# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_section_title ; Cyclic amino aryl carbene complexes from isoquinolines: Electronically tuneable ligands ; # # by Rosario Ferandez, Christophe Pichon, Silvia Gomez-Bujedo, # Manuel Alcarazo, Eleuterio Alvarez, and Jose M. Lassaletta # # To be submitted to Angew.Chem.,Int.Ed. # Manuscript number ........... #=============================================================================80 # # Person for contact _publ_contact_author_name 'Eleuterio Alvarez, Rosario Fernandez' _publ_contact_author_address ; Instituto de Investigaciones Quimicas, C.S.I.C-Universidad de Sevilla, Avd. Americo Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain ; _publ_contact_author_phone '+34 954 489560' _publ_contact_author_fax '+34 954 460565' _publ_contact_author_email 'ealvarez@iiq.csic.es, ffernan@us.es' #=============================================================================80 # Publication details loop_ _publ_author_name _publ_author_address 'Rosario Fernandez' ; Departamento de Quimica Organica, Facultad de Quimica, Universidad de Sevilla, Apartado de Correos No. 553, E-41071, Sevilla, Spain ; 'Christophe Pichon' ; Instituto de Investigaciones Quimicas, C.S.I.C-Universidad de Sevilla, Avd. Americo Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain ; 'Silvia Gomez-Bujedo' ; Instituto de Investigaciones Quimicas, C.S.I.C-Universidad de Sevilla, Avd. Americo Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain ; 'Manuel Alcarazo' ; Instituto de Investigaciones Quimicas, C.S.I.C-Universidad de Sevilla, Avd. Americo Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain ; 'Eleuterio Alvarez' ; Instituto de Investigaciones Quimicas, C.S.I.C-Universidad de Sevilla, Avd. Americo Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain ; ; J.M.Lassaletta ; ; Instituto de Investigaciones Quimicas, C.S.I.C-Universidad de Sevilla, Avd. Americo Vespucio, 49., Isla de la Cartuja, 41092 Sevilla, Spain ; _journal_volume ? _journal_page_first ? _journal_page_last ? _journal_year ? _publ_section_references ; Bruker, Programs SMART, version 5.054; SAINT+, version 6.04; SADABS version 2.03; XPREP, version 5.1; SHELXTL, version 6.1. Bruker AXS Inc., Madison, WI, USA, 2001. G.M. Sheldrick, Programs SHELXS97 (crystal structure solution) and SHELXL97 (crystal structure refinement), University of Gottingen, Germany, 1997. WINGX, v. 1.64.05 An integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-Ray Diffraction Data. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. ; #========================================================================= # Data for compound 8e (local labelling ea03806a) #========================================================================= data_8e _database_code_depnum_ccdc_archive 'CCDC 621896' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H17 N O2 Se' _chemical_formula_sum 'C14 H17 N O2 Se' _chemical_formula_weight 310.25 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' Se Se -0.0929 2.2259 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4152(4) _cell_length_b 11.5802(5) _cell_length_c 11.8762(5) _cell_angle_alpha 80.836(1) _cell_angle_beta 89.391(1) _cell_angle_gamma 79.542(1) _cell_volume 1390.37(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8959 _cell_measurement_theta_min 2.67 _cell_measurement_theta_max 30.49 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 2.695 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3835 _exptl_absorpt_correction_T_max 0.5299 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. Bruker-AXS within v. 7.06 a (Bruker AXS, 2003). ; _diffrn_ambient_temperature 100(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 'Bruker-Nonius X8kappa APEX II CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 0 _diffrn_reflns_number 35132 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0162 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 30.52 _reflns_number_total 8353 _reflns_number_gt 7381 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-W2K-NT v. 1.0 (Bruker AXS, 2004)' _computing_cell_refinement 'SAINT+ v. 7.06 a (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 7.06 a (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.12 (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+0.4050P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8353 _refine_ls_number_parameters 325 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0279 _refine_ls_R_factor_gt 0.0225 _refine_ls_wR_factor_ref 0.0614 _refine_ls_wR_factor_gt 0.0584 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Se1 Se 0.301999(11) 0.260042(11) 0.631965(11) 0.02029(4) Uani 1 1 d . . . N1 N 0.05127(10) 0.28722(9) 0.72877(8) 0.01657(18) Uani 1 1 d . . . O1 O 0.00867(9) 0.83718(8) 0.52895(8) 0.02246(18) Uani 1 1 d . . . O2 O 0.22695(9) 0.72504(9) 0.46465(8) 0.02339(19) Uani 1 1 d . . . C1 C 0.13980(11) 0.34238(10) 0.66565(9) 0.0159(2) Uani 1 1 d . . . C2 C -0.06426(12) 0.34949(11) 0.76281(10) 0.0195(2) Uani 1 1 d . . . H2 H -0.1210 0.3072 0.8090 0.023 Uiso 1 1 d R . . C3 C -0.09953(12) 0.46811(11) 0.73280(10) 0.0187(2) Uani 1 1 d . . . H3 H -0.1793 0.5086 0.7584 0.022 Uiso 1 1 d R . . C4 C -0.01665(11) 0.53215(10) 0.66266(9) 0.0153(2) Uani 1 1 d . . . C5 C -0.05115(11) 0.65642(10) 0.62914(10) 0.0169(2) Uani 1 1 d . . . H5 H -0.1320 0.6978 0.6521 0.020 Uiso 1 1 d R . . C6 C 0.03124(11) 0.71783(11) 0.56376(10) 0.0173(2) Uani 1 1 d . . . C7 C 0.15194(11) 0.65488(11) 0.52801(10) 0.0177(2) Uani 1 1 d . . . C8 C 0.18531(11) 0.53406(11) 0.55868(9) 0.0170(2) Uani 1 1 d . . . H8 H 0.2648 0.4931 0.5330 0.020 Uiso 1 1 d R . . C9 C 0.10261(11) 0.46937(10) 0.62837(9) 0.0151(2) Uani 1 1 d . . . C10 C 0.07994(12) 0.15596(10) 0.77137(10) 0.0189(2) Uani 1 1 d . . . H10 H 0.1454 0.1188 0.7194 0.023 Uiso 1 1 d R . . C11 C -0.04011(13) 0.09863(12) 0.76863(12) 0.0253(3) Uani 1 1 d . . . H11A H -0.0968 0.1178 0.8320 0.038 Uiso 1 1 d R . . H11B H -0.0130 0.0121 0.7759 0.038 Uiso 1 1 d R . . H11C H -0.0878 0.1291 0.6962 0.038 Uiso 1 1 d R . . C12 C 0.14290(15) 0.13339(12) 0.88963(12) 0.0284(3) Uani 1 1 d . . . H12A H 0.2212 0.1696 0.8868 0.043 Uiso 1 1 d R . . H12B H 0.1672 0.0475 0.9155 0.043 Uiso 1 1 d R . . H12C H 0.0809 0.1686 0.9429 0.043 Uiso 1 1 d R . . C13 C -0.11403(13) 0.90220(11) 0.56043(12) 0.0235(2) Uani 1 1 d . . . H13A H -0.1858 0.8742 0.5267 0.035 Uiso 1 1 d R . . H13B H -0.1190 0.9872 0.5323 0.035 Uiso 1 1 d R . . H13C H -0.1208 0.8895 0.6437 0.035 Uiso 1 1 d R . . C14 C 0.34756(13) 0.66573(14) 0.42431(12) 0.0280(3) Uani 1 1 d . . . H14A H 0.4033 0.6238 0.4895 0.042 Uiso 1 1 d R . . H14B H 0.3921 0.7245 0.3790 0.042 Uiso 1 1 d R . . H14C H 0.3296 0.6084 0.3768 0.042 Uiso 1 1 d R . . Se2 Se 0.703795(12) 0.741218(11) 0.897544(12) 0.02266(4) Uani 1 1 d . . . N2 N 0.48018(10) 0.71013(9) 0.78147(8) 0.01681(18) Uani 1 1 d . . . O3 O 0.67271(9) 0.15908(8) 0.96466(8) 0.02269(18) Uani 1 1 d . . . O4 O 0.82331(9) 0.27566(8) 1.05273(8) 0.02211(18) Uani 1 1 d . . . C15 C 0.58466(11) 0.65641(10) 0.85142(9) 0.0158(2) Uani 1 1 d . . . C16 C 0.39723(12) 0.64625(11) 0.73936(10) 0.0188(2) Uani 1 1 d . . . H16 H 0.3267 0.6878 0.6903 0.023 Uiso 1 1 d R . . C17 C 0.41277(11) 0.52716(11) 0.76543(10) 0.0179(2) Uani 1 1 d . . . H17 H 0.3546 0.4855 0.7345 0.021 Uiso 1 1 d R . . C18 C 0.51723(11) 0.46400(10) 0.83984(9) 0.0142(2) Uani 1 1 d . . . C19 C 0.53815(11) 0.33878(10) 0.86668(10) 0.0159(2) Uani 1 1 d . . . H19 H 0.4811 0.2958 0.8361 0.019 Uiso 1 1 d R . . C20 C 0.64076(11) 0.27904(10) 0.93685(10) 0.0167(2) Uani 1 1 d . . . C21 C 0.72403(11) 0.34418(11) 0.98534(9) 