# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Michael Doyle' 'Yang Liu.' 'Yinxin Sun.' 'Huai Sun.' 'Jian-Hua Xie.' 'Peter Zavalij' 'Lei Zhou.' _publ_contact_author_name 'Michael Doyle' _publ_contact_author_email MDOYLE3@UMD.EDU _publ_section_title ; Conformational Isomers of Extraordinary Stability: Carboxamidate-Bridged Dimetalloorganic Compounds ; # Attachment 'Cif_file_of_the_x-ray_structural_analysis_of_ACOBF4.cif.txt' data_1710 _database_code_depnum_ccdc_archive 'CCDC 722154' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Rh2-complex ; _chemical_name_common Rh2-complex _chemical_formula_moiety 'C32 H54 N6 O4 Rh2, B F4, 2(C2 H3 N)' _chemical_formula_sum 'C36 H60 B F4 N8 O4 Rh2' _chemical_formula_weight 961.55 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 24.381(2) _cell_length_b 7.1609(6) _cell_length_c 24.440(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.4465(13) _cell_angle_gamma 90.00 _cell_volume 4150.0(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 8249 _cell_measurement_theta_min 2.7 _cell_measurement_theta_max 30.7 _exptl_crystal_description needle _exptl_crystal_colour purple _exptl_crystal_size_max 0.255 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.025 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.539 _exptl_crystal_density_method not-measured _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 0.861 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 200(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 'three-circle diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 11.198 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19810 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0254 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3653 _reflns_number_gt 3296 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker, 2004)' _computing_publication_material SHELXL-97 _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 'w=1/[\s^2^(Fo^2^)+(0.015P)^2^+25.946P], P=(max(Fo^2^,0)+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 3653 _refine_ls_number_parameters 274 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 0.996 _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 0.263738(10) 0.15140(3) 0.040695(10) 0.01643(8) Uani 1 1 d . . . N1 N 0.28744(11) -0.0587(4) 0.11101(11) 0.0238(6) Uani 1 1 d . . . C1 C 0.29874(14) -0.1656(5) 0.14581(15) 0.0289(8) Uani 1 1 d . . . C2 C 0.31362(19) -0.3003(6) 0.19135(18) 0.0534(12) Uani 1 1 d . . . H2A H 0.3530 -0.2820 0.2113 0.080 Uiso 1 1 calc R . . H2B H 0.3087 -0.4271 0.1759 0.080 Uiso 1 1 calc R . . H2C H 0.2892 -0.2826 0.2176 0.080 Uiso 1 1 calc R . . O11 O 0.19168(8) 0.5020(3) 0.00286(9) 0.0205(5) Uani 1 1 d . . . N11 N 0.21831(10) 0.3154(3) 0.08007(10) 0.0184(5) Uani 1 1 d . . . C11 C 0.19254(12) 0.4644(4) 0.05472(13) 0.0189(6) Uani 1 1 d . . . C12 C 0.16195(14) 0.6062(4) 0.08260(14) 0.0252(7) Uani 1 1 d . . . H12A H 0.1620 0.7274 0.0632 0.030 Uiso 1 1 calc R . . H12B H 0.1833 0.6230 0.1220 0.030 Uiso 1 1 calc R . . C13 C 0.10082(14) 0.5561(5) 0.08287(15) 0.0328(8) Uani 1 1 d . . . H13A H 0.0825 0.6695 0.0934 0.039 Uiso 1 1 calc R . . H13B H 0.0810 0.5234 0.0439 0.039 Uiso 1 1 calc R . . C14 C 0.09149(15) 0.3973(5) 0.12148(17) 0.0385(9) Uani 1 1 d . . . H14A H 0.1125 0.4271 0.1603 0.046 Uiso 1 1 calc R . . H14B H 0.0509 0.3939 0.1216 0.046 Uiso 1 1 calc R . . C15 C 0.10896(16) 0.2033(5) 0.10671(17) 0.0383(9) Uani 1 1 d . . . H15A H 0.1082 0.2007 0.0660 0.046 Uiso 1 1 calc R . . H15B H 0.0805 0.1128 0.1132 0.046 Uiso 1 1 calc R . . C16 C 0.16694(15) 0.1375(5) 0.13908(14) 0.0311(8) Uani 1 1 d . . . H16A H 0.1656 0.1155 0.1787 0.037 Uiso 1 1 calc R . . H16B H 0.1754 0.0165 0.1232 0.037 Uiso 1 1 calc R . . C17 C 0.21490(13) 0.2728(5) 0.13795(13) 0.0230(7) Uani 1 1 d . . . H17A H 0.2089 0.3899 0.1573 0.028 Uiso 1 1 calc R . . H17B H 0.2510 0.2174 0.1586 0.028 Uiso 1 1 calc R . . O21 O 0.30393(8) 0.5088(3) -0.00810(9) 0.0210(5) Uani 1 1 d . . . N21 N 0.32969(10) 0.3215(4) 0.06888(10) 0.0187(5) Uani 1 1 d . . . C21 C 0.33672(12) 0.4714(4) 0.04007(13) 0.0201(7) Uani 1 1 d . . . C22 C 0.38305(13) 0.6141(4) 0.05949(14) 0.0250(7) Uani 1 1 d . . . H22A H 0.3904 0.6257 0.1009 0.030 Uiso 1 1 calc R . . H22B H 0.3696 0.7369 0.0431 0.030 Uiso 1 1 calc R . . C23 C 0.43858(14) 0.5669(5) 0.04345(15) 0.0314(8) Uani 1 1 d . . . H23A H 0.4300 0.5381 0.0027 0.038 Uiso 1 1 calc R . . H23B H 0.4627 0.6798 0.0494 0.038 Uiso 1 1 calc R . . C24 C 0.47266(14) 0.4048(5) 0.07499(17) 0.0352(9) Uani 1 1 d . . . H24A H 0.4803 0.4321 0.1158 0.042 Uiso 1 1 calc R . . H24B H 0.5095 0.4007 0.0645 0.042 Uiso 1 1 calc R . . C25 C 0.44588(14) 0.2108(5) 0.06513(16) 0.0331(8) Uani 1 1 d . . . H25A H 0.4182 0.2116 0.0284 0.040 Uiso 1 1 calc R . . H25B H 0.4757 0.1200 0.0624 0.040 Uiso 1 1 calc R . . C26 C 0.41625(14) 0.1420(5) 0.10960(15) 0.0323(8) Uani 1 1 d . . . H26A H 0.4448 0.1212 0.1452 0.039 Uiso 1 1 calc R . . H26B H 0.3982 0.0203 0.0974 0.039 Uiso 1 1 calc R . . C27 C 0.37166(13) 0.2758(5) 0.12080(13) 0.0243(7) Uani 1 1 d . . . H27A H 0.3524 0.2184 0.1481 0.029 Uiso 1 1 calc R . . H27B H 0.3901 0.3920 0.1377 0.029 Uiso 1 1 calc R . . N1A N 0.18200(19) 0.7046(7) 0.23776(16) 0.0726(14) Uani 1 1 d . . . C1A C 0.1358(2) 0.7350(7) 0.23172(16) 