh' _chemical_formula_sum 'C32 H28 I2 Ir N6 O4 Rh' _chemical_formula_weight 1109.51 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' O O 0.0106 0.0060 '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' 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.513(5) _cell_length_b 8.4782(15) _cell_length_c 21.624(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.566(15) _cell_angle_gamma 90.00 _cell_volume 3521.0(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needles _exptl_crystal_colour 'Dark red' _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.093 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2088 _exptl_absorpt_coefficient_mu 6.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.577 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10979 _diffrn_reflns_av_R_equivalents 0.0360 _diffrn_reflns_av_sigmaI/netI 0.0356 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 27.58 _reflns_number_total 4051 _reflns_number_gt 2958 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^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 SHELXL _refine_ls_extinction_coef 0.00023(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4051 _refine_ls_number_parameters 211 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0492 _refine_ls_R_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0788 _refine_ls_wR_factor_gt 0.0721 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 -0.010965(11) 0.31576(2) 0.306442(9) 0.02080(8) Uani 0.50 1 d P . . Ir1 Ir -0.010965(11) 0.31576(2) 0.306442(9) 0.02080(8) Uani 0.50 1 d P . . I1 I -0.033456(17) 0.32569(4) 0.424584(14) 0.03697(11) Uani 1 1 d . . . C1 C -0.0972(3) 0.2072(5) 0.2740(2) 0.0313(10) Uani 1 1 d . . . O1 O -0.14781(18) 0.1442(4) 0.25587(16) 0.0444(8) Uani 1 1 d . . . C2 C 0.0382(2) 0.1235(5) 0.3369(2) 0.0321(10) Uani 1 1 d . . . O2 O 0.06515(19) 0.0115(3) 0.35282(17) 0.0470(9) Uani 1 1 d . . . N1 N 0.06765(17) 0.5235(3) 0.23461(15) 0.0219(7) Uani 1 1 d . . . N2 N 0.09816(18) 0.5413(4) 0.29804(15) 0.0247(7) Uani 1 1 d . . . N3 N 0.08059(17) 0.4500(4) 0.33741(15) 0.0232(7) Uani 1 1 d . . . C11 C 0.0946(2) 0.6355(5) 0.19970(18) 0.0243(9) Uani 1 1 d . . . C12 C 0.1647(2) 0.6754(5) 0.2220(2) 0.0330(10) Uani 1 1 d . . . H12A H 0.1961 0.6259 0.2602 0.040 Uiso 1 1 calc R . . C13 C 0.1888(3) 0.7869(5) 0.1887(2) 0.0369(11) Uani 1 1 d . . . H13A H 0.2366 0.8154 0.2053 0.044 Uiso 1 1 calc R . . C14 C 0.1447(2) 0.8586(5) 0.1314(2) 0.0319(10) Uani 1 1 d . . . C15 C 0.0754(3) 0.8160(5) 0.1097(2) 0.0348(11) Uani 1 1 d . . . H15A H 0.0440 0.8639 0.0710 0.042 Uiso 1 1 calc R . . C16 C 0.0506(2) 0.7062(5) 0.1426(2) 0.0335(10) Uani 1 1 d . . . H16A H 0.0027 0.6784 0.1260 0.040 Uiso 1 1 calc R . . C17 C 0.1714(3) 0.9784(5) 0.0951(2) 0.0447(13) Uani 1 1 d . . . H17A H 0.1499 0.9606 0.0474 0.067 Uiso 1 1 calc R . . H17B H 0.2221 0.9682 0.1083 0.067 Uiso 1 1 calc R . . H17C H 0.1598 1.0846 0.1059 0.067 Uiso 1 1 calc R . . C18 C 0.1218(2) 0.4835(4) 0.40560(18) 0.0238(9) Uani 1 1 d . . . C19 C 0.1347(2) 0.6377(5) 0.42839(19) 0.0258(9) Uani 1 1 d . . . H19A H 0.1164 0.7230 0.3989 0.031 Uiso 1 1 calc R . . C20 C 0.1738(2) 0.6676(5) 0.4934(2) 0.0291(10) Uani 1 1 d . . . H20A H 0.1822 0.7737 0.5082 0.035 Uiso 1 1 calc R . . C21 C 0.2012(2) 0.5458(5) 0.53795(19) 0.0299(9) Uani 1 1 d . . . C22 C 0.1894(2) 0.3925(5) 0.5144(2) 0.0341(10) Uani 1 1 d . . . H22A H 0.2087 0.3074 0.5437 0.041 Uiso 1 1 calc R . . C23 C 0.1499(2) 0.3607(5) 0.4488(2) 0.0311(10) Uani 1 1 d . . . H23A H 0.1423 0.2548 0.4336 0.037 Uiso 1 1 calc R . . C24 C 0.2425(3) 0.5774(6) 0.61005(19) 0.0437(12) Uani 1 1 d . . . H24A H 0.2736 0.4882 0.6286 0.066 Uiso 1 1 calc R . . H24B H 0.2104 0.5909 0.6342 0.066 Uiso 1 1 calc R . . H24C H 0.2701 0.6736 0.6140 0.066 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 0.02090(13) 0.02040(12) 0.02076(12) 0.00156(8) 0.00688(9) -0.00036(8) Ir1 0.02090(13) 0.02040(12) 0.02076(12) 0.00156(8) 0.00688(9) -0.00036(8) I1 0.0385(2) 0.0488(2) 0.02708(17) 0.00311(12) 0.01584(14) -0.00271(14) C1 0.036(3) 0.030(2) 0.029(2) 0.0060(18) 0.012(2) 0.004(2) O1 0.032(2) 0.0450(19) 0.048(2) 0.0044(16) 0.0043(16) -0.0093(16) C2 0.032(3) 0.032(2) 0.030(2) 0.0023(19) 0.009(2) -0.008(2) O2 0.051(2) 0.0220(17) 0.065(2) 0.0106(15) 0.0172(19) 0.0052(15) N1 0.0225(19) 0.0219(16) 0.0203(16) 0.0003(13) 0.0062(14) -0.0003(13) N2 0.024(2) 0.0269(17) 0.0229(16) -0.0007(14) 0.0081(15) 0.0001(14) N3 0.0236(19) 0.0235(17) 0.0225(16) 0.0019(14) 0.0079(14) -0.0023(14) C11 0.027(2) 0.0238(19) 0.024(2) 0.0001(16) 0.0119(18) -0.0007(17) C12 0.027(3) 0.033(2) 0.036(2) 0.0095(19) 0.008(2) 0.0031(18) C13 0.029(3) 0.033(2) 0.050(3) 0.008(2) 0.015(2) -0.0032(19) C14 0.040(3) 0.023(2) 0.040(3) 0.0015(18) 0.024(2) 0.0005(19) C15 0.043(3) 0.033(2) 0.027(2) 0.0057(18) 0.010(2) 0.000(2) C16 0.030(3) 0.038(3) 0.028(2) 0.0067(18) 0.005(2) -0.007(2) C17 0.060(4) 0.029(2) 0.058(3) 0.007(2) 0.037(3) 0.004(2) C18 0.023(2) 0.027(2) 0.0209(19) 0.0010(15) 0.0074(17) 0.0007(16) C19 0.025(2) 0.026(2) 0.024(2) 0.0012(16) 0.0066(18) 0.0048(17) C20 0.027(3) 0.031(2) 0.026(2) -0.0074(17) 0.0057(18) -0.0005(18) C21 0.022(2) 0.044(3) 0.023(2) 0.0013(19) 0.0075(17) -0.003(2) C22 0.032(3) 0.037(2) 0.029(2) 0.0116(19) 0.0061(19) -0.001(2) C23 0.034(3) 0.026(2) 0.029(2) 0.0023(17) 0.006(2) -0.0047(19) C24 0.042(3) 0.063(3) 0.023(2) 0.001(2) 0.007(2) -0.004(2) _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 1.897(5) . ? Rh1 C2 1.908(5) . ? Rh1 N3 2.094(3) . ? Rh1 N1 2.125(3) 2 ? Rh1 Ir1 2.6329(5) 2 ? Rh1 Rh1 2.6329(5) 2 ? Rh1 I1 2.7522(5) . ? C1 O1 1.109(5) . ? C2 O2 1.092(5) . ? N1 N2 1.301(4) . ? N1 C11 1.439(5) . ? N1 Ir1 2.125(3) 2 ? N1 Rh1 2.125(3) 2 ? N2 N3 1.292(4) . ? N3 C18 1.447(5) . ? C11 C16 1.383(5) . ? C11 C12 1.388(6) . ? C12 C13 1.381(6) . ? C13 C14 1.391(6) . ? C14 C15 1.379(6) . ? C14 C17 1.500(6) . ? C15 C16 1.374(6) . ? C18 C23 1.382(5) . ? C18 C19 1.389(5) . ? C19 C20 1.376(5) . ? C20 C21 1.389(5) . ? C21 C22 1.386(6) . ? C21 C24 1.514(5) . ? C22 C23 1.391(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 C2 91.43(17) . . ? C1 Rh1 N3 175.59(14) . . ? C2 Rh1 N3 92.72(16) . . ? C1 Rh1 N1 86.85(15) . 2 ? C2 Rh1 N1 175.83(15) . 2 ? N3 Rh1 N1 88.91(12) . 2 ? C1 Rh1 Ir1 95.64(13) . 2 ? C2 Rh1 Ir1 94.48(13) . 2 ? N3 Rh1 Ir1 82.55(9) . 2 ? N1 Rh1 Ir1 81.92(8) 2 2 ? C1 Rh1 Rh1 95.64(13) . 2 ? C2 Rh1 Rh1 94.48(13) . 2 ? N3 Rh1 Rh1 82.55(9) . 2 ? N1 Rh1 Rh1 81.92(8) 2 2 ? Ir1 Rh1 Rh1 0.000(8) 2 2 ? C1 Rh1 I1 85.36(13) . . ? C2 Rh1 I1 86.93(13) . . ? N3 Rh1 I1 96.34(9) . . ? N1 Rh1 I1 96.71(8) 2 . ? Ir1 Rh1 I1 178.238(7) 2 . ? Rh1 Rh1 I1 178.238(7) 2 . ? O1 C1 Rh1 179.0(4) . . ? O2 C2 Rh1 178.0(4) . . ? N2 N1 C11 110.2(3) . . ? N2 N1 Ir1 121.8(2) . 