#------------------------------------------------------------------------------ #$Date: 2014-07-11 21:33:45 +0300 (Fri, 11 Jul 2014) $ #$Revision: 120075 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/07/51/4075161.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_4075161 loop_ _publ_author_name 'Herrmann, Wolfgang A.' 'Sch\"utz, Jan' 'Frey, Guido D.' 'Herdtweck, Eberhardt' _publ_section_title ; N-Heterocyclic Carbenes:  Synthesis, Structures, and Electronic Ligand Properties†,‡ ; _journal_issue 10 _journal_name_full Organometallics _journal_page_first 2437 _journal_volume 25 _journal_year 2006 _chemical_formula_moiety 'C13 H20 I N2 Rh, C H2 Cl2' _chemical_formula_sum 'C14 H22 Cl2 I N2 Rh' _chemical_formula_weight 519.05 _chemical_name_systematic ; ; _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90 _cell_angle_beta 116.8930(4) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.9166(2) _cell_length_b 7.1008(1) _cell_length_c 22.5135(2) _cell_measurement_reflns_used 7089 _cell_measurement_temperature 123(1) _cell_measurement_theta_max 25.37 _cell_measurement_theta_min 1.81 _cell_volume 3552.49(7) _computing_cell_refinement 'DENZO (Nonius, 2001b)' _computing_data_collection 'Kappa-CCD Control Software (Nonius, 2001a)' _computing_data_reduction 'DENZO (Nonius, 2001b)' _computing_molecular_graphics 'PLATON (Spek, 2001)' _computing_publication_material 'PLATON (Spek, 2001)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1998)' _computing_structure_solution 'SIR92 (Altomare, 1994)' _diffrn_ambient_temperature 123(1) _diffrn_detector ' CCD plate ' _diffrn_detector_area_resol_mean 18 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device ' \k-geometry diffractometer ' _diffrn_measurement_device_type ' Nonius \k-CCD diffractometer' _diffrn_measurement_method ' phi- and omega-rotation ' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'NONIUS FR 591 rotating anode' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.070 _diffrn_reflns_av_sigmaI/netI 0.0299 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 65917 _diffrn_reflns_theta_full 25.37 _diffrn_reflns_theta_max 25.37 _diffrn_reflns_theta_min 1.81 _diffrn_standards_decay_% 0 _exptl_absorpt_coefficient_mu 2.993 _exptl_absorpt_correction_T_max 0.863 _exptl_absorpt_correction_T_min 0.