Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_cc _database_code_CSD 192036 _journal_coden_Cambridge 182 loop_ _publ_author_name 'Kim R. Dunbar' 'Jitendra K. Bera' 'Cristian Saul Campos-Fernandez' _publ_contact_author_name 'Dr Kim R. Dunbar' _publ_contact_author_address ; Department of Chemistry Texas A & M University College Station Texas TX77842-3012 UNITED STATES OF AMERICA ; _publ_contact_author_email 'DUNBAR@MAIL.CHEM.TAMU.EDU' _publ_requested_journal 'Chemical Communications' _publ_section_title ; Coupling Dirhodium Units Through Terpyridine Bridges: Synthesis and Structure of a Novel Molecular Rectangle ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H59 F24 N12 O10 P4 Rh4' _chemical_formula_weight 2075.64 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' 'B' 'B' 0.0013 0.0007 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 15.604(5) _cell_length_b 23.279(5) _cell_length_c 21.081(5) _cell_angle_alpha 90.000 _cell_angle_beta 110.158(5) _cell_angle_gamma 90.000 _cell_volume 7189(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.892 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4036 _exptl_absorpt_coefficient_mu 1.115 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.8731 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART 1K CCD Area Detector Diffractometer' _diffrn_measurement_method 'Omega Scans' _diffrn_detector_area_resol_mean '5.7 pixels mm-1' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0002 _diffrn_reflns_number 32054 _diffrn_reflns_av_R_equivalents 0.0788 _diffrn_reflns_av_sigmaI/netI 0.0578 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 24.72 _reflns_number_total 6107 _reflns_number_gt 4569 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART v4.05 (Siemens, 1996)' _computing_cell_refinement 'SAINT v4.05 (Siemens, 1996)' _computing_data_reduction 'XPREP SHELXTL v5 (Siemens, 1994)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'Ciftab (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0853P)^2^+105.6410P] 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 6107 _refine_ls_number_parameters 483 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1084 _refine_ls_R_factor_gt 0.0755 _refine_ls_wR_factor_ref 0.1906 _refine_ls_wR_factor_gt 0.1734 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.113 