0.0487(11) Uani 1 1 d . . . C2A C 0.0759(2) 0.7708(8) 0.2238(2) 0.0644(14) Uani 1 1 d . . . H2D H 0.0609 0.8217 0.1860 0.097 Uiso 1 1 calc R . . H2E H 0.0698 0.8609 0.2520 0.097 Uiso 1 1 calc R . . H2F H 0.0564 0.6539 0.2280 0.097 Uiso 1 1 calc R . . B1 B 0.4983(5) 0.7356(9) 0.2504(6) 0.052(2) Uani 1 2 d SDU A -1 F1 F 0.5184(5) 0.9048(10) 0.2438(6) 0.135(4) Uani 0.50 1 d PDU A -1 F2 F 0.4878(7) 0.642(2) 0.2024(6) 0.143(7) Uani 0.50 1 d PDU A -1 F3 F 0.4503(3) 0.7518(15) 0.2667(5) 0.132(3) Uani 0.50 1 d PDU A -1 F4 F 0.5358(6) 0.640(2) 0.2881(7) 0.126(6) Uani 0.50 1 d PDU A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01461(12) 0.01697(12) 0.01735(13) 0.00297(11) 0.00295(9) 0.00165(10) N1 0.0195(14) 0.0241(15) 0.0272(15) 0.0028(13) 0.0045(11) 0.0015(12) C1 0.0252(17) 0.0291(19) 0.0325(19) 0.0036(17) 0.0072(15) 0.0025(15) C2 0.054(3) 0.056(3) 0.050(3) 0.032(2) 0.010(2) 0.011(2) O11 0.0200(11) 0.0198(11) 0.0219(11) 0.0028(9) 0.0056(9) 0.0056(9) N11 0.0181(13) 0.0177(14) 0.0195(13) 0.0015(11) 0.0048(10) 0.0010(10) C11 0.0143(15) 0.0182(16) 0.0237(16) -0.0007(13) 0.0035(12) -0.0005(12) C12 0.0289(18) 0.0207(17) 0.0262(18) -0.0006(14) 0.0069(14) 0.0048(14) C13 0.0243(18) 0.038(2) 0.037(2) -0.0032(17) 0.0091(15) 0.0094(16) C14 0.0254(19) 0.046(2) 0.047(2) -0.0052(19) 0.0149(17) -0.0014(17) C15 0.033(2) 0.038(2) 0.045(2) -0.0079(18) 0.0129(17) -0.0150(17) C16 0.042(2) 0.0289(19) 0.0268(18) 0.0003(16) 0.0163(16) -0.0020(17) C17 0.0269(17) 0.0234(17) 0.0183(16) -0.0001(13) 0.0042(13) 0.0029(14) O21 0.0184(11) 0.0211(11) 0.0217(11) 0.0030(9) 0.0014(9) -0.0011(9) N21 0.0146(12) 0.0208(14) 0.0194(13) 0.0018(11) 0.0015(10) 0.0008(11) C21 0.0184(15) 0.0202(16) 0.0226(16) -0.0010(13) 0.0064(13) 0.0009(13) C22 0.0261(17) 0.0181(17) 0.0281(18) 0.0008(13) 0.0008(14) -0.0027(13) C23 0.0240(18) 0.034(2) 0.035(2) 0.0020(16) 0.0049(15) -0.0106(16) C24 0.0175(17) 0.041(2) 0.047(2) -0.0004(18) 0.0069(16) -0.0013(15) C25 0.0210(17) 0.032(2) 0.045(2) -0.0055(17) 0.0041(16) 0.0048(15) C26 0.0231(17) 0.0282(19) 0.039(2) 0.0043(17) -0.0064(15) 0.0001(15) C27 0.0224(16) 0.0255(17) 0.0216(16) 0.0022(14) -0.0019(13) -0.0044(14) N1A 0.058(3) 0.113(4) 0.042(2) -0.016(2) 0.001(2) -0.004(3) C1A 0.064(3) 0.052(3) 0.027(2) -0.0037(19) 0.003(2) -0.002(2) C2A 0.062(3) 0.079(4) 0.047(3) -0.007(3) 0.002(2) 0.018(3) B1 0.057(5) 0.047(5) 0.053(5) -0.016(14) 0.016(4) 0.006(14) F1 0.170(14) 0.072(5) 0.180(10) 0.009(7) 0.073(9) -0.043(6) F2 0.216(18) 0.135(11) 0.062(6) -0.051(7) 0.002(8) 0.056(10) F3 0.081(5) 0.154(9) 0.180(9) -0.041(8) 0.067(6) -0.002(6) F4 0.119(9) 0.121(10) 0.109(10) -0.011(7) -0.034(7) 0.067(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N21 2.007(2) . ? Rh1 N11 2.007(2) . ? Rh1 O11 2.015(2) 7 ? Rh1 O21 2.015(2) 7 ? Rh1 N1 2.256(3) . ? Rh1 Rh1 2.4041(5) 7 ? N1 C1 1.130(4) . ? C1 C2 1.454(5) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? O11 C11 1.291(4) . ? O11 Rh1 2.015(2) 7 ? N11 C11 1.317(4) . ? N11 C17 1.468(4) . ? C11 C12 1.513(4) . ? C12 C13 1.534(5) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C13 C14 1.528(5) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.521(5) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.525(5) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.524(5) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? O21 C21 1.288(4) . ? O21 Rh1 2.015(2) 7 ? N21 C21 1.317(4) . ? N21 C27 1.470(4) . ? C21 C22 1.515(4) . ? C22 C23 1.532(5) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.528(5) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.530(5) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.520(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.521(5) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? N1A C1A 1.122(6) . ? C1A C2A 1.452(7) . ? C2A H2D 0.9800 . ? C2A H2E 0.9800 . ? C2A H2F 0.9800 . ? B1 F2 1.326(9) . ? B1 F4 1.326(9) . ? B1 F3 1.326(9) . ? B1 F1 1.331(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 N21 Rh1 N11 88.15(10) . . ? N21 Rh1 O11 91.41(9) . 7 ? N11 Rh1 O11 176.44(9) . 7 ? N21 Rh1 O21 176.38(9) . 7 ? N11 Rh1 O21 91.74(9) . 7 ? O11 Rh1 O21 88.47(8) 7 7 ? N21 Rh1 N1 95.76(10) . . ? N11 Rh1 N1 95.58(10) . . ? O11 Rh1 N1 87.98(9) 7 . ? O21 Rh1 N1 87.85(9) 7 . ? N21 Rh1 Rh1 88.53(7) . 7 ? N11 Rh1 Rh1 88.53(7) . 7 ? O11 Rh1 Rh1 87.93(6) 7 7 ? O21 Rh1 Rh1 87.84(6) 7 7 ? N1 Rh1 Rh1 174.14(7) . 7 ? C1 N1 Rh1 179.0(3) . . ? N1 C1 C2 178.9(4) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C11 O11 Rh1 121.13(19) . 7 ? C11 N11 C17 119.6(3) . . ? C11 N11 Rh1 120.3(2) . . ? C17 N11 Rh1 120.09(19) . . ? O11 C11 N11 121.9(3) . . ? O11 C11 C12 113.9(3) . . ? N11 C11 C12 124.3(3) . . ? C11 C12 C13 115.2(3) . . ? C11 C12 H12A 108.5 . . ? C13 C12 H12A 108.5 . . ? C11 C12 H12B 108.5 . . ? C13 C12 H12B 108.5 . . ? H12A C12 H12B 107.5 . . ? C14 C13 C12 117.4(3) . . ? C14 C13 H13A 107.9 . . ? C12 C13 H13A 107.9 . . ? C14 C13 H13B 107.9 . . ? C12 C13 H13B 107.9 . . ? H13A C13 H13B 107.2 . . ? C15 C14 C13 116.3(3) . . ? C15 C14 H14A 108.2 . . ? C13 C14 H14A 108.2 . . ? C15 C14 H14B 108.2 . . ? C13 C14 H14B 108.2 . . ? H14A C14 H14B 107.4 . . ? C14 C15 C16 115.9(3) . . ? C14 C15 H15A 108.3 . . ? C16 C15 H15A 108.3 . . ? C14 C15 H15B 108.3 . . ? C16 C15 H15B 108.3 . . ? H15A C15 H15B 107.4 . . ? C17 C16 C15 114.6(3) . . ? C17 C16 H16A 108.6 . . ? C15 C16 H16A 108.6 . . ? C17 C16 H16B 108.6 . . ? C15 C16 H16B 108.6 . . ? H16A C16 H16B 107.6 . . ? N11 C17 C16 111.4(3) . . ? N11 C17 H17A 109.3 . . ? C16 C17 H17A 109.3 . . ? N11 C17 H17B 109.3 . . ? C16 C17 H17B 109.3 . . ? H17A C17 H17B 108.0 . . ? C21 O21 Rh1 121.33(19) . 