# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Joseph Fox' _publ_contact_author_email JMFOX@UDEL.EDU _publ_section_title ; The chiral crown conformation in paddlewheel complexes ; loop_ _publ_author_name 'Joseph Fox' 'David T. Boruta' 'Andrew DeAngelis' 'Jean-Bernard Lubin' 'James N. Plampin' 'Glenn P. A. Yap' # Attachment 'joef086.cif' data_joef086 _database_code_depnum_ccdc_archive 'CCDC 761719' #TrackingRef 'joef086.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C85 H84 N6 O16 Rh2' _chemical_formula_weight 1651.40 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 13.412(3) _cell_length_b 21.783(5) _cell_length_c 27.323(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7982(3) _cell_formula_units_Z 4 _cell_measurement_temperature 170(2) _cell_measurement_reflns_used 1024 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 28.19 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3416 _exptl_absorpt_coefficient_mu 0.483 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8986 _exptl_absorpt_correction_T_max 0.9206 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 170(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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 94308 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 28.31 _reflns_number_total 19746 _reflns_number_gt 18922 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0455P)^2^+1.8574P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881; 9019 Friedel pairs measured' _refine_ls_abs_structure_Flack -0.043(11) _refine_ls_number_reflns 19746 _refine_ls_number_parameters 997 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0317 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0772 _refine_ls_wR_factor_gt 0.0748 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.003 _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 0.660739(12) 0.040182(7) 0.024841(5) 0.01842(4) Uani 1 1 d . . . Rh2 Rh 0.655716(12) -0.015420(7) 0.100417(5) 0.01840(4) Uani 1 1 d . . . N1 N 0.44468(14) 0.18228(8) 0.09628(7) 0.0254(4) Uani 1 1 d . . . N2 N 0.36791(13) -0.05466(8) -0.02575(7) 0.0272(4) Uani 1 1 d . . . N3 N 0.75296(14) -0.14986(8) -0.05314(7) 0.0250(4) Uani 1 1 d . . . N4 N 0.92442(14) 0.15229(9) 0.09928(7) 0.0279(4) Uani 1 1 d . . . N5 N 0.67586(14) 0.08262(8) -0.04903(6) 0.0259(4) Uani 1 1 d . . . N6 N 0.84003(16) 0.06197(8) -0.32659(6) 0.0253(3) Uani 1 1 d . . . O1 O 0.59629(11) 0.11223(7) 0.06112(5) 0.0222(3) Uani 1 1 d . . . O2 O 0.58923(12) 0.05851(7) 0.13183(5) 0.0239(3) Uani 1 1 d . . . O3 O 0.37189(13) 0.08910(8) 0.07659(7) 0.0324(4) Uani 1 1 d . . . O4 O 0.48956(15) 0.28484(8) 0.09512(7) 0.0380(4) Uani 1 1 d . . . O5 O 0.52319(11) 0.00839(7) 0.00902(5) 0.0237(3) Uani 1 1 d . . . O6 O 0.51838(11) -0.04580(7) 0.07958(5) 0.0246(3) Uani 1 1 d . . . O7 O 0.50400(14) -0.11979(9) -0.03564(7) 0.0401(4) Uani 1 1 d . . . O8 O 0.24543(14) 0.01720(9) -0.04317(7) 0.0416(4) Uani 1 1 d . . . O9 O 0.71988(11) -0.03660(7) -0.00648(5) 0.0241(3) Uani 1 1 d . . . O10 O 0.71852(12) -0.08751(7) 0.06554(5) 0.0239(3) Uani 1 1 d . . . O11 O 0.82212(14) -0.06970(8) -0.09875(6) 0.0391(4) Uani 1 1 d . . . O12 O 0.66798(14) -0.24015(7) -0.03435(6) 0.0358(4) Uani 1 1 d . . . O13 O 0.79771(11) 0.07243(7) 0.04509(5) 0.0238(3) Uani 1 1 d . . . O14 O 0.79369(11) 0.01995(7) 0.11609(5) 0.0248(3) Uani 1 1 d . . . O15 O 1.03791(15) 0.17371(10) 0.03783(8) 0.0486(5) Uani 1 1 d . . . O16 O 0.79074(15) 0.16315(9) 0.15214(7) 0.0411(4) Uani 1 1 d . . . C1 C 0.57326(15) 0.10502(9) 0.10563(8) 0.0219(4) Uani 1 1 d . . . C2 C 0.52298(17) 0.16091(10) 0.12972(7) 0.0240(4) Uani 1 1 d . . . H2A H 0.5746 0.1940 0.1299 0.029 Uiso 1 1 calc R . . C3 C 0.48674(18) 0.15509(11) 0.18354(8) 0.0303(5) Uani 1 1 d . . . C4 C 0.5776(2) 0.14196(14) 0.21618(9) 0.0385(6) Uani 1 1 d . . . H4A H 0.5569 0.1415 0.2506 0.058 Uiso 1 1 calc R . . H4B H 0.6279 0.1740 0.2113 0.058 Uiso 1 1 calc R . . H4C H 0.6060 0.1020 0.2075 0.058 Uiso 1 1 calc R . . C5 C 0.4066(2) 0.10574(13) 0.19004(9) 0.0390(6) Uani 1 1 d . . . H5A H 0.3882 0.1029 0.2247 0.058 Uiso 1 1 calc R . . H5B H 0.4327 0.0661 0.1789 0.058 Uiso 1 1 calc R . . H5C H 0.3477 0.1166 0.1707 0.058 Uiso 1 1 calc R . . C6 C 0.4433(2) 0.21746(13) 0.19913(10) 0.0432(6) Uani 1 1 d . . . H6A H 0.4245 0.2158 0.2338 0.065 Uiso 1 1 calc R . . H6B H 0.3844 0.2267 0.1793 0.065 Uiso 1 1 calc R . . H6C H 0.4935 0.2496 0.1943 0.065 Uiso 1 1 calc R . . C7 C 0.37792(17) 0.14428(11) 0.07085(8) 0.0272(4) Uani 1 1 d . . . C8 C 0.32087(17) 0.18518(11) 0.03803(8) 0.0283(5) Uani 1 1 d . . . C9 C 0.24679(18) 0.17140(13) 0.00470(9) 0.0339(5) Uani 1 1 d . . . H9A H 0.2241 0.1306 -0.0003 0.041 Uiso 1 1 calc R . . C10 C 0.20708(19) 0.22089(14) -0.02124(10) 0.0394(6) Uani 1 1 d . . . H10A H 0.1558 0.2134 -0.0445 0.047 Uiso 1 1 calc R . . C11 C 0.2395(2) 0.28020(14) -0.01434(10) 0.0422(6) Uani 1 1 d . . . H11A H 0.2097 0.3125 -0.0325 0.051 Uiso 1 1 calc R . . C12 C 0.3149(2) 0.29369(12) 0.01867(10) 0.0384(6) Uani 1 1 d . . . H12A H 0.3383 0.3345 0.0231 0.046 Uiso 1 1 calc R . . C13 C 0.35468(18) 0.24488(10) 0.04490(8) 0.0304(5) Uani 1 1 d . . . C14 C 0.43734(18) 0.24358(10) 0.08075(8) 0.0287(4) Uani 1 1 d . . . C15 C 0.48165(16) -0.02644(9) 0.03984(7) 0.0228(4) Uani 1 1 d . . . C16 C 0.37282(15) -0.04257(10) 0.02729(8) 0.0257(4) Uani 1 1 d . . . H16A H 0.3346 -0.0037 0.0323 0.031 Uiso 1 1 calc R . . C17 C 0.31871(17) -0.09119(11) 0.05898(9) 0.0319(5) Uani 1 1 d . . . C18 C 0.3122(2) -0.06757(15) 0.11158(10) 0.0428(6) Uani 1 1 d . . . H18A H 0.2700 -0.0952 0.1309 0.064 Uiso 1 1 calc R . . H18B H 0.2831 -0.0263 0.1116 0.064 Uiso 1 1 calc R . . H18C H 0.3791 -0.0661 0.1259 0.064 Uiso 1 1 calc R . . C19 C 0.2118(2) -0.09666(15) 0.03894(12) 0.0463(7) Uani 1 1 d . . . H19A H 0.1736 -0.1250 0.0595 0.069 Uiso 1 1 calc R . . H19B H 0.2140 -0.1122 0.0053 0.069 Uiso 1 1 calc R . . H19C H 0.1800 -0.0562 0.0393 0.069 Uiso 1 1 calc R . . C20 C 0.3687(2) -0.15436(12) 0.05644(12) 0.0433(7) Uani 1 1 d . . . H20A H 0.3329 -0.1831 0.0777 0.065 Uiso 1 1 calc R . . H20B H 0.4381 -0.1509 0.0674 0.065 Uiso 1 1 calc R . . H20C H 0.3671 -0.1694 0.0227 0.065 Uiso 1 1 calc R . . C21 C 0.43610(18) -0.08998(11) -0.05256(9) 0.0312(5) Uani 1 1 d . . . C22 C 0.40683(19) -0.08270(12) -0.10496(9) 0.0344(5) Uani 1 1 d . . . C23 C 0.4441(2) -0.11092(15) -0.14620(11) 0.0466(7) Uani 1 1 d . . . H23A H 0.4978 -0.1393 -0.1445 0.056 Uiso 1 1 calc R . . C24 C 0.3984(3) -0.09552(17) -0.19090(11) 0.0537(8) Uani 1 1 d . . . H24A H 0.4220 -0.1138 -0.2203 0.064 Uiso 1 1 calc R . . C25 C 0.3206(3) -0.05476(15) -0.19311(10) 0.0523(8) Uani 1 1 d . . . H25A H 0.2917 -0.0455 -0.2240 0.063 Uiso 1 1 calc R . . C26 C 0.2829(2) -0.02643(13) -0.15119(10) 0.0434(6) Uani 1 1 d . . . H26A H 0.2292 0.0019 -0.1528 0.052 Uiso 1 1 calc R . . C27 C 0.32778(18) -0.04185(11) -0.10715(9) 0.0331(5) Uani 1 1 d . . . C28 C 0.30500(18) -0.02093(11) -0.05654(9) 0.0311(5) Uani 1 1 d . . . C29 C 0.73571(15) -0.08290(10) 0.02000(8) 0.0226(4) Uani 1 1 d . . . C30 C 0.78483(17) -0.13979(10) -0.00230(7) 0.0231(4) Uani 1 1 d . . . H30A H 0.7577 -0.1754 0.0166 0.028 Uiso 1 1 calc R . . C31 C 0.89989(18) -0.14094(11) 0.00677(9) 0.0294(5) Uani 1 1 d . . . C32 C 0.9180(2) -0.15862(16) 0.06043(10) 0.0456(7) Uani 1 1 d . . . H32A H 0.9892 -0.1549 0.0679 0.068 Uiso 1 1 calc R . . H32B H 0.8966 -0.2011 0.0658 0.068 Uiso 1 1 calc R . . H32C H 0.8798 -0.1312 0.0818 0.068 