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 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 0.26901(4) 0.71385(3) 0.23132(4) 0.0270(2) Uani 1 1 d . . . Rh2 Rh 0.37308(5) 0.70532(3) 0.35769(4) 0.0277(2) Uani 1 1 d . . . P2 P 0.1027(3) 0.52886(17) 0.3904(2) 0.0768(11) Uani 1 1 d . . . F21 F 0.0282(5) 0.4838(3) 0.3467(4) 0.077(2) Uani 1 1 d . . . F22 F 0.0785(9) 0.5159(4) 0.4529(6) 0.134(4) Uani 1 1 d . . . F23 F 0.1737(6) 0.4789(4) 0.4083(5) 0.115(3) Uani 1 1 d . . . F24 F 0.1289(6) 0.5440(4) 0.3282(5) 0.098(3) Uani 1 1 d . . . F25 F 0.1773(7) 0.5738(4) 0.4316(6) 0.118(4) Uani 1 1 d . . . F26 F 0.0304(8) 0.5775(4) 0.3743(8) 0.161(6) Uani 1 1 d . . . O12 O 0.1631(4) 0.7143(3) 0.2684(4) 0.0408(17) Uani 1 1 d . . . C12 C 0.1748(6) 0.7085(4) 0.3297(5) 0.036(2) Uani 1 1 d . . . O1 O 0.1583(5) 0.7237(4) 0.1321(4) 0.056(2) Uani 1 1 d . . . C111 C 0.1901(6) 0.5934(4) 0.1985(5) 0.040(2) Uani 1 1 d . . . H111 H 0.1497 0.6016 0.2223 0.048 Uiso 1 1 calc R . . C122 C 0.2519(6) 0.8397(4) 0.2537(5) 0.037(2) Uani 1 1 d . . . H122 H 0.2023 0.8296 0.2679 0.044 Uiso 1 1 calc R . . C121 C 0.2776(7) 0.8972(4) 0.2552(5) 0.038(2) Uani 1 1 d . . . H121 H 0.2465 0.9260 0.2707 0.046 Uiso 1 1 calc R . . O11 O 0.2524(4) 0.7033(3) 0.3764(4) 0.0412(16) Uani 1 1 d . . . P1 P 0.2500 0.7500 0.0000 0.0581(12) Uani 1 2 d S . . F11 F 0.2413(6) 0.6925(3) 0.0446(4) 0.084(3) Uani 1 1 d . . . F12 F 0.2615(4) 0.7930(3) 0.0665(3) 0.0594(17) Uani 1 1 d . . . N3 N 0.2954(5) 0.7989(3) 0.2328(4) 0.0314(17) Uani 1 1 d . . . C120 C 0.3473(6) 0.9114(4) 0.2343(5) 0.036(2) Uani 1 1 d . . . H120 H 0.3666 0.9502 0.2364 0.043 Uiso 1 1 calc R . . N1 N 0.2625(5) 0.6290(3) 0.2054(4) 0.0324(18) Uani 1 1 d . . . C222 C 0.3660(7) 0.8242(4) 0.4127(5) 0.038(2) Uani 1 1 d . . . H222 H 0.3072 0.8148 0.4137 0.045 Uiso 1 1 calc R . . C221 C 0.4096(7) 0.8718(4) 0.4464(5) 0.045(3) Uani 1 1 d . . . H221 H 0.3808 0.8953 0.4700 0.054 Uiso 1 1 calc R . . C211 C 0.3321(7) 0.5796(4) 0.3536(5) 0.039(2) Uani 1 1 d . . . H211 H 0.2797 0.5901 0.3642 0.047 Uiso 1 1 calc R . . C118 C 0.3635(5) 0.8128(4) 0.2089(4) 0.0248(19) Uani 1 1 d . . . C114 C 0.3024(6) 0.5695(4) 0.1265(5) 0.036(2) Uani 1 1 d . . . H114 H 0.3407 0.5624 0.1007 0.043 Uiso 1 1 calc R . . C119 C 0.3902(6) 0.8703(4) 0.2102(5) 0.029(2) Uani 1 1 d . . . H119 H 0.4381 0.8807 0.1942 0.035 Uiso 1 1 calc R . . C115 C 0.3199(6) 0.6159(4) 