# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Guy Lavigne' _publ_contact_author_email LAVIGNE@LCC-TOULOUSE.FR _publ_section_title ; Imidazol-2-ylidene-4-olate: an anionic N-heterocyclic carbene pre-programmed for further derivatization ; loop_ _publ_author_name 'Guy Lavigne' 'Laure Benhamou' 'Vincent Cesar' 'Heinz Gornitzka' 'Noel Lugan' # Attachment 'B907908D.cif' #\#CIF_1.1 data_3a _database_code_depnum_ccdc_archive 'CCDC 728893' _audit_creation_date 2009-02-26T17:23:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C21 H25 Cl N2 O' _chemical_formula_moiety 'C21 H25 N2 O, Cl' _chemical_formula_weight 356.88 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 _cell_measurement_temperature 180(2) _cell_measurement_theta_min 1.37 _cell_measurement_reflns_used 9999 _cell_measurement_theta_max 38.28 _cell_measurement_wavelength 0.71073 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.5416(3) _cell_length_b 29.645(1) _cell_length_c 8.7375(3) _cell_angle_alpha 90 _cell_angle_beta 118.109(2) _cell_angle_gamma 90 _cell_volume 1951.52(12) _cell_formula_units_Z 4 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.215 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.206 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; 'SADABS, Sheldrick, Bruker, 2000' ; _exptl_absorpt_correction_T_min 0.92 _exptl_absorpt_correction_T_max 0.94 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Bruker APEX II' _diffrn_measurement_method 'phi and omega scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 32567 _diffrn_reflns_av_R_equivalents 0.0198 _diffrn_reflns_av_sigmaI/netI 0.0175 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 38 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 29.83 _reflns_number_total 5587 _reflns_number_gt 4769 _reflns_threshold_expression >2sigma(I) _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.83 _diffrn_measured_fraction_theta_full 0.997 #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0520P)^2^+1.2293P] 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 5592 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0680 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1464 _refine_ls_wR_factor_gt 0.1414 _refine_ls_goodness_of_fit_ref 1.133 _refine_ls_restrained_S_all 1.133 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0. _refine_diff_density_min -0.221 _refine_diff_density_rms 0.049 _refine_diff_density_max 0.301 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 C1 C 0.3763(2) 0.12515(6) 0.7305(2) 0.0300(3) Uani 1 1 d . A 4 H1 H 0.4831 0.1259 0.8331 0.036 Uiso 1 1 calc R A 4 C2 C 0.1012(2) 0.10836(6) 0.5338(2) 0.0300(3) Uani 1 1 d . A 4 H2 H -0.0111 0.0953 0.4807 0.036 Uiso 0.50 1 calc PR A 4 C3 C 0.1671(2) 0.13856(6) 0.4617(2) 0.0294(3) Uani 1 1 d . A 4 H3 H 0.1081 0.1504 0.3501 0.035 Uiso 0.50 1 calc PR A 4 C11 C 0.2209(2) 0.07296(6) 0.8317(2) 0.0277(3) Uani 1 1 d . A 4 C12 C 0.1734(3) 0.09366(6) 0.9464(2) 0.0385(4) Uani 1 1 d . A 4 C13 C 0.1699(3) 0.06684(8) 1.0750(2) 0.0429(4) Uani 1 1 d . A 4 H13 H 0.1370 0.0797 1.1527 0.051 Uiso 1 1 calc R A 4 C14 C 0.2139(2) 0.02162(7) 1.0910(2) 0.0380(4) Uani 1 1 d . A 4 C15 C 0.2552(2) 0.00200(6) 0.9703(2) 0.0356(4) Uani 1 1 d . A 4 H15 H 0.2815 -0.0286 0.9784 0.043 Uiso 1 1 calc R A 4 C16 C 0.2581(2) 0.02725(6) 0.8372(2) 0.0296(3) Uani 1 1 d . A 4 C17 C 0.1282(5) 0.14296(8) 0.9335(4) 0.0734(9) Uani 1 1 d . A 4 H17A H 0.2315 0.1605 0.9564 0.110 Uiso 1 1 calc R A 4 H17B H 0.0890 0.1503 1.0170 0.110 Uiso 1 1 calc R A 4 H17C H 0.0354 0.1496 0.8189 0.110 Uiso 1 1 calc R A 4 C18 C 0.2191(3) -0.00603(9) 1.2387(3) 0.0561(6) Uani 1 1 d . A 4 H18A H 0.3329 -0.0026 1.3391 0.084 Uiso 1 1 calc R A 4 H18B H 0.2000 -0.0372 1.2056 0.084 Uiso 1 1 calc R A 4 H18C H 0.1279 0.0042 1.2651 0.084 Uiso 1 1 calc R A 4 C19 C 0.2978(3) 0.00523(7) 0.7044(3) 0.0443(5) Uani 1 1 d . A 4 H19A H 0.1904 0.0028 0.5964 0.066 Uiso 1 1 calc R A 4 H19B H 0.3461 -0.0243 0.7439 0.066 Uiso 1 1 calc R A 4 H19C H 0.3824 0.0232 0.6881 0.066 Uiso 1 1 calc R A 4 C21 C 0.4642(2) 0.17729(5) 0.5662(2) 0.0277(3) Uani 1 1 d . A 4 C22 C 0.5796(2) 0.15789(6) 0.5139(2) 0.0330(4) Uani 1 1 d . A 4 C23 C 0.7042(2) 0.18623(6) 0.5033(3) 0.0362(4) Uani 1 1 d . A 4 H23 H 0.7836 0.1742 0.4693 0.043 Uiso 1 1 calc R A 4 C24 C 0.7134(2) 0.23193(6) 0.5418(2) 0.0346(4) Uani 1 1 d . A 4 C25 C 0.5916(2) 0.24992(6) 0.5885(2) 0.0343(4) Uani 1 1 d . A 4 H25 H 0.5957 0.2806 0.6126 0.041 Uiso 1 1 calc R A 4 C26 C 0.4641(2) 0.22320(6) 0.6002(2) 0.0297(3) Uani 1 1 d . A 4 C27 C 0.5739(3) 0.10863(7) 0.4705(4) 0.0513(5) Uani 1 1 d . A 4 H27A H 0.6818 0.0944 0.5528 0.077 Uiso 1 1 calc R A 4 H27B H 0.5614 0.1054 0.3559 0.077 Uiso 1 1 calc R A 4 H27C H 0.4748 0.0947 0.4750 0.077 Uiso 1 1 calc R A 4 C28 C 0.8546(3) 0.26106(8) 0.5355(3) 0.0497(5) Uani 1 1 d . A 4 H28A H 0.9551 0.2627 0.6491 0.075 Uiso 1 1 calc R A 4 H28B H 0.8082 0.2908 0.4972 0.075 Uiso 1 1 calc R A 4 H28C H 0.8905 0.2482 0.4561 0.075 Uiso 1 1 calc R A 4 C29 C 0.3271(3) 0.24351(7) 0.6421(3) 0.0413(4) Uani 1 1 d . A 4 H29A H 0.3646 0.2731 0.6899 0.062 Uiso 1 1 calc R A 4 H29B H 0.3139 0.2248 0.7250 0.062 Uiso 1 1 calc R A 4 H29C H 0.2156 0.2455 0.5381 0.062 Uiso 1 1 calc R A 4 N1 N 0.23389(18) 0.10070(5) 0.70196(17) 0.0286(3) Uani 1 1 d . A 4 N2 N 0.33898(17) 0.14834(5) 0.58645(17) 0.0281(3) Uani 1 1 d . A 4 Cl1 Cl -0.25794(6) 0.121947(16) 0.12556(6) 0.04400(14) Uani 1 1 d . B 4 O1A O -0.0433(3) 0.08635(9) 0.4689(3) 0.0402(6) Uani 0.50 1 d P C 2 O1B O 0.0956(3) 0.15871(8) 0.3151(3) 0.0290(5) Uani 0.50 1 d P D 1 H1A H -0.1117 0.0974 0.3614 0.050 Uiso 0.50 1 d P E 2 H1B H -0.0115 0.1474 0.2552 0.050 Uiso 0.50 1 d P F 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0238(7) 0.0372(8) 0.0211(7) 0.0031(6) 0.0041(6) -0.0026(6) C2 0.0249(7) 0.0327(8) 0.0223(7) 0.0012(6) 0.0028(6) -0.0026(6) C3 0.0238(7) 0.0326(8) 0.0214(7) 0.0030(6) 0.0021(6) -0.0004(6) C11 0.0270(7) 0.0337(8) 0.0199(7) 0.0023(6) 0.0089(6) -0.0026(6) C12 0.0474(10) 0.0378(9) 0.0284(8) -0.0046(7) 0.0164(8) 0.0008(8) C13 0.0481(11) 0.0591(12) 0.0253(8) -0.0055(8) 0.0204(8) -0.0021(9) C14 0.0337(9) 0.0538(11) 0.0217(8) 0.0059(7) 0.0091(7) -0.0077(8) C15 0.0365(9) 0.0356(9) 0.0301(8) 0.0065(7) 0.0118(7) -0.0013(7) C16 0.0270(7) 0.0351(8) 0.0242(7) 0.0015(6) 0.0100(6) 0.0009(6) C17 0.124(3) 0.0450(13) 0.0610(16) -0.0053(11) 0.0519(17) 0.0167(15) C18 0.0515(12) 0.0822(17) 0.0315(10) 0.0157(10) 0.0168(9) -0.0127(11) C19 0.0525(11) 0.0479(11) 0.0367(10) 0.0027(8) 0.0244(9) 0.0124(9) C21 0.0228(7) 0.0316(8) 0.0247(7) 0.0037(6) 0.0080(6) -0.0016(6) C22 0.0290(8) 0.0301(8) 0.0368(9) 0.0028(7) 0.0130(7) 0.0033(6) C23 0.0286(8) 0.0391(9) 0.0439(10) 0.0008(8) 0.0196(7) 0.0035(7) C24 0.0259(7) 0.0378(9) 