Uiso 1 1 calc R . . C33 C 0.9489(2) -0.07824(14) -0.00235(13) 0.0488(7) Uani 1 1 d . . . H33A H 1.0209 -0.0814 0.0033 0.073 Uiso 1 1 calc R . . H33B H 0.9204 -0.0478 0.0200 0.073 Uiso 1 1 calc R . . H33C H 0.9368 -0.0655 -0.0362 0.073 Uiso 1 1 calc R . . C34 C 0.9468(2) -0.18981(15) -0.02525(12) 0.0520(8) Uani 1 1 d . . . H34A H 1.0181 -0.1929 -0.0177 0.078 Uiso 1 1 calc R . . H34B H 0.9383 -0.1787 -0.0598 0.078 Uiso 1 1 calc R . . H34C H 0.9145 -0.2294 -0.0190 0.078 Uiso 1 1 calc R . . C35 C 0.69526(18) -0.20260(11) -0.06368(9) 0.0285(5) Uani 1 1 d . . . C36 C 0.67877(19) -0.20171(12) -0.11780(9) 0.0332(5) Uani 1 1 d . . . C37 C 0.6289(2) -0.24298(14) -0.14769(11) 0.0445(7) Uani 1 1 d . . . H37A H 0.5959 -0.2781 -0.1348 0.053 Uiso 1 1 calc R . . C38 C 0.6297(3) -0.22999(16) -0.19792(12) 0.0533(8) Uani 1 1 d . . . H38A H 0.5957 -0.2569 -0.2196 0.064 Uiso 1 1 calc R . . C39 C 0.6782(2) -0.17953(16) -0.21686(10) 0.0498(8) Uani 1 1 d . . . H39A H 0.6779 -0.1727 -0.2512 0.060 Uiso 1 1 calc R . . C40 C 0.7277(2) -0.13846(14) -0.18624(9) 0.0408(6) Uani 1 1 d . . . H40A H 0.7610 -0.1034 -0.1989 0.049 Uiso 1 1 calc R . . C41 C 0.72624(19) -0.15086(12) -0.13665(8) 0.0310(5) Uani 1 1 d . . . C42 C 0.77388(17) -0.11618(11) -0.09538(8) 0.0281(4) Uani 1 1 d . . . C43 C 0.83285(16) 0.05640(9) 0.08611(7) 0.0226(4) Uani 1 1 d . . . C44 C 0.93555(16) 0.08536(10) 0.09673(9) 0.0267(4) Uani 1 1 d . . . H44A H 0.9757 0.0778 0.0665 0.032 Uiso 1 1 calc R . . C45 C 0.99905(18) 0.05837(12) 0.13914(10) 0.0343(5) Uani 1 1 d . . . C46 C 1.0140(2) -0.01035(13) 0.12938(12) 0.0441(6) Uani 1 1 d . . . H46A H 1.0617 -0.0271 0.1531 0.066 Uiso 1 1 calc R . . H46B H 1.0399 -0.0161 0.0962 0.066 Uiso 1 1 calc R . . H46C H 0.9501 -0.0317 0.1327 0.066 Uiso 1 1 calc R . . C47 C 0.9516(2) 0.06807(15) 0.18947(10) 0.0463(7) Uani 1 1 d . . . H47A H 0.9489 0.1121 0.1968 0.069 Uiso 1 1 calc R . . H47B H 0.9916 0.0472 0.2144 0.069 Uiso 1 1 calc R . . H47C H 0.8839 0.0512 0.1895 0.069 Uiso 1 1 calc R . . C48 C 1.1019(2) 0.08951(16) 0.13815(14) 0.0528(8) Uani 1 1 d . . . H48A H 1.0943 0.1334 0.1450 0.079 Uiso 1 1 calc R . . H48B H 1.1321 0.0840 0.1058 0.079 Uiso 1 1 calc R . . H48C H 1.1449 0.0709 0.1631 0.079 Uiso 1 1 calc R . . C49 C 0.98030(19) 0.19125(12) 0.06828(10) 0.0347(5) Uani 1 1 d . . . C50 C 0.9490(2) 0.25479(12) 0.08075(10) 0.0361(5) Uani 1 1 d . . . C51 C 0.9803(2) 0.31070(13) 0.06183(12) 0.0451(7) Uani 1 1 d . . . H51A H 1.0316 0.3130 0.0379 0.054 Uiso 1 1 calc R . . C52 C 0.9331(3) 0.36324(14) 0.07942(13) 0.0524(8) Uani 1 1 d . . . H52A H 0.9532 0.4023 0.0676 0.063 Uiso 1 1 calc R . . C53 C 0.8580(3) 0.35960(13) 0.11365(13) 0.0522(8) Uani 1 1 d . . . H53A H 0.8267 0.3963 0.1245 0.063 Uiso 1 1 calc R . . C54 C 0.8268(2) 0.30331(13) 0.13282(11) 0.0438(6) Uani 1 1 d . . . H54A H 0.7755 0.3009 0.1567 0.053 Uiso 1 1 calc R . . C55 C 0.87401(19) 0.25131(12) 0.11534(9) 0.0348(5) Uani 1 1 d . . . C56 C 0.85444(18) 0.18538(11) 0.12622(9) 0.0307(5) Uani 1 1 d . . . C57 C 0.70275(18) 0.08197(10) -0.08872(8) 0.0270(4) Uani 1 1 d . . . C58 C 0.73329(19) 0.08005(11) -0.13943(8) 0.0292(5) Uani 1 1 d . . . C59 C 0.6925(2) 0.03507(13) -0.16935(9) 0.0428(6) Uani 1 1 d . . . H59A H 0.6459 0.0064 -0.1566 0.051 Uiso 1 1 calc R . . C60 C 0.7206(2) 0.03244(13) -0.21805(9) 0.0444(7) Uani 1 1 d . . . H60A H 0.6930 0.0021 -0.2390 0.053 Uiso 1 1 calc R . . C61 C 0.78915(19) 0.07437(11) -0.23606(8) 0.0296(5) Uani 1 1 d . . . C62 C 0.8305(2) 0.11928(11) -0.20615(8) 0.0321(5) Uani 1 1 d . . . H62A H 0.8774 0.1478 -0.2189 0.039 Uiso 1 1 calc R . . C63 C 0.8020(2) 0.12182(12) -0.15719(8) 0.0324(5) Uani 1 1 d . . . H63A H 0.8296 0.1521 -0.1361 0.039 Uiso 1 1 calc R . . C64 C 0.81915(18) 0.06922(11) -0.28671(8) 0.0289(5) Uani 1 1 d . . . C65 C 0.4751(4) 0.18664(19) 0.34415(13) 0.0679(11) Uani 1 1 d . . . H65A H 0.5228 0.1612 0.3284 0.082 Uiso 1 1 calc R . . C66 C 0.3962(5) 0.1610(2) 0.36762(17) 0.0855(14) Uani 1 1 d . . . H66A H 0.3893 0.1176 0.3685 0.103 Uiso 1 1 calc R . . C67 C 0.3260(5) 0.1974(4) 0.3902(2) 0.115(2) Uani 1 1 d . . . H67A H 0.2697 0.1793 0.4056 0.138 Uiso 1 1 calc R . . C68 C 0.3376(6) 0.2582(5) 0.3903(3) 0.143(4) Uani 1 1 d . . . H68A H 0.2905 0.2832 0.4070 0.171 Uiso 1 1 calc R . . C69 C 0.4134(5) 0.2842(2) 0.3678(2) 0.096(2) Uani 1 1 d . . . H69A H 0.4192 0.3276 0.3681 0.115 Uiso 1 1 calc R . . C70 C 0.4860(4) 0.2495(2) 0.34318(14) 0.0754(13) Uani 1 1 d . . . C71 C 0.5714(5) 0.2758(3) 0.31820(19) 0.124(3) Uani 1 1 d . . . H71A H 0.5591 0.3195 0.3119 0.186 Uiso 1 1 calc R . . H71B H 0.5819 0.2544 0.2871 0.186 Uiso 1 1 calc R . . H71C H 0.6308 0.2714 0.3388 0.186 Uiso 1 1 calc R . . C72 C 0.5021(2) 0.49036(15) 0.16141(14) 0.0546(8) Uani 1 1 d . . . H72A H 0.4637 0.5222 0.1470 0.066 Uiso 1 1 calc R . . C73 C 0.5254(3) 0.49310(17) 0.21027(15) 0.0626(9) Uani 1 1 d . . . H73A H 0.5026 0.5269 0.2292 0.075 Uiso 1 1 calc R . . C74 C 0.5807(3) 0.44840(19) 0.23214(14) 0.0641(10) Uani 1 1 d . . . H74A H 0.5970 0.4511 0.2659 0.077 Uiso 1 1 calc R . . C75 C 0.6129(3) 0.39898(16) 0.20449(13) 0.0542(8) Uani 1 1 d . . . H75A H 0.6509 0.3673 0.2194 0.065 Uiso 1 1 calc R . . C76 C 0.5901(2) 0.39558(13) 0.15533(12) 0.0441(6) Uani 1 1 d . . . H76A H 0.6129 0.3616 0.1366 0.053 Uiso 1 1 calc R . . C77 C 0.5341(2) 0.44131(12) 0.13289(12) 0.0424(6) Uani 1 1 d . . . C78 C 0.5092(3) 0.43813(16) 0.07896(13) 0.0533(8) Uani 1 1 d . . . H78A H 0.4448 0.4581 0.0731 0.080 Uiso 1 1 calc R . . H78B H 0.5055 0.3951 0.0687 0.080 Uiso 1 1 calc R . . H78C H 0.5612 0.4591 0.0601 0.080 Uiso 1 1 calc R . . C79 C 1.0679(3) 0.30915(19) 0.20818(15) 0.0651(10) Uani 1 1 d . . . H79A H 1.0396 0.3149 0.1767 0.078 Uiso 1 1 calc R . . C80 C 1.1359(5) 0.2608(3) 0.2156(3) 0.113(2) Uani 1 1 d . . . H80A H 1.1540 0.2334 0.1901 0.135 Uiso 1 1 calc R . . C81 C 1.1776(4) 0.2551(3) 0.2658(3) 0.1007(18) Uani 1 1 d . . . H81A H 1.2236 0.2236 0.2743 0.121 Uiso 1 1 calc R . . C82 C 1.1462(4) 0.2973(3) 0.2987(2) 0.0942(16) Uani 1 1 d . . . H82A H 1.1737 0.2951 0.3307 0.113 Uiso 1 1 calc R . . C83 C 1.0801(5) 0.3418(3) 0.2902(2) 0.1011(18) Uani 1 1 d . . . H83A H 1.0601 0.3689 0.3157 0.121 Uiso 1 1 calc R . . C84 C 1.0422(4) 0.3475(2) 0.24476(16) 0.0781(13) Uani 1 1 d . . . C85 C 0.9674(5) 0.3986(3) 0.2353(3) 0.119(2) Uani 1 1 d . . . H85A H 0.9674 0.4089 0.2004 0.179 Uiso 1 1 calc R . . H85B H 0.9859 0.4349 0.2544 0.179 Uiso 1 1 calc R . . H85C H 0.9007 0.3848 0.2450 0.179 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 0.01827(7) 0.02110(7) 0.01588(6) 0.00121(5) -0.00014(6) 0.00012(6) Rh2 0.01767(7) 0.02158(7) 0.01595(6) 0.00150(5) -0.00066(6) 0.00017(6) N1 0.0254(9) 0.0243(8) 0.0265(9) 0.0006(7) 0.0004(7) 0.0037(7) N2 0.0225(9) 0.0283(9) 0.0306(9) -0.0038(7) -0.0065(7) 0.0019(7) N3 0.0253(9) 0.0244(9) 0.0253(8) -0.0024(7) -0.0004(7) -0.0002(7) N4 0.0227(9) 0.0284(9) 0.0325(9) -0.0013(8) 0.0020(8) -0.0043(7) N5 0.0297(10) 0.0289(9) 0.0191(8) -0.0006(7) 0.0008(7) -0.0037(7) N6 0.0276(9) 0.0285(8) 0.0199(7) -0.0015(6) 0.0013(8) 0.0027(8) O1 0.0243(8) 0.0224(7) 0.0201(6) 0.0003(5) 0.0028(5) 0.0005(6) O2 0.0247(7) 0.0270(7) 0.0200(6) 0.0009(6) 0.0020(6) 0.0034(6) O3 0.0322(9) 0.0250(8) 0.0401(9) 0.0014(7) -0.0031(7) -0.0002(6) O4 0.0483(11) 0.0259(8) 0.0396(9) -0.0006(7) -0.0001(8) -0.0012(7) O5 0.0207(7) 0.0271(7) 0.0233(6) 0.0012(6) -0.0038(5) -0.0020(6) O6 0.0195(7) 0.0288(7) 0.0257(7) 0.0032(6) -0.0019(6) -0.0033(6) O7 0.0332(10) 0.0427(10) 