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(applied during the scaling procedure; Nonius, 2001b)' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.941 _exptl_crystal_density_meas none _exptl_crystal_density_method none _exptl_crystal_description needle _exptl_crystal_F_000 2016 _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.665 _refine_diff_density_min -0.841 _refine_diff_density_rms 0.124 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.273 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 365 _refine_ls_number_reflns 6529 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.273 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0422 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(Fo^2^)+(0.0000P)^2^+13.9193P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme sigma _refine_ls_wR_factor_gt 0.0605 _refine_ls_wR_factor_ref 0.0621 _reflns_number_gt 5968 _reflns_number_total 6529 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file om0600801si20060125_122734.cif _[local]_cod_data_source_block JSCA-4255-123 _[local]_cod_cif_authors_sg_H-M 'P 21/c' _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana ; _cod_database_code 4075161 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,1/2+y,1/2-z -x,-y,-z x,1/2-y,1/2+z 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 I1 0.0136(2) 0.0175(2) 0.0222(2) 0.0046(1) 0.0063(1) 0.0002(1) Rh1 0.0135(2) 0.0098(2) 0.0136(2) 0.0022(2) 0.0077(2) 0.0005(2) N1 0.013(2) 0.015(2) 0.013(2) -0.0023(17) 0.0075(17) -0.0045(17) N2 0.016(2) 0.016(2) 0.018(2) 0.0045(18) 0.0100(19) -0.0030(17) C1 0.014(2) 0.010(2) 0.016(2) 0.0026(19) 0.008(2) 0.0021(19) C2 0.020(3) 0.013(3) 0.020(3) -0.001(2) 0.009(2) 0.000(2) C3 0.015(3) 0.012(2) 0.021(3) 0.004(2) 0.004(2) -0.001(2) C4 0.026(3) 0.020(3) 0.023(3) -0.006(2) 0.014(2) -0.010(2) C5 0.028(3) 0.027(3) 0.024(3) 0.001(2) 0.019(3) -0.004(2) C6 0.016(3) 0.015(3) 0.026(3) 0.008(2) 0.010(2) 0.005(2) C7 0.015(3) 0.020(3) 0.016(2) 0.006(2) 0.008(2) 0.009(2) C8 0.017(3) 0.020(3) 0.020(3) 0.003(2) 0.004(2) 0.003(2) C9 0.017(3) 0.013(2) 0.028(3) 0.002(2) 0.009(2) -0.002(2) C10 0.013(3) 0.014(2) 0.025(3) 0.009(2) 0.011(2) 0.002(2) C11 0.017(3) 0.020(3) 0.016(3) 0.005(2) 0.010(2) -0.003(2) C12 0.023(3) 0.023(3) 0.020(3) -0.001(2) 0.013(2) 0.000(2) C13 0.024(3) 0.016(3) 0.034(3) 0.000(2) 0.019(3) 0.006(2) I2 0.0155(2) 0.0158(2) 0.0220(2) 0.0020(1) 0.0071(1) 0.0016(1) Rh2 0.0128(2) 0.0124(2) 0.0139(2) 0.0014(2) 0.0069(2) -0.0007(2) N3 0.016(2) 0.016(2) 0.018(2) 0.0044(17) 0.0093(18) -0.0006(17) N4 0.015(2) 0.022(2) 0.024(2) 0.0088(19) 0.0123(19) 0.0024(18) C21 0.011(2) 0.017(3) 0.013(2) 0.004(2) 0.004(2) 0.001(2) C22 0.011(2) 0.017(3) 0.018(3) 0.003(2) 0.003(2) 0.000(2) C23 0.016(3) 0.017(3) 0.028(3) 