2 ? C11 N1 Ir1 125.6(2) . 2 ? N2 N1 Rh1 121.8(2) . 2 ? C11 N1 Rh1 125.6(2) . 2 ? Ir1 N1 Rh1 0.000(18) 2 2 ? N3 N2 N1 118.9(3) . . ? N2 N3 C18 110.8(3) . . ? N2 N3 Rh1 122.8(2) . . ? C18 N3 Rh1 124.7(2) . . ? C16 C11 C12 118.4(4) . . ? C16 C11 N1 120.2(4) . . ? C12 C11 N1 121.4(4) . . ? C13 C12 C11 120.2(4) . . ? C12 C13 C14 121.5(5) . . ? C15 C14 C13 117.3(4) . . ? C15 C14 C17 121.5(4) . . ? C13 C14 C17 121.2(4) . . ? C16 C15 C14 121.7(4) . . ? C15 C16 C11 120.8(4) . . ? C23 C18 C19 119.1(4) . . ? C23 C18 N3 119.8(3) . . ? C19 C18 N3 121.1(3) . . ? C20 C19 C18 120.4(4) . . ? C19 C20 C21 121.3(4) . . ? C22 C21 C20 117.8(4) . . ? C22 C21 C24 120.5(4) . . ? C20 C21 C24 121.7(4) . . ? C21 C22 C23 121.4(4) . . ? C18 C23 C22 119.9(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.409 _refine_diff_density_min -0.815 _refine_diff_density_rms 0.138 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 633933' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 I3 N6 O2 Rh2, 1.5(C16 H36 N), 0.5(P F6), O' _chemical_formula_sum 'C54 H82 F3 I3 N7.5 O3 P0.5 Rh2' _chemical_formula_weight 1543.31 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' O O 0.0106 0.0060 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 30.696(4) _cell_length_b 11.6049(15) _cell_length_c 18.233(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6495.0(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 209 _cell_measurement_theta_min 2.183 _cell_measurement_theta_max 21.951 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3064 _exptl_absorpt_coefficient_mu 1.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.903 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 68787 _diffrn_reflns_av_R_equivalents 0.0746 _diffrn_reflns_av_sigmaI/netI 0.0702 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.53 _reflns_number_total 14959 _reflns_number_gt 10516 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker, 1998)' _computing_cell_refinement 'Bruker SMART (Bruker, 1998)' _computing_data_reduction 'Bruker SAINT (Bruker, 1998)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1998)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1998)' _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^)+(0.0780P)^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(2) _refine_ls_number_reflns 14959 _refine_ls_number_parameters 655 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1389 _refine_ls_wR_factor_gt 0.1148 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.15944(2) 0.52649(5) 0.82886(3) 0.03584(15) Uani 1 1 d . . . Rh2 Rh 0.147789(19) 0.59489(5) 0.69587(3) 0.03471(14) Uani 1 1 d . . . I1 I 0.139283(18) 0.65733(5) 0.55344(3) 0.04662(15) Uani 1 1 d . . . I2 I 0.072633(19) 0.70186(6) 0.72211(4) 0.05556(17) Uani 1 1 d . . . I3 I 0.234976(19) 0.62268(5) 0.86129(3) 0.04894(15) Uani 1 1 d . . . C1 C 0.1748(3) 0.7372(8) 0.7085(5) 0.046(2) Uani 1 1 d . . . O1 O 0.1906(2) 0.8252(5) 0.7147(4) 0.0548(16) Uani 1 1 d . . . C2 C 0.1317(3) 0.6491(8) 0.8768(4) 0.043(2) Uani 1 1 d . . . O2 O 0.1172(2) 0.7216(6) 0.9087(4) 0.0613(17) Uani 1 1 d . . . N1 N 0.1119(2) 0.4395(6) 0.6909(4) 0.0406(16) Uani 1 1 d . . . N2 N 0.0903(2) 0.4021(7) 0.7457(4) 0.0454(17) Uani 1 1 d . . . N3 N 0.1039(2) 0.4360(6) 0.8100(4) 0.0428(17) Uani 1 1 d . . . N4 N 0.20368(19) 0.4961(5) 0.6775(3) 0.0343(14) Uani 1 1 d . . . N5 N 0.21264(19) 0.4049(5) 0.7164(3) 0.0327(13) Uani 1 1 d . . . N6 N 0.19350(19) 0.3950(5) 0.7778(3) 0.0354(14) Uani 1 1 d . . . C11 C 0.0950(3) 0.3948(8) 0.6231(4) 0.046(2) Uani 1 1 d . . . C12 C 0.0512(3) 0.3886(11) 0.6086(5) 0.066(3) Uani 1 1 d . . . H12A H 0.0310 0.4146 0.6445 0.079 Uiso 1 1 calc R . . C13 C 0.0360(3) 0.3458(12) 0.5436(7) 0.085(4) Uani 1 1 d . . . H13A H 0.0055 0.3412 0.5356 0.102 Uiso 1 1 calc R . . C14 C 0.0649(3) 0.3081(12) 0.4881(7) 0.081(4) Uani 1 1 d . . . C15 C 0.1088(3) 0.3152(8) 0.5035(5) 0.056(2) Uani 1 1 d . . . H15A H 0.1291 0.2897 0.4676 0.067 Uiso 1 1 calc R . . C16 C 0.1243(3) 0.3580(8) 0.5692(4) 0.045(2) Uani 1 1 d . . . H16A H 0.1547 0.3625 0.5778 0.054 Uiso 1 1 calc R . . C17 C 0.0494(4) 0.2679(16) 0.4131(8) 0.121(6) Uani 1 1 d . . . H17A H 0.0686 0.2993 0.3751 0.181 Uiso 1 1 calc R . . H17B H 0.0196 0.2950 0.4047 0.181 Uiso 1 1 calc R . . H17C H 0.0500 0.1835 0.4111 0.181 Uiso 1 1 calc R . . C18 C 0.0755(3) 0.4025(8) 0.8689(5) 0.048(2) Uani 1 1 d . . . C19 C 0.0310(3) 0.3881(10) 0.8565(6) 0.073(3) Uani 1 1 d . . . H19A H 0.0195 0.3965 0.8085 0.088 Uiso 1 1 calc R . . C20 C 0.0039(4) 0.3616(11) 0.9141(6) 0.076(3) Uani 1 1 d . . . H20A H -0.0262 0.3479 0.9052 0.091 Uiso 1 1 calc R . . C21 C 0.0196(4) 0.3548(8) 0.9835(8) 0.086(4) Uani 1 1 d . . . C22 C 0.0658(4) 0.3673(9) 0.9985(6) 0.076(3) Uani 1 1 d . . . H22A H 0.0776 0.3582 1.0464 0.091 Uiso 1 1 calc R . . C23 C 0.0918(3) 0.3936(8) 0.9378(5) 0.059(3) Uani 1 1 d . . . H23A H 0.1221 0.4058 0.9452 0.070 Uiso 1 1 calc R . . C24 C -0.0087(5) 0.3279(11) 1.0529(7) 0.098(5) Uani 1 1 d . . . H24A H -0.0388 0.3121 1.0378 0.147 Uiso 1 1 calc R . . H24B H -0.0083 0.3944 1.0860 0.147 Uiso 1 1 calc R . . H24C H 0.0032 0.2604 1.0782 0.147 Uiso 1 1 calc R . . C25 C 0.2010(3) 0.2898(6) 0.8145(4) 0.0370(17) Uani 1 1 d . . . C26 C 0.2033(3) 0.1845(8) 0.7765(5) 0.054(2) Uani 1 1 d . . . H26A H 0.1992 0.1829 0.7249 0.065 Uiso 1 1 calc R . . C27 C 0.2116(3) 0.0837(8) 0.8140(6) 0.062(3) Uani 1 1 d . . . H27A H 0.2139 0.0140 0.7869 0.074 Uiso 1 1 calc R . . C28 C 0.2166(3) 0.0794(8) 0.8895(5) 0.050(2) Uani 1 1 d . . . C29 C 0.2147(3) 0.1860(7) 0.9268(5) 0.043(2) Uani 1 1 d . . . H29A H 0.2193 0.1868 0.9783 0.052 Uiso 1 1 calc R . . C30 C 0.2067(3) 0.2865(8) 0.8924(5) 0.047(2) Uani 1 1 d . . . H30A H 0.2048 0.3557 0.9201 0.056 Uiso 1 1 calc R . . C31 C 0.2255(4) -0.0335(9) 0.9315(7) 0.080(3) Uani 1 1 d . . . H31C H 0.2474 -0.0788 0.9050 0.120 Uiso 1 1 calc R . . H31D H 0.1985 -0.0781 0.9353 0.120 Uiso 1 1 calc R . . H31E H 0.2363 -0.0155 0.9807 0.120 Uiso 1 1 calc R . . C32 C 0.2324(2) 0.5050(6) 0.6153(4) 0.0330(16) Uani 1 1 d . . . C33 C 0.2437(2) 0.4081(6) 0.5734(4) 0.0337(16) Uani 1 1 d . . . H33C H 0.2312 0.3349 0.5835 0.040 Uiso 1 1 calc R . . C34 C 0.2735(2) 0.4214(7) 0.5170(4) 0.0394(18) Uani 1 1 d . . . H34D H 0.2815 0.3550 0.4897 0.047 Uiso 1 1 calc R . . C35 C 0.2921(2) 0.5247(8) 0.4982(4) 0.0401(18) Uani 1 1 d . . . C36 C 0.2807(3) 0.6208(7) 0.5410(4) 0.0410(19) Uani 1 1 d . . . H36C H 0.2935 0.6935 0.5305 0.049 Uiso 1 1 calc R . . C37 C 0.2513(2) 0.6114(7) 0.5979(4) 