0.0445(10) -0.0069(8) -0.0077(8) 0.0136(8) O8 0.0374(10) 0.0421(10) 0.0453(10) -0.0056(8) -0.0123(8) 0.0147(8) O9 0.0266(7) 0.0252(7) 0.0206(6) -0.0006(6) 0.0009(6) 0.0030(6) O10 0.0265(8) 0.0241(7) 0.0210(7) 0.0004(6) 0.0010(6) 0.0034(6) O11 0.0468(11) 0.0380(9) 0.0325(8) 0.0032(7) 0.0033(8) -0.0118(8) O12 0.0400(10) 0.0297(8) 0.0378(8) 0.0014(7) 0.0005(8) -0.0077(7) O13 0.0202(7) 0.0291(7) 0.0222(7) 0.0015(6) -0.0003(6) -0.0030(6) O14 0.0204(7) 0.0300(8) 0.0239(7) 0.0013(6) -0.0041(5) -0.0037(6) O15 0.0364(10) 0.0469(11) 0.0625(13) 0.0004(10) 0.0233(10) -0.0049(9) O16 0.0366(10) 0.0425(10) 0.0441(10) -0.0013(8) 0.0143(8) -0.0004(8) C1 0.0177(9) 0.0250(9) 0.0230(9) -0.0014(8) 0.0008(7) -0.0013(7) C2 0.0235(10) 0.0252(10) 0.0233(9) -0.0021(8) 0.0014(8) 0.0001(8) C3 0.0317(12) 0.0354(12) 0.0239(10) -0.0026(9) 0.0049(9) 0.0053(9) C4 0.0408(15) 0.0503(15) 0.0246(11) -0.0053(10) -0.0016(10) 0.0071(12) C5 0.0344(13) 0.0508(16) 0.0318(12) 0.0078(11) 0.0077(10) 0.0024(11) C6 0.0535(17) 0.0435(15) 0.0325(12) -0.0051(11) 0.0080(12) 0.0165(13) C7 0.0232(10) 0.0305(11) 0.0280(10) 0.0004(9) 0.0039(8) 0.0045(8) C8 0.0249(11) 0.0304(10) 0.0297(10) 0.0041(9) 0.0036(8) 0.0053(8) C9 0.0241(11) 0.0412(13) 0.0363(12) 0.0061(10) 0.0014(9) 0.0029(10) C10 0.0246(12) 0.0594(16) 0.0341(12) 0.0116(12) 0.0000(10) 0.0089(11) C11 0.0387(14) 0.0467(15) 0.0413(14) 0.0182(12) 0.0051(11) 0.0175(12) C12 0.0455(15) 0.0319(12) 0.0379(12) 0.0092(10) 0.0088(11) 0.0108(10) C13 0.0318(12) 0.0306(10) 0.0290(10) 0.0035(8) 0.0063(9) 0.0068(9) C14 0.0327(12) 0.0257(10) 0.0277(10) 0.0002(8) 0.0052(9) 0.0036(9) C15 0.0215(9) 0.0229(9) 0.0240(9) -0.0018(7) -0.0015(7) 0.0014(7) C16 0.0184(9) 0.0291(10) 0.0296(10) -0.0045(9) -0.0033(8) -0.0005(8) C17 0.0213(11) 0.0342(12) 0.0404(12) 0.0021(10) -0.0016(9) -0.0065(9) C18 0.0319(13) 0.0551(16) 0.0414(14) 0.0037(12) 0.0078(10) -0.0082(11) C19 0.0235(12) 0.0540(16) 0.0614(18) 0.0061(14) -0.0049(12) -0.0099(11) C20 0.0450(17) 0.0314(13) 0.0535(16) 0.0063(12) -0.0043(12) -0.0059(11) C21 0.0261(11) 0.0330(11) 0.0345(11) -0.0046(10) -0.0033(9) 0.0014(9) C22 0.0314(12) 0.0385(13) 0.0333(11) -0.0034(10) -0.0049(10) -0.0016(10) C23 0.0409(16) 0.0577(18) 0.0412(14) -0.0053(13) 0.0003(12) 0.0043(13) C24 0.060(2) 0.069(2) 0.0324(13) -0.0064(14) 0.0028(13) -0.0023(17) C25 0.066(2) 0.0572(18) 0.0339(13) 0.0041(12) -0.0119(13) -0.0067(15) C26 0.0472(16) 0.0431(15) 0.0399(13) 0.0029(11) -0.0130(12) 0.0020(12) C27 0.0332(12) 0.0326(11) 0.0335(11) -0.0011(9) -0.0068(9) -0.0024(10) C28 0.0274(11) 0.0305(11) 0.0353(11) -0.0031(9) -0.0096(9) -0.0006(9) C29 0.0187(9) 0.0257(10) 0.0235(9) -0.0027(8) 0.0003(7) -0.0005(7) C30 0.0261(11) 0.0214(9) 0.0220(9) -0.0019(8) -0.0004(8) 0.0028(8) C31 0.0231(11) 0.0343(12) 0.0309(11) -0.0011(9) -0.0037(9) 0.0063(9) C32 0.0382(15) 0.0607(18) 0.0379(14) 0.0074(13) -0.0087(11) 0.0081(13) C33 0.0279(13) 0.0489(16) 0.070(2) 0.0091(15) -0.0171(13) -0.0088(12) C34 0.0346(14) 0.0611(18) 0.0605(18) -0.0221(16) -0.0036(13) 0.0195(13) C35 0.0244(11) 0.0290(11) 0.0321(11) -0.0072(9) -0.0010(8) 0.0004(9) C36 0.0314(13) 0.0354(12) 0.0327(11) -0.0068(9) -0.0028(9) 0.0014(9) C37 0.0460(17) 0.0450(15) 0.0426(14) -0.0128(12) -0.0072(12) -0.0058(12) C38 0.055(2) 0.0598(19) 0.0451(15) -0.0195(14) -0.0173(13) -0.0024(15) C39 0.054(2) 0.0670(19) 0.0289(12) -0.0097(12) -0.0081(12) 0.0111(15) C40 0.0420(15) 0.0497(15) 0.0306(12) 0.0008(11) -0.0026(10) 0.0055(12) C41 0.0296(12) 0.0376(12) 0.0259(10) -0.0025(9) -0.0024(9) 0.0024(10) C42 0.0267(11) 0.0313(11) 0.0263(10) -0.0024(9) 0.0013(8) 0.0020(9) C43 0.0177(9) 0.0252(9) 0.0248(8) -0.0022(7) 0.0001(8) 0.0006(8) C44 0.0175(9) 0.0294(10) 0.0330(11) -0.0050(9) 0.0004(8) -0.0031(8) C45 0.0233(11) 0.0386(13) 0.0410(12) -0.0038(10) -0.0099(9) -0.0008(9) C46 0.0361(14) 0.0383(14) 0.0578(16) -0.0018(13) -0.0132(12) 0.0086(11) C47 0.0530(18) 0.0536(16) 0.0323(12) -0.0026(12) -0.0152(12) 0.0036(14) C48 0.0278(14) 0.0543(18) 0.076(2) 0.0025(16) -0.0192(14) -0.0047(12) C49 0.0262(12) 0.0354(12) 0.0425(13) 0.0003(10) 0.0024(10) -0.0055(10) C50 0.0325(13) 0.0321(12) 0.0437(13) 0.0000(10) -0.0056(10) -0.0058(10) C51 0.0383(15) 0.0412(14) 0.0556(17) 0.0065(12) -0.0073(12) -0.0111(12) C52 0.0539(19) 0.0338(14) 0.069(2) 0.0048(14) -0.0173(16) -0.0075(13) C53 0.056(2) 0.0325(13) 0.0684(19) -0.0088(13) -0.0145(16) 0.0068(13) C54 0.0431(16) 0.0406(14) 0.0477(14) -0.0066(11) -0.0042(12) 0.0054(12) C55 0.0318(12) 0.0345(12) 0.0380(12) -0.0029(10) -0.0059(9) -0.0004(10) C56 0.0270(12) 0.0331(11) 0.0319(10) -0.0032(9) -0.0008(9) 0.0001(9) C57 0.0296(11) 0.0298(11) 0.0217(10) 0.0011(8) -0.0004(8) 0.0019(9) C58 0.0358(12) 0.0343(12) 0.0175(9) 0.0012(8) 0.0010(8) 0.0019(10) C59 0.0597(18) 0.0422(14) 0.0265(11) -0.0017(10) 0.0089(11) -0.0176(13) C60 0.070(2) 0.0394(14) 0.0233(11) -0.0076(10) 0.0036(11) -0.0198(14) C61 0.0382(13) 0.0331(11) 0.0175(9) -0.0017(8) 0.0017(8) 0.0036(10) C62 0.0362(13) 0.0363(11) 0.0238(9) -0.0040(8) 0.0048(9) -0.0071(10) C63 0.0397(13) 0.0371(12) 0.0205(10) -0.0061(9) 0.0022(9) -0.0050(10) C64 0.0351(13) 0.0305(11) 0.0213(9) -0.0029(8) 0.0004(8) 0.0016(9) C65 0.085(3) 0.074(2) 0.0447(17) -0.0214(17) -0.0060(18) 0.012(2) C66 0.122(4) 0.069(3) 0.065(3) -0.007(2) -0.013(3) -0.007(3) C67 0.095(4) 0.175(7) 0.074(3) -0.034(4) -0.008(3) -0.013(5) C68 0.079(4) 0.224(9) 0.126(5) -0.105(6) -0.036(4) 0.052(5) C69 0.118(4) 0.064(2) 0.106(4) -0.036(3) -0.072(4) 0.041(3) C70 0.090(3) 0.090(3) 0.0463(19) 0.012(2) -0.028(2) -0.021(3) C71 0.160(6) 0.146(5) 0.066(3) 0.009(3) -0.026(4) -0.063(5) C72 0.0415(16) 0.0399(15) 0.082(2) -0.0077(16) -0.0061(15) 0.0030(13) C73 0.0508(19) 0.058(2) 0.079(2) -0.0264(18) 0.0026(17) -0.0013(16) C74 0.060(2) 0.078(2) 0.0541(18) -0.0151(18) -0.0012(16) -0.0170(19) C75 0.0492(18) 0.0533(18) 0.0600(19) 0.0090(15) -0.0134(15) -0.0052(14) C76 0.0406(15) 0.0368(14) 0.0548(16) -0.0025(12) -0.0025(13) -0.0028(11) C77 0.0362(14) 0.0334(13) 0.0575(16) 0.0036(12) -0.0025(12) -0.0071(11) C78 0.0505(19) 0.0461(16) 0.0633(19) 0.0119(15) -0.0071(15) -0.0053(14) C79 0.063(2) 0.067(2) 0.065(2) -0.0049(19) -0.0037(18) -0.0218(19) C80 0.087(4) 0.095(4) 0.157(6) -0.017(4) 0.038(4) -0.034(3) C81 0.073(3) 0.094(4) 0.135(5) 0.042(4) -0.005(3) -0.023(3) C82 0.078(3) 0.103(4) 0.101(4) 0.038(3) -0.004(3) -0.010(3) C83 0.099(4) 0.119(5) 0.086(3) 0.015(3) -0.018(3) -0.036(4) C84 0.082(3) 0.081(3) 0.071(3) 0.004(2) -0.007(2) -0.038(2) C85 0.140(6) 0.093(4) 0.125(5) -0.012(4) -0.022(4) -0.001(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 O5 2.0173(15) . ? Rh1 O9 2.0393(15) . ? Rh1 O13 2.0431(15) . ? Rh1 O1 2.0477(15) . ? Rh1 N5 2.2292(18) . ? Rh1 Rh2 2.3949(5) . ? Rh2 O10 2.0208(15) . ? Rh2 O2 2.0310(15) . ? Rh2 O6 2.0383(15) . ? Rh2 O14 2.0497(15) . ? Rh2 N6 2.2380(17) 2_655 ? N1 C7 1.404(3) . ? N1 C14 1.405(3) . ? N1 C2 1.468(3) . ? N2 C28 1.400(3) . ? N2 C21 1.402(3) . ? N2 C16 1.474(3) . ? N3 C42 1.396(3) . ? N3 C35 1.415(3) . ? N3 C30 1.470(3) . ? N4 C56 1.394(3) . ? N4 C49 1.414(3) . ? N4 C44 1.467(3) . ? N5 C57 1.143(3) . ? N6 C64 1.136(3) . ? N6 Rh2 2.2380(17) 2_654 ? O1 C1 1.264(3) . ? O2 C1 1.259(3) . ? O3 C7 1.215(3) . ? O4 C14 1.205(3) . ? O5 C15 1.263(3) . ? O6 C15 1.265(2) . ? O7 C21 1.210(3) . ? O8 C28 1.209(3) . ? O9 C29 1.259(3) . ? O10 C29 1.269(3) . ? O11 C42 1.205(3) . ? O12 C35 1.202(3) . ? O13 C43 1.265(2) . ? O14 C43 1.256(2) . ? O15 C49 1.198(3) . ? O16 C56 1.211(3) . ? C1 