# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 182/1442 data_tmcg17 _publ-contact_author_name ; R. P. Bonar-Law ; _publ_contact_author_address ; Department of Chemistry, University of Liverpool Liverpool L69 7ZD, U.K. ; _publ_section_journal ' Chem Comm' _publ_section_title ; Dinuclear carboxylates as connectors for acids. Self-assembly of a molecular box. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C172 H212 N8 O40 Rh8' _chemical_formula_weight 3855.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0020 0.0020 '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' 'O' 'O' 0.0080 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.2870 0.9190 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0040 0.0030 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.485(2) _cell_length_b 19.834(3) _cell_length_c 23.522(5) _cell_angle_alpha 69.66(2) _cell_angle_beta 75.12(2) _cell_angle_gamma 83.331(19) _cell_volume 5698.5(18) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1980 _exptl_absorpt_coefficient_mu 0.623 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Stoe-IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31032 _diffrn_reflns_av_R_equivalents 0.1765 _diffrn_reflns_av_sigmaI/netI 0.4949 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 22.49 _reflns_number_total 14190 _reflns_number_gt 3238 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _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 w=1/[\s^2^(Fo^2^)+(0.0600P)^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 SHELXL _refine_ls_extinction_coef 0.00077(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 14190 _refine_ls_number_parameters 478 _refine_ls_number_restraints 438 _refine_ls_R_factor_all 0.2313 _refine_ls_R_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.1913 _refine_ls_wR_factor_gt 0.1521 _refine_ls_goodness_of_fit_ref 0.628 _refine_ls_restrained_S_all 0.624 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.20362(13) 0.17378(11) 0.37173(7) 0.0380(6) Uani 1 d . . . Rh2 Rh 0.36069(13) 0.20502(11) 0.38631(8) 0.0377(6) Uani 1 d . . . Rh3 Rh -0.21078(12) 0.22255(10) 0.82238(7) 0.0360(5) Uani 1 d . . . Rh4 Rh -0.05323(12) 0.24133(10) 0.84444(7) 0.0365(5) Uani 1 d . . . O1 O 0.1325(9) 0.1777(7) 0.4578(5) 0.042(4) Uiso 1 d . . . O2 O 0.2829(9) 0.2063(7) 0.4722(5) 0.042(4) Uiso 1 d . . . O3 O 0.1697(10) 0.2809(8) 0.3346(6) 0.050(4) Uiso 1 d . . . O4 O 0.3214(9) 0.3090(7) 0.3488(5) 0.040(4) Uiso 1 d . . . O5 O 0.4322(9) 0.1992(8) 0.3007(6) 0.045(4) Uiso 1 d . . . O6 O 0.2837(9) 0.1735(7) 0.2854(5) 0.038(3) Uiso 1 d . . . O7 O 0.2463(10) 0.0668(8) 0.4106(6) 0.048(4) Uiso 1 d . . . O8 O 0.3971(9) 0.0989(7) 0.4196(5) 0.042(3) Uiso 1 d . . . O9 O 0.3258(9) -0.0663(8) 0.4102(6) 0.060(4) Uiso 1 d . . . O10 O 0.3927(10) 0.1113(8) 0.1995(6) 0.065(4) Uiso 1 d . . . O11 O -0.1275(10) 0.2126(7) 0.7406(6) 0.044(4) Uiso 1 d . . . O12 O 0.0214(9) 0.2296(7) 0.7609(5) 0.041(4) Uiso 1 d . . . O13 O -0.2256(9) 0.3298(7) 0.7819(5) 0.044(4) Uiso 1 d . . . O14 O -0.0744(10) 0.3481(8) 0.8013(6) 0.048(4) Uiso 1 d . . . O15 O -0.2869(10) 0.2341(8) 0.9067(6) 0.047(4) Uiso 1 d . . . O16 O -0.1363(10) 0.2494(7) 0.9273(6) 0.046(4) Uiso 1 d . . . O17 O -0.1889(10) 0.1160(8) 0.8636(6) 0.051(4) Uiso 1 d . . . O18 O -0.0445(9) 0.1311(7) 0.8886(5) 0.043(3) Uiso 1 d . . . O19 O -0.1502(10) -0.0047(8) 0.9894(6) 0.068(4) Uiso 1 d . . . O20 O -0.3701(10) 0.1882(9) 1.0343(6) 0.063(4) Uiso 1 d . . . C1 C 0.1314(12) 0.1991(10) 0.5506(8) 0.034(5) Uiso 1 d . . . C2 C 0.0270(13) 0.1878(10) 0.5725(8) 0.036(5) Uiso 1 d . . . H2 H -0.0084 0.1752 0.5487 0.044 Uiso 1 calc R . . C3 C -0.0257(15) 0.1947(12) 0.6289(9) 0.050(6) Uiso 1 d . . . H3 H -0.0961 0.1881 0.6423 0.060 Uiso 1 calc R . . C4 C 0.0259(12) 0.2115(10) 0.6654(7) 0.031(5) Uiso 1 d . . . C5 C 0.1276(15) 0.2252(12) 0.6427(9) 0.052(6) Uiso 1 d . . . H5 H 0.1620 0.2404 0.6654 0.062 Uiso 1 calc R . . C6 C 0.1819(16) 0.2169(12) 0.5863(9) 0.050(6) Uiso 1 d . . . H6 H 0.2524 0.2235 0.5731 0.060 Uiso 1 calc R . . C7 C 0.1879(13) 0.1947(10) 0.4890(8) 0.033(5) Uiso 1 d . . . C8 C -0.0319(15) 0.2178(11) 0.7255(9) 0.047(6) Uiso 1 d . . . C9 C 0.2379(15) 0.3224(12) 0.3303(8) 0.048(6) Uiso 1 d . . . C10 C 0.2142(15) 0.4013(12) 0.3026(8) 0.054(6) Uiso 1 d . . . C11 C 0.2869(18) 0.4534(15) 0.2921(10) 0.078(7) Uiso 1 d . . . H11 H 0.3479 0.4385 0.3048 0.094 Uiso 1 calc R . . C12 C 0.1230(17) 0.4256(14) 0.2849(10) 0.069(7) Uiso 