# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1461 data_global _publ_section_title ; Bi-edge Condensation of Imido-Rhodium Clusters Leading to Novel Planar Hexametallic Structures ; _publ_section_abstract 'included in the manuscript' #------------------------------------------------------------ # Person for contact _publ_contact_author 'Dr. Fernando J. Lahoz' _publ_author_address ; Departamento de Qu\'imica Inorg\'anica - I. C. M. A. Facultad de Ciencias Universidad de Zaragoza - C.S.I.C. 50009 Zaragoza, Spain ; _publ_contact_author_email LAHOZ@POSTA.UNIZAR.ES #------------------------------------------------------------- # Publication details loop_ _publ_author_name 'Bordonaba, M.' 'Ciriano, M.A.' 'Lahoz, F.J.' 'Oro, L.A.' 'Tejel, C.' _publ_requested_journal 'Chem. Comm.' _journal_name_full 'Chemical Communications' _journal_volume '?' _journal_page_first '?' _journal_page_last '?' _journal_year '1999' #---------------------------------------------------------------------- # Data for compound 2 (local labelling as 'fer5p') data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C40 H28 N4 O12 Rh6' _chemical_formula_sum 'C40 H28 N4 O12 Rh6' _chemical_formula_weight 1374.12 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 tetragonal _symmetry_space_group_name_H-M 'P 43 21 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.1187(8) _cell_length_b 12.1187(8) _cell_length_c 29.753(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4369.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 83 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_crystal_description 'laminar' _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 2.089 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2648 _exptl_absorpt_coefficient_mu 2.278 _exptl_absorpt_correction_type 'empirical' _exptl_absorpt_correction_T_min 0.8212 _exptl_absorpt_correction_T_max 0.9559 _exptl_absorpt_process_details 'North, Phillips and Mathews, Acta Cryst. 1968, A24, 351' _diffrn_ambient_temperature 153(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 'Siemens SMART CCD Diffractometer' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 15970 _diffrn_reflns_av_R_equivalents 0.1223 _diffrn_reflns_av_sigmaI/netI 0.1663 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 28.31 _reflns_number_total 5400 _reflns_number_gt 3329 _reflns_threshold_expression 2sigma(I) _computing_data_collection 'XSCANS, Siemens SMART' _computing_cell_refinement 