7 ? C21 N21 C27 119.5(3) . . ? C21 N21 Rh1 120.3(2) . . ? C27 N21 Rh1 120.2(2) . . ? O21 C21 N21 121.9(3) . . ? O21 C21 C22 113.9(3) . . ? N21 C21 C22 124.2(3) . . ? C21 C22 C23 114.2(3) . . ? C21 C22 H22A 108.7 . . ? C23 C22 H22A 108.7 . . ? C21 C22 H22B 108.7 . . ? C23 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? C24 C23 C22 116.6(3) . . ? C24 C23 H23A 108.1 . . ? C22 C23 H23A 108.1 . . ? C24 C23 H23B 108.1 . . ? C22 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? C23 C24 C25 116.6(3) . . ? C23 C24 H24A 108.1 . . ? C25 C24 H24A 108.1 . . ? C23 C24 H24B 108.1 . . ? C25 C24 H24B 108.1 . . ? H24A C24 H24B 107.3 . . ? C26 C25 C24 116.0(3) . . ? C26 C25 H25A 108.3 . . ? C24 C25 H25A 108.3 . . ? C26 C25 H25B 108.3 . . ? C24 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? C25 C26 C27 113.8(3) . . ? C25 C26 H26A 108.8 . . ? C27 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? C27 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? N21 C27 C26 111.6(3) . . ? N21 C27 H27A 109.3 . . ? C26 C27 H27A 109.3 . . ? N21 C27 H27B 109.3 . . ? C26 C27 H27B 109.3 . . ? H27A C27 H27B 108.0 . . ? N1A C1A C2A 179.0(6) . . ? C1A C2A H2D 109.5 . . ? C1A C2A H2E 109.5 . . ? H2D C2A H2E 109.5 . . ? C1A C2A H2F 109.5 . . ? H2D C2A H2F 109.5 . . ? H2E C2A H2F 109.5 . . ? F2 B1 F4 108.3(7) . . ? F2 B1 F3 108.0(10) . . ? F4 B1 F3 110.5(10) . . ? F2 B1 F1 110.8(11) . . ? F4 B1 F1 109.8(11) . . ? F3 B1 F1 109.5(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N21 Rh1 N11 C11 86.2(2) . . . . ? O21 Rh1 N11 C11 -90.2(2) 7 . . . ? N1 Rh1 N11 C11 -178.2(2) . . . . ? Rh1 Rh1 N11 C11 -2.4(2) 7 . . . ? N21 Rh1 N11 C17 -92.1(2) . . . . ? O21 Rh1 N11 C17 91.5(2) 7 . . . ? N1 Rh1 N11 C17 3.5(2) . . . . ? Rh1 Rh1 N11 C17 179.3(2) 7 . . . ? Rh1 O11 C11 N11 -6.1(4) 7 . . . ? Rh1 O11 C11 C12 173.60(19) 7 . . . ? C17 N11 C11 O11 -176.1(3) . . . . ? Rh1 N11 C11 O11 5.6(4) . . . . ? C17 N11 C11 C12 4.3(4) . . . . ? Rh1 N11 C11 C12 -174.0(2) . . . . ? O11 C11 C12 C13 96.0(3) . . . . ? N11 C11 C12 C13 -84.4(4) . . . . ? C11 C12 C13 C14 71.2(4) . . . . ? C12 C13 C14 C15 -66.5(4) . . . . ? C13 C14 C15 C16 97.4(4) . . . . ? C14 C15 C16 C17 -52.3(4) . . . . ? C11 N11 C17 C16 94.2(3) . . . . ? Rh1 N11 C17 C16 -87.5(3) . . . . ? C15 C16 C17 N11 -56.8(4) . . . . ? N11 Rh1 N21 C21 -86.7(2) . . . . ? O11 Rh1 N21 C21 89.8(2) 7 . . . ? N1 Rh1 N21 C21 177.9(2) . . . . ? Rh1 Rh1 N21 C21 1.9(2) 7 . . . ? N11 Rh1 N21 C27 95.6(2) . . . . ? O11 Rh1 N21 C27 -88.0(2) 7 . . . ? N1 Rh1 N21 C27 0.1(2) . . . . ? Rh1 Rh1 N21 C27 -175.9(2) 7 . . . ? Rh1 O21 C21 N21 4.0(4) 7 . . . ? Rh1 O21 C21 C22 -176.15(19) 7 . . . ? C27 N21 C21 O21 173.8(3) . . . . ? Rh1 N21 C21 O21 -3.9(4) . . . . ? C27 N21 C21 C22 -6.0(4) . . . . ? Rh1 N21 C21 C22 176.2(2) . . . . ? O21 C21 C22 C23 -93.0(3) . . . . ? N21 C21 C22 C23 86.9(4) . . . . ? C21 C22 C23 C24 -71.5(4) . . . . ? C22 C23 C24 C25 65.6(4) . . . . ? C23 C24 C25 C26 -98.4(4) . . . . ? C24 C25 C26 C27 54.3(4) . . . . ? C21 N21 C27 C26 -93.5(3) . . . . ? Rh1 N21 C27 C26 84.3(3) . . . . ? C25 C26 C27 N21 55.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.633 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.075 _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 -0.0407392 _diffrn_orient_matrix_UB_12 0.0350636 _diffrn_orient_matrix_UB_13 -0.0120117 _diffrn_orient_matrix_UB_21 -0.0026063 _diffrn_orient_matrix_UB_22 -0.0641292 _diffrn_orient_matrix_UB_23 -0.0368613 _diffrn_orient_matrix_UB_31 -0.0105821 _diffrn_orient_matrix_UB_32 -0.1189938 _diffrn_orient_matrix_UB_33 0.0163348 _symmetry_space_group_name_Hall '-C 2yc' _exptl_crystal_id 'Doyle/Zhou Rh2 + 8 member ring + CH3CN' _diffrn_measurement_frame_width-CCD -0.5 _diffrn_measurement_details 366,366,366,720 _diffrn_measurement_total_frames-CCD 1818 _diffrn_measurement_frame_time-CCD 40 _diffrn_measurement_total_time-CCD 23.2 _diffrn_source_voltage 50.00 _diffrn_source_current 30.00 _diffrn_detector_distance-CCD 5.0000 _diffrn_measurement_frame_size-CCD 512 _diffrn_measurement_specimen_support 'glass capillary' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart Apex II' _publ_section_references ; Bruker (2005). Apex2. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Spek, A. L. (1990). Acta Cryst., A46, C-34. ; #~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~~ # Attachment 'Cif_file_of_the_x-ray_structural_analysis_of_O.cif.txt' data_1613 _database_code_depnum_ccdc_archive 'CCDC 722155' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Rh2-complex ; _chemical_name_common Rh2-complex _chemical_formula_moiety 'C36 H50 N4 O4 Rh2' _chemical_formula_sum 'C36 H50 N4 O4 Rh2' _chemical_formula_weight 808.62 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5366(8) _cell_length_b 20.8840(19) _cell_length_c 10.0597(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.8290(10) _cell_angle_gamma 90.00 _cell_volume 1664.