0.1714(5) 0.031(2) Uani 1 1 d . . . C212 C 0.3485(7) 0.5229(5) 0.3447(6) 0.049(3) Uani 1 1 d . . . H212 H 0.3086 0.4943 0.3508 0.059 Uiso 1 1 calc R . . N6 N 0.4040(5) 0.7902(3) 0.3781(4) 0.0293(17) Uani 1 1 d . . . N2 N 0.3666(4) 0.7123(3) 0.1944(3) 0.0242(15) Uani 1 1 d . . . F13 F 0.3626(5) 0.7398(4) 0.0246(3) 0.078(2) Uani 1 1 d . . . N4 N 0.3894(5) 0.6207(3) 0.3476(4) 0.0329(18) Uani 1 1 d . . . C220 C 0.4957(7) 0.8860(4) 0.4462(5) 0.044(3) Uani 1 1 d . . . H220 H 0.5270 0.9188 0.4698 0.053 Uiso 1 1 calc R . . O2 O 0.4438(5) 0.6948(3) 0.4699(4) 0.0510(19) Uani 1 1 d . . . C117 C 0.4040(5) 0.7632(4) 0.1854(4) 0.0238(19) Uani 1 1 d . . . C116 C 0.3909(5) 0.6596(4) 0.1772(4) 0.0251(19) Uani 1 1 d . . . C218 C 0.4867(6) 0.8040(4) 0.3749(4) 0.0270(19) Uani 1 1 d . . . C213 C 0.4229(7) 0.5069(4) 0.3270(5) 0.042(3) Uani 1 1 d . . . H213 H 0.4320 0.4680 0.3173 0.050 Uiso 1 1 calc R . . C219 C 0.5350(6) 0.8511(4) 0.4108(5) 0.033(2) Uani 1 1 d . . . H219 H 0.5947 0.8591 0.4109 0.040 Uiso 1 1 calc R . . C215 C 0.4674(6) 0.6067(4) 0.3351(4) 0.027(2) Uani 1 1 d . . . N5 N 0.4871(5) 0.7079(3) 0.3409(4) 0.0251(16) Uani 1 1 d . . . C214 C 0.4837(7) 0.5496(4) 0.3240(5) 0.037(2) Uani 1 1 d . . . H214 H 0.5369 0.5396 0.3142 0.045 Uiso 1 1 calc R . . C217 C 0.5266(5) 0.7599(4) 0.3419(4) 0.0254(19) Uani 1 1 d . . . C216 C 0.5254(6) 0.6569(4) 0.3330(4) 0.0262(19) Uani 1 1 d . . . O1S O 0.5927(7) 0.6309(5) 0.4858(5) 0.093(3) Uani 1 1 d . . . C113 C 0.2293(7) 0.5346(4) 0.1202(5) 0.043(3) Uani 1 1 d . . . H113 H 0.2168 0.5030 0.0900 0.051 Uiso 1 1 calc R . . C112 C 0.1750(7) 0.5450(4) 0.1567(6) 0.047(3) Uani 1 1 d . . . H112 H 0.1265 0.5195 0.1540 0.056 Uiso 1 1 calc R . . C2 C 0.0923(8) 0.7076(6) 0.3513(7) 0.062(3) Uani 1 1 d . . . H2A H 0.0756 0.7470 0.3585 0.094 Uiso 1 1 calc R . . H2B H 0.1064 0.6858 0.3935 0.094 Uiso 1 1 calc R . . H2C H 0.0413 0.6893 0.3161 0.094 Uiso 1 1 calc R . . C1S C 0.6333(15) 0.5923(8) 0.5433(11) 0.144(9) Uani 1 1 d . . . H1S1 H 0.6939 0.5802 0.5443 0.216 Uiso 1 1 calc R . . H1S2 H 0.5942 0.5585 0.5387 0.216 Uiso 1 1 calc R . . H1S3 H 0.6390 0.6125 0.5854 0.216 Uiso 1 1 calc R . . C21 C 0.390(3) 0.6752(18) 0.508(2) 0.29(2) Uiso 1 1 d . . . H21A H 0.3356 0.6993 0.4981 0.428 Uiso 1 1 calc R . . H21B H 0.4262 0.6777 0.5564 0.428 Uiso 1 1 calc R . . H21C H 0.3721 0.6353 0.4962 0.428 Uiso 1 1 calc R . . C11 