1 d . . . H12 H 0.0752 0.3931 0.2887 0.083 Uiso 1 calc R . . C13 C -0.1586(15) 0.3686(12) 0.7811(8) 0.050(6) Uiso 1 d . . . C14 C -0.1727(13) 0.4490(11) 0.7511(8) 0.044(5) Uiso 1 d . . . C15 C -0.1036(17) 0.5013(13) 0.7386(9) 0.068(7) Uiso 1 d . . . H15 H -0.0391 0.4862 0.7467 0.081 Uiso 1 calc R . . C16 C -0.2679(17) 0.4728(14) 0.7375(9) 0.067(7) Uiso 1 d . . . H16 H -0.3191 0.4400 0.7480 0.081 Uiso 1 calc R . . C17 C 0.3793(14) 0.1815(10) 0.2706(8) 0.035(5) Uiso 1 d . . . C18 C 0.4394(15) 0.1662(12) 0.2081(9) 0.054(6) Uiso 1 d . . . C19 C 0.4276(18) 0.2335(14) 0.1577(10) 0.095(8) Uiso 1 d . . . H19A H 0.3559 0.2445 0.1590 0.142 Uiso 1 calc R . . H19B H 0.4613 0.2281 0.1182 0.142 Uiso 1 calc R . . H19C H 0.4577 0.2719 0.1628 0.142 Uiso 1 calc R . . C20 C 0.5502(15) 0.1463(13) 0.2079(9) 0.069(7) Uiso 1 d . . . H20A H 0.5550 0.1018 0.2409 0.103 Uiso 1 calc R . . H20B H 0.5814 0.1835 0.2142 0.103 Uiso 1 calc R . . H20C H 0.5850 0.1408 0.1687 0.103 Uiso 1 calc R . . C21 C 0.3600(14) 0.0458(12) 0.2453(9) 0.058(5) Uiso 1 d . . . C22 C 0.3722(14) 0.0204(11) 0.3066(8) 0.056(5) Uiso 1 d . . . H22 H 0.4124 0.0457 0.3187 0.067 Uiso 1 calc R . . C23 C 0.3283(14) -0.0377(12) 0.3471(9) 0.061(6) Uiso 1 d . . . C24 C 0.2681(15) -0.0786(13) 0.3299(10) 0.076(6) Uiso 1 d . . . H24 H 0.2343 -0.1196 0.3583 0.091 Uiso 1 calc R . . C25 C 0.2639(16) -0.0536(14) 0.2698(11) 0.085(7) Uiso 1 d . . . H25 H 0.2319 -0.0824 0.2563 0.102 Uiso 1 calc R . . C26 C 0.3015(18) 0.0097(15) 0.2260(12) 0.083(7) Uiso 1 d . . . H26 H 0.2885 0.0269 0.1864 0.100 Uiso 1 calc R . . C27 C 0.3720(13) -0.0238(11) 0.4386(8) 0.049(5) Uiso 1 d . . . C28 C 0.3295(17) -0.0626(14) 0.5092(10) 0.089(7) Uiso 1 d . . . H28A H 0.3528 -0.1120 0.5199 0.133 Uiso 1 calc R . . H28B H 0.2558 -0.0601 0.5185 0.133 Uiso 1 calc R . . H28C H 0.3536 -0.0397 0.5328 0.133 Uiso 1 calc R . . C29 C 0.4856(15) -0.0336(13) 0.4237(9) 0.070(7) Uiso 1 d . . . H29A H 0.5036 -0.0840 0.4356 0.104 Uiso 1 calc R . . H29B H 0.5143 -0.0116 0.4461 0.104 Uiso 1 calc R . . H29C H 0.5122 -0.0114 0.3797 0.104 Uiso 1 calc R . . C30 C 0.3352(14) 0.0524(11) 0.4228(8) 0.043(5) Uiso 1 d . . . C31 C -0.2352(16) 0.2385(13) 0.9426(10) 0.057(6) Uiso 1 d . . . C32 C -0.2906(15) 0.2410(12) 1.0063(9) 0.051(6) Uiso 1 d . . . C33 C -0.2172(15) 0.2302(13) 1.0499(9) 0.068(7) Uiso 1 d . . . H33A H -0.2561 0.2323 1.0897 0.102 Uiso 1 calc R . . H33B H -0.1678 0.2675 1.0318 0.102 Uiso 1 calc R . . H33C H -0.1823 0.1842 1.0553 0.102 Uiso 1 calc R . . C34 C -0.3458(16) 0.3114(13) 0.9962(10) 0.079(7) Uiso 1 d . . . H34A H -0.3832 0.3153 1.0357 0.119 Uiso 1 calc R . . H34B H -0.3927 0.3155 0.9706 0.119 Uiso 1 calc R . . H34C H -0.2973 0.3492 0.9759 0.119 Uiso 1 calc R . . C35 C -0.3513(15) 0.1226(12) 1.0311(8) 0.054(5) Uiso 1 d . . . C36 C -0.2588(15) 0.0920(12) 1.0125(8) 0.061(6) Uiso 1 d . . . H36 H -0.2008 0.1188 1.0024 0.073 Uiso 1 calc R . . C37 C -0.2451(14) 0.0266(12) 1.0077(8) 0.054(5) Uiso 1 d . . . C38 C -0.3338(19) -0.0151(16) 1.0225(11) 0.102(8) Uiso 1 d . . . H38 H -0.3300 -0.0605 1.0187 0.122 Uiso 1 calc R . . C39 C -0.421(2) 0.0161(17) 1.0417(11) 0.107(9) Uiso 1 d . . . H39 H -0.4786 -0.0109 1.0525 0.128 Uiso 1 calc R . . C40 C -0.4386(17) 0.0833(13) 1.0483(9) 0.076(7) Uiso 1 d . . . H40 H -0.5038 0.1005 1.0630 0.091 Uiso 1 calc R . . C41 C -0.1045(14) 0.0111(11) 0.9229(8) 0.051(5) Uiso 1 d . . . C42 C 0.0054(16) -0.0144(13) 0.9173(10) 0.078(7) Uiso 1 d . . . H42A H 0.0086 -0.0650 0.9396 0.117 Uiso 1 calc R . . H42B H 0.0395 0.0110 0.9346 0.117 Uiso 1 calc R . . H42C H 0.0386 -0.0054 0.8742 0.117 Uiso 1 calc R . . C43 C -0.1620(16) -0.0309(14) 0.8968(10) 0.078(7) Uiso 1 d . . . H43A H -0.2322 -0.0139 0.9005 0.117 Uiso 1 calc R . . H43B H -0.1595 -0.0813 0.9201 0.117 Uiso 1 calc R . . H43C H -0.1297 -0.0233 0.8537 0.117 Uiso 1 calc R . . C44 C -0.1137(14) 0.0932(11) 0.8872(8) 0.045(5) Uiso 1 d . . . N1 N 0.0666(11) 0.1396(9) 0.3529(7) 0.047(5) Uiso 1 d DU . . C45 C 0.0303(16) 0.0760(11) 0.3821(9) 0.088(7) Uiso 1 d DU . . H45 H 0.0464 0.0503 0.4201 0.106 Uiso 1 calc R . . C46 C -0.0338(18) 0.0420(12) 0.3598(10) 0.124(10) Uiso 1 d DU . . H46 H -0.0466 -0.0068 0.3781 0.149 Uiso 1 calc R . . C47 C -0.0741(13) 0.0822(10) 0.3124(8) 0.062(6) Uiso 1 d DU . . C48 C -0.0374(17) 0.1471(11) 0.2804(10) 0.110(9) Uiso 1 d DU . . H48 H -0.0574 0.1750 0.2441 0.132 Uiso 1 calc R . . C49 C 0.0345(17) 0.1736(11) 0.3033(9) 0.100(8) Uiso 1 d DU . . H49 H 0.0596 