Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email DUNBAR@MAIL.CHEM.TAMU.EDU _publ_contact_author_name 'Prof Kim Dunbar' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_address ; Department of Chemistry Texas A&M University College Station TX 77843 UNITED STATES OF AMERICA ; _publ_section_title ; Structural Evidence for Monodentate Binding of Guanine to the Dirhodium(II,II) Core in a Manner Akin to that of Cisplatin ; loop_ _publ_author_name 'Kim Dunbar' 'Alfredo M. Angeles-Boza' 'Helen T. Chifotides' 'Jose-Ramon Galan-Mascaros' ; J.S.Hess ; 'Karn Sorasaenee' data_compound_1 _database_code_CSD 218354 _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety [Rh2(OAc)2(bpy)(9-EtGH)(H2O)2(CH3SO4)][CH3SO4](H2O) _chemical_formula_sum 'C23 H35 N7 O16 Rh2 S2' _chemical_formula_weight 935.52 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 7.9053(16) _cell_length_b 18.003(4) _cell_length_c 11.724(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.68(3) _cell_angle_gamma 90.00 _cell_volume 1667.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour green _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.863 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 944 _exptl_absorpt_coefficient_mu 1.198 _exptl_absorpt_correction_type multiscan _exptl_absorpt_correction_T_min 0.6862 _exptl_absorpt_correction_T_max 0.8223 _exptl_absorpt_process_details 'SADABS (Bruker, 2000)' _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 4.97 cm. Coverage of the unique set was over 98% complete to at least 27\% in \q. Crystal decay was monitored by repeating the initial 50 frames at the end of data collection and analyzing the duplicate reflections. Decay was found to be less than 1%, and no decay correction was therefore applied. ; _diffrn_ambient_temperature 103(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 'SMART CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14064 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0765 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 27.57 _reflns_number_total 7347 _reflns_number_gt 6394 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2000)' _computing_cell_refinement 'SAINT (Bruker, 2001)' _computing_data_reduction 'SAINT (Bruker, 2001)' _computing_structure_solution 'SIR97 (Giacovazzo et al, 1997)' _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^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(3) _refine_ls_number_reflns 7347 _refine_ls_number_parameters 480 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0437 _refine_ls_wR_factor_ref 0.0801 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.002 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 0.61709(5) 0.77347(2) 0.86246(3) 0.01095(10) Uani 1 