0.0381(9) -0.0011(7) 0.0134(7) -0.0035(6) C25 0.0323(8) 0.0313(8) 0.0382(9) -0.0046(7) 0.0158(7) -0.0038(6) C26 0.0257(7) 0.0343(8) 0.0276(8) -0.0015(6) 0.0114(6) 0.0008(6) C27 0.0544(12) 0.0315(9) 0.0755(16) -0.0012(10) 0.0368(12) 0.0033(8) C28 0.0370(10) 0.0506(12) 0.0680(14) -0.0084(10) 0.0301(10) -0.0129(9) C29 0.0372(9) 0.0449(10) 0.0477(11) -0.0080(8) 0.0248(9) -0.0007(8) N1 0.0258(6) 0.0333(7) 0.0214(6) 0.0027(5) 0.0069(5) -0.0024(5) N2 0.0228(6) 0.0332(7) 0.0218(6) 0.0036(5) 0.0053(5) -0.0018(5) Cl1 0.0356(2) 0.0433(3) 0.0310(2) 0.00429(18) -0.00244(17) -0.00414(18) O1A 0.0279(12) 0.0503(15) 0.0324(13) 0.0089(11) 0.0061(10) -0.0085(11) O1B 0.0232(10) 0.0380(12) 0.0172(10) 0.0109(9) 0.0025(8) -0.0035(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N2 1.334(2) . ? C1 N1 1.335(2) . ? C1 H1 0.9300 . ? C2 C3 1.360(2) . ? C2 N1 1.3876(19) . ? C2 O1A 1.269(3) . ? C2 H2 0.9300 . ? C3 N2 1.3856(19) . ? C3 O1B 1.278(3) . ? C3 H3 0.9300 . ? C11 C16 1.387(2) . ? C11 C12 1.389(2) . ? C11 N1 1.446(2) . ? C12 C13 1.388(3) . ? C12 C17 1.502(3) . ? C13 C14 1.381(3) . ? C13 H13 0.9300 . ? C14 C15 1.388(3) . ? C14 C18 1.511(3) . ? C15 C16 1.393(2) . ? C15 H15 0.9300 . ? C16 C19 1.503(2) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C21 C22 1.391(2) . ? C21 C26 1.393(2) . ? C21 N2 1.446(2) . ? C22 C23 1.393(2) . ? C22 C27 1.504(3) . ? C23 C24 1.390(3) . ? C23 H23 0.9300 . ? C24 C25 1.390(3) . ? C24 C28 1.505(3) . ? C25 C26 1.389(2) . ? C25 H25 0.9300 . ? C26 C29 1.506(2) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O1A H1A 0.902(2) . ? O1B H1B 0.879(2) . ? 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 N2 C1 N1 108.16(13) . . ? N2 C1 H1 125.9 . . ? N1 C1 H1 125.9 . . ? C3 C2 N1 106.76(14) . . ? C3 C2 O1A 131.23(18) . . ? C3 C2 H2 126.6 . . ? N1 C2 H2 126.6 . . ? C2 C3 N2 106.85(13) . . ? C2 C3 O1B 131.7(2) . . ? C2 C3 H3 126.6 . . ? N2 C3 H3 126.6 . . ? C16 C11 C12 123.13(15) . . ? C16 C11 N1 118.78(14) . . ? C12 C11 N1 118.09(15) . . ? C13 C12 C11 117.13(17) . . ? C13 C12 C17 121.02(19) . . ? C11 C12 C17 121.85(18) . . ? C14 C13 C12 121.97(17) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 118.94(16) . . ? C13 C14 C18 120.69(19) . . ? C15 C14 C18 120.4(2) . . ? C14 C15 C16 121.36(17) . . ? C14 C15 H15 119.3 . . ? C16 C15 H15 119.3 . . ? C11 C16 C15 117.36(16) . . ? C11 C16 C19 121.94(15) . . ? C15 C16 C19 120.69(16) . . ? C22 C21 C26 123.06(15) . . ? C22 C21 N2 118.32(15) . . ? C26 C21 N2 118.62(14) . . ? C21 C22 C23 117.03(16) . . ? C21 C22 C27 122.71(16) . . ? C23 C22 C27 120.26(17) . . ? C24 C23 C22 121.97(16) . . ? C24 C23 H23 119.0 . . ? C22 C23 H23 119.0 . . ? C23 C24 C25 118.74(16) . . ? C23 C24 C28 120.32(17) . . ? C25 C24 C28 120.94(17) . . ? C26 C25 C24 121.58(16) . . ? C26 C25 H25 119.2 . . ? C24 C25 H25 119.2 . . ? C25 C26 C21 117.54(15) . . ? C25 C26 C29 121.04(16) . . ? C21 C26 C29 121.38(15) . . ? C1 N1 C2 109.08(13) . . ? C1 N1 C11 124.18(13) . . ? C2 N1 C11 126.66(13) . . ? C1 N2 C3 109.14(13) . . ? C1 N2 C21 124.03(13) . . ? C3 N2 C21 126.78(13) . . ? #===END data_4a _database_code_depnum_ccdc_archive 'CCDC 728894' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C69 H78 N6 O3' _chemical_formula_moiety '3(C21 H24 N2 O), C6 H6' _chemical_formula_weight 1039.37 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' _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 14.6090(8) _cell_length_b 15.3434(10) _cell_length_c 15.8721(8) _cell_angle_alpha 111.925(3) _cell_angle_beta 98.312(3) _cell_angle_gamma 108.340(3) _cell_volume 2990.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5684 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.154 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1116 _exptl_absorpt_coefficient_mu 0.071 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21995 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0538 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 5.10 _diffrn_reflns_theta_max 23.26 _reflns_number_total 8489 _reflns_number_gt 6026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+0.8297P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8489 _refine_ls_number_parameters 799 _refine_ls_number_restraints 318 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1265 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group N1 N 0.85103(13) 0.78810(14) 0.45271(12) 0.0309(5) Uani 1 1 d . . . N2 N 0.70540(14) 0.76794(15) 0.47522(12) 0.0347(5) Uani 1 1 d . . . O1 O 0.80630(12) 0.64774(12) 0.30279(11) 0.0437(4) Uani 1 1 d . . . C1 C 0.80338(18) 0.82582(19) 0.51341(16) 0.0330(6) Uani 1 1 d . . . H1 H 0.8350(18) 0.8834(19) 0.5756(18) 0.048(7) Uiso 1 1 d . . . C2 C 0.77936(17) 0.69839(18) 0.36963(15) 0.0348(6) Uani 1 1 d . . . C3 C 0.6879(2) 0.68920(19) 0.38653(16) 0.0380(6) Uani 1 1 d . . . H3 H 0.6213(19) 0.6429(18) 0.3504(16) 0.041(7) Uiso 1 1 d . . . C4 C 0.95799(16) 0.82717(17) 0.46793(15) 0.0313(5) Uani 1 1 d . . . C5 C 0.99635(17) 0.87441(17) 0.41370(15) 0.0313(5) Uani 1 1 d . . . C6 C 1.09923(18) 0.90348(18) 0.42324(16) 0.0380(6) Uani 1 1 d . . . H6 H 1.1272 0.9353 0.3864 0.046 Uiso 1 1 calc R . . C7 C 1.16163(18) 0.88745(19) 0.48458(16) 0.0418(6) Uani 1 1 d . . . C8 C 1.12092(18) 0.8443(2) 0.54043(17) 0.0445(7) Uani 1 1 d . . . H8 H 1.1641 0.8360 0.5850 0.053 Uiso 1 1 calc R . . C9 C 1.01860(18) 0.81265(19) 0.53285(16) 0.0388(6) Uani 1 1 d . . . C10 C 0.93021(18) 0.89373(19) 0.34741(16) 0.0392(6) Uani 1 1 d . . . H10A H 0.8803 0.8281 0.2963 0.059 Uiso 1 1 calc R . . H10B H 0.9718 0.9328 0.3199 0.059 Uiso 1 1 calc R . . H10C H 0.8953 0.9330 0.3826 0.059 Uiso 1 1 calc R . . C11 C 1.27097(19) 0.9115(3) 0.48813(19) 0.0646(9) Uani 1 1 d . . . H11A H 1.3134 0.9493 0.5546 0.097 Uiso 1 1 calc R . . H11B H 1.2908 0.9533 0.4547 0.097 Uiso 1 1 calc R . . H11C H 1.2797 0.8474 0.4574 0.097 Uiso 1 1 calc R . . C12 C 0.9760(2) 0.7645(2) 0.59333(19) 0.0588(8) Uani 1 1 d . . . H12A H 1.0249 0.7437 0.6209 0.088 Uiso 1 1 calc R . . H12B H 0.9130 0.7041 0.5539 0.088 Uiso 1 1 calc R . . H12C H 0.9625 0.8143 0.6445 0.088 Uiso 1 1 calc R . . C13 C 0.63121(17) 0.78521(18) 0.52216(16) 0.0344(6) Uani 1 1 d . . . C14 C 0.63035(18) 0.76812(18) 0.60219(16) 0.0376(6) Uani 1 1 d . . . C15 C 0.56152(19) 0.7908(2) 0.64884(17) 0.0430(6) Uani 1 1 d . . . H15 H 0.5598 0.7805 0.7041 0.052 Uiso 1 1 calc R . . C16 C 0.49570(19) 0.8276(2) 0.61827(18) 0.0450(7) Uani 1 1 d . . . C17 C 0.49814(19) 0.8415(2) 0.53690(18) 0.0467(7) Uani 1 1 d . . . H17 H 0.4526 0.8663 0.5147 0.056 Uiso 1 1 calc R . . C18 C 0.56504(17) 0.82028(19) 0.48722(16) 0.0390(6) Uani 1 1 d . . . C19 C 0.7007(2) 0.7269(2) 0.63649(18) 0.0479(7) Uani 1 1 d . . . H19A H 0.7675 0.7828 0.6728 0.072 Uiso 1 1 calc R . . H19B H 0.7066 0.6739 