C2 1.539(3) . ? C2 C3 1.554(3) . ? C3 C5 1.530(4) . ? C3 C4 1.537(3) . ? C3 C6 1.538(3) . ? C7 C8 1.478(3) . ? C8 C9 1.381(3) . ? C8 C13 1.390(3) . ? C9 C10 1.396(4) . ? C10 C11 1.376(4) . ? C11 C12 1.386(4) . ? C12 C13 1.389(3) . ? C13 C14 1.480(3) . ? C15 C16 1.540(3) . ? C16 C17 1.549(3) . ? C17 C18 1.529(4) . ? C17 C20 1.532(4) . ? C17 C19 1.539(3) . ? C21 C22 1.493(3) . ? C22 C23 1.377(4) . ? C22 C27 1.385(3) . ? C23 C24 1.407(4) . ? C24 C25 1.371(5) . ? C25 C26 1.396(4) . ? C26 C27 1.387(3) . ? C27 C28 1.488(3) . ? C29 C30 1.530(3) . ? C30 C31 1.563(3) . ? C31 C34 1.515(4) . ? C31 C32 1.535(4) . ? C31 C33 1.536(4) . ? C35 C36 1.495(3) . ? C36 C41 1.378(4) . ? C36 C37 1.387(4) . ? C37 C38 1.401(4) . ? C38 C39 1.378(5) . ? C39 C40 1.393(4) . ? C40 C41 1.382(3) . ? C41 C42 1.500(3) . ? C43 C44 1.543(3) . ? C44 C45 1.554(3) . ? C45 C47 1.530(4) . ? C45 C46 1.534(4) . ? C45 C48 1.538(4) . ? C49 C50 1.486(4) . ? C50 C55 1.382(4) . ? C50 C51 1.388(4) . ? C51 C52 1.393(5) . ? C52 C53 1.377(5) . ? C53 C54 1.398(4) . ? C54 C55 1.383(4) . ? C55 C56 1.490(3) . ? C57 C58 1.446(3) . ? C58 C63 1.383(3) . ? C58 C59 1.388(4) . ? C59 C60 1.384(3) . ? C60 C61 1.386(4) . ? C61 C62 1.390(3) . ? C61 C64 1.446(3) . ? C62 C63 1.392(3) . ? C65 C66 1.358(7) . ? C65 C70 1.377(6) . ? C66 C67 1.375(8) . ? C67 C68 1.335(10) . ? C68 C69 1.317(10) . ? C69 C70 1.403(8) . ? C70 C71 1.452(7) . ? C72 C73 1.373(5) . ? C72 C77 1.390(4) . ? C73 C74 1.362(6) . ? C74 C75 1.384(5) . ? C75 C76 1.380(5) . ? C76 C77 1.390(4) . ? C77 C78 1.512(4) . ? C79 C84 1.347(6) . ? C79 C80 1.408(8) . ? C80 C81 1.486(9) . ? C81 C82 1.354(8) . ? C82 C83 1.334(8) . ? C83 C84 1.348(7) . ? C84 C85 1.521(8) . ? 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 O5 Rh1 O9 89.10(6) . . ? O5 Rh1 O13 176.64(6) . . ? O9 Rh1 O13 92.63(6) . . ? O5 Rh1 O1 88.90(6) . . ? O9 Rh1 O1 174.83(6) . . ? O13 Rh1 O1 89.14(6) . . ? O5 Rh1 N5 91.80(6) . . ? O9 Rh1 N5 85.69(6) . . ? O13 Rh1 N5 91.20(6) . . ? O1 Rh1 N5 99.14(6) . . ? O5 Rh1 Rh2 89.17(4) . . ? O9 Rh1 Rh2 87.59(4) . . ? O13 Rh1 Rh2 88.03(4) . . ? O1 Rh1 Rh2 87.61(4) . . ? N5 Rh1 Rh2 173.19(5) . . ? O10 Rh2 O2 176.79(6) . . ? O10 Rh2 O6 89.58(6) . . ? O2 Rh2 O6 88.78(6) . . ? O10 Rh2 O14 90.82(7) . . ? O2 Rh2 O14 90.58(6) . . ? O6 Rh2 O14 175.01(6) . . ? O10 Rh2 N6 93.30(6) . 2_655 ? O2 Rh2 N6 89.65(6) . 2_655 ? O6 Rh2 N6 97.17(7) . 2_655 ? O14 Rh2 N6 87.77(7) . 2_655 ? O10 Rh2 Rh1 88.55(4) . . ? O2 Rh2 Rh1 88.61(4) . . ? O6 Rh2 Rh1 87.07(4) . . ? O14 Rh2 Rh1 87.97(4) . . ? N6 Rh2 Rh1 175.39(5) 2_655 . ? C7 N1 C14 111.49(19) . . ? C7 N1 C2 125.27(18) . . ? C14 N1 C2 122.68(19) . . ? C28 N2 C21 111.55(19) . . ? C28 N2 C16 121.59(18) . . ? C21 N2 C16 125.63(18) . . ? C42 N3 C35 111.63(19) . . ? C42 N3 C30 130.12(18) . . ? C35 N3 C30 118.19(18) . . ? C56 N4 C49 111.29(19) . . ? C56 N4 C44 127.41(19) . . ? C49 N4 C44 120.9(2) . . ? C57 N5 Rh1 151.96(18) . . ? C64 N6 Rh2 157.51(19) . 2_654 ? C1 O1 Rh1 118.26(13) . . ? C1 O2 Rh2 118.20(13) . . ? C15 O5 Rh1 117.83(13) . . ? C15 O6 Rh2 118.91(14) . . ? C29 O9 Rh1 118.77(13) . . ? C29 O10 Rh2 118.46(14) . . ? C43 O13 Rh1 118.69(13) . . ? C43 O14 Rh2 118.61(13) . . ? O2 C1 O1 127.25(19) . . ? O2 C1 C2 117.89(18) . . ? O1 C1 C2 114.84(18) . . ? N1 C2 C1 107.35(16) . . ? N1 C2 C3 113.03(18) . . ? C1 C2 C3 118.50(18) . . ? C5 C3 C4 111.0(2) . . ? C5 C3 C6 108.8(2) . . ? C4 C3 C6 107.7(2) . . ? C5 C3 C2 112.76(19) . . ? C4 C3 C2 108.44(19) . . ? C6 C3 C2 107.97(19) . . ? O3 C7 N1 124.2(2) . . ? O3 C7 C8 129.8(2) . . ? N1 C7 C8 105.97(19) . . ? C9 C8 C13 121.8(2) . . ? C9 C8 C7 129.9(2) . . ? C13 C8 C7 108.3(2) . . ? C8 C9 C10 116.2(2) . . ? C11 C10 C9 122.3(3) . . ? C10 C11 C12 121.3(2) . . ? C11 C12 C13 117.0(3) . . ? C12 C13 C8 121.4(2) . . ? C12 C13 C14 130.1(2) . . ? C8 C13 C14 108.41(19) . . ? O4 C14 N1 124.7(2) . . ? O4 C14 C13 129.6(2) . . ? N1 C14 C13 105.71(19) . . ? O5 C15 O6 126.9(2) . . ? O5 C15 C16 114.00(18) . . ? O6 C15 C16 118.97(19) . . ? N2 C16 C15 107.57(17) . . ? N2 C16 C17 113.99(18) . . ? C15 C16 C17 118.40(18) . . ? C18 C17 C20 111.7(2) . . ? C18 C17 C19 107.9(2) . . ? C20 C17 C19 108.8(2) . . ? C18 C17 C16 108.8(2) . . ? C20 C17 C16 112.6(2) . . ? C19 C17 C16 106.9(2) . . ? O7 C21 N2 125.9(2) . . ? O7 C21 C22 128.4(2) . . ? N2 C21 C22 105.7(2) . . ? C23 C22 C27 121.9(2) . . ? C23 C22 C21 129.9(2) . . ? C27 C22 C21 108.1(2) . . ? C22 C23 C24 116.4(3) . . ? C25 C24 C23 121.6(3) . . ? C24 C25 C26 121.7(3) . . ? C27 C26 C25 116.6(3) . . ? C22 C27 C26 121.7(2) . . ? C22 C27 C28 108.3(2) . . ? C26 C27 C28 130.0(2) . . ? O8 C28 N2 125.3(2) . . ? O8 C28 C27 128.8(2) . . ? N2 C28 C27 105.9(2) . . ? O9 C29 O10 126.6(2) . . ? O9 C29 C30 119.50(18) . . ? O10 C29 C30 113.87(18) . . ? N3 C30 C29 111.84(17) . . ? N3 C30 C31 115.76(18) . . ? C29 C30 C31 112.01(19) . . ? C34 C31 C32 108.0(2) . . ? C34 C31 C33 110.7(2) . . ? C32 C31 C33 108.1(2) . . ? C34 C31 C30 109.3(2) . . ? C32 C31 C30 108.2(2) . . ? C33 C31 C30 112.5(2) . . ? O12 C35 N3 125.7(2) . . ? O12 C35 C36 128.5(2) . . ? N3 C35 C36 105.8(2) . . ? C41 C36 C37 121.6(2) . . ? C41 C36 C35 108.2(2) . . ? C37 C36 C35 130.2(3) . . ? C36 C37 C38 116.2(3) . . ? C39 C38 C37 122.2(3) . . ? C38 C39 C40 120.8(3) . . ? C41 C40 C39 117.2(3) . . ? C36 C41 C40 122.0(2) . . ? C36 C41 C42 108.7(2) . . ? C40 C41 C42 129.2(2) . . ? O11 C42 N3 127.8(2) . . ? O11 C42 C41 126.5(2) . . ? N3 C42 C41 105.73(19) . . ? O14 C43 O13 126.6(2) . . ? O14 C43 C44 120.61(18) . . ? O13 C43 C44 112.74(18) . . ? N4 C44 C43 108.93(17) . . ? N4 C44 C45 113.35(19) . . ? C43 C44 C45 118.36(19) . . ? C47 C45 C46 110.2(2) . . ? C47 C45 C48 109.2(2) . . ? C46 C45 C48 108.0(2) . . ? C47 C45 C44 113.0(2) . . ? C46 C45 C44 108.1(2) . . ? C48 C45 C44 108.2(2) . . ? O15 C49 N4 124.5(2) . . ? O15 C49 C50 129.7(2) . . ? N4 C49 C50 105.8(2) . . ? C55 C50 C51 121.5(3) . . ? C55 C50 C49 108.2(2) . . ? C51 C50 C49 130.2(3) . . ? C50 C51 C52 117.1(3) . . ? C53 C52 C51 121.3(3) . . ? C52 C53 C54 121.6(3) . . ? C55 C54 C53 116.9(3) . . ? C50 C55 C54 121.6(3) . . ? C50 C55 C56 108.5(2) . . ? C54 C55 C56 129.8(3) . . ? O16 C56 N4 125.3(2) . . ? O16 C56 C55 128.8(2) . . ? N4 C56 C55 105.9(2) . . ? N5 C57 C58 177.9(3) . . ? C63 C58 C59 121.3(2) . . ? C63 C58 C57 120.4(2) . . ? C59 C58 C57 118.2(2) . . ? C60 C59 C58 119.2(2) . . ? C59 C60 C61 119.6(2) . . ? C60 C61 C62 121.3(2) . . ? C60 C61 C64 118.2(2) . . ? C62 C61 C64 120.4(2) . . ? C61 C62 C63 118.9(2) . . ? C58 C63 C62 119.6(2) . . ? N6 C64 C61 176.0(3) . . ? C66 C65 C70 120.0(4) . . ? C65 C66 C67 120.6(5) . . ? C68 C67 C66 119.5(7) . . ? C69 C68 C67 121.0(6) . . ? C68 C69 C70 121.9(5) . . ? C65 C70 C69 116.9(5) . . ? C65 C70 C71 119.1(5) . . ? C69 C70 C71 124.0(6) . . ? C73 C72 C77 120.5(3) . . ? C74 C73 C72 121.3(3) . . ? C73 C74 C75 119.1(3) . . ? C76 C75 C74 120.3(3) . . ? C75 C76 C77 120.7(3) . . ? C72 C77 C76 118.1(3) . . ? C72 C77 C78 120.9(3) . . ? C76 C77 C78 121.1(3) . . ? C84 C79 C80 121.5(5) . . ? C79 C80 C81 116.1(6) . . ? C82 C81 C80 116.0(6) . . ? C83 C82 C81 125.9(6) . . ? C82 C83 C84 118.4(7) . . ? C79 C84 C83 122.1(6) . . ? C79 C84 C85 119.7(5) . . ? C83 C84 C85 118.2(6) . . ? 