0.0370(17) Uani 1 1 d . . . H37C H 0.2439 0.6778 0.6256 0.044 Uiso 1 1 calc R . . C38 C 0.3241(3) 0.5356(9) 0.4372(5) 0.056(2) Uani 1 1 d . . . H38D H 0.3374 0.4604 0.4276 0.084 Uiso 1 1 calc R . . H38E H 0.3467 0.5911 0.4509 0.084 Uiso 1 1 calc R . . H38F H 0.3091 0.5625 0.3929 0.084 Uiso 1 1 calc R . . N7 N 0.6482(2) 0.6578(6) 0.7151(4) 0.0448(16) Uani 1 1 d . . . C41 C 0.6803(3) 0.7373(7) 0.6769(5) 0.046(2) Uani 1 1 d . . . H41A H 0.7095 0.7234 0.6985 0.055 Uiso 1 1 calc R . . H41B H 0.6818 0.7141 0.6247 0.055 Uiso 1 1 calc R . . C42 C 0.6718(3) 0.8647(8) 0.6795(5) 0.051(2) Uani 1 1 d . . . H42A H 0.6720 0.8912 0.7311 0.062 Uiso 1 1 calc R . . H42B H 0.6427 0.8811 0.6587 0.062 Uiso 1 1 calc R . . C43 C 0.7066(3) 0.9304(7) 0.6358(5) 0.046(2) Uani 1 1 d . . . H4A H 0.7048 0.9077 0.5836 0.055 Uiso 1 1 calc R . . H4B H 0.7358 0.9085 0.6541 0.055 Uiso 1 1 calc R . . C44 C 0.7012(4) 1.0637(9) 0.6420(7) 0.073(3) Uani 1 1 d . . . H44A H 0.7239 1.1019 0.6131 0.109 Uiso 1 1 calc R . . H44B H 0.7038 1.0869 0.6935 0.109 Uiso 1 1 calc R . . H44C H 0.6724 1.0860 0.6233 0.109 Uiso 1 1 calc R . . C45 C 0.6662(3) 0.5362(7) 0.7141(5) 0.048(2) Uani 1 1 d . . . H45A H 0.6712 0.5133 0.6625 0.057 Uiso 1 1 calc R . . H45B H 0.6948 0.5361 0.7392 0.057 Uiso 1 1 calc R . . C46 C 0.6377(4) 0.4479(8) 0.7495(6) 0.065(3) Uani 1 1 d . . . H46A H 0.6076 0.4552 0.7306 0.078 Uiso 1 1 calc R . . H46B H 0.6370 0.4606 0.8032 0.078 Uiso 1 1 calc R . . C47 C 0.6552(3) 0.3258(7) 0.7331(6) 0.058(2) Uani 1 1 d . . . H47A H 0.6539 0.3120 0.6795 0.069 Uiso 1 1 calc R . . H47B H 0.6861 0.3216 0.7482 0.069 Uiso 1 1 calc R . . C48 C 0.6297(5) 0.2317(10) 0.7724(8) 0.097(5) Uani 1 1 d . . . H48A H 0.6427 0.1565 0.7614 0.145 Uiso 1 1 calc R . . H48B H 0.5994 0.2327 0.7556 0.145 Uiso 1 1 calc R . . H48C H 0.6306 0.2453 0.8254 0.145 Uiso 1 1 calc R . . C49 C 0.6039(3) 0.6634(9) 0.6752(6) 0.055(2) Uani 1 1 d . . . H49A H 0.5818 0.6247 0.7061 0.066 Uiso 1 1 calc R . . H49B H 0.5953 0.7453 0.6707 0.066 Uiso 1 1 calc R . . C50 C 0.6027(3) 0.6086(9) 0.5983(6) 0.059(2) Uani 1 1 d . . . H50A H 0.6256 0.6428 0.5668 0.070 Uiso 1 1 calc R . . H50B H 0.6079 0.5246 0.6018 0.070 Uiso 1 1 calc R . . C51 C 0.5579(3) 0.6319(10) 0.5662(7) 0.073(3) Uani 1 1 d . . . H51A H 0.5530 0.7160 0.5629 0.087 Uiso 1 1 calc R . . H51B H 0.5353 0.5989 0.5986 0.087 Uiso 1 1 calc R . . C52 C 0.5544(4) 0.5773(13) 0.4887(8) 0.093(4) Uani 1 1 d . . . H52A H 0.5304 0.6133 0.4618 0.139 Uiso 1 1 calc R . . H52B H 0.5489 0.4944 0.4934 0.139 Uiso 1 1 calc R . . H52C H 0.5818 0.5895 0.4620 0.139 Uiso 1 1 calc R . . C53 C 0.6389(3) 0.6976(7) 0.7924(5) 0.050(2) Uani 1 1 d . . . H53A H 0.6183 0.6428 0.8153 0.060 Uiso 1 1 calc R . . H53B H 0.6243 0.7736 0.7900 0.060 Uiso 1 1 calc R . . C54 C 0.6792(3) 0.7084(9) 0.8421(5) 0.058(2) Uani 1 1 d . . . H54A H 0.7015 0.7560 0.8172 0.069 Uiso 1 1 calc R . . H54B H 0.6918 0.6310 0.8505 0.069 Uiso 1 1 calc R . . C55 C 0.6675(4) 0.7644(10) 0.9176(6) 0.070(3) Uani 1 1 d . . . H55A H 0.6419 0.7244 0.9385 0.084 Uiso 1 1 calc R . . H55B H 0.6922 0.7535 0.9518 0.084 Uiso 1 1 calc R . . C56 C 0.6578(4) 0.8886(10) 0.9116(6) 0.082(4) Uani 1 1 d . . . H56A H 0.6433 0.9149 0.9565 0.123 Uiso 1 1 calc R . . H56B H 0.6386 0.9019 0.8695 0.123 Uiso 1 1 calc R . . H56C H 0.6850 0.9315 0.9048 0.123 Uiso 1 1 calc R . . C57 C 0.0164(7) 0.0946(17) 0.8245(10) 0.171(11) Uani 1 1 d . . . H57A H 0.0235 0.1625 0.8551 0.206 Uiso 1 1 calc R . . H57B H -0.0069 0.1174 0.7897 0.206 Uiso 1 1 calc R . . C58 C 0.0591(10) 0.056(2) 0.7790(11) 0.242(17) Uani 1 1 d . . . H58A H 0.0860 0.0865 0.8019 0.291 Uiso 1 1 calc R . . H58B H 0.0612 -0.0288 0.7754 0.291 Uiso 1 1 calc R . . C59 C 0.0512(6) 0.1114(14) 0.7030(18) 0.242(18) Uani 1 1 d . . . H59A H 0.0300 0.0668 0.6735 0.291 Uiso 1 1 calc R . . H59B H 0.0413 0.1924 0.7071 0.291 Uiso 1 1 calc R . . C60 C 0.0908(5) 0.1039(17) 0.6763(13) 0.169(9) Uani 1 1 d . . . H60A H 0.0894 0.0920 0.6232 0.253 Uiso 1 1 calc R . . H60B H 0.1060 0.0388 0.6992 0.253 Uiso 1 1 calc R . . H60C H 0.1067 0.1753 0.6867 0.253 Uiso 1 1 calc R . . C61 C -0.0359(4) 0.0484(10) 0.9179(7) 0.082(4) Uani 1 1 d . . . H61A H -0.0566 0.0896 0.8854 0.098 Uiso 1 1 calc R . . H61B H -0.0235 0.1055 0.9525 0.098 Uiso 1 1 calc R . . C62 C -0.0605(4) -0.0403(11) 0.9607(7) 0.089(4) Uani 1 1 d . . . H62A H -0.0405 -0.0761 0.9967 0.107 Uiso 1 1 calc R . . H62B H -0.0703 -0.1016 0.9267 0.107 Uiso 1 1 calc R . . C63 C -0.1008(4) 0.0082(12) 1.0022(8) 0.099(5) Uani 1 1 d . . . H63A H -0.0904 0.0659 1.0382 0.119 Uiso 1 1 calc R . . H63B H -0.1193 0.0492 0.9664 0.119 Uiso 1 1 calc R . . C64 C -0.1284(5) -0.0767(12) 1.0419(8) 0.100(4) Uani 1 1 d . . . H64A H -0.1526 -0.0365 1.0659 0.150 Uiso 1 1 calc R . . H64B H -0.1109 -0.1166 1.0789 0.150 Uiso 1 1 calc R . . H64C H -0.1401 -0.1331 1.0069 0.150 Uiso 1 1 calc R . . N8 N 0.0000 0.0000 0.8724(7) 0.096(5) Uani 1 2 d S . . P1 P 0.4980(2) 0.5356(4) 0.8065(3) 0.0532(16) Uani 0.50 1 d P . . F1 F 0.5000 0.5000 0.8866(12) 0.219(9) Uiso 1 2 d S . . F2 F 0.5214(5) 0.4534(14) 0.7362(9) 0.111(5) Uiso 0.50 1 d P . . F3 F 0.4638(5) 0.6141(14) 0.8185(8) 0.214(6) Uiso 1 1 d . . . F4 F 0.5371(4) 0.5844(10) 0.8054(6) 0.160(4) Uiso 1 1 d . . . O3 O -0.0455(3) 0.4742(8) 1.2430(5) 0.089(2) Uiso 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 0.0402(3) 0.0367(3) 0.0305(3) -0.0100(3) 0.0052(3) -0.0049(3) Rh2 0.0322(3) 0.0397(3) 0.0323(3) -0.0067(3) 0.0022(2) -0.0015(2) I1 0.0406(3) 0.0610(4) 0.0382(3) 0.0029(3) -0.0013(2) 0.0031(3) I2 0.0428(3) 0.0685(4) 0.0554(4) -0.0054(3) 0.0094(3) 0.0126(3) I3 0.0498(3) 0.0477(3) 0.0493(3) -0.0100(3) -0.0084(3) -0.0103(3) C1 0.049(5) 0.041(5) 0.048(5) 0.000(4) 0.001(4) 0.003(4) O1 0.066(4) 0.044(4) 0.054(4) -0.007(3) 0.002(3) -0.005(3) C2 0.042(5) 0.049(5) 0.039(5) -0.012(4) 0.008(4) -0.005(4) O2 0.069(4) 0.057(4) 0.057(4) -0.025(4) -0.005(3) 0.004(4) N1 0.031(3) 0.059(4) 0.031(3) -0.011(3) 0.002(3) -0.012(3) N2 0.046(4) 0.050(4) 0.040(4) -0.015(3) 0.012(3) -0.005(3) N3 0.038(3) 0.052(4) 0.037(4) -0.011(3) 0.017(3) -0.006(3) N4 0.033(3) 0.038(3) 0.032(3) -0.007(3) 0.000(3) -0.003(3) N5 0.034(3) 0.035(3) 0.029(3) 0.002(3) -0.001(3) -0.006(3) N6 0.036(3) 0.038(3) 0.032(3) -0.011(3) 0.004(3) -0.006(3) C11 0.037(4) 0.060(6) 0.040(5) -0.020(4) 0.002(4) -0.008(4) C12 0.034(5) 0.108(9) 0.057(6) -0.015(6) 0.006(4) -0.003(5) C13 0.044(6) 0.129(11) 0.083(8) -0.043(8) -0.008(6) -0.001(6) C14 0.045(6) 0.122(10) 0.076(8) -0.035(7) 0.009(5) -0.030(6) C15 0.053(5) 0.067(6) 0.048(5) -0.021(5) 0.007(4) -0.013(5) C16 0.034(4) 0.065(6) 0.036(5) -0.013(4) 0.002(3) -0.004(4) C17 