0.0164(2) Uani 1 1 d . . . C22 C 0.70381(11) 0.46593(10) 0.96019(9) 0.0156(2) Uani 1 1 d . . . H22 H 0.7593 0.5084 0.9935 0.019 Uiso 1 1 d R . . C23 C 0.60082(11) 0.52889(10) 0.88496(9) 0.01416(19) Uani 1 1 d . . . C24 C 0.45824(13) 0.84130(11) 0.73959(11) 0.0221(2) Uani 1 1 d . . . H24 H 0.4990 0.8791 0.7967 0.026 Uiso 1 1 d R . . C25 C 0.31434(14) 0.89742(12) 0.72846(14) 0.0310(3) Uani 1 1 d . . . H25A H 0.2756 0.8743 0.6625 0.047 Uiso 1 1 d R . . H25B H 0.3051 0.9842 0.7180 0.047 Uiso 1 1 d R . . H25C H 0.2695 0.8699 0.7978 0.047 Uiso 1 1 d R . . C26 C 0.52858(17) 0.86380(14) 0.62795(14) 0.0383(4) Uani 1 1 d . . . H26A H 0.6205 0.8254 0.6383 0.057 Uiso 1 1 d R . . H26B H 0.5228 0.9496 0.6042 0.057 Uiso 1 1 d R . . H26C H 0.4879 0.8309 0.5693 0.057 Uiso 1 1 d R . . C27 C 0.59857(15) 0.09157(12) 0.90794(13) 0.0294(3) Uani 1 1 d . . . H27A H 0.5065 0.1102 0.9281 0.044 Uiso 1 1 d R . . H27B H 0.6317 0.0065 0.9317 0.044 Uiso 1 1 d R . . H27C H 0.6069 0.1120 0.8252 0.044 Uiso 1 1 d R . . C28 C 0.91369(13) 0.33668(13) 1.09793(12) 0.0286(3) Uani 1 1 d . . . H28A H 0.9541 0.3822 1.0351 0.043 Uiso 1 1 d R . . H28B H 0.9815 0.2786 1.1432 0.043 Uiso 1 1 d R . . H28C H 0.8674 0.3910 1.1465 0.043 Uiso 1 1 d 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 Se1 0.01285(6) 0.02143(7) 0.02734(7) -0.00994(5) 0.00121(4) 0.00015(4) N1 0.0159(4) 0.0161(4) 0.0175(4) -0.0042(3) -0.0003(3) -0.0009(3) O1 0.0216(4) 0.0180(4) 0.0275(5) -0.0017(3) 0.0018(3) -0.0046(3) O2 0.0177(4) 0.0279(5) 0.0238(4) 0.0015(4) 0.0032(3) -0.0072(3) C1 0.0134(5) 0.0203(5) 0.0146(5) -0.0065(4) -0.0012(4) -0.0018(4) C2 0.0170(5) 0.0213(6) 0.0194(5) -0.0034(4) 0.0048(4) -0.0013(4) C3 0.0158(5) 0.0203(5) 0.0194(5) -0.0037(4) 0.0045(4) -0.0011(4) C4 0.0135(5) 0.0186(5) 0.0141(5) -0.0049(4) -0.0001(4) -0.0018(4) C5 0.0153(5) 0.0183(5) 0.0170(5) -0.0048(4) 0.0001(4) -0.0013(4) C6 0.0172(5) 0.0187(5) 0.0168(5) -0.0036(4) -0.0022(4) -0.0043(4) C7 0.0152(5) 0.0240(6) 0.0149(5) -0.0025(4) -0.0003(4) -0.0064(4) C8 0.0124(5) 0.0245(6) 0.0147(5) -0.0052(4) 0.0001(4) -0.0030(4) C9 0.0131(5) 0.0190(5) 0.0137(5) -0.0051(4) -0.0008(4) -0.0024(4) C10 0.0202(5) 0.0159(5) 0.0201(5) -0.0042(4) -0.0018(4) -0.0010(4) C11 0.0267(6) 0.0210(6) 0.0289(6) -0.0022(5) -0.0037(5) -0.0070(5) C12 0.0349(7) 0.0250(6) 0.0237(6) -0.0031(5) -0.0109(5) -0.0014(5) C13 0.0231(6) 0.0180(6) 0.0297(6) -0.0054(5) 0.0004(5) -0.0030(5) C14 0.0191(6) 0.0404(8) 0.0247(6) -0.0026(5) 0.0063(5) -0.0090(5) Se2 0.01947(6) 0.01880(6) 0.03233(7) -0.00930(5) -0.00078(5) -0.00578(5) N2 0.0181(4) 0.0142(4) 0.0170(4) -0.0026(3) 0.0007(3) 0.0000(3) O3 0.0244(4) 0.0148(4) 0.0270(5) -0.0013(3) -0.0042(4) -0.0003(3) O4 0.0171(4) 0.0240(4) 0.0223(4) 0.0000(3) -0.0068(3) 0.0011(3) C15 0.0149(5) 0.0170(5) 0.0161(5) -0.0054(4) 0.0028(4) -0.0024(4) C16 0.0174(5) 0.0202(5) 0.0174(5) -0.0029(4) -0.0034(4) 0.0004(4) C17 0.0168(5) 0.0195(5) 0.0171(5) -0.0039(4) -0.0037(4) -0.0015(4) C18 0.0136(5) 0.0158(5) 0.0131(4) -0.0037(4) 0.0008(4) -0.0014(4) C19 0.0163(5) 0.0159(5) 0.0160(5) -0.0042(4) -0.0005(4) -0.0024(4) C20 0.0172(5) 0.0153(5) 0.0165(5) -0.0022(4) 0.0012(4) -0.0004(4) C21 0.0128(5) 0.0207(5) 0.0139(5) -0.0015(4) -0.0006(4) 0.0007(4) C22 0.0125(5) 0.0202(5) 0.0148(5) -0.0050(4) -0.0008(4) -0.0024(4) C23 0.0124(5) 0.0164(5) 0.0138(5) -0.0042(4) 0.0016(4) -0.0017(4) C24 0.0256(6) 0.0135(5) 0.0251(6) -0.0013(4) 0.0022(5) 0.0002(4) C25 0.0290(7) 0.0202(6) 0.0377(8) 0.0019(5) 0.0033(6) 0.0057(5) C26 0.0428(9) 0.0280(7) 0.0376(8) 0.0068(6) 0.0167(7) -0.0010(6) C27 0.0337(7) 0.0165(6) 0.0380(7) -0.0038(5) -0.0055(6) -0.0048(5) C28 0.0196(6) 0.0360(7) 0.0289(7) -0.0058(5) -0.0101(5) -0.0004(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 Se1 C1 1.8562(11) . ? N1 C1 1.3663(16) . ? N1 C2 1.3779(14) . ? N1 C10 1.4997(15) . ? O1 C6 1.3559(14) . ? O1 C13 1.4388(15) . ? O2 C7 1.3638(15) . ? O2 C14 1.4345(16) . ? C1 C9 1.4485(16) . ? C2 C3 1.3463(17) . ? C2 H2 0.9500 . ? C3 C4 1.4175(17) . ? C3 H3 0.9500 . ? C4 C5 1.4112(16) . ? C4 C9 1.4117(15) . ? C5 C6 1.3698(17) . ? C5 H5 0.9500 . ? C6 C7 1.4306(16) . ? C7 C8 1.3693(17) . ? C8 C9 1.4177(16) . ? C8 H8 0.9500 . ? C10 C12 1.5204(17) . ? C10 C11 1.5213(18) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? Se2 C15 1.8527(12) . ? N2 C15 1.3675(14) . ? N2 C16 1.3795(16) . ? N2 C24 1.4975(15) . ? O3 C20 1.3558(14) . ? O3 C27 1.4349(17) . ? O4 C21 1.3627(13) . ? O4 C28 1.4306(17) . ? C15 C23 1.4461(16) . ? C16 C17 1.3446(17) . ? C16 H16 0.9500 . ? C17 C18 1.4231(15) . ? C17 H17 0.9500 . ? C18 C23 1.4091(16) . ? C18 C19 1.4111(15) . ? C19 C20 1.3720(15) . ? C19 H19 0.9500 . ? C20 C21 1.4280(17) . ? C21 C22 1.3714(16) . ? C22 C23 1.4175(15) . ? C22 H22 0.9500 . ? C24 C26 1.5170(19) . ? C24 C25 1.5196(18) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 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 C1 N1 C2 122.16(10) . . ? C1 N1 C10 121.12(9) . . ? C2 N1 C10 116.59(10) . . ? C6 O1 C13 116.52(10) . . ? C7 O2 C14 116.66(10) . . ? N1 C1 C9 116.84(10) . . ? N1 C1 Se1 121.91(8) . . ? C9 C1 Se1 121.23(9) . . ? C3 C2 N1 122.29(11) . . ? C3 C2 H2 118.9 . . ? N1 C2 H2 118.9 . . ? C2 C3 C4 119.51(11) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.2 . . ? C5 C4 C9 120.45(11) . . ? C5 C4 C3 120.90(10) . . ? C9 C4 C3 118.64(10) . . ? C6 C5 C4 120.40(10) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? O1 C6 C5 125.08(11) . . ? O1 C6 C7 115.36(11) . . ? C5 C6 C7 119.55(11) . . ? O2 C7 C8 125.01(11) . . ? O2 C7 C6 114.54(11) . . ? C8 C7 C6 120.45(11) . . ? C7 C8 C9 120.78(10) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C4 C9 C8 118.35(10) . . ? C4 C9 C1 120.42(10) . . ? C8 C9 C1 121.22(10) . . ? N1 C10 C12 109.35(10) . . ? N1 C10 C11 112.58(10) . . ? C12 C10 C11 112.30(11) . . ? N1 C10 H10 107.5 . . ? C12 C10 H10 107.4 . . ? C11 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.4 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.4 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 H13A 109.5 . . ? O1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O2 C14 H14A 109.5 . . ? O2 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O2 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C15 N2 C16 122.22(10) . . ? C15 N2 C24 120.48(10) . . ? C16 N2 C24 117.11(10) . . ? C20 O3 C27 116.13(10) . . ? C21 O4 C28 116.68(10) . . ? N2 C15 C23 116.86(10) . . ? N2 C15 Se2 121.96(9) . . ? C23 C15 Se2 121.15(8) . . ? C17 C16 N2 122.24(10) . . ? C17 C16 H16 118.9 . . ? N2 C16 H16 118.9 . . ? C16 C17 C18 119.41(11) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C23 C18 C19 120.53(10) . . ? C23 C18 C17 118.66(10) . . ? C19 C18 C17 120.80(11) . . ? C20 C19 C18 120.10(11) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 120.0 . . ? O3 C20 C19 124.99(11) . . ? O3 C20 C21 115.22(10) . . ? C19 C20 C21 119.79(10) . . ? O4 C21 C22 124.87(11) . . ? O4 C21 C20 114.69(10) . . ? C22 C21 C20 120.41(10) . . ? C21 C22 C23 120.57(11) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 118.56(10) . . ? C18 C23 C15 120.48(10) . . ? C22 C23 C15 120.92(10) . . ? N2 C24 C26 108.93(10) . . ? N2 C24 C25 112.75(11) . . ? C26 C24 C25 111.92(12) . . ? N2 C24 H24 107.7 . . ? C26 C24 H24 107.7 . . ? C25 C24 H24 107.7 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.4 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.4 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O3 C27 H27A 109.5 . . ? O3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O4 C28 H28A 109.5 . . ? O4 C28 H28B 109.4 . . ? H28A C28 H28B 109.5 . . ? O4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 N1 C1 C9 -4.48(16) . . . . ? C10 N1 C1 C9 