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 O5 Rh1 Rh2 O10 90.75(6) . . . . ? O9 Rh1 Rh2 O10 1.61(6) . . . . ? O13 Rh1 Rh2 O10 -91.10(6) . . . . ? O1 Rh1 Rh2 O10 179.68(6) . . . . ? N5 Rh1 Rh2 O10 -7.5(4) . . . . ? O5 Rh1 Rh2 O2 -87.76(6) . . . . ? O9 Rh1 Rh2 O2 -176.89(6) . . . . ? O13 Rh1 Rh2 O2 90.39(6) . . . . ? O1 Rh1 Rh2 O2 1.17(6) . . . . ? N5 Rh1 Rh2 O2 174.0(4) . . . . ? O5 Rh1 Rh2 O6 1.09(6) . . . . ? O9 Rh1 Rh2 O6 -88.04(6) . . . . ? O13 Rh1 Rh2 O6 179.24(6) . . . . ? O1 Rh1 Rh2 O6 90.02(6) . . . . ? N5 Rh1 Rh2 O6 -97.2(4) . . . . ? O5 Rh1 Rh2 O14 -178.38(6) . . . . ? O9 Rh1 Rh2 O14 92.48(6) . . . . ? O13 Rh1 Rh2 O14 -0.23(6) . . . . ? O1 Rh1 Rh2 O14 -89.45(6) . . . . ? N5 Rh1 Rh2 O14 83.4(4) . . . . ? O5 Rh1 Rh2 N6 -155.6(6) . . . 2_655 ? O9 Rh1 Rh2 N6 115.3(6) . . . 2_655 ? O13 Rh1 Rh2 N6 22.5(6) . . . 2_655 ? O1 Rh1 Rh2 N6 -66.7(6) . . . 2_655 ? N5 Rh1 Rh2 N6 106.1(8) . . . 2_655 ? O5 Rh1 N5 C57 -96.5(4) . . . . ? O9 Rh1 N5 C57 -7.5(4) . . . . ? O13 Rh1 N5 C57 85.0(4) . . . . ? O1 Rh1 N5 C57 174.3(4) . . . . ? Rh2 Rh1 N5 C57 1.6(7) . . . . ? O5 Rh1 O1 C1 86.69(15) . . . . ? O9 Rh1 O1 C1 19.5(8) . . . . ? O13 Rh1 O1 C1 -90.58(15) . . . . ? N5 Rh1 O1 C1 178.35(15) . . . . ? Rh2 Rh1 O1 C1 -2.52(14) . . . . ? O10 Rh2 O2 C1 -27.9(12) . . . . ? O6 Rh2 O2 C1 -87.32(15) . . . . ? O14 Rh2 O2 C1 87.73(15) . . . . ? N6 Rh2 O2 C1 175.50(16) 2_655 . . . ? Rh1 Rh2 O2 C1 -0.23(15) . . . . ? O9 Rh1 O5 C15 87.79(15) . . . . ? O13 Rh1 O5 C15 -33.2(11) . . . . ? O1 Rh1 O5 C15 -87.44(15) . . . . ? N5 Rh1 O5 C15 173.45(15) . . . . ? Rh2 Rh1 O5 C15 0.19(14) . . . . ? O10 Rh2 O6 C15 -91.31(15) . . . . ? O2 Rh2 O6 C15 85.92(15) . . . . ? O14 Rh2 O6 C15 3.3(8) . . . . ? N6 Rh2 O6 C15 175.42(15) 2_655 . . . ? Rh1 Rh2 O6 C15 -2.75(15) . . . . ? O5 Rh1 O9 C29 -90.64(16) . . . . ? O13 Rh1 O9 C29 86.47(16) . . . . ? O1 Rh1 O9 C29 -23.4(8) . . . . ? N5 Rh1 O9 C29 177.48(16) . . . . ? Rh2 Rh1 O9 C29 -1.44(15) . . . . ? O2 Rh2 O10 C29 25.4(12) . . . . ? O6 Rh2 O10 C29 84.74(16) . . . . ? O14 Rh2 O10 C29 -90.29(16) . . . . ? N6 Rh2 O10 C29 -178.10(16) 2_655 . . . ? Rh1 Rh2 O10 C29 -2.33(15) . . . . ? O5 Rh1 O13 C43 32.4(11) . . . . ? O9 Rh1 O13 C43 -88.59(15) . . . . ? O1 Rh1 O13 C43 86.55(15) . . . . ? N5 Rh1 O13 C43 -174.32(15) . . . . ? Rh2 Rh1 O13 C43 -1.09(15) . . . . ? O10 Rh2 O14 C43 90.17(15) . . . . ? O2 Rh2 O14 C43 -86.93(15) . . . . ? O6 Rh2 O14 C43 -4.4(8) . . . . ? N6 Rh2 O14 C43 -176.56(16) 2_655 . . . ? Rh1 Rh2 O14 C43 1.65(15) . . . . ? Rh2 O2 C1 O1 -1.9(3) . . . . ? Rh2 O2 C1 C2 -179.92(14) . . . . ? Rh1 O1 C1 O2 3.3(3) . . . . ? Rh1 O1 C1 C2 -178.62(13) . . . . ? C7 N1 C2 C1 42.9(3) . . . . ? C14 N1 C2 C1 -127.8(2) . . . . ? C7 N1 C2 C3 -89.6(2) . . . . ? C14 N1 C2 C3 99.7(2) . . . . ? O2 C1 C2 N1 -134.52(19) . . . . ? O1 C1 C2 N1 47.2(2) . . . . ? O2 C1 C2 C3 -5.0(3) . . . . ? O1 C1 C2 C3 176.69(19) . . . . ? N1 C2 C3 C5 65.0(3) . . . . ? C1 C2 C3 C5 -61.8(3) . . . . ? N1 C2 C3 C4 -171.6(2) . . . . ? C1 C2 C3 C4 61.5(3) . . . . ? N1 C2 C3 C6 -55.2(3) . . . . ? C1 C2 C3 C6 177.9(2) . . . . ? C14 N1 C7 O3 177.8(2) . . . . ? C2 N1 C7 O3 6.2(4) . . . . ? C14 N1 C7 C8 -2.5(2) . . . . ? C2 N1 C7 C8 -174.03(19) . . . . ? O3 C7 C8 C9 -1.1(4) . . . . ? N1 C7 C8 C9 179.1(2) . . . . ? O3 C7 C8 C13 179.7(2) . . . . ? N1 C7 C8 C13 -0.1(2) . . . . ? C13 C8 C9 C10 -0.7(4) . . . . ? C7 C8 C9 C10 -179.8(2) . . . . ? C8 C9 C10 C11 0.1(4) . . . . ? C9 C10 C11 C12 0.8(4) . . . . ? C10 C11 C12 C13 -1.1(4) . . . . ? C11 C12 C13 C8 0.5(4) . . . . ? C11 C12 C13 C14 177.1(2) . . . . ? C9 C8 C13 C12 0.4(4) . . . . ? C7 C8 C13 C12 179.7(2) . . . . ? C9 C8 C13 C14 -176.9(2) . . . . ? C7 C8 C13 C14 2.4(3) . . . . ? C7 N1 C14 O4 -176.4(2) . . . . ? C2 N1 C14 O4 -4.6(3) . . . . ? C7 N1 C14 C13 3.9(2) . . . . ? C2 N1 C14 C13 175.70(18) . . . . ? C12 C13 C14 O4 -0.5(4) . . . . ? C8 C13 C14 O4 176.5(2) . . . . ? C12 C13 C14 N1 179.2(2) . . . . ? C8 C13 C14 N1 -3.8(2) . . . . ? Rh1 O5 C15 O6 -2.6(3) . . . . ? Rh1 O5 C15 C16 173.63(13) . . . . ? Rh2 O6 C15 O5 4.0(3) . . . . ? Rh2 O6 C15 C16 -172.12(14) . . . . ? C28 N2 C16 C15 -121.7(2) . . . . ? C21 N2 C16 C15 44.5(3) . . . . ? C28 N2 C16 C17 104.9(2) . . . . ? C21 N2 C16 C17 -88.9(3) . . . . ? O5 C15 C16 N2 41.6(2) . . . . ? O6 C15 C16 N2 -141.81(19) . . . . ? O5 C15 C16 C17 172.63(19) . . . . ? O6 C15 C16 C17 -10.8(3) . . . . ? N2 C16 C17 C18 -169.5(2) . . . . ? C15 C16 C17 C18 62.5(3) . . . . ? N2 C16 C17 C20 66.1(3) . . . . ? C15 C16 C17 C20 -61.9(3) . . . . ? N2 C16 C17 C19 -53.2(3) . . . . ? C15 C16 C17 C19 178.7(2) . . . . ? C28 N2 C21 O7 173.9(2) . . . . ? C16 N2 C21 O7 6.5(4) . . . . ? C28 N2 C21 C22 -6.1(3) . . . . ? C16 N2 C21 C22 -173.5(2) . . . . ? O7 C21 C22 C23 5.3(5) . . . . ? N2 C21 C22 C23 -174.7(3) . . . . ? O7 C21 C22 C27 -177.0(3) . . . . ? N2 C21 C22 C27 3.0(3) . . . . ? C27 C22 C23 C24 0.7(4) . . . . ? C21 C22 C23 C24 178.2(3) . . . . ? C22 C23 C24 C25 -0.2(5) . . . . ? C23 C24 C25 C26 0.0(5) . . . . ? C24 C25 C26 C27 -0.3(5) . . . . ? C23 C22 C27 C26 -1.0(4) . . . . ? C21 C22 C27 C26 -179.0(2) . . . . ? C23 C22 C27 C28 178.9(3) . . . . ? C21 C22 C27 C28 0.9(3) . . . . ? C25 C26 C27 C22 0.8(4) . . . . ? C25 C26 C27 C28 -179.1(3) . . . . ? C21 N2 C28 O8 -173.2(2) . . . . ? C16 N2 C28 O8 -5.2(4) . . . . ? C21 N2 C28 C27 6.6(3) . . . . ? C16 N2 C28 C27 174.64(19) . . . . ? C22 C27 C28 O8 175.3(3) . . . . ? C26 C27 C28 O8 -4.8(5) . . . . ? C22 C27 C28 N2 -4.5(3) . . . . ? C26 C27 C28 N2 175.4(3) . . . . ? Rh1 O9 C29 O10 0.0(3) . . . . ? Rh1 O9 C29 C30 -176.97(14) . . . . ? Rh2 O10 C29 O9 2.0(3) . . . . ? Rh2 O10 C29 C30 179.06(13) . . . . ? C42 N3 C30 C29 69.4(3) . . . . ? C35 N3 C30 C29 -113.6(2) . . . . ? C42 N3 C30 C31 -60.5(3) . . . . ? C35 N3 C30 C31 116.5(2) . . . . ? O9 C29 C30 N3 -35.7(3) . . . . ? O10 C29 C30 N3 146.92(18) . . . . ? O9 C29 C30 C31 96.1(2) . . . . ? O10 C29 C30 C31 -81.2(2) . . . . ? N3 C30 C31 C34 -37.7(3) . . . . ? C29 C30 C31 C34 -167.5(2) . . . . ? N3 C30 C31 C32 -155.0(2) . . . . ? C29 C30 C31 C32 75.1(3) . . . . ? N3 C30 C31 C33 85.7(3) . . . . ? C29 C30 C31 C33 -44.1(3) . . . . ? C42 N3 C35 O12 178.8(2) . . . . ? C30 N3 C35 O12 1.3(3) . . . . ? C42 N3 C35 C36 0.1(3) . . . . ? C30 N3 C35 C36 -177.44(19) . . . . ? O12 C35 C36 C41 -178.1(3) . . . . ? N3 C35 C36 C41 0.6(3) . . . . ? O12 C35 C36 C37 0.0(5) . . . . ? N3 C35 C36 C37 178.7(3) . . . . ? C41 C36 C37 C38 0.1(4) . . . . ? C35 C36 C37 C38 -177.8(3) . . . . ? C36 C37 C38 C39 0.7(5) . . . . ? C37 C38 C39 C40 -1.0(5) . . . . ? C38 C39 C40 C41 0.4(4) . . . . ? C37 C36 C41 C40 -0.7(4) . . . . ? C35 C36 C41 C40 177.6(2) . . . . ? C37 C36 C41 C42 -179.3(2) . . . . ? C35 C36 C41 C42 -1.0(3) . . . . ? C39 C40 C41 C36 0.5(4) . . . . ? C39 C40 C41 C42 178.7(3) . . . . ? C35 N3 C42 O11 -179.0(2) . . . . ? C30 N3 C42 O11 -1.8(4) . . . . ? C35 N3 C42 C41 -0.7(2) . . . . ? C30 N3 C42 C41 176.5(2) . . . . ? C36 C41 C42 O11 179.4(2) . . . . ? C40 C41 C42 O11 0.9(4) . . . . ? C36 C41 C42 N3 1.0(3) . . . . ? C40 C41 C42 N3 -177.4(3) . . . . ? Rh2 O14 C43 O13 -3.2(3) . . . . ? Rh2 O14 C43 C44 178.68(14) . . . . ? Rh1 O13 C43 O14 2.9(3) . . . . ? Rh1 O13 C43 C44 -178.83(13) . . . . ? C56 N4 C44 C43 49.5(3) . . . . ? C49 N4 C44 C43 -122.8(2) . . . . ? C56 N4 C44 C45 -84.5(3) . . . . ? C49 N4 C44 C45 103.2(3) . . . . ? O14 C43 C44 N4 -118.6(2) . . . . ? O13 C43 C44 N4 63.0(2) . . . . ? O14 C43 C44 C45 12.8(3) . . . . ? O13 C43 C44 C45 -165.56(19) . . . . ? N4 C44 C45 C47 63.5(3) . . . . ? C43 C44 C45 C47 -65.9(3) . . . . ? N4 C44 C45 C46 -174.2(2) . . . . ? C43 C44 C45 C46 56.4(3) . . . . ? N4 C44 C45 C48 -57.4(3) . . . . ? C43 C44 C45 C48 173.2(2) . . . . ? C56 N4 C49 O15 -172.1(3) . . . . ? C44 