0.5817 0.072 Uiso 1 1 calc R . . H19C H 0.6741 0.6971 0.6772 0.072 Uiso 1 1 calc R . . C20 C 0.4220(2) 0.8516(3) 0.6716(2) 0.0693(9) Uani 1 1 d . . . H20A H 0.4180 0.8204 0.7155 0.104 Uiso 1 1 calc R . . H20B H 0.3552 0.8238 0.6262 0.104 Uiso 1 1 calc R . . H20C H 0.4453 0.9261 0.7077 0.104 Uiso 1 1 calc R . . C21 C 0.5662(2) 0.8348(2) 0.39855(18) 0.0543(7) Uani 1 1 d . . . H21A H 0.6362 0.8691 0.4008 0.081 Uiso 1 1 calc R . . H21B H 0.5290 0.8770 0.3946 0.081 Uiso 1 1 calc R . . H21C H 0.5342 0.7678 0.3426 0.081 Uiso 1 1 calc R . . N3 N 0.16067(13) 0.91088(14) 0.14408(12) 0.0288(4) Uani 1 1 d . . . N4 N 0.21109(13) 0.98821(14) 0.06027(12) 0.0273(4) Uani 1 1 d . . . O2 O 0.12287(12) 1.03315(12) 0.25978(10) 0.0394(4) Uani 1 1 d . . . C22 C 0.19519(16) 0.90324(19) 0.06903(16) 0.0300(5) Uani 1 1 d . . . H22 H 0.2084(15) 0.8493(17) 0.0307(15) 0.031(6) Uiso 1 1 d . . . C23 C 0.15366(16) 1.00788(17) 0.18742(15) 0.0283(5) Uani 1 1 d . . . C24 C 0.18624(17) 1.05511(18) 0.13171(15) 0.0312(5) Uani 1 1 d . . . H24 H 0.1922(16) 1.1245(18) 0.1337(15) 0.037 Uiso 1 1 d . . . C25 C 0.13076(17) 0.83217(17) 0.17523(14) 0.0290(5) Uani 1 1 d . . . C26 C 0.20479(17) 0.81603(17) 0.22525(15) 0.0319(6) Uani 1 1 d . . . C27 C 0.17219(19) 0.74158(18) 0.25676(15) 0.0365(6) Uani 1 1 d . . . H27 H 0.2212 0.7270 0.2889 0.044 Uiso 1 1 calc R . . C28 C 0.07097(19) 0.68783(18) 0.24298(15) 0.0362(6) Uani 1 1 d . . . C29 C -0.00008(18) 0.70621(18) 0.19224(16) 0.0364(6) Uani 1 1 d . . . H29 H -0.0698 0.6693 0.1816 0.044 Uiso 1 1 calc R . . C30 C 0.02809(17) 0.77716(17) 0.15659(15) 0.0310(5) Uani 1 1 d . . . C31 C 0.31535(17) 0.8793(2) 0.24721(17) 0.0427(6) Uani 1 1 d . . . H31A H 0.3348 0.8604 0.1885 0.064 Uiso 1 1 calc R . . H31B H 0.3554 0.8664 0.2927 0.064 Uiso 1 1 calc R . . H31C H 0.3277 0.9522 0.2747 0.064 Uiso 1 1 calc R . . C32 C 0.0392(2) 0.6170(2) 0.28825(18) 0.0500(7) Uani 1 1 d . . . H32A H 0.0495 0.6576 0.3560 0.075 Uiso 1 1 calc R . . H32B H 0.0799 0.5761 0.2813 0.075 Uiso 1 1 calc R . . H32C H -0.0323 0.5712 0.2569 0.075 Uiso 1 1 calc R . . C33 C -0.05066(18) 0.7962(2) 0.10221(17) 0.0415(6) Uani 1 1 d . . . H33A H -0.0498 0.8634 0.1414 0.062 Uiso 1 1 calc R . . H33B H -0.1175 0.7427 0.0863 0.062 Uiso 1 1 calc R . . H33C H -0.0360 0.7949 0.0435 0.062 Uiso 1 1 calc R . . C34 C 0.24490(16) 1.00848(16) -0.01440(14) 0.0277(5) Uani 1 1 d . . . C35 C 0.17219(16) 0.99478(17) -0.09124(15) 0.0312(5) Uani 1 1 d . . . C36 C 0.20604(18) 1.01842(18) -0.16036(16) 0.0366(6) Uani 1 1 d . . . H36 H 0.1582 1.0101 -0.2132 0.044 Uiso 1 1 calc R . . C37 C 0.30759(19) 1.05387(17) -0.15480(16) 0.0364(6) Uani 1 1 d . . . C38 C 0.37658(17) 1.06354(17) -0.07862(16) 0.0341(6) Uani 1 1 d . . . H38 H 0.4460 1.0855 -0.0755 0.041 Uiso 1 1 calc R . . C39 C 0.34730(16) 1.04206(16) -0.00652(15) 0.0304(5) Uani 1 1 d . . . C40 C 0.06213(17) 0.9576(2) -0.09864(17) 0.0411(6) Uani 1 1 d . . . H40A H 0.0430 0.8988 -0.0841 0.062 Uiso 1 1 calc R . . H40B H 0.0224 0.9368 -0.1634 0.062 Uiso 1 1 calc R . . H40C H 0.0490 1.0129 -0.0533 0.062 Uiso 1 1 calc R . . C41 C 0.3419(2) 1.0836(2) -0.22913(18) 0.0527(7) Uani 1 1 d . . . H41A H 0.3022 1.0277 -0.2926 0.079 Uiso 1 1 calc R . . H41B H 0.4136 1.0965 -0.2200 0.079 Uiso 1 1 calc R . . H41C H 0.3324 1.1458 -0.2230 0.079 Uiso 1 1 calc R . . C42 C 0.42310(17) 1.05495(19) 0.07618(17) 0.0395(6) Uani 1 1 d . . . H42A H 0.4182 0.9874 0.0695 0.059 Uiso 1 1 calc R . . H42B H 0.4096 1.0911 0.1353 0.059 Uiso 1 1 calc R . . H42C H 0.4912 1.0948 0.0779 0.059 Uiso 1 1 calc R . . N5 N 0.27455(13) 0.64859(14) 0.90368(12) 0.0307(4) Uani 1 1 d . . . N6 N 0.39347(14) 0.59411(14) 0.89615(12) 0.0312(5) Uani 1 1 d . . . O3 O 0.35670(12) 0.81010(12) 1.03639(11) 0.0435(4) Uani 1 1 d . . . C43 C 0.29785(18) 0.57024(18) 0.85452(17) 0.0313(5) Uani 1 1 d . . . H43 H 0.2544(16) 0.5061(18) 0.7981(16) 0.033(6) Uiso 1 1 d . . . C44 C 0.36032(17) 0.72842(18) 0.98122(16) 0.0333(6) Uani 1 1 d . . . C45 C 0.43398(19) 0.69011(18) 0.97407(17) 0.0341(6) Uani 1 1 d . . . H45 H 0.5030(18) 0.7202(17) 1.0111(16) 0.038(7) Uiso 1 1 d . . . C46 C 0.17803(16) 0.65423(17) 0.88387(15) 0.0300(5) Uani 1 1 d . . . C47 C 0.10910(17) 0.61937(17) 0.92818(15) 0.0331(6) Uani 1 1 d . . . C48 C 0.01596(17) 0.62486(18) 0.90704(17) 0.0393(6) Uani 1 1 d . . . H48 H -0.0324 0.6015 0.9362 0.047 Uiso 1 1 calc R . . C49 C -0.00841(18) 0.66313(19) 0.84506(17) 0.0419(6) Uani 1 1 d . . . C50 C 0.06460(19) 0.7016(2) 0.80668(17) 0.0444(6) Uani 1 1 d . . . H50 H 0.0493 0.7306 0.7659 0.053 Uiso 1 1 calc R . . C51 C 0.15913(18) 0.69915(19) 0.82564(16) 0.0390(6) Uani 1 1 d . . . C52 C 0.13469(19) 0.5791(2) 0.99683(17) 0.0436(6) Uani 1 1 d . . . H52A H 0.2049 0.6211 1.0368 0.065 Uiso 1 1 calc R . . H52B H 0.1262 0.5079 0.9616 0.065 Uiso 1 1 calc R . . H52C H 0.0897 0.5819 1.0371 0.065 Uiso 1 1 calc R . . C53 C -0.11207(19) 0.6634(2) 0.8194(2) 0.0631(8) Uani 1 1 d . . . H53A H -0.1054 0.7287 0.8188 0.095 Uiso 1 1 calc R . . H53B H -0.1459 0.6547 0.8665 0.095 Uiso 1 1 calc R . . H53C H -0.1521 0.6069 0.7563 0.095 Uiso 1 1 calc R . . C54 C 0.2397(2) 0.7474(2) 0.7879(2) 0.0549(7) Uani 1 1 d . . . H54A H 0.2105 0.7685 0.7433 0.082 Uiso 1 1 calc R . . H54B H 0.2665 0.6975 0.7550 0.082 Uiso 1 1 calc R . . H54C H 0.2945 0.8075 0.8409 0.082 Uiso 1 1 calc R . . C55 C 0.45173(17) 0.53438(17) 0.86500(15) 0.0323(5) Uani 1 1 d . . . C56 C 0.53016(19) 0.5739(2) 0.83163(18) 0.0439(6) Uani 1 1 d . . . C57 C 0.59135(19) 0.5211(2) 0.80850(19) 0.0493(7) Uani 1 1 d . . . H57 H 0.6446 0.5465 0.7847 0.059 Uiso 1 1 calc R . . C58 C 0.57756(19) 0.4335(2) 0.81879(17) 0.0450(7) Uani 1 1 d . . . C59 C 0.49736(19) 0.39536(19) 0.84973(16) 0.0423(6) Uani 1 1 d . . . H59 H 0.4858 0.3332 0.8547 0.051 Uiso 1 1 calc R . . C60 C 0.43238(17) 0.44466(18) 0.87405(15) 0.0339(6) Uani 1 1 d . . . C61 C 0.5487(3) 0.6699(2) 0.8189(3) 0.0720(10) Uani 1 1 d . . . H61A H 0.4838 0.6709 0.7938 0.108 Uiso 1 1 calc R . . H61B H 0.5883 0.6710 0.7742 0.108 Uiso 1 1 calc R . . H61C H 0.5860 0.7302 0.8804 0.108 Uiso 1 1 calc R . . C62 C 0.6490(2) 0.3811(3) 0.7979(2) 0.0722(9) Uani 1 1 d . . . H62A H 0.7187 0.4312 0.8327 0.108 Uiso 1 1 calc R . . H62B H 0.6410 0.3518 0.7294 0.108 Uiso 1 1 calc R . . H62C H 0.6339 0.3262 0.8178 0.108 Uiso 1 1 calc R . . C63 C 0.34575(19) 0.40020(19) 0.90716(18) 0.0461(7) Uani 1 1 d . . . H63A H 0.3409 0.4554 0.9606 0.069 Uiso 1 1 calc R . . H63B H 0.3571 0.3506 0.9276 0.069 Uiso 1 1 calc R . . H63C H 0.2828 0.3656 0.8548 0.069 Uiso 1 1 calc R . . C64 C 0.6558(11) 0.4291(8) 0.5271(7) 0.158(5) Uani 0.597(13) 1 d PDU A 1 H64 H 0.6010 0.4164 0.5529 0.189 Uiso 0.597(13) 1 calc PR A 1 C65 C 0.7423(14) 0.4198(14) 0.5581(11) 0.190(7) Uani 0.597(13) 1 d PDU A 1 H65 H 0.7473 0.3969 