# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Kam-Hung Low' _publ_contact_author_email khlow@hku.hk loop_ _publ_author_name F.-M.Siu I.W.-S.Lin K.Yan C.-N.Lok K.-H.Low Yu.C.Leung ; T.L.Lam ; C.-M.Che # Attachment 'web_deposit_cif_file_3_Kam-HungLow_1308561056.iris8.cif' data_iris8 _database_code_depnum_ccdc_archive 'CCDC 830690' #TrackingRef 'web_deposit_cif_file_3_Kam-HungLow_1308561056.iris8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H60 N4 O6 Rh2' _chemical_formula_sum 'C32 H60 N4 O6 Rh2' _chemical_formula_weight 802.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/C' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 6.9865(4) _cell_length_b 19.2728(11) _cell_length_c 14.2390(8) _cell_angle_alpha 90.00 _cell_angle_beta 103.327(2) _cell_angle_gamma 90.00 _cell_volume 1865.64(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 118 _cell_measurement_theta_min 3 _cell_measurement_theta_max 45 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.429 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 836 _exptl_absorpt_coefficient_mu 7.508 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.612 _exptl_absorpt_correction_T_max 0.741 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19337 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.0361 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.93 _diffrn_reflns_theta_max 66.20 _reflns_number_total 3193 _reflns_number_gt 3086 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0964P)^2^+7.9609P] 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 3193 _refine_ls_number_parameters 230 _refine_ls_number_restraints 71 _refine_ls_R_factor_all 0.0619 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1652 _refine_ls_wR_factor_gt 0.1633 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.066 _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 0.14528(5) 0.46888(2) 0.98859(3) 0.0316(2) Uani 1 1 d . . . N1 N -0.0308(7) 0.4345(2) 0.8662(3) 0.0350(10) Uani 1 1 d . . . N2 N -0.0623(7) 0.6061(2) 0.9305(3) 0.0368(11) Uani 1 1 d . . . O1 O 0.3136(6) 0.5111(2) 1.1151(3) 0.0381(9) Uani 1 1 d . . . O2 O 0.2188(6) 0.5513(2) 0.9102(3) 0.0405(9) Uani 1 1 d . . . O3 O 0.4255(6) 0.4139(2) 0.9676(3) 0.0394(9) Uani 1 1 d D . . C1 C -0.2154(10) 0.4508(3) 0.8385(5) 0.0436(14) Uani 1 1 d . . . C3 C -0.1458(13) 0.3886(5) 0.7089(6) 0.069(2) Uani 1 1 d . A . H3A H -0.1190 0.4155 0.6540 0.083 Uiso 1 1 calc R . . H3B H -0.1752 0.3401 0.6877 0.083 Uiso 1 1 calc R . . C4 C 0.0321(13) 0.3910(5) 0.7940(6) 0.067(2) Uani 1 1 d . . . H4A H 0.0676 0.3438 0.8197 0.080 Uiso 1 1 calc R . . H4B H 0.1468 0.4118 0.7747 