C 0.0953(15) 0.7668(9) 0.1187(11) 0.062(5) Uiso 0.60 1 d P . . C11A C 0.092(2) 0.6930(13) 0.0927(16) 0.057(8) Uiso 0.40 1 d P . . P3 P 0.5000 0.3732(12) 0.2500 0.393(15) Uiso 1 2 d SD . . F31 F 0.5359(11) 0.3759(8) 0.1880(8) 0.218(7) Uiso 1 1 d D . . F32 F 0.4244(11) 0.4269(7) 0.2072(8) 0.186(6) Uiso 1 1 d D . . F33 F 0.4097(18) 0.3396(12) 0.1919(15) 0.213(14) Uiso 0.50 1 d PD . . 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 0.0176(4) 0.0256(4) 0.0347(4) 0.0039(3) 0.0049(3) -0.0001(3) Rh2 0.0211(4) 0.0266(4) 0.0335(4) 0.0011(3) 0.0070(3) 0.0002(3) P2 0.072(2) 0.063(2) 0.104(3) -0.015(2) 0.041(2) -0.0066(19) F21 0.059(4) 0.054(4) 0.117(7) -0.011(4) 0.029(4) -0.009(3) F22 0.208(12) 0.094(7) 0.147(9) -0.055(7) 0.122(9) -0.068(8) F23 0.081(6) 0.089(7) 0.145(9) -0.022(6) 0.003(6) 0.025(5) F24 0.083(6) 0.113(7) 0.108(7) -0.006(6) 0.047(5) -0.037(5) F25 0.117(8) 0.104(7) 0.158(9) -0.058(7) 0.079(7) -0.052(6) F26 0.115(8) 0.075(7) 0.330(19) -0.048(9) 0.124(11) -0.009(6) O12 0.023(3) 0.043(4) 0.059(5) 0.006(3) 0.018(3) -0.002(3) C12 0.028(5) 0.037(5) 0.050(7) -0.001(5) 0.021(5) 0.007(4) O1 0.026(4) 0.076(6) 0.051(5) 0.010(4) -0.006(3) 0.005(4) C111 0.025(5) 0.036(6) 0.050(6) 0.010(5) 0.004(5) -0.009(4) C122 0.029(5) 0.034(5) 0.048(6) 0.001(4) 0.015(5) 0.006(4) C121 0.046(6) 0.026(5) 0.048(6) -0.004(4) 0.022(5) 0.012(4) O11 0.034(4) 0.044(4) 0.049(4) 0.000(3) 0.018(3) -0.002(3) P1 0.053(3) 0.066(3) 0.039(2) 0.006(2) -0.004(2) -0.013(2) F11 0.120(7) 0.065(5) 0.051(4) 0.014(4) 0.008(4) -0.026(5) F12 0.052(4) 0.062(4) 0.048(4) 0.000(3) -0.003(3) -0.006(3) N3 0.024(4) 0.033(4) 0.034(4) 0.007(3) 0.006(3) 0.005(3) C120 0.037(5) 0.032(5) 0.034(5) -0.001(4) 0.007(4) 0.001(4) N1 0.027(4) 0.027(4) 0.038(5) 0.006(3) 0.005(4) -0.004(3) C222 0.034(5) 0.034(5) 0.046(6) -0.004(5) 0.015(5) 0.010(4) C221 0.047(6) 0.040(6) 0.052(7) -0.013(5) 0.021(5) 0.004(5) C211 0.030(5) 0.040(6) 0.044(6) 0.014(5) 0.007(5) -0.001(4) C118 0.018(4) 0.027(4) 0.026(5) 0.007(4) 0.002(4) 0.003(3) C114 0.035(5) 0.028(5) 0.039(6) -0.006(4) 0.005(4) -0.008(4) C119 0.026(5) 0.022(4) 0.035(5) 0.004(4) 0.004(4) 0.000(4) C115 0.027(5) 0.027(5) 0.036(5) 0.006(4) 0.008(4) -0.006(4) C212 0.036(6) 0.045(6) 0.060(7) 0.007(5) 0.009(5) -0.009(5) N6 0.024(4) 0.026(4) 0.033(4) -0.004(3) 0.004(3) 0.003(3) N2 0.017(3) 0.024(4) 0.028(4) 0.002(3) 0.003(3) -0.004(3) F13 