0.6058 0.228 Uiso 0.597(13) 1 calc PR A 1 C66 C 0.8221(13) 0.4420(14) 0.5235(12) 0.189(6) Uani 0.597(13) 1 d PDU A 1 H66 H 0.8826 0.4395 0.5519 0.227 Uiso 0.597(13) 1 calc PR A 1 C67 C 0.8188(13) 0.4677(12) 0.4494(11) 0.170(5) Uani 0.597(13) 1 d PDU A 1 H67 H 0.8728 0.4772 0.4221 0.204 Uiso 0.597(13) 1 calc PR A 1 C68 C 0.7314(14) 0.4791(16) 0.4163(13) 0.135(5) Uani 0.597(13) 1 d PDU A 1 H68 H 0.7260 0.5009 0.3677 0.162 Uiso 0.597(13) 1 calc PR A 1 C69 C 0.6540(12) 0.4588(7) 0.4541(6) 0.146(4) Uani 0.597(13) 1 d PDU A 1 H69 H 0.5947 0.4653 0.4291 0.175 Uiso 0.597(13) 1 calc PR A 1 C64' C 0.8859(16) 0.4717(16) 0.4475(13) 0.133(5) Uani 0.403(13) 1 d PDU A 2 H64' H 0.9512 0.4895 0.4392 0.160 Uiso 0.403(13) 1 calc PR A 2 C65' C 0.8178(15) 0.5013(11) 0.4091(10) 0.133(6) Uani 0.403(13) 1 d PDU A 2 H65' H 0.8315 0.5326 0.3682 0.159 Uiso 0.403(13) 1 calc PR A 2 C66' C 0.7281(19) 0.484(2) 0.433(2) 0.136(6) Uani 0.403(13) 1 d PDU A 2 H66' H 0.6813 0.5074 0.4108 0.163 Uiso 0.403(13) 1 calc PR A 2 C67' C 0.7058(15) 0.4327(14) 0.4864(14) 0.146(5) Uani 0.403(13) 1 d PDU A 2 H67' H 0.6440 0.4220 0.5018 0.176 Uiso 0.403(13) 1 calc PR A 2 C68' C 0.7707(14) 0.3970(14) 0.5183(14) 0.131(6) Uani 0.403(13) 1 d PDU A 2 H68' H 0.7542 0.3595 0.5540 0.157 Uiso 0.403(13) 1 calc PR A 2 C69' C 0.8604(15) 0.4167(15) 0.4975(14) 0.134(5) Uani 0.403(13) 1 d PDU A 2 H69' H 0.9063 0.3915 0.5184 0.161 Uiso 0.403(13) 1 calc PR A 2 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 N1 0.0318(11) 0.0350(11) 0.0231(10) 0.0105(9) 0.0096(9) 0.0127(9) N2 0.0331(12) 0.0406(12) 0.0269(10) 0.0117(9) 0.0117(9) 0.0132(10) O1 0.0438(10) 0.0431(10) 0.0323(9) 0.0048(8) 0.0149(8) 0.0158(8) C1 0.0399(16) 0.0360(14) 0.0215(12) 0.0106(11) 0.0101(11) 0.0155(13) C2 0.0394(14) 0.0343(14) 0.0274(13) 0.0107(11) 0.0113(11) 0.0138(12) C3 0.0339(15) 0.0400(15) 0.0276(13) 0.0074(12) 0.0085(12) 0.0091(13) C4 0.0334(13) 0.0320(13) 0.0231(12) 0.0072(10) 0.0073(10) 0.0132(11) C5 0.0373(14) 0.0310(13) 0.0238(12) 0.0075(10) 0.0112(10) 0.0163(11) C6 0.0441(15) 0.0345(14) 0.0303(13) 0.0086(11) 0.0182(12) 0.0135(12) C7 0.0349(14) 0.0476(16) 0.0289(13) 0.0038(12) 0.0067(11) 0.0169(12) C8 0.0403(16) 0.0546(17) 0.0316(14) 0.0127(13) 0.0022(12) 0.0221(13) C9 0.0437(15) 0.0446(15) 0.0281(13) 0.0155(12) 0.0090(11) 0.0193(12) C10 0.0487(15) 0.0433(15) 0.0344(13) 0.0195(12) 0.0181(12) 0.0239(13) C11 0.0364(16) 0.088(2) 0.0424(16) 0.0080(15) 0.0070(13) 0.0192(15) C12 0.0614(19) 0.077(2) 0.0470(16) 0.0420(16) 0.0107(14) 0.0236(16) C13 0.0343(13) 0.0378(14) 0.0308(13) 0.0137(11) 0.0145(11) 0.0137(11) C14 0.0396(14) 0.0410(15) 0.0338(13) 0.0157(12) 0.0157(11) 0.0171(12) C15 0.0486(16) 0.0543(17) 0.0371(14) 0.0258(13) 0.0234(13) 0.0230(14) C16 0.0412(15) 0.0583(18) 0.0429(15) 0.0241(14) 0.0212(12) 0.0233(14) C17 0.0412(15) 0.0627(19) 0.0455(15) 0.0277(14) 0.0151(13) 0.0269(14) C18 0.0357(14) 0.0462(16) 0.0348(14) 0.0194(12) 0.0118(11) 0.0139(12) C19 0.0613(18) 0.0610(18) 0.0418(15) 0.0310(14) 0.0271(13) 0.0346(15) C20 0.066(2) 0.108(3) 0.068(2) 0.049(2) 0.0407(17) 0.055(2) C21 0.0609(18) 0.072(2) 0.0388(15) 0.0303(15) 0.0157(14) 0.0306(16) N3 0.0325(10) 0.0337(11) 0.0299(10) 0.0172(9) 0.0159(9) 0.0187(9) N4 0.0297(10) 0.0312(11) 0.0279(10) 0.0150(9) 0.0130(8) 0.0163(9) O2 0.0496(10) 0.0432(10) 0.0321(9) 0.0157(8) 0.0217(8) 0.0237(8) C22 0.0343(13) 0.0321(14) 0.0299(13) 0.0135(11) 0.0151(11) 0.0190(11) C23 0.0288(12) 0.0321(13) 0.0270(12) 0.0114(10) 0.0114(10) 0.0167(11) C24 0.0375(14) 0.0327(14) 0.0314(13) 0.0154(11) 0.0174(11) 0.0196(11) C25 0.0384(14) 0.0307(13) 0.0257(12) 0.0146(10) 0.0156(10) 0.0183(11) C26 0.0390(14) 0.0372(14) 0.0272(12) 0.0141(11) 0.0159(11) 0.0223(12) C27 0.0493(16) 0.0397(15) 0.0304(13) 0.0157(12) 0.0131(12) 0.0296(13) C28 0.0533(17) 0.0309(14) 0.0291(13) 0.0120(11) 0.0191(12) 0.0212(13) C29 0.0402(14) 0.0335(14) 0.0335(13) 0.0127(11) 0.0169(12) 0.0126(12) C30 0.0358(14) 0.0346(14) 0.0257(12) 0.0124(11) 0.0140(10) 0.0170(11) C31 0.0381(15) 0.0524(17) 0.0440(15) 0.0236(13) 0.0118(12) 0.0235(13) C32 0.0731(19) 0.0388(16) 0.0459(15) 0.0237(13) 0.0230(14) 0.0239(14) C33 0.0377(14) 0.0498(16) 0.0418(14) 0.0233(13) 0.0139(12) 0.0192(13) C34 0.0335(13) 0.0294(13) 0.0268(12) 0.0135(10) 0.0160(10) 0.0165(11) C35 0.0342(13) 0.0345(14) 0.0326(13) 0.0173(11) 0.0156(11) 0.0181(11) C36 0.0454(15) 0.0408(15) 0.0301(13) 0.0183(11) 0.0134(11) 0.0214(12) C37 0.0506(16) 0.0323(14) 0.0347(14) 0.0174(11) 0.0245(12) 0.0190(12) C38 0.0352(14) 0.0272(13) 0.0418(14) 0.0140(11) 0.0209(12) 0.0123(11) C39 0.0331(13) 0.0271(13) 0.0308(12) 0.0096(10) 0.0125(11) 0.0145(11) C40 0.0358(14) 0.0549(17) 0.0409(14) 0.0247(13) 0.0125(12) 0.0239(13) C41 0.0721(19) 0.0492(17) 0.0444(15) 0.0261(13) 0.0332(15) 0.0204(15) C42 0.0317(13) 0.0408(15) 0.0442(15) 0.0176(12) 0.0095(11) 0.0145(12) N5 0.0292(11) 0.0292(11) 0.0331(10) 0.0100(9) 0.0126(9) 0.0145(9) N6 0.0341(12) 0.0291(11) 0.0346(11) 0.0130(9) 0.0149(9) 0.0174(9) O3 0.0401(10) 0.0321(10) 0.0477(10) 0.0039(8) 0.0154(8) 0.0177(8) C43 0.0322(14) 0.0312(14) 0.0312(13) 0.0118(12) 0.0130(12) 0.0147(12) C44 0.0310(13) 0.0320(14) 0.0347(13) 0.0127(12) 0.0129(11) 0.0113(11) C45 0.0297(14) 0.0306(14) 0.0370(14) 0.0101(11) 0.0106(12) 0.0118(12) C46 0.0297(13) 0.0297(13) 0.0289(12) 0.0093(10) 0.0109(10) 0.0135(11) C47 0.0339(14) 0.0284(13) 0.0332(13) 0.0109(11) 0.0124(11) 0.0101(11) C48 0.0317(14) 0.0391(15) 0.0416(14) 0.0123(12) 0.0158(12) 0.0121(12) C49 0.0342(14) 0.0455(16) 0.0424(15) 0.0139(13) 0.0090(12) 0.0197(12) C50 0.0473(16) 0.0562(17) 0.0401(15) 0.0245(13) 0.0139(13) 0.0293(14) C51 0.0442(15) 0.0422(15) 0.0349(13) 0.0176(12) 0.0166(12) 0.0201(12) C52 0.0462(15) 0.0461(16) 0.0470(15) 0.0266(13) 0.0210(13) 0.0185(13) C53 0.0371(16) 0.079(2) 0.068(2) 0.0286(17) 0.0083(14) 0.0266(15) C54 0.0604(18) 0.069(2) 0.0610(18) 0.0420(16) 0.0348(15) 0.0343(16) C55 0.0359(13) 0.0342(14) 0.0335(13) 0.0154(11) 0.0143(11) 0.0203(11) C56 0.0466(15) 0.0480(16) 0.0544(16) 0.0290(14) 0.0266(13) 0.0277(13) C57 0.0461(16) 0.0560(18) 0.0577(17) 0.0257(15) 0.0285(14) 0.0287(14) C58 0.0429(15) 0.0498(17) 0.0404(15) 0.0114(13) 0.0075(12) 0.0287(13) C59 0.0542(17) 0.0309(14) 0.0389(14) 0.0118(12) 0.0034(13) 0.0230(13) C60 0.0379(14) 0.0328(14) 0.0267(12) 0.0111(11) 0.0045(11) 0.0140(11) C61 0.086(2) 0.074(2) 0.113(3) 0.068(2) 0.073(2) 0.0502(19) C62 0.061(2) 0.075(2) 0.081(2) 0.0195(18) 0.0142(17) 0.0498(18) C63 0.0542(17) 0.0382(15) 0.0428(15) 0.0202(13) 0.0122(13) 0.0134(13) C64 0.204(11) 0.081(6) 0.096(7) 0.030(5) -0.007(6) -0.022(7) C65 0.229(13) 0.154(11) 0.116(11) 0.063(9) -0.010(9) 0.013(10) C66 0.217(13) 0.169(13) 0.141(11) 0.091(10) -0.011(9) 0.030(10) C67 0.220(11) 0.113(8) 0.122(8) 0.054(6) -0.005(10) 0.021(10) C68 