0.080(9) 0.196(17) 0.085(10) -0.062(11) -0.021(8) -0.040(10) C18 0.064(6) 0.046(5) 0.035(5) -0.020(4) 0.021(4) -0.016(4) C19 0.067(6) 0.102(8) 0.050(6) -0.029(6) 0.027(5) -0.043(6) C20 0.072(7) 0.097(9) 0.058(6) -0.029(7) 0.030(6) -0.034(7) C21 0.094(9) 0.036(5) 0.127(12) -0.017(6) 0.068(9) -0.013(6) C22 0.124(10) 0.056(6) 0.049(6) -0.001(5) 0.040(7) -0.007(7) C23 0.077(6) 0.052(5) 0.046(5) -0.010(5) 0.025(5) -0.018(5) C24 0.119(11) 0.085(9) 0.089(9) -0.028(7) 0.060(8) -0.030(8) C25 0.045(4) 0.032(4) 0.034(4) -0.008(3) 0.005(3) 0.000(3) C26 0.073(6) 0.048(5) 0.041(5) -0.013(4) 0.013(5) -0.020(5) C27 0.076(7) 0.038(5) 0.071(7) -0.006(5) 0.026(6) -0.008(5) C28 0.056(5) 0.039(5) 0.057(6) 0.005(4) 0.020(5) -0.003(4) C29 0.045(5) 0.049(5) 0.036(5) 0.002(4) 0.002(4) -0.001(4) C30 0.050(5) 0.043(5) 0.048(5) -0.011(4) 0.015(4) -0.002(4) C31 0.106(9) 0.050(6) 0.083(8) 0.015(6) 0.004(7) 0.002(6) C32 0.032(4) 0.037(4) 0.030(4) -0.006(3) 0.001(3) 0.000(3) C33 0.034(4) 0.036(4) 0.031(4) 0.000(3) -0.003(3) -0.005(3) C34 0.037(4) 0.048(5) 0.033(4) -0.013(4) -0.001(3) 0.006(4) C35 0.028(4) 0.058(5) 0.034(4) 0.009(4) 0.005(3) 0.003(4) C36 0.040(4) 0.041(4) 0.042(5) 0.008(4) 0.001(4) 0.000(4) C37 0.028(4) 0.048(5) 0.035(4) 0.001(4) 0.003(3) 0.000(3) C38 0.061(6) 0.070(6) 0.037(5) 0.004(5) 0.009(4) 0.013(5) N7 0.039(4) 0.044(4) 0.052(4) -0.005(3) 0.017(3) -0.002(3) C41 0.042(4) 0.052(5) 0.045(5) -0.005(4) 0.012(4) -0.001(4) C42 0.051(5) 0.053(5) 0.050(5) -0.001(4) 0.021(4) 0.003(4) C43 0.044(5) 0.041(4) 0.053(5) -0.003(4) 0.005(4) -0.001(4) C44 0.086(8) 0.061(6) 0.071(7) -0.011(6) 0.020(6) -0.004(6) C45 0.039(4) 0.054(5) 0.051(5) -0.003(4) 0.015(4) 0.001(4) C46 0.075(7) 0.054(6) 0.066(7) 0.000(5) 0.030(5) -0.009(5) C47 0.056(6) 0.053(5) 0.063(6) 0.002(5) 0.012(5) -0.005(5) C48 0.131(12) 0.058(7) 0.101(10) -0.007(7) 0.054(9) -0.024(7) C49 0.031(4) 0.061(6) 0.072(6) -0.005(5) 0.012(4) -0.007(4) C50 0.048(5) 0.065(6) 0.063(6) -0.005(5) 0.007(5) 0.001(5) C51 0.041(5) 0.072(7) 0.105(10) 0.007(7) -0.008(6) -0.009(5) C52 0.057(7) 0.110(10) 0.111(11) 0.002(9) -0.028(7) -0.026(7) C53 0.059(5) 0.039(4) 0.053(5) 0.001(4) 0.022(5) -0.003(4) C54 0.064(6) 0.055(5) 0.054(6) -0.008(5) 0.001(5) -0.008(5) C55 0.083(8) 0.082(8) 0.045(6) -0.011(5) 0.012(5) -0.014(6) C56 0.112(10) 0.072(7) 0.062(7) -0.027(6) 0.029(7) 0.001(7) C57 0.23(2) 0.165(17) 0.120(13) 0.083(13) 0.066(15) 0.125(18) C58 0.35(4) 0.25(3) 0.132(17) 0.12(2) 0.10(2) 0.14(3) C59 0.096(13) 0.062(10) 0.57(6) 0.01(2) 0.10(2) 0.004(9) C60 0.099(12) 0.145(16) 0.26(3) 0.039(17) 0.024(15) -0.071(12) C61 0.101(9) 0.065(7) 0.080(8) -0.007(6) -0.019(7) 0.032(7) C62 0.113(10) 0.079(8) 0.076(8) -0.025(7) -0.055(8) 0.033(8) C63 0.077(8) 0.094(10) 0.127(12) -0.035(9) -0.023(8) 0.040(8) C64 0.115(11) 0.092(10) 0.094(10) -0.002(8) 0.006(9) -0.008(9) N8 0.157(14) 0.075(9) 0.056(8) 0.000 0.000 0.071(10) P1 0.039(2) 0.073(5) 0.048(2) -0.003(2) 0.007(2) -0.013(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C2 1.875(9) . ? Rh1 N3 2.032(7) . ? Rh1 N6 2.070(6) . ? Rh1 Rh2 2.5764(9) . ? Rh1 I3 2.6404(9) . ? Rh2 C1 1.862(9) . ? Rh2 N4 2.090(6) . ? Rh2 N1 2.115(6) . ? Rh2 I2 2.6631(8) . ? Rh2 I1 2.7088(9) . ? C1 O1 1.137(10) . ? C2 O2 1.116(10) . ? N1 N2 1.275(9) . ? N1 C11 1.438(10) . ? N2 N3 1.305(9) . ? N3 C18 1.437(10) . ? N4 N5 1.303(8) . ? N4 C32 1.441(9) . ? N5 N6 1.270(8) . ? N6 C25 1.411(10) . ? C11 C12 1.373(12) . ? C11 C16 1.397(11) . ? C12 C13 1.367(14) . ? C12 H12A 0.9500 . ? C13 C14 1.414(15) . ? C13 H13A 0.9500 . ? C14 C15 1.379(13) . ? C14 C17 1.522(16) . ? C15 C16 1.382(12) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C23 1.355(13) . ? C18 C19 1.396(14) . ? C19 C20 1.376(13) . ? C19 H19A 0.9500 . ? C20 C21 1.355(18) . ? C20 H20A 0.9500 . ? C21 C22 1.454(18) . ? C21 C24 1.566(15) . ? C22 C23 1.397(13) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.407(11) . ? C25 C30 1.432(12) . ? C26 C27 1.379(14) . ? C26 H26A 0.9500 . ? C27 C28 1.387(14) . ? C27 H27A 0.9500 . ? C28 C29 1.412(12) . ? C28 C31 1.541(13) . ? C29 C30 1.347(12) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 H31C 0.9800 . ? C31 H31D 0.9800 . ? C31 H31E 0.9800 . ? C32 C37 1.402(11) . ? C32 C33 1.402(10) . ? C33 C34 1.385(10) . ? C33 H33C 0.9500 . ? C34 C35 1.371(12) . ? C34 H34D 0.9500 . ? C35 C36 1.404(12) . ? C35 C38 1.490(11) . ? C36 C37 1.379(11) . ? C36 H36C 0.9500 . ? C37 H37C 0.9500 . ? C38 H38D 0.9800 . ? C38 H38E 0.9800 . ? C38 H38F 0.9800 . ? N7 C53 1.510(11) . ? N7 C45 1.515(11) . ? N7 C41 1.519(10) . ? N7 C49 1.543(11) . ? C41 C42 1.502(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.536(12) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.560(13) . ? C43 H4A 0.9900 . ? C43 H4B 0.9900 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.496(12) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 C47 1.544(13) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.523(13) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.539(14) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.519(13) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.553(18) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.538(13) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 C55 1.563(13) . ? C54 H54A 0.9900 . ? C54 H54B 0.9900 . ? C55 C56 1.476(16) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 N8 1.490(18) . ? C57 C58 1.62(3) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 C59 1.55(3) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 C60 1.31(2) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 N8 1.490(14) . ? C61 C62 1.495(18) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.555(17) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.489(19) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? N8 C57 1.490(18) 2 ? N8 C61 1.490(14) 2 ? P1 P1 0.835(10) 2_665 ? P1 F4 1.327(14) . ? P1 F3 1.407(17) . ? P1 F2 1.420(17) 2_665 ? P1 F1 1.52(2) . ? P1 F2 1.752(17) . ? P1 F4 1.761(14) 2_665 ? P1 F3 2.107(18) 2_665 ? F1 P1 1.52(2) 2_665 ? F2 P1 1.420(17) 2_665 ? F2 F2 1.70(3) 2_665 ? F2 F3 1.75(2) 2_665 ? F3 F2 1.75(2) 2_665 ? F3 P1 2.107(18) 2_665 ? F4 P1 1.761(13) 2_665 ? 