N4 C49 O15 1.4(4) . . . . ? C56 N4 C49 C50 6.0(3) . . . . ? C44 N4 C49 C50 179.4(2) . . . . ? O15 C49 C50 C55 174.4(3) . . . . ? N4 C49 C50 C55 -3.4(3) . . . . ? O15 C49 C50 C51 -2.6(5) . . . . ? N4 C49 C50 C51 179.6(3) . . . . ? C55 C50 C51 C52 0.3(4) . . . . ? C49 C50 C51 C52 176.9(3) . . . . ? C50 C51 C52 C53 -0.7(5) . . . . ? C51 C52 C53 C54 1.0(5) . . . . ? C52 C53 C54 C55 -0.8(5) . . . . ? C51 C50 C55 C54 -0.1(4) . . . . ? C49 C50 C55 C54 -177.4(2) . . . . ? C51 C50 C55 C56 177.2(2) . . . . ? C49 C50 C55 C56 -0.1(3) . . . . ? C53 C54 C55 C50 0.3(4) . . . . ? C53 C54 C55 C56 -176.3(3) . . . . ? C49 N4 C56 O16 172.8(3) . . . . ? C44 N4 C56 O16 -0.1(4) . . . . ? C49 N4 C56 C55 -6.0(3) . . . . ? C44 N4 C56 C55 -179.0(2) . . . . ? C50 C55 C56 O16 -175.1(3) . . . . ? C54 C55 C56 O16 1.9(5) . . . . ? C50 C55 C56 N4 3.7(3) . . . . ? C54 C55 C56 N4 -179.3(3) . . . . ? Rh1 N5 C57 C58 89(7) . . . . ? N5 C57 C58 C63 155(7) . . . . ? N5 C57 C58 C59 -26(7) . . . . ? C63 C58 C59 C60 -0.6(4) . . . . ? C57 C58 C59 C60 179.9(3) . . . . ? C58 C59 C60 C61 0.4(5) . . . . ? C59 C60 C61 C62 0.0(5) . . . . ? C59 C60 C61 C64 178.2(3) . . . . ? C60 C61 C62 C63 0.0(4) . . . . ? C64 C61 C62 C63 -178.2(2) . . . . ? C59 C58 C63 C62 0.6(4) . . . . ? C57 C58 C63 C62 -180.0(2) . . . . ? C61 C62 C63 C58 -0.3(4) . . . . ? Rh2 N6 C64 C61 4(4) 2_654 . . . ? C60 C61 C64 N6 -11(4) . . . . ? C62 C61 C64 N6 167(4) . . . . ? C70 C65 C66 C67 0.6(7) . . . . ? C65 C66 C67 C68 -2.2(8) . . . . ? C66 C67 C68 C69 2.3(9) . . . . ? C67 C68 C69 C70 -0.8(9) . . . . ? C66 C65 C70 C69 0.8(6) . . . . ? C66 C65 C70 C71 179.5(4) . . . . ? C68 C69 C70 C65 -0.7(7) . . . . ? C68 C69 C70 C71 -179.3(5) . . . . ? C77 C72 C73 C74 0.4(6) . . . . ? C72 C73 C74 C75 -0.7(6) . . . . ? C73 C74 C75 C76 0.7(5) . . . . ? C74 C75 C76 C77 -0.4(5) . . . . ? C73 C72 C77 C76 -0.1(5) . . . . ? C73 C72 C77 C78 -179.6(3) . . . . ? C75 C76 C77 C72 0.1(4) . . . . ? C75 C76 C77 C78 179.7(3) . . . . ? C84 C79 C80 C81 -0.4(6) . . . . ? C79 C80 C81 C82 -0.5(7) . . . . ? C80 C81 C82 C83 1.8(8) . . . . ? C81 C82 C83 C84 -2.2(9) . . . . ? C80 C79 C84 C83 0.2(7) . . . . ? C80 C79 C84 C85 -179.1(5) . . . . ? C82 C83 C84 C79 1.1(8) . . . . ? C82 C83 C84 C85 -179.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.917 _refine_diff_density_min -0.348 _refine_diff_density_rms 0.070 # Attachment 'joef094a.cif' data_joef094a _database_code_depnum_ccdc_archive 'CCDC 761720' #TrackingRef 'joef094a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C84 H88 N4 O21 Rh2' _chemical_formula_weight 1695.40 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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 21.627(10) _cell_length_b 21.826(10) _cell_length_c 17.238(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8137(6) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 1023 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 24.40 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.384 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3512 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8694 _exptl_absorpt_correction_T_max 0.9622 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 111612 _diffrn_reflns_av_R_equivalents 0.0526 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 28.27 _reflns_number_total 20130 _reflns_number_gt 18072 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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. Thf molecule disordered 52/48 SIMU/DELU applied/ ; _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^)+(0.0533P)^2^+1.7852P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881: 9231 Friedel pairs' _refine_ls_abs_structure_Flack -0.035(17) _refine_ls_number_reflns 20130 _refine_ls_number_parameters 1032 _refine_ls_number_restraints 181 _refine_ls_R_factor_all 0.0479 _refine_ls_R_factor_gt 0.0401 _refine_ls_wR_factor_ref 0.1038 _refine_ls_wR_factor_gt 0.0975 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.003 _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 0.256561(11) 0.234048(9) 0.203486(11) 0.02445(5) Uani 1 1 d . A . Rh2 Rh 0.257848(12) 0.200389(10) 0.335064(12) 0.02771(6) Uani 1 1 d D . . C1 C 0.20854(16) 0.11314(15) 0.22980(18) 0.0329(7) Uani 1 1 d . . . C2 C 0.17860(17) 0.05277(16) 0.2035(2) 0.0360(7) Uani 1 1 d . A . H2A H 0.1370 0.0649 0.1834 0.043 Uiso 1 1 calc R . . C3 C 0.1650(2) 0.00405(19) 0.2668(2) 0.0542(11) Uani 1 1 d . . . C4 C 0.2234(3) -0.0197(2) 0.3073(3) 0.0764(17) Uani 1 1 d . A . H4A H 0.2117 -0.0470 0.3500 0.115 Uiso 1 1 calc R . . H4B H 0.2471 0.0150 0.3279 0.115 Uiso 1 1 calc R . . H4C H 0.2489 -0.0423 0.2700 0.115 Uiso 1 1 calc R . . C5 C 0.1317(3) -0.0507(2) 0.2282(3) 0.0778(17) Uani 1 1 d . A . H5A H 0.1214 -0.0813 0.2677 0.117 Uiso 1 1 calc R . . H5B H 0.1590 -0.0692 0.1892 0.117 Uiso 1 1 calc R . . H5C H 0.0937 -0.0364 0.2031 0.117 Uiso 1 1 calc R . . C6 C 0.1198(3) 0.0313(2) 0.3261(3) 0.0713(15) Uani 1 1 d . A . H6A H 0.1068 -0.0006 0.3626 0.107 Uiso 1 1 calc R . . H6B H 0.0835 0.0476 0.2991 0.107 Uiso 1 1 calc R . . H6C H 0.1403 0.0645 0.3547 0.107 Uiso 1 1 calc R . . C7 C 0.17594(18) 0.01199(16) 0.0705(2) 0.0361(8) Uani 1 1 d . A . C8 C 0.2090(2) -0.02025(15) 0.00669(19) 0.0382(8) Uani 1 1 d . . . C9 C 0.1744(2) -0.04840(18) -0.0511(2) 0.0440(9) Uani 1 1 d . . . H9A H 0.1307 -0.0443 -0.0517 0.053 Uiso 1 1 calc R . . C10 C 0.2042(2) -0.08270(18) -0.1082(2) 0.0532(11) Uani 1 1 d . . . H10A H 0.1802 -0.1045 -0.1453 0.064 Uiso 1 1 calc R . . C11 C 0.2661(2) -0.08550(17) -0.1116(2) 0.0538(11) Uani 1 1 d . . . H11A H 0.2853 -0.1084 -0.1518 0.065 Uiso 1 1 calc R . . C12 C 0.3036(2) -0.05471(18) -0.0558(2) 0.0494(10) Uani 1 1 d . . . C13 C 0.2729(2) -0.02392(16) 0.0071(2) 0.0408(9) Uani 1 1 d . . . C14 C 0.30881(18) 0.00131(16) 0.0673(2) 0.0407(8) Uani 1 1 d . . . C15 C 0.3718(2) -0.0012(2) 0.0656(3) 0.0534(10) Uani 1 1 d . . . H15A H 0.3954 0.0158 0.1068 0.064 Uiso 1 1 calc R . . C16 C 0.4019(2) -0.0293(2) 0.0020(3) 0.0647(13) Uani 1 1 d . . . H16A H 0.4458 -0.0302 0.0001 0.078 Uiso 1 1 calc R . . C17 C 0.3690(2) -0.0548(2) -0.0559(3) 0.0614(12) Uani 1 1 d . . . H17A H 0.3903 -0.0734 -0.0979 0.074 Uiso 1 1 calc R . . C18 C 0.27667(17) 0.02799(16) 0.1355(2) 0.0376(8) Uani 1 1 d . A . C19 C 0.36885(15) 0.17446(14) 0.25023(19) 0.0308(6) Uani 1 1 d . . . C20 C 0.43472(15) 0.14964(15) 0.2379(2) 0.0338(7) Uani 1 1 d . A . H20A H 0.4298 0.1142 0.2016 0.041 Uiso 1 1 calc R . . C21 C 0.46836(18) 0.12288(18) 0.3103(2) 0.0451(9) Uani 1 1 d . . . C22 C 0.4748(2) 0.1680(2) 0.3764(2) 0.0563(11) Uani 1 1 d . A . H22A H 0.5019 0.2017 0.3605 0.084 Uiso 1 1 calc R . . H22B H 0.4927 0.1472 0.4216 0.084 Uiso 1 1 calc R . . H22C H 0.4340 0.1843 0.3901 0.084 Uiso 1 1 calc R . . C23 C 0.5338(2) 0.1018(2) 0.2859(3) 0.0644(13) Uani 1 1 d . A . H23A H 0.5583 0.1374 0.2701 0.097 Uiso 1 1 calc R . . H23B H 0.5306 0.0731 0.2424 0.097 Uiso 1 1 calc R . . H23C H 0.5541 0.0814 0.3298 0.097 Uiso 1 1 calc R . . C24 C 0.4317(2) 0.06619(19) 0.3371(3) 0.0575(11) Uani 1 1 d . A . H24A H 0.3912 0.0790 0.3567 0.086 Uiso 1 1 calc R . . H24B H 0.4546 0.0452 0.3784 0.086 Uiso 1 1 calc R . . H24C H 0.4261 0.0382 0.2932 0.086 Uiso 1 1 calc R . . C25 C 0.50630(16) 0.17450(17) 0.1316(2) 0.0385(8) Uani 1 1 d . A . C26 C 0.54057(16) 0.22149(18) 0.0854(2) 0.0408(8) Uani 1 1 d . . . C27 C 0.57680(16) 0.2028(2) 0.0243(2) 0.0481(9) Uani 1 1 d . . . H27A H 0.5829 