1 d . . . Rh2 Rh 0.50491(5) 0.87804(2) 0.98015(3) 0.01069(10) Uani 1 1 d . . . S1 S 0.8301(2) 1.04328(9) 1.57065(14) 0.0232(3) Uani 1 1 d . . . S2 S 0.26344(18) 0.98981(8) 1.15075(12) 0.0149(3) Uani 1 1 d . . . O1 O 0.7238(5) 0.9310(2) 0.9501(3) 0.0146(9) Uani 1 1 d . . . O2 O 0.8272(5) 0.8386(2) 0.8442(3) 0.0153(9) Uani 1 1 d . . . O3 O 0.4126(5) 0.9205(2) 0.8298(3) 0.0156(9) Uani 1 1 d . . . O4 O 0.5161(5) 0.8277(2) 0.7240(3) 0.0159(9) Uani 1 1 d . . . O5 O 0.4000(5) 0.9846(2) 1.0701(3) 0.0150(9) Uani 1 1 d . . . O6 O 0.3056(5) 0.7312(2) 1.1549(3) 0.0141(8) Uani 1 1 d . . . O7 O 0.1241(5) 0.9385(2) 1.1256(4) 0.0190(9) Uani 1 1 d . . . O8 O 0.2088(5) 1.0654(2) 1.1677(4) 0.0209(9) Uani 1 1 d . . . O9 O 0.3364(5) 0.9600(2) 1.2701(3) 0.0214(9) Uani 1 1 d . . . O10 O 1.0262(5) 1.0319(2) 1.5464(4) 0.0256(10) Uani 1 1 d . . . O11 O 0.8246(6) 1.0980(3) 1.6613(4) 0.0316(11) Uani 1 1 d . . . O12 O 0.7794(7) 0.9703(3) 1.6026(4) 0.0393(13) Uani 1 1 d . . . O13 O 0.7522(6) 1.0704(3) 1.4644(4) 0.0374(12) Uani 1 1 d . . . O1W O 0.2694(5) 0.8307(2) 1.0002(3) 0.0130(9) Uani 1 1 d D . . O2W O 0.7132(5) 0.6948(2) 0.7303(4) 0.0157(9) Uani 1 1 d D . . O3W O 0.8990(5) 0.7867(2) 0.6132(4) 0.0256(10) Uani 1 1 d D . . N1 N 0.4110(6) 0.7136(3) 1.3346(4) 0.0147(10) Uani 1 1 d . . . H1 H 0.3316 0.6801 1.3441 0.018 Uiso 1 1 calc R . . N1A N 0.7059(6) 0.7121(2) 0.9934(4) 0.0093(10) Uani 1 1 d . . . N1A' N 0.4219(6) 0.7035(3) 0.8785(4) 0.0132(10) Uani 1 1 d . . . N2 N 0.4900(6) 0.6904(3) 1.5218(4) 0.0218(12) Uani 1 1 d . . . H2'B H 0.5549 0.6978 1.5830 0.026 Uiso 1 1 calc R . . H2B H 0.4050 0.6590 1.5241 0.026 Uiso 1 1 calc R . . N3 N 0.6488(5) 0.7744(3) 1.4218(4) 0.0163(9) Uani 1 1 d . . . N7 N 0.6036(6) 0.8472(3) 1.1361(4) 0.0121(11) Uani 1 1 d . . . N9 N 0.7755(6) 0.8593(2) 1.2899(4) 0.0147(11) Uani 1 1 d . . . C1A C 0.8603(7) 0.7196(3) 1.0465(5) 0.0143(12) Uani 1 1 d . . . H1A H 0.9349 0.7570 1.0206 0.017 Uiso 1 1 calc R . . C1A' C 0.2826(7) 0.7024(3) 0.8100(5) 0.0202(13) Uani 1 1 d . . . H1A' H 0.2689 0.7396 0.7529 0.024 Uiso 1 1 calc R . . C2 C 0.5204(7) 0.7268(3) 1.4257(5) 0.0149(12) Uani 1 1 d . . . C2A C 0.9124(7) 0.6752(3) 1.1361(5) 0.0187(13) Uani 1 1 d . . . H2A H 1.0201 0.6820 1.1726 0.022 Uiso 1 1 calc R . . C2A' C 0.1604(8) 0.6496(3) 0.8199(6) 0.0241(15) Uani 1 1 d . . . H2A' H 0.0643 0.6494 0.7693 0.029 Uiso 1 1 calc R . . C3A C 0.8032(8) 0.6201(3) 1.1717(5) 0.0184(13) Uani 1 1 d . . . H3A H 0.8363 0.5887 1.2335 0.022 Uiso 1 1 calc R . . C3A' C 0.1780(8) 0.5960(3) 0.9050(5) 0.0216(14) Uani 1 1 d . . . H3A' H 0.0938 0.5590 0.9140 0.026 Uiso 1 1 calc R . . C4 C 0.6569(7) 0.8079(3) 1.3182(5) 0.0132(12) Uani 1 1 d . . . C4A C 0.6472(7) 0.6106(3) 1.1182(5) 0.0138(12) Uani 1 1 d . . . H4A H 0.5725 0.5728 1.1425 