0.050(4) 0.111(6) 0.055(4) -0.019(4) -0.007(3) -0.015(4) N4 0.030(4) 0.026(4) 0.039(5) 0.008(3) 0.006(4) -0.002(3) C220 0.043(6) 0.039(6) 0.047(6) -0.016(5) 0.011(5) -0.004(5) O2 0.055(5) 0.062(5) 0.032(4) 0.001(3) 0.010(3) -0.005(4) C117 0.019(4) 0.024(4) 0.021(4) 0.006(3) -0.002(3) 0.001(3) C116 0.021(4) 0.025(5) 0.022(5) -0.003(4) -0.001(4) -0.001(3) C218 0.023(5) 0.024(4) 0.029(5) 0.000(4) 0.002(4) 0.000(4) C213 0.045(6) 0.022(5) 0.049(6) 0.006(4) 0.003(5) -0.005(4) C219 0.023(5) 0.030(5) 0.043(6) -0.004(4) 0.006(4) -0.004(4) C215 0.024(5) 0.025(5) 0.029(5) 0.005(4) 0.004(4) -0.003(4) N5 0.019(4) 0.022(4) 0.029(4) 0.000(3) 0.001(3) 0.002(3) C214 0.039(6) 0.027(5) 0.044(6) 0.008(4) 0.014(5) 0.005(4) C217 0.017(4) 0.029(5) 0.025(5) 0.001(4) 0.000(4) 0.000(4) C216 0.026(5) 0.025(5) 0.022(5) 0.003(4) 0.002(4) -0.001(4) O1S 0.091(7) 0.094(8) 0.079(7) 0.019(6) 0.011(6) 0.003(6) C113 0.036(6) 0.033(5) 0.054(7) -0.011(5) 0.009(5) -0.013(4) C112 0.034(6) 0.032(6) 0.067(8) -0.001(5) 0.009(5) -0.020(5) C2 0.043(7) 0.077(9) 0.073(9) 0.004(7) 0.027(6) 0.006(6) C1S 0.16(2) 0.102(14) 0.145(19) 0.085(14) 0.024(15) 0.028(13) _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 N2 1.934(7) . ? Rh1 N3 2.019(8) . ? Rh1 N1 2.042(8) . ? Rh1 O12 2.058(6) . ? Rh1 O1 2.219(7) . ? Rh1 Rh2 2.6060(11) . ? Rh2 N5 1.930(7) . ? Rh2 N4 2.007(7) . ? Rh2 N6 2.044(7) . ? Rh2 O11 2.054(7) . ? Rh2 O2 2.252(7) . ? P2 F22 1.520(10) . ? P2 F24 1.544(9) . ? P2 F26 1.550(11) . ? P2 F23 1.560(9) . ? P2 F25 1.583(10) . ? P2 F21 1.600(8) . ? O12 C12 1.249(12) . ? C12 O11 1.275(12) . ? C12 C2 1.506(14) . ? O1 C11A 1.29(3) . ? O1 C11 1.36(2) . ? C111 N1 1.367(11) . ? C111 C112 1.400(14) . ? C122 N3 1.329(12) . ? C122 C121 1.395(13) . ? C121 C120 1.346(13) . ? P1 F11 1.667(7) . ? P1 F11 1.667(7) 7_565 ? P1 F13 1.669(7) 7_565 ? P1 F13 1.669(7) . ? P1 F12 1.682(7) 7_565 ? P1 F12 1.682(7) . ? N3 C118 1.365(11) . ? C120 C119 1.361(13) . ? N1 C115 1.361(12) . ? C222 N6 1.344(12) . ? C222 C221 1.365(14) . ? C221 C220 1.386(14) . ? C211 N4 1.345(12) . ? C211 C212 1.370(15) . ? C118 C119 1.399(12) . ? C118 C117 1.482(12) . ? C114 C113 1.369(13) . ? C114 C115 1.400(13) . ? C115 C116 1.478(12) . ? C212 C213 1.387(15) . ? N6 C218 1.355(11) . ? N2 C117 1.363(10) . ? N2 C116 1.368(10) . ? N4 C215 1.370(11) . ? C220 C219 1.380(13) . ? O2 C21 1.42(4) . ? C117 