0.080 Uiso 1 1 calc R . . C2 C -0.3180(14) 0.4197(5) 0.7416(7) 0.079(3) Uani 1 1 d D . . H2A H -0.28(3) 0.461(6) 0.709(12) 0.04(3) Uiso 0.409(10) 1 d PD A 1 C5A C -0.500(3) 0.4068(13) 0.7047(14) 0.069(3) Uani 0.409(10) 1 d PDU A 1 H5A1 H -0.5741 0.4319 0.7458 0.083 Uiso 0.409(10) 1 calc PR A 1 H5A2 H -0.5173 0.3568 0.7163 0.083 Uiso 0.409(10) 1 calc PR A 1 C6A C -0.614(5) 0.4201(19) 0.600(2) 0.096(5) Uani 0.409(10) 1 d PDU A 1 H6A1 H -0.6766 0.3746 0.5815 0.115 Uiso 0.409(10) 1 calc PR A 1 H6A2 H -0.5067 0.4232 0.5656 0.115 Uiso 0.409(10) 1 calc PR A 1 C7A C -0.768(4) 0.4715(12) 0.5439(17) 0.093(4) Uani 0.409(10) 1 d PDU A 1 H7A1 H -0.8440 0.4915 0.5880 0.112 Uiso 0.409(10) 1 calc PR A 1 H7A2 H -0.6991 0.5101 0.5193 0.112 Uiso 0.409(10) 1 calc PR A 1 C8A C -0.908(6) 0.436(2) 0.460(2) 0.129(7) Uani 0.409(10) 1 d PDU A 1 H8A1 H -0.8319 0.4142 0.4179 0.193 Uiso 0.409(10) 1 calc PR A 1 H8A2 H -0.9963 0.4711 0.4225 0.193 Uiso 0.409(10) 1 calc PR A 1 H8A3 H -0.9848 0.4012 0.4842 0.193 Uiso 0.409(10) 1 calc PR A 1 H2B H -0.383(17) 0.377(4) 0.762(8) 0.04(3) Uiso 0.591(10) 1 d PD A 2 C5B C -0.473(2) 0.4638(8) 0.6822(11) 0.069(3) Uani 0.591(10) 1 d PDU A 2 H5B1 H -0.4145 0.5091 0.6716 0.083 Uiso 0.591(10) 1 calc PR A 2 H5B2 H -0.5757 0.4724 0.7183 0.083 Uiso 0.591(10) 1 calc PR A 2 C6B C -0.570(3) 0.4318(13) 0.5830(14) 0.096(5) Uani 0.591(10) 1 d PDU A 2 H6B1 H -0.6461 0.4686 0.5421 0.115 Uiso 0.591(10) 1 calc PR A 2 H6B2 H -0.4648 0.4166 0.5515 0.115 Uiso 0.591(10) 1 calc PR A 2 C7B C -0.705(3) 0.3714(10) 0.5853(11) 0.093(4) Uani 0.591(10) 1 d PDU A 2 H7B1 H -0.7940 0.3821 0.6281 0.112 Uiso 0.591(10) 1 calc PR A 2 H7B2 H -0.6262 0.3299 0.6111 0.112 Uiso 0.591(10) 1 calc PR A 2 C8B C -0.826(4) 0.3566(15) 0.4820(14) 0.129(7) Uani 0.591(10) 1 d PDU A 2 H8B1 H -0.8801 0.4001 0.4516 0.193 Uiso 0.591(10) 1 calc PR A 2 H8B2 H -0.9334 0.3246 0.4849 0.193 Uiso 0.591(10) 1 calc PR A 2 H8B3 H -0.7406 0.3355 0.4439 0.193 Uiso 0.591(10) 1 calc PR A 2 C9 C 0.0925(10) 0.6009(3) 0.8946(5) 0.0418(14) Uani 1 1 d . . . C10 C 0.1156(16) 0.6610(5) 0.8310(8) 0.083(3) Uani 1 1 d . . . H10 H 0.2068 0.6911 0.8784 0.100 Uiso 1 1 calc R . . C11 C -0.0717(13) 0.6995(5) 0.8219(7) 0.075(3) Uani 1 1 d . . . H11A H -0.1554 0.6943 0.7560 0.091 Uiso 1 1 calc R . . H11B H -0.0455 0.7495 0.8348 0.091 Uiso 1 1 calc R . . C12 C -0.1740(12) 0.6683(4) 0.8964(6) 0.060(2) Uani 1 1 d . . . H12A H -0.1709 0.7011 0.9502 0.072 Uiso 1 1 calc R . . H12B H -0.3126 0.6567 0.8663 0.072 Uiso 1 1 calc R . . C13 C 0.2306(18) 0.6498(7) 0.7618(8) 0.104(4) Uani 1 1 d . . . H13A H 0.1648 0.6126 0.7182 0.125 Uiso 1 1 calc R . . H13B