0.2193 0.2801 0.120 Uiso 1 calc R . . C50 C -0.1458(13) 0.0449(10) 0.2856(8) 0.077(6) Uiso 1 d DU . . C51 C -0.164(2) 0.0965(14) 0.2297(10) 0.144(12) Uiso 1 d DU . . H51A H -0.1000 0.1073 0.1991 0.215 Uiso 1 calc R . . H51B H -0.1937 0.1396 0.2376 0.215 Uiso 1 calc R . . H51C H -0.2100 0.0775 0.2144 0.215 Uiso 1 calc R . . C52 C -0.0898(18) -0.0152(12) 0.2725(11) 0.131(10) Uiso 1 d DU . . H52A H -0.0297 0.0010 0.2397 0.196 Uiso 1 calc R . . H52B H -0.1321 -0.0403 0.2597 0.196 Uiso 1 calc R . . H52C H -0.0696 -0.0470 0.3093 0.196 Uiso 1 calc R . . C53 C -0.2350(16) 0.0238(16) 0.3345(11) 0.153(12) Uiso 1 d DU . . H53A H -0.2162 -0.0111 0.3704 0.230 Uiso 1 calc R . . H53B H -0.2821 0.0031 0.3212 0.230 Uiso 1 calc R . . H53C H -0.2671 0.0651 0.3450 0.230 Uiso 1 calc R . . N2 N 0.5056(11) 0.2350(10) 0.4020(7) 0.055(5) Uiso 1 d DU . . C54 C 0.5042(14) 0.2522(14) 0.4495(10) 0.091(8) Uiso 1 d DU . . H54 H 0.4423 0.2511 0.4786 0.109 Uiso 1 calc R . . C55 C 0.5944(14) 0.2733(14) 0.4601(10) 0.099(8) Uiso 1 d DU . . H55 H 0.5884 0.2911 0.4926 0.119 Uiso 1 calc R . . C56 C 0.6854(12) 0.2679(12) 0.4242(8) 0.074(7) Uiso 1 d DU . . C57 C 0.6892(13) 0.2469(12) 0.3760(8) 0.069(6) Uiso 1 d DU . . H57 H 0.7513 0.2427 0.3487 0.082 Uiso 1 calc R . . C58 C 0.5948(12) 0.2308(12) 0.3675(8) 0.069(6) Uiso 1 d DU . . H58 H 0.5984 0.2158 0.3337 0.083 Uiso 1 calc R . . C59 C 0.7928(15) 0.2813(12) 0.4379(10) 0.126(10) Uiso 1 d DU . . C60 C 0.770(2) 0.292(2) 0.4961(12) 0.214(19) Uiso 1 d DU . . H60A H 0.7404 0.2489 0.5280 0.320 Uiso 1 calc R . . H60B H 0.7220 0.3315 0.4955 0.320 Uiso 1 calc R . . H60C H 0.8318 0.3014 0.5045 0.320 Uiso 1 calc R . . C61 C 0.836(2) 0.3418(15) 0.3882(13) 0.211(18) Uiso 1 d DU . . H61A H 0.8515 0.3312 0.3500 0.317 Uiso 1 calc R . . H61B H 0.8974 0.3537 0.3954 0.317 Uiso 1 calc R . . H61C H 0.7875 0.3817 0.3854 0.317 Uiso 1 calc R . . C62 C 0.857(2) 0.2182(15) 0.4411(14) 0.178(15) Uiso 1 d DU . . H62A H 0.8255 0.1783 0.4755 0.267 Uiso 1 calc R . . H62B H 0.9225 0.2261 0.4469 0.267 Uiso 1 calc R . . H62C H 0.8678 0.2078 0.4030 0.267 Uiso 1 calc R . . N3 N -0.3518(11) 0.2034(9) 0.8003(7) 0.050(5) Uiso 1 d DU . . C63 C -0.3729(14) 0.2379(11) 0.7474(8) 0.074(7) Uiso 1 d DU . . H63 H -0.3320 0.2763 0.7208 0.089 Uiso 1 calc R . . C64 C -0.4550(15) 0.2216(12) 0.7262(9) 0.094(8) Uiso 1 d DU . . H64 H -0.4642 0.2474 0.6864 0.113 Uiso 1 calc R . . C65 C -0.5179(13) 0.1690(10) 0.7644(8) 0.065(6) Uiso 1 d DU . . C66 C -0.4977(15) 0.1326(12) 0.8200(9) 0.093(8) Uiso 1 d DU . . H66 H -0.5359 0.0930 0.8470 0.111 Uiso 1 calc R . . C67 C -0.4164(14) 0.1555(11) 0.8374(8) 0.070(6) Uiso 1 d DU . . H67 H -0.4098 0.1341 0.8783 0.084 Uiso 1 calc R . . C68 C -0.6137(14) 0.1455(11) 0.7455(8) 0.094(8) Uiso 1 d DU . . C69 C -0.625(2) 0.0694(12) 0.7738(12) 0.152(12) Uiso 1 d DU . . H69A H -0.6399 0.0569 0.8183 0.229 Uiso 1 calc R . . H69B H -0.5629 0.0450 0.7599 0.229 Uiso 1 calc R . . H69C H -0.6808 0.0552 0.7622 0.229 Uiso 1 calc R . . C70 C -0.5917(19) 0.1664(15) 0.6794(8) 0.130(11) Uiso 1 d DU . . H70A H -0.5321 0.1399 0.6650 0.195 Uiso 1 calc R . . H70B H -0.5788 0.2170 0.6618 0.195 Uiso 1 calc R . . H70C H -0.6492 0.1566 0.6668 0.195 Uiso 1 calc R . . C71 C -0.7012(16) 0.1821(15) 0.7708(11) 0.139(11) Uiso 1 d DU . . H71A H -0.7125 0.1655 0.8154 0.208 Uiso 1 calc R . . H71B H -0.7602 0.1727 0.7593 0.208 Uiso 1 calc R . . H71C H -0.6900 0.2329 0.7548 0.208 Uiso 1 calc R . . N4 N 0.0889(11) 0.2550(9) 0.8714(7) 0.047(5) Uiso 1 d DU . . C72 C 0.1374(15) 0.3137(11) 0.8467(9) 0.084(7) Uiso 1 d DU . . H72 H 0.1141 0.3498 0.8149 0.100 Uiso 1 calc R . . C73 C 0.2254(16) 0.3285(12) 0.8643(10) 0.106(9) Uiso 1 d DU . . H73 H 0.2548 0.3734 0.8455 0.127 Uiso 1 calc R . . C74 C 0.2643(13) 0.2773(10) 0.9077(9) 0.076(7) Uiso 1 d DU . . C75 C 0.2052(14) 0.2208(11) 0.9399(9) 0.083(7) Uiso 1 d DU . . H75 H 0.2173 0.1892 0.9774 0.100 Uiso 1 calc R . . C76 C 0.1229(13) 0.2086(10) 0.9166(8) 0.060(6) Uiso 1 d DU . . H76 H 0.0920 0.1642 0.9354 0.072 Uiso 1 calc R . . C77 C 0.3697(14) 0.2916(11) 0.9232(9) 0.106(8) Uiso 1 d DU . . C78 C 0.4443(16) 0.3237(14) 0.8664(10) 0.133(11) Uiso 1 d DU . . H78A H 0.4641 0.2903 0.8438 0.199 Uiso 1 calc R . . H78B H 0.5036 0.3355 0.8761 0.199 Uiso 1 calc R . . H78C H 0.4150 0.3666 0.8413 0.199 Uiso 1 calc R . . C79 C 0.4082(18) 0.2249(12) 0.9584(11) 0.127(10) Uiso 1 d DU . . H79A H 0.4260 0.1936 0.9338 0.191 Uiso 1 calc R . . H79B H 0.3566 0.2031 0.9953 0.191 