'XSCANS, Siemens' _computing_data_reduction 'SAINT program, v. 4.0 (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 5.0 (Siemens, 1994)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. All non-hydrogen atoms were refined with anisotropic displacement parameters. Hydrogens were included in calculated positions, and refined riding on carbon atoms with two common adps. An extinction parameter was also included in the final steps of refinement. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0085P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00027(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.11(6) _refine_ls_number_reflns 5400 _refine_ls_number_parameters 285 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1251 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.0722 _refine_ls_wR_factor_gt 0.0613 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _refine_ls_shift/su_max 0.002 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.09027(6) 0.85057(6) 0.02310(2) 0.01678(17) Uani 1 d . . . Rh2 Rh -0.01307(5) 0.91757(5) -0.06871(2) 0.01651(17) Uani 1 d . . . Rh3 Rh 0.15597(6) 0.77400(6) -0.05852(2) 0.01860(17) Uani 1 d . . . N1 N 0.0046(5) 0.7795(5) -0.0278(2) 0.0144(16) Uani 1 d . . . N2 N 0.1332(5) 0.9327(5) -0.03528(19) 0.0144(16) Uani 1 d . . . O1 O 0.0663(5) 0.6610(5) 0.08803(19) 0.0370(19) Uani 1 d . . . O2 O 0.2735(5) 0.9326(5) 0.0842(2) 0.0334(18) Uani 1 d . . . O3 O -0.2009(5) 0.8250(5) -0.1243(2) 0.0303(17) Uani 1 d . . . O4 O 0.0276(5) 1.0699(5) -0.1472(2) 0.0429(19) Uani 1 d . . . O5 O 0.1797(6) 0.5340(6) -0.0843(2) 0.052(2) Uani 1 d . . . O6 O 0.3764(5) 0.8087(5) -0.1032(2) 0.041(2) Uani 1 d . . . C1 C 0.0687(7) 0.7350(7) 0.0651(3) 0.021(2) Uani 1 d . . . C2 C 0.2021(7) 0.9079(7) 0.0616(3) 0.024(2) Uani 1 d . . . C3 C -0.1330(7) 0.8623(7) -0.1029(3) 0.020(2) Uani 1 d . . . C4 C 0.0112(7) 1.0196(7) -0.1149(3) 0.023(2) Uani 1 d . . . C5 C 0.1655(8) 0.6231(7) -0.0748(3) 0.027(2) Uani 1 d . . . C6 C 0.2933(8) 0.7944(8) -0.0856(3) 0.025(2) Uani 1 d . . . C7 C -0.0737(7) 0.6941(6) -0.0249(3) 0.016(2) Uani 1 d . . . C8 C -0.0937(7) 0.6200(7) -0.0598(3) 0.022(2) Uani 1 d . . . H8 H -0.0539 0.6276 -0.0871 0.032(10) Uiso 1 calc R . . C9 C -0.1696(7) 0.5358(7) -0.0556(3) 0.027(2) Uani 1 d . . . H9 H -0.1792 0.4854 -0.0797 0.032(10) Uiso 1 calc R . . C10 C -0.2325(7) 0.5233(7) -0.0168(3) 0.018(2) Uani 1 d . . . C11 C -0.2149(7) 0.5973(7) 0.0178(3) 0.022(2) Uani 1 d . . . H11 H -0.2575 0.5913 0.0445 0.032(10) Uiso 