H 0.3585 0.6308 0.7973 0.125 Uiso 1 1 calc R . . C14 C 0.2759(19) 0.7072(5) 0.6985(8) 0.092(3) Uani 1 1 d U . . H14A H 0.1486 0.7266 0.6628 0.111 Uiso 1 1 calc R . . H14B H 0.3436 0.7444 0.7417 0.111 Uiso 1 1 calc R . . C15 C 0.388(3) 0.6940(9) 0.6310(11) 0.149(6) Uani 1 1 d U . . H15A H 0.3203 0.6572 0.5871 0.178 Uiso 1 1 calc R . . H15B H 0.5156 0.6745 0.6663 0.178 Uiso 1 1 calc R . . C16 C 0.430(3) 0.7513(7) 0.5712(9) 0.133(6) Uani 1 1 d U . . H16A H 0.3770 0.7405 0.5029 0.200 Uiso 1 1 calc R . . H16B H 0.5729 0.7580 0.5827 0.200 Uiso 1 1 calc R . . H16C H 0.3692 0.7940 0.5879 0.200 Uiso 1 1 calc R . . H31 H 0.443(12) 0.444(3) 0.919(4) 0.06(2) Uiso 1 1 d D . . H32 H 0.508(11) 0.431(4) 1.024(4) 0.07(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0282(3) 0.0339(3) 0.0410(3) 0.00266(15) 0.0249(2) 0.00121(15) N1 0.031(2) 0.041(3) 0.037(2) -0.004(2) 0.017(2) 0.000(2) N2 0.038(3) 0.037(2) 0.042(3) 0.008(2) 0.023(2) 0.003(2) O1 0.029(2) 0.046(2) 0.043(2) -0.0061(18) 0.0134(17) 0.0009(17) O2 0.042(2) 0.042(2) 0.050(2) 0.0090(19) 0.035(2) 0.0014(19) O3 0.028(2) 0.043(2) 0.054(3) 0.002(2) 0.0242(19) 0.0006(17) C1 0.044(4) 0.046(3) 0.047(3) -0.002(3) 0.021(3) 0.002(3) C3 0.070(5) 0.094(6) 0.051(4) -0.021(4) 0.030(4) 0.007(4) C4 0.067(5) 0.081(5) 0.055(4) -0.029(4) 0.021(4) 0.011(4) C2 0.067(6) 0.088(7) 0.075(6) -0.039(5) 0.002(5) 0.014(5) C5A 0.062(7) 0.081(7) 0.067(6) -0.014(5) 0.018(5) 0.009(6) C6A 0.090(11) 0.121(10) 0.075(8) 0.001(7) 0.014(8) -0.023(7) C7A 0.121(11) 0.095(9) 0.067(7) 0.002(6) 0.026(6) -0.017(7) C8A 0.120(14) 0.151(17) 0.098(10) -0.005(11) -0.009(9) -0.027(12) C5B 0.062(7) 0.081(7) 0.067(6) -0.014(5) 0.018(5) 0.009(6) C6B 0.090(11) 0.121(10) 0.075(8) 0.001(7) 0.014(8) -0.023(7) C7B 0.121(11) 0.095(9) 0.067(7) 0.002(6) 0.026(6) -0.017(7) C8B 0.120(14) 0.151(17) 0.098(10) -0.005(11) -0.009(9) -0.027(12) C9 0.046(3) 0.040(3) 0.047(3) 0.007(3) 0.027(3) -0.001(3) C10 0.098(7) 0.065(5) 0.112(7) 0.036(5) 0.079(6) 0.020(5) C11 0.064(5) 0.067(5) 0.103(7) 0.044(5) 0.035(5) 0.007(4) C12 0.060(4) 0.053(4) 0.080(5) 0.026(4) 0.039(4) 0.016(3) C13 0.093(7) 0.141(10) 0.097(7) 0.056(7) 0.061(6) 0.014(7) C14 0.116(8) 0.079(6) 0.096(7) 0.020(5) 0.051(6) -0.010(6) C15 0.149(12) 0.191(14) 0.130(10) 0.071(10) 0.081(9) -0.002(11) C16 0.209(16) 0.122(10) 0.083(7) 0.013(7) 0.064(9) -0.051(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 Rh1 N1 2.000(5) . ? Rh1 N2 2.014(5) 3_567 ? Rh1 O2 2.073(4) . ? Rh1 O1 2.076(4) . ? Rh1 O3 2.305(4) . ? Rh1 Rh1 2.4432(7) 3_567 ? N1 C1 1.297(8) . ? N1 C4 1.470(8) . ? N2 C9 1.302(8) . ? N2 C12 1.452(8) . ? N2 Rh1 2.014(5) 3_567 ? O1 C1 