179.85(10) . . . . ? C2 N1 C1 Se1 173.98(9) . . . . ? C10 N1 C1 Se1 -1.69(15) . . . . ? C1 N1 C2 C3 2.37(19) . . . . ? C10 N1 C2 C3 178.23(11) . . . . ? N1 C2 C3 C4 0.77(19) . . . . ? C2 C3 C4 C5 179.63(12) . . . . ? C2 C3 C4 C9 -1.43(17) . . . . ? C9 C4 C5 C6 -0.59(17) . . . . ? C3 C4 C5 C6 178.33(11) . . . . ? C13 O1 C6 C5 -2.44(17) . . . . ? C13 O1 C6 C7 177.95(10) . . . . ? C4 C5 C6 O1 -178.63(11) . . . . ? C4 C5 C6 C7 0.97(17) . . . . ? C14 O2 C7 C8 2.36(17) . . . . ? C14 O2 C7 C6 -178.49(11) . . . . ? O1 C6 C7 O2 0.48(15) . . . . ? C5 C6 C7 O2 -179.16(10) . . . . ? O1 C6 C7 C8 179.66(10) . . . . ? C5 C6 C7 C8 0.02(17) . . . . ? O2 C7 C8 C9 177.69(11) . . . . ? C6 C7 C8 C9 -1.41(17) . . . . ? C5 C4 C9 C8 -0.76(16) . . . . ? C3 C4 C9 C8 -179.70(10) . . . . ? C5 C4 C9 C1 178.12(10) . . . . ? C3 C4 C9 C1 -0.83(16) . . . . ? C7 C8 C9 C4 1.75(16) . . . . ? C7 C8 C9 C1 -177.11(11) . . . . ? N1 C1 C9 C4 3.70(16) . . . . ? Se1 C1 C9 C4 -174.77(8) . . . . ? N1 C1 C9 C8 -177.46(10) . . . . ? Se1 C1 C9 C8 4.07(15) . . . . ? C1 N1 C10 C12 91.52(13) . . . . ? C2 N1 C10 C12 -84.38(13) . . . . ? C1 N1 C10 C11 -142.91(11) . . . . ? C2 N1 C10 C11 41.19(14) . . . . ? C16 N2 C15 C23 -3.31(16) . . . . ? C24 N2 C15 C23 -178.11(10) . . . . ? C16 N2 C15 Se2 174.61(9) . . . . ? C24 N2 C15 Se2 -0.18(14) . . . . ? C15 N2 C16 C17 0.81(18) . . . . ? C24 N2 C16 C17 175.77(11) . . . . ? N2 C16 C17 C18 0.66(18) . . . . ? C16 C17 C18 C23 0.60(17) . . . . ? C16 C17 C18 C19 -178.44(11) . . . . ? C23 C18 C19 C20 -0.24(17) . . . . ? C17 C18 C19 C20 178.77(11) . . . . ? C27 O3 C20 C19 5.29(17) . . . . ? C27 O3 C20 C21 -173.96(11) . . . . ? C18 C19 C20 O3 -177.38(11) . . . . ? C18 C19 C20 C21 1.84(17) . . . . ? C28 O4 C21 C22 -1.34(17) . . . . ? C28 O4 C21 C20 176.54(11) . . . . ? O3 C20 C21 O4 -0.13(15) . . . . ? C19 C20 C21 O4 -179.42(10) . . . . ? O3 C20 C21 C22 177.84(10) . . . . ? C19 C20 C21 C22 -1.44(17) . . . . ? O4 C21 C22 C23 177.18(10) . . . . ? C20 C21 C22 C23 -0.58(17) . . . . ? C19 C18 C23 C22 -1.74(16) . . . . ? C17 C18 C23 C22 179.22(10) . . . . ? C19 C18 C23 C15 175.83(10) . . . . ? C17 C18 C23 C15 -3.20(16) . . . . ? C21 C22 C23 C18 2.14(16) . . . . ? C21 C22 C23 C15 -175.43(10) . . . . ? N2 C15 C23 C18 4.50(15) . . . . ? Se2 C15 C23 C18 -173.44(8) . . . . ? N2 C15 C23 C22 -177.98(10) . . . . ? Se2 C15 C23 C22 4.08(14) . . . . ? C15 N2 C24 C26 89.98(14) . . . . ? C16 N2 C24 C26 -85.08(14) . . . . ? C15 N2 C24 C25 -145.15(12) . . . . ? C16 N2 C24 C25 39.79(15) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 30.52 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.847 _refine_diff_density_min -0.238 _refine_diff_density_rms 0.064 ###END #========================================================================= # Data for compound 9a (local labelling ea03205a) #========================================================================= data_9a _database_code_depnum_ccdc_archive 'CCDC 621897' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H25 I N Rh' _chemical_formula_sum 'C20 H25 I N Rh' _chemical_formula_weight 509.22 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.6805(7) _cell_length_b 14.9418(14) _cell_length_c 14.7924(13) _cell_angle_alpha 90.00 _cell_angle_beta 103.803(3) _cell_angle_gamma 90.00 _cell_volume 1863.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6421 _cell_measurement_theta_min 2.49 _cell_measurement_theta_max 30.53 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.815 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1000 _exptl_absorpt_coefficient_mu 2.573 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4042 _exptl_absorpt_correction_T_max 0.5124 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. Bruker-AXS within v. 7.06 a (Bruker AXS, 2003). ; _diffrn_ambient_temperature 100(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 ; Bruker-Nonius X8kappa APEX II CCD area detector' ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17579 _diffrn_reflns_av_R_equivalents 0.0208 _diffrn_reflns_av_sigmaI/netI 0.0215 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 30.55 _reflns_number_total 5469 _reflns_number_gt 5185 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-W2K-NT v. 1.0 (Bruker AXS, 2004)' _computing_cell_refinement 'SAINT+ v. 7.06 a (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 7.06 a (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.12 (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0237P)^2^+1.3184P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0028(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5469 _refine_ls_number_parameters 209 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0228 _refine_ls_R_factor_gt 0.0208 _refine_ls_wR_factor_ref 0.0538 _refine_ls_wR_factor_gt 0.0529 _refine_ls_goodness_of_fit_ref 1.127 _refine_ls_restrained_S_all 1.127 _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 I1 I 0.482018(13) 0.591950(8) 0.263713(8) 0.01899(5) Uani 1 1 d . . . Rh1 Rh 0.259401(13) 0.465481(8) 0.249587(8) 0.01078(5) Uani 1 1 d . . . N1 N 0.51342(16) 0.33213(10) 0.32439(9) 0.0131(2) Uani 1 1 d . . . C1 C 0.42889(18) 0.37314(11) 0.24692(11) 0.0127(3) Uani 1 1 d . . . C2 C 0.46727(18) 0.34625(11) 0.16072(11) 0.0139(3) Uani 1 1 d . . . C3 C 0.3981(2) 0.39166(12) 0.07700(12) 0.0178(3) Uani 1 1 d . . . H3 H 0.3249 0.4388 0.0774 0.021 Uiso 1 1 d R . . C4 C 0.4360(2) 0.36807(13) -0.00520(12) 0.0203(3) Uani 1 1 d . . . H4 H 0.3920 0.4005 -0.0606 0.024 Uiso 1 1 d R . . C5 C 0.5396(2) 0.29611(13) -0.00744(13) 0.0206(3) Uani 1 1 d . . . H5 H 0.5626 0.2790 -0.0647 0.025 Uiso 1 1 d R . . C6 C 0.6078(2) 0.25039(12) 0.07273(13) 0.0191(3) Uani 1 1 d . . . H6 H 0.6761 0.2012 0.0705 0.023 Uiso 1 1 d R . . C7 C 0.57657(19) 0.27645(11) 0.15843(12) 0.0148(3) Uani 1 1 d . . . C8 C 0.6566(2) 0.23685(12) 0.24432(12) 0.0172(3) Uani 1 1 d . . . H8 H 0.7307 0.1898 0.2452 0.021 Uiso 1 1 d R . . C9 C 0.62641(19) 0.26661(11) 0.32420(12) 0.0158(3) Uani 1 1 d . . . H9 H 0.6838 0.2422 0.3817 0.019 Uiso 1 1 d R . . C10 C 0.49347(19) 0.36024(12) 0.41800(11) 0.0153(3) Uani 1 1 d . . . H10 H 0.4018 0.4026 0.4081 0.018 Uiso 1 1 d R . . C11 C 0.6409(2) 0.41047(13) 0.46984(13) 0.0214(4) Uani 1 1 d . . . H11A H 0.7326 0.3701 0.4812 0.032 Uiso 1 1 d R . . H11B H 0.6249 0.4322 0.5294 0.032 Uiso 1 1 d R . . H11C H 0.6602 0.4614 0.4322 0.032 Uiso 1 1 d R . . C12 C 0.4552(2) 0.28072(13) 0.47295(13) 0.0230(4) Uani 1 1 d . . . H12A H 0.3660 0.2473 0.4347 0.034 Uiso 1 1 d R . . H12B H 0.4269 0.3021 0.5295 0.034 Uiso 1 1 d R . . H12C H 0.5482 0.2415 0.4900 0.034 Uiso 1 1 d R . . C13 C 0.0823(2) 0.37407(12) 0.18096(13) 0.0178(3) Uani 1 1 d . . . H13 H 0.1624 0.3433 0.1593 0.021 Uiso 1 1 d R . . C14 C 0.0910(2) 0.37092(11) 0.27703(13) 0.0174(3) Uani 1 1 d . . . H14 H 0.1790 0.3413 0.3161 0.021 Uiso 1 1 d R . . C15 C -0.0330(2) 0.41235(12) 0.32189(14) 0.0208(3) Uani 1 1 d . . . H15A H -0.0425 0.3752 0.3757 0.025 Uiso 1 1 d R . . H15B H -0.1371 0.4118 0.2763 0.025 Uiso 1 1 d R . . C16 C 0.0068(2) 0.50878(13) 0.35510(13) 0.0201(3) Uani 1 1 d . . . H16A H -0.0932 0.5411 0.3541 0.024 Uiso 1 1 d R . . H16B H 0.0699 0.5074 0.4204 0.024 Uiso 1 1 d R . . C17 C 0.0981(2) 0.55992(12) 0.29690(12) 0.0164(3) Uani 1 1 d . . . H17 H 0.1878 0.5933 0.3289 0.020 Uiso 1 1 d R . . C18 C 0.0616(2) 0.56197(12) 0.20101(12) 0.0179(3) Uani 1 1 d . . . H18 H 0.1303 0.5940 0.1713 0.021 Uiso 1 1 d R . . C19 C -0.0825(2) 0.51583(14) 0.14017(13) 0.0232(4) Uani 1 1 d . . . H19A H -0.1249 0.5531 0.0845 0.028 Uiso 1 1 d R . . H19B H -0.1660 0.5107 0.1752 0.028 Uiso 1 1 d R . . C20 C -0.0438(2) 0.42225(14) 0.10891(14) 0.0238(4) Uani 