0.017 Uiso 1 1 calc R . . C4A' C 0.3213(7) 0.5977(3) 0.9765(5) 0.0168(12) Uani 1 1 d . . . H4A' H 0.3365 0.5621 1.0356 0.020 Uiso 1 1 calc R . . C5 C 0.5491(7) 0.7999(3) 1.2235(5) 0.0137(12) Uani 1 1 d . . . C5A C 0.6012(7) 0.6572(3) 1.0282(5) 0.0164(13) Uani 1 1 d . . . C5A' C 0.4404(7) 0.6518(3) 0.9603(4) 0.0089(11) Uani 1 1 d . . . C6 C 0.4147(7) 0.7481(3) 1.2298(5) 0.0152(12) Uani 1 1 d . . . C8 C 0.7391(6) 0.8801(4) 1.1810(4) 0.0145(10) Uani 1 1 d . . . H8 H 0.8049 0.9150 1.1407 0.017 Uiso 1 1 calc R . . C9 C 0.9220(7) 0.8846(3) 1.3607(4) 0.0179(12) Uani 1 1 d . . . H9A H 0.8862 0.8925 1.4400 0.021 Uiso 1 1 calc R . . H9B H 0.9631 0.9326 1.3311 0.021 Uiso 1 1 calc R . . C10 C 1.0648(8) 0.8282(4) 1.3605(5) 0.0241(15) Uani 1 1 d . . . H10A H 1.0988 0.8195 1.2819 0.036 Uiso 1 1 calc R . . H10B H 1.0261 0.7814 1.3936 0.036 Uiso 1 1 calc R . . H10C H 1.1615 0.8472 1.4057 0.036 Uiso 1 1 calc R . . C11 C 0.8353(7) 0.9032(3) 0.8841(5) 0.0142(12) Uani 1 1 d . . . C12 C 0.9820(7) 0.9508(3) 0.8551(5) 0.0210(13) Uani 1 1 d . . . H12A H 0.9554 0.9783 0.7847 0.032 Uiso 1 1 calc R . . H12B H 1.0816 0.9195 0.8441 0.032 Uiso 1 1 calc R . . H12C H 1.0057 0.9859 0.9174 0.032 Uiso 1 1 calc R . . C13 C 0.4379(7) 0.8889(3) 0.7356(5) 0.0188(13) Uani 1 1 d . . . C14 C 0.3705(8) 0.9261(4) 0.6284(5) 0.0254(15) Uani 1 1 d . . . H14A H 0.4033 0.8972 0.5617 0.038 Uiso 1 1 calc R . . H14B H 0.4176 0.9763 0.6235 0.038 Uiso 1 1 calc R . . H14C H 0.2468 0.9290 0.6302 0.038 Uiso 1 1 calc R . . C15 C 0.4784(8) 1.0021(4) 1.3203(5) 0.0276(15) Uani 1 1 d . . . H15A H 0.4392 1.0514 1.3429 0.041 Uiso 1 1 calc R . . H15B H 0.5670 1.0073 1.2640 0.041 Uiso 1 1 calc R . . H15C H 0.5242 0.9758 1.3875 0.041 Uiso 1 1 calc R . . C16 C 1.1089(10) 1.0940(4) 1.5006(7) 0.048(2) Uani 1 1 d . . . H16A H 1.0831 1.1382 1.5455 0.072 Uiso 1 1 calc R . . H16B H 1.0698 1.1015 1.4213 0.072 Uiso 1 1 calc R . . H16C H 1.2314 1.0854 1.5030 0.072 Uiso 1 1 calc R . . H1WA H 0.296(7) 0.7882(19) 1.048(4) 0.017(17) Uiso 1 1 d D . . H1WB H 0.198(7) 0.865(3) 1.039(4) 0.05(2) Uiso 1 1 d D . . H2WA H 0.812(7) 0.719(4) 0.700(9) 0.13(4) Uiso 1 1 d D . . H2WB H 0.740(8) 0.6474(19) 0.762(5) 0.03(2) Uiso 1 1 d D . . H3WA H 0.877(9) 0.830(3) 0.658(4) 0.06(3) Uiso 1 1 d D . . H3WB H 0.832(6) 0.787(3) 0.544(3) 0.010(15) 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 0.0101(2) 0.0109(2) 0.0118(2) 0.00075(19) -0.00048(16) 0.0001(2) Rh2 0.0094(2) 0.0106(2) 0.0121(2) 0.0020(2) 0.00063(16) 0.0005(2) S1 0.0170(8) 0.0269(9) 0.0256(8) -0.0100(7) -0.0032(6) 0.0055(7) S2 0.0145(8) 0.0131(7) 0.0172(7) -0.0002(6) 0.0029(6) 0.0002(6) O1 0.014(2) 0.0089(19) 0.021(2) 0.0034(16) 0.0008(17) -0.0007(16) O2 0.014(2) 0.009(2) 0.023(2) 0.0015(18) 0.0001(18) -0.0010(16) O3 0.016(2) 