0.1603 0.0150 0.058 Uiso 1 1 calc R . . C28 C 0.60503(18) 0.2465(3) -0.0248(3) 0.0603(12) Uani 1 1 d . . . H28A H 0.6300 0.2335 -0.0670 0.072 Uiso 1 1 calc R . . C29 C 0.5962(2) 0.3073(3) -0.0113(3) 0.0638(14) Uani 1 1 d . . . H29A H 0.6150 0.3363 -0.0449 0.077 Uiso 1 1 calc R . . C30 C 0.55982(19) 0.3287(2) 0.0516(3) 0.0530(10) Uani 1 1 d . . . C31 C 0.53182(16) 0.28409(18) 0.1007(2) 0.0421(8) Uani 1 1 d . . . C32 C 0.49393(17) 0.30353(17) 0.1624(2) 0.0428(8) Uani 1 1 d . . . C33 C 0.4832(2) 0.36499(18) 0.1760(3) 0.0540(10) Uani 1 1 d . . . H33A H 0.4575 0.3777 0.2177 0.065 Uiso 1 1 calc R . . C34 C 0.5111(3) 0.4082(2) 0.1268(3) 0.0707(14) Uani 1 1 d . . . H34A H 0.5036 0.4506 0.1353 0.085 Uiso 1 1 calc R . . C35 C 0.5479(2) 0.3913(2) 0.0680(3) 0.0661(13) Uani 1 1 d . . . H35A H 0.5665 0.4220 0.0366 0.079 Uiso 1 1 calc R . . C36 C 0.46476(16) 0.25771(16) 0.2144(2) 0.0387(8) Uani 1 1 d . A . C37 C 0.30387(14) 0.32123(14) 0.31399(18) 0.0295(6) Uani 1 1 d . . . C38 C 0.33284(16) 0.38211(14) 0.3402(2) 0.0345(7) Uani 1 1 d . A . H38A H 0.3746 0.3833 0.3153 0.041 Uiso 1 1 calc R . . C39 C 0.3452(2) 0.38978(17) 0.4296(2) 0.0461(9) Uani 1 1 d . . . C40 C 0.3931(2) 0.3418(2) 0.4540(3) 0.0613(12) Uani 1 1 d . A . H40A H 0.4056 0.3493 0.5078 0.092 Uiso 1 1 calc R . . H40B H 0.4294 0.3447 0.4201 0.092 Uiso 1 1 calc R . . H40C H 0.3750 0.3008 0.4497 0.092 Uiso 1 1 calc R . . C41 C 0.3751(3) 0.4536(2) 0.4423(3) 0.0679(14) Uani 1 1 d . A . H41A H 0.3874 0.4578 0.4967 0.102 Uiso 1 1 calc R . . H41B H 0.3452 0.4857 0.4292 0.102 Uiso 1 1 calc R . . H41C H 0.4116 0.4576 0.4090 0.102 Uiso 1 1 calc R . . C42 C 0.2877(2) 0.3851(2) 0.4797(2) 0.0627(12) Uani 1 1 d . A . H42A H 0.2996 0.3865 0.5345 0.094 Uiso 1 1 calc R . . H42B H 0.2665 0.3464 0.4688 0.094 Uiso 1 1 calc R . . H42C H 0.2600 0.4194 0.4681 0.094 Uiso 1 1 calc R . . C43 C 0.23351(16) 0.43350(15) 0.30910(19) 0.0349(7) Uani 1 1 d . A . C44 C 0.20067(18) 0.48893(17) 0.2792(2) 0.0402(8) Uani 1 1 d . . . C45 C 0.1368(2) 0.4904(2) 0.2810(3) 0.0530(11) Uani 1 1 d . . . H45A H 0.1141 0.4559 0.2988 0.064 Uiso 1 1 calc R . . C46 C 0.1059(2) 0.5432(2) 0.2562(3) 0.0657(13) Uani 1 1 d . . . H46A H 0.0620 0.5445 0.2573 0.079 Uiso 1 1 calc R . . C47 C 0.1381(3) 0.5926(2) 0.2306(3) 0.0664(14) Uani 1 1 d . . . H47A H 0.1162 0.6283 0.2155 0.080 Uiso 1 1 calc R . . C48 C 0.2025(2) 0.59224(19) 0.2259(2) 0.0503(10) Uani 1 1 d . . . C49 C 0.23498(19) 0.53845(15) 0.25043(19) 0.0396(8) Uani 1 1 d . . . C50 C 0.29926(19) 0.53569(16) 0.2441(2) 0.0412(8) Uani 1 1 d . . . C51 C 0.3323(2) 0.5849(2) 0.2150(3) 0.0571(11) Uani 1 1 d . . . H51A H 0.3760 0.5824 0.2100 0.069 Uiso 1 1 calc R . . C52 C 0.3010(3) 0.6385(2) 0.1928(3) 0.0696(14) Uani 1 1 d . . . H52A H 0.3238 0.6728 0.1744 0.083 Uiso 1 1 calc R . . C53 C 0.2386(3) 0.64178(18) 0.1975(2) 0.0648(13) Uani 1 1 d . . . H53A H 0.2184 0.6782 0.1813 0.078 Uiso 1 1 calc R . . C54 C 0.33319(18) 0.48004(16) 0.2691(2) 0.0377(8) Uani 1 1 d . A . C55 C 0.14711(15) 0.26205(15) 0.29042(18) 0.0331(6) Uani 1 1 d . . . C56 C 0.08490(15) 0.29357(17) 0.3020(2) 0.0368(7) Uani 1 1 d . A . H56A H 0.0941 0.3383 0.2965 0.044 Uiso 1 1 calc R . . C57 C 0.05227(19) 0.2879(2) 0.3826(2) 0.0537(11) Uani 1 1 d . . . C58 C 0.0940(2) 0.3194(3) 0.4424(2) 0.0693(15) Uani 1 1 d . A . H58A H 0.0727 0.3209 0.4926 0.104 Uiso 1 1 calc R . . H58B H 0.1032 0.3611 0.4251 0.104 Uiso 1 1 calc R . . H58C H 0.1325 0.2962 0.4477 0.104 Uiso 1 1 calc R . . C59 C 0.0378(3) 0.2226(3) 0.4075(3) 0.0793(17) Uani 1 1 d . A . H59A H 0.0241 0.2225 0.4617 0.119 Uiso 1 1 calc R . . H59B H 0.0750 0.1972 0.4023 0.119 Uiso 1 1 calc R . . H59C H 0.0049 0.2059 0.3745 0.119 Uiso 1 1 calc R . . C60 C -0.0087(2) 0.3242(3) 0.3781(3) 0.0836(19) Uani 1 1 d . A . H60A H -0.0266 0.3278 0.4301 0.125 Uiso 1 1 calc R . . H60B H -0.0378 0.3028 0.3440 0.125 Uiso 1 1 calc R . . H60C H -0.0005 0.3652 0.3573 0.125 Uiso 1 1 calc R . . C61 C 0.03722(16) 0.21704(18) 0.2144(2) 0.0409(8) Uani 1 1 d . A . C62 C -0.00723(16) 0.20300(17) 0.1515(2) 0.0393(7) Uani 1 1 d . . . C63 C -0.02053(19) 0.1428(2) 0.1336(3) 0.0510(10) Uani 1 1 d . . . H63A H -0.0026 0.1106 0.1632 0.061 Uiso 1 1 calc R . . C64 C -0.0605(2) 0.1289(2) 0.0719(3) 0.0589(11) Uani 1 1 d . . . H64A H -0.0702 0.0874 0.0603 0.071 Uiso 1 1 calc R . . C65 C -0.08568(19) 0.1752(2) 0.0284(3) 0.0539(11) Uani 1 1 d . . . H65A H -0.1122 0.1652 -0.0136 0.065 Uiso 1 1 calc R . . C66 C -0.07327(16) 0.2367(2) 0.0443(2) 0.0455(9) Uani 1 1 d . . . C67 C -0.03414(15) 0.25127(18) 0.1086(2) 0.0411(8) Uani 1 1 d . . . C68 C -0.02003(16) 0.31238(18) 0.1256(2) 0.0406(8) Uani 1 1 d . . . C69 C -0.04396(18) 0.3592(2) 0.0801(2) 0.0478(9) Uani 1 1 d . . . H69A H -0.0345 0.4007 0.0918 0.057 Uiso 1 1 calc R . . C70 C -0.08191(18) 0.3451(2) 0.0173(3) 0.0539(11) Uani 1 1 d . . . H70A H -0.0983 0.3774 -0.0134 0.065 Uiso 1 1 calc R . . C71 C -0.09605(17) 0.2864(2) -0.0011(2) 0.0515(11) Uani 1 1 d . . . H71A H -0.1215 0.2783 -0.0449 0.062 Uiso 1 1 calc R . . C72 C 0.02082(15) 0.32785(18) 0.1907(2) 0.0390(8) Uani 1 1 d . A . C73 C 0.25540(15) 0.23014(14) 0.01234(16) 0.0324(6) Uani 1 1 d . A . C74 C 0.26049(18) 0.16169(14) 0.0115(2) 0.0402(7) Uani 1 1 d . . . H74A H 0.2844 0.1481 0.0566 0.060 Uiso 1 1 calc R . . H74B H 0.2813 0.1486 -0.0362 0.060 Uiso 1 1 calc R . . H74C H 0.2190 0.1436 0.0135 0.060 Uiso 1 1 calc R . . C75 C 0.2406(2) 0.31854(15) -0.0659(2) 0.0439(8) Uani 1 1 d . A . H75A H 0.2790 0.3402 -0.0508 0.053 Uiso 1 1 calc R . . H75B H 0.2068 0.3323 -0.0313 0.053 Uiso 1 1 calc R . . C76 C 0.2249(3) 0.3323(2) -0.1486(3) 0.0812(18) Uani 1 1 d . . . H76A H 0.2188 0.3765 -0.1549 0.122 Uiso 1 1 calc R . . H76B H 0.1868 0.3107 -0.1628 0.122 Uiso 1 1 calc R . . H76C H 0.2587 0.3187 -0.1823 0.122 Uiso 1 1 calc R . . C81 C 0.1340(4) 0.2480(4) 0.6665(5) 0.108(2) Uani 1 1 d . . . C82 C 0.1857(5) 0.2875(6) 0.6363(5) 0.172(5) Uani 1 1 d . . . H82A H 0.1805 0.3295 0.6555 0.258 Uiso 1 1 calc R . . H82B H 0.1848 0.2876 0.5795 0.258 Uiso 1 1 calc R . . H82C H 0.2254 0.2712 0.6543 0.258 Uiso 1 1 calc R . . C83 C 0.0685(3) 0.1646(3) 0.6413(4) 0.098(2) Uani 1 1 d . . . H83A H 0.0290 0.1870 0.6354 0.118 Uiso 1 1 calc R . . H83B H 0.0736 0.1535 0.6966 0.118 Uiso 1 1 calc R . . C84 C 0.0678(5) 0.1094(4) 0.5937(7) 0.166(4) Uani 1 1 d . . . H84A H 0.0422 0.0781 0.6188 0.249 Uiso 1 1 calc R . . H84B H 0.1101 0.0939 0.5877 0.249 Uiso 1 1 calc R . . H84C H 0.0506 0.1190 0.5425 0.249 Uiso 1 1 calc R . . N1 N 0.21180(15) 0.02885(13) 0.13521(17) 0.0357(6) Uani 1 1 d . . . N2 N 0.47123(12) 0.19567(13) 0.19406(18) 0.0355(6) Uani 1 1 d . . . N3 N 0.29836(13) 0.43450(12) 0.30625(16) 0.0325(6) Uani 1 1 d . . . N4 N 0.04388(13) 0.27901(15) 0.23474(17) 0.0375(7) Uani 1 1 d . . . O1 O 0.21694(10) 0.15195(10) 0.17633(12) 0.0306(5) Uani 1 1 d . A . O2 O 0.22012(11) 0.12026(10) 0.30075(13) 0.0354(5) Uani 1 1 d . A . O3 O 0.12067(13) 0.02179(13) 0.06934(16) 0.0465(6) Uani 1 1 d . . . O4 O 0.30496(13) 0.04872(13) 0.19105(17) 0.0477(7) Uani 1 1 d . . . O5 O 0.34321(10) 0.19755(10) 0.19072(12) 0.0300(4) Uani 1 1 d . A . O6 O 0.34416(11) 0.16692(10) 0.31566(12) 0.0328(5) Uani 1 1 d . A . O7 O 0.50784(13) 0.12028(12) 0.11513(17) 0.0504(7) Uani 1 1 d . . . O8 O 0.43524(12) 0.27224(12) 0.27113(15) 0.0427(6) Uani 1 1 d . . . O9 O 0.29452(10) 0.31536(10) 0.24189(12) 0.0300(5) Uani 1 1 d . A . O10 O 0.29526(11) 0.28121(9) 0.36561(12) 0.0328(5) Uani 1 1 d . A . O11 O 0.20644(11) 