0.006(2) 0.009(2) -0.002(2) C24 0.028(3) 0.019(3) 0.023(3) -0.004(2) 0.016(3) 0.001(2) C25 0.030(3) 0.034(3) 0.030(3) 0.010(3) 0.023(3) 0.004(3) C26 0.012(3) 0.020(3) 0.024(3) 0.006(2) 0.008(2) 0.005(2) C27 0.012(3) 0.027(3) 0.023(3) 0.005(2) 0.008(2) 0.009(2) C28 0.016(3) 0.037(3) 0.019(3) -0.003(2) 0.004(2) -0.001(2) C29 0.022(3) 0.029(3) 0.023(3) -0.010(2) 0.010(2) -0.011(2) C30 0.020(3) 0.018(3) 0.024(3) 0.002(2) 0.015(2) -0.003(2) C31 0.016(3) 0.023(3) 0.015(2) 0.004(2) 0.011(2) -0.004(2) C32 0.023(3) 0.025(3) 0.019(3) 0.001(2) 0.013(2) 0.000(2) C33 0.021(3) 0.020(3) 0.030(3) -0.001(2) 0.015(2) 0.002(2) Cl1 0.0352(9) 0.0559(10) 0.0294(8) 0.0040(7) 0.0163(7) -0.0162(7) Cl2 0.0462(10) 0.0351(8) 0.0335(8) 0.0115(7) 0.0118(8) -0.0006(7) C41 0.031(3) 0.031(3) 0.031(3) 0.001(3) 0.021(3) -0.002(3) Cl3 0.0328(8) 0.0354(8) 0.0434(9) 0.0147(7) 0.0147(7) 0.0084(7) Cl4 0.0389(9) 0.0657(11) 0.0407(9) -0.0047(8) 0.0198(8) -0.0262(8) C51 0.025(3) 0.029(3) 0.022(3) 0.005(2) 0.012(2) 0.003(2) loop_ _atom_site_label _atom_site_type_symbol _atom_site_thermal_displace_type _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_occupancy _atom_site_U_iso_or_equiv _atom_site_calc_flag _atom_site_refinement_flags I1 I Uani 0.29532(1) 0.83628(4) 0.28190(2) 1.000 0.0185(1) . . Rh1 Rh Uani 0.40586(2) 0.69702(5) 0.35429(2) 1.000 0.0117(1) . . N1 N Uani 0.35540(17) 0.5579(5) 0.44494(18) 1.000 0.0131(12) . . N2 N Uani 0.32572(17) 0.4122(5) 0.45770(19) 1.000 0.0158(12) . . C1 C Uani 0.3679(2) 0.5162(6) 0.3945(2) 1.000 0.0129(12) . . C2 C Uani 0.3449(2) 0.3314(7) 0.3748(2) 1.000 0.0177(17) . . C3 C Uani 0.3195(2) 0.2750(7) 0.4146(2) 1.000 0.0176(16) . . C4 C Uani 0.3686(2) 0.7319(7) 0.4835(3) 1.000 0.0219(17) . . C5 C Uani 0.3055(2) 0.4212(7) 0.5089(3) 1.000 0.0236(17) . . C6 C Uani 0.4803(2) 0.5139(7) 0.3855(2) 1.000 0.0188(17) . . C7 C Uani 0.4948(2) 0.6596(7) 0.4322(2) 1.000 0.0166(16) . . C8 C Uani 0.5369(2) 0.8220(7) 0.4385(2) 1.000 0.0207(17) . . C9 C Uani 0.5022(2) 0.9948(7) 0.3997(3) 1.000 0.0198(16) . . C10 C Uani 0.4484(2) 0.9466(7) 0.3350(2) 1.000 0.0164(16) . . C11 C Uani 0.4453(2) 0.8098(7) 0.2903(2) 1.000 0.0167(17) . . C12 C Uani 0.4967(2) 0.6882(7) 0.2959(2) 1.000 0.0208(17) . . C13 C Uani 0.5008(2) 0.5000(7) 0.3317(3) 1.000 0.0224(17) . . I2 I Uani 0.20362(1) -0.05981(4) 0.45697(2) 1.000 0.0183(1) . . Rh2 Rh Uani 0.09902(2) 0.12870(5) 0.39274(2) 1.000 0.0127(1) . . N3 N Uani 0.14649(17) 0.2118(5) 0.29345(19) 1.000 0.0161(12) . . N4 N Uani 0.17729(18) 0.3433(6) 0.2755(2) 1.000 0.0190(12) . . C21 