0.020(2) 0.011(2) 0.0021(17) 0.0018(16) 0.0028(18) O4 0.019(2) 0.017(2) 0.012(2) 0.0017(17) -0.0009(17) -0.0014(17) O5 0.013(2) 0.013(2) 0.020(2) 0.0031(17) 0.0050(16) -0.0004(18) O6 0.014(2) 0.012(2) 0.016(2) -0.0014(16) -0.0035(16) -0.0050(17) O7 0.012(2) 0.018(2) 0.027(2) -0.0043(18) 0.0005(17) 0.0016(17) O8 0.020(2) 0.012(2) 0.030(2) -0.0032(18) -0.0027(19) 0.0049(17) O9 0.024(2) 0.021(2) 0.019(2) 0.0040(18) 0.0006(18) -0.0042(18) O10 0.017(3) 0.025(2) 0.034(3) -0.001(2) 0.0012(19) 0.0033(18) O11 0.025(3) 0.044(3) 0.026(3) -0.013(2) -0.004(2) 0.012(2) O12 0.043(3) 0.035(3) 0.040(3) -0.005(2) 0.011(2) -0.008(2) O13 0.038(3) 0.046(3) 0.027(3) -0.011(2) -0.011(2) 0.020(2) O1W 0.009(2) 0.014(2) 0.016(2) 0.0004(17) 0.0005(16) 0.0030(16) O2W 0.016(2) 0.011(2) 0.020(2) 0.0032(17) -0.0009(17) 0.0046(17) O3W 0.027(2) 0.026(3) 0.023(2) -0.001(2) 0.0036(19) -0.001(2) N1 0.012(2) 0.015(3) 0.017(3) 0.003(2) -0.0035(19) -0.004(2) N1A 0.010(2) 0.005(2) 0.013(2) -0.0008(19) -0.0011(19) -0.0043(18) N1A' 0.013(2) 0.011(2) 0.015(3) -0.001(2) 0.0025(19) -0.0006(19) N2 0.025(3) 0.026(3) 0.014(3) 0.008(2) -0.004(2) -0.014(2) N3 0.018(2) 0.016(2) 0.015(2) 0.004(2) -0.0024(18) 0.002(2) N7 0.014(3) 0.009(2) 0.014(3) 0.0001(19) 0.000(2) 0.004(2) N9 0.017(3) 0.013(3) 0.014(2) -0.0016(19) 0.0001(19) -0.0031(19) C1A 0.011(3) 0.014(3) 0.018(3) 0.000(2) 0.001(2) 0.000(2) C1A' 0.018(3) 0.024(3) 0.019(3) -0.005(3) 0.001(2) 0.001(3) C2 0.013(3) 0.014(3) 0.018(3) 0.001(2) -0.005(2) 0.007(2) C2A 0.017(3) 0.022(3) 0.017(3) -0.004(3) -0.005(2) 0.000(2) C2A' 0.011(3) 0.030(4) 0.031(4) -0.008(3) -0.005(3) 0.002(3) C3A 0.026(3) 0.016(3) 0.012(3) -0.003(2) -0.004(3) 0.007(3) C3A' 0.021(3) 0.010(3) 0.034(4) -0.003(3) 0.003(3) -0.004(2) C4 0.010(3) 0.011(3) 0.019(3) -0.001(2) 0.004(2) 0.003(2) C4A 0.021(3) 0.010(3) 0.011(3) -0.005(2) 0.009(2) -0.002(2) C4A' 0.017(3) 0.016(3) 0.017(3) -0.002(2) 0.001(2) 0.002(2) C5 0.011(3) 0.012(3) 0.018(3) -0.001(2) 0.003(2) 0.002(2) C5A 0.011(3) 0.023(3) 0.015(3) -0.007(3) 0.002(2) 0.002(2) C5A' 0.010(3) 0.009(3) 0.008(3) -0.003(2) 0.001(2) -0.004(2) C6 0.014(3) 0.014(3) 0.018(3) 0.000(2) 0.003(2) 0.000(2) C8 0.014(3) 0.012(3) 0.017(3) 0.000(3) 0.003(2) 0.003(3) C9 0.023(3) 0.019(3) 0.012(3) 0.001(3) 0.000(2) -0.003(3) C10 0.025(4) 0.032(4) 0.015(3) -0.001(3) -0.002(3) -0.001(3) C11 0.017(3) 0.013(3) 0.013(3) 0.009(2) 0.000(2) 0.003(2) C12 0.013(3) 0.024(3) 0.026(3) 0.001(3) 0.009(2) -0.004(2) C13 0.018(3) 0.023(4) 0.015(3) 0.003(3) 0.002(2) -0.007(3) C14 0.032(4) 0.028(4) 0.016(3) 0.000(3) 0.005(3) 0.004(3) C15 0.028(4) 0.029(4) 0.026(3) -0.007(3) -0.003(3) 0.003(3) C16 0.045(5) 0.048(5) 0.050(5) 0.023(4) 0.006(4) -0.014(4) _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 N1A 