0.229(11) 0.056(7) 0.065(6) 0.014(5) 0.003(6) 0.023(8) C69 0.228(11) 0.058(5) 0.076(5) 0.009(4) 0.006(6) 0.009(7) C64' 0.198(14) 0.116(10) 0.089(8) 0.053(7) 0.008(10) 0.073(12) C65' 0.222(13) 0.077(8) 0.072(8) 0.034(6) -0.021(9) 0.054(10) C66' 0.205(12) 0.057(10) 0.121(14) 0.030(9) -0.026(11) 0.069(10) C67' 0.174(11) 0.106(9) 0.139(12) 0.055(8) -0.008(9) 0.054(8) C68' 0.186(13) 0.084(9) 0.109(12) 0.058(9) -0.013(9) 0.045(9) C69' 0.206(13) 0.107(9) 0.106(10) 0.061(7) 0.009(9) 0.084(10) _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 N1 C1 1.334(3) . ? N1 C4 1.433(3) . ? N1 C2 1.438(3) . ? N2 C1 1.324(3) . ? N2 C3 1.392(3) . ? N2 C13 1.438(3) . ? O1 C2 1.258(3) . ? C2 C3 1.374(3) . ? C4 C9 1.388(3) . ? C4 C5 1.389(3) . ? C5 C6 1.394(3) . ? C5 C10 1.499(3) . ? C6 C7 1.379(3) . ? C7 C8 1.386(3) . ? C7 C11 1.509(3) . ? C8 C9 1.390(3) . ? C9 C12 1.506(3) . ? C13 C18 1.388(3) . ? C13 C14 1.391(3) . ? C14 C15 1.387(3) . ? C14 C19 1.502(3) . ? C15 C16 1.375(3) . ? C16 C17 1.389(3) . ? C16 C20 1.513(3) . ? C17 C18 1.384(3) . ? C18 C21 1.507(3) . ? N3 C22 1.339(3) . ? N3 C23 1.432(3) . ? N3 C25 1.439(3) . ? N4 C22 1.314(3) . ? N4 C24 1.398(3) . ? N4 C34 1.447(3) . ? O2 C23 1.264(2) . ? C23 C24 1.384(3) . ? C25 C26 1.389(3) . ? C25 C30 1.392(3) . ? C26 C27 1.391(3) . ? C26 C31 1.507(3) . ? C27 C28 1.385(3) . ? C28 C29 1.385(3) . ? C28 C32 1.508(3) . ? C29 C30 1.386(3) . ? C30 C33 1.506(3) . ? C34 C39 1.390(3) . ? C34 C35 1.398(3) . ? C35 C36 1.386(3) . ? C35 C40 1.498(3) . ? C36 C37 1.387(3) . ? C37 C38 1.386(3) . ? C37 C41 1.510(3) . ? C38 C39 1.391(3) . ? C39 C42 1.495(3) . ? N5 C43 1.343(3) . ? N5 C44 1.431(3) . ? N5 C46 1.437(3) . ? N6 C43 1.324(3) . ? N6 C45 1.389(3) . ? N6 C55 1.443(3) . ? O3 C44 1.255(3) . ? C44 C45 1.378(3) . ? C46 C51 1.388(3) . ? C46 C47 1.393(3) . ? C47 C48 1.390(3) . ? C47 C52 1.496(3) . ? C48 C49 1.379(3) . ? C49 C50 1.384(3) . ? C49 C53 1.512(3) . ? C50 C51 1.386(3) . ? C51 C54 1.510(3) . ? C55 C60 1.382(3) . ? C55 C56 1.393(3) . ? C56 C57 1.385(3) . ? C56 C61 1.506(4) . ? C57 C58 1.370(4) . ? C58 C59 1.381(3) . ? C58 C62 1.509(3) . ? C59 C60 1.401(3) . ? C60 C63 1.503(3) . ? C64 C65 1.359(11) . ? C64 C69 1.393(10) . ? C65 C66 1.360(11) . ? C66 C67 1.374(11) . ? C67 C68 1.398(12) . ? C68 C69 1.361(11) . ? C64' C69' 1.368(12) . ? C64' C65' 1.372(12) . ? C65' C66' 1.386(13) . ? C66' C67' 1.366(13) . ? C67' C68' 1.362(12) . ? C68' C69' 1.366(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 N1 C4 125.97(19) . . ? C1 N1 C2 110.00(18) . . ? C4 N1 C2 123.98(17) . . ? C1 N2 C3 109.73(19) . . ? C1 N2 C13 123.39(18) . . ? C3 N2 C13 126.87(19) . . ? N2 C1 N1 108.3(2) . . ? O1 C2 C3 134.3(2) . . ? O1 C2 N1 122.0(2) . . ? C3 C2 N1 103.70(19) . . ? C2 C3 N2 108.3(2) . . ? C9 C4 C5 122.6(2) . . ? C9 C4 N1 119.1(2) . . ? C5 C4 N1 118.3(2) . . ? C4 C5 C6 117.4(2) . . ? C4 C5 C10 121.6(2) . . ? C6 C5 C10 121.0(2) . . ? C7 C6 C5 121.9(2) . . ? C6 C7 C8 118.7(2) . . ? C6 C7 C11 121.2(2) . . ? C8 C7 C11 120.1(2) . . ? C7 C8 C9 121.7(2) . . ? C4 C9 C8 117.6(2) . . ? C4 C9 C12 121.7(2) . . ? C8 C9 C12 120.7(2) . . ? C18 C13 C14 122.7(2) . . ? C18 C13 N2 118.87(19) . . ? C14 C13 N2 118.4(2) . . ? C15 C14 C13 116.9(2) . . ? C15 C14 C19 121.6(2) . . ? C13 C14 C19 121.5(2) . . ? C16 C15 C14 122.6(2) . . ? C15 C16 C17 118.3(2) . . ? C15 C16 C20 120.8(2) . . ? C17 C16 C20 121.0(2) . . ? C18 C17 C16 121.9(2) . . ? C17 C18 C13 117.5(2) . . ? C17 C18 C21 121.3(2) . . ? C13 C18 C21 121.2(2) . . ? C22 N3 C23 110.16(18) . . ? C22 N3 C25 125.50(18) . . ? C23 N3 C25 124.29(16) . . ? C22 N4 C24 109.91(18) . . ? C22 N4 C34 125.43(18) . . ? C24 N4 C34 124.60(18) . . ? N4 C22 N3 108.4(2) . . ? O2 C23 C24 134.4(2) . . ? O2 C23 N3 122.03(19) . . ? C24 C23 N3 103.62(17) . . ? C23 C24 N4 107.9(2) . . ? C26 C25 C30 122.4(2) . . ? C26 C25 N3 119.13(19) . . ? C30 C25 N3 118.43(19) . . ? C25 C26 C27 117.0(2) . . ? C25 C26 C31 121.2(2) . . ? C27 C26 C31 121.8(2) . . ? C28 C27 C26 122.5(2) . . ? C29 C28 C27 118.3(2) . . ? C29 C28 C32 120.7(2) . . ? C27 C28 C32 120.8(2) . . ? C28 C29 C30 121.6(2) . . ? C29 C30 C25 118.1(2) . . ? C29 C30 C33 120.5(2) . . ? C25 C30 C33 121.3(2) . . ? C39 C34 C35 122.76(19) . . ? C39 C34 N4 119.35(19) . . ? C35 C34 N4 117.88(18) . . ? C36 C35 C34 117.3(2) . . ? C36 C35 C40 120.9(2) . . ? C34 C35 C40 121.82(19) . . ? C35 C36 C37 122.1(2) . . ? C38 C37 C36 118.5(2) . . ? C38 C37 C41 121.0(2) . . ? C36 C37 C41 120.4(2) . . ? C37 C38 C39 122.0(2) . . ? C34 C39 C38 117.3(2) . . ? C34 C39 C42 121.44(19) . . ? C38 C39 C42 121.3(2) . . ? C43 N5 C44 110.51(18) . . ? C43 N5 C46 126.26(19) . . ? C44 N5 C46 123.23(18) . . ? C43 N6 C45 110.01(19) . . ? C43 N6 C55 126.77(19) . . ? C45 N6 C55 123.15(19) . . ? N6 C43 N5 107.6(2) . . ? O3 C44 C45 134.8(2) . . ? O3 C44 N5 121.8(2) . . ? C45 C44 N5 103.4(2) . . ? C44 C45 N6 108.5(2) . . ? C51 C46 C47 122.5(2) . . ? C51 C46 N5 118.87(19) . . ? C47 C46 N5 118.5(2) . . ? C48 C47 C46 117.3(2) . . ? C48 C47 C52 121.3(2) . . ? C46 C47 C52 121.5(2) . . ? C49 C48 C47 122.1(2) . . ? C48 C49 C50 118.3(2) . . ? C48 C49 C53 121.1(2) . . ? C50 C49 C53 120.6(2) . . ? C49 C50 C51 122.3(2) . . ? C50 C51 C46 117.3(2) . . ? C50 C51 C54 121.3(2) . . ? C46 C51 C54 121.4(2) . . ? C60 C55 C56 122.5(2) . . ? C60 C55 N6 119.90(19) . . ? C56 C55 N6 117.5(2) . . ? C57 C56 C55 117.8(2) . . ? C57 C56 C61 119.9(2) . . ? C55 C56 C61 122.2(2) . . ? C58 C57 C56 122.1(2) . . ? C57 C58 C59 118.2(2) . . ? C57 C58 C62 120.7(3) . . ? C59 C58 C62 121.1(3) . . ? C58 C59 C60 122.6(2) . . ? C55 C60 C59 116.6(2) . . ? C55 C60 C63 122.5(2) . . ? C59 C60 C63 120.8(2) . . ? C65 C64 C69 114.4(11) . . ? C64 C65 C66 122.7(13) . . ? C65 C66 C67 122.6(13) . . ? C66 C67 C68 116.1(12) . . ? C69 C68 C67 119.5(11) . . ? C68 C69 C64 124.5(11) . . ? C69' C64' C65' 120.5(12) . . ? C64' C65' C66' 117.2(12) . . ? C67' C66' C65' 121.2(13) . . ? C68' C67' C66' 121.1(13) . . ? C67' C68' C69' 117.8(13) . . ? C68' C69' C64' 121.8(12) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.194 _refine_diff_density_min -0.185 _refine_diff_density_rms 0.036 _vrf_THETM01_4a ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575 RESPONSE: Poorly diffracting crystals forced us to use data with a resolution down to 0.9 Angstrom only. ; _vrf_PLAT023_4a ; PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6].. 