C Uani 0.1380(2) 0.2743(7) 0.3452(2) 1.000 0.0142(14) . . C22 C Uani 0.1641(2) 0.4561(7) 0.3592(2) 1.000 0.0167(16) . . C23 C Uani 0.1876(2) 0.4905(7) 0.3159(3) 1.000 0.0207(17) . . C24 C Uani 0.1298(2) 0.0296(7) 0.2599(3) 1.000 0.0216(17) . . C25 C Uani 0.1932(2) 0.3173(8) 0.2212(3) 1.000 0.0278(17) . . C26 C Uani 0.0358(2) 0.3490(7) 0.3706(2) 1.000 0.0187(17) . . C27 C Uani 0.0111(2) 0.2076(7) 0.3219(3) 1.000 0.0206(17) . . C28 C Uani -0.0374(2) 0.0707(8) 0.3187(3) 1.000 0.0255(17) . . C29 C Uani -0.0113(2) -0.1120(7) 0.3574(3) 1.000 0.0247(17) . . C30 C Uani 0.0491(2) -0.0883(7) 0.4175(2) 1.000 0.0188(17) . . C31 C Uani 0.0636(2) 0.0512(7) 0.4641(2) 1.000 0.0165(16) . . C32 C Uani 0.0196(2) 0.1988(7) 0.4641(2) 1.000 0.0210(17) . . C33 C Uani 0.0202(2) 0.3818(7) 0.4273(3) 1.000 0.0224(17) . . Cl1 Cl Uani 0.35992(7) 0.5718(2) 0.12598(7) 1.000 0.0395(5) . . Cl2 Cl Uani 0.33477(7) 0.2497(2) 0.18970(7) 1.000 0.0406(5) . . C41 C Uani 0.3091(3) 0.4696(8) 0.1515(3) 1.000 0.0284(17) . . Cl3 Cl Uani 0.18178(7) 1.1184(2) 0.04939(8) 1.000 0.0382(5) . . Cl4 Cl Uani 0.14437(7) 0.8126(3) 0.10931(8) 1.000 0.0478(6) . . C51 C Uani 0.2028(2) 0.9057(7) 0.0938(3) 1.000 0.0248(17) . . H21 H Uiso 0.34680 0.25960 0.34020 1.000 0.0210 calc R H31 H Uiso 0.30040 0.15720 0.41190 1.000 0.0210 calc R H41 H Uiso 0.33100 0.78840 0.47860 1.000 0.0330 calc R H42 H Uiso 0.38920 0.82010 0.46720 1.000 0.0330 calc R H43 H Uiso 0.39450 0.70400 0.53060 1.000 0.0330 calc R H51 H Uiso 0.27900 0.53020 0.50070 1.000 0.0350 calc R H52 H Uiso 0.34040 0.43380 0.55270 1.000 0.0350 calc R H53 H Uiso 0.28350 0.30580 0.50780 1.000 0.0350 calc R H61 H Uiso 0.45560 0.41530 0.38770 1.000 0.0220 calc R H71 H Uiso 0.47720 0.65690 0.46190 1.000 0.0200 calc R H81 H Uiso 0.56540 0.78160 0.42140 1.000 0.0240 calc R H82 H Uiso 0.56060 0.85560 0.48600 1.000 0.0240 calc R H91 H Uiso 0.48850 1.06760 0.42780 1.000 0.0240 calc R H92 H Uiso 0.52960 1.07630 0.39020 1.000 0.0240 calc R H101 H Uiso 0.41290 1.01830 0.32380 1.000 0.0200 calc R H111 H Uiso 0.40740 0.79050 0.25280 1.000 0.0200 calc R H121 H Uiso 0.53490 0.75820 0.32040 1.000 0.0250 calc R H122 H Uiso 0.49210 0.66190 0.25060 1.000 0.0250 calc R H131 H Uiso 0.47570 0.40530 0.29840 1.000 0.0270 calc R H132 H Uiso 0.54290 0.45510 0.35190 1.000 0.0270 calc R H221 H Uiso 0.16500 0.53930 0.39270 1.000 0.0200 calc R H231 H Uiso 0.20810 0.60220 0.31480 1.000 0.0250 calc R H241 H Uiso 0.16600 -0.03540 0.26410 1.000 0.0330 calc R H242 H Uiso 0.10220 0.04880 0.21270 1.000 0.0330 calc R H243 H Uiso 