2.001(5) . ? Rh1 N1A' 2.005(5) . ? Rh1 O4 2.038(4) . ? Rh1 O2 2.050(4) . ? Rh1 O2W 2.248(4) . ? Rh1 Rh2 2.5112(7) . ? Rh2 O1 2.015(4) . ? Rh2 O3 2.037(4) . ? Rh2 N7 2.043(5) . ? Rh2 O1W 2.067(4) . ? Rh2 O5 2.351(4) . ? S1 O12 1.427(5) . ? S1 O11 1.451(5) . ? S1 O13 1.457(5) . ? S1 O10 1.598(5) . ? S2 O8 1.443(4) . ? S2 O5 1.459(4) . ? S2 O7 1.461(4) . ? S2 O9 1.591(4) . ? O1 C11 1.291(7) . ? O2 C11 1.254(7) . ? O3 C13 1.264(7) . ? O4 C13 1.271(7) . ? O6 C6 1.251(6) . ? O9 C15 1.464(7) . ? O10 C16 1.410(8) . ? O1W H1WA 0.969(19) . ? O1W H1WB 0.959(19) . ? O2W H2WA 0.97(2) . ? O2W H2WB 0.952(19) . ? O3W H3WA 0.964(19) . ? O3W H3WB 0.954(19) . ? N1 C2 1.375(7) . ? N1 C6 1.378(7) . ? N1 H1 0.8800 . ? N1A C5A 1.359(7) . ? N1A C1A 1.361(7) . ? N1A' C5A' 1.340(7) . ? N1A' C1A' 1.344(7) . ? N2 C2 1.332(7) . ? N2 H2'B 0.8800 . ? N2 H2B 0.8800 . ? N3 C2 1.330(7) . ? N3 C4 1.359(7) . ? N7 C8 1.320(7) . ? N7 C5 1.410(7) . ? N9 C8 1.353(7) . ? N9 C4 1.365(7) . ? N9 C9 1.477(7) . ? C1A C2A 1.374(8) . ? C1A H1A 0.9500 . ? C1A' C2A' 1.362(9) . ? C1A' H1A' 0.9500 . ? C2A C3A 1.387(9) . ? C2A H2A 0.9500 . ? C2A' C3A' 1.393(8) . ? C2A' H2A' 0.9500 . ? C3A C4A 1.378(8) . ? C3A H3A 0.9500 . ? C3A' C4A' 1.390(8) . ? C3A' H3A' 0.9500 . ? C4 C5 1.387(8) . ? C4A C5A 1.389(8) . ? C4A H4A 0.9500 . ? C4A' C5A' 1.372(8) . ? C4A' H4A' 0.9500 . ? C5 C6 1.416(8) . ? C5A C5A' 1.483(8) . ? C8 H8 0.9500 . ? C9 C10 1.518(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.490(8) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.508(8) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A Rh1 N1A' 80.50(19) . . ? N1A Rh1 O4 174.95(17) . . ? N1A' Rh1 O4 95.23(17) . . ? N1A Rh1 O2 97.39(17) . . ? N1A' Rh1 O2 175.96(18) . . ? O4 Rh1 O2 86.71(16) . . ? N1A Rh1 O2W 93.62(17) . . ? N1A' Rh1 O2W 86.85(17) . . ? O4 Rh1 O2W 83.42(15) . . ? O2 Rh1 O2W 89.85(16) . . ? N1A Rh1 Rh2 96.53(13) . . ? N1A' Rh1 Rh2 97.74(13) . . ? O4 Rh1 Rh2 86.67(11) . . ? O2 Rh1 Rh2 85.91(12) . . ? O2W Rh1 Rh2 169.43(10) . . ? O1 Rh2 O3 87.63(16) . . ? O1 Rh2 N7 88.73(18) . . ? O3 Rh2 N7 173.67(19) . . ? O1 Rh2 O1W 174.54(16) . . ? O3 Rh2 O1W 87.25(16) . . ? N7 Rh2 O1W 96.19(17) . . ? O1 Rh2 O5 90.48(15) . . ? O3 Rh2 O5 87.68(15) . . ? N7 Rh2 O5 87.17(16) . . ? O1W Rh2 O5 87.41(14) . . ? O1 Rh2 Rh1 86.55(11) . . ? O3 Rh2 Rh1 85.95(12) . . ? N7 Rh2 Rh1 99.00(13) . . ? O1W Rh2 Rh1 94.99(11) . . ? O5 Rh2 Rh1 173.08(9) . . ? O12 S1 O11 114.7(3) . . ? O12 S1 O13 114.7(3) . . ? O11 S1 O13 112.2(3) . . ? O12 S1 O10 102.1(3) . . ? O11 S1 O10 105.5(3) . . ? O13 S1 O10 106.2(3) . . ? O8 S2 O5 112.3(3) . . ? O8 S2 O7 113.4(2) . . ? O5 S2 O7 113.3(2) . . ? O8 S2 O9 107.4(2) . . ? O5 S2 O9 107.0(2) . . ? O7 S2 O9 102.5(2) . . ? C11 O1 Rh2 121.7(4) . . ? C11 O2 Rh1 121.6(4) . . ? C13 