Uiso 1 calc R . . H79C H 0.4681 0.2326 0.9700 0.191 Uiso 1 calc R . . C80 C 0.341(2) 0.3402(15) 0.9567(13) 0.196(16) Uiso 1 d DU . . H80A H 0.3157 0.3845 0.9308 0.294 Uiso 1 calc R . . H80B H 0.3994 0.3494 0.9688 0.294 Uiso 1 calc R . . H80C H 0.2880 0.3199 0.9932 0.294 Uiso 1 calc R . . C1H C 0.712(4) 0.384(5) 0.193(3) 0.52(5) Uiso 1 d DU . . H1H1 H 0.7346 0.3648 0.2309 0.778 Uiso 1 calc R . . H1H2 H 0.7422 0.4291 0.1681 0.778 Uiso 1 calc R . . H1H3 H 0.7311 0.3505 0.1699 0.778 Uiso 1 calc R . . C2H C 0.596(4) 0.394(6) 0.208(2) 0.49(4) Uiso 1 d DU . . H2H1 H 0.5648 0.3477 0.2328 0.590 Uiso 1 calc R . . H2H2 H 0.5759 0.4259 0.2320 0.590 Uiso 1 calc R . . C3H C 0.556(4) 0.424(5) 0.150(2) 0.46(3) Uiso 1 d DU . . H3H1 H 0.5653 0.4756 0.1332 0.554 Uiso 1 calc R . . H3H2 H 0.5972 0.4039 0.1187 0.554 Uiso 1 calc R . . C4H C 0.446(5) 0.411(4) 0.157(3) 0.50(4) Uiso 1 d DU . . H4H1 H 0.4083 0.4116 0.1977 0.605 Uiso 1 calc R . . H4H2 H 0.4414 0.3633 0.1552 0.605 Uiso 1 calc R . . C5H C 0.397(4) 0.464(3) 0.109(3) 0.46(4) Uiso 1 d DU . . H5H1 H 0.4401 0.4688 0.0680 0.547 Uiso 1 calc R . . H5H2 H 0.3926 0.5107 0.1145 0.547 Uiso 1 calc R . . C6H C 0.290(4) 0.446(4) 0.110(3) 0.38(4) Uiso 1 d DU . . H6H1 H 0.2727 0.4736 0.0715 0.573 Uiso 1 calc R . . H6H2 H 0.2418 0.4565 0.1439 0.573 Uiso 1 calc R . . H6H3 H 0.2890 0.3955 0.1161 0.573 Uiso 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 0.0364(11) 0.0475(15) 0.0356(10) -0.0175(9) -0.0089(8) -0.0092(9) Rh2 0.0350(11) 0.0448(15) 0.0385(10) -0.0188(9) -0.0085(8) -0.0062(9) Rh3 0.0330(10) 0.0444(15) 0.0331(10) -0.0136(9) -0.0091(8) -0.0053(9) Rh4 0.0326(11) 0.0482(15) 0.0329(10) -0.0163(9) -0.0096(8) -0.0038(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 Rh1 O1 2.030(12) . ? Rh1 O6 2.042(12) . ? Rh1 O3 2.044(14) . ? Rh1 O7 2.075(14) . ? Rh1 Rh2 2.411(3) . ? Rh2 O4 2.008(14) . ? Rh2 O8 2.024(13) . ? Rh2 O2 2.032(12) . ? Rh2 O5 2.033(12) . ? Rh3 O13 2.016(14) . ? Rh3 O17 2.018(15) . ? Rh3 O11 2.026(12) . ? Rh3 O15 2.062(12) . ? Rh3 Rh4 2.410(3) . ? Rh4 O14 2.027(14) . ? Rh4 O16 2.033(12) . ? Rh4 O12 2.044(12) . ? Rh4 O18 2.073(14) . ? O1 C7 1.313(18) . ? O2 C7 1.263(18) . ? O3 C9 1.27(2) . ? O4 C9 1.28(2) . ? O5 C17 1.277(19) . ? O6 C17 1.259(18) . ? O7 C30 1.281(19) . ? O8 C30 1.29(2) . ? O9 C23 1.38(2) . ? O9 C27 1.51(2) . ? O10 C21 1.40(2) . ? O10 C18 1.42(2) . ? O11 C8 1.253(19) . ? O12 C8 1.32(2) . ? O13 C13 1.25(2) . ? O14 C13 1.31(2) . ? O15 C31 1.26(2) . ? O16 C31 1.31(2) . ? O17 C44 1.24(2) . ? O18 C44 1.28(2) . ? O19 C37 1.39(2) . ? O19 C41 1.46(2) . ? O20 C35 1.32(2) . ? O20 C32 1.45(2) . ? C1 C6 1.36(2) . ? C1 C2 1.39(2) . ? C1 C7 1.48(2) . ? C2 C3 1.38(2) . ? C3 C4 1.37(2) . ? C4 C5 1.36(2) . ? C4 C8 1.47(2) . ? C5 C6 1.40(2) . ? C9 C10 1.50(3) . ? C10 C12 1.38(3) . ? C10 C11 1.42(3) . ? C11 C16 1.41(3) 2_566 ? C12 C15 1.38(3) 2_566 ? C13 C14 1.51(3) . ? C14 C15 1.38(3) . ? C14 C16 1.39(3) . ? C15 C12 1.38(3) 2_566 ? C16 C11 1.41(3) 2_566 ? C17 C18 1.60(2) . ? C18 C19 1.47(3) . ? C18 C20 1.50(3) . ? C21 C26 1.37(3) . ? C21 C22 1.40(2) . ? C22 C23 1.30(2) . ? C23 C24 1.43(3) . ? C24 C25 1.34(3) . ? C25 C26 1.37(3) . ? C27 C30 1.48(2) . ? C27 C29 1.49(2) . ? C27 C28 1.55(3) . ? C31 C32 1.51(2) . ? C32 C34 1.47(3) . ? C32 C33 1.55(2) . ? C35 C36 1.36(2) . ? C35 C40 1.38(2) . ? C36 C37 1.33(3) . ? C37 C38 1.43(3) . ? C38 C39 1.31(3) . ? C39 C40 1.38(3) . ? C41 C42 1.50(3) . ? C41 C43 1.55(3) . ? C41 C44 1.56(3) . ? N1 C49 1.283(13) . ? N1 C45 1.293(14) . ? C45 C46 1.446(15) . ? C46 C47 1.328(15) . ? C47 C48 1.323(15) . ? C47 C50 1.639(17) . ? C48 C49 1.446(14) . ? C50 C51 1.417(14) . ? C50 C53 1.420(14) . ? C50 C52 1.420(14) . ? N2 C54 1.273(14) . ? N2 C58 1.279(13) . ? C54 C55 1.436(14) . ? C55 C56 1.316(14) . ? C56 C57 1.324(14) . ? C56 C59 1.632(17) . ? C57 C58 1.426(14) . ? C59 C60 1.404(15) . ? C59 C61 1.407(15) . ? C59 C62 1.431(15) . ? N3 C67 1.284(13) . ? N3 C63 1.282(13) . ? C63 C64 1.434(14) . ? C64 C65 1.334(14) . ? C65 C66 1.336(14) . ? C65 C68 1.632(17) . ? C66 C67 1.432(14) . ? C68 C70 1.420(14) . ? C68 C71 1.420(15) . ? C68 C69 1.431(15) . ? N4 C72 1.278(14) . ? N4 C76 1.289(13) . ? C72 C73 1.443(14) . ? C73 C74 1.333(15) . ? C74 C75 1.331(14) . ? C74 C77 1.633(17) . ? C75 C76 1.434(14) . ? C77 C80 1.408(15) . ? C77 C79 1.416(15) . ? C77 C78 1.439(15) . ? C1H C2H 1.52(2) . ? C2H C3H 1.50(2) . ? C3H C4H 1.48(2) . ? C4H C5H 1.49(2) . ? C5H C6H 1.508(19) . ? 