0.11000 -0.04690 0.28050 1.000 0.0330 calc R H251 H Uiso 0.22110 0.21130 0.23150 1.000 0.0420 calc R H252 H Uiso 0.21230 0.43200 0.21570 1.000 0.0420 calc R H253 H Uiso 0.15670 0.29120 0.17990 1.000 0.0420 calc R H261 H Uiso 0.06470 0.43060 0.36760 1.000 0.0230 calc R H271 H Uiso 0.02530 0.19670 0.28940 1.000 0.0250 calc R H281 H Uiso -0.06410 0.03940 0.27150 1.000 0.0300 calc R H282 H Uiso -0.06220 0.13320 0.33700 1.000 0.0300 calc R H291 H Uiso -0.04020 -0.16400 0.37220 1.000 0.0290 calc R H292 H Uiso -0.00720 -0.20500 0.32700 1.000 0.0290 calc R H301 H Uiso 0.07950 -0.17750 0.42340 1.000 0.0220 calc R H311 H Uiso 0.10370 0.05580 0.49870 1.000 0.0190 calc R H321 H Uiso 0.02940 0.23010 0.51070 1.000 0.0250 calc R H322 H Uiso -0.02150 0.14520 0.44280 1.000 0.0250 calc R H331 H Uiso -0.01990 0.44190 0.40960 1.000 0.0270 calc R H332 H Uiso 0.04990 0.47020 0.45950 1.000 0.0270 calc R H411 H Uiso 0.30390 0.55520 0.18320 1.000 0.0340 calc R H412 H Uiso 0.26950 0.45370 0.11230 1.000 0.0340 calc R H511 H Uiso 0.23890 0.92720 0.13680 1.000 0.0300 calc R H512 H Uiso 0.21350 0.81290 0.06810 1.000 0.0300 calc R loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Rh Rh -1.1178 0.9187 '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' 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' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag I1 Rh1 C1 86.94(14) yes I1 Rh1 C6 159.87(12) yes I1 Rh1 C7 161.46(13) yes I1 Rh1 C10 92.12(13) yes I1 Rh1 C11 96.14(13) yes C1 Rh1 C6 88.8(2) yes C1 Rh1 C7 94.29(19) yes C1 Rh1 C10 162.94(17) yes C1 Rh1 C11 160.85(17) yes C6 Rh1 C7 38.59(18) yes C6 Rh1 C10 97.6(2) yes C6 Rh1 C11 81.86(18) yes C7 Rh1 C10 81.31(18) yes C7 Rh1 C11 88.76(18) yes C10 Rh1 C11 36.14(17) yes I2 Rh2 C30 92.09(13) yes I2 Rh2 C31 95.33(13) yes C21 Rh2 C26 89.0(2) yes C21 Rh2 C27 92.7(2) yes C21 Rh2 C30 162.03(17) yes C21 Rh2 C31 161.88(18) yes C26 Rh2 C27 38.81(19) yes C26 Rh2 C30 97.6(2) yes C26 Rh2 C31 81.75(18) yes C27 Rh2 C30 82.28(19) yes C27 Rh2 C31 89.8(2) yes C30 Rh2 C31 35.97(17) yes I2 Rh2 C21 87.62(14) yes I2 Rh2 C26 158.55(12) yes I2 Rh2 C27 162.56(15) yes N2 N1 C1 111.3(4) yes N2 N1 C4 120.7(4) yes C1 N1 C4 128.0(4) yes N1 N2 C3 107.1(4) yes N1 N2 C5 123.0(4) yes C3 N2 C5 129.9(4) yes N4 N3 C24 120.9(4) yes C21 N3 C24 128.2(4) yes N4 N3 C21 110.8(4) yes N3 N4 C23 107.0(4) yes C23 N4 C25 129.1(5) yes N3 N4 C25 123.9(4) yes Rh1 C1 C2 130.4(3) yes Rh1 C1 N1 124.8(3) yes N1 C1 C2 104.7(4) yes C1 C2 C3 107.8(4) no N2 C3 C2 109.0(4) yes Rh1 C6 C7 71.6(3) yes Rh1 C6 C13 