1.287(8) 3_567 ? O2 C9 1.285(8) . ? C1 O1 1.287(8) 3_567 ? C1 C2 1.523(11) . ? C3 C2 1.511(12) . ? C3 C4 1.524(12) . ? C2 C5A 1.28(2) . ? C2 C5B 1.478(18) . ? C5A C6A 1.535(18) . ? C6A C7A 1.546(19) . ? C7A C8A 1.521(19) . ? C5B C6B 1.548(17) . ? C6B C7B 1.501(17) . ? C7B C8B 1.546(16) . ? C9 C10 1.503(9) . ? C10 C13 1.424(12) . ? C10 C11 1.483(12) . ? C11 C12 1.532(10) . ? C13 C14 1.506(13) . ? C14 C15 1.397(17) . ? C15 C16 1.467(16) . ? 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 N1 Rh1 N2 93.5(2) . 3_567 ? N1 Rh1 O2 87.94(19) . . ? N2 Rh1 O2 175.65(17) 3_567 . ? N1 Rh1 O1 175.60(17) . . ? N2 Rh1 O1 87.98(19) 3_567 . ? O2 Rh1 O1 90.33(18) . . ? N1 Rh1 O3 96.02(17) . . ? N2 Rh1 O3 96.31(17) 3_567 . ? O2 Rh1 O3 87.63(15) . . ? O1 Rh1 O3 87.95(16) . . ? N1 Rh1 Rh1 85.16(13) . 3_567 ? N2 Rh1 Rh1 85.33(14) 3_567 3_567 ? O2 Rh1 Rh1 90.69(11) . 3_567 ? O1 Rh1 Rh1 90.81(11) . 3_567 ? O3 Rh1 Rh1 177.91(10) . 3_567 ? C1 N1 C4 111.2(5) . . ? C1 N1 Rh1 123.6(4) . . ? C4 N1 Rh1 125.1(4) . . ? C9 N2 C12 111.3(5) . . ? C9 N2 Rh1 122.9(4) . 3_567 ? C12 N2 Rh1 125.5(4) . 3_567 ? C1 O1 Rh1 114.0(4) 3_567 . ? C9 O2 Rh1 114.7(3) . . ? O1 C1 N1 126.3(6) 3_567 . ? O1 C1 C2 119.6(6) 3_567 . ? N1 C1 C2 114.1(6) . . ? C2 C3 C4 107.7(6) . . ? N1 C4 C3 104.7(6) . . ? C5A C2 C5B 49.6(12) . . ? C5A C2 C3 125.6(12) . . ? C5B C2 C3 125.5(10) . . ? C5A C2 C1 131.4(12) . . ? C5B C2 C1 115.0(8) . . ? C3 C2 C1 101.2(7) . . ? C2 C5A C6A 127(2) . . ? C5A C6A C7A 139(3) . . ? C8A C7A C6A 112(2) . . ? C2 C5B C6B 113.8(14) . . ? C7B C6B C5B 115.7(15) . . ? C6B C7B C8B 109.3(16) . . ? O2 C9 N2 126.1(5) . . ? O2 C9 C10 120.9(6) . . ? N2 C9 C10 113.1(6) . . ? C13 C10 C11 130.0(9) . . ? C13 C10 C9 117.2(8) . . ? C11 C10 C9 102.9(6) . . ? C10 C11 C12 106.6(6) . . ? N2 C12 C11 104.8(6) . . ? C10 C13 C14 122.2(10) . . ? C15 C14 C13 120.3(11) . . ? C14 C15 C16 118.8(15) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 66.20 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.240 _refine_diff_density_min -1.704 _refine_diff_density_rms 0.167 data_iris3 _database_code_depnum_ccdc_archive 'CCDC 840241' #TrackingRef 'web_deposit_cif_file_0_Kam-HungLow_1313658494.iris3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 N6 O4 Rh2, 2(H2 O)' _chemical_formula_sum 'C20 H34 N6 O6 Rh2' _chemical_formula_weight 660.