1 1 d . . . H20A H -0.1419 0.3858 0.0952 0.029 Uiso 1 1 d R . . H20B H -0.0074 0.4278 0.0506 0.029 Uiso 1 1 d 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 I1 0.02044(7) 0.01771(7) 0.02124(7) -0.00149(4) 0.00976(4) -0.00726(4) Rh1 0.01095(6) 0.01042(7) 0.01176(7) -0.00013(4) 0.00425(4) 0.00072(4) N1 0.0131(5) 0.0139(6) 0.0133(6) 0.0010(5) 0.0053(5) 0.0005(5) C1 0.0117(6) 0.0137(7) 0.0133(7) -0.0010(5) 0.0039(5) -0.0003(5) C2 0.0128(6) 0.0154(7) 0.0143(7) -0.0013(5) 0.0046(5) 0.0005(5) C3 0.0162(7) 0.0224(8) 0.0152(7) -0.0003(6) 0.0046(6) 0.0032(6) C4 0.0195(7) 0.0288(10) 0.0130(7) -0.0012(6) 0.0046(6) 0.0024(7) C5 0.0199(8) 0.0272(9) 0.0167(8) -0.0059(7) 0.0081(6) -0.0008(7) C6 0.0195(7) 0.0185(8) 0.0219(8) -0.0040(6) 0.0101(6) 0.0014(6) C7 0.0139(6) 0.0142(7) 0.0180(7) -0.0018(6) 0.0070(6) -0.0009(5) C8 0.0160(7) 0.0149(7) 0.0222(8) 0.0011(6) 0.0076(6) 0.0033(6) C9 0.0142(7) 0.0146(7) 0.0188(7) 0.0037(6) 0.0044(6) 0.0021(6) C10 0.0170(7) 0.0174(7) 0.0126(7) 0.0000(6) 0.0055(6) 0.0014(6) C11 0.0211(8) 0.0269(9) 0.0156(7) -0.0032(6) 0.0032(6) -0.0023(7) C12 0.0268(9) 0.0256(9) 0.0195(8) 0.0049(7) 0.0112(7) 0.0011(7) C13 0.0145(7) 0.0174(8) 0.0215(8) -0.0041(6) 0.0043(6) -0.0026(6) C14 0.0167(7) 0.0136(7) 0.0236(8) 0.0009(6) 0.0083(6) -0.0020(6) C15 0.0186(8) 0.0225(9) 0.0240(9) 0.0023(7) 0.0101(7) -0.0018(6) C16 0.0194(7) 0.0231(9) 0.0207(8) -0.0023(7) 0.0107(7) 0.0009(6) C17 0.0155(7) 0.0138(7) 0.0210(8) -0.0017(6) 0.0063(6) 0.0037(6) C18 0.0172(7) 0.0170(8) 0.0207(8) 0.0031(6) 0.0070(6) 0.0071(6) C19 0.0168(7) 0.0321(10) 0.0194(8) 0.0019(7) 0.0016(6) 0.0049(7) C20 0.0177(8) 0.0311(10) 0.0203(8) -0.0038(7) 0.0002(6) -0.0018(7) _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 I1 Rh1 2.6751(2) . ? Rh1 C1 2.0242(16) . ? Rh1 C13 2.1249(17) . ? Rh1 C14 2.1404(17) . ? Rh1 C17 2.2154(16) . ? Rh1 C18 2.2255(16) . ? N1 C1 1.351(2) . ? N1 C9 1.386(2) . ? N1 C10 1.496(2) . ? C1 C2 1.449(2) . ? C2 C3 1.414(2) . ? C2 C7 1.416(2) . ? C3 C4 1.379(2) . ? C3 H3 0.9500 . ? C4 C5 1.407(3) . ? C4 H4 0.9500 . ? C5 C6 1.374(3) . ? C5 H5 0.9500 . ? C6 C7 1.413(2) . ? C6 H6 0.9500 . ? C7 C8 1.423(2) . ? C8 C9 1.346(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C12 1.520(2) . ? C10 C11 1.524(2) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.406(3) . ? C13 C20 1.515(3) . ? C13 H13 0.9500 . ? C14 C15 1.524(3) . ? C14 H14 0.9500 . ? C15 C16 1.535(3) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.510(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.378(2) . ? C17 H17 0.9500 . ? C18 C19 1.521(3) . ? C18 H18 0.9500 . ? C19 C20 1.535(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? 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 C13 89.94(7) . . ? C1 Rh1 C14 94.95(7) . . ? C13 Rh1 C14 38.49(7) . . ? C1 Rh1 C17 163.19(6) . . ? C13 Rh1 C17 96.93(7) . . ? C14 Rh1 C17 81.31(7) . . ? C1 Rh1 C18 160.64(7) . . ? C13 Rh1 C18 81.24(7) . . ? C14 Rh1 C18 88.84(7) . . ? C17 Rh1 C18 36.15(6) . . ? C1 Rh1 I1 88.17(5) . . ? C13 Rh1 I1 156.67(5) . . ? C14 Rh1 I1 164.76(5) . . ? C17 Rh1 I1 91.40(5) . . ? C18 Rh1 I1 93.14(5) . . ? C1 N1 C9 124.05(14) . . ? C1 N1 C10 119.89(13) . . ? C9 N1 C10 115.99(13) . . ? N1 C1 C2 115.34(14) . . ? N1 C1 Rh1 122.87(11) . . ? C2 C1 Rh1 121.79(11) . . ? C3 C2 C7 118.64(15) . . ? C3 C2 C1 119.91(15) . . ? C7 C2 C1 121.42(15) . . ? C4 C3 C2 120.59(16) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 120.28(17) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C6 C5 C4 120.37(16) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C7 120.13(16) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? C6 C7 C2 119.85(16) . . ? C6 C7 C8 121.94(15) . . ? C2 C7 C8 118.17(15) . . ? C9 C8 C7 119.38(15) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 N1 121.42(15) . . ? C8 C9 H9 119.3 . . ? N1 C9 H9 119.3 . . ? N1 C10 C12 111.33(14) . . ? N1 C10 C11 109.59(14) . . ? C12 C10 C11 112.35(15) . . ? N1 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C20 125.63(16) . . ? C14 C13 Rh1 71.35(10) . . ? C20 C13 Rh1 110.47(12) . . ? C14 C13 H13 117.2 . . ? C20 C13 H13 117.2 . . ? Rh1 C13 H13 88.1 . . ? C13 C14 C15 123.59(16) . . ? C13 C14 Rh1 70.16(10) . . ? C15 C14 Rh1 113.56(12) . . ? C13 C14 H14 118.2 . . ? C15 C14 H14 118.2 . . ? Rh1 C14 H14 86.3 . . ? C14 C15 C16 113.07(15) . . ? C14 C15 H15A 109.0 . . ? C16 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C17 C16 C15 113.67(15) . . ? C17 C16 H16A 108.8 . . ? C15 C16 H16A 108.8 . . ? C17 C16 H16B 108.8 . . ? C15 C16 H16B 108.8 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C16 125.11(16) . . ? C18 C17 Rh1 72.33(10) . . ? C16 C17 Rh1 108.37(11) . . ? C18 C17 H17 117.4 . . ? C16 C17 H17 117.4 . . ? Rh1 C17 H17 89.3 . . ? C17 C18 C19 123.62(17) . . ? C17 C18 Rh1 71.52(10) . . ? C19 C18 Rh1 111.07(12) . . ? C17 C18 H18 118.2 . . ? C19 C18 H18 118.2 . . ? Rh1 C18 H18 87.4 . . ? C18 C19 C20 112.54(15) . . ? C18 C19 H19A 109.1 . . ? C20 C19 H19A 109.1 . . ? C18 C19 H19B 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.8 . . ? C13 C20 C19 113.21(15) . . ? C13 C20 H20A 108.9 . . ? C19 C20 H20A 108.9 . . ? C13 C20 H20B 108.9 . . ? C19 C20 H20B 108.9 . . ? H20A C20 H20B 107.7 . . ? 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 C9 N1 C1 C2 -2.0(2) . . . . ? C10 N1 C1 C2 174.84(14) . . . . ? C9 N1 C1 Rh1 177.80(12) . . . . ? C10 N1 C1 Rh1 -5.4(2) . . . . ? C13 Rh1 C1 N1 -110.84(14) . . . . ? C14 Rh1 C1 N1 -72.63(14) . . . . ? C17 Rh1 C1 N1 3.6(3) . . . . ? C18 Rh1 C1 N1 -173.30(16) . . . . ? I1 Rh1 C1 N1 92.42(13) . . . . ? C13 Rh1 C1 C2 68.90(14) . . . . ? C14 Rh1 C1 C2 107.11(13) . . . . ? C17 Rh1 C1 C2 -176.65(18) . . . . ? C18 Rh1 C1 C2 6.4(3) . . . . ? I1 Rh1 C1 C2 -87.84(13) . . . . ? N1 C1 C2 C3 -173.30(15) . . . . ? Rh1 C1 C2 C3 6.9(2) . . . . ? N1 C1 C2 C7 5.0(2) . . . . ? Rh1 C1 C2 C7 -174.74(12) . . . . ? C7 C2 C3 C4 0.3(3) . . . . ? C1 C2 C3 C4 178.64(16) . . . . ? C2 C3 C4 C5 2.4(3) . . . . ? C3 C4 C5 C6 -2.0(3) . . . . ? C4 C5 C6 C7 -1.2(3) . . . . ? C5 C6 C7 C2 3.9(3) . . . . ? C5 C6 C7 C8 -173.66(17) . . . . ? C3 C2 C7 C6 -3.4(2) . . . . ? C1 C2 C7 C6 178.27(15) . . . . ? C3 C2 C7 C8 174.22(16) . . . . ? C1 C2 C7 C8 -4.1(2) . . . . ? C6 C7 C8 C9 177.54(17) . . . . ? C2 C7 C8 C9 0.0(2) . . . . ? C7 C8 C9 N1 3.1(3) . . . . ? C1 N1 C9 C8 -2.1(3) . . . . ? C10 N1 C9 C8 -179.01(16) . . . . ? C1 N1 C10 C12 126.73(16) . . . . ? C9 N1 C10 C12 -56.23(19) . . . . ? C1 N1 C10 C11 -108.36(17) . . . . ? C9 N1 C10 C11 68.68(18) . . . . ? C1 Rh1 C13 C14 98.04(11) . . . . ? C17 Rh1 C13 C14 -66.58(11) . . . . ? C18 Rh1 C13 C14 -99.26(11) . . . . ? I1 Rh1 C13 C14 -176.71(9) . . . . ? C1 Rh1 C13 C20 -139.94(13) . . . . ? C14 Rh1 C13 C20 122.02(17) . . . . ? C17 Rh1 C13 C20 55.44(14) . . . . ? C18 Rh1 C13 C20 22.76(13) . . . . ? I1 Rh1 C13 C20 -54.7(2) . . . . ? C20 C13 C14 C15 3.4(3) . . . . ? Rh1 C13 C14 C15 105.70(16) . . . . ? C20 C13 C14 Rh1 -102.25(18) . . . . ? C1 Rh1 C14 C13 -83.65(11) . . . . ? C17 Rh1 C14 C13 112.85(11) . . . . ? C18 Rh1 C14 C13 77.33(11) . . . . ? I1 Rh1 C14 C13 175.04(14) . . . . ? C1 Rh1 C14 C15 157.38(13) . . . . ? C13 Rh1 C14 C15 -118.97(17) . . . . ? C17 Rh1 C14 C15 -6.11(13) . . . . ? C18 Rh1 C14 C15 -41.64(13) . . . . ? I1 Rh1 C14 C15 56.1(3) . . . . ? C13 C14 C15 C16 -92.2(2) . . . . ? Rh1 C14 C15 C16 -11.1(2) . . . . ? C14 C15 C16 C17 31.1(2) . . . . ? C15 C16 C17 C18 46.2(2) . . . . ? C15 C16 C17 Rh1 -34.71(18) . . . . ? C1 Rh1 C17 C18 -178.3(2) . . . . ? C13 Rh1 C17 C18 -64.76(12) . . . . ? C14 Rh1 C17 C18 -100.05(12) . . . . ? I1 Rh1 C17 C18 93.40(10) . . . . ? C1 Rh1 C17 C16 -56.2(3) . . . . ? C13 Rh1 C17 C16 57.26(13) . . . . ? C14 Rh1 C17 C16 21.97(12) . . . . ? C18 Rh1 C17 C16 122.02(17) . . . . ? I1 Rh1 C17 C16 -144.58(11) . . . . ? C16 C17 C18 C19 3.1(3) . . . . ? Rh1 C17 C18 C19 103.48(17) . . . . ? C16 C17 C18 Rh1 -100.39(16) . . . . ? C1 Rh1 C18 C17 178.49(17) . . . . ? C13 Rh1 C18 C17 114.70(12) . . . . ? C14 Rh1 C18 C17 76.80(11) . . . . ? I1 Rh1 C18 C17 -88.08(10) . . . . ? C1 Rh1 C18 C19 58.7(3) . . . . ? C13 Rh1 C18 C19 -5.09(13) . . . . ? C14 Rh1 C18 C19 -43.00(13) . . . . ? C17 Rh1 C18 C19 -119.79(18) . . . . ? I1 Rh1 C18 C19 152.13(12) . . . . ? C17 C18 C19 C20 -94.8(2) . . . . ? Rh1 C18 C19 C20 -13.5(2) . . . . ? C14 C13 C20 C19 43.6(3) . . . . ? Rh1 C13 C20 C19 -37.6(2) . . . . ? C18 C19 C20 C13 33.