C217 1.392(12) 2_655 ? C116 C216 1.397(12) 2_655 ? C218 C219 1.396(12) . ? C218 C217 1.491(12) . ? C213 C214 1.391(13) . ? C215 C214 1.388(12) . ? C215 C216 1.488(12) . ? N5 C217 1.357(11) . ? N5 C216 1.364(11) . ? C217 C117 1.392(12) 2_655 ? C216 C116 1.397(12) 2_655 ? O1S C1S 1.466(17) . ? C113 C112 1.347(15) . ? C11 C11A 1.80(4) . ? P3 F31 1.591(14) 2_655 ? P3 F31 1.591(14) . ? P3 F33 1.706(18) . ? P3 F33 1.706(18) 2_655 ? P3 F32 1.743(16) . ? P3 F32 1.743(16) 2_655 ? 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 Rh1 N3 80.8(3) . . ? N2 Rh1 N1 81.2(3) . . ? N3 Rh1 N1 160.6(3) . . ? N2 Rh1 O12 178.5(3) . . ? N3 Rh1 O12 100.1(3) . . ? N1 Rh1 O12 97.7(3) . . ? N2 Rh1 O1 95.0(3) . . ? N3 Rh1 O1 90.1(3) . . ? N1 Rh1 O1 84.1(3) . . ? O12 Rh1 O1 83.8(3) . . ? N2 Rh1 Rh2 96.3(2) . . ? N3 Rh1 Rh2 90.4(2) . . ? N1 Rh1 Rh2 99.0(2) . . ? O12 Rh1 Rh2 84.9(2) . . ? O1 Rh1 Rh2 168.6(2) . . ? N5 Rh2 N4 81.5(3) . . ? N5 Rh2 N6 81.0(3) . . ? N4 Rh2 N6 160.3(3) . . ? N5 Rh2 O11 179.3(3) . . ? N4 Rh2 O11 99.0(3) . . ? N6 Rh2 O11 98.4(3) . . ? N5 Rh2 O2 92.7(3) . . ? N4 Rh2 O2 88.3(3) . . ? N6 Rh2 O2 83.7(3) . . ? O11 Rh2 O2 86.9(3) . . ? N5 Rh2 Rh1 95.7(2) . . ? N4 Rh2 Rh1 91.3(2) . . ? N6 Rh2 Rh1 99.2(2) . . ? O11 Rh2 Rh1 84.8(2) . . ? O2 Rh2 Rh1 171.5(2) . . ? F22 P2 F24 177.9(6) . . ? F22 P2 F26 87.4(8) . . ? F24 P2 F26 91.9(7) . . ? F22 P2 F23 90.6(7) . . ? F24 P2 F23 90.0(6) . . ? F26 P2 F23 177.9(8) . . ? F22 P2 F25 90.6(6) . . ? F24 P2 F25 87.4(5) . . ? F26 P2 F25 88.8(6) . . ? F23 P2 F25 91.9(6) . . ? F22 P2 F21 91.2(5) . . ? F24 P2 F21 90.8(5) . . ? F26 P2 F21 91.3(6) . . ? F23 P2 F21 88.0(5) . . ? F25 P2 F21 178.2(6) . . ? C12 O12 Rh1 122.8(6) . . ? O12 C12 O11 124.8(9) . . ? O12 C12 C2 118.6(9) . . ? O11 C12 C2 116.6(10) . . ? C11A O1 C11 85.2(17) . . ? C11A O1 Rh1 137.5(15) . . ? C11 O1 Rh1 122.8(10) . . ? N1 C111 C112 120.5(10) . . ? N3 C122 C121 121.2(9) . . ? C120 C121 C122 119.1(9) . . ? C12 O11 Rh2 122.6(6) . . ? F11 P1 F11 180.0(5) . 7_565 ? F11 P1 F13 90.4(4) . 7_565 ? F11 P1 F13 89.6(4) 7_565 7_565 ? F11 P1 F13 89.6(4) . . ? F11 P1 F13 90.4(4) 7_565 . ? F13 P1 F13 180.000(1) 7_565 . ? F11 P1 F12 89.2(4) . 7_565 ? F11 P1 F12 90.8(4) 7_565 7_565 ? F13 P1 F12 91.6(3) 7_565 7_565 ? F13 P1 F12 88.4(3) . 