23.26 Deg. RESPONSE: Poorly diffracting crystals forced us to use data with a resolution down to 0.9 Angstrom only. ; #===END data_7a _database_code_depnum_ccdc_archive 'CCDC 728895' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_sum 'C29 H36 Cl N2 O Rh' _chemical_formula_moiety 'C29 H36 Cl N2 O Rh' _chemical_formula_weight 566.96 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 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 12.5523(5) _cell_length_b 13.1214(4) _cell_length_c 17.4887(7) _cell_angle_alpha 73.019(2) _cell_angle_beta 89.9200(10) _cell_angle_gamma 77.013(2) _cell_volume 2678.02(17) _cell_formula_units_Z 4 _cell_measurement_temperature 176(2) _cell_measurement_reflns_used 7935 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 28.73 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.406 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.761 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 176(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17559 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 5.11 _diffrn_reflns_theta_max 24.71 _reflns_number_total 8754 _reflns_number_gt 7128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+1.8940P] 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 8754 _refine_ls_number_parameters 624 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0687 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _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 0.820718(19) 0.823215(19) 0.029660(13) 0.02623(8) Uani 1 1 d . . . Rh2 Rh 0.377253(18) 0.256691(18) 0.423388(13) 0.02440(7) Uani 1 1 d . . . Cl1 Cl 1.01423(6) 0.76117(7) 0.04702(5) 0.03697(19) Uani 1 1 d . . . Cl2 Cl 0.39237(7) 0.23871(7) 0.56236(5) 0.0388(2) Uani 1 1 d . . . N1 N 0.8019(2) 0.62476(19) 0.17135(14) 0.0268(6) Uani 1 1 d . . . N2 N 0.81841(19) 0.76568(19) 0.20793(14) 0.0259(5) Uani 1 1 d . . . N3 N 0.17769(19) 0.43776(19) 0.40964(14) 0.0258(6) Uani 1 1 d . . . N4 N 0.12915(19) 0.28244(18) 0.43375(14) 0.0255(5) Uani 1 1 d . . . O1 O 0.8147(2) 0.4918(2) 0.29353(14) 0.0542(7) Uani 1 1 d . . . O2 O 0.01283(18) 0.55878(18) 0.41196(14) 0.0428(6) Uani 1 1 d . . . C1 C 0.8088(2) 0.7328(2) 0.14332(17) 0.0248(6) Uani 1 1 d . . . C2 C 0.8111(3) 0.5847(3) 0.25471(18) 0.0323(7) Uani 1 1 d . . . C3 C 0.8197(3) 0.6801(2) 0.28325(17) 0.0311(7) Uani 1 1 d . . . H3A H 0.7567 0.7004 0.3143 0.037 Uiso 1 1 calc R . . H3B H 0.8886 0.6641 0.3165 0.037 Uiso 1 1 calc R . . C4 C 0.7733(2) 0.5610(2) 0.12256(17) 0.0274(7) Uani 1 1 d . . . C5 C 0.6638(3) 0.5596(3) 0.11365(19) 0.0339(7) Uani 1 1 d . . . C6 C 0.6358(3) 0.4993(3) 0.0668(2) 0.0427(9) Uani 1 1 d . . . H6 H 0.5613 0.4970 0.0605 0.051 Uiso 1 1 calc R . . C7 C 0.7151(3) 0.4418(3) 0.0289(2) 0.0416(9) Uani 1 1 d . . . C8 C 0.8233(3) 0.4419(3) 0.04231(19) 0.0338(7) Uani 1 1 d . . . H8 H 0.8778 0.4015 0.0178 0.041 Uiso 1 1 calc R . . C9 C 0.8553(2) 0.4987(2) 0.09012(17) 0.0281(7) Uani 1 1 d . . . C10 C 0.5770(3) 0.6171(3) 0.1569(2) 0.0441(9) Uani 1 1 d . . . H10A H 0.5901 0.5815 0.2148 0.066 Uiso 1 1 calc R . . H10B H 0.5045 0.6131 0.1391 0.066 Uiso 1 1 calc R . . H10C H 0.5803 0.6941 0.1448 0.066 Uiso 1 1 calc R . . C11 C 0.6836(3) 0.3769(4) -0.0224(3) 0.0658(13) Uani 1 1 d . . . H11A H 0.6545 0.4266 -0.0754 0.099 Uiso 1 1 calc R . . H11B H 0.6276 0.3394 0.0031 0.099 Uiso 1 1 calc R . . H11C H 0.7484 0.3225 -0.0280 0.099 Uiso 1 1 calc R . . C12 C 0.9745(3) 0.4877(3) 0.1098(2) 0.0363(8) Uani 1 1 d . . . H12A H 0.9909 0.5603 0.0929 0.054 Uiso 1 1 calc R . . H12B H 1.0192 0.4406 0.0816 0.054 Uiso 1 1 calc R . . H12C H 0.9913 0.4550 0.1677 0.054 Uiso 1 1 calc R . . C13 C 0.8172(2) 0.8767(2) 0.20552(16) 0.0240(6) Uani 1 1 d . . . C14 C 0.7157(2) 0.9483(2) 0.20343(16) 0.0251(6) Uani 1 1 d . . . C15 C 0.7139(3) 1.0564(2) 0.19767(18) 0.0320(7) Uani 1 1 d . . . H15 H 0.6452 1.1068 0.1938 0.038 Uiso 1 1 calc R . . C16 C 0.8096(3) 1.0930(3) 0.19746(19) 0.0355(8) Uani 1 1 d . . . C17 C 0.9087(3) 1.0175(3) 0.20412(18) 0.0342(8) Uani 1 1 d . . . H17 H 0.9746 1.0413 0.2051 0.041 Uiso 1 1 calc R . . C18 C 0.9153(2) 0.9089(3) 0.20943(17) 0.0276(7) Uani 1 1 d . . . C19 C 0.6103(2) 0.9099(3) 0.21384(19) 0.0320(7) Uani 1 1 d . . . H19A H 0.5967 0.8881 0.2709 0.048 Uiso 1 1 calc R . . H19B H 0.6165 0.8471 0.1932 0.048 Uiso 1 1 calc R . . H19C H 0.5495 0.9696 0.1842 0.048 Uiso 1 1 calc R . . C20 C 0.8063(3) 1.2094(3) 0.1944(3) 0.0647(12) Uani 1 1 d . . . H20A H 0.8229 1.2123 0.2484 0.097 Uiso 1 1 calc R . . H20B H 0.7330 1.2554 0.1743 0.097 Uiso 1 1 calc R . . H20C H 0.8606 1.2364 0.1587 0.097 Uiso 1 1 calc R . . C21 C 1.0252(3) 0.8280(3) 0.2237(2) 0.0409(8) Uani 1 1 d . . . H21A H 1.0836 0.8668 0.2225 0.061 Uiso 1 1 calc R . . H21B H 1.0339 0.7917 0.1816 0.061 Uiso 1 1 calc R . . H21C H 1.0292 0.7730 0.2761 0.061 Uiso 1 1 calc R . . C22 C 0.6609(3) 0.8292(3) -0.0116(2) 0.0414(8) Uani 1 1 d . . . H22 H 0.6257 0.7743 0.0253 0.050 Uiso 1 1 calc R . . C23 C 0.6587(3) 0.9216(3) 0.01324(19) 0.0386(8) Uani 1 1 d . . . H23 H 0.6230 0.9187 0.0647 0.046 Uiso 1 1 calc R . . C24 C 0.6482(3) 1.0374(3) -0.0409(2) 0.0513(10) Uani 1 1 d . . . H24A H 0.6056 1.0896 -0.0149 0.062 Uiso 1 1 calc R . . H24B H 0.6071 1.0467 -0.0918 0.062 Uiso 1 1 calc R . . C25 C 0.7589(3) 1.0645(3) -0.0595(3) 0.0618(12) Uani 1 1 d . . . H25A H 0.7507 1.1235 -0.1111 0.074 Uiso 1 1 calc R . . H25B H 0.7828 1.0926 -0.0173 0.074 Uiso 1 1 calc R . . C26 C 0.8461(3) 0.9670(3) -0.0646(2) 0.0485(9) Uani 1 1 d . . . H26 H 0.9224 0.9778 -0.0632 0.058 Uiso 1 1 calc R . . C27 C 0.8339(3) 0.8914(3) -0.10161(19) 0.0479(9) Uani 1 1 d . . . H27 H 0.9032 0.8565 -0.1215 0.057 Uiso 1 1 calc R . . C28 C 0.7318(3) 0.8967(4) -0.1488(2) 0.0621(12) Uani 1 1 d . . . H28A H 0.7523 0.8714 -0.1961 0.074 Uiso 1 1 calc R . . H28B H 0.6889 0.9736 -0.1683 0.074 Uiso 1 1 calc R . . C29 C 0.6604(3) 0.8247(4) -0.0973(2) 0.0594(11) Uani 1 1 d . . . H29A H 0.5842 0.8499 -0.1214 0.071 Uiso 1 1 calc R . . H29B H 0.6882 0.7478 -0.0973 0.071 Uiso 1 1 calc R . . C30 C 0.2168(2) 0.3260(2) 0.41950(16) 0.0216(6) Uani 1 1 d . . . C31 C 0.0660(3) 0.4665(2) 0.41847(19) 0.0324(7) Uani 1 1 d . . . C32 C 0.0277(3) 0.3621(2) 0.4368(2) 0.0354(8) Uani 1 1 d . . . H32A H -0.0013 0.3440 0.4905 0.042 Uiso 1 1 calc R . . H32B H -0.0292 0.3664 0.3961 0.042 Uiso 1 1 calc R . . C33 C 0.2396(2) 0.5194(2) 0.37751(17) 0.0255(7) Uani 1 1 d . . . C34 C 0.2321(2) 0.5666(2) 0.29426(18) 0.0272(7) Uani 1 1 d . . . C35 C 0.2904(2) 0.6448(2) 0.26309(18) 0.0296(7) Uani 1 1 d . . . H35 H 0.2877 0.6761 0.2066 0.035 Uiso 1 1 calc R . . C36 C 0.3531(2) 0.6793(2) 0.31142(18) 0.0300(7) Uani 1 1 d . . . C37 C 0.3556(2) 0.6325(2) 0.39378(18) 0.0306(7) Uani 1 1 d . . . H37 H 0.3991 0.6546 0.4276 0.037 Uiso 1 1 calc R . . C38 C 0.2970(2) 0.5548(2) 0.42866(17) 0.0275(7) Uani 1 1 d . . . C39 C 0.1575(3) 0.5377(3) 0.2401(2) 0.0392(8) Uani 1 1 d . . . H39A H 0.1756 0.5645 0.1844 0.059 Uiso 1 1 calc R . . H39B H 0.0811 0.5720 0.2454 0.059 Uiso 1 1 calc R . . H39C H 0.1674 0.4580 0.2555 0.059 Uiso 1 1 calc R . . C40 C 0.4133(3) 0.7671(3) 0.2771(2) 0.0477(9) Uani 1 1 d . . . H40A H 0.3775 0.8339 0.2901 