1 calc R . . C12 C -0.1363(7) 0.6803(7) 0.0144(3) 0.025(2) Uani 1 d . . . H12 H -0.1245 0.7285 0.0391 0.032(10) Uiso 1 calc R . . C13 C -0.3201(7) 0.4351(7) -0.0135(3) 0.035(3) Uani 1 d . . . H13A H -0.3797 0.4515 -0.0348 0.075(14) Uiso 1 calc R . . H13B H -0.3497 0.4332 0.0171 0.075(14) Uiso 1 calc R . . H13C H -0.2876 0.3632 -0.0209 0.075(14) Uiso 1 calc R . . C14 C 0.2143(7) 1.0179(7) -0.0373(3) 0.017(2) Uani 1 d . . . C15 C 0.1893(7) 1.1237(7) -0.0515(2) 0.020(2) Uani 1 d . . . H15 H 0.1158 1.1411 -0.0601 0.032(10) Uiso 1 calc R . . C16 C 0.2697(7) 1.2046(7) -0.0535(3) 0.021(2) Uani 1 d . . . H16 H 0.2508 1.2767 -0.0633 0.032(10) Uiso 1 calc R . . C17 C 0.3785(8) 1.1811(8) -0.0411(3) 0.027(3) Uani 1 d . . . C18 C 0.4006(7) 1.0753(7) -0.0250(3) 0.027(2) Uani 1 d . . . H18 H 0.4730 1.0585 -0.0149 0.032(10) Uiso 1 calc R . . C19 C 0.3222(8) 0.9958(7) -0.0234(3) 0.029(3) Uani 1 d . . . H19 H 0.3408 0.9243 -0.0127 0.032(10) Uiso 1 calc R . . C20 C 0.4638(8) 1.2719(8) -0.0428(3) 0.044(3) Uani 1 d . . . H20A H 0.5013 1.2703 -0.0720 0.075(14) Uiso 1 calc R . . H20B H 0.5179 1.2609 -0.0187 0.075(14) Uiso 1 calc R . . H20C H 0.4274 1.3435 -0.0388 0.075(14) Uiso 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 0.0171(4) 0.0160(4) 0.0173(4) -0.0004(3) -0.0007(3) -0.0017(3) Rh2 0.0172(4) 0.0155(4) 0.0168(4) 0.0003(3) -0.0004(3) -0.0015(3) Rh3 0.0185(4) 0.0168(4) 0.0205(4) -0.0009(3) 0.0016(4) 0.0000(3) N1 0.015(4) 0.014(4) 0.014(4) 0.000(3) -0.006(3) -0.003(3) N2 0.018(5) 0.011(4) 0.015(4) -0.004(3) -0.002(3) -0.001(3) O1 0.051(5) 0.030(4) 0.030(4) 0.015(3) -0.002(4) -0.002(4) O2 0.033(4) 0.027(4) 0.040(5) -0.013(3) -0.013(4) -0.006(4) O3 0.023(4) 0.034(4) 0.034(4) -0.002(3) -0.011(3) -0.008(3) O4 0.064(5) 0.028(5) 0.037(4) 0.006(4) -0.004(4) -0.005(4) O5 0.061(6) 0.024(4) 0.071(6) -0.015(4) 0.006(4) 0.008(4) O6 0.031(5) 0.045(5) 0.046(5) -0.006(4) 0.014(4) 0.004(4) C1 0.029(6) 0.019(5) 0.015(5) -0.003(4) -0.002(5) 0.002(5) C2 0.037(6) 0.013(5) 0.023(6) -0.006(5) 0.003(5) -0.001(5) C3 0.023(6) 0.017(5) 0.021(5) 0.002(4) -0.001(4) 0.005(5) C4 0.024(5) 0.020(5) 0.024(6) 0.004(4) -0.011(5) -0.004(5) C5 0.032(6) 0.018(6) 0.031(6) -0.003(5) -0.002(5) 0.011(5) C6 0.026(6) 0.024(6) 0.025(6) -0.002(5) 0.004(5) 0.003(5) C7 0.020(5) 0.009(5) 0.020(5) 0.002(4) 0.001(5) -0.007(4) C8 0.027(6) 0.028(6) 0.012(5) -0.003(4) 0.001(5) -0.004(5) C9 0.025(6) 0.029(6) 0.026(6) -0.005(5) -0.012(5) -0.011(5) C10 0.011(5) 0.021(5) 0.022(6) 