109.7(3) yes C7 C6 C13 125.6(5) no C6 C7 C8 124.2(4) no Rh1 C7 C6 69.8(3) yes Rh1 C7 C8 113.5(3) yes C7 C8 C9 111.6(4) no C8 C9 C10 113.4(4) no Rh1 C10 C9 106.8(3) yes Rh1 C10 C11 72.8(3) yes C9 C10 C11 126.8(5) no Rh1 C11 C10 71.1(3) yes C10 C11 C12 125.5(4) no Rh1 C11 C12 110.4(3) yes C11 C12 C13 113.3(4) no C6 C13 C12 113.3(4) no C1 C2 H21 126.10 no C3 C2 H21 126.06 no C2 C3 H31 125.55 no N2 C3 H31 125.41 no H41 C4 H42 109.43 no H41 C4 H43 109.46 no H42 C4 H43 109.52 no N1 C4 H43 109.47 no N1 C4 H41 109.47 no N1 C4 H42 109.48 no N2 C5 H53 109.50 no N2 C5 H51 109.35 no N2 C5 H52 109.50 no H52 C5 H53 109.47 no H51 C5 H52 109.47 no H51 C5 H53 109.54 no Rh1 C6 H61 88.79 no C7 C6 H61 117.34 no C13 C6 H61 117.06 no Rh1 C7 H71 86.71 no C8 C7 H71 117.86 no C6 C7 H71 117.92 no C7 C8 H82 109.44 no C9 C8 H81 109.28 no C7 C8 H81 109.23 no H81 C8 H82 107.91 no C9 C8 H82 109.35 no H91 C9 H92 107.69 no C10 C9 H92 108.85 no C8 C9 H91 108.89 no C8 C9 H92 109.03 no C10 C9 H91 108.87 no Rh1 C10 H101 90.58 no C9 C10 H101 116.69 no C11 C10 H101 116.53 no C12 C11 H111 117.32 no C10 C11 H111 117.16 no Rh1 C11 H111 88.33 no C13 C12 H121 108.92 no C11 C12 H122 108.94 no C11 C12 H121 109.04 no C13 C12 H122 108.93 no H121 C12 H122 107.58 no H131 C13 H132 107.73 no C6 C13 H131 108.87 no C6 C13 H132 108.93 no C12 C13 H131 108.86 no C12 C13 H132 109.03 no Rh2 C21 N3 126.0(4) yes Rh2 C21 C22 129.1(3) yes N3 C21 C22 104.9(4) yes C21 C22 C23 107.8(4) no N4 C23 C22 109.5(5) yes Rh2 C26 C27 70.9(3) yes Rh2 C26 C33 111.3(3) yes C27 C26 C33 125.4(5) no Rh2 C27 C26 70.3(3) yes Rh2 C27 C28 113.2(4) yes C26 C27 C28 123.3(5) no C27 C28 C29 112.9(5) no C28 C29 C30 114.2(4) no Rh2 C30 C29 107.4(3) yes Rh2 C30 C31 72.8(3) yes C29 C30 C31 125.3(5) no Rh2 C31 C30 71.2(3) yes Rh2 C31 C32 110.6(3) yes C30 C31 C32 124.1(4) no C31 C32 C33 113.5(4) no C26 C33 C32 113.1(4) no C21 C22 H221 125.96 no C23 C22 H221 126.22 no N4 C23 H231 125.27 no C22 C23 H231 125.21 no N3 C24 H241 109.47 no N3 C24 H242 109.49 no N3 C24 H243 109.44 no H241 C24 H242 109.54 no H241 C24 H243 109.39 no H242 C24 H243 109.50 no N4 C25 H251 109.41 no N4 C25 H252 109.45 no N4 C25 H253 109.38 no H251 C25 H252 109.63 no H251 C25 H253 109.52 no H252 C25 H253 109.44 no Rh2 C26 H261 87.72 no C27 C26 H261 117.28 no C33 C26 H261 117.31 no Rh2 C27 H271 86.54 no C26 C27 H271 118.35 no C28 C27 H271 118.34 no C27 C28 H281 109.06 no C27 C28 H282 108.95 no C29 C28 H281 109.03 no C29 C28 H282 109.09 no H281 C28 H282 107.72 no C28 C29 H291 108.67 no C28 C29 H292 108.76 no C30 