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.927 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.080 ###END #========================================================================= # Data for compound 10c (local labelling ea05605b) #========================================================================= data_10c _database_code_depnum_ccdc_archive 'CCDC 621898' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H27 Cl N O Rh' _chemical_formula_sum 'C21 H27 Cl N O Rh' _chemical_formula_weight 447.80 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_int_tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' 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 11.3168(5) _cell_length_b 11.1197(5) _cell_length_c 16.5538(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.178(2) _cell_angle_gamma 90.00 _cell_volume 1979.16(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8451 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 36.07 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.503 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 1.006 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7134 _exptl_absorpt_correction_T_max 0.8165 _exptl_absorpt_process_details ; SADABS: Area-Detector Absorption Correction. Bruker-AXS within v. 7.06 a (Bruker AXS, 2003); ratio of minimum to maximum apparent transmission: 0.557670m ; _diffrn_ambient_temperature 100(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 ; Bruker-Nonius X8kappa APEX II CCD area detector' ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 41044 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0138 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 36.25 _reflns_number_total 9537 _reflns_number_gt 7943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-W2K-NT v. 1.0 (Bruker AXS, 2004)' _computing_cell_refinement 'SAINT+ v. 7.06 a (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 7.06 a (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.12 (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0348P)^2^+1.9016P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9537 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0824 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.793094(10) 0.239981(10) 0.417024(6) 0.01755(4) Uani 1 1 d . . . Cl1 Cl 0.71308(4) 0.33055(4) 0.27970(2) 0.02324(7) Uani 1 1 d . . . O1 O 1.36732(13) 0.21905(13) 0.36685(11) 0.0328(3) Uani 1 1 d . . . N1 N 0.82504(12) 0.02026(12) 0.32117(8) 0.0192(2) Uani 1 1 d . . . C1 C 0.88057(13) 0.11903(13) 0.36431(8) 0.0174(2) Uani 1 1 d . . . C2 C 1.00617(13) 0.14040(13) 0.36416(9) 0.0179(2) Uani 1 1 d . . . C3 C 1.07471(15) 0.23893(13) 0.41000(10) 0.0207(2) Uani 1 1 d . . . H3 H 1.0374 0.2904 0.4409 0.025 Uiso 1 1 d R . . C4 C 1.19449(16) 0.26102(14) 0.41039(11) 0.0239(3) Uani 1 1 d . . . H4 H 1.2399 0.3264 0.4423 0.029 Uiso 1 1 d R . . C5 C 1.25012(15) 0.18624(15) 0.36309(11) 0.0240(3) Uani 1 1 d . . . C6 C 1.18662(15) 0.09017(15) 0.31722(10) 0.0223(3) Uani 1 1 d . . . H6 H 1.2243 0.0409 0.2853 0.027 Uiso 1 1 d R . . C7 C 1.06451(14) 0.06579(13) 0.31825(9) 0.0187(2) Uani 1 1 d . . . C8 C 0.99719(15) -0.03466(14) 0.27417(9) 0.0215(3) Uani 1 1 d . . . H8 H 1.0334 -0.0868 0.2430 0.026 Uiso 1 1 d R . . C9 C 0.88131(15) -0.05503(14) 0.27713(9) 0.0219(3) Uani 1 1 d . . . H9 H 0.8368 -0.1229 0.2482 0.026 Uiso 1 1 d R . . C10 C 0.69438(14) -0.01048(15) 0.31615(10) 0.0225(3) Uani 1 1 d . . . H10 H 0.6666 0.0498 0.3513 0.027 Uiso 1 1 d R . . C11 C 0.6886(2) -0.13429(18) 0.35472(13) 0.0335(4) Uani 1 1 d . . . H11A H 0.7175 -0.1954 0.3226 0.050 Uiso 1 1 d R . . H11B H 0.6027 -0.1519 0.3522 0.050 Uiso 1 1 d R . . H11C H 0.7419 -0.1350 0.4141 0.050 Uiso 1 1 d R . . C12 C 0.60818(16) 0.00117(18) 0.22495(11) 0.0276(3) Uani 1 1 d . . . H12A H 0.6094 0.0843 0.2056 0.041 Uiso 1 1 d R . . H12B H 0.5233 -0.0205 0.2227 0.041 Uiso 1 1 d R . . H12C H 0.6365 -0.0528 0.1880 0.041 Uiso 1 1 d R . . C13 C 1.42877(18) 0.14471(19) 0.32116(15) 0.0359(4) Uani 1 1 d . . . H13A H 1.4464 0.0658 0.3486 0.054 Uiso 1 1 d R . . H13B H 1.5069 0.1829 0.3214 0.054 Uiso 1 1 d R . . H13C H 1.3749 0.1348 0.2624 0.054 Uiso 1 1 d R . . C14 C 0.7725(2) 0.41024(16) 0.47928(11) 0.0330(4) Uani 1 1 d . . . H14 H 0.7815 0.4520 0.4315 0.040 Uiso 1 1 d R . . C15 C 0.6644(2) 0.34766(19) 0.46802(11) 0.0334(4) Uani 1 1 d . . . H15 H 0.6048 0.3477 0.4130 0.040 Uiso 1 1 d R . . C16 C 0.6334(2) 0.2782(2) 0.53797(13) 0.0393(5) Uani 1 1 d . . . H16A H 0.5429 0.2838 0.5290 0.047 Uiso 1 1 d R . . H16B H 0.6771 0.3157 0.5935 0.047 Uiso 1 1 d R . . C17 C 0.67060(19) 0.1448(2) 0.54067(12) 0.0337(4) Uani 1 1 d . . . H17A H 0.6840 0.1136 0.5989 0.040 Uiso 1 1 d R . . H17B H 0.6012 0.0989 0.5016 0.040 Uiso 1 1 d R . . C18 C 0.78700(15) 0.12357(15) 0.51623(9) 0.0228(3) Uani 1 1 d . . . H18 H 0.7857 0.0581 0.4791 0.027 Uiso 1 1 d R . . C19 C 0.89732(16) 0.19221(15) 0.54345(9) 0.0232(3) Uani 1 1 d . . . H19 H 0.9630 0.1724 0.5214 0.028 Uiso 1 1 d R . . C20 C 0.9171(2) 0.29630(18) 0.60617(11) 0.0336(4) Uani 1 1 d . . . H20A H 1.0059 0.2994 0.6408 0.040 Uiso 1 1 d R . . H20B H 0.8677 0.2817 0.6452 0.040 Uiso 1 1 d R . . C21 C 0.8791(3) 0.41836(18) 0.56157(12) 0.0405(5) Uani 1 1 d . . . H21A H 0.8549 0.4733 0.6008 0.049 Uiso 1 1 d R . . H21B H 0.9520 0.4539 0.5496 0.049 Uiso 1 1 d 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 0.02302(6) 0.01677(6) 0.01264(5) 0.00102(3) 0.00522(4) 0.00462(3) Cl1 0.02733(16) 0.02593(17) 0.01664(13) 0.00667(12) 0.00713(12) 0.00403(13) O1 0.0241(5) 0.0282(6) 0.0491(8) 0.0039(6) 0.0159(6) 0.0003(5) N1 0.0221(5) 0.0191(5) 0.0154(5) -0.0014(4) 0.0047(4) 0.0003(4) C1 0.0216(6) 0.0165(6) 0.0131(5) 0.0009(4) 0.0038(4) 0.0022(4) C2 0.0210(6) 0.0164(6) 0.0152(5) 0.0011(4) 0.0043(4) 0.0032(4) C3 0.0232(6) 0.0171(6) 0.0207(6) -0.0004(5) 0.0051(5) 0.0021(5) C4 0.0239(6) 0.0189(6) 0.0275(7) 0.0014(5) 0.0061(5) -0.0003(5) C5 0.0218(6) 0.0215(7) 0.0290(7) 0.0074(5) 0.0083(5) 0.0031(5) C6 0.0239(6) 0.0216(7) 0.0226(6) 0.0045(5) 0.0092(5) 0.0064(5) C7 0.0219(6) 0.0180(6) 0.0156(5) 0.0020(4) 0.0050(4) 0.0043(5) C8 0.0269(7) 0.0201(6) 0.0167(5) -0.0017(5) 0.0055(5) 0.0057(5) C9 0.0266(7) 0.0196(6) 0.0177(6) -0.0038(5) 0.0045(5) 0.0021(5) C10 0.0220(6) 0.0257(7) 0.0191(6) -0.0021(5) 0.0053(5) -0.0039(5) C11 0.0402(9) 0.0297(9) 0.0299(8) 0.0014(7) 0.0101(7) -0.0091(7) C12 0.0240(7) 0.0349(9) 0.0212(6) -0.0033(6) 0.0031(5) -0.0027(6) C13 0.0285(8) 0.0330(9) 0.0518(12) 0.0094(8) 0.0205(8) 0.0064(7) C14 0.0569(12) 0.0210(7) 0.0200(6) 0.0004(5) 0.0102(7) 0.0147(7) C15 0.0460(10) 0.0356(9) 0.0211(7) 0.0056(6) 0.0140(7) 0.0227(8) C16 0.0479(11) 0.0502(12) 0.0260(8) 0.0103(8) 0.0207(8) 0.0239(10) C17 0.0395(9) 0.0430(10) 0.0232(7) 0.0111(7) 0.0165(7) 0.0106(8) C18 0.0300(7) 0.0246(7) 0.0137(5) 0.0028(5) 0.0068(5) 0.0055(5) C19 0.0323(7) 0.0203(7) 0.0143(5) -0.0003(5) 0.0031(5) 0.0061(5) C20 0.0528(11) 0.0244(8) 0.0170(6) -0.0030(6) 0.0015(7) 0.0070(7) C21 0.0697(15) 0.0214(8) 0.0228(7) -0.0040(6) 0.0035(8) 0.0085(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 2.0223(14) . ? Rh1 C18 2.1090(15) . ? Rh1 C19 2.1244(15) . ? Rh1 C14 2.2023(17) . ? Rh1 C15 2.2440(17) . ? Rh1 Cl1 2.3912(4) . ? O1 C5 1.358(2) . ? O1 C13 1.438(2) . ? N1 C1 1.3532(19) . ? N1 C9 1.3883(19) . ? N1 C10 1.495(2) . ? C1 C2 1.442(2) . ? C2 C3 1.418(2) . ? C2 C7 1.420(2) . ? C3 C4 1.376(2) . ? C3 H3 0.9500 . ? C4 C5 1.417(2) . ? C4 H4 0.9500 . ? C5 C6 1.376(2) . ? C6 C7 1.414(2) . ? C6 H6 0.9500 . ? C7 C8 1.419(2) . ? C8 C9 1.347(2) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C12 1.526(2) . ? C10 C11 1.527(3) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.369(3) . ? C14 C21 1.514(3) . ? C14 H14 0.9500 . ? C15 C16 1.521(3) . ? C15 H15 0.9500 . ? C16 C17 1.538(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.512(2) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.412(2) . ? C18 H18 0.9500 . ? C19 C20 1.524(2) . ? C19 H19 0.9500 . ? C20 C21 1.541(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? 