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6253 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.9 _exptl_crystal_description prism _exptl_crystal_colour orange/green _exptl_crystal_size_max 0.147 _exptl_crystal_size_mid 0.092 _exptl_crystal_size_min 0.041 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method not-measured _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 1.037 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'three-circle diffractometer' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12334 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2923 _reflns_number_gt 2684 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker, 2004)' _computing_publication_material SHELXL-97 _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 'w=1/[\s^2^(Fo^2^)+(0.008P)^2^+17.6P], P=(max(Fo^2^,0)+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 2923 _refine_ls_number_parameters 208 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0557 _refine_ls_R_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.1176 _refine_ls_wR_factor_gt 0.1162 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 1.02301(6) 0.05348(2) 0.45453(5) 0.03395(17) Uani 1 1 d . . . C1 C 1.1472(8) 0.1238(3) 0.4038(7) 0.0372(14) Uani 1 1 d . . . C2 C 1.2782(9) 0.1560(3) 0.5086(8) 0.0430(16) Uani 1 1 d . . . H2 H 1.3138 0.1426 0.6056 0.052 Uiso 1 1 calc R . . C3 C 1.3566(10) 0.2070(3) 0.4725(9) 0.0512(18) Uani 1 1 d . . . H3 H 1.4422 0.2299 0.5454 0.061 Uiso 1 1 calc R . . C4 C 1.3120(10) 0.2249(4) 0.3324(9) 0.056(2) Uani 1 1 d . . . H4 H 1.3683 0.2596 0.3081 0.068 Uiso 1 1 calc R . . C5 C 1.1845(10) 0.1924(4) 0.2254(9) 0.0534(19) Uani 1 1 d . . . H5 H 1.1529 0.2048 0.1281 0.064 Uiso 1 1 calc R . . C6 C 1.1034(9) 0.1413(3) 0.2623(7) 0.0412(15) Uani 1 1 d . . . H6 H 1.0175 0.1184 0.1895 0.049 Uiso 1 1 calc R . . N1 N 0.7809(6) 0.0788(2) 0.3592(6) 0.0357(12) Uani 1 1 d . . . O1 O 0.7328(5) -0.0179(2) 0.4410(5) 0.0419(11) Uani 1 1 d . . . C11 C 0.6798(8) 0.0350(3) 0.3730(7) 0.0371(14) Uani 1 1 d . . . C12 C 0.4903(8) 0.0431(4) 0.3085(8) 0.0485(17) Uani 1 1 d . . . H12A H 0.4371 0.0096 0.3473 0.058 Uiso 1 1 calc R . . H12B H 0.4602 0.0852 0.3374 0.058 Uiso 1 1 calc R . . C13 C 0.4203(11) 0.0388(4) 0.1472(9) 0.065(2) Uani 1 1 d . . . H13A H 0.2981 0.0293 0.1143 0.078 Uiso 1 1 calc R . . H13B H 0.4752 0.0025 0.1184 0.078 Uiso 1 1 calc R . . C14 C 0.4438(11) 0.0987(4) 0.0713(10) 0.068(2) Uani 1 1 d . . . H14A H 0.3971 0.0906 -0.0332 0.082 Uiso 1 1 calc R . . H14B H 0.3770 0.1338 0.0905 0.082 Uiso 1 1 calc R . . C15 C 0.6248(11) 0.1214(4) 0.1133(10) 0.070(2) Uani 1 1 d . . . H15A H 0.6260 0.1603 0.0573 0.084 Uiso 1 1 calc R . . H15B H 0.6903 0.0879 0.0873 0.084 Uiso 1 1 calc R . . C16 C 0.7117(10) 0.1367(4) 0.2727(10) 0.062(2) Uani 1 1 d . . . H16A H 0.8045 0.1675 0.2859 0.075 Uiso 1 1 calc R . . H16B H 0.6295 0.1572 0.3073 0.075 Uiso 1 1 calc R . . N2 N 1.0208(7) 0.0928(2) 0.6376(6) 0.0386(13) Uani 1 1 d . . . O2 O 0.9917(6) -0.0050(2) 0.7265(5) 0.0409(11) Uani 1 1 d . . . C21 C 1.0008(9) 0.0570(3) 0.7334(7) 0.0421(15) Uani 1 1 d . . . C22 C 0.9844(11) 0.0849(4) 0.8652(8) 0.056(2) Uani 1 1 d . . . H22A H 1.0725 0.1180 0.9048 0.067 Uiso 1 1 calc R . . H22B H 1.0060 0.0507 0.9380 0.067 Uiso 1 1 calc R . . C23 C 0.8116(15) 0.1150(5) 0.8402(12) 0.090(3) Uani 1 1 d . . . H23A H 0.7935 0.1154 0.9319 0.108 Uiso 1 1 calc R . . H23B H 0.7224 0.0880 0.7720 0.108 Uiso 1 1 calc R . . C24 C 0.7940(13) 0.1837(5) 0.7813(10) 0.076(3) Uani 1 1 d . . . H24A H 0.6805 0.2001 0.7686 0.091 Uiso 1 1 calc R . . H24B H 0.8783 0.2113 0.8525 0.091 Uiso 1 1 calc R . . C25 C 0.8183(12) 0.1886(5) 0.6385(10) 0.071(2) Uani 1 1 d . . . H25A H 0.8042 0.2338 0.6068 0.086 Uiso 1 1 calc R . . H25B H 0.7293 0.1632 0.5657 0.086 Uiso 1 1 calc R . . C26 C 0.9930(13) 0.1646(4) 0.6464(11) 0.075(3) Uani 1 1 d . . . H26A H 1.0175 0.1855 0.5679 0.090 Uiso 1 1 calc R . . H26B H 1.0782 0.1803 0.7375 0.090 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 0.0377(3) 0.0281(3) 0.0404(3) -0.0026(2) 0.0195(2) -0.0022(2) C1 0.043(4) 0.026(3) 0.051(4) 0.001(3) 0.027(3) 0.001(3) C2 0.044(4) 0.038(4) 0.047(4) 0.000(3) 0.019(3) -0.004(3) C3 0.050(4) 0.042(4) 0.061(5) 0.001(4) 0.021(4) -0.007(3) C4 0.060(5) 0.041(4) 0.073(6) 0.009(4) 0.030(4) -0.006(4) C5 0.064(5) 0.049(4) 0.054(5) 0.012(4) 0.029(4) 0.002(4) C6 0.042(4) 0.040(4) 0.043(4) 0.000(3) 0.018(3) -0.002(3) N1 0.030(3) 0.027(3) 0.050(3) -0.002(2) 0.015(2) 0.005(2) O1 0.030(2) 0.045(3) 0.051(3) 0.008(2) 0.016(2) 0.000(2) C11 0.034(3) 0.034(3) 0.045(4) -0.004(3) 0.017(3) -0.001(3) C12 0.039(4) 0.046(4) 0.063(5) 0.004(3) 0.022(3) 0.005(3) C13 0.059(5) 0.062(5) 0.075(6) 0.000(4) 0.026(4) 0.001(4) C14 0.067(6) 0.069(6) 0.072(6) 0.013(5) 0.030(5) 0.017(5) C15 0.073(6) 0.062(5) 0.085(7) 0.018(5) 0.040(5) 0.016(5) C16 0.049(5) 0.041(4) 0.103(7) 0.004(4) 0.035(5) 0.007(4) N2 0.054(3) 0.028(3) 0.042(3) -0.009(2) 0.027(3) -0.011(2) O2 0.054(3) 0.031(2) 0.041(3) -0.0019(19) 0.022(2) 0.000(2) C21 0.047(4) 0.038(4) 0.039(4) -0.007(3) 0.013(3) 0.002(3) C22 0.077(6) 0.044(4) 0.049(4) -0.008(3) 0.026(4) 0.001(4) C23 0.124(9) 0.077(7) 0.095(8) -0.005(6) 0.072(7) -0.003(6) C24 0.083(7) 0.070(6) 0.078(6) -0.005(5) 0.034(5) 0.012(5) C25 0.077(6) 0.068(6) 0.072(6) -0.002(5) 0.031(5) 