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 O1 Rh1 O6 175.9(5) . . ? O1 Rh1 O3 89.4(5) . . ? O6 Rh1 O3 89.6(5) . . ? O1 Rh1 O7 90.2(5) . . ? O6 Rh1 O7 90.6(5) . . ? O3 Rh1 O7 176.3(5) . . ? O1 Rh1 Rh2 88.6(4) . . ? O6 Rh1 Rh2 87.5(3) . . ? O3 Rh1 Rh2 89.0(4) . . ? O7 Rh1 Rh2 87.4(4) . . ? O4 Rh2 O8 176.2(5) . . ? O4 Rh2 O2 90.3(5) . . ? O8 Rh2 O2 92.2(5) . . ? O4 Rh2 O5 91.2(5) . . ? O8 Rh2 O5 86.1(5) . . ? O2 Rh2 O5 176.4(5) . . ? O4 Rh2 Rh1 88.3(4) . . ? O8 Rh2 Rh1 89.0(3) . . ? O2 Rh2 Rh1 88.4(4) . . ? O5 Rh2 Rh1 88.4(4) . . ? O13 Rh3 O17 177.0(5) . . ? O13 Rh3 O11 90.9(5) . . ? O17 Rh3 O11 88.9(5) . . ? O13 Rh3 O15 88.9(5) . . ? O17 Rh3 O15 91.2(5) . . ? O11 Rh3 O15 176.3(5) . . ? O13 Rh3 Rh4 88.8(4) . . ? O17 Rh3 Rh4 88.3(4) . . ? O11 Rh3 Rh4 88.5(4) . . ? O15 Rh3 Rh4 87.8(4) . . ? O14 Rh4 O16 91.0(5) . . ? O14 Rh4 O12 90.2(5) . . ? O16 Rh4 O12 175.8(5) . . ? O14 Rh4 O18 175.1(5) . . ? O16 Rh4 O18 87.7(5) . . ? O12 Rh4 O18 90.7(5) . . ? O14 Rh4 Rh3 88.0(4) . . ? O16 Rh4 Rh3 88.6(4) . . ? O12 Rh4 Rh3 87.5(4) . . ? O18 Rh4 Rh3 87.3(3) . . ? C7 O1 Rh1 117.5(11) . . ? C7 O2 Rh2 118.7(11) . . ? C9 O3 Rh1 114.7(14) . . ? C9 O4 Rh2 117.0(13) . . ? C17 O5 Rh2 118.0(11) . . ? C17 O6 Rh1 118.8(11) . . ? C30 O7 Rh1 118.5(13) . . ? C30 O8 Rh2 119.4(12) . . ? C23 O9 C27 118.1(15) . . ? C21 O10 C18 125.8(15) . . ? C8 O11 Rh3 121.1(12) . . ? C8 O12 Rh4 119.6(11) . . ? C13 O13 Rh3 118.3(14) . . ? C13 O14 Rh4 117.1(13) . . ? C31 O15 Rh3 118.8(13) . . ? C31 O16 Rh4 118.4(12) . . ? C44 O17 Rh3 120.2(14) . . ? C44 O18 Rh4 117.7(13) . . ? C37 O19 C41 118.8(14) . . ? C35 O20 C32 120.3(16) . . ? C6 C1 C2 118.4(16) . . ? C6 C1 C7 119.6(16) . . ? C2 C1 C7 121.9(16) . . ? C3 C2 C1 121.4(18) . . ? C4 C3 C2 120.1(19) . . ? C5 C4 C3 118.3(17) . . ? C5 C4 C8 122.7(17) . . ? C3 C4 C8 118.9(16) . . ? C4 C5 C6 122(2) . . ? C1 C6 C5 120(2) . . ? O2 C7 O1 126.7(15) . . ? O2 C7 C1 118.0(15) . . ? O1 C7 C1 115.2(15) . . ? O11 C8 O12 123.4(16) . . ? O11 C8 C4 119.7(17) . . ? O12 C8 C4 117.0(17) . . ? O3 C9 O4 131(2) . . ? O3 C9 C10 115.2(18) . . ? O4 C9 C10 113.7(18) . . ? C12 C10 C11 118(2) . . ? C12 C10 C9 121(2) . . ? C11 C10 C9 121(2) . . ? C16 C11 C10 121(2) 2_566 . ? C10 C12 C15 119(2) . 2_566 ? O13 C13 O14 128(2) . . ? O13 C13 C14 116.9(18) . . ? O14 C13 C14 115.3(18) . . ? C15 C14 C16 117(2) . . ? C15 C14 C13 127.1(19) . . ? C16 C14 C13 116.2(19) . . ? C14 C15 C12 125(2) . 2_566 ? C14 C16 C11 120(2) . 2_566 ? O6 C17 O5 126.7(15) . . ? O6 C17 C18 115.8(16) . . ? O5 C17 C18 117.4(16) . . ? O10 C18 C19 107.9(17) . . ? O10 C18 C20 109.7(18) . . ? C19 C18 C20 111.7(19) . . ? O10 C18 C17 111.0(15) . . ? C19 C18 C17 104.7(18) . . ? C20 C18 C17 111.6(16) . . ? C26 C21 O10 111.8(19) . . ? C26 C21 C22 121(2) . . ? O10 C21 C22 127.0(18) . . ? C23 C22 C21 121.3(19) . . ? C22 C23 O9 128.2(19) . . ? C22 C23 C24 121(2) . . ? O9 C23 C24 110.8(19) . . ? C25 C24 C23 115(2) . . ? C24 C25 C26 127(2) . . ? C25 C26 C21 115(2) . . ? C30 C27 C29 114.3(17) . . ? C30 C27 O9 113.0(15) . . ? C29 C27 O9 109.5(15) . . ? C30 C27 C28 108.8(15) . . ? C29 C27 C28 109.0(16) . . ? O9 C27 C28 101.5(15) . . ? O7 C30 O8 125.4(19) . . ? O7 C30 C27 117.4(17) . . ? O8 C30 C27 117.2(17) . . ? O15 C31 O16 125.3(18) . . ? O15 C31 C32 118.8(19) . . ? O16 C31 C32 115.4(18) . . ? O20 C32 C34 105.2(16) . . ? O20 C32 C31 110.0(17) . . ? C34 C32 C31 106.4(17) . . ? O20 C32 C33 110.6(16) . . ? C34 C32 C33 111.5(18) . . ? C31 C32 C33 112.7(17) . . ? O20 C35 C36 127.6(19) . . ? O20 C35 C40 113.5(19) . . ? C36 C35 C40 119(2) . . ? C37 C36 C35 125(2) . . ? C36 C37 O19 124.6(19) . . ? C36 C37 C38 118(2) . . ? O19 C37 C38 117(2) . . ? C39 C38 C37 114(3) . . ? C38 C39 C40 129(3) . . ? C35 C40 C39 114(2) . . ? O19 C41 C42 106.5(15) . . ? O19 C41 C43 108.9(16) . . ? C42 C41 C43 110.3(17) . . ? O19 C41 C44 110.6(14) . . ? C42 C41 C44 111.3(17) . . ? C43 C41 C44 109.2(16) . . ? O17 C44 O18 126(2) . . ? O17 C44 C41 118.3(17) . . ? O18 C44 C41 115.1(17) . . ? C49 N1 C45 114.0(15) . . ? N1 C45 C46 124.5(16) . . ? C47 C46 C45 118.5(17) . . ? C48 C47 C46 117.7(16) . . ? C48 C47 C50 121.2(13) . . ? C46 C47 C50 119.5(14) . . ? C47 C48 C49 118.4(16) . . ? N1 C49 C48 125.5(17) . . ? C51 C50 C53 114.8(16) . . ? C51 C50 C52 109.6(15) . . ? C53 C50 C52 111.7(16) . . ? C51 C50 C47 107.4(14) . . ? C53 C50 C47 105.1(14) . . ? C52 C50 C47 107.7(14) . . ? C54 N2 C58 115.1(15) . . ? N2 C54 C55 122.6(16) . . ? C56 C55 C54 120.7(17) . . ? C55 C56 C57 