0.072 Uiso 1 1 calc R . . H40B H 0.4125 0.7825 0.2187 0.072 Uiso 1 1 calc R . . H40C H 0.4892 0.7425 0.2999 0.072 Uiso 1 1 calc R . . C41 C 0.2938(3) 0.5155(3) 0.51866(18) 0.0410(8) Uani 1 1 d . . . H41A H 0.2285 0.4863 0.5324 0.061 Uiso 1 1 calc R . . H41B H 0.2910 0.5768 0.5404 0.061 Uiso 1 1 calc R . . H41C H 0.3596 0.4577 0.5416 0.061 Uiso 1 1 calc R . . C42 C 0.1305(2) 0.1694(2) 0.44209(18) 0.0253(7) Uani 1 1 d . . . C43 C 0.1518(2) 0.0920(2) 0.51706(18) 0.0287(7) Uani 1 1 d . . . C44 C 0.1579(2) -0.0160(3) 0.5208(2) 0.0362(8) Uani 1 1 d . . . H44 H 0.1736 -0.0706 0.5714 0.043 Uiso 1 1 calc R . . C45 C 0.1419(3) -0.0471(3) 0.4537(2) 0.0390(8) Uani 1 1 d . . . C46 C 0.1133(3) 0.0337(3) 0.3812(2) 0.0399(8) Uani 1 1 d . . . H46 H 0.0982 0.0135 0.3351 0.048 Uiso 1 1 calc R . . C47 C 0.1058(2) 0.1425(3) 0.37346(19) 0.0319(7) Uani 1 1 d . . . C48 C 0.1630(3) 0.1247(3) 0.59149(19) 0.0399(8) Uani 1 1 d . . . H48A H 0.2244 0.1601 0.5881 0.060 Uiso 1 1 calc R . . H48B H 0.1765 0.0594 0.6384 0.060 Uiso 1 1 calc R . . H48C H 0.0953 0.1759 0.5966 0.060 Uiso 1 1 calc R . . C49 C 0.1536(3) -0.1667(3) 0.4603(3) 0.0644(12) Uani 1 1 d . . . H49A H 0.0914 -0.1745 0.4305 0.097 Uiso 1 1 calc R . . H49B H 0.1549 -0.2091 0.5168 0.097 Uiso 1 1 calc R . . H49C H 0.2220 -0.1939 0.4380 0.097 Uiso 1 1 calc R . . C50 C 0.0696(3) 0.2303(3) 0.29413(19) 0.0426(9) Uani 1 1 d . . . H50A H 0.0701 0.1958 0.2513 0.064 Uiso 1 1 calc R . . H50B H 0.1200 0.2793 0.2830 0.064 Uiso 1 1 calc R . . H50C H -0.0046 0.2725 0.2967 0.064 Uiso 1 1 calc R . . C51 C 0.3882(3) 0.2978(3) 0.29735(18) 0.0393(8) Uani 1 1 d . . . H51 H 0.3242 0.3555 0.2663 0.047 Uiso 1 1 calc R . . C52 C 0.3664(3) 0.1950(3) 0.32647(18) 0.0342(8) Uani 1 1 d . . . H52 H 0.2901 0.1929 0.3117 0.041 Uiso 1 1 calc R . . C53 C 0.4482(3) 0.0875(3) 0.3394(2) 0.0460(9) Uani 1 1 d . . . H53A H 0.4606 0.0739 0.2870 0.055 Uiso 1 1 calc R . . H53B H 0.4168 0.0281 0.3732 0.055 Uiso 1 1 calc R . . C54 C 0.5582(3) 0.0823(3) 0.3790(2) 0.0505(10) Uani 1 1 d . . . H54A H 0.5936 0.0050 0.4079 0.061 Uiso 1 1 calc R . . H54B H 0.6066 0.1100 0.3372 0.061 Uiso 1 1 calc R . . C55 C 0.5454(3) 0.1493(3) 0.4374(2) 0.0445(9) Uani 1 1 d . . . H55 H 0.5707 0.1052 0.4940 0.053 Uiso 1 1 calc R . . C56 C 0.5525(3) 0.2553(4) 0.4189(2) 0.0519(10) Uani 1 1 d . . . H56 H 0.5827 0.2740 0.4646 0.062 Uiso 1 1 calc R . . C57 C 0.5680(4) 0.3292(4) 0.3376(3) 0.0688(13) Uani 1 1 d . . . H57A H 0.6462 0.3112 0.3263 0.083 Uiso 1 1 calc R . . H57B H 0.5491 0.4062 0.3387 0.083 Uiso 1 1 calc R . . C58 C 0.4984(3) 0.3189(3) 0.2705(2) 0.0552(11) Uani 1 1 d . . . H58A H 0.4865 0.3872 0.2251 0.066 Uiso 1 1 calc R . . H58B H 0.5383 0.2579 0.2513 0.066 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02537(14) 0.03000(14) 0.02155(13) -0.00684(10) 0.00311(10) -0.00407(10) Rh2 0.02357(14) 0.02498(13) 0.02442(14) -0.00900(10) -0.00060(10) -0.00308(10) Cl1 0.0270(4) 0.0372(4) 0.0435(5) -0.0108(4) 0.0062(4) -0.0026(3) Cl2 0.0422(5) 0.0461(5) 0.0275(4) -0.0136(4) -0.0044(4) -0.0055(4) N1 0.0330(15) 0.0270(13) 0.0227(13) -0.0102(11) 0.0020(11) -0.0076(11) N2 0.0303(14) 0.0266(13) 0.0212(13) -0.0095(11) 0.0035(11) -0.0047(11) N3 0.0263(14) 0.0193(12) 0.0305(14) -0.0061(11) 0.0025(11) -0.0041(10) N4 0.0249(14) 0.0199(13) 0.0315(14) -0.0089(11) 0.0030(11) -0.0032(11) O1 0.087(2) 0.0387(15) 0.0370(14) -0.0088(12) 0.0031(13) -0.0192(14) O2 0.0416(14) 0.0310(13) 0.0541(15) -0.0144(11) 0.0085(11) -0.0031(11) C1 0.0166(15) 0.0287(16) 0.0289(16) -0.0111(13) 0.0012(12) -0.0012(12) C2 0.043(2) 0.0264(18) 0.0269(17) -0.0064(14) 0.0035(14) -0.0081(15) C3 0.0430(19) 0.0266(16) 0.0229(16) -0.0069(13) 0.0037(14) -0.0077(14) C4 0.0355(18) 0.0253(16) 0.0229(16) -0.0092(13) 0.0016(13) -0.0077(14) C5 0.0320(19) 0.0334(18) 0.0394(19) -0.0164(15) 0.0038(15) -0.0065(14) C6 0.0313(19) 0.051(2) 0.053(2) -0.0265(18) 0.0010(16) -0.0087(16) C7 0.039(2) 0.047(2) 0.047(2) -0.0280(18) 0.0001(16) -0.0081(16) C8 0.0307(18) 0.0383(19) 0.0354(18) -0.0186(15) 0.0057(14) -0.0040(15) C9 0.0301(17) 0.0276(16) 0.0253(16) -0.0058(13) 0.0019(13) -0.0071(13) C10 0.036(2) 0.050(2) 0.056(2) -0.0299(19) 0.0135(17) -0.0118(17) C11 0.042(2) 0.091(3) 0.089(3) -0.068(3) 0.002(2) -0.009(2) C12 0.0348(19) 0.0379(19) 0.0389(19) -0.0163(16) 0.0013(15) -0.0078(15) C13 0.0284(17) 0.0251(15) 0.0200(15) -0.0084(12) 0.0034(12) -0.0071(13) C14 0.0261(16) 0.0321(17) 0.0186(15) -0.0087(13) 0.0006(12) -0.0087(13) C15 0.0294(18) 0.0284(17) 0.0333(18) -0.0063(14) 0.0019(14) -0.0010(14) C16 0.040(2) 0.0279(17) 0.0377(19) -0.0051(14) 0.0026(15) -0.0126(15) C17 0.0332(19) 0.042(2) 0.0324(18) -0.0100(15) 0.0080(14) -0.0204(16) C18 0.0260(17) 0.0372(18) 0.0211(15) -0.0096(13) 0.0058(13) -0.0093(14) C19 0.0257(17) 0.0385(18) 0.0357(18) -0.0155(15) 0.0069(14) -0.0094(14) C20 0.059(3) 0.032(2) 0.103(4) -0.014(2) 0.004(2) -0.0177(19) C21 0.0261(18) 0.051(2) 0.049(2) -0.0217(18) 0.0023(15) -0.0068(16) C22 0.0280(18) 0.053(2) 0.035(2) -0.0032(17) -0.0046(15) -0.0075(16) C23 0.0273(18) 0.052(2) 0.0286(18) -0.0089(16) 0.0004(14) 0.0023(16) C24 0.046(2) 0.044(2) 0.055(2) -0.0105(19) -0.0071(19) 0.0037(18) C25 0.059(3) 0.034(2) 0.076(3) 0.004(2) -0.017(2) -0.0046(19) C26 0.042(2) 0.052(2) 0.042(2) 0.0052(18) 0.0043(17) -0.0172(18) C27 0.046(2) 0.069(3) 0.0233(18) -0.0060(18) 0.0111(16) -0.0121(19) C28 0.069(3) 0.086(3) 0.033(2) -0.023(2) 0.003(2) -0.013(2) C29 0.056(3) 0.067(3) 0.054(3) -0.024(2) -0.019(2) -0.006(2) C30 0.0285(16) 0.0194(14) 0.0170(14) -0.0058(12) 0.0005(12) -0.0052(12) C31 0.0302(18) 0.0231(17) 0.042(2) -0.0105(14) 0.0057(15) -0.0016(14) C32 0.0303(18) 0.0265(17) 0.048(2) -0.0124(15) 0.0067(15) -0.0021(14) C33 0.0252(16) 0.0169(14) 0.0313(17) -0.0041(13) 0.0034(13) -0.0029(12) C34 0.0274(17) 0.0226(15) 0.0302(17) -0.0074(13) -0.0042(13) -0.0037(13) C35 0.0318(18) 0.0285(17) 0.0248(16) -0.0041(13) 0.0007(13) -0.0052(14) C36 0.0260(17) 0.0284(17) 0.0364(19) -0.0111(14) 0.0070(14) -0.0062(13) C37 0.0335(18) 0.0317(17) 0.0321(18) -0.0158(14) -0.0009(14) -0.0107(14) C38 0.0345(18) 0.0222(15) 0.0256(16) -0.0091(13) 0.0015(13) -0.0036(13) C39 0.044(2) 0.0343(18) 0.0371(19) -0.0055(15) -0.0123(16) -0.0110(16) C40 0.054(2) 0.055(2) 0.043(2) -0.0129(18) 0.0109(18) -0.0328(19) C41 0.063(2) 0.0348(19) 0.0285(18) -0.0117(15) 0.0023(16) -0.0161(17) C42 0.0209(16) 0.0222(15) 0.0348(18) -0.0119(13) 0.0042(13) -0.0045(12) C43 0.0234(16) 0.0265(16) 0.0357(18) -0.0092(14) 0.0019(13) -0.0050(13) C44 0.0254(17) 0.0249(17) 0.052(2) -0.0025(15) 0.0023(15) -0.0047(13) C45 0.0232(17) 0.0299(18) 0.071(3) -0.0227(18) 0.0077(17) -0.0094(14) C46 0.0329(19) 0.044(2) 0.055(2) -0.0325(19) 0.0040(16) -0.0120(16) C47 0.0255(17) 0.0363(18) 0.0366(18) -0.0147(15) 0.0024(14) -0.0078(14) C48 