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 C2 Rh1 N3 95.1(3) . . ? C2 Rh1 N6 176.7(3) . . ? N3 Rh1 N6 88.1(3) . . ? C2 Rh1 Rh2 98.2(3) . . ? N3 Rh1 Rh2 83.3(2) . . ? N6 Rh1 Rh2 82.78(18) . . ? C2 Rh1 I3 88.5(2) . . ? N3 Rh1 I3 173.4(2) . . ? N6 Rh1 I3 88.22(16) . . ? Rh2 Rh1 I3 101.68(3) . . ? C1 Rh2 N4 98.1(3) . . ? C1 Rh2 N1 173.4(3) . . ? N4 Rh2 N1 87.3(2) . . ? C1 Rh2 Rh1 95.4(3) . . ? N4 Rh2 Rh1 82.38(17) . . ? N1 Rh2 Rh1 81.36(18) . . ? C1 Rh2 I2 87.1(3) . . ? N4 Rh2 I2 174.49(17) . . ? N1 Rh2 I2 87.37(18) . . ? Rh1 Rh2 I2 95.44(3) . . ? C1 Rh2 I1 85.7(3) . . ? N4 Rh2 I1 94.16(17) . . ? N1 Rh2 I1 97.87(18) . . ? Rh1 Rh2 I1 176.49(3) . . ? I2 Rh2 I1 87.94(3) . . ? O1 C1 Rh2 178.1(9) . . ? O2 C2 Rh1 175.5(8) . . ? N2 N1 C11 111.3(6) . . ? N2 N1 Rh2 121.9(5) . . ? C11 N1 Rh2 122.1(5) . . ? N1 N2 N3 115.7(6) . . ? N2 N3 C18 113.4(6) . . ? N2 N3 Rh1 125.2(5) . . ? C18 N3 Rh1 121.4(5) . . ? N5 N4 C32 111.0(6) . . ? N5 N4 Rh2 122.1(5) . . ? C32 N4 Rh2 126.0(5) . . ? N6 N5 N4 117.1(6) . . ? N5 N6 C25 114.9(6) . . ? N5 N6 Rh1 124.3(5) . . ? C25 N6 Rh1 120.5(5) . . ? C12 C11 C16 118.6(8) . . ? C12 C11 N1 122.5(8) . . ? C16 C11 N1 118.9(7) . . ? C13 C12 C11 121.3(9) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C12 C13 C14 121.3(9) . . ? C12 C13 H13A 119.3 . . ? C14 C13 H13A 119.3 . . ? C15 C14 C13 116.6(10) . . ? C15 C14 C17 120.4(10) . . ? C13 C14 C17 122.9(10) . . ? C14 C15 C16 122.3(9) . . ? C14 C15 H15A 118.9 . . ? C16 C15 H15A 118.9 . . ? C15 C16 C11 119.9(8) . . ? C15 C16 H16A 120.0 . . ? C11 C16 H16A 120.0 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.1(8) . . ? C23 C18 N3 119.4(8) . . ? C19 C18 N3 120.3(8) . . ? C20 C19 C18 119.7(11) . . ? C20 C19 H19A 120.1 . . ? C18 C19 H19A 120.1 . . ? C21 C20 C19 120.7(11) . . ? C21 C20 H20A 119.7 . . ? C19 C20 H20A 119.7 . . ? C20 C21 C22 121.2(10) . . ? C20 C21 C24 124.6(12) . . ? C22 C21 C24 114.2(13) . . ? C23 C22 C21 115.4(11) . . ? C23 C22 H22A 122.3 . . ? C21 C22 H22A 122.3 . . ? C18 C23 C22 122.8(10) . . ? C18 C23 H23A 118.6 . . ? C22 C23 H23A 118.6 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 N6 121.8(7) . . ? C26 C25 C30 117.3(8) . . ? N6 C25 C30 120.9(7) . . ? C27 C26 C25 120.2(9) . . ? C27 C26 H26A 119.9 . . ? C25 C26 H26A 119.9 . . ? C26 C27 C28 122.9(9) . . ? C26 C27 H27A 118.6 . . ? C28 C27 H27A 118.6 . . ? C27 C28 C29 116.2(8) . . ? C27 C28 C31 122.9(9) . . ? C29 C28 C31 120.9(9) . . ? C30 C29 C28 122.9(8) . . ? C30 C29 H29A 118.5 . . ? C28 C29 H29A 118.5 . . ? C29 C30 C25 120.4(8) . . ? C29 C30 H30A 119.8 . . ? C25 C30 H30A 119.8 . . ? C28 C31 H31C 109.5 . . ? C28 C31 H31D 109.5 . . ? H31C C31 H31D 109.5 . . ? C28 C31 H31E 109.5 . . ? H31C C31 H31E 109.5 . . ? H31D C31 H31E 109.5 . . ? C37 C32 C33 118.7(7) . . ? C37 C32 N4 119.7(6) . . ? C33 C32 N4 121.6(7) . . ? C34 C33 C32 118.6(7) . . ? C34 C33 H33C 120.7 . . ? C32 C33 H33C 120.7 . . ? C35 C34 C33 123.9(7) . . ? C35 C34 H34D 118.1 . . ? C33 C34 H34D 118.1 . . ? C34 C35 C36 116.9(7) . . ? C34 C35 C38 122.3(8) . . ? C36 C35 C38 120.7(8) . . ? C37 C36 C35 121.2(8) . . ? C37 C36 H36C 119.4 . . ? C35 C36 H36C 119.4 . . ? C36 C37 C32 120.8(7) . . ? C36 C37 H37C 119.6 . . ? C32 C37 H37C 119.6 . . ? C35 C38 H38D 109.5 . . ? C35 C38 H38E 109.5 . . ? H38D C38 H38E 109.5 . . ? C35 C38 H38F 109.5 . . ? H38D C38 H38F 109.5 . . ? H38E C38 H38F 109.5 . . ? C53 N7 C45 111.4(7) . . ? C53 N7 C41 111.3(6) . . ? C45 N7 C41 108.9(6) . . ? C53 N7 C49 105.2(6) . . ? C45 N7 C49 110.8(7) . . ? C41 N7 C49 109.3(7) . . ? C42 C41 N7 118.1(7) . . ? C42 C41 H41A 107.8 . . ? N7 C41 H41A 107.8 . . ? C42 C41 H41B 107.8 . . ? N7 C41 H41B 107.8 . . ? H41A C41 H41B 107.1 . . ? C41 C42 C43 110.6(7) . . ? C41 C42 H42A 109.5 . . ? C43 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 108.1 . . ? C42 C43 C44 112.3(8) . . ? C42 C43 H4A 109.1 . . ? C44 C43 H4A 109.1 . . ? C42 C43 H4B 109.1 . . ? C44 C43 H4B 109.1 . . ? H4A C43 H4B 107.9 . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C46 C45 N7 114.8(7) . . ? C46 C45 H45A 108.6 . . ? N7 C45 H45A 108.6 . . ? C46 C45 H45B 108.6 . . ? N7 C45 H45B 108.6 . . ? H45A C45 H45B 107.5 . . ? C45 C46 C47 109.9(7) . . ? C45 C46 H46A 109.7 . . ? C47 C46 H46A 109.7 . . ? C45 C46 H46B 109.7 . . ? C47 C46 H46B 109.7 . . ? H46A C46 H46B 108.2 . . ? C48 C47 C46 112.8(8) . . ? C48 C47 H47A 109.0 . . ? C46 C47 H47A 109.0 . . ? C48 C47 H47B 109.0 . . ? C46 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C50 C49 N7 115.6(7) . . ? C50 C49 H49A 108.4 . . ? N7 C49 H49A 108.4 . . ? C50 C49 H49B 108.4 . . ? N7 C49 H49B 108.4 . . ? H49A C49 H49B 107.4 . . ? C51 C50 C49 107.4(8) . . ? C51 C50 H50A 110.2 . . ? C49 C50 H50A 110.2 . . ? C51 C50 H50B 110.2 . . ? C49 C50 H50B 110.2 . . ? H50A C50 H50B 108.5 . . ? C50 C51 C52 109.9(9) . . ? C50 C51 H51A 109.7 . . ? C52 C51 H51A 109.7 . . ? C50 C51 H51B 109.7 . . ? C52 C51 H51B 109.7 . . ? H51A C51 H51B 108.2 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N7 C53 C54 115.1(7) . . ? N7 C53 H53A 108.5 . . ? C54 C53 H53A 108.5 . . ? N7 C53 H53B 108.5 . . ? C54 C53 H53B 108.5 . . ? H53A C53 H53B 107.5 . . ? C53 C54 C55 111.7(8) . . ? C53 C54 H54A 109.3 . . ? C55 C54 H54A 109.3 . . ? C53 C54 H54B 109.3 . . ? C55 C54 H54B 109.3 . . ? H54A C54 H54B 107.9 . . ? C56 C55 C54 112.7(9) . . ? C56 C55 H55A 109.0 . . ? C54 C55 H55A 109.0 . . ? C56 C55 H55B 109.0 . . ? C54 C55 H55B 109.0 . . ? H55A C55 H55B 107.8 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N8 C57 C58 111.8(13) . . ? N8 C57 H57A 109.3 . . ? C58 C57 H57A 109.3 . . ? N8 C57 H57B 109.3 . . ? C58 C57 H57B 109.3 . . ? H57A C57 H57B 107.9 . . ? C59 C58 C57 102.6(18) . . ? C59 C58 H58A 111.3 . . ? C57 C58 H58A 111.3 . . ? C59 C58 H58B 111.3 . . ? C57 C58 H58B 111.3 . . ? H58A C58 H58B 109.2 . . ? C60 C59 C58 99(2) . . ? C60 C59 H59A 112.0 . . ? C58 C59 H59A 112.0 . . ? C60 C59 H59B 112.0 . . ? C58 C59 H59B 112.0 . . ? H59A C59 H59B 109.6 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N8 C61 C62 113.8(9) . . ? N8 C61 H61A 108.8 . . ? C62 C61 H61A 108.8 . . ? N8 C61 H61B 108.8 . . ? C62 C61 H61B 108.8 . . ? H61A C61 H61B 107.7 . . ? C61 C62 C63 113.9(10) . . ? C61 C62 H62A 108.8 . . ? C63 C62 H62A 108.8 . . ? C61 C62 H62B 108.8 . . ? C63 C62 H62B 108.8 . . ? H62A C62 H62B 107.7 . . ? C64 C63 C62 116.8(11) . . ? C64 C63 H63A 108.1 . . ? C62 C63 H63A 108.1 . . ? C64 C63 H63B 108.1 . . ? C62 C63 H63B 108.1 . . ? H63A C63 H63B 107.3 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C57 N8 C57 108(2) 2 . ? C57 N8 C61 110.8(10) 2 . ? C57 N8 C61 107.4(8) . . ? C57 N8 C61 107.4(8) 2 2 ? C57 N8 C61 110.8(10) . 2 ? C61 N8 C61 112.3(13) . 2 ? P1 P1 F4 106.9(12) 2_665 . ? P1 P1 F3 138.5(12) 2_665 . ? F4 P1 F3 113.6(8) . . ? P1 P1 F2 98.7(8) 2_665 2_665 ? F4 P1 F2 109.1(9) . 2_665 ? F3 P1 F2 76.6(9) . 2_665 ? P1 P1 F1 74.0(3) 2_665 . ? F4 P1 F1 95.5(6) . . ? F3 P1 F1 93.3(7) . . ? F2 P1 F1 155.5(8) 2_665 . ? P1 P1 F2 53.2(6) 2_665 . ? F4 P1 F2 81.4(8) . . ? F3 P1 F2 140.5(9) . . ? F2 P1 F2 63.9(12) 2_665 . ? F1 P1 F2 122.6(7) . . ? P1 P1 F4 46.1(8) 2_665 2_665 ? F4 P1 F4 153.0(5) . 