117.4(16) . . ? C55 C56 C59 123.8(14) . . ? C57 C56 C59 118.8(13) . . ? C56 C57 C58 117.7(15) . . ? N2 C58 C57 126.1(15) . . ? C60 C59 C61 113.2(18) . . ? C60 C59 C62 108.8(17) . . ? C61 C59 C62 112.1(18) . . ? C60 C59 C56 108.0(16) . . ? C61 C59 C56 106.2(16) . . ? C62 C59 C56 108.4(16) . . ? C67 N3 C63 114.9(15) . . ? N3 C63 C64 124.8(16) . . ? C65 C64 C63 119.0(16) . . ? C64 C65 C66 117.2(15) . . ? C64 C65 C68 123.4(13) . . ? C66 C65 C68 119.4(13) . . ? C65 C66 C67 119.0(16) . . ? N3 C67 C66 124.5(16) . . ? C70 C68 C71 113.2(16) . . ? C70 C68 C69 111.5(16) . . ? C71 C68 C69 109.9(16) . . ? C70 C68 C65 107.8(14) . . ? C71 C68 C65 105.1(15) . . ? C69 C68 C65 109.2(15) . . ? C72 N4 C76 114.0(15) . . ? N4 C72 C73 125.1(17) . . ? C74 C73 C72 119.6(17) . . ? C75 C74 C73 114.9(16) . . ? C75 C74 C77 125.1(14) . . ? C73 C74 C77 119.5(14) . . ? C74 C75 C76 120.0(16) . . ? N4 C76 C75 124.4(15) . . ? C80 C77 C79 112.7(17) . . ? C80 C77 C78 109.7(17) . . ? C79 C77 C78 110.3(16) . . ? C80 C77 C74 105.3(16) . . ? C79 C77 C74 108.4(15) . . ? C78 C77 C74 110.3(15) . . ? C3H C2H C1H 112(2) . . ? C4H C3H C2H 116(2) . . ? C3H C4H C5H 115(2) . . ? C4H C5H C6H 115(2) . . ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 22.49 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.593 _refine_diff_density_min -0.531 _refine_diff_density_rms 0.119 data_r3 _publ-contact_author_name ; R. P. Bonar-Law ; _publ_contact_author_address ; Department of Chemistry, University of Liverpool Liverpool L69 7ZD, U.K. ; _publ_section_journal ' Chem Comm' _publ_section_title ; Dinuclear carboxylates as connectors for acids. Self-assembly of a molecular box. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H48 N2 O10 Rh2' _chemical_formula_weight 874.58 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' 'O' 'O' 0.0106 0.0060 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting rhombohedral _symmetry_space_group_name_H-M R3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' _cell_length_a 31.600(4) _cell_length_b 31.600(4) _cell_length_c 12.700(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 10983(3) _cell_formula_units_Z 9 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description cubic _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.4 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.190 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4032 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'STOE IPDS' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19768 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0260 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 22.48 _reflns_number_total 6376 _reflns_number_gt 5500 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE, 1997)' _computing_cell_refinement ? _computing_data_reduction 'X-RED (STOE, 1996)' _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 w=1/[\s^2^(Fo^2^)+(0.0899P)^2^+155.4622P] 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 0.34(13) _refine_ls_number_reflns 6376 _refine_ls_number_parameters 211 _refine_ls_number_restraints 152 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1767 _refine_ls_wR_factor_gt 0.1535 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.114 _refine_ls_shift/su_max 5.379 _refine_ls_shift/su_mean 0.779 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.46189(7) 0.00015(9) 0.8027(3) 0.0422(7) Uani 1 d . . . Rh2 Rh 0.53795(7) -0.00019(9) 0.8036(2) 0.0418(7) Uani 1 d . . . O1 O 0.4781(6) 0.0259(6) 0.6502(13) 0.040(4) Uiso 1 d U . . O2 O 0.5514(6) 0.0314(6) 0.6470(12) 0.056(4) Uiso 1 d U . . O3 O 0.4994(7) 0.0707(7) 0.8580(17) 0.065(6) Uiso 1 d U . . O4 O 0.5702(8) 0.0730(8) 0.8499(17) 0.060(6) Uiso 1 d U . . O5 O 0.5847(9) 0.0985(8) 0.4872(19) 0.106(8) Uiso 1 d DU . . O6 O 0.6230(8) 0.1780(8) 0.8330(17) 0.102(7) Uiso 1 d DU . . C1 C 0.5185(12) 0.0384(7) 0.6129(14) 0.058(5) Uiso 1 d U . . C2 C 0.5355(15) 0.0681(6) 0.5061(12) 0.064(4) Uiso 1 d U . . C3 C 0.5145(13) 0.0302(5) 0.4188(13) 0.073(4) Uiso 1 d U . . H3A H 0.5275 0.0085 0.4244 0.110 Uiso 1 calc R . . H3B H 0.5233 0.0464 0.3516 0.110 Uiso 1 calc R . . H3C H 0.4796 0.0119 0.4250 0.110 Uiso 1 calc R . . C4 C 0.5112(8) 0.1016(7) 0.4939(17) 0.038(5) Uiso 1 d U . . H4A H 0.5235 0.1262 0.5477 0.057 Uiso 1 calc R . . H4B H 0.4764 0.0817 0.5008 0.057 Uiso 1 calc R . . H4C H 0.5190 0.1169 0.4259 0.057 Uiso 1 calc R . . C5 C 0.5993(9) 0.1378(8) 0.6625(19) 0.091(6) Uiso 1 d DU . . H5 