0.008(5) -0.011(4) -0.002(4) C11 0.021(5) 0.024(6) 0.022(6) 0.014(5) 0.005(5) 0.001(5) C12 0.026(6) 0.017(6) 0.031(6) -0.004(4) -0.010(5) -0.005(5) C13 0.034(7) 0.024(6) 0.046(7) 0.005(5) -0.008(5) -0.017(5) C14 0.014(5) 0.028(6) 0.009(5) -0.002(4) 0.001(4) -0.010(5) C15 0.017(6) 0.026(6) 0.016(5) 0.004(4) -0.008(4) -0.007(4) C16 0.027(6) 0.022(6) 0.016(5) -0.001(4) 0.001(5) -0.008(5) C17 0.025(6) 0.034(7) 0.020(6) -0.003(5) 0.007(4) -0.013(5) C18 0.019(5) 0.024(6) 0.038(6) -0.015(5) 0.004(5) -0.003(5) C19 0.033(6) 0.015(6) 0.039(6) 0.001(5) -0.012(5) -0.013(5) C20 0.036(7) 0.039(7) 0.056(8) 0.000(6) -0.004(5) -0.022(6) _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 1.895(9) . ? Rh1 C2 1.906(9) . ? Rh1 N1 2.028(6) . ? Rh1 N2 2.069(6) . ? Rh1 Rh3 2.7188(10) . ? Rh1 Rh2 2.9921(9) 7_465 ? Rh1 Rh2 3.1127(10) . ? Rh2 C4 1.873(9) . ? Rh2 C3 1.897(9) . ? Rh2 N2 2.041(6) . ? Rh2 N1 2.081(6) . ? Rh2 Rh3 2.7048(9) . ? Rh2 Rh1 2.9921(9) 7_465 ? Rh3 C6 1.865(10) . ? Rh3 C5 1.895(9) . ? Rh3 N1 2.051(7) . ? Rh3 N2 2.063(6) . ? N1 C7 1.407(9) . ? N2 C14 1.427(11) . ? O1 C1 1.127(9) . ? O2 C2 1.137(9) . ? O3 C3 1.134(9) . ? O4 C4 1.155(9) . ? O5 C5 1.129(9) . ? O6 C6 1.148(10) . ? C7 C8 1.393(10) . ? C7 C12 1.405(11) . ? C8 C9 1.379(11) . ? C9 C10 1.393(11) . ? C10 C11 1.380(11) . ? C10 C13 1.510(10) . ? C11 C12 1.390(11) . ? C14 C15 1.384(11) . ? C14 C19 1.398(11) . ? C15 C16 1.383(10) . ? C16 C17 1.399(12) . ? C17 C18 1.394(11) . ? C17 C20 1.510(11) . ? C18 C19 1.354(11) . ? 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 88.4(4) . . ? C1 Rh1 N1 96.2(3) . . ? C2 Rh1 N1 165.4(3) . . ? C1 Rh1 N2 160.7(3) . . ? C2 Rh1 N2 98.7(3) . . ? N1 Rh1 N2 72.9(2) . . ? C1 Rh1 Rh3 112.1(3) . . ? C2 Rh1 Rh3 116.9(3) . . ? N1 Rh1 Rh3 48.56(19) . . ? N2 Rh1 Rh3 48.75(17) . . ? C1 Rh1 Rh2 90.7(3) . 7_465 ? C2 Rh1 Rh2 91.3(3) . 7_465 ? N1 Rh1 Rh2 102.43(19) . 7_465 ? N2 Rh1 Rh2 106.91(17) . 7_465 ? Rh3 Rh1 Rh2 142.98(3) . 7_465 ? C1 Rh1 Rh2 135.7(3) . . ? C2 Rh1 Rh2 135.9(3) . . ? N1 Rh1 Rh2 41.39(18) . . ? N2 Rh1 Rh2 40.42(18) . . ? Rh3 Rh1 Rh2 54.77(2) . . ? Rh2 Rh1 Rh2 88.43(3) 7_465 . ? C4 Rh2 C3 87.7(4) . . ? C4 Rh2 N2 99.3(3) . . ? C3 Rh2 N2 163.5(3) . . ? C4 Rh2 N1 160.8(3) . . ? C3 Rh2 N1 96.3(3) . . ? N2 Rh2 N1 72.4(2) . . ? C4 Rh2 Rh3 112.8(3) . . ? C3 Rh2 Rh3 114.4(2) . . ? N2 Rh2 Rh3 49.12(17) . . ? N1 Rh2 Rh3 48.63(18) . . ? C4 Rh2 Rh1 87.6(3) . 7_465 ? C3 Rh2 Rh1 93.8(2) . 7_465 ? N2 Rh2 Rh1 101.28(17) . 7_465 ? N1 Rh2 Rh1 110.74(18) . 