2_665 ? F3 P1 F4 93.2(8) . 2_665 ? F2 P1 F4 78.7(8) 2_665 2_665 ? F1 P1 F4 79.7(5) . 2_665 ? F2 P1 F4 79.1(7) . 2_665 ? P1 P1 F3 26.3(8) 2_665 2_665 ? F4 P1 F3 81.4(7) . 2_665 ? F3 P1 F3 158.9(9) . 2_665 ? F2 P1 F3 113.7(9) 2_665 2_665 ? F1 P1 F3 69.8(5) . 2_665 ? F2 P1 F3 53.0(7) . 2_665 ? F4 P1 F3 71.9(5) 2_665 2_665 ? P1 F1 P1 31.9(6) 2_665 . ? P1 F2 F2 67.6(7) 2_665 2_665 ? P1 F2 F3 51.4(8) 2_665 2_665 ? F2 F2 F3 119.0(8) 2_665 2_665 ? P1 F2 P1 28.1(5) 2_665 . ? F2 F2 P1 48.5(6) 2_665 . ? F3 F2 P1 73.9(9) 2_665 . ? P1 F3 F2 52.0(8) . 2_665 ? P1 F3 P1 15.2(4) . 2_665 ? F2 F3 P1 53.1(7) 2_665 2_665 ? P1 F4 P1 27.0(5) . 2_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.081 _refine_diff_density_min -0.743 _refine_diff_density_rms 0.189 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 633934' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 I4 Ir2 N6 O4, C H2 Cl2' _chemical_formula_sum 'C33 H32 Cl2 I4 Ir2 N6 O4' _chemical_formula_weight 1539.55 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' O O 0.0106 0.0060 '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' 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 8.9001(15) _cell_length_b 9.642(2) _cell_length_c 13.510(5) _cell_angle_alpha 94.177(18) _cell_angle_beta 100.254(14) _cell_angle_gamma 98.35(2) _cell_volume 1123.0(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 8.827 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .257 _exptl_absorpt_correction_T_max .492 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 11700 _diffrn_reflns_av_R_equivalents 0.0311 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.15 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5076 _reflns_number_gt 3926 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0612P)^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 5076 _refine_ls_number_parameters 247 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0969 _refine_ls_wR_factor_gt 0.0924 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _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 0.58645(2) 0.99800(2) 0.871547(15) 0.02392(8) Uani 1 1 d . . . I1 I 0.31885(4) 1.04379(4) 0.92230(3) 0.02698(11) Uani 1 1 d . . . I2 I 0.85549(5) 0.95767(4) 0.82484(3) 0.03522(12) Uani 1 1 d . . . O1 O 0.4776(6) 0.6877(5) 0.8207(4) 0.0469(12) Uani 1 1 d . . . O2 O 0.4377(5) 0.9562(4) 0.6586(3) 0.0385(11) Uani 1 1 d . . . N1 N 0.5284(6) 1.1847(5) 0.7231(3) 0.0296(11) Uani 1 1 d . . . N2 N 0.6075(5) 1.2727(5) 0.8018(3) 0.0262(10) Uani 1 1 d . . . H2A H 0.6263 1.3644 0.7994 0.031 Uiso 1 1 calc R . . N3 N 0.6541(5) 1.2141(5) 0.8814(3) 0.0243(10) Uani 1 1 d . . . C1 C 0.5174(7) 0.8009(7) 0.8417(5) 0.0320(13) Uani 1 1 d . . . C2 C 0.5047(6) 1.0331(6) 0.7310(4) 0.0283(12) Uani 1 1 d . . . C11 C 0.4590(7) 1.2489(6) 0.6372(4) 0.0309(13) Uani 1 1 d . . . C12 C 0.3726(8) 1.3565(7) 0.6535(5) 0.0381(15) Uani 1 1 d . . . H12A H 0.3604 1.3864 0.7198 0.046 Uiso 1 1 calc R . . C13 C 0.3068(8) 1.4167(8) 0.5722(5) 0.0475(18) Uani 1 1 d . . . H13A H 0.2468 1.4884 0.5825 0.057 Uiso 1 1 calc R . . C14 C 0.3244(8) 1.3766(7) 0.4739(5) 0.0453(17) Uani 1 1 d . . . C15 C 0.4101(9) 1.2700(7) 0.4615(5) 0.0452(17) Uani 1 1 d . . . H15A H 0.4214 1.2389 0.3952 0.054 Uiso 1 1 calc R . . C16 C 0.4790(8) 1.2078(7) 0.5415(5) 0.0386(15) Uani 1 1 d . . . H16A H 0.5401 1.1370 0.5310 0.046 Uiso 1 1 calc R . . C17 C 0.2536(10) 1.4484(9) 0.3834(6) 0.060(2) Uani 1 1 d . . . H17A H 0.3173 1.4455 0.3314 0.091 Uiso 1 1 calc R . . H17B H 0.2494 1.5466 0.4055 0.091 Uiso 1 1 calc R . . H17C H 0.1487 1.3989 0.3556 0.091 Uiso 1 1 calc R . . C18 C 0.7339(6) 1.3153(6) 0.9640(4) 0.0261(12) Uani 1 1 d . . . C19 C 0.6802(7) 1.4393(6) 0.9823(4) 0.0301(13) Uani 1 1 d . . . H19A H 0.5886 1.4577 0.9409 0.036 Uiso 1 1 calc R . . C20 C 0.7598(7) 1.5384(6) 1.0616(4) 0.0322(13) Uani 1 1 d . . . H20A H 0.7219 1.6239 1.0740 0.039 Uiso 1 1 calc R . . C21 C 0.8945(7) 1.5130(6) 1.1226(4) 0.0308(13) Uani 1 1 d . . . C22 C 0.9480(7) 1.3871(6) 1.1029(4) 0.0286(12) Uani 1 1 d . . . H22A H 1.0401 1.3686 1.1437 0.034 Uiso 1 1 calc R . . C23 C 0.8678(6) 1.2879(6) 1.0240(4) 0.0285(12) Uani 1 1 d . . . H23A H 0.9046 1.2019 1.0113 0.034 Uiso 1 1 calc R . . C24 C 0.9797(8) 1.6190(7) 1.2108(5) 0.0402(15) Uani 1 1 d . . . H24A H 1.0908 1.6333 1.2100 0.060 Uiso 1 1 calc R . . H24B H 0.9621 1.5832 1.2745 0.060 Uiso 1 1 calc R . . H24C H 0.9413 1.7088 1.2047 0.060 Uiso 1 1 calc R . . C99 C 0.0637(13) 0.8684(13) 0.5922(8) 0.031(3) Uani 0.50 1 d P . . H99A H 0.1221 0.9640 0.6157 0.038 Uiso 0.50 1 calc PR . . H99B H -0.0472 0.8706 0.5922 0.038 Uiso 0.50 1 calc PR . . Cl1 Cl 0.1317(5) 0.7455(5) 0.6745(4) 0.0803(14) Uani 0.50 1 d P . . Cl2 Cl 0.0897(6) 0.8163(7) 0.4660(4) 0.103(2) Uani 0.50 1 d P . . 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 0.02531(13) 0.02136(13) 0.02574(13) 0.00219(8) 0.00535(9) 0.00537(9) I1 0.02387(19) 0.0292(2) 0.0295(2) 0.00699(16) 0.00529(15) 0.00745(16) I2 0.0319(2) 0.0357(2) 0.0420(2) 0.00185(18) 0.01366(18) 0.01139(18) O1 0.066(3) 0.025(3) 0.048(3) 0.002(2) 0.012(2) 0.002(2) O2 0.050(3) 0.031(2) 0.028(2) -0.0026(18) -0.0012(19) -0.001(2) N1 0.036(3) 0.027(3) 0.023(2) 0.001(2) -0.001(2) 0.006(2) N2 0.031(2) 0.020(2) 0.029(2) 0.0045(19) 0.0058(19) 0.0047(19) N3 0.025(2) 0.026(3) 0.024(2) 0.0066(19) 0.0056(18) 0.007(2) C1 0.034(3) 0.029(4) 0.035(3) 0.008(3) 0.009(3) 0.006(3) C2 0.025(3) 0.031(3) 0.030(3) 0.001(2) 0.006(2) 0.007(2) C11 0.033(3) 0.032(3) 0.027(3) 0.006(2) 0.002(2) 0.005(3) C12 0.044(4) 0.043(4) 0.031(3) 0.006(3) 0.008(3) 0.013(3) C13 0.049(4) 0.050(5) 0.048(4) 0.009(3) 0.006(3) 0.023(4) C14 0.049(4) 0.040(4) 0.039(4) 0.014(3) -0.011(3) -0.002(3) C15 0.060(5) 0.042(4) 0.029(3) 0.006(3) -0.001(3) 0.005(3) C16 0.047(4) 0.034(4) 0.035(3) 0.006(3) 0.008(3) 0.007(3) C17 0.071(6) 0.054(5) 0.048(4) 0.017(4) -0.012(4) 0.006(4) C18 0.027(3) 0.023(3) 0.028(3) 0.006(2) 0.006(2) 0.000(2) C19 0.030(3) 0.030(3) 0.031(3) 0.004(2) 0.001(2) 0.008(3) C20 0.036(3) 0.024(3) 0.036(3) 0.004(2) 0.006(3) 0.006(3) C21 0.033(3) 0.032(3) 0.026(3) 0.005(2) 0.007(2) 0.000(3) C22 0.030(3) 0.030(3) 0.026(3) 0.009(2) 0.001(2) 0.007(2) C23 0.027(3) 0.027(3) 0.032(3) 0.006(2) 0.005(2) 0.008(2) C24 0.042(4) 0.035(4) 0.038(3) 0.000(3) 0.000(3) 0.000(3) C99 0.020(6) 0.037(7) 0.033(6) 0.003(5) 0.002(5) -0.005(5) Cl1 0.057(3) 0.074(3) 0.109(4) 0.022(3) 0.019(3) -0.001(2) Cl2 0.074(3) 0.155(6) 0.070(3) -0.032(4) 0.008(3) 0.015(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ir1 C1 1.901(7) . ? Ir1 C2 1.980(6) . ? Ir1 N3 2.071(5) . ? Ir1 I2 2.6562(6) . ? Ir1 I1 2.6795(6) . ? Ir1 I1 2.8384(11) 2_677 ? I1 Ir1 2.8384(11) 2_677 ? O1 C1 1.097(7) . ? O2 C2 1.193(6) . ? N1 N2 1.331(6) . ? N1 C11 1.439(7) . ? N1 C2 1.461(7) . ? N2 N3 1.283(6) . ? N3 C18 1.435(7) . ? C11 C16 1.375(8) . ? C11 C12 1.405(8) . ? C12 C13 1.361(9) . ? C13 C14 1.398(10) . ? C14 C15 1.384(9) . ? C14 C17 1.531(9) . ? C15 C16 1.367(8) . ? C18 C19 1.372(8) . ? C18 C23 1.388(7) . ? C19 C20 1.396(8) . ? C20 C21 1.393(8) . ? C21 C22 1.392(7) . ? C21 C24 1.522(8) . ? C22 C23 1.395(8) . ? C99 Cl1 1.780(12) . ? C99 Cl2 1.805(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ir1 C2 91.7(2) . . ? C1 Ir1 N3 171.6(2) . . ? C2 Ir1 N3 80.0(2) . . ? C1 Ir1 I2 88.29(19) . . ? C2 Ir1 I2 91.58(16) . . ? N3 Ir1 I2 90.34(12) . . ? C1 Ir1 I1 92.89(19) . . ? C2 Ir1 I1 89.22(16) . . ? N3 Ir1 I1 88.61(12) . . ? I2 Ir1 I1 178.558(15) . . ? C1 Ir1 I1 89.35(18) . 