H 0.5660 0.1222 0.6774 0.109 Uiso 1 calc R . . C6 C 0.6168(8) 0.1318(6) 0.5659(16) 0.073(5) Uiso 1 d DU . . C7 C 0.6656(10) 0.1566(9) 0.550(2) 0.111(8) Uiso 1 d DU . . H7 H 0.6766 0.1532 0.4843 0.134 Uiso 1 calc R . . C8 C 0.7017(12) 0.1875(11) 0.624(2) 0.121(9) Uiso 1 d DU . . H8 H 0.7347 0.2047 0.6061 0.145 Uiso 1 calc R . . C9 C 0.6857(9) 0.1905(9) 0.720(2) 0.091(6) Uiso 1 d DU . . H9 H 0.7079 0.2064 0.7741 0.109 Uiso 1 calc R . . C10 C 0.6356(9) 0.1696(9) 0.738(2) 0.090(6) Uiso 1 d DU . . C11 C 0.5750(11) 0.1519(4) 0.8738(10) 0.044(3) Uiso 1 d U . . C12 C 0.5820(14) 0.1618(5) 0.9967(11) 0.069(3) Uiso 1 d U . . H12A H 0.5994 0.1468 1.0253 0.103 Uiso 1 calc R . . H12B H 0.5506 0.1482 1.0299 0.103 Uiso 1 calc R . . H12C H 0.6002 0.1964 1.0093 0.103 Uiso 1 calc R . . C13 C 0.5490(6) 0.1765(6) 0.8364(13) 0.031(4) Uiso 1 d U . . H13A H 0.5460 0.1739 0.7612 0.047 Uiso 1 calc R . . H13B H 0.5668 0.2104 0.8561 0.047 Uiso 1 calc R . . H13C H 0.5170 0.1614 0.8675 0.047 Uiso 1 calc R . . C14 C 0.5451(11) 0.0934(5) 0.8590(11) 0.041(4) Uiso 1 d U . . O7 O 0.4298(6) -0.0685(5) 0.7532(13) 0.049(4) Uiso 1 d DU . . O8 O 0.5004(6) -0.0721(6) 0.7575(15) 0.049(5) Uiso 1 d DU . . C15 C 0.4552(7) -0.0886(6) 0.7392(12) 0.061(6) Uiso 1 d DU . . C16 C 0.4312(11) -0.1380(5) 0.6932(14) 0.076(5) Uiso 1 d DU . . H16A H 0.4540 -0.1498 0.6911 0.114 Uiso 1 calc R . . H16B H 0.4206 -0.1369 0.6230 0.114 Uiso 1 calc R . . H16C H 0.4036 -0.1596 0.7354 0.114 Uiso 1 calc R . . O9 O 0.4560(5) -0.0165(5) 0.9535(11) 0.042(4) Uiso 1 d DU . . O10 O 0.5223(6) -0.0272(6) 0.9523(12) 0.043(4) Uiso 1 d DU . . C17 C 0.4841(6) -0.0302(5) 0.9965(12) 0.050(5) Uiso 1 d DU . . C18 C 0.4742(12) -0.0490(7) 1.1069(11) 0.076(5) Uiso 1 d DU . . H18A H 0.4988 -0.0565 1.1286 0.114 Uiso 1 calc R . . H18B H 0.4427 -0.0779 1.1104 0.114 Uiso 1 calc R . . H18C H 0.4749 -0.0245 1.1527 0.114 Uiso 1 calc R . . N1 N 0.3908(5) -0.0001(7) 0.8065(18) 0.054(7) Uiso 1 d DU . . C21 C 0.3852(6) 0.0364(8) 0.770(3) 0.076(9) Uiso 1 d DU . . H21 H 0.4130 0.0658 0.7533 0.091 Uiso 1 calc R . . C22 C 0.3409(5) 0.0328(7) 0.7561(18) 0.065(7) Uiso 1 d DU . . H22 H 0.3386 0.0562 0.7163 0.079 Uiso 1 calc R . . C23 C 0.2991(5) -0.0054(6) 0.8006(16) 0.042(6) Uiso 1 d DU . . C24 C 0.3061(6) -0.0407(7) 0.840(2) 0.045(6) Uiso 1 d DU . . H24 H 0.2792 -0.0690 0.8652 0.054 Uiso 1 calc R . . C25 C 0.3508(6) -0.0370(7) 0.844(2) 0.053(7) Uiso 1 d DU . . H25 H 0.3531 -0.0622 0.8761 0.063 Uiso 1 calc R . . C26 C 0.2499(5) -0.0085(5) 0.7958(11) 0.051(6) Uiso 1 d DU . . C27 C 0.2494(8) 0.0222(8) 0.7069(15) 0.071(5) Uiso 1 d DU . . H27A H 0.2178 0.0195 0.7027 0.106 Uiso 1 calc R . . H27B H 0.2562 0.0112 0.6421 0.106 Uiso 1 calc R . . H27C H 0.2738 0.0557 0.7188 0.106 Uiso 1 calc R . . C28 C 0.2415(10) 0.0129(11) 0.8988(17) 0.120(12) Uiso 1 d DU . . H28A H 0.2100 0.0107 0.8960 0.180 Uiso 1 calc R . . H28B H 0.2665 0.0466 0.9057 0.180 Uiso 1 calc R . . H28C H 0.2427 -0.0052 0.9582 0.180 Uiso 1 calc R . . C29 C 0.2061(6) -0.0600(6) 0.7878(18) 0.076(5) Uiso 1 d DU . . H29A H 0.1766 -0.0583 0.7847 0.114 Uiso 1 calc R . . H29B H 0.2052 -0.0786 0.8485 0.114 Uiso 1 calc R . . H29C H 0.2089 -0.0755 0.7253 0.114 Uiso 1 calc R . . N2 N 0.6095(6) 0.0029(7) 0.808(2) 0.049(7) Uiso 1 d DU . . C31 C 0.6507(6) 0.0402(7) 0.774(2) 0.039(7) Uiso 1 d DU . . H31 H 0.6498 0.0675 0.7498 0.046 Uiso 1 calc R . . C32 C 0.6951(6) 0.0420(6) 0.7719(17) 0.043(6) Uiso 1 d DU . . H32 H 0.7230 0.0700 0.7490 0.051 Uiso 1 calc R . . C33 C 0.6976(5) 0.0007(7) 0.805(2) 0.043(7) Uiso 1 d DU . . C34 C 0.6538(7) -0.0400(8) 0.832(3) 0.061(10) Uiso 1 d DU . . H34 H 0.6525 -0.0695 0.8467 0.073 Uiso 1 calc R . . C35 C 0.6113(7) -0.0367(8) 0.839(2) 0.043(8) Uiso 1 d DU . . H35 H 0.5831 -0.0632 0.8654 0.051 Uiso 1 calc R . . C36 C 0.7468(5) 0.0027(6) 0.8051(13) 0.042(6) Uiso 1 d DU . . C37 C 0.7871(7) 0.0456(8) 0.7502(18) 0.083(6) Uiso 1 d DU . . H37A H 0.8168 0.0445 0.7571 0.124 Uiso 1 calc R . . H37B H 0.7914 0.0752 0.7812 0.124 Uiso 1 calc R . . H37C H 0.7791 0.0446 0.6770 0.124 Uiso 1 calc R . . C38 C 0.7425(12) -0.0418(11) 0.748(2) 0.157(15) Uiso 1 d DU . . H38A H 0.7737 -0.0401 0.7482 0.236 Uiso 1 calc R . . H38B H 0.7322 -0.0422 0.6768 0.236 Uiso 1 calc R . . H38C H 0.7189 -0.0710 0.7834 0.236 Uiso 1 calc R . . C39 C 0.7611(7) 0.0010(8) 0.9179(12) 0.061(5) Uiso 1 d DU . . H39A H 0.7930 0.0043 0.9194 0.091 Uiso 1 calc R . . H39B H 0.7379 -0.0297 0.9489 0.091 Uiso 1 calc R . . H39C