7_465 ? Rh3 Rh2 Rh1 144.83(3) . 7_465 ? C4 Rh2 Rh1 138.9(3) . . ? C3 Rh2 Rh1 133.4(3) . . ? N2 Rh2 Rh1 41.09(18) . . ? N1 Rh2 Rh1 40.11(17) . . ? Rh3 Rh2 Rh1 55.19(2) . . ? Rh1 Rh2 Rh1 90.38(3) 7_465 . ? C6 Rh3 C5 87.9(4) . . ? C6 Rh3 N1 170.5(3) . . ? C5 Rh3 N1 101.5(4) . . ? C6 Rh3 N2 98.1(3) . . ? C5 Rh3 N2 173.6(3) . . ? N1 Rh3 N2 72.6(2) . . ? C6 Rh3 Rh2 122.8(3) . . ? C5 Rh3 Rh2 129.6(3) . . ? N1 Rh3 Rh2 49.59(18) . . ? N2 Rh3 Rh2 48.41(18) . . ? C6 Rh3 Rh1 127.0(3) . . ? C5 Rh3 Rh1 125.2(3) . . ? N1 Rh3 Rh1 47.83(17) . . ? N2 Rh3 Rh1 48.94(17) . . ? Rh2 Rh3 Rh1 70.05(3) . . ? C7 N1 Rh1 127.8(5) . . ? C7 N1 Rh3 127.4(5) . . ? Rh1 N1 Rh3 83.6(2) . . ? C7 N1 Rh2 123.8(5) . . ? Rh1 N1 Rh2 98.5(3) . . ? Rh3 N1 Rh2 81.8(2) . . ? C14 N2 Rh2 130.0(5) . . ? C14 N2 Rh3 124.6(5) . . ? Rh2 N2 Rh3 82.5(2) . . ? C14 N2 Rh1 123.8(5) . . ? Rh2 N2 Rh1 98.5(3) . . ? Rh3 N2 Rh1 82.3(2) . . ? O1 C1 Rh1 172.2(8) . . ? O2 C2 Rh1 173.5(8) . . ? O3 C3 Rh2 176.2(8) . . ? O4 C4 Rh2 170.6(8) . . ? O5 C5 Rh3 174.7(9) . . ? O6 C6 Rh3 178.1(8) . . ? C8 C7 C12 116.7(8) . . ? C8 C7 N1 123.1(8) . . ? C12 C7 N1 120.1(8) . . ? C9 C8 C7 121.7(8) . . ? C8 C9 C10 121.4(8) . . ? C11 C10 C9 117.6(8) . . ? C11 C10 C13 121.4(8) . . ? C9 C10 C13 120.9(8) . . ? C10 C11 C12 121.4(8) . . ? C11 C12 C7 121.1(8) . . ? C15 C14 C19 118.2(9) . . ? C15 C14 N2 122.2(8) . . ? C19 C14 N2 119.6(8) . . ? C16 C15 C14 121.0(9) . . ? C15 C16 C17 120.6(9) . . ? C18 C17 C16 117.3(8) . . ? C18 C17 C20 123.4(9) . . ? C16 C17 C20 119.2(9) . . ? C19 C18 C17 122.2(9) . . ? C18 C19 C14 120.6(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 C1 Rh1 Rh2 C4 -171.9(6) . . . . ? C2 Rh1 Rh2 C4 8.4(5) . . . . ? N1 Rh1 Rh2 C4 -150.4(5) . . . . ? N2 Rh1 Rh2 C4 -20.1(5) . . . . ? Rh3 Rh1 Rh2 C4 -85.5(4) . . . . ? Rh2 Rh1 Rh2 C4 98.7(4) 7_465 . . . ? C1 Rh1 Rh2 C3 5.7(5) . . . . ? C2 Rh1 Rh2 C3 -174.1(5) . . . . ? N1 Rh1 Rh2 C3 27.2(4) . . . . ? N2 Rh1 Rh2 C3 157.5(4) . . . . ? Rh3 Rh1 Rh2 C3 92.1(3) . . . . ? Rh2 Rh1 Rh2 C3 -83.8(3) 7_465 . . . ? C1 Rh1 Rh2 N2 -151.8(4) . . . . ? C2 Rh1 Rh2 N2 28.4(4) . . . . ? N1 Rh1 Rh2 N2 -130.3(4) . . . . ? Rh3 Rh1 Rh2 N2 -65.4(3) . . . . ? Rh2 Rh1 Rh2 N2 118.7(3) 7_465 . . . ? C1 Rh1 Rh2 N1 -21.5(5) . . . . ? C2 Rh1 Rh2 N1 158.8(5) . . . . ? N2 Rh1 Rh2 N1 130.3(4) . . . . ? Rh3 Rh1 Rh2 N1 64.9(3) . . . . ? Rh2 Rh1 Rh2 N1 -110.9(3) 7_465 . . . ? C1 Rh1 Rh2 Rh3 -86.4(4) . . . . ? C2 Rh1 Rh2 Rh3 93.9(4) . . . . ? N1 Rh1 Rh2 Rh3 -64.9(3) . . . . ? N2 Rh1 Rh2 Rh3 65.4(3) . . . . ? Rh2 Rh1 Rh2 Rh3 -175.81(3) 7_465 . . . ? C1 Rh1 Rh2 Rh1 101.3(4) . . . 