2_677 ? C2 Ir1 I1 175.08(15) . 2_677 ? N3 Ir1 I1 98.98(12) . 2_677 ? I2 Ir1 I1 93.25(2) . 2_677 ? I1 Ir1 I1 85.93(2) . 2_677 ? Ir1 I1 Ir1 94.07(2) . 2_677 ? N2 N1 C11 116.1(5) . . ? N2 N1 C2 119.8(4) . . ? C11 N1 C2 123.8(5) . . ? N3 N2 N1 115.2(5) . . ? N2 N3 C18 112.2(4) . . ? N2 N3 Ir1 115.5(4) . . ? C18 N3 Ir1 132.1(3) . . ? O1 C1 Ir1 177.3(6) . . ? O2 C2 N1 118.6(5) . . ? O2 C2 Ir1 132.2(5) . . ? N1 C2 Ir1 109.2(4) . . ? C16 C11 C12 120.6(5) . . ? C16 C11 N1 120.8(5) . . ? C12 C11 N1 118.5(5) . . ? C13 C12 C11 118.4(6) . . ? C12 C13 C14 122.3(6) . . ? C15 C14 C13 117.3(6) . . ? C15 C14 C17 121.1(7) . . ? C13 C14 C17 121.6(7) . . ? C16 C15 C14 122.1(7) . . ? C15 C16 C11 119.3(6) . . ? C19 C18 C23 120.3(5) . . ? C19 C18 N3 120.4(5) . . ? C23 C18 N3 119.3(5) . . ? C18 C19 C20 120.1(5) . . ? C21 C20 C19 120.5(5) . . ? C22 C21 C20 118.7(5) . . ? C22 C21 C24 120.4(5) . . ? C20 C21 C24 120.8(5) . . ? C21 C22 C23 120.7(5) . . ? C18 C23 C22 119.7(5) . . ? Cl1 C99 Cl2 108.9(7) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.892 _refine_diff_density_min -2.963 _refine_diff_density_rms 0.200 #===END data_8 _database_code_depnum_ccdc_archive 'CCDC 633935' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H29 I2 N3 O P Rh' _chemical_formula_weight 871.27 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' O O 0.0106 0.0060 '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' Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.252(2) _cell_length_b 18.050(3) _cell_length_c 19.716(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.006(14) _cell_angle_gamma 90.00 _cell_volume 3268.1(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.771 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1688 _exptl_absorpt_coefficient_mu 2.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5 _exptl_absorpt_correction_T_max 0.679 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 21320 _diffrn_reflns_av_R_equivalents 0.0935 _diffrn_reflns_av_sigmaI/netI 0.1223 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 27.55 _reflns_number_total 7520 _reflns_number_gt 4285 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0165P)^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 7520 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.0750 _refine_ls_wR_factor_gt 0.0624 _refine_ls_goodness_of_fit_ref 0.876 _refine_ls_restrained_S_all 0.876 _refine_ls_shift/su_max 0.011 _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 0.77800(5) 0.88581(2) 0.77098(2) 0.02158(11) Uani 1 1 d . . . C1 C 0.8948(6) 0.9336(3) 0.7128(3) 0.0286(14) Uani 1 1 d . . . O1 O 0.9662(4) 0.9640(2) 0.6808(2) 0.0382(11) Uani 1 1 d . . . I1 I 1.03173(4) 0.82478(2) 0.82647(2) 0.03172(11) Uani 1 1 d . . . I2 I 0.74866(4) 0.78004(2) 0.67505(2) 0.03410(11) Uani 1 1 d . . . P1 P 0.55800(16) 0.94392(8) 0.72662(8) 0.0257(4) Uani 1 1 d . . . N1 N 0.7866(5) 0.9484(2) 0.8581(2) 0.0271(11) Uani 1 1 d . . . N2 N 0.7148(5) 0.9050(3) 0.8952(2) 0.0282(12) Uani 1 1 d . . . N3 N 0.6749(5) 0.8483(3) 0.8536(2) 0.0275(11) Uani 1 1 d . . . C11 C 0.8546(6) 1.0129(3) 0.8885(3) 0.0287(14) Uani 1 1 d . . . C12 C 0.8349(8) 1.0354(4) 0.9541(3) 0.063(2) Uani 1 1 d . . . H12A H 0.7774 1.0064 0.9808 0.076 Uiso 1 1 calc R . . C13 C 0.8986(9) 1.0994(4) 0.9803(3) 0.067(2) Uani 1 1 d . . . H13A H 0.8833 1.1142 1.0251 0.081 Uiso 1 1 calc R . . C14 C 0.9841(6) 1.1433(3) 0.9441(3) 0.0346(16) Uani 1 1 d . . . C15 C 0.9997(6) 1.1205(3) 0.8790(3) 0.0396(16) Uani 1 1 d . . . H15A H 1.0561 1.1501 0.8522 0.047 Uiso 1 1 calc R . . C16 C 0.9365(6) 1.0563(3) 0.8507(3) 0.0352(15) Uani 1 1 d . . . H16A H 0.9498 1.0423 0.8055 0.042 Uiso 1 1 calc R . . C17 C 1.0532(7) 1.2136(3) 0.9733(3) 0.0498(19) Uani 1 1 d . . . H17A H 1.0795 1.2449 0.9361 0.075 Uiso 1 1 calc R . . H17B H 1.1410 1.2015 1.0044 0.075 Uiso 1 1 calc R . . H17C H 0.9842 1.2401 0.9985 0.075 Uiso 1 1 calc R . . C18 C 0.5958(6) 0.7911(3) 0.8806(3) 0.0314(15) Uani 1 1 d . . . C19 C 0.5056(6) 0.8051(4) 0.9310(3) 0.0429(17) Uani 1 1 d . . . H19A H 0.4958 0.8539 0.9479 0.051 Uiso 1 1 calc R . . C20 C 0.4301(7) 0.7464(4) 0.9562(3) 0.051(2) Uani 1 1 d . . . H20A H 0.3705 0.7557 0.9913 0.061 Uiso 1 1 calc R . . C21 C 0.4395(7) 0.6756(4) 0.9319(4) 0.0497(19) Uani 1 1 d . . . C22 C 0.5287(7) 0.6630(4) 0.8814(4) 0.0504(19) Uani 1 1 d . . . H22A H 0.5366 0.6143 0.8639 0.060 Uiso 1 1 calc R . . C23 C 0.6075(6) 0.7207(3) 0.8558(3) 0.0376(16) Uani 1 1 d . . . H23A H 0.6687 0.7111 0.8214 0.045 Uiso 1 1 calc R . . C24 C 0.3566(8) 0.6131(4) 0.9590(4) 0.081(3) Uani 1 1 d . . . H24A H 0.3734 0.6131 1.0090 0.121 Uiso 1 1 calc R . . H24B H 0.3898 0.5659 0.9417 0.121 Uiso 1 1 calc R . . H24C H 0.2524 0.6193 0.9440 0.121 Uiso 1 1 calc R . . C25 C 0.4111(6) 0.8840(3) 0.6890(3) 0.0271(13) Uani 1 1 d . . . C26 C 0.3865(6) 0.8151(3) 0.7171(3) 0.0318(15) Uani 1 1 d . . . H26A H 0.4511 0.7972 0.7547 0.038 Uiso 1 1 calc R . . C27 C 0.2687(6) 0.7724(4) 0.6907(3) 0.0377(16) Uani 1 1 d . . . H27A H 0.2522 0.7255 0.7103 0.045 Uiso 1 1 calc R . . C28 C 0.1751(7) 0.7980(4) 0.6357(3) 0.0452(18) Uani 1 1 d . . . H28A H 0.0944 0.7686 0.6175 0.054 Uiso 1 1 calc R . . C29 C 0.1984(6) 0.8660(4) 0.6072(3) 0.0442(18) Uani 1 1 d . . . H29A H 0.1341 0.8829 0.5691 0.053 Uiso 1 1 calc R . . C30 C 0.3152(6) 0.9099(4) 0.6337(3) 0.0353(16) Uani 1 1 d . . . H30A H 0.3298 0.9571 0.6144 0.042 Uiso 1 1 calc R . . C31 C 0.5824(6) 1.0085(3) 0.6585(3) 0.0268(14) Uani 1 1 d . . . C32 C 0.6442(6) 0.9823(3) 0.6021(3) 0.0305(14) Uani 1 1 d . . . H32A H 0.6746 0.9321 0.6012 0.037 Uiso 1 1 calc R . . C33 C 0.6621(6) 1.0284(3) 0.5470(3) 0.0360(16) Uani 1 1 d . . . H33A H 0.7059 1.0097 0.5093 0.043 Uiso 1 1 calc R . . C34 C 