0.044(2) 0.044(2) 0.0289(18) -0.0059(15) 0.0028(15) -0.0117(16) C49 0.049(2) 0.031(2) 0.122(4) -0.035(2) 0.006(2) -0.0105(18) C50 0.043(2) 0.055(2) 0.0326(19) -0.0155(17) -0.0040(16) -0.0134(17) C51 0.044(2) 0.042(2) 0.0232(17) -0.0069(15) 0.0034(15) 0.0050(16) C52 0.0319(18) 0.044(2) 0.0306(18) -0.0203(16) 0.0008(14) -0.0048(15) C53 0.058(2) 0.038(2) 0.045(2) -0.0230(17) 0.0078(18) -0.0042(17) C54 0.041(2) 0.047(2) 0.051(2) -0.0134(18) 0.0038(18) 0.0130(18) C55 0.0256(18) 0.061(3) 0.038(2) -0.0143(18) -0.0062(15) 0.0084(17) C56 0.027(2) 0.083(3) 0.058(3) -0.036(2) 0.0040(17) -0.0197(19) C57 0.065(3) 0.082(3) 0.083(3) -0.041(3) 0.036(3) -0.044(2) C58 0.073(3) 0.043(2) 0.046(2) -0.0075(18) 0.026(2) -0.015(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 C1 2.020(3) . ? Rh1 C22 2.110(3) . ? Rh1 C23 2.119(3) . ? Rh1 C26 2.198(3) . ? Rh1 C27 2.228(3) . ? Rh1 Cl1 2.3715(8) . ? Rh2 C30 2.008(3) . ? Rh2 C52 2.097(3) . ? Rh2 C51 2.123(3) . ? Rh2 C56 2.197(3) . ? Rh2 C55 2.228(3) . ? Rh2 Cl2 2.3760(8) . ? N1 C1 1.381(4) . ? N1 C2 1.393(4) . ? N1 C4 1.452(4) . ? N2 C1 1.336(3) . ? N2 C13 1.442(4) . ? N2 C3 1.458(4) . ? N3 C31 1.388(4) . ? N3 C30 1.396(3) . ? N3 C33 1.445(4) . ? N4 C30 1.341(4) . ? N4 C42 1.443(3) . ? N4 C32 1.467(4) . ? O1 C2 1.200(4) . ? O2 C31 1.217(3) . ? C2 C3 1.501(4) . ? C4 C5 1.388(4) . ? C4 C9 1.394(4) . ? C5 C6 1.387(4) . ? C5 C10 1.514(4) . ? C6 C7 1.397(4) . ? C7 C8 1.379(4) . ? C7 C11 1.512(5) . ? C8 C9 1.384(4) . ? C9 C12 1.501(4) . ? C13 C18 1.396(4) . ? C13 C14 1.397(4) . ? C14 C15 1.387(4) . ? C14 C19 1.510(4) . ? C15 C16 1.390(4) . ? C16 C17 1.386(4) . ? C16 C20 1.504(4) . ? C17 C18 1.384(4) . ? C18 C21 1.509(4) . ? C22 C23 1.397(5) . ? C22 C29 1.518(5) . ? C23 C24 1.514(5) . ? C24 C25 1.522(5) . ? C25 C26 1.510(5) . ? C26 C27 1.368(5) . ? C27 C28 1.503(5) . ? C28 C29 1.546(6) . ? C31 C32 1.500(4) . ? C33 C38 1.389(4) . ? C33 C34 1.400(4) . ? C34 C35 1.377(4) . ? C34 C39 1.513(4) . ? C35 C36 1.387(4) . ? C36 C37 1.388(4) . ? C36 C40 1.499(4) . ? C37 C38 1.388(4) . ? C38 C41 1.510(4) . ? C42 C43 1.387(4) . ? C42 C47 1.400(4) . ? C43 C44 1.383(4) . ? C43 C48 1.501(4) . ? C44 C45 1.378(5) . ? C45 C46 1.381(5) . ? C45 C49 1.513(4) . ? C46 C47 1.376(4) . ? C47 C50 1.513(4) . ? C51 C52 1.385(5) . ? C51 C58 1.519(5) . ? C52 C53 1.503(4) . ? C53 C54 1.524(5) . ? C54 C55 1.517(5) . ? C55 C56 1.356(5) . ? C56 C57 1.511(6) . ? C57 C58 1.519(6) . ? 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 C22 95.44(12) . . ? C1 Rh1 C23 96.12(12) . . ? C22 Rh1 C23 38.59(13) . . ? C1 Rh1 C26 155.56(14) . . ? C22 Rh1 C26 97.18(14) . . ? C23 Rh1 C26 81.15(14) . . ? C1 Rh1 C27 168.29(14) . . ? C22 Rh1 C27 80.73(13) . . ? C23 Rh1 C27 87.79(13) . . ? C26 Rh1 C27 36.00(14) . . ? C1 Rh1 Cl1 89.82(8) . . ? C22 Rh1 Cl1 156.00(10) . . ? C23 Rh1 Cl1 163.58(10) . . ? C26 Rh1 Cl1 87.11(10) . . ? C27 Rh1 Cl1 89.42(10) . . ? C30 Rh2 C52 95.97(12) . . ? C30 Rh2 C51 95.94(12) . . ? C52 Rh2 C51 38.31(13) . . ? C30 Rh2 C56 155.23(14) . . ? C52 Rh2 C56 96.60(13) . . ? C51 Rh2 C56 81.10(14) . . ? C30 Rh2 C55 168.87(13) . . ? C52 Rh2 C55 80.98(13) . . ? C51 Rh2 C55 88.29(13) . . ? C56 Rh2 C55 35.68(14) . . ? C30 Rh2 Cl2 89.68(8) . . ? C52 Rh2 Cl2 153.01(9) . . ? C51 Rh2 Cl2 166.69(10) . . ? C56 Rh2 Cl2 88.74(10) . . ? C55 Rh2 Cl2 88.42(9) . . ? C1 N1 C2 112.8(2) . . ? C1 N1 C4 125.4(2) . . ? C2 N1 C4 121.3(3) . . ? C1 N2 C13 124.5(2) . . ? C1 N2 C3 113.4(2) . . ? C13 N2 C3 121.8(2) . . ? C31 N3 C30 113.0(2) . . ? C31 N3 C33 121.8(2) . . ? C30 N3 C33 124.0(2) . . ? C30 N4 C42 124.6(2) . . ? C30 N4 C32 113.6(2) . . ? C42 N4 C32 121.8(2) . . ? N2 C1 N1 106.4(2) . . ? N2 C1 Rh1 124.5(2) . . ? N1 C1 Rh1 128.8(2) . . ? O1 C2 N1 125.7(3) . . ? O1 C2 C3 128.8(3) . . ? N1 C2 C3 105.5(2) . . ? N2 C3 C2 101.9(2) . . ? C5 C4 C9 121.9(3) . . ? C5 C4 N1 118.0(3) . . ? C9 C4 N1 120.0(3) . . ? C6 C5 C4 118.3(3) . . ? C6 C5 C10 120.1(3) . . ? C4 C5 C10 121.5(3) . . ? C5 C6 C7 121.2(3) . . ? C8 C7 C6 118.3(3) . . ? C8 C7 C11 120.8(3) . . ? C6 C7 C11 120.8(3) . . ? C7 C8 C9 122.4(3) . . ? C8 C9 C4 117.6(3) . . ? C8 C9 C12 120.7(3) . . ? C4 C9 C12 121.6(3) . . ? C18 C13 C14 121.6(3) . . ? C18 C13 N2 120.4(3) . . ? C14 C13 N2 117.9(2) . . ? C15 C14 C13 118.1(3) . . ? C15 C14 C19 119.5(3) . . ? C13 C14 C19 122.2(3) . . ? C14 C15 C16 121.9(3) . . ? C17 C16 C15 117.9(3) . . ? C17 C16 C20 120.8(3) . . ? C15 C16 C20 121.2(3) . . ? C18 C17 C16 122.6(3) . . ? C17 C18 C13 117.6(3) . . ? C17 C18 C21 120.4(3) . . ? C13 C18 C21 121.9(3) . . ? C23 C22 C29 126.5(3) . . ? C23 C22 Rh1 71.07(19) . . ? C29 C22 Rh1 110.0(2) . . ? C22 C23 C24 126.1(3) . . ? C22 C23 Rh1 70.34(19) . . ? C24 C23 Rh1 113.6(2) . . ? C23 C24 C25 112.6(3) . . ? C26 C25 C24 112.9(3) . . ? C27 C26 C25 126.4(4) . . ? C27 C26 Rh1 73.2(2) . . ? C25 C26 Rh1 107.2(2) . . ? C26 C27 C28 124.8(4) . . ? C26 C27 Rh1 70.8(2) . . ? C28 C27 Rh1 111.6(2) . . ? C27 C28 C29 111.3(3) . . ? C22 C29 C28 111.9(3) . . ? N4 C30 N3 105.7(2) . . ? N4 C30 Rh2 131.7(2) . . ? N3 C30 Rh2 122.3(2) . . ? O2 C31 N3 125.5(3) . . ? O2 C31 C32 128.7(3) . . ? N3 C31 C32 105.9(2) . . ? N4 C32 C31 101.8(2) . . ? C38 C33 C34 122.0(3) . . ? C38 C33 N3 120.3(3) . . ? C34 C33 N3 117.5(3) . . ? C35 C34 C33 118.0(3) . . ? C35 C34 C39 120.6(3) . . ? C33 C34 C39 121.3(3) . . ? C34 C35 C36 122.2(3) . . ? C35 C36 C37 117.8(3) . . ? C35 C36 C40 121.8(3) . . ? C37 C36 C40 120.3(3) . . ? C38 C37 C36 122.5(3) . . ? C37 C38 C33 117.3(3) . . ? C37 C38 C41 120.0(3) . . ? C33 C38 C41 122.6(3) . . ? C43 C42 C47 121.9(3) . . ? C43 C42 N4 120.0(3) . . ? C47 C42 N4 118.1(3) . . ? C44 C43 C42 117.4(3) . . ? C44 C43 C48 121.4(3) . . ? C42 C43 C48 121.2(3) . . ? C45 C44 C43 122.4(3) . . ? C44 C45 C46 118.3(3) . . ? C44 C45 C49 120.4(3) . . ? C46 C45 C49 121.3(3) . . ? C47 C46 C45 122.1(3) . . ? C46 C47 C42 117.6(3) . . ? C46 C47 C50 121.3(3) . . ? C42 C47 C50 121.1(3) . . ? C52 C51 C58 124.8(3) . . ? C52 C51 Rh2 69.85(18) . . ? C58 C51 Rh2 113.7(2) . . ? C51 C52 C53 125.7(3) . . ? C51 C52 Rh2 71.84(18) . . ? C53 C52 Rh2 110.8(2) . . ? C52 C53 C54 113.9(3) . . ? C55 C54 C53 111.8(3) . . ? C56 C55 C54 125.0(3) . . ? C56 C55 Rh2 70.9(2) . . ? C54 C55 Rh2 111.1(2) . . ? C55 C56 C57 127.1(4) . . ? C55 C56 Rh2 73.4(2) . . ? C57 C56 Rh2 107.2(3) . . ? C56 C57 C58 113.0(3) . . ? C51 C58 C57 112.1(3) . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.958 _refine_diff_density_max 0.739 _refine_diff_density_min -0.361 _refine_diff_density_rms 0.062 _vrf_PLAT029_7a ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.96 RESPONSE: Due to the triclinic system, some data are missing and we have only 96 % completness up to 24.71 degree in theta, but the data/parameter ration is about 14. ; #===END