7_465 ? C2 Rh1 Rh2 Rh1 -78.4(4) . . . 7_465 ? N1 Rh1 Rh2 Rh1 122.8(3) . . . 7_465 ? N2 Rh1 Rh2 Rh1 -106.9(3) . . . 7_465 ? Rh3 Rh1 Rh2 Rh1 -172.30(3) . . . 7_465 ? Rh2 Rh1 Rh2 Rh1 11.89(4) 7_465 . . 7_465 ? C4 Rh2 Rh3 C6 12.8(4) . . . . ? C3 Rh2 Rh3 C6 111.0(5) . . . . ? N2 Rh2 Rh3 C6 -69.6(4) . . . . ? N1 Rh2 Rh3 C6 -172.9(4) . . . . ? Rh1 Rh2 Rh3 C6 -108.4(3) 7_465 . . . ? Rh1 Rh2 Rh3 C6 -121.9(3) . . . . ? C4 Rh2 Rh3 C5 -105.7(5) . . . . ? C3 Rh2 Rh3 C5 -7.4(5) . . . . ? N2 Rh2 Rh3 C5 171.9(4) . . . . ? N1 Rh2 Rh3 C5 68.6(4) . . . . ? Rh1 Rh2 Rh3 C5 133.1(4) 7_465 . . . ? Rh1 Rh2 Rh3 C5 119.7(4) . . . . ? C4 Rh2 Rh3 N1 -174.3(4) . . . . ? C3 Rh2 Rh3 N1 -76.1(4) . . . . ? N2 Rh2 Rh3 N1 103.3(3) . . . . ? Rh1 Rh2 Rh3 N1 64.5(2) 7_465 . . . ? Rh1 Rh2 Rh3 N1 51.0(2) . . . . ? C4 Rh2 Rh3 N2 82.4(4) . . . . ? C3 Rh2 Rh3 N2 -179.4(4) . . . . ? N1 Rh2 Rh3 N2 -103.3(3) . . . . ? Rh1 Rh2 Rh3 N2 -38.8(2) 7_465 . . . ? Rh1 Rh2 Rh3 N2 -52.3(2) . . . . ? C4 Rh2 Rh3 Rh1 134.7(3) . . . . ? C3 Rh2 Rh3 Rh1 -127.1(3) . . . . ? N2 Rh2 Rh3 Rh1 52.3(2) . . . . ? N1 Rh2 Rh3 Rh1 -51.0(2) . . . . ? Rh1 Rh2 Rh3 Rh1 13.45(5) 7_465 . . . ? C1 Rh1 Rh3 C6 -112.2(4) . . . . ? C2 Rh1 Rh3 C6 -12.3(5) . . . . ? N1 Rh1 Rh3 C6 169.6(4) . . . . ? N2 Rh1 Rh3 C6 65.0(4) . . . . ? Rh2 Rh1 Rh3 C6 123.6(3) 7_465 . . . ? Rh2 Rh1 Rh3 C6 116.6(3) . . . . ? C1 Rh1 Rh3 C5 6.1(5) . . . . ? C2 Rh1 Rh3 C5 106.0(5) . . . . ? N1 Rh1 Rh3 C5 -72.0(4) . . . . ? N2 Rh1 Rh3 C5 -176.7(5) . . . . ? Rh2 Rh1 Rh3 C5 -118.1(4) 7_465 . . . ? Rh2 Rh1 Rh3 C5 -125.1(4) . . . . ? C1 Rh1 Rh3 N1 78.2(4) . . . . ? C2 Rh1 Rh3 N1 178.1(4) . . . . ? N2 Rh1 Rh3 N1 -104.7(3) . . . . ? Rh2 Rh1 Rh3 N1 -46.0(2) 7_465 . . . ? Rh2 Rh1 Rh3 N1 -53.0(2) . . . . ? C1 Rh1 Rh3 N2 -177.1(4) . . . . ? C2 Rh1 Rh3 N2 -77.2(4) . . . . ? N1 Rh1 Rh3 N2 104.7(3) . . . . ? Rh2 Rh1 Rh3 N2 58.6(2) 7_465 . . . ? Rh2 Rh1 Rh3 N2 51.7(2) . . . . ? C1 Rh1 Rh3 Rh2 131.2(3) . . . . ? C2 Rh1 Rh3 Rh2 -128.9(3) . . . . ? N1 Rh1 Rh3 Rh2 53.0(2) . . . . ? N2 Rh1 Rh3 Rh2 -51.7(2) . . . . ? Rh2 Rh1 Rh3 Rh2 6.97(5) 7_465 . . . ? C1 Rh1 N1 C7 19.1(7) . . . . ? C2 Rh1 N1 C7 126.6(13) . . . . ? N2 Rh1 N1 C7 -177.1(7) . . . . ? Rh3 Rh1 N1 C7 133.3(7) . . . . ? Rh2 Rh1 N1 C7 -73.0(7) 7_465 . . . ? Rh2 Rh1 N1 C7 -146.0(8) . . . . ? C1 Rh1 N1 Rh3 -114.2(3) . . . . ? C2 Rh1 N1 Rh3 -6.8(14) . . . . ? N2 Rh1 N1 Rh3 49.5(2) . . . . ? Rh2 Rh1 N1 Rh3 153.65(13) 7_465 . . . ? Rh2 