0.6165(6) 1.1008(3) 0.5472(3) 0.0368(16) Uani 1 1 d . . . H34A H 0.6294 1.1327 0.5101 0.044 Uiso 1 1 calc R . . C35 C 0.5523(7) 1.1265(3) 0.6017(3) 0.0407(17) Uani 1 1 d . . . H35A H 0.5187 1.1763 0.6016 0.049 Uiso 1 1 calc R . . C36 C 0.5352(6) 1.0809(3) 0.6574(3) 0.0338(15) Uani 1 1 d . . . H36A H 0.4908 1.0999 0.6948 0.041 Uiso 1 1 calc R . . C37 C 0.4814(6) 0.9955(3) 0.7924(3) 0.0260(14) Uani 1 1 d . . . C38 C 0.3609(6) 0.9676(3) 0.8209(3) 0.0305(14) Uani 1 1 d . . . H38A H 0.3142 0.9237 0.8029 0.037 Uiso 1 1 calc R . . C39 C 0.3102(6) 1.0035(4) 0.8745(3) 0.0405(17) Uani 1 1 d . . . H39A H 0.2296 0.9835 0.8939 0.049 Uiso 1 1 calc R . . C40 C 0.3743(7) 1.0682(4) 0.9008(3) 0.0427(17) Uani 1 1 d . . . H40A H 0.3375 1.0928 0.9377 0.051 Uiso 1 1 calc R . . C41 C 0.4931(6) 1.0968(3) 0.8727(3) 0.0360(16) Uani 1 1 d . . . H41A H 0.5383 1.1411 0.8904 0.043 Uiso 1 1 calc R . . C42 C 0.5455(6) 1.0607(3) 0.8192(3) 0.0313(15) Uani 1 1 d . . . H42A H 0.6266 1.0807 0.8002 0.038 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 0.0247(2) 0.0186(2) 0.0221(2) -0.0003(2) 0.00533(18) -0.0021(2) C1 0.030(4) 0.026(4) 0.029(4) -0.008(3) 0.000(3) 0.000(3) O1 0.040(3) 0.041(3) 0.037(3) 0.003(2) 0.015(2) -0.004(2) I1 0.0297(2) 0.0322(2) 0.0332(2) 0.00351(19) 0.00361(17) 0.0013(2) I2 0.0367(2) 0.0288(2) 0.0370(2) -0.0100(2) 0.00549(18) 0.0008(2) P1 0.0252(8) 0.0244(9) 0.0280(9) -0.0013(7) 0.0057(7) 0.0001(7) N1 0.034(3) 0.022(3) 0.026(3) 0.002(2) 0.008(2) -0.009(2) N2 0.031(3) 0.025(3) 0.029(3) 0.002(2) 0.002(2) -0.001(2) N3 0.028(3) 0.028(3) 0.027(3) -0.004(2) 0.006(2) -0.005(2) C11 0.029(3) 0.020(3) 0.037(4) 0.000(3) 0.003(3) 0.000(3) C12 0.109(7) 0.058(5) 0.027(4) -0.008(4) 0.024(4) -0.052(5) C13 0.127(7) 0.061(6) 0.014(3) -0.016(3) 0.010(4) -0.047(5) C14 0.041(4) 0.027(4) 0.031(4) -0.003(3) -0.011(3) -0.008(3) C15 0.045(4) 0.024(4) 0.051(4) 0.000(3) 0.010(3) -0.008(3) C16 0.042(4) 0.030(4) 0.034(4) -0.007(3) 0.010(3) -0.008(3) C17 0.075(5) 0.036(4) 0.036(4) -0.007(3) -0.003(4) -0.018(4) C18 0.030(3) 0.030(4) 0.034(4) 0.005(3) 0.001(3) -0.007(3) C19 0.043(4) 0.048(5) 0.038(4) 0.003(3) 0.008(3) -0.014(3) C20 0.039(4) 0.071(6) 0.044(4) 0.009(4) 0.011(3) -0.022(4) C21 0.043(4) 0.055(5) 0.047(5) 0.020(4) -0.009(4) -0.017(4) C22 0.060(5) 0.022(4) 0.066(5) 0.008(4) -0.004(4) -0.008(4) C23 0.043(4) 0.029(4) 0.042(4) 0.013(3) 0.006(3) 0.001(3) C24 0.070(6) 0.074(6) 0.092(7) 0.047(5) -0.021(5) -0.044(5) C25 0.027(3) 0.024(3) 0.031(3) -0.007(3) 0.005(3) 0.002(3) C26 0.031(3) 0.031(4) 0.034(4) -0.008(3) 0.008(3) -0.004(3) C27 0.036(4) 0.040(4) 0.040(4) -0.013(3) 0.013(3) 0.001(3) C28 0.028(4) 0.053(5) 0.057(5) -0.014(4) 0.014(3) -0.008(3) C29 0.031(4) 0.059(5) 0.040(4) -0.006(4) -0.006(3) 0.000(4) C30 0.032(3) 0.045(4) 0.029(3) 0.001(3) 0.004(3) -0.002(3) C31 0.032(3) 0.028(4) 0.021(3) 0.005(3) 0.003(3) 0.001(3) C32 0.045(4) 0.021(3) 0.026(3) 0.000(3) 0.002(3) 0.011(3) C33 0.048(4) 0.034(4) 0.029(4) 0.002(3) 0.016(3) 0.015(3) C34 0.053(4) 0.025(4) 0.033(4) 0.006(3) 0.010(3) 0.004(3) C35 0.065(5) 0.022(4) 0.037(4) 0.003(3) 0.014(3) 0.007(3) C36 0.041(4) 0.024(4) 0.036(4) -0.004(3) 0.006(3) 0.007(3) C37 0.024(3) 0.029(4) 0.025(3) -0.007(3) 0.005(3) 0.005(3) C38 0.039(4) 0.025(4) 0.029(3) -0.005(3) 0.010(3) -0.001(3) C39 0.039(4) 0.047(4) 0.039(4) -0.012(3) 0.021(3) -0.018(3) C40 0.046(4) 0.051(5) 0.033(4) -0.018(3) 0.014(3) -0.002(4) C41 0.039(4) 0.035(4) 0.033(4) -0.014(3) 0.003(3) -0.003(3) C42 0.026(3) 0.031(4) 0.037(4) -0.004(3) 0.004(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 1.879(6) . ? Rh1 N1 2.050(5) . ? Rh1 N3 2.097(5) . ? Rh1 P1 2.3610(16) . ? Rh1 I2 2.6778(7) . ? Rh1 I1 2.7010(8) . ? C1 O1 1.113(6) . ? P1 C37 1.810(5) . ? P1 C31 1.812(5) . ? P1 C25 1.822(6) . ? N1 N2 1.307(6) . ? N1 C11 1.420(7) . ? N2 N3 1.336(6) . ? N3 C18 1.408(7) . ? C11 C16 1.370(7) . ? C11 C12 1.389(8) . ? C12 C13 1.370(8) . ? C13 C14 1.378(8) . ? C14 C15 1.372(8) . ? C14 C17 1.504(8) . ? C15 C16 1.385(7) . ? C18 C23 1.370(8) . ? C18 C19 1.397(8) . ? C19 C20 1.393(8) . ? C20 C21 1.372(9) . ? C21 C22 1.387(9) . ? C21 C24 1.500(9) . ? C22 C23 1.400(8) . ? C25 C26 1.391(8) . ? C25 C30 1.400(7) . ? C26 C27 1.384(7) . ? C27 C28 1.382(8) . ? C28 C29 1.377(9) . ? C29 C30 1.390(8) . ? C31 C36 1.377(7) . ? C31 C32 1.395(7) . ? C32 C33 1.394(7) . ? C33 C34 1.374(8) . ? C34 C35 1.370(8) . ? C35 C36 1.397(8) . ? C37 C42 1.393(7) . ? C37 C38 1.401(7) . ? C38 C39 1.370(7) . ? C39 C40 1.382(8) . ? C40 C41 1.390(8) . ? C41 C42 1.377(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 N1 107.0(2) . . ? C1 Rh1 N3 166.5(2) . . ? N1 Rh1 N3 60.15(17) . . ? C1 Rh1 P1 95.95(17) . . ? N1 Rh1 P1 90.53(13) . . ? N3 Rh1 P1 88.73(12) . . ? C1 Rh1 I2 84.96(17) . . ? N1 Rh1 I2 167.25(13) . . ? N3 Rh1 I2 107.57(13) . . ? P1 Rh1 I2 92.67(4) . . ? C1 Rh1 I1 84.18(17) . . ? N1 Rh1 I1 86.69(13) . . ? N3 Rh1 I1 90.51(12) . . ? P1 Rh1 I1 177.13(4) . . ? I2 Rh1 I1 90.20(2) . . ? O1 C1 Rh1 176.7(5) . . ? C37 P1 C31 107.2(3) . . ? C37 P1 C25 105.0(3) . . ? C31 P1 C25 103.6(3) . . ? C37 P1 Rh1 110.97(18) . . ? C31 P1 Rh1 112.35(19) . . ? C25 P1 Rh1 116.97(19) . . ? N2 N1 C11 119.0(5) . . ? N2 N1 Rh1 99.6(3) . . ? C11 N1 Rh1 140.8(4) . . ? N1 N2 N3 103.7(4) . . ? N2 N3 C18 116.6(5) . . ? N2 N3 Rh1 96.4(3) . . ? C18 N3 Rh1 146.8(4) . . ? C16 C11 C12 118.9(6) . . ? C16 C11 N1 119.0(5) . . ? C12 C11 N1 122.0(5) . . ? C13 C12 C11 119.9(6) . . ? C12 C13 C14 122.5(6) . . ? C15 C14 C13 116.5(6) . . ? C15 C14 C17 121.5(6) . . ? C13 C14 C17 122.0(6) . . ? C14 C15 C16 122.6(6) . . ? C11 C16 C15 119.6(6) . . ? C23 C18 C19 120.2(6) . . ? C23 C18 N3 118.5(6) . . ? C19 C18 N3 121.3(6) . . ? C20 C19 C18 119.0(6) . . ? C21 C20 C19 121.8(7) . . ? C20 C21 C22 118.2(6) . . ? C20 C21 C24 121.3(7) . . ? C22 C21 C24 120.5(8) . . ? C21 C22 C23 121.2(7) . . ? C18 C23 C22 119.6(6) . . ? C26 C25 C30 119.3(5) . . ? C26 C25 P1 121.3(4) . . ? C30 C25 P1 119.3(5) . . ? C27 C26 C25 120.5(6) . . ? C28 C27 C26 119.9(6) . . ? C29 C28 C27 120.3(6) . . ? C28 C29 C30 120.5(6) . . ? C29 C30 C25 119.5(6) . . ? C36 C31 C32 118.0(5) . . ? C36 C31 P1 123.7(4) . . ? C32 C31 P1 118.2(4) . . ? C33 C32 C31 121.2(5) . . ? C34 C33 C32 120.0(6) . . ? C35 C34 C33 119.2(6) . . ? C34 C35 C36 121.2(6) . . ? C31 C36 C35 120.4(6) . . ? C42 C37 C38 118.3(5) . . ? C42 C37 P1 121.4(4) . . ? C38 C37 P1 120.2(4) . . ? C39 C38 C37 120.2(5) . . ? C38 C39 C40 121.2(6) . . ? C39 C40 C41 119.2(6) . . ? C42 C41 C40 120.0(6) . . ? C41 C42 C37 121.1(6) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.699 _refine_diff_density_min -0.714 _refine_diff_density_rms 0.150