0.007(5) C26 0.087(7) 0.058(5) 0.092(7) -0.010(5) 0.047(6) -0.010(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 1.986(6) . ? Rh1 N1 1.999(5) . ? Rh1 N2 2.023(5) . ? Rh1 O2 2.047(4) 3_756 ? Rh1 O1 2.091(4) 3_756 ? Rh1 Rh1 2.4994(10) 3_756 ? C1 C6 1.380(9) . ? C1 C2 1.391(9) . ? C2 C3 1.376(9) . ? C3 C4 1.369(11) . ? C4 C5 1.390(11) . ? C5 C6 1.396(10) . ? N1 C11 1.300(8) . ? N1 C16 1.478(9) . ? O1 C11 1.289(8) . ? O1 Rh1 2.091(4) 3_756 ? C11 C12 1.512(9) . ? C12 C13 1.509(11) . ? C13 C14 1.518(11) . ? C14 C15 1.518(12) . ? C15 C16 1.530(12) . ? N2 C21 1.281(8) . ? N2 C26 1.526(10) . ? O2 C21 1.296(8) . ? O2 Rh1 2.047(4) 3_756 ? C21 C22 1.502(9) . ? C22 C23 1.536(13) . ? C23 C24 1.538(13) . ? C24 C25 1.529(12) . ? C25 C26 1.547(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 Rh1 N1 103.7(2) . . ? C1 Rh1 N2 96.9(2) . . ? N1 Rh1 N2 88.4(2) . . ? C1 Rh1 O2 90.0(2) . 3_756 ? N1 Rh1 O2 89.6(2) . 3_756 ? N2 Rh1 O2 173.13(19) . 3_756 ? C1 Rh1 O1 82.2(2) . 3_756 ? N1 Rh1 O1 174.05(19) . 3_756 ? N2 Rh1 O1 91.8(2) . 3_756 ? O2 Rh1 O1 89.50(19) 3_756 3_756 ? C1 Rh1 Rh1 157.90(19) . 3_756 ? N1 Rh1 Rh1 97.86(15) . 3_756 ? N2 Rh1 Rh1 88.51(15) . 3_756 ? O2 Rh1 Rh1 85.26(12) 3_756 3_756 ? O1 Rh1 Rh1 76.21(12) 3_756 3_756 ? C6 C1 C2 119.2(6) . . ? C6 C1 Rh1 119.6(5) . . ? C2 C1 Rh1 121.2(5) . . ? C3 C2 C1 120.5(7) . . ? C4 C3 C2 120.4(7) . . ? C3 C4 C5 120.1(7) . . ? C4 C5 C6 119.4(7) . . ? C1 C6 C5 120.4(7) . . ? C11 N1 C16 120.2(6) . . ? C11 N1 Rh1 111.8(4) . . ? C16 N1 Rh1 127.9(4) . . ? C11 O1 Rh1 131.2(4) . 3_756 ? O1 C11 N1 122.9(6) . . ? O1 C11 C12 115.6(6) . . ? N1 C11 C12 121.5(6) . . ? C13 C12 C11 112.8(6) . . ? C12 C13 C14 114.8(7) . . ? C15 C14 C13 115.4(7) . . ? C14 C15 C16 113.8(7) . . ? N1 C16 C15 112.3(7) . . ? C21 N2 C26 117.6(6) . . ? C21 N2 Rh1 119.7(4) . . ? C26 N2 Rh1 120.4(5) . . ? C21 O2 Rh1 121.6(4) . 3_756 ? N2 C21 O2 124.4(6) . . ? N2 C21 C22 121.3(6) . . ? O2 C21 C22 114.3(6) . . ? C21 C22 C23 114.4(7) . . ? C22 C23 C24 113.3(8) . . ? C25 C24 C23 113.4(8) . . ? C24 C25 C26 113.3(8) . . ? N2 C26 C25 118.9(7) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.600 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.099 _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 0.1225302 _diffrn_orient_matrix_UB_12 -0.0000644 _diffrn_orient_matrix_UB_13 0.0624308 _diffrn_orient_matrix_UB_21 0.0086237 _diffrn_orient_matrix_UB_22 0.0459420 _diffrn_orient_matrix_UB_23 -0.0244473 _diffrn_orient_matrix_UB_31 -0.0289148 _diffrn_orient_matrix_UB_32 0.0134937 _diffrn_orient_matrix_UB_33 0.0834970 _symmetry_space_group_name_Hall '-P 2ybc' _exptl_crystal_id 'Doyle/Xie JXie-01-57' _diffrn_measurement_frame_width-CCD 0.3 _diffrn_measurement_details 151,360,610,610 _diffrn_measurement_total_frames-CCD 1731 _diffrn_measurement_frame_time-CCD 30 _diffrn_measurement_total_time-CCD 21.9 _diffrn_source_voltage 50 _diffrn_source_current 30 _diffrn_detector_distance-CCD 5.2000 _diffrn_measurement_frame_size-CCD 1024 _diffrn_measurement_specimen_support 'cactus needle' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart Apex II' _publ_section_references ; Bruker (2005). Apex2. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (1990). Acta Cryst. A46, 467-473. Sheldrick, G. M. (1996). SADABS. University of G\"ottingen, Germany. Sheldrick, G. M. (1997). SHELXL-97. University of G\"ottingen, Germany. Spek, A. L. (1990). Acta Cryst., A46, C-34. ; # Attachment 'Cif_file_of_the_x-ray_structural_analysis_of_PhACO.cif.txt' data_1701 _database_code_depnum_ccdc_archive 'CCDC 722156' _audit_creation_method 'SHELXL-97 & ZCIF' _chemical_name_systematic ; Rh2 complex ; _chemical_name_common 'Rh2 complex' _chemical_formula_moiety 'C40 H58 N4 O4 Rh2, 2(C H2 Cl2)' _chemical_formula_sum 'C42 H62 Cl4 N4 O4 Rh2' _chemical_formula_weight 1034.58 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' 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 10.0542(3) _cell_length_b 11.0233(3) _cell_length_c 11.6576(3) _cell_angle_alpha 88.0671(4) _cell_angle_beta 65.9778(3) _cell_angle_gamma 69.4042(4) _cell_volume 1095.59(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 21281 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 32.1 _exptl_crystal_description prism _exptl_crystal_colour purple _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.275 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.568 _exptl_crystal_density_method not-measured _exptl_crystal_F_000 532 _exptl_absorpt_coefficient_mu 1.043 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.686 _exptl_absorpt_correction_T_max 0.751 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _diffrn_ambient_temperature 200(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 'three-circle diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 11.198 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22338 _diffrn_reflns_av_R_equivalents 0.0580 _diffrn_reflns_av_sigmaI/netI 0.0328 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 30.00 _reflns_number_total 6347 _reflns_number_gt 6166 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (Bruker, 2005)' _computing_cell_refinement Apex2 _computing_data_reduction Apex2 _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHEL (Bruker, 