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 C18 93.85(6) . . ? C1 Rh1 C19 93.60(6) . . ? C18 Rh1 C19 38.96(7) . . ? C1 Rh1 C14 155.65(8) . . ? C18 Rh1 C14 97.43(6) . . ? C19 Rh1 C14 82.02(6) . . ? C1 Rh1 C15 168.48(8) . . ? C18 Rh1 C15 81.48(6) . . ? C19 Rh1 C15 89.36(6) . . ? C14 Rh1 C15 35.86(9) . . ? C1 Rh1 Cl1 87.77(4) . . ? C18 Rh1 Cl1 154.70(5) . . ? C19 Rh1 Cl1 166.19(5) . . ? C14 Rh1 Cl1 91.08(5) . . ? C15 Rh1 Cl1 92.02(5) . . ? C5 O1 C13 116.56(16) . . ? C1 N1 C9 123.57(13) . . ? C1 N1 C10 120.23(12) . . ? C9 N1 C10 116.15(13) . . ? N1 C1 C2 115.38(12) . . ? N1 C1 Rh1 123.94(11) . . ? C2 C1 Rh1 120.44(10) . . ? C3 C2 C7 118.03(13) . . ? C3 C2 C1 120.09(13) . . ? C7 C2 C1 121.87(13) . . ? C4 C3 C2 120.95(14) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.97(15) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? O1 C5 C6 124.63(16) . . ? O1 C5 C4 114.38(16) . . ? C6 C5 C4 120.98(15) . . ? C5 C6 C7 119.11(14) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.4 . . ? C6 C7 C8 120.99(14) . . ? C6 C7 C2 120.94(14) . . ? C8 C7 C2 118.07(13) . . ? C9 C8 C7 119.10(14) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.4 . . ? C8 C9 N1 121.94(14) . . ? C8 C9 H9 119.0 . . ? N1 C9 H9 119.0 . . ? N1 C10 C12 110.58(13) . . ? N1 C10 C11 110.71(14) . . ? C12 C10 C11 113.11(14) . . ? N1 C10 H10 107.4 . . ? C12 C10 H10 107.4 . . ? C11 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.4 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O1 C13 H13A 109.4 . . ? O1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? O1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C21 125.43(18) . . ? C15 C14 Rh1 73.73(11) . . ? C21 C14 Rh1 107.55(12) . . ? C15 C14 H14 117.3 . . ? C21 C14 H14 117.3 . . ? Rh1 C14 H14 88.6 . . ? C14 C15 C16 124.26(19) . . ? C14 C15 Rh1 70.41(10) . . ? C16 C15 Rh1 110.25(12) . . ? C14 C15 H15 117.9 . . ? C16 C15 H15 117.9 . . ? Rh1 C15 H15 89.4 . . ? C15 C16 C17 112.70(15) . . ? C15 C16 H16A 109.0 . . ? C17 C16 H16A 109.0 . . ? C15 C16 H16B 109.1 . . ? C17 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? C18 C17 C16 113.33(17) . . ? C18 C17 H17A 108.9 . . ? C16 C17 H17A 108.9 . . ? C18 C17 H17B 108.9 . . ? C16 C17 H17B 108.9 . . ? H17A C17 H17B 107.7 . . ? C19 C18 C17 125.97(16) . . ? C19 C18 Rh1 71.11(9) . . ? C17 C18 Rh1 110.80(11) . . ? C19 C18 H18 117.0 . . ? C17 C18 H18 117.0 . . ? Rh1 C18 H18 88.0 . . ? C18 C19 C20 123.73(16) . . ? C18 C19 Rh1 69.93(8) . . ? C20 C19 Rh1 113.56(11) . . ? C18 C19 H19 118.1 . . ? C20 C19 H19 118.1 . . ? Rh1 C19 H19 86.5 . . ? C19 C20 C21 112.51(14) . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C14 C21 C20 113.80(17) . . ? C14 C21 H21A 108.8 . . ? C20 C21 H21A 108.8 . . ? C14 C21 H21B 108.8 . . ? C20 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? 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 C9 N1 C1 C2 -1.8(2) . . . . ? C10 N1 C1 C2 -179.42(12) . . . . ? C9 N1 C1 Rh1 172.54(11) . . . . ? C10 N1 C1 Rh1 -5.05(18) . . . . ? C18 Rh1 C1 N1 72.61(12) . . . . ? C19 Rh1 C1 N1 111.66(12) . . . . ? C14 Rh1 C1 N1 -169.78(13) . . . . ? C15 Rh1 C1 N1 7.0(4) . . . . ? Cl1 Rh1 C1 N1 -82.10(11) . . . . ? C18 Rh1 C1 C2 -113.29(11) . . . . ? C19 Rh1 C1 C2 -74.24(12) . . . . ? C14 Rh1 C1 C2 4.3(2) . . . . ? C15 Rh1 C1 C2 -178.9(3) . . . . ? Cl1 Rh1 C1 C2 91.99(10) . . . . ? N1 C1 C2 C3 -177.71(13) . . . . ? Rh1 C1 C2 C3 7.71(18) . . . . ? N1 C1 C2 C7 2.98(19) . . . . ? Rh1 C1 C2 C7 -171.60(10) . . . . ? C7 C2 C3 C4 -0.4(2) . . . . ? C1 C2 C3 C4 -179.77(14) . . . . ? C2 C3 C4 C5 1.3(2) . . . . ? C13 O1 C5 C6 -1.9(3) . . . . ? C13 O1 C5 C4 178.90(16) . . . . ? C3 C4 C5 O1 178.42(15) . . . . ? C3 C4 C5 C6 -0.8(2) . . . . ? O1 C5 C6 C7 -179.71(15) . . . . ? C4 C5 C6 C7 -0.5(2) . . . . ? C5 C6 C7 C8 -177.89(14) . . . . ? C5 C6 C7 C2 1.4(2) . . . . ? C3 C2 C7 C6 -1.0(2) . . . . ? C1 C2 C7 C6 178.37(13) . . . . ? C3 C2 C7 C8 178.39(13) . . . . ? C1 C2 C7 C8 -2.3(2) . . . . ? C6 C7 C8 C9 179.66(14) . . . . ? C2 C7 C8 C9 0.3(2) . . . . ? C7 C8 C9 N1 0.8(2) . . . . ? C1 N1 C9 C8 0.0(2) . . . . ? C10 N1 C9 C8 177.65(14) . . . . ? C1 N1 C10 C12 113.65(15) . . . . ? C9 N1 C10 C12 -64.11(18) . . . . ? C1 N1 C10 C11 -120.18(16) . . . . ? C9 N1 C10 C11 62.06(17) . . . . ? C1 Rh1 C14 C15 178.91(12) . . . . ? C18 Rh1 C14 C15 -64.17(11) . . . . ? C19 Rh1 C14 C15 -100.06(11) . . . . ? Cl1 Rh1 C14 C15 91.95(10) . . . . ? C1 Rh1 C14 C21 -58.3(2) . . . . ? C18 Rh1 C14 C21 58.59(16) . . . . ? C19 Rh1 C14 C21 22.69(15) . . . . ? C15 Rh1 C14 C21 122.76(19) . . . . ? Cl1 Rh1 C14 C21 -145.29(15) . . . . ? C21 C14 C15 C16 1.4(3) . . . . ? Rh1 C14 C15 C16 101.66(17) . . . . ? C21 C14 C15 Rh1 -100.25(17) . . . . ? C1 Rh1 C15 C14 -177.8(3) . . . . ? C18 Rh1 C15 C14 115.51(11) . . . . ? C19 Rh1 C15 C14 77.20(11) . . . . ? Cl1 Rh1 C15 C14 -89.05(10) . . . . ? C1 Rh1 C15 C16 61.9(4) . . . . ? C18 Rh1 C15 C16 -4.86(16) . . . . ? C19 Rh1 C15 C16 -43.17(17) . . . . ? C14 Rh1 C15 C16 -120.4(2) . . . . ? Cl1 Rh1 C15 C16 150.58(16) . . . . ? C14 C15 C16 C17 -93.3(3) . . . . ? Rh1 C15 C16 C17 -13.7(2) . . . . ? C15 C16 C17 C18 33.8(3) . . . . ? C16 C17 C18 C19 43.6(2) . . . . ? C16 C17 C18 Rh1 -37.63(19) . . . . ? C1 Rh1 C18 C19 90.96(9) . . . . ? C14 Rh1 C18 C19 -67.42(11) . . . . ? C15 Rh1 C18 C19 -99.64(11) . . . . ? Cl1 Rh1 C18 C19 -176.12(8) . . . . ? C1 Rh1 C18 C17 -146.76(13) . . . . ? C19 Rh1 C18 C17 122.29(17) . . . . ? C14 Rh1 C18 C17 54.86(14) . . . . ? C15 Rh1 C18 C17 22.65(14) . . . . ? Cl1 Rh1 C18 C17 -53.83(18) . . . . ? C17 C18 C19 C20 3.1(2) . . . . ? Rh1 C18 C19 C20 105.52(15) . . . . ? C17 C18 C19 Rh1 -102.44(15) . . . . ? C1 Rh1 C19 C18 -91.68(10) . . . . ? C14 Rh1 C19 C18 112.40(11) . . . . ? C15 Rh1 C19 C18 77.17(11) . . . . ? Cl1 Rh1 C19 C18 173.04(15) . . . . ? C1 Rh1 C19 C20 149.27(14) . . . . ? C18 Rh1 C19 C20 -119.05(18) . . . . ? C14 Rh1 C19 C20 -6.66(15) . . . . ? C15 Rh1 C19 C20 -41.88(15) . . . . ? Cl1 Rh1 C19 C20 54.0(3) . . . . ? C18 C19 C20 C21 -91.8(2) . . . . ? Rh1 C19 C20 C21 -10.9(2) . . . . ? C15 C14 C21 C20 46.6(3) . . . . ? Rh1 C14 C21 C20 -35.6(2) . . . . ? C19 C20 C21 C14 31.