H 0.7616 0.0272 0.9570 0.091 Uiso 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 0.0397(13) 0.0688(16) 0.0276(14) -0.0075(9) -0.0049(9) 0.0342(12) Rh2 0.0386(13) 0.0702(15) 0.0270(15) -0.0028(10) -0.0009(9) 0.0350(12) _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 O7 1.981(15) . ? Rh1 O1 2.064(17) . ? Rh1 O3 2.056(19) . ? Rh1 O9 1.969(14) . ? Rh1 N1 2.243(13) . ? Rh1 Rh2 2.4088(9) . ? Rh2 O10 2.029(16) . ? Rh2 O8 2.054(18) . ? Rh2 O4 2.09(2) . ? Rh2 O2 2.170(15) . ? Rh2 N2 2.213(14) . ? O1 C1 1.23(4) . ? O2 C1 1.24(4) . ? O3 C14 1.25(3) . ? O4 C14 1.25(3) . ? O5 C2 1.38(4) . ? O5 C6 1.44(3) . ? O6 C10 1.33(3) . ? O6 C11 1.41(3) . ? C1 C2 1.58(2) . ? C2 C3 1.52(2) . ? C2 C4 1.60(4) . ? C5 C6 1.40(3) . ? C5 C10 1.45(3) . ? C6 C7 1.35(3) . ? C7 C8 1.42(4) . ? C8 C9 1.35(4) . ? C9 C10 1.40(3) . ? C11 C13 1.46(4) . ? C11 C12 1.585(18) . ? C11 C14 1.615(19) . ? O7 C15 1.261(14) . ? O8 C15 1.274(14) . ? C15 C16 1.474(19) . ? O9 C17 1.291(14) . ? O10 C17 1.289(14) . ? C17 C18 1.493(19) . ? N1 C25 1.307(12) . ? N1 C21 1.334(13) . ? C21 C22 1.356(13) . ? C22 C23 1.389(13) . ? C23 C24 1.335(12) . ? C23 C26 1.508(12) . ? C24 C25 1.360(12) . ? C26 C27 1.496(13) . ? C26 C29 1.524(14) . ? C26 C28 1.557(15) . ? N2 C31 1.319(12) . ? N2 C35 1.340(13) . ? C31 C32 1.374(13) . ? C32 C33 1.412(12) . ? C33 C34 1.382(13) . ? C33 C36 1.523(12) . ? C34 C35 1.398(13) . ? C36 C37 1.489(14) . ? C36 C39 1.512(14) . ? C36 C38 1.526(15) . ? 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 O7 Rh1 O1 91.4(7) . . ? O7 Rh1 O3 175.7(7) . . ? O1 Rh1 O3 89.9(7) . . ? O7 Rh1 O9 95.1(6) . . ? O1 Rh1 O9 171.6(7) . . ? O3 Rh1 O9 83.3(7) . . ? O7 Rh1 N1 92.3(7) . . ? O1 Rh1 N1 94.1(7) . . ? O3 Rh1 N1 91.8(8) . . ? O9 Rh1 N1 91.0(6) . . ? O7 Rh1 Rh2 87.8(5) . . ? O1 Rh1 Rh2 87.4(5) . . ? O3 Rh1 Rh2 88.1(6) . . ? O9 Rh1 Rh2 87.5(4) . . ? N1 Rh1 Rh2 178.4(5) . . ? O10 Rh2 O8 85.1(7) . . ? O10 Rh2 O4 94.9(8) . . ? O8 Rh2 O4 174.9(7) . . ? O10 Rh2 O2 175.6(6) . . ? O8 Rh2 O2 96.8(7) . . ? O4 Rh2 O2 82.8(7) . . ? O10 Rh2 N2 91.4(7) . . ? O8 Rh2 N2 93.9(8) . . ? O4 Rh2 N2 91.3(8) . . ? O2 Rh2 N2 92.4(7) . . ? O10 Rh2 Rh1 88.4(4) . . ? O8 Rh2 Rh1 88.8(5) . . ? O4 Rh2 Rh1 86.1(6) . . ? O2 Rh2 Rh1 87.7(5) . . ? N2 Rh2 Rh1 177.3(6) . . ? C1 O1 Rh1 120.1(16) . . ? C1 O2 Rh2 114.3(15) . . ? C14 O3 Rh1 119.9(15) . . ? C14 O4 Rh2 120.7(17) . . ? C2 O5 C6 122(2) . . ? C10 O6 C11 124(2) . . ? O1 C1 O2 129.6(18) . . ? O1 C1 C2 121(3) . . ? O2 C1 C2 110(3) . . ? O5 C2 C3 109(3) . . ? O5 C2 C1 119(3) . . ? C3 C2 C1 105.8(14) . . ? O5 C2 C4 105.7(13) . . ? C3 C2 C4 107(3) . . ? C1 C2 C4 110(3) . . ? C6 C5 C10 117(2) . . ? C7 C6 C5 118(2) . . ? C7 C6 O5 120(2) . . ? C5 C6 O5 122(2) . . ? C6 C7 C8 126(3) . . ? C9 C8 C7 117(3) . . ? C8 C9 C10 120(3) . . ? C9 C10 O6 116(2) . . ? C9 C10 C5 122(2) . . ? O6 C10 C5 122(2) . . ? O6 C11 C13 107.3(11) . . ? O6 C11 C12 104(2) . . ? C13 C11 C12 106(2) . . ? O6 C11 C14 118(2) . . ? C13 C11 C14 114(2) . . ? C12 C11 C14 106.5(11) . . ? O3 C14 O4 123.5(15) . . ? O3 C14 C11 120(3) . . ? O4 C14 C11 116(3) . . ? C15 O7 Rh1 119.4(12) . . ? C15 O8 Rh2 114.4(13) . . ? O7 C15 O8 129.4(16) . . ? O7 C15 C16 118.1(17) . . ? O8 C15 C16 112.5(16) . . ? C17 O9 Rh1 120.8(10) . . ? C17 O10 Rh2 117.3(12) . . ? O9 C17 O10 124.5(14) . . ? O9 C17 C18 119.2(16) . . ? O10 C17 C18 116.2(16) . . ? C25 N1 C21 114.2(12) . . ? C25 N1 Rh1 122.1(11) . . ? C21 N1 Rh1 123.7(11) . . ? N1 C21 C22 123.4(15) . . ? C21 C22 C23 120.9(14) . . ? C24 C23 C22 113.2(10) . . ? C24 C23 C26 123.8(11) . . ? C22 C23 C26 122.8(11) . . ? C23 C24 C25 122.8(13) . . ? N1 C25 C24 124.2(14) . . ? C27 C26 C23 109.6(11) . . ? C27 C26 C29 110.1(13) . . ? C23 C26 C29 115.4(12) . . ? C27 C26 C28 106.9(14) . . ? C23 C26 C28 109.5(14) . . ? C29 C26 C28 105.0(13) . . ? C31 N2 C35 116.4(12) . . ? C31 N2 Rh2 124.2(12) . . ? C35 N2 Rh2 119.1(11) . . ? N2 C31 C32 125.0(14) . . ? C31 C32 C33 119.0(13) . . ? C34 C33 C32 116.2(11) . . ? C34 C33 C36 124.5(13) . . ? C32 C33 C36 119.3(12) . . ? C33 C34 C35 119.9(15) . . ? N2 C35 C34 123.0(15) . . ? C37 C36 C39 109.9(13) . . ? C37 C36 C33 115.5(12) . . ? C39 C36 C33 108.5(13) . . ? C37 C36 C38 104.8(14) . . ? C39 C36 C38 107.8(14) . . ? C33 C36 C38 110.0(15) . . ? _diffrn_measured_fraction_theta_max 0.333 _diffrn_reflns_theta_full 22.48 _diffrn_measured_fraction_theta_full 0.333 _refine_diff_density_max 1.179 _refine_diff_density_min -0.614 _refine_diff_density_rms 0.141