2004)' _computing_publication_material SHELXL-97 _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 'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+1.091P], P=(max(Fo^2^,0)+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment refU _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6347 _refine_ls_number_parameters 290 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0207 _refine_ls_R_factor_gt 0.0199 _refine_ls_wR_factor_ref 0.0466 _refine_ls_wR_factor_gt 0.0464 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.003 _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 0.430393(11) 0.421754(9) 0.043074(9) 0.01432(3) Uani 1 1 d . . . N1 N 0.23041(13) 0.58538(10) 0.13268(10) 0.01771(19) Uani 1 1 d . B . O1 O 0.35742(11) 0.72644(9) 0.04471(9) 0.02028(18) Uani 1 1 d . . . C11 C 0.23351(15) 0.70314(12) 0.11439(12) 0.0180(2) Uani 1 1 d . B . C12 C 0.08951(16) 0.82788(13) 0.17310(15) 0.0248(3) Uani 1 1 d . . . H12A H -0.0041 0.8081 0.1908 0.039(4) Uiso 1 1 calc R A 1 H12B H 0.0946 0.8908 0.1115 0.039(4) Uiso 1 1 calc R A 1 C13 C 0.0728(2) 0.89071(16) 0.29485(17) 0.0349(3) Uani 0.718(5) 1 d PDU B 1 H13A H 0.0020 0.9823 0.3109 0.033(5) Uiso 0.718(5) 1 calc PR B 1 H13B H 0.1755 0.8894 0.2833 0.033(5) Uiso 0.718(5) 1 calc PR B 1 C14 C 0.0101(3) 0.8237(3) 0.4111(2) 0.0392(6) Uani 0.718(5) 1 d PDU B 1 H14A H -0.0110 0.8770 0.4866 0.046(6) Uiso 0.718(5) 1 calc PR B 1 H14B H -0.0898 0.8207 0.4198 0.046(6) Uiso 0.718(5) 1 calc PR B 1 C15 C 0.1205(3) 0.6848(3) 0.4067(2) 0.0421(7) Uani 0.718(5) 1 d PDU B 1 H15A H 0.1181 0.6725 0.4910 0.049(6) Uiso 0.718(5) 1 calc PR B 1 H15B H 0.2277 0.6745 0.3483 0.049(6) Uiso 0.718(5) 1 calc PR B 1 C16 C 0.0780(2) 0.57775(17) 0.36418(16) 0.0380(4) Uani 0.718(5) 1 d PDU B 1 H16A H 0.1480 0.4926 0.3713 0.039(5) Uiso 0.718(5) 1 calc PR B 1 H16B H -0.0290 0.5886 0.4237 0.039(5) Uiso 0.718(5) 1 calc PR B 1 C13A C 0.0728(2) 0.89071(16) 0.29485(17) 0.0349(3) Uani 0.282(5) 1 d PDU B 2 H13C H -0.0346 0.9545 0.3378 0.033(5) Uiso 0.282(5) 1 calc PR B 2 H13D H 0.1432 0.9392 0.2721 0.033(5) Uiso 0.282(5) 1 calc PR B 2 C14A C 0.1077(9) 0.7972(6) 0.3919(5) 0.0365(15) Uani 0.282(5) 1 d PDU B 2 H14C H 0.2166 0.7355 0.3516 0.046(6) Uiso 0.282(5) 1 calc PR B 2 H14D H 0.0964 0.8490 0.4644 0.046(6) Uiso 0.282(5) 1 calc PR B 2 C15A C -0.0007(7) 0.7209(5) 0.4394(5) 0.0344(14) Uani 0.282(5) 1 d PDU B 2 H15C H -0.0977 0.7684 0.4300 0.049(6) Uiso 0.282(5) 1 calc PR B 2 H15D H -0.0282 0.7145 0.5296 0.049(6) Uiso 0.282(5) 1 calc PR B 2 C16A C 0.0780(2) 0.57775(17) 0.36418(16) 0.0380(4) Uani 0.282(5) 1 d PDU B 2 H16C H 0.1843 0.5372 0.3591 0.039(5) Uiso 0.282(5) 1 calc PR B 2 H16D H 0.0180 0.5253 0.4122 0.039(5) Uiso 0.282(5) 1 calc PR B 2 C17 C 0.08684(17) 0.57422(14) 0.23106(14) 0.0253(3) Uani 1 1 d . . . H17A H 0.0803 0.4920 0.2093 0.037(4) Uiso 1 1 calc R B 1 H17B H -0.0043 0.6458 0.2303 0.037(4) Uiso 1 1 calc R B 1 N2 N 0.45856(13) 0.39575(11) 0.20473(10) 0.0183(2) Uani 1 1 d . . . O2 O 0.56468(12) 0.55123(9) 0.13796(9) 0.02083(18) Uani 1 1 d . . . C21 C 0.52397(15) 0.47414(12) 0.21950(12) 0.0182(2) Uani 1 1 d . . . C22 C 0.55523(18) 0.48609(14) 0.33449(13) 0.0236(3) Uani 1 1 d . . . H22A H 0.4829 0.4585 0.4060 0.030(3) Uiso 1 1 calc R . . H22B H 0.5334 0.5781 0.3571 0.030(3) Uiso 1 1 calc R . . C23 C 0.72368(19) 0.40451(16) 0.31396(15) 0.0296(3) Uani 1 1 d . . . H23A H 0.7955 0.4175 0.2318 0.031(3) Uiso 1 1 calc R . . H23B H 0.7447 0.4373 0.3794 0.031(3) Uiso 1 1 calc R . . C24 C 0.7597(2) 0.25848(17) 0.31725(18) 0.0359(4) Uani 1 1 d . . . H24A H 0.6872 0.2455 0.3991 0.045(4) Uiso 1 1 calc R . . H24B H 0.8660 0.2165 0.3118 0.045(4) Uiso 1 1 calc R . . C25 C 0.7477(2) 0.18945(16) 0.21132(17) 0.0332(3) Uani 1 1 d . . . H25A H 0.7656 0.2399 0.1394 0.037(4) Uiso 1 1 calc R . . H25B H 0.8328 0.1035 0.1832 0.037(4) Uiso 1 1 calc R . . C26 C 0.5933(2) 0.16984(15) 0.24409(18) 0.0326(3) Uani 1 1 d . . . H26A H 0.5796 0.1139 0.3118 0.042(4) Uiso 1 1 calc R . . H26B H 0.6040 0.1218 0.1696 0.042(4) Uiso 1 1 calc R . . C27 C 0.44272(18) 0.29270(14) 0.28619(14) 0.0245(3) Uani 1 1 d . . . H27A H 0.3578 0.2682 0.2866 0.028(3) Uiso 1 1 calc R . . H27B H 0.4132 0.3273 0.3730 0.028(3) Uiso 1 1 calc R . . C31 C 0.31543(15) 0.30861(12) 0.03735(12) 0.0177(2) Uani 1 1 d . . . C32 C 0.36004(17) 0.18097(13) 0.06540(14) 0.0228(3) Uani 1 1 d . . . H32 H 0.4458 0.1471 0.0866 0.028(5) Uiso 1 1 calc R . . C33 C 0.27779(18) 0.10292(14) 0.06224(16) 0.0277(3) Uani 1 1 d . . . H33 H 0.3076 0.0171 0.0824 0.038(5) Uiso 1 1 calc R . . C34 C 0.15270(18) 0.15130(15) 0.02954(16) 0.0283(3) Uani 1 1 d . . . H34 H 0.0973 0.0987 0.0278 0.034(5) Uiso 1 1 calc R . . C35 C 0.10948(17) 0.27837(14) -0.00078(15) 0.0256(3) Uani 1 1 d . . . H35 H 0.0247 0.3115 -0.0231 0.031(5) Uiso 1 1 calc R . . C36 C 0.19097(16) 0.35657(13) 0.00177(13) 0.0211(2) Uani 1 1 d . . . H36 H 0.1625 0.4417 -0.0204 0.031(5) Uiso 1 1 calc R . . C1 C 0.4672(2) 0.15378(18) 0.72168(18) 0.0388(4) Uani 1 1 d . . . H1A H 0.4873 0.2248 0.7513 0.051(5) Uiso 1 1 calc R . . H1B H 0.4137 0.1163 0.7958 0.051(5) Uiso 1 1 calc R . . Cl1 Cl 0.64585(6) 0.03320(6) 0.62097(6) 0.05963(15) Uani 1 1 d . . . Cl2 Cl 0.34564(7) 0.21663(6) 0.64222(6) 0.05770(14) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01686(5) 