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 32.25 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 2.615 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.093 ###END #========================================================================= # Data for compound 11a (local labelling ea03705a) #========================================================================= data_11a _database_code_depnum_ccdc_archive 'CCDC 621899' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H27 Cl N Rh' _chemical_formula_sum 'C25 H27 Cl N Rh' _chemical_formula_weight 479.84 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(1)2(1)2 _symmetry_space_group_name_Hall 'P 4abw 2nw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 10.6791(1) _cell_length_b 10.6791(1) _cell_length_c 36.8984(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4208.01(9) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6239 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 30.27 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1968 _exptl_absorpt_coefficient_mu 0.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6747 _exptl_absorpt_correction_T_max 0.8042 _exptl_absorpt_process_details ; Correction for absorption, crystal decay (insignificant) and effects of the CCD detector by semi-empirical method from equivalents using program SADABS (G.M. Sheldrick, 1996, Univ. of Goettingen, Germany). ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEX CCD system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_number 0 _diffrn_reflns_number 24766 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 51 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 30.49 _reflns_number_total 6277 _reflns_number_gt 5826 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX-W2K-NT v. 1.0 (Bruker AXS, 2004)' _computing_cell_refinement 'SAINT+ v. 7.06 a (Bruker AXS, 2003)' _computing_data_reduction 'SAINT+ v. 7.06 a (Bruker AXS, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP, SHELXTL v. 6.10 (Bruker, 2000)' _computing_publication_material 'XCIF, SHELXTL v. 6.12 (Bruker, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+0.8337P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.020(19) _refine_ls_number_reflns 6277 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0216 _refine_ls_wR_factor_ref 0.0493 _refine_ls_wR_factor_gt 0.0487 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.008 _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 0.756421(12) 0.819232(11) 0.795203(3) 0.02082(4) Uani 1 1 d . . . Cl1 Cl 0.76078(5) 0.79537(4) 0.730778(10) 0.03743(11) Uani 1 1 d . . . N1 N 0.67442(14) 0.55345(13) 0.79733(4) 0.0235(3) Uani 1 1 d . . . C1 C 0.63622(15) 0.67339(16) 0.79716(4) 0.0231(3) Uani 1 1 d . . . C2 C 0.50217(16) 0.69209(17) 0.79658(5) 0.0251(3) Uani 1 1 d . . . C3 C 0.45256(18) 0.81517(19) 0.79622(5) 0.0309(4) Uani 1 1 d . . . H3 H 0.5077 0.8850 0.7965 0.037 Uiso 1 1 d R . . C4 C 0.3247(2) 0.8348(2) 0.79546(5) 0.0409(4) Uani 1 1 d . . . H4 H 0.2922 0.9175 0.7952 0.049 Uiso 1 1 d R . . C5 C 0.24326(19) 0.7321(2) 0.79513(5) 0.0434(5) Uani 1 1 d . . . H5 H 0.1555 0.7462 0.7944 0.052 Uiso 1 1 d R . . C6 C 0.28764(17) 0.6118(2) 0.79561(5) 0.0362(4) Uani 1 1 d . . . H6 H 0.2308 0.5434 0.7957 0.043 Uiso 1 1 d R . . C7 C 0.41791(17) 0.58993(17) 0.79606(5) 0.0274(4) Uani 1 1 d . . . C8 C 0.46869(18) 0.46711(17) 0.79572(5) 0.0297(4) Uani 1 1 d . . . H8 H 0.4149 0.3963 0.7950 0.036 Uiso 1 1 d R . . C9 C 0.59284(18) 0.45165(16) 0.79630(5) 0.0284(4) Uani 1 1 d . . . H9 H 0.6266 0.3693 0.7959 0.034 Uiso 1 1 d R . . C10 C 0.81149(18) 0.52457(16) 0.79642(5) 0.0257(3) Uani 1 1 d . . . H10 H 0.8568 0.6059 0.7992 0.031 Uiso 1 1 d R . . C11 C 0.84881(17) 0.44245(16) 0.82837(5) 0.0264(4) Uani 1 1 d . . . C12 C 0.95544(19) 0.36692(18) 0.82575(6) 0.0355(4) Uani 1 1 d . . . H12 H 1.0014 0.3642 0.8037 0.043 Uiso 1 1 d R . . C13 C 0.9933(2) 0.2960(2) 0.85509(8) 0.0512(7) Uani 1 1 d . . . H13 H 1.0660 0.2454 0.8531 0.061 Uiso 1 1 d R . . C14 C 0.9276(2) 0.2981(2) 0.88719(7) 0.0519(7) Uani 1 1 d . . . H14 H 0.9548 0.2489 0.9071 0.062 Uiso 1 1 d R . . C15 C 0.8220(2) 0.3720(2) 0.89010(5) 0.0440(5) Uani 1 1 d . . . H15 H 0.7760 0.3731 0.9121 0.053 Uiso 1 1 d R . . C16 C 0.7830(2) 0.44473(18) 0.86085(5) 0.0336(4) Uani 1 1 d . . . H16 H 0.7108 0.4961 0.8631 0.040 Uiso 1 1 d R . . C17 C 0.8459(2) 0.4726(2) 0.75930(5) 0.0403(5) Uani 1 1 d . . . H17A H 0.8085 0.3895 0.7563 0.060 Uiso 1 1 d R . . H17B H 0.9372 0.4662 0.7573 0.060 Uiso 1 1 d R . . H17C H 0.8141 0.5288 0.7404 0.060 Uiso 1 1 d R . . C18 C 0.92153(17) 0.94990(17) 0.79517(5) 0.0304(4) Uani 1 1 d . . . H18 H 0.9546 0.9060 0.7749 0.037 Uiso 1 1 d R . . C19 C 0.81380(19) 1.01765(16) 0.79038(5) 0.0295(4) Uani 1 1 d . . . H19 H 0.7808 1.0211 0.7665 0.035 Uiso 1 1 d R . . C20 C 0.7422(2) 1.08848(16) 0.81927(5) 0.0329(4) Uani 1 1 d . . . H20A H 0.7841 1.1696 0.8238 0.039 Uiso 1 1 d R . . H20B H 0.6568 1.1065 0.8102 0.039 Uiso 1 1 d R . . C21 C 0.7318(2) 1.01703(17) 0.85494(5) 0.0329(4) Uani 1 1 d . . . H21A H 0.6592 1.0492 0.8688 0.039 Uiso 1 1 d R . . H21B H 0.8081 1.0326 0.8695 0.039 Uiso 1 1 d R . . C22 C 0.71655(18) 0.87641(18) 0.84940(4) 0.0286(4) Uani 1 1 d . . . H22 H 0.6344 0.8444 0.8459 0.034 Uiso 1 1 d R . . C23 C 0.81689(19) 0.79188(16) 0.84927(4) 0.0302(4) Uani 1 1 d . . . H23 H 0.7972 0.7057 0.8464 0.036 Uiso 1 1 d R . . C24 C 0.9530(2) 0.8257(2) 0.85287(5) 0.0366(4) Uani 1 1 d . . . H24A H 1.0046 0.7537 0.8450 0.044 Uiso 1 1 d R . . H24B H 0.9715 0.8416 0.8788 0.044 Uiso 1 1 d R . . C25 C 0.99060(18) 0.9411(2) 0.83070(5) 0.0348(4) Uani 1 1 d . . . H25A H 0.9730 1.0173 0.8451 0.042 Uiso 1 1 d R . . H25B H 1.0818 0.9383 0.8260 0.042 Uiso 1 1 d 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 0.02540(7) 0.01863(6) 0.01844(5) 0.00159(4) 0.00090(6) -0.00115(5) Cl1 0.0560(3) 0.0363(2) 0.01993(16) 0.00192(15) 0.0010(2) -0.0091(2) N1 0.0278(7) 0.0212(6) 0.0214(6) 0.0016(6) 0.0005(6) -0.0021(6) C1 0.0313(8) 0.0217(8) 0.0163(6) 0.0008(7) 0.0028(6) -0.0017(6) C2 0.0288(8) 0.0277(8) 0.0188(7) -0.0021(7) 0.0013(7) -0.0012(7) C3 0.0336(9) 0.0281(9) 0.0312(8) -0.0043(9) 0.0015(8) 0.0014(7) C4 0.0359(10) 0.0416(11) 0.0452(10) -0.0092(10) 0.0027(10) 0.0110(9) C5 0.0273(9) 0.0562(13) 0.0466(10) -0.0114(10) 0.0056(10) 0.0025(10) C6 0.0304(10) 0.0477(12) 0.0305(8) -0.0043(9) 0.0043(8) -0.0092(8) C7 0.0319(9) 0.0325(10) 0.0177(7) -0.0006(7) 0.0036(7) -0.0041(7) C8 0.0393(10) 0.0260(9) 0.0236(7) 0.0028(7) -0.0021(8) -0.0101(7) C9 0.0411(11) 0.0184(8) 0.0258(7) 0.0011(7) -0.0008(8) -0.0046(7) C10 0.0279(9) 0.0215(8) 0.0277(8) 0.0007(7) 0.0032(8) 0.0021(7) C11 0.0295(10) 0.0180(8) 0.0316(8) 0.0006(7) -0.0049(7) -0.0030(6) C12 0.0283(10) 0.0252(9) 0.0530(11) -0.0037(9) -0.0077(9) -0.0025(7) C13 0.0355(12) 0.0279(11) 0.0902(19) 0.0068(11) -0.0283(13) -0.0026(9) C14 0.0585(15) 0.0343(12) 0.0631(15) 0.0224(11) -0.0344(13) -0.0169(10) C15 0.0592(15) 0.0383(12) 0.0345(9) 0.0128(9) -0.0142(10) -0.0171(11) C16 0.0455(13) 0.0265(9) 0.0286(9) 0.0037(8) -0.0041(8) -0.0026(8) C17 0.0452(13) 0.0457(13) 0.0301(9) -0.0034(9) 0.0068(9) 0.0089(9) C18 0.0281(9) 0.0317(10) 0.0315(8) 0.0000(8) 0.0000(8) -0.0064(7) C19 0.0322(9) 0.0228(8) 0.0334(9) 0.0050(7) -0.0052(8) -0.0065(7) C20 0.0341(10) 0.0209(8) 0.0437(9) -0.0025(7) -0.0085(10) 0.0025(8) C21 0.0344(11) 0.0285(9) 0.0357(9) -0.0099(7) 0.0023(8) 0.0058(8) C22 0.0331(10) 0.0297(9) 0.0230(7) -0.0034(7) 0.0024(7) -0.0023(7) C23 0.0465(11) 0.0249(9) 0.0191(7) -0.0008(6) -0.0015(8) 0.0016(8) C24 0.0430(11) 0.0405(11) 0.0264(8) -0.0055(9) -0.0087(8) 0.0141(9) C25 0.0254(10) 0.0386(11) 0.0404(10) -0.0068(8) -0.0050(8) 0.0029(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 2.0196(17) . ? Rh1 C23 2.1171(16) . ? Rh1 C22 2.1337(16) . ? Rh1 C19 2.2129(17) . ? Rh1 C18 2.2486(18) . ? Rh1 Cl1 2.3913(4) . ? N1 C1 1.344(2) . ? N1 C9 1.394(2) . ? N1 C10 1.496(2) . ? C1 C2 1.446(2) . ? C2 C7 1.414(3) . ? C2 C3 1.417(2) . ? C3 C4 1.381(3) . ? C3 H3 0.9500 . ? C4 C5 1.399(3) . ? C4 H4 0.9500 . ? C5 C6 1.370(3) . ? C5 H5 0.9500 . ? C6 C7 1.411(3) . ? C6 H6 0.9500 . ? C7 C8 1.419(3) . ? C8 C9 1.336(3) . ? C8 H8 0.9500 . ? C9 H9 0.9500 . ? C10 C11 1.522(2) . ? C10 C17 1.523(2) . ? C10 H10 1.0000 . ? C11 C16 1.390(3) . ? C11 C12 1.399(3) . ? C12 C13 1.381(3) . ? C12 H12 0.9500 . ? C13 C14 1.377(4) . ? C13 H13 0.9500 . ? C14 C15 1.380(4) . ? C14 H14 0.9500 . ? C15 C16 1.393(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.371(3) . ? C18 C25 1.507(3) . ? C18 H18 0.9500 . ? C19 C20 1.515(3) . ? C19 H19 0.9500 . ? C20 C21 1.525(3) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.524(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.401(3) . ? C22 H22 0.9500 . ? C23 C24 1.503(3) . ? C23 H23 0.9500 . ? C24 C25 1.533(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? 