O3 Rh2 121.7(4) . . ? C13 O4 Rh1 120.7(3) . . ? S2 O5 Rh2 128.4(2) . . ? C15 O9 S2 115.6(4) . . ? C16 O10 S1 115.4(5) . . ? Rh2 O1W H1WA 102(3) . . ? Rh2 O1W H1WB 109(4) . . ? H1WA O1W H1WB 111(3) . . ? Rh1 O2W H2WA 105(6) . . ? Rh1 O2W H2WB 112(4) . . ? H2WA O2W H2WB 112(3) . . ? H3WA O3W H3WB 111(3) . . ? C2 N1 C6 125.8(5) . . ? C2 N1 H1 117.1 . . ? C6 N1 H1 117.1 . . ? C5A N1A C1A 118.7(5) . . ? C5A N1A Rh1 115.4(4) . . ? C1A N1A Rh1 125.9(4) . . ? C5A' N1A' C1A' 119.2(5) . . ? C5A' N1A' Rh1 115.8(4) . . ? C1A' N1A' Rh1 124.9(4) . . ? C2 N2 H2'B 120.0 . . ? C2 N2 H2B 120.0 . . ? H2'B N2 H2B 120.0 . . ? C2 N3 C4 111.9(5) . . ? C8 N7 C5 104.0(5) . . ? C8 N7 Rh2 121.3(4) . . ? C5 N7 Rh2 134.3(4) . . ? C8 N9 C4 106.7(5) . . ? C8 N9 C9 125.9(5) . . ? C4 N9 C9 127.2(5) . . ? N1A C1A C2A 122.5(5) . . ? N1A C1A H1A 118.8 . . ? C2A C1A H1A 118.8 . . ? N1A' C1A' C2A' 122.0(6) . . ? N1A' C1A' H1A' 119.0 . . ? C2A' C1A' H1A' 119.0 . . ? N3 C2 N2 120.2(5) . . ? N3 C2 N1 123.2(5) . . ? N2 C2 N1 116.6(5) . . ? C1A C2A C3A 118.1(5) . . ? C1A C2A H2A 120.9 . . ? C3A C2A H2A 120.9 . . ? C1A' C2A' C3A' 119.3(6) . . ? C1A' C2A' H2A' 120.4 . . ? C3A' C2A' H2A' 120.4 . . ? C4A C3A C2A 120.6(5) . . ? C4A C3A H3A 119.7 . . ? C2A C3A H3A 119.7 . . ? C4A' C3A' C2A' 118.6(6) . . ? C4A' C3A' H3A' 120.7 . . ? C2A' C3A' H3A' 120.7 . . ? N3 C4 N9 124.6(5) . . ? N3 C4 C5 128.7(5) . . ? N9 C4 C5 106.7(5) . . ? C3A C4A C5A 118.8(5) . . ? C3A C4A H4A 120.6 . . ? C5A C4A H4A 120.6 . . ? C5A' C4A' C3A' 118.9(5) . . ? C5A' C4A' H4A' 120.6 . . ? C3A' C4A' H4A' 120.6 . . ? C4 C5 N7 109.0(5) . . ? C4 C5 C6 118.1(5) . . ? N7 C5 C6 132.9(5) . . ? N1A C5A C4A 121.3(5) . . ? N1A C5A C5A' 113.9(5) . . ? C4A C5A C5A' 124.7(5) . . ? N1A' C5A' C4A' 122.0(5) . . ? N1A' C5A' C5A 114.4(5) . . ? C4A' C5A' C5A 123.6(5) . . ? O6 C6 N1 118.9(5) . . ? O6 C6 C5 128.8(5) . . ? N1 C6 C5 112.3(5) . . ? N7 C8 N9 113.6(5) . . ? N7 C8 H8 123.2 . . ? N9 C8 H8 123.2 . . ? N9 C9 C10 111.3(5) . . ? N9 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N9 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O2 C11 O1 123.7(5) . . ? O2 C11 C12 118.7(5) . . ? O1 C11 C12 117.6(5) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 O4 125.0(5) . . ? O3 C13 C14 117.8(5) . . ? O4 C13 C14 117.2(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O9 C15 H15A 109.5 . . ? O9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O10 C16 H16A 109.5 . . ? O10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1A Rh1 Rh2 O1 96.86(17) . . . . ? N1A' Rh1 Rh2 O1 178.11(19) . . . . ? O4 Rh1 Rh2 O1 -87.06(16) . . . . ? O2 Rh1 Rh2 O1 -0.13(16) . . . . ? O2W Rh1 Rh2 O1 -66.7(6) . . . . ? N1A Rh1 Rh2 O3 -175.27(19) . . . . ? N1A' Rh1 Rh2 O3 -94.02(18) . . . . ? O4 Rh1 