Rh1 N1 Rh3 80.7(2) . . . . ? C1 Rh1 N1 Rh2 165.1(3) . . . . ? C2 Rh1 N1 Rh2 -87.4(13) . . . . ? N2 Rh1 N1 Rh2 -31.1(2) . . . . ? Rh3 Rh1 N1 Rh2 -80.7(2) . . . . ? Rh2 Rh1 N1 Rh2 73.0(2) 7_465 . . . ? C6 Rh3 N1 C7 165.8(19) . . . . ? C5 Rh3 N1 C7 -6.2(7) . . . . ? N2 Rh3 N1 C7 176.4(7) . . . . ? Rh2 Rh3 N1 C7 126.7(7) . . . . ? Rh1 Rh3 N1 C7 -133.7(7) . . . . ? C6 Rh3 N1 Rh1 -60(2) . . . . ? C5 Rh3 N1 Rh1 127.5(3) . . . . ? N2 Rh3 N1 Rh1 -49.9(2) . . . . ? Rh2 Rh3 N1 Rh1 -99.6(2) . . . . ? C6 Rh3 N1 Rh2 39(2) . . . . ? C5 Rh3 N1 Rh2 -133.0(3) . . . . ? N2 Rh3 N1 Rh2 49.7(2) . . . . ? Rh1 Rh3 N1 Rh2 99.6(2) . . . . ? C4 Rh2 N1 C7 -113.7(10) . . . . ? C3 Rh2 N1 C7 -12.6(7) . . . . ? N2 Rh2 N1 C7 179.6(7) . . . . ? Rh3 Rh2 N1 C7 -129.9(7) . . . . ? Rh1 Rh2 N1 C7 83.9(6) 7_465 . . . ? Rh1 Rh2 N1 C7 147.9(8) . . . . ? C4 Rh2 N1 Rh1 98.4(9) . . . . ? C3 Rh2 N1 Rh1 -160.5(3) . . . . ? N2 Rh2 N1 Rh1 31.7(2) . . . . ? Rh3 Rh2 N1 Rh1 82.2(2) . . . . ? Rh1 Rh2 N1 Rh1 -64.0(3) 7_465 . . . ? C4 Rh2 N1 Rh3 16.2(10) . . . . ? C3 Rh2 N1 Rh3 117.3(3) . . . . ? N2 Rh2 N1 Rh3 -50.5(2) . . . . ? Rh1 Rh2 N1 Rh3 -146.23(11) 7_465 . . . ? Rh1 Rh2 N1 Rh3 -82.2(2) . . . . ? C4 Rh2 N2 C14 17.4(7) . . . . ? C3 Rh2 N2 C14 131.7(11) . . . . ? N1 Rh2 N2 C14 179.7(7) . . . . ? Rh3 Rh2 N2 C14 129.6(7) . . . . ? Rh1 Rh2 N2 C14 -72.0(6) 7_465 . . . ? Rh1 Rh2 N2 C14 -149.3(7) . . . . ? C4 Rh2 N2 Rh3 -112.2(3) . . . . ? C3 Rh2 N2 Rh3 2.0(12) . . . . ? N1 Rh2 N2 Rh3 50.0(2) . . . . ? Rh1 Rh2 N2 Rh3 158.40(12) 7_465 . . . ? Rh1 Rh2 N2 Rh3 81.0(2) . . . . ? C4 Rh2 N2 Rh1 166.8(3) . . . . ? C3 Rh2 N2 Rh1 -79.0(11) . . . . ? N1 Rh2 N2 Rh1 -31.0(2) . . . . ? Rh3 Rh2 N2 Rh1 -81.0(2) . . . . ? Rh1 Rh2 N2 Rh1 77.4(2) 7_465 . . . ? C6 Rh3 N2 C14 -6.9(6) . . . . ? C5 Rh3 N2 C14 151(3) . . . . ? N1 Rh3 N2 C14 174.8(6) . . . . ? Rh2 Rh3 N2 C14 -134.2(6) . . . . ? Rh1 Rh3 N2 C14 126.1(6) . . . . ? C6 Rh3 N2 Rh2 127.3(3) . . . . ? C5 Rh3 N2 Rh2 -75(3) . . . . ? N1 Rh3 N2 Rh2 -51.0(2) . . . . ? Rh1 Rh3 N2 Rh2 -99.7(3) . . . . ? C6 Rh3 N2 Rh1 -133.0(3) . . . . ? C5 Rh3 N2 Rh1 25(3) . . . . ? N1 Rh3 N2 Rh1 48.7(2) . . . . ? Rh2 Rh3 N2 Rh1 99.7(3) . . . . ? C1 Rh1 N2 C14 -118.8(10) . . . . ? C2 Rh1 N2 C14 -8.4(6) . . . . ? N1 Rh1 N2 C14 -176.2(6) . . . . ? Rh3 Rh1 N2 C14 -126.9(6) . . . . ? Rh2 Rh1 N2 C14 85.6(6) 7_465 . . . ? Rh2 Rh1 N2 C14 152.0(7) . . . . ? C1 Rh1 N2 Rh2 89.2(9) . . . . ? C2 Rh1 N2 Rh2 -160.4(3) . . . . ? N1 Rh1 N2 Rh2 31.8(2) . . . . ? Rh3 Rh1 N2 Rh2 81.2(2) . . . . ? Rh2 