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' 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 16.3720(4) _cell_length_b 8.7441(2) _cell_length_c 17.2355(5) _cell_angle_alpha 90.00 _cell_angle_beta 104.0390(10) _cell_angle_gamma 90.00 _cell_volume 2393.71(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 174 _cell_measurement_theta_min 3 _cell_measurement_theta_max 45 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.832 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 11.577 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.602 _exptl_absorpt_correction_T_max 0.629 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30491 _diffrn_reflns_av_R_equivalents 0.0442 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 66.26 _reflns_number_total 4091 _reflns_number_gt 3864 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0462P)^2^+5.0305P] 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 4091 _refine_ls_number_parameters 321 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0904 _refine_ls_wR_factor_gt 0.0886 _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.988968(14) 0.98936(3) 0.067621(14) 0.01547(11) Uani 1 1 d . . . Rh2 Rh 0.523401(17) -0.00486(3) 0.073248(15) 0.02338(12) Uani 1 1 d . . . N1 N 1.10476(16) 0.9003(3) 0.09720(15) 0.0189(6) Uani 1 1 d . . . N2 N 0.96374(16) 0.7981(3) -0.08350(15) 0.0193(6) Uani 1 1 d . . . N3 N 0.41189(18) 0.0914(3) 0.07211(16) 0.0243(6) Uani 1 1 d . . . N4 N 0.46968(17) -0.2132(3) 0.06310(16) 0.0226(6) Uani 1 1 d . . . N5 N 0.9563(2) 0.9610(4) 0.18532(18) 0.0304(7) Uani 1 1 d . . . N6 N 0.5713(2) -0.0057(4) 0.2060(2) 0.0334(8) Uani 1 1 d . . . O1 O 1.13049(13) 0.9156(3) -0.02755(13) 0.0242(5) Uani 1 1 d . . . O2 O 0.94066(14) 0.7698(3) 0.04200(12) 0.0215(5) Uani 1 1 d . . . O3 O 0.36314(15) 0.1002(3) -0.06436(14) 0.0347(6) Uani 1 1 d . . . O4 O 0.42271(18) -0.2099(3) -0.07361(14) 0.0403(7) Uani 1 1 d . . . O5 O 1.22936(18) 0.8159(4) -0.13400(17) 0.0428(7) Uani 1 1 d D . . H51 H 1.194(2) 0.863(5) -0.103(3) 0.064 Uiso 1 1 d D . . H52 H 1.2840(15) 0.860(5) -0.114(3) 0.064 Uiso 1 1 d D . . O6 O 0.3056(4) 0.2999(8) -0.1883(3) 0.123(2) Uani 1 1 d D . . H61 H 0.328(6) 0.232(9) -0.142(3) 0.184 Uiso 1 1 d D . . H62 H 0.328(6) 0.265(11) -0.234(3) 0.184 Uiso 1 1 d D . . C1 C 1.15056(19) 0.8775(4) 0.04656(19) 0.0208(7) Uani 1 1 d . . . C2 C 1.2319(2) 0.7950(4) 0.0828(2) 0.0272(8) Uani 1 1 d . . . H2A H 1.2808 0.8520 0.0734 0.033 Uiso 1 1 calc R . . H2B H 1.2317 0.6907 0.0604 0.033 Uiso 1 1 calc R . . C3 C 1.2340(2) 0.7894(5) 0.1720(2) 0.0349(9) Uani 1 1 d . . . H3A H 1.2783 0.8576 0.2028 0.042 Uiso 1 1 calc R . . H3B H 1.2447 0.6839 0.1929 0.042 Uiso 1 1 calc R . . C4 C 1.1462(2) 0.8442(4) 0.17706(19) 0.0255(7) Uani 1 1 d . . . H4A H 1.1137 0.7589 0.1926 0.031 Uiso 1 1 calc R . . H4B H 1.1510 0.9271 0.2171 0.031 Uiso 1 1 calc R . . C5 C 0.93716(18) 0.7232(4) -0.02897(18) 0.0188(6) Uani 1 1 d . . . C6 C 0.8990(2) 0.5700(4) -0.0590(2) 0.0247(7) Uani 1 1 d . . . H6A H 0.8373 0.5700 -0.0649 0.030 Uiso 1 1 calc R . . H6B H 0.9245 0.4863 -0.0224 0.030 Uiso 1 1 calc R . . C7 C 0.9203(3) 0.5539(4) -0.1397(2) 0.0333(8) Uani 1 1 d . . . H7A H 0.8708 0.5181 -0.1809 0.040 Uiso 1 1 calc R . . H7B H 0.9672 0.4807 -0.1365 0.040 Uiso 1 1 calc R . . C8 C 0.9463(3) 0.7159(4) -0.1594(2) 0.0305(8) Uani 1 1 d . . . H8A H 0.9971 0.7122 -0.1810 0.037 Uiso 1 1 calc R . . H8B H 0.9002 0.7660 -0.1992 0.037 Uiso 1 1 calc R . . C9 C 0.3562(2) 0.1274(4) 0.00680(19) 0.0252(7) Uani 1 1 d . . . C10 C 0.2807(2) 0.2082(4) 0.0224(2) 0.0275(8) Uani 1 1 d . . . H10A H 0.2278 0.1569 -0.0055 0.033 Uiso 1 1 calc R . . H10B H 0.2788 0.3163 0.0049 0.033 Uiso 1 1 calc R . . C11 C 0.2942(2) 0.1969(4) 0.1143(2) 0.0283(8) Uani 1 1 d . . . H11A H 0.2871 0.2980 0.1376 0.034 Uiso 1 1 calc R . . H11B H 0.2541 0.1237 0.1286 0.034 Uiso 1 1 calc R . . C12 C 0.3855(2) 0.1396(4) 0.14349(19) 0.0279(8) Uani 1 1 d . . . H12A H 0.4223 0.2225 0.1714 0.034 Uiso 1 1 calc R . . H12B H 0.3882 0.0527 0.1808 0.034 Uiso 1 1 calc R . . C13 C 0.4307(2) -0.2722(4) -0.0050(2) 0.0273(8) Uani 1 1 d . . . C14 C 0.3917(2) -0.4251(4) 0.0033(2) 0.0300(8) Uani 1 1 d . . . H14A H 0.4119 -0.5041 -0.0287 0.036 Uiso 1 1 calc R . . H14B H 0.3295 -0.4198 -0.0137 0.036 Uiso 1 1 calc R . . C15 C 0.4212(3) -0.4584(5) 0.0922(2) 0.0327(8) Uani 1 1 d . . . H15A H 0.4624 -0.5434 0.1020 0.039 Uiso 1 1 calc R . . H15B H 0.3731 -0.4860 0.1147 0.039 Uiso 1 1 calc R . . C16 C 0.4626(2) -0.3087(4) 0.1296(2) 0.0296(8) Uani 1 1 d . . . H16A H 0.4273 -0.2585 0.1613 0.036 Uiso 1 1 calc R . . H16B H 0.5189 -0.3294 0.1649 0.036 Uiso 1 1 calc R . . C17 C 0.6053(3) 0.0082(5) 0.2714(2) 0.0374(11) Uani 1 1 d . . . C18 C 0.6490(3) 0.0270(7) 0.3556(3) 0.0553(14) Uani 1 1 d . . . H18A H 0.6197 0.1039 0.3802 0.083 Uiso 1 1 calc R . . H18B H 0.7070 0.0605 0.3595 0.083 Uiso 1 1 calc R . . H18C H 0.6496 -0.0708 0.3835 0.083 Uiso 1 1 calc R . . C19 C 0.9107(3) 0.9358(6) 0.2224(3) 0.0515(12) Uani 1 1 d . . . C20 C 0.8505(5) 0.9039(12) 0.2692(4) 0.126(4) Uani 1 1 d . . . H20A H 0.8017 0.8509 0.2359 0.189 Uiso 1 1 calc R . . H20B H 0.8322 1.0002 0.2887 0.189 Uiso 1 1 calc R . . H20C H 0.8768 0.8391 0.3148 0.189 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 0.01418(17) 0.02227(16) 0.01014(16) -0.00104(8) 0.00332(11) -0.00093(8) Rh2 0.02535(19) 0.03432(19) 0.00962(17) 0.00130(9) 0.00256(12) -0.01179(10) N1 0.0173(12) 0.0231(14) 0.0148(13) 0.0005(11) 0.0011(10) -0.0026(11) N2 0.0197(13) 0.0238(14) 0.0133(13) -0.0034(11) 0.0018(10) 0.0020(11) N3 0.0305(15) 0.0280(15) 