0.01331(4) 0.01436(5) 0.00328(3) -0.00728(3) -0.00667(3) N1 0.0175(5) 0.0171(5) 0.0175(5) 0.0020(4) -0.0064(4) -0.0065(4) O1 0.0197(4) 0.0159(4) 0.0230(5) 0.0036(3) -0.0073(4) -0.0062(3) C11 0.0193(5) 0.0170(5) 0.0180(5) 0.0014(4) -0.0098(5) -0.0047(4) C12 0.0200(6) 0.0179(6) 0.0323(7) 0.0009(5) -0.0110(5) -0.0022(5) C13 0.0344(8) 0.0245(7) 0.0398(9) -0.0094(6) -0.0135(7) -0.0055(6) C14 0.0325(14) 0.0424(13) 0.0300(12) -0.0144(9) -0.0130(10) 0.0020(10) C15 0.0385(14) 0.0512(14) 0.0230(11) -0.0048(10) -0.0169(10) 0.0042(11) C16 0.0411(9) 0.0349(8) 0.0225(7) 0.0093(6) -0.0043(7) -0.0079(7) C13A 0.0344(8) 0.0245(7) 0.0398(9) -0.0094(6) -0.0135(7) -0.0055(6) C14A 0.046(4) 0.042(3) 0.025(3) -0.003(2) -0.016(3) -0.017(3) C15A 0.034(3) 0.040(3) 0.020(2) -0.0021(19) -0.007(2) -0.008(2) C16A 0.0411(9) 0.0349(8) 0.0225(7) 0.0093(6) -0.0043(7) -0.0079(7) C17 0.0213(6) 0.0247(6) 0.0231(6) 0.0008(5) -0.0018(5) -0.0096(5) N2 0.0216(5) 0.0184(5) 0.0165(5) 0.0057(4) -0.0094(4) -0.0079(4) O2 0.0289(5) 0.0222(4) 0.0172(4) 0.0066(3) -0.0121(4) -0.0135(4) C21 0.0201(5) 0.0187(5) 0.0150(5) 0.0028(4) -0.0082(4) -0.0056(4) C22 0.0314(7) 0.0262(6) 0.0173(6) 0.0039(5) -0.0137(5) -0.0113(5) C23 0.0324(7) 0.0353(8) 0.0292(7) 0.0059(6) -0.0199(6) -0.0135(6) C24 0.0386(9) 0.0346(8) 0.0416(9) 0.0089(7) -0.0278(8) -0.0091(7) C25 0.0319(8) 0.0283(7) 0.0396(9) 0.0029(6) -0.0208(7) -0.0044(6) C26 0.0411(9) 0.0224(7) 0.0447(9) 0.0128(6) -0.0284(8) -0.0120(6) C27 0.0317(7) 0.0246(6) 0.0234(6) 0.0117(5) -0.0146(6) -0.0149(6) C31 0.0191(5) 0.0169(5) 0.0183(5) 0.0023(4) -0.0071(5) -0.0087(4) C32 0.0243(6) 0.0186(6) 0.0290(7) 0.0063(5) -0.0136(5) -0.0093(5) C33 0.0313(7) 0.0199(6) 0.0357(8) 0.0074(5) -0.0147(6) -0.0137(5) C34 0.0287(7) 0.0260(7) 0.0355(8) 0.0035(6) -0.0128(6) -0.0169(6) C35 0.0240(6) 0.0270(7) 0.0307(7) 0.0029(5) -0.0142(6) -0.0118(5) C36 0.0224(6) 0.0187(5) 0.0239(6) 0.0032(5) -0.0113(5) -0.0077(5) C1 0.0437(10) 0.0371(9) 0.0325(8) -0.0003(7) -0.0124(7) -0.0153(8) Cl1 0.0351(2) 0.0642(3) 0.0683(4) -0.0157(3) -0.0149(2) -0.0117(2) Cl2 0.0453(3) 0.0679(4) 0.0621(3) 0.0021(3) -0.0276(3) -0.0171(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 C31 1.9947(12) . ? Rh1 N2 2.0137(11) . ? Rh1 O1 2.0373(9) 2_665 ? Rh1 N1 2.0623(11) . ? Rh1 O2 2.1043(9) 2_665 ? Rh1 Rh1 2.52606(19) 2_665 ? N1 C11 1.3175(16) . ? N1 C17 1.4770(17) . ? O1 C11 1.2903(16) . ? O1 Rh1 2.0373(9) 2_665 ? C11 C12 1.5204(18) . ? C12 C13 1.521(2) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 C14 1.531(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 C15 1.531(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C15 C16 1.545(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C16 C17 1.519(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C14A C15A 1.525(7) . ? C14A H14C 0.9800 . ? C14A H14D 0.9800 . ? C15A H15C 0.9800 . ? C15A H15D 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? N2 C21 1.3079(17) . ? N2 C27 1.4659(16) . ? O2 C21 1.2911(15) . ? O2 Rh1 2.1043(9) 2_665 ? C21 C22 1.5157(18) . ? C22 C23 1.532(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C23 C24 1.523(2) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C24 C25 1.539(2) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C25 C26 1.533(2) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C26 C27 1.538(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C31 C32 1.3900(17) . ? C31 C36 1.3998(18) . ? C32 C33 1.3975(19) . ? C32 H32 0.9400 . ? C33 C34 1.384(2) . ? C33 H33 0.9400 . ? C34 C35 1.393(2) . ? C34 H34 0.9400 . ? C35 C36 1.3906(19) . ? C35 H35 0.9400 . ? C36 H36 0.9400 . ? C1 Cl1 1.7550(19) . ? C1 Cl2 1.765(2) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C31 Rh1 N2 105.55(5) . . ? C31 Rh1 O1 92.28(4) . 2_665 ? N2 Rh1 O1 87.34(4) . 2_665 ? C31 Rh1 N1 94.62(5) . . ? N2 Rh1 N1 90.73(4) . . ? O1 Rh1 N1 173.10(4) 2_665 . ? C31 Rh1 O2 81.10(4) . 2_665 ? N2 Rh1 O2 171.41(4) . 2_665 ? O1 Rh1 O2 86.97(4) 2_665 2_665 ? N1 Rh1 O2 94.17(4) . 2_665 ? C31 Rh1 Rh1 154.42(4) . 2_665 ? N2 Rh1 Rh1 99.99(3) . 2_665 ? O1 Rh1 Rh1 87.47(3) 2_665 2_665 ? N1 Rh1 Rh1 86.33(3) . 2_665 ? O2 Rh1 Rh1 73.34(3) 2_665 2_665 ? C11 N1 C17 118.17(11) . . ? C11 N1 Rh1 120.48(9) . . ? C17 N1 Rh1 120.86(8) . . ? C11 O1 Rh1 121.10(8) . 2_665 ? O1 C11 N1 124.43(12) . . ? O1 C11 C12 112.18(11) . . ? N1 C11 C12 123.39(12) . . ? C11 C12 C13 113.75(12) . . ? C11 C12 H12A 108.8 . . ? C13 C12 H12A 108.8 . . ? C11 C12 H12B 108.8 . . ? C13 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? C12 C13 C14 113.99(15) . . ? C12 C13 H13A 108.8 . . ? C14 C13 H13A 108.8 . . ? C12 C13 H13B 108.8 . . ? C14 C13 H13B 108.8 . . ? H13A C13 H13B 107.6 . . ? C15 C14 C13 114.4(2) . . ? C15 C14 H14A 108.6 . . ? C13 C14 H14A 108.6 . . ? C15 C14 H14B 108.6 . . ? C13 C14 H14B 108.6 . . ? H14A C14 H14B 107.6 . . ? C14 C15 C16 113.4(2) . . ? C14 C15 H15A 108.9 . . ? C16 C15 H15A 108.9 . . ? C14 C15 H15B 108.9 . . ? C16 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? C17 C16 C15 116.86(15) . . ? C17 C16 H16A 108.1 . . ? C15 C16 H16A 108.1 . . ? C17 C16 H16B 108.1 . . ? C15 C16 H16B 108.1 . . ? H16A C16 H16B 107.3 . . ? C15A C14A H14C 109.0 . . ? C15A C14A H14D 109.0 . . ? H14C C14A H14D 107.8 . . ? C14A C15A H15C 109.2 . . ? C14A C15A H15D 109.2 . . ? H15C C15A H15D 107.9 . . ? N1 C17 C16 114.47(13) . . ? N1 C17 H17A 108.6 . . ? C16 C17 H17A 108.6 . . ? N1 C17 H17B 108.6 . . ? C16 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C21 N2 C27 120.39(11) . . ? C21 N2 Rh1 109.07(8) . . ? C27 N2 Rh1 129.53(9) . . ? C21 O2 Rh1 134.27(8) . 