Rh2 O3 0.81(16) . . . . ? O2 Rh1 Rh2 O3 87.74(16) . . . . ? O2W Rh1 Rh2 O3 21.2(6) . . . . ? N1A Rh1 Rh2 N7 8.70(19) . . . . ? N1A' Rh1 Rh2 N7 89.9(2) . . . . ? O4 Rh1 Rh2 N7 -175.22(19) . . . . ? O2 Rh1 Rh2 N7 -88.29(18) . . . . ? O2W Rh1 Rh2 N7 -154.8(6) . . . . ? N1A Rh1 Rh2 O1W -88.39(17) . . . . ? N1A' Rh1 Rh2 O1W -7.14(17) . . . . ? O4 Rh1 Rh2 O1W 87.69(16) . . . . ? O2 Rh1 Rh2 O1W 174.62(17) . . . . ? O2W Rh1 Rh2 O1W 108.1(6) . . . . ? N1A Rh1 Rh2 O5 161.5(8) . . . . ? N1A' Rh1 Rh2 O5 -117.2(8) . . . . ? O4 Rh1 Rh2 O5 -22.4(8) . . . . ? O2 Rh1 Rh2 O5 64.6(8) . . . . ? O2W Rh1 Rh2 O5 -2.0(10) . . . . ? O3 Rh2 O1 C11 -82.1(4) . . . . ? N7 Rh2 O1 C11 103.1(4) . . . . ? O1W Rh2 O1 C11 -102.5(18) . . . . ? O5 Rh2 O1 C11 -169.7(4) . . . . ? Rh1 Rh2 O1 C11 4.0(4) . . . . ? N1A Rh1 O2 C11 -99.9(4) . . . . ? N1A' Rh1 O2 C11 -158(2) . . . . ? O4 Rh1 O2 C11 83.1(4) . . . . ? O2W Rh1 O2 C11 166.5(4) . . . . ? Rh2 Rh1 O2 C11 -3.8(4) . . . . ? O1 Rh2 O3 C13 84.8(4) . . . . ? N7 Rh2 O3 C13 139.8(16) . . . . ? O1W Rh2 O3 C13 -97.1(4) . . . . ? O5 Rh2 O3 C13 175.4(4) . . . . ? Rh1 Rh2 O3 C13 -1.9(4) . . . . ? N1A Rh1 O4 C13 129(2) . . . . ? N1A' Rh1 O4 C13 97.4(4) . . . . ? O2 Rh1 O4 C13 -86.2(4) . . . . ? O2W Rh1 O4 C13 -176.4(4) . . . . ? Rh2 Rh1 O4 C13 -0.1(4) . . . . ? O8 S2 O5 Rh2 -166.7(3) . . . . ? O7 S2 O5 Rh2 -36.5(4) . . . . ? O9 S2 O5 Rh2 75.6(3) . . . . ? O1 Rh2 O5 S2 -159.2(3) . . . . ? O3 Rh2 O5 S2 113.2(3) . . . . ? N7 Rh2 O5 S2 -70.5(3) . . . . ? O1W Rh2 O5 S2 25.8(3) . . . . ? Rh1 Rh2 O5 S2 136.3(6) . . . . ? O8 S2 O9 C15 -58.9(5) . . . . ? O5 S2 O9 C15 61.9(4) . . . . ? O7 S2 O9 C15 -178.6(4) . . . . ? O12 S1 O10 C16 173.5(5) . . . . ? O11 S1 O10 C16 -66.3(5) . . . . ? O13 S1 O10 C16 53.0(5) . . . . ? N1A' Rh1 N1A C5A -0.2(4) . . . . ? O4 Rh1 N1A C5A -32(2) . . . . ? O2 Rh1 N1A C5A -176.7(4) . . . . ? O2W Rh1 N1A C5A -86.4(4) . . . . ? Rh2 Rh1 N1A C5A 96.6(4) . . . . ? N1A' Rh1 N1A C1A 177.9(5) . . . . ? O4 Rh1 N1A C1A 145.6(19) . . . . ? O2 Rh1 N1A C1A 1.4(5) . . . . ? O2W Rh1 N1A C1A 91.7(5) . . . . ? Rh2 Rh1 N1A C1A -85.3(4) . . . . ? N1A Rh1 N1A' C5A' -1.1(4) . . . . ? O4 Rh1 N1A' C5A' 176.2(4) . . . . ? O2 Rh1 N1A' C5A' 58(3) . . . . ? O2W Rh1 N1A' C5A' 93.1(4) . . . . ? Rh2 Rh1 N1A' C5A' -96.5(4) . . . . ? N1A Rh1 N1A' C1A' -177.1(5) . . . . ? O4 Rh1 N1A' C1A' 0.2(5) . . . . ? O2 Rh1 N1A' C1A' -118(3) . . . . ? O2W Rh1 N1A' C1A' -82.9(5) . . . . ? Rh2 Rh1 N1A' C1A' 87.6(4) . . . . ? O1 Rh2 N7 C8 15.9(4) . . . . ? O3 Rh2 N7 C8 -39.0(19) . . . . ? O1W Rh2 N7 C8 -161.7(4) . . . . ? O5 Rh2 N7 C8 -74.7(4) . . . . ? Rh1 Rh2 N7 C8 102.2(4) . . . . ? O1 Rh2 N7 C5 -172.9(5) . . . . ? O3 Rh2 N7 C5 132.2(16) . . . . ? O1W Rh2 N7 C5 9.5(5) . . . . ? O5 Rh2 N7 C5 96.6(5) . . . . ? Rh1 Rh2 