0.0141(13) -0.0005(11) 0.0049(12) -0.0087(12) N4 0.0209(13) 0.0301(15) 0.0177(14) 0.0032(12) 0.0065(11) -0.0018(12) N5 0.0412(18) 0.0380(17) 0.0146(15) 0.0009(13) 0.0115(14) 0.0055(15) N6 0.0319(18) 0.051(2) 0.0158(18) 0.0000(12) 0.0036(15) -0.0089(13) O1 0.0180(11) 0.0342(13) 0.0219(12) 0.0016(10) 0.0082(9) 0.0022(10) O2 0.0212(11) 0.0275(12) 0.0161(11) -0.0017(9) 0.0054(9) -0.0065(9) O3 0.0239(12) 0.0646(19) 0.0147(12) 0.0035(12) 0.0030(10) -0.0110(12) O4 0.0524(17) 0.0482(17) 0.0163(12) 0.0009(12) 0.0005(11) -0.0297(14) O5 0.0351(15) 0.0590(19) 0.0370(16) -0.0066(14) 0.0140(13) 0.0054(14) O6 0.130(5) 0.148(5) 0.093(4) 0.029(4) 0.033(4) 0.051(4) C1 0.0140(14) 0.0219(16) 0.0249(17) -0.0010(14) 0.0019(13) -0.0047(13) C2 0.0167(15) 0.0262(18) 0.037(2) 0.0029(15) 0.0025(14) 0.0013(14) C3 0.0223(18) 0.040(2) 0.038(2) 0.0164(17) -0.0016(16) 0.0004(16) C4 0.0285(18) 0.0251(17) 0.0185(16) 0.0027(14) -0.0026(14) -0.0021(14) C5 0.0135(14) 0.0234(16) 0.0182(16) 0.0013(13) 0.0016(12) 0.0008(13) C6 0.0231(16) 0.0233(18) 0.0242(17) -0.0010(14) -0.0011(14) -0.0017(14) C7 0.047(2) 0.0249(19) 0.0265(19) -0.0044(16) 0.0063(17) -0.0011(17) C8 0.048(2) 0.0259(18) 0.0171(16) -0.0044(14) 0.0072(15) 0.0006(16) C9 0.0267(17) 0.0309(19) 0.0186(17) 0.0023(14) 0.0065(14) -0.0130(15) C10 0.0263(17) 0.0331(19) 0.0223(17) 0.0027(15) 0.0045(14) -0.0088(15) C11 0.0338(19) 0.0283(18) 0.0240(18) -0.0020(15) 0.0093(15) -0.0055(15) C12 0.041(2) 0.0275(18) 0.0157(16) 0.0003(14) 0.0069(15) -0.0049(16) C13 0.0261(17) 0.0327(19) 0.0241(18) 0.0004(15) 0.0084(14) -0.0069(15) C14 0.0292(18) 0.0291(19) 0.034(2) -0.0020(16) 0.0118(16) -0.0043(15) C15 0.034(2) 0.0304(19) 0.036(2) 0.0071(17) 0.0123(17) -0.0008(17) C16 0.0352(19) 0.0292(19) 0.0253(18) 0.0084(15) 0.0090(15) 0.0001(15) C17 0.028(2) 0.066(3) 0.018(2) -0.0025(16) 0.0055(18) 0.0081(17) C18 0.043(3) 0.096(4) 0.021(2) -0.016(2) -0.0035(19) 0.027(3) C19 0.063(3) 0.069(3) 0.026(2) 0.018(2) 0.017(2) 0.013(3) C20 0.105(6) 0.210(10) 0.085(5) 0.082(6) 0.069(5) 0.031(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N1 1.998(3) . ? Rh1 N2 2.006(3) 3_775 ? Rh1 O2 2.082(2) . ? Rh1 O1 2.083(2) 3_775 ? Rh1 N5 2.234(3) . ? Rh1 Rh1 2.4509(5) 3_775 ? Rh2 N3 2.006(3) . ? Rh2 N4 2.012(3) . ? Rh2 O4 2.074(3) 3_655 ? Rh2 O3 2.075(3) 3_655 ? Rh2 N6 2.231(3) . ? Rh2 Rh2 2.4558(5) 3_655 ? N1 C1 1.297(4) . ? N1 C4 1.464(4) . ? N2 C5 1.304(4) . ? N2 C8 1.458(4) . ? N2 Rh1 2.006(3) 3_775 ? N3 C9 1.304(4) . ? N3 C12 1.462(4) . ? N4 C13 1.300(4) . ? N4 C16 1.445(4) . ? N5 C19 1.115(6) . ? N6 C17 1.136(5) . ? O1 C1 1.283(4) . ? O1 Rh1 2.083(2) 3_775 ? O2 C5 1.277(4) . ? O3 C9 1.281(4) . ? O3 Rh2 2.075(3) 3_655 ? O4 C13 1.279(4) . ? O4 Rh2 2.074(3) 3_655 ? C1 C2 1.509(4) . ? C2 C3 1.529(5) . ? C3 C4 1.537(5) . ? C5 C6 1.516(5) . ? C6 C7 1.521(5) . ? C7 C8 1.540(5) . ? C9 C10 1.504(5) . ? C10 C11 1.547(5) . ? C11 C12 1.540(5) . ? C13 C14 1.503(5) . ? C14 C15 1.519(5) . ? C15 C16 1.541(5) . ? C17 C18 1.463(6) . ? C19 C20 1.444(7) . ? 