C29 H291 108.74 no C30 C29 H292 108.74 no H291 C29 H292 107.58 no Rh2 C30 H301 89.77 no C29 C30 H301 117.36 no C31 C30 H301 117.31 no Rh2 C31 H311 88.28 no C30 C31 H311 117.97 no C32 C31 H311 117.94 no C31 C32 H321 108.89 no C31 C32 H322 108.89 no C33 C32 H321 108.80 no C33 C32 H322 108.82 no H321 C32 H322 107.78 no C26 C33 H331 108.96 no C26 C33 H332 108.86 no C32 C33 H331 109.02 no C32 C33 H332 109.01 no H331 C33 H332 107.78 no Cl1 C41 Cl2 111.6(4) yes Cl1 C41 H411 109.23 no Cl1 C41 H412 109.24 no Cl2 C41 H411 109.28 no Cl2 C41 H412 109.31 no H411 C41 H412 108.09 no Cl3 C51 Cl4 111.9(3) yes Cl3 C51 H511 109.21 no Cl3 C51 H512 109.25 no Cl4 C51 H511 109.19 no Cl4 C51 H512 109.24 no H511 C51 H512 107.95 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag I1 Rh1 2.6757(6) yes I2 Rh2 2.6956(6) yes Rh1 C1 2.034(5) yes Rh1 C6 2.109(5) yes Rh1 C10 2.207(5) yes Rh1 C11 2.228(5) yes Rh1 C7 2.131(5) yes Rh2 C27 2.120(6) yes Rh2 C31 2.224(5) yes Rh2 C26 2.113(5) yes Rh2 C30 2.204(5) yes Rh2 C21 2.024(5) yes Cl1 C41 1.766(8) yes Cl2 C41 1.758(6) yes Cl3 C51 1.755(5) yes Cl4 C51 1.772(6) yes N1 C1 1.340(6) yes N1 N2 1.376(6) yes N1 C4 1.460(6) yes N2 C3 1.334(6) yes N2 C5 1.453(7) yes N3 C24 1.461(6) yes N3 C21 1.350(6) yes N3 N4 1.380(6) yes N4 C23 1.332(7) yes N4 C25 1.457(7) yes C1 C2 1.420(7) no C2 C3 1.370(7) no C6 C7 1.401(6) no C6 C13 1.516(8) no C7 C8 1.522(7) no C8 C9 1.527(7) no C9 C10 1.507(7) no C10 C11 1.376(7) no C11 C12 1.502(7) no C12 C13 1.540(7) no C2 H21 0.9499 no C3 H31 0.9506 no C4 H43 0.9803 no C4 H41 0.9784 no C4 H42 0.9802 no C5 H52 0.9802 no C5 H53 0.9799 no C5 H51 0.9792 no C6 H61 0.9482 no C7 H71 0.9513 no C8 H81 0.9910 no C8 H82 0.9889 no C9 H91 0.9896 no C9 H92 0.9894 no C10 H101 0.9505 no C11 H111 0.9498 no C12 H121 0.9911 no C12 H122 0.9912 no C13 H132 0.9886 no C13 H131 0.9906 no C21 C22 1.415(7) no C22 C23 1.367(8) no C26 C27 1.407(7) no C26 C33 1.511(8) no C27 C28 1.527(8) no C28 C29 1.534(8) no C29 C30 1.511(7) no C30 C31 1.367(6) no C31 C32 1.517(7) no C32 C33 1.545(7) no C22 H221 0.9503 no C23 H231 0.9498 no C24 H243 0.9801 no C24 H242 0.9796 no C24 H241 0.9790 no C25 H252 0.9790 no C25 H253 0.9803 no C25 H251 0.9786 no C26 H261 0.9502 no C27 H271 0.9491 no C28 H281 0.9908 no C28 H282 0.9894 no C29 H291 0.9914 no C29 H292 0.9890 no C30 H301 0.9495 no C31 H311 0.9498 no C32 H321 0.9889 no C32 H322 0.9896 no C33 H332 0.9909 no C33 H331 0.9895 no C41 H412 0.9886 no C41 H411 0.9896 no C51 H511 0.9909 no C51 H512 0.9898 no _journal_paper_doi 10.1021/om0600801