2_665 ? O2 C21 N2 122.70(12) . . ? O2 C21 C22 113.64(11) . . ? N2 C21 C22 123.64(12) . . ? C21 C22 C23 113.44(12) . . ? C21 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? C24 C23 C22 114.85(13) . . ? C24 C23 H23A 108.6 . . ? C22 C23 H23A 108.6 . . ? C24 C23 H23B 108.6 . . ? C22 C23 H23B 108.6 . . ? H23A C23 H23B 107.5 . . ? C23 C24 C25 114.91(13) . . ? C23 C24 H24A 108.5 . . ? C25 C24 H24A 108.5 . . ? C23 C24 H24B 108.5 . . ? C25 C24 H24B 108.5 . . ? H24A C24 H24B 107.5 . . ? C26 C25 C24 116.85(15) . . ? C26 C25 H25A 108.1 . . ? C24 C25 H25A 108.1 . . ? C26 C25 H25B 108.1 . . ? C24 C25 H25B 108.1 . . ? H25A C25 H25B 107.3 . . ? C25 C26 C27 117.52(13) . . ? C25 C26 H26A 107.9 . . ? C27 C26 H26A 107.9 . . ? C25 C26 H26B 107.9 . . ? C27 C26 H26B 107.9 . . ? H26A C26 H26B 107.2 . . ? N2 C27 C26 113.38(12) . . ? N2 C27 H27A 108.9 . . ? C26 C27 H27A 108.9 . . ? N2 C27 H27B 108.9 . . ? C26 C27 H27B 108.9 . . ? H27A C27 H27B 107.7 . . ? C32 C31 C36 119.39(12) . . ? C32 C31 Rh1 120.64(10) . . ? C36 C31 Rh1 119.95(9) . . ? C31 C32 C33 120.18(13) . . ? C31 C32 H32 119.9 . . ? C33 C32 H32 119.9 . . ? C34 C33 C32 120.38(13) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C33 C34 C35 119.56(13) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C36 C35 C34 120.43(13) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C31 120.02(12) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? Cl1 C1 Cl2 110.77(10) . . ? Cl1 C1 H1A 109.5 . . ? Cl2 C1 H1A 109.5 . . ? Cl1 C1 H1B 109.5 . . ? Cl2 C1 H1B 109.5 . . ? H1A C1 H1B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C31 Rh1 N1 C11 -150.74(10) . . . . ? N2 Rh1 N1 C11 103.60(10) . . . . ? O2 Rh1 N1 C11 -69.34(10) 2_665 . . . ? Rh1 Rh1 N1 C11 3.64(10) 2_665 . . . ? C31 Rh1 N1 C17 37.42(11) . . . . ? N2 Rh1 N1 C17 -68.24(10) . . . . ? O2 Rh1 N1 C17 118.81(10) 2_665 . . . ? Rh1 Rh1 N1 C17 -168.21(10) 2_665 . . . ? Rh1 O1 C11 N1 -1.86(18) 2_665 . . . ? Rh1 O1 C11 C12 178.53(8) 2_665 . . . ? C17 N1 C11 O1 170.03(12) . . . . ? Rh1 N1 C11 O1 -2.03(18) . . . . ? C17 N1 C11 C12 -10.40(19) . . . . ? Rh1 N1 C11 C12 177.54(10) . . . . ? O1 C11 C12 C13 -84.10(16) . . . . ? N1 C11 C12 C13 96.29(16) . . . . ? C11 C12 C13 C14 -77.72(19) . . . . ? C12 C13 C14 C15 66.2(3) . . . . ? C13 C14 C15 C16 -98.8(3) . . . . ? C14 C15 C16 C17 62.9(3) . . . . ? C11 N1 C17 C16 -84.17(16) . . . . ? Rh1 N1 C17 C16 87.85(13) . . . . ? C15 C16 C17 N1 46.0(2) . . . . ? C31 Rh1 N2 C21 -175.67(9) . . . . ? O1 Rh1 N2 C21 92.70(9) 2_665 . . . ? N1 Rh1 N2 C21 -80.67(9) . . . . ? Rh1 Rh1 N2 C21 5.73(9) 2_665 . . . ? C31 Rh1 N2 C27 16.04(13) . . . . ? O1 Rh1 N2 C27 -75.59(12) 2_665 . . . ? N1 Rh1 N2 C27 111.04(12) . . . . ? Rh1 Rh1 N2 C27 -162.55(11) 2_665 . . . ? Rh1 O2 C21 N2 -6.2(2) 2_665 . . . ? Rh1 O2 C21 C22 175.32(9) 2_665 . . . ? C27 N2 C21 O2 167.98(12) . . . . ? Rh1 N2 C21 O2 -1.56(16) . . . . ? C27 N2 C21 C22 -13.7(2) . . . . ? Rh1 N2 C21 C22 176.75(10) . . . . ? O2 C21 C22 C23 -83.94(15) . . . . ? N2 C21 C22 C23 97.62(16) . . . . ? C21 C22 C23 C24 -76.02(17) . . . . ? C22 C23 C24 C25 63.9(2) . . . . ? C23 C24 C25 C26 -96.66(18) . . . . ? C24 C25 C26 C27 60.2(2) . . . . ? C21 N2 C27 C26 -81.17(16) . . . . ? Rh1 N2 C27 C26 85.98(15) . . . . ? C25 C26 C27 N2 46.73(19) . . . . ? N2 Rh1 C31 C32 -45.27(12) . . . . ? O1 Rh1 C31 C32 42.60(11) 2_665 . . . ? N1 Rh1 C31 C32 -137.32(11) . . . . ? O2 Rh1 C31 C32 129.17(12) 2_665 . . . ? Rh1 Rh1 C31 C32 131.52(10) 2_665 . . . ? N2 Rh1 C31 C36 136.32(11) . . . . ? O1 Rh1 C31 C36 -135.82(11) 2_665 . . . ? N1 Rh1 C31 C36 44.27(11) . . . . ? O2 Rh1 C31 C36 -49.24(11) 2_665 . . . ? Rh1 Rh1 C31 C36 -46.90(16) 2_665 . . . ? C36 C31 C32 C33 -2.2(2) . . . . ? Rh1 C31 C32 C33 179.41(11) . . . . ? C31 C32 C33 C34 0.9(2) . . . . ? C32 C33 C34 C35 0.3(2) . . . . ? C33 C34 C35 C36 -0.1(2) . . . . ? C34 C35 C36 C31 -1.2(2) . . . . ? C32 C31 C36 C35 2.3(2) . . . . ? Rh1 C31 C36 C35 -179.22(11) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.721 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.060 _diffrn_orient_matrix_type standard _diffrn_orient_matrix_UB_11 0.0769525 _diffrn_orient_matrix_UB_12 0.0387287 _diffrn_orient_matrix_UB_13 -0.0017815 _diffrn_orient_matrix_UB_21 0.0518242 _diffrn_orient_matrix_UB_22 -0.0177729 _diffrn_orient_matrix_UB_23 -0.0945536 _diffrn_orient_matrix_UB_31 -0.0716557 _diffrn_orient_matrix_UB_32 0.0879345 _diffrn_orient_matrix_UB_33 -0.0048529 _symmetry_space_group_name_Hall '-P 1' _exptl_crystal_id 'Doyle/Zhou Rh2hep4' _diffrn_measurement_frame_width-CCD -0.5 _diffrn_measurement_details 366,366,366,366,720 _diffrn_measurement_total_frames-CCD 2184 _diffrn_measurement_frame_time-CCD 13 _diffrn_measurement_total_time-CCD 11.5 _diffrn_source_voltage 50.00 _diffrn_source_current 30.00 _diffrn_detector_distance-CCD 5.0000 _diffrn_measurement_frame_size-CCD 512 _diffrn_measurement_specimen_support 'glass capillary' _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker Smart Apex II'