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 N1 Rh1 N2 90.87(11) . 3_775 ? N1 Rh1 O2 89.02(10) . . ? N2 Rh1 O2 175.56(9) 3_775 . ? N1 Rh1 O1 175.42(9) . 3_775 ? N2 Rh1 O1 88.61(10) 3_775 3_775 ? O2 Rh1 O1 91.14(9) . 3_775 ? N1 Rh1 N5 98.43(11) . . ? N2 Rh1 N5 98.54(11) 3_775 . ? O2 Rh1 N5 85.86(10) . . ? O1 Rh1 N5 86.15(10) 3_775 . ? N1 Rh1 Rh1 85.56(7) . 3_775 ? N2 Rh1 Rh1 85.32(7) 3_775 3_775 ? O2 Rh1 Rh1 90.25(6) . 3_775 ? O1 Rh1 Rh1 89.86(6) 3_775 3_775 ? N5 Rh1 Rh1 174.36(9) . 3_775 ? N3 Rh2 N4 90.09(11) . . ? N3 Rh2 O4 90.31(12) . 3_655 ? N4 Rh2 O4 175.31(10) . 3_655 ? N3 Rh2 O3 175.23(10) . 3_655 ? N4 Rh2 O3 90.58(11) . 3_655 ? O4 Rh2 O3 88.64(12) 3_655 3_655 ? N3 Rh2 N6 95.96(12) . . ? N4 Rh2 N6 97.11(11) . . ? O4 Rh2 N6 87.50(10) 3_655 . ? O3 Rh2 N6 88.64(11) 3_655 . ? N3 Rh2 Rh2 85.37(8) . 3_655 ? N4 Rh2 Rh2 85.48(8) . 3_655 ? O4 Rh2 Rh2 89.89(7) 3_655 3_655 ? O3 Rh2 Rh2 89.98(6) 3_655 3_655 ? N6 Rh2 Rh2 177.08(9) . 3_655 ? C1 N1 C4 111.7(3) . . ? C1 N1 Rh1 123.8(2) . . ? C4 N1 Rh1 124.4(2) . . ? C5 N2 C8 111.9(3) . . ? C5 N2 Rh1 123.5(2) . 3_775 ? C8 N2 Rh1 124.3(2) . 3_775 ? C9 N3 C12 111.7(3) . . ? C9 N3 Rh2 123.7(2) . . ? C12 N3 Rh2 124.6(2) . . ? C13 N4 C16 111.7(3) . . ? C13 N4 Rh2 123.1(2) . . ? C16 N4 Rh2 124.9(2) . . ? C19 N5 Rh1 152.0(3) . . ? C17 N6 Rh2 169.3(3) . . ? C1 O1 Rh1 115.26(19) . 3_775 ? C5 O2 Rh1 115.1(2) . . ? C9 O3 Rh2 115.7(2) . 3_655 ? C13 O4 Rh2 115.8(2) . 3_655 ? O1 C1 N1 125.4(3) . . ? O1 C1 C2 121.5(3) . . ? N1 C1 C2 113.0(3) . . ? C1 C2 C3 103.5(3) . . ? C2 C3 C4 104.7(3) . . ? N1 C4 C3 106.1(3) . . ? O2 C5 N2 125.8(3) . . ? O2 C5 C6 121.9(3) . . ? N2 C5 C6 112.3(3) . . ? C5 C6 C7 103.1(3) . . ? C6 C7 C8 104.7(3) . . ? N2 C8 C7 105.1(3) . . ? O3 C9 N3 125.1(3) . . ? O3 C9 C10 121.8(3) . . ? N3 C9 C10 113.1(3) . . ? C9 C10 C11 103.5(3) . . ? C12 C11 C10 104.0(3) . . ? N3 C12 C11 106.3(3) . . ? O4 C13 N4 125.7(3) . . ? O4 C13 C14 121.1(3) . . ? N4 C13 C14 113.2(3) . . ? C13 C14 C15 103.1(3) . . ? C14 C15 C16 105.1(3) . . ? N4 C16 C15 105.7(3) . . ? N6 C17 C18 179.7(5) . . ? N5 C19 C20 179.0(6) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 66.26 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.922 _refine_diff_density_min -1.027 _refine_diff_density_rms 0.178