7_565 ? F11 P1 F12 90.8(4) . . ? F11 P1 F12 89.2(4) 7_565 . ? F13 P1 F12 88.4(3) 7_565 . ? F13 P1 F12 91.6(3) . . ? F12 P1 F12 180.0(4) 7_565 . ? C122 N3 C118 120.3(8) . . ? C122 N3 Rh1 125.6(7) . . ? C118 N3 Rh1 114.1(6) . . ? C121 C120 C119 120.5(9) . . ? C115 N1 C111 118.5(8) . . ? C115 N1 Rh1 112.1(5) . . ? C111 N1 Rh1 125.3(7) . . ? N6 C222 C221 121.8(9) . . ? C222 C221 C220 120.1(9) . . ? N4 C211 C212 120.7(10) . . ? N3 C118 C119 119.0(8) . . ? N3 C118 C117 114.4(7) . . ? C119 C118 C117 126.5(8) . . ? C113 C114 C115 119.0(10) . . ? C120 C119 C118 119.8(9) . . ? N1 C115 C114 121.3(8) . . ? N1 C115 C116 114.3(8) . . ? C114 C115 C116 123.6(8) . . ? C211 C212 C213 120.5(10) . . ? C222 N6 C218 119.5(8) . . ? C222 N6 Rh2 124.6(7) . . ? C218 N6 Rh2 112.2(5) . . ? C117 N2 C116 124.8(7) . . ? C117 N2 Rh1 118.3(6) . . ? C116 N2 Rh1 116.9(5) . . ? C211 N4 C215 120.8(8) . . ? C211 N4 Rh2 125.1(7) . . ? C215 N4 Rh2 114.1(6) . . ? C219 C220 C221 118.3(9) . . ? C21 O2 Rh2 117.4(18) . . ? N2 C117 C217 116.2(7) . 2_655 ? N2 C117 C118 112.3(7) . . ? C217 C117 C118 131.5(8) 2_655 . ? N2 C116 C216 116.2(7) . 2_655 ? N2 C116 C115 111.8(7) . . ? C216 C116 C115 132.0(8) 2_655 . ? N6 C218 C219 120.3(8) . . ? N6 C218 C217 114.7(7) . . ? C219 C218 C217 124.0(8) . . ? C212 C213 C214 117.9(9) . . ? C220 C219 C218 119.9(9) . . ? N4 C215 C214 119.1(8) . . ? N4 C215 C216 114.0(7) . . ? C214 C215 C216 126.8(8) . . ? C217 N5 C216 124.2(7) . . ? C217 N5 Rh2 117.9(6) . . ? C216 N5 Rh2 117.8(6) . . ? C215 C214 C213 120.6(9) . . ? N5 C217 C117 117.1(8) . 2_655 ? N5 C217 C218 111.2(7) . . ? C117 C217 C218 131.7(8) 2_655 . ? N5 C216 C116 116.9(7) . 2_655 ? N5 C216 C215 112.6(7) . . ? C116 C216 C215 130.5(8) 2_655 . ? C112 C113 C114 120.4(9) . . ? C113 C112 C111 120.1(9) . . ? O1 C11 C11A 45.7(12) . . ? O1 C11A C11 49.1(13) . . ? F31 P3 F31 175(2) 2_655 . ? F31 P3 F33 99.9(14) 2_655 . ? F31 P3 F33 82.3(11) . . ? F31 P3 F33 82.3(11) 2_655 2_655 ? F31 P3 F33 99.9(14) . 2_655 ? F33 P3 F33 125(3) . 2_655 ? F31 P3 F32 91.7(12) 2_655 . ? F31 P3 F32 85.0(10) . . ? F33 P3 F32 73.3(11) . . ? F33 P3 F32 161(2) 2_655 . ? F31 P3 F32 85.0(10) 2_655 2_655 ? F31 P3 F32 91.7(12) . 2_655 ? F33 P3 F32 161(2) . 2_655 ? F33 P3 F32 73.3(11) 2_655 2_655 ? F32 P3 F32 88.3(17) . 2_655 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.72 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.967 _refine_diff_density_min -0.963 _refine_diff_density_rms 0.171