N7 C5 -86.6(5) . . . . ? C5A N1A C1A C2A -2.0(8) . . . . ? Rh1 N1A C1A C2A -180.0(4) . . . . ? C5A' N1A' C1A' C2A' -1.1(8) . . . . ? Rh1 N1A' C1A' C2A' 174.7(4) . . . . ? C4 N3 C2 N2 -178.0(5) . . . . ? C4 N3 C2 N1 0.4(8) . . . . ? C6 N1 C2 N3 -1.9(9) . . . . ? C6 N1 C2 N2 176.5(5) . . . . ? N1A C1A C2A C3A 1.0(9) . . . . ? N1A' C1A' C2A' C3A' 1.4(9) . . . . ? C1A C2A C3A C4A 0.0(9) . . . . ? C1A' C2A' C3A' C4A' -0.6(9) . . . . ? C2 N3 C4 N9 179.9(5) . . . . ? C2 N3 C4 C5 2.1(8) . . . . ? C8 N9 C4 N3 -179.0(5) . . . . ? C9 N9 C4 N3 4.5(9) . . . . ? C8 N9 C4 C5 -0.7(6) . . . . ? C9 N9 C4 C5 -177.3(5) . . . . ? C2A C3A C4A C5A -0.1(8) . . . . ? C2A' C3A' C4A' C5A' -0.4(8) . . . . ? N3 C4 C5 N7 178.2(5) . . . . ? N9 C4 C5 N7 0.1(6) . . . . ? N3 C4 C5 C6 -2.9(9) . . . . ? N9 C4 C5 C6 178.9(5) . . . . ? C8 N7 C5 C4 0.6(6) . . . . ? Rh2 N7 C5 C4 -171.7(4) . . . . ? C8 N7 C5 C6 -178.0(6) . . . . ? Rh2 N7 C5 C6 9.7(9) . . . . ? C1A N1A C5A C4A 1.8(8) . . . . ? Rh1 N1A C5A C4A -180.0(4) . . . . ? C1A N1A C5A C5A' -176.9(5) . . . . ? Rh1 N1A C5A C5A' 1.3(6) . . . . ? C3A C4A C5A N1A -0.8(8) . . . . ? C3A C4A C5A C5A' 177.8(5) . . . . ? C1A' N1A' C5A' C4A' 0.0(8) . . . . ? Rh1 N1A' C5A' C4A' -176.2(4) . . . . ? C1A' N1A' C5A' C5A 178.3(5) . . . . ? Rh1 N1A' C5A' C5A 2.1(6) . . . . ? C3A' C4A' C5A' N1A' 0.7(8) . . . . ? C3A' C4A' C5A' C5A -177.4(5) . . . . ? N1A C5A C5A' N1A' -2.2(7) . . . . ? C4A C5A C5A' N1A' 179.1(5) . . . . ? N1A C5A C5A' C4A' 176.1(5) . . . . ? C4A C5A C5A' C4A' -2.7(9) . . . . ? C2 N1 C6 O6 -179.2(5) . . . . ? C2 N1 C6 C5 1.0(8) . . . . ? C4 C5 C6 O6 -178.6(5) . . . . ? N7 C5 C6 O6 -0.2(10) . . . . ? C4 C5 C6 N1 1.1(7) . . . . ? N7 C5 C6 N1 179.6(5) . . . . ? C5 N7 C8 N9 -1.1(6) . . . . ? Rh2 N7 C8 N9 172.5(4) . . . . ? C4 N9 C8 N7 1.2(6) . . . . ? C9 N9 C8 N7 177.8(5) . . . . ? C8 N9 C9 C10 -98.1(6) . . . . ? C4 N9 C9 C10 77.8(7) . . . . ? Rh1 O2 C11 O1 8.3(7) . . . . ? Rh1 O2 C11 C12 -172.3(4) . . . . ? Rh2 O1 C11 O2 -8.4(7) . . . . ? Rh2 O1 C11 C12 172.1(4) . . . . ? Rh2 O3 C13 O4 2.5(8) . . . . ? Rh2 O3 C13 C14 -177.6(4) . . . . ? Rh1 O4 C13 O3 -1.4(8) . . . . ? Rh1 O4 C13 C14 178.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2'B O2W 0.88 2.10 2.974(6) 169.8 1_556 N2 H2B O13 0.88 2.03 2.894(7) 168.0 2_648 O2W H2WA O3W 0.97(2) 1.75(4) 2.626(6) 149(7) . O2W H2WB O8 0.952(19) 1.73(2) 2.683(5) 175(6) 2_647 O3W H3WB N3 0.954(19) 2.02(2) 2.957(6) 166(5) 1_554 O3W H3WA O2 0.964(19) 2.23(5) 2.936(6) 129(5) . O1W H1WB O7 0.959(19) 1.78(3) 2.711(6) 163(6) . O1W H1WA O6 0.969(19) 1.62(3) 2.560(5) 163(4) . _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.57 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.261 _refine_diff_density_min -0.844 _refine_diff_density_rms 0.128