Rh1 N2 Rh2 -66.3(2) 7_465 . . . ? C1 Rh1 N2 Rh3 8.1(10) . . . . ? C2 Rh1 N2 Rh3 118.4(3) . . . . ? N1 Rh1 N2 Rh3 -49.3(2) . . . . ? Rh2 Rh1 N2 Rh3 -147.50(12) 7_465 . . . ? Rh2 Rh1 N2 Rh3 -81.2(2) . . . . ? C2 Rh1 C1 O1 -78(6) . . . . ? N1 Rh1 C1 O1 88(6) . . . . ? N2 Rh1 C1 O1 34(7) . . . . ? Rh3 Rh1 C1 O1 40(6) . . . . ? Rh2 Rh1 C1 O1 -170(6) 7_465 . . . ? Rh2 Rh1 C1 O1 102(6) . . . . ? C1 Rh1 C2 O2 56(7) . . . . ? N1 Rh1 C2 O2 -52(8) . . . . ? N2 Rh1 C2 O2 -106(7) . . . . ? Rh3 Rh1 C2 O2 -58(7) . . . . ? Rh2 Rh1 C2 O2 147(7) 7_465 . . . ? Rh2 Rh1 C2 O2 -124(7) . . . . ? C4 Rh2 C3 O3 95(12) . . . . ? N2 Rh2 C3 O3 -20(12) . . . . ? N1 Rh2 C3 O3 -66(12) . . . . ? Rh3 Rh2 C3 O3 -19(12) . . . . ? Rh1 Rh2 C3 O3 -177(100) 7_465 . . . ? Rh1 Rh2 C3 O3 -83(12) . . . . ? C3 Rh2 C4 O4 -57(5) . . . . ? N2 Rh2 C4 O4 108(5) . . . . ? N1 Rh2 C4 O4 45(5) . . . . ? Rh3 Rh2 C4 O4 58(5) . . . . ? Rh1 Rh2 C4 O4 -151(5) 7_465 . . . ? Rh1 Rh2 C4 O4 121(5) . . . . ? C6 Rh3 C5 O5 30(10) . . . . ? N1 Rh3 C5 O5 -151(10) . . . . ? N2 Rh3 C5 O5 -128(9) . . . . ? Rh2 Rh3 C5 O5 163(10) . . . . ? Rh1 Rh3 C5 O5 -105(10) . . . . ? C5 Rh3 C6 O6 112(27) . . . . ? N1 Rh3 C6 O6 -60(28) . . . . ? N2 Rh3 C6 O6 -70(27) . . . . ? Rh2 Rh3 C6 O6 -25(27) . . . . ? Rh1 Rh3 C6 O6 -114(27) . . . . ? Rh1 N1 C7 C8 -151.9(7) . . . . ? Rh3 N1 C7 C8 -37.3(11) . . . . ? Rh2 N1 C7 C8 69.9(10) . . . . ? Rh1 N1 C7 C12 28.0(11) . . . . ? Rh3 N1 C7 C12 142.5(7) . . . . ? Rh2 N1 C7 C12 -110.3(8) . . . . ? C12 C7 C8 C9 -1.1(13) . . . . ? N1 C7 C8 C9 178.7(8) . . . . ? C7 C8 C9 C10 2.1(13) . . . . ? C8 C9 C10 C11 -1.0(13) . . . . ? C8 C9 C10 C13 176.4(8) . . . . ? C9 C10 C11 C12 -1.0(12) . . . . ? C13 C10 C11 C12 -178.3(8) . . . . ? C10 C11 C12 C7 1.9(13) . . . . ? C8 C7 C12 C11 -0.8(13) . . . . ? N1 C7 C12 C11 179.3(7) . . . . ? Rh2 N2 C14 C15 22.6(11) . . . . ? Rh3 N2 C14 C15 134.5(7) . . . . ? Rh1 N2 C14 C15 -120.0(7) . . . . ? Rh2 N2 C14 C19 -159.1(6) . . . . ? Rh3 N2 C14 C19 -47.2(10) . . . . ? Rh1 N2 C14 C19 58.2(9) . . . . ? C19 C14 C15 C16 2.2(12) . . . . ? N2 C14 C15 C16 -179.5(7) . . . . ? C14 C15 C16 C17 0.1(13) . . . . ? C15 C16 C17 C18 -2.8(13) . . . . ? C15 C16 C17 C20 -178.8(8) . . . . ? C16 C17 C18 C19 3.4(14) . . . . ? C20 C17 C18 C19 179.2(8) . . . . ? C17 C18 C19 C14 -1.1(15) . . . . ? C15 C14 C19 C18 -1.7(13) . . . . ? N2 C14 C19 C18 179.9(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.797 _refine_diff_density_min -0.840 _refine_diff_density_rms 0.196