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 C23 93.09(7) . . ? C1 Rh1 C22 93.46(7) . . ? C23 Rh1 C22 38.49(7) . . ? C1 Rh1 C19 156.53(7) . . ? C23 Rh1 C19 97.09(7) . . ? C22 Rh1 C19 81.76(7) . . ? C1 Rh1 C18 167.69(7) . . ? C23 Rh1 C18 81.20(7) . . ? C22 Rh1 C18 88.82(7) . . ? C19 Rh1 C18 35.77(7) . . ? C1 Rh1 Cl1 88.03(4) . . ? C23 Rh1 Cl1 156.37(6) . . ? C22 Rh1 Cl1 165.02(5) . . ? C19 Rh1 Cl1 90.95(5) . . ? C18 Rh1 Cl1 92.88(5) . . ? C1 N1 C9 123.60(16) . . ? C1 N1 C10 119.55(13) . . ? C9 N1 C10 116.75(14) . . ? N1 C1 C2 115.61(15) . . ? N1 C1 Rh1 122.83(12) . . ? C2 C1 Rh1 121.49(13) . . ? C7 C2 C3 118.52(17) . . ? C7 C2 C1 121.58(17) . . ? C3 C2 C1 119.90(16) . . ? C4 C3 C2 120.67(19) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 119.7(2) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.1 . . ? C6 C5 C4 121.3(2) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 119.78(18) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 119.99(18) . . ? C6 C7 C8 121.99(17) . . ? C2 C7 C8 118.02(17) . . ? C9 C8 C7 119.55(16) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.3 . . ? C8 C9 N1 121.62(16) . . ? C8 C9 H9 119.4 . . ? N1 C9 H9 119.0 . . ? N1 C10 C11 110.95(15) . . ? N1 C10 C17 109.33(16) . . ? C11 C10 C17 115.07(15) . . ? N1 C10 H10 107.0 . . ? C11 C10 H10 107.1 . . ? C17 C10 H10 107.0 . . ? C16 C11 C12 118.77(18) . . ? C16 C11 C10 121.70(17) . . ? C12 C11 C10 119.46(17) . . ? C13 C12 C11 120.0(2) . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 121.1(2) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.4 . . ? C13 C14 C15 119.5(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 120.2(2) . . ? C14 C15 H15 119.7 . . ? C16 C15 H15 120.1 . . ? C11 C16 C15 120.5(2) . . ? C11 C16 H16 119.7 . . ? C15 C16 H16 119.9 . . ? C10 C17 H17A 109.5 . . ? C10 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C10 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C25 123.77(18) . . ? C19 C18 Rh1 70.70(10) . . ? C25 C18 Rh1 110.16(12) . . ? C19 C18 H18 118.1 . . ? C25 C18 H18 118.1 . . ? Rh1 C18 H18 89.2 . . ? C18 C19 C20 126.63(18) . . ? C18 C19 Rh1 73.53(11) . . ? C20 C19 Rh1 106.36(12) . . ? C18 C19 H19 116.9 . . ? C20 C19 H19 116.5 . . ? Rh1 C19 H19 90.5 . . ? C19 C20 C21 113.21(15) . . ? C19 C20 H20A 109.2 . . ? C21 C20 H20A 108.9 . . ? C19 C20 H20B 108.9 . . ? C21 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C22 C21 C20 112.63(14) . . ? C22 C21 H21A 109.1 . . ? C20 C21 H21A 109.2 . . ? C22 C21 H21B 109.0 . . ? C20 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C23 C22 C21 123.59(18) . . ? C23 C22 Rh1 70.11(9) . . ? C21 C22 Rh1 112.72(12) . . ? C23 C22 H22 118.3 . . ? C21 C22 H22 118.1 . . ? Rh1 C22 H22 87.5 . . ? C22 C23 C24 125.74(17) . . ? C22 C23 Rh1 71.40(10) . . ? C24 C23 Rh1 110.18(12) . . ? C22 C23 H23 117.1 . . ? C24 C23 H23 117.2 . . ? Rh1 C23 H23 87.8 . . ? C23 C24 C25 113.54(15) . . ? C23 C24 H24A 109.0 . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24B 108.6 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C18 C25 C24 112.71(16) . . ? C18 C25 H25A 108.8 . . ? C24 C25 H25A 109.0 . . ? C18 C25 H25B 109.3 . . ? C24 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C9 N1 C1 C2 1.3(2) . . . . ? C10 N1 C1 C2 177.57(15) . . . . ? C9 N1 C1 Rh1 -175.68(13) . . . . ? C10 N1 C1 Rh1 0.6(2) . . . . ? C23 Rh1 C1 N1 -72.12(14) . . . . ? C22 Rh1 C1 N1 -110.67(13) . . . . ? C19 Rh1 C1 N1 172.11(15) . . . . ? C18 Rh1 C1 N1 -10.3(4) . . . . ? Cl1 Rh1 C1 N1 84.25(13) . . . . ? C23 Rh1 C1 C2 111.12(13) . . . . ? C22 Rh1 C1 C2 72.57(13) . . . . ? C19 Rh1 C1 C2 -4.6(2) . . . . ? C18 Rh1 C1 C2 173.0(3) . . . . ? Cl1 Rh1 C1 C2 -92.51(12) . . . . ? N1 C1 C2 C7 -0.3(2) . . . . ? Rh1 C1 C2 C7 176.68(13) . . . . ? N1 C1 C2 C3 -179.76(16) . . . . ? Rh1 C1 C2 C3 -2.8(2) . . . . ? C7 C2 C3 C4 0.1(3) . . . . ? C1 C2 C3 C4 179.62(16) . . . . ? C2 C3 C4 C5 0.2(3) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? C4 C5 C6 C7 -0.7(3) . . . . ? C5 C6 C7 C2 1.0(3) . . . . ? C5 C6 C7 C8 -178.53(18) . . . . ? C3 C2 C7 C6 -0.7(3) . . . . ? C1 C2 C7 C6 179.82(16) . . . . ? C3 C2 C7 C8 178.81(16) . . . . ? C1 C2 C7 C8 -0.7(2) . . . . ? C6 C7 C8 C9 -179.78(18) . . . . ? C2 C7 C8 C9 0.7(2) . . . . ? C7 C8 C9 N1 0.2(3) . . . . ? C1 N1 C9 C8 -1.3(3) . . . . ? C10 N1 C9 C8 -177.67(16) . . . . ? C1 N1 C10 C11 124.11(15) . . . . ? C9 N1 C10 C11 -59.3(2) . . . . ? C1 N1 C10 C17 -107.93(18) . . . . ? C9 N1 C10 C17 68.6(2) . . . . ? N1 C10 C11 C16 -27.4(2) . . . . ? C17 C10 C11 C16 -152.18(18) . . . . ? N1 C10 C11 C12 155.68(16) . . . . ? C17 C10 C11 C12 30.9(2) . . . . ? C16 C11 C12 C13 0.2(3) . . . . ? C10 C11 C12 C13 177.25(17) . . . . ? C11 C12 C13 C14 0.1(3) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C13 C14 C15 C16 -0.5(3) . . . . ? C12 C11 C16 C15 -0.7(3) . . . . ? C10 C11 C16 C15 -177.63(17) . . . . ? C14 C15 C16 C11 0.8(3) . . . . ? C1 Rh1 C18 C19 -178.4(4) . . . . ? C23 Rh1 C18 C19 -115.39(13) . . . . ? C22 Rh1 C18 C19 -77.49(12) . . . . ? Cl1 Rh1 C18 C19 87.63(12) . . . . ? C1 Rh1 C18 C25 -58.4(3) . . . . ? C23 Rh1 C18 C25 4.54(13) . . . . ? C22 Rh1 C18 C25 42.44(14) . . . . ? C19 Rh1 C18 C25 119.9(2) . . . . ? Cl1 Rh1 C18 C25 -152.45(13) . . . . ? C25 C18 C19 C20 -3.4(3) . . . . ? Rh1 C18 C19 C20 98.41(18) . . . . ? C25 C18 C19 Rh1 -101.83(17) . . . . ? C1 Rh1 C19 C18 179.13(14) . . . . ? C23 Rh1 C19 C18 64.11(13) . . . . ? C22 Rh1 C19 C18 99.52(13) . . . . ? Cl1 Rh1 C19 C18 -93.61(12) . . . . ? C1 Rh1 C19 C20 55.0(2) . . . . ? C23 Rh1 C19 C20 -60.06(13) . . . . ? C22 Rh1 C19 C20 -24.65(13) . . . . ? C18 Rh1 C19 C20 -124.17(18) . . . . ? Cl1 Rh1 C19 C20 142.21(12) . . . . ? C18 C19 C20 C21 -41.8(3) . . . . ? Rh1 C19 C20 C21 39.60(19) . . . . ? C19 C20 C21 C22 -36.3(2) . . . . ? C20 C21 C22 C23 93.8(2) . . . . ? C20 C21 C22 Rh1 13.3(2) . . . . ? C1 Rh1 C22 C23 90.61(12) . . . . ? C19 Rh1 C22 C23 -112.50(12) . . . . ? C18 Rh1 C22 C23 -77.29(12) . . . . ? Cl1 Rh1 C22 C23 -174.05(16) . . . . ? C1 Rh1 C22 C21 -150.30(14) . . . . ? C23 Rh1 C22 C21 119.10(19) . . . . ? C19 Rh1 C22 C21 6.60(14) . . . . ? C18 Rh1 C22 C21 41.81(14) . . . . ? Cl1 Rh1 C22 C21 -55.0(3) . . . . ? C21 C22 C23 C24 -2.7(3) . . . . ? Rh1 C22 C23 C24 101.91(16) . . . . ? C21 C22 C23 Rh1 -104.65(16) . . . . ? C1 Rh1 C23 C22 -91.68(12) . . . . ? C19 Rh1 C23 C22 67.13(12) . . . . ? C18 Rh1 C23 C22 99.28(12) . . . . ? Cl1 Rh1 C23 C22 176.17(10) . . . . ? C1 Rh1 C23 C24 146.11(13) . . . . ? C22 Rh1 C23 C24 -122.20(18) . . . . ? C19 Rh1 C23 C24 -55.07(14) . . . . ? C18 Rh1 C23 C24 -22.92(13) . . . . ? Cl1 Rh1 C23 C24 54.0(2) . . . . ? C22 C23 C24 C25 -42.5(2) . . . . ? Rh1 C23 C24 C25 38.68(19) . . . . ? C19 C18 C25 C24 94.4(2) . . . . ? Rh1 C18 C25 C24 14.6(2) . . . . ? C23 C24 C25 C18 -35.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.408 _refine_diff_density_min -0.381 _refine_diff_density_rms 0.049 ###END