0.38946(11) 0.33519(16) 0.0427(6) Uani 1 1 d . . . O12 O 0.38865(13) 0.47404(13) 0.25919(19) 0.0521(7) Uani 1 1 d . . . O13 O 0.17045(10) 0.26910(11) 0.22347(12) 0.0310(5) Uani 1 1 d . A . O14 O 0.17221(10) 0.23655(11) 0.34772(13) 0.0355(5) Uani 1 1 d . A . O15 O 0.06713(13) 0.17773(13) 0.24750(17) 0.0514(7) Uani 1 1 d . . . O16 O 0.03411(12) 0.38099(12) 0.20777(17) 0.0484(6) Uani 1 1 d . . . O17 O 0.25597(10) 0.26272(9) 0.06980(11) 0.0307(4) Uani 1 1 d . . . O18 O 0.24907(13) 0.25308(10) -0.05898(12) 0.0412(5) Uani 1 1 d . . . O20 O 0.1095(2) 0.2549(3) 0.7289(3) 0.1105(15) Uani 1 1 d . . . O21 O 0.1187(2) 0.2023(3) 0.6168(3) 0.1173(17) Uani 1 1 d . . . O19 O 0.2594(11) 0.1675(14) 0.4612(10) 0.0473(10) Uani 0.519(9) 1 d PDU A 1 C77 C 0.2373(8) 0.1095(8) 0.4791(7) 0.094(4) Uani 0.519(9) 1 d PDU A 1 H77A H 0.2612 0.0771 0.4523 0.113 Uiso 0.519(9) 1 calc PR A 1 H77B H 0.1930 0.1053 0.4659 0.113 Uiso 0.519(9) 1 calc PR A 1 C78 C 0.2481(8) 0.1077(9) 0.5701(8) 0.114(5) Uani 0.519(9) 1 d PDU A 1 H78A H 0.2364 0.0685 0.5949 0.137 Uiso 0.519(9) 1 calc PR A 1 H78B H 0.2304 0.1431 0.5983 0.137 Uiso 0.519(9) 1 calc PR A 1 C79 C 0.3208(7) 0.1140(7) 0.5510(8) 0.112(4) Uani 0.519(9) 1 d PDU A 1 H79A H 0.3472 0.1145 0.5979 0.135 Uiso 0.519(9) 1 calc PR A 1 H79B H 0.3358 0.0832 0.5133 0.135 Uiso 0.519(9) 1 calc PR A 1 C80 C 0.3103(8) 0.1826(8) 0.5125(9) 0.097(4) Uani 0.519(9) 1 d PDU A 1 H80A H 0.2985 0.2135 0.5519 0.116 Uiso 0.519(9) 1 calc PR A 1 H80B H 0.3472 0.1969 0.4836 0.116 Uiso 0.519(9) 1 calc PR A 1 O19' O 0.2610(12) 0.1710(15) 0.4621(11) 0.0473(10) Uani 0.481(9) 1 d PDU A 2 C77' C 0.2208(8) 0.1314(9) 0.4972(9) 0.094(4) Uani 0.481(9) 1 d PDU A 2 H77C H 0.1990 0.1058 0.4584 0.113 Uiso 0.481(9) 1 calc PR A 2 H77D H 0.1899 0.1536 0.5288 0.113 Uiso 0.481(9) 1 calc PR A 2 C78' C 0.2650(9) 0.0909(9) 0.5503(10) 0.114(5) Uani 0.481(9) 1 d PDU A 2 H78C H 0.2906 0.0619 0.5201 0.137 Uiso 0.481(9) 1 calc PR A 2 H78D H 0.2424 0.0690 0.5919 0.137 Uiso 0.481(9) 1 calc PR A 2 C79' C 0.3040(8) 0.1490(8) 0.5823(7) 0.112(4) Uani 0.481(9) 1 d PDU A 2 H79C H 0.2783 0.1812 0.6065 0.135 Uiso 0.481(9) 1 calc PR A 2 H79D H 0.3393 0.1378 0.6159 0.135 Uiso 0.481(9) 1 calc PR A 2 C80' C 0.3226(8) 0.1627(10) 0.4938(9) 0.097(4) Uani 0.481(9) 1 d PDU A 2 H80C H 0.3481 0.2002 0.4889 0.116 Uiso 0.481(9) 1 calc PR A 2 H80D H 0.3444 0.1277 0.4696 0.116 Uiso 0.481(9) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02767(11) 0.02584(10) 0.01984(9) 0.00028(7) -0.00064(9) 0.00128(9) Rh2 0.03389(12) 0.02925(10) 0.02000(9) 0.00106(8) -0.00104(10) 0.00181(10) C1 0.0356(17) 0.0343(16) 0.0289(15) 0.0009(12) 0.0028(13) -0.0019(14) C2 0.050(2) 0.0330(16) 0.0254(15) 0.0010(14) 0.0022(15) -0.0083(14) C3 0.085(3) 0.042(2) 0.0354(19) 0.0055(16) -0.002(2) -0.020(2) C4 0.134(5) 0.050(2) 0.046(2) 0.021(2) -0.015(3) -0.013(3) C5 0.131(5) 0.053(3) 0.049(3) 0.005(2) 0.004(3) -0.046(3) C6 0.091(4) 0.078(3) 0.045(2) 0.003(2) 0.014(2) -0.039(3) C7 0.052(2) 0.0258(16) 0.0301(17) 0.0010(13) -0.0043(15) -0.0049(14) C8 0.065(2) 0.0241(16) 0.0260(16) 0.0053(13) -0.0026(16) -0.0026(15) C9 0.065(3) 0.0374(19) 0.0300(18) 0.0043(15) -0.0046(17) -0.0053(17) C10 0.097(4) 0.037(2) 0.0263(18) -0.0014(15) -0.002(2) -0.005(2) C11 0.096(4) 0.0365(18) 0.0286(17) 0.0055(14) 0.007(2) 0.005(2) C12 0.078(3) 0.0331(19) 0.037(2) 0.0052(16) 0.013(2) 0.0102(18) C13 0.064(3) 0.0264(16) 0.0318(18) 0.0033(13) 0.0021(16) 0.0054(15) C14 0.049(2) 0.0287(17) 0.044(2) 0.0022(15) 0.0006(17) 0.0023(15) C15 0.054(2) 0.045(2) 0.061(3) 0.001(2) 0.002(2) 0.0062(18) C16 0.058(3) 0.058(3) 0.078(3) 0.006(3) 0.016(2) 0.015(2) C17 0.079(3) 0.048(2) 0.058(3) 0.003(2) 0.017(2) 0.017(2) C18 0.047(2) 0.0288(16) 0.0372(19) -0.0009(14) -0.0046(15) -0.0010(13) C19 0.0326(16) 0.0250(14) 0.0350(16) -0.0025(13) -0.0041(13) 0.0017(12) C20 0.0336(16) 0.0295(16) 0.0382(17) 0.0018(13) -0.0007(14) 0.0057(13) C21 0.046(2) 0.045(2) 0.044(2) 0.0095(16) -0.0068(16) 0.0118(16) C22 0.055(2) 0.069(3) 0.045(2) 0.002(2) -0.0206(19) 0.008(2) C23 0.047(2) 0.075(3) 0.071(3) 0.015(3) -0.007(2) 0.024(2) C24 0.063(3) 0.047(2) 0.062(3) 0.018(2) -0.004(2) 0.0103(19) C25 0.0325(17) 0.0409(19) 0.0420(19) 0.0004(16) -0.0021(14) 0.0088(14) C26 0.0273(16) 0.053(2) 0.043(2) 0.0059(16) -0.0035(14) 0.0022(14) C27 0.0293(17) 0.066(3) 0.049(2) 0.002(2) -0.0021(15) 0.0028(17) C28 0.0274(18) 0.102(4) 0.052(2) 0.006(3) -0.0053(16) -0.006(2) C29 0.038(2) 0.095(4) 0.059(3) 0.023(3) -0.0079(19) -0.022(2) C30 0.041(2) 0.064(3) 0.055(2) 0.016(2) -0.0118(18) -0.0133(19) C31 0.0312(17) 0.048(2) 0.047(2) 0.0058(17) -0.0096(15) -0.0030(14) C32 0.0390(18) 0.0384(18) 0.051(2) 0.0001(18) -0.0101(17) -0.0017(15) C33 0.061(3) 0.036(2) 0.066(3) 0.0031(19) -0.005(2) -0.0017(17) C34 0.085(4) 0.040(2) 0.087(4) 0.009(2) -0.012(3) -0.006(2) C35 0.072(3) 0.053(3) 0.073(3) 0.019(2) -0.010(3) -0.024(2) C36 0.0333(16) 0.0349(18) 0.048(2) -0.0023(16) -0.0069(15) 0.0036(14) C37 0.0277(14) 0.0314(15) 0.0295(15) -0.0028(12) -0.0022(11) 0.0071(12) C38 0.0364(17) 0.0292(15) 0.0381(17) -0.0049(14) -0.0064(15) 0.0033(13) C39 0.061(2) 0.0399(19) 0.0380(19) -0.0072(15) -0.0176(18) 0.0000(17) C40 0.071(3) 0.055(3) 0.057(3) -0.001(2) -0.033(2) 0.003(2) C41 0.103(4) 0.046(2) 0.055(3) -0.014(2) -0.036(3) -0.004(2) C42 0.088(3) 0.071(3) 0.0297(19) -0.0140(19) 0.000(2) 0.013(3) C43 0.0395(18) 0.0337(15) 0.0315(15) -0.0062(12) -0.0021(13) 0.0044(14) C44 0.048(2) 0.0357(18) 0.0371(18) -0.0081(14) -0.0041(15) 0.0086(15) C45 0.048(2) 0.046(2) 0.065(3) -0.010(2) -0.007(2) 0.0130(18) C46 0.054(3) 0.066(3) 0.077(3) -0.012(3) -0.019(2) 0.023(2) C47 0.089(4) 0.056(3) 0.055(3) -0.005(2) -0.024(3) 0.034(3) C48 0.076(3) 0.042(2) 0.0334(18) -0.0035(15) -0.0105(18) 0.017(2) C49 0.055(2) 0.0343(16) 0.0292(15) -0.0048(13) -0.0091(15) 0.0085(16) C50 0.061(2) 0.0331(17) 0.0300(17) -0.0037(14) -0.0012(16) -0.0012(16) C51 0.080(3) 0.043(2) 0.049(2) 0.0003(19) 0.008(2) -0.006(2) C52 0.113(5) 0.042(2) 0.053(3) 0.004(2) 0.007(3) -0.007(3) C53 0.116(4) 0.0368(19) 0.042(2) 0.0089(16) -0.004(3) 0.015(2) C54 0.046(2) 0.0310(17) 0.0362(18) -0.0047(13) -0.0005(15) -0.0047(15) C55 0.0348(15) 0.0351(16) 0.0293(15) -0.0023(14) 0.0008(13) -0.0005(13) C56 0.0334(16) 0.0457(19) 0.0314(16) -0.0030(15) 0.0029(14) 0.0023(14) C57 0.039(2) 0.086(3) 0.0358(19) -0.003(2) 0.0107(16) 0.0084(19) C58 0.056(3) 0.118(5) 0.034(2) -0.010(3) 0.0058(19) 0.018(3) C59 0.065(3) 0.120(5) 0.053(3) 0.018(3) 0.020(2) -0.005(3) C60 0.046(3) 0.153(6) 0.051(3) -0.005(3) 0.016(2) 0.031(3) C61 0.0331(17) 0.049(2) 0.041(2) 0.0090(17) 0.0022(14) -0.0061(14) C62 0.0329(16) 0.0443(19) 0.0407(19) 0.0036(16) 0.0041(14) -0.0085(15) C63 0.046(2) 0.054(2) 0.053(2) 0.009(2) -0.0033(18) -0.0180(18) C64 0.061(3) 0.059(3) 0.057(3) 0.001(2) 0.003(2) -0.026(2) C65 0.040(2) 0.076(3) 0.046(2) 0.001(2) 0.0016(17) -0.019(2) C66 0.0285(16) 0.067(3) 0.0406(19) 0.0007(19) 0.0032(14) -0.0074(17) C67 0.0245(15) 0.059(2) 0.0400(19) 0.0030(17) 0.0045(13) -0.0039(14) C68 0.0299(17) 0.051(2) 0.0414(19) 0.0021(16) 0.0046(14) 0.0038(14) C69 0.0381(19) 0.055(2) 0.050(2) 0.0023(19) 0.0040(17) 0.0074(17) C70 0.038(2) 0.074(3) 0.049(2) 0.014(2) 0.0010(17) 0.0125(19) C71 0.0321(18) 0.083(3) 0.039(2) 0.003(2) -0.0028(15) -0.0008(18) C72 0.0292(16) 0.045(2) 0.0426(19) 0.0042(16) 0.0049(14) 0.0062(14) C73 0.0309(15) 0.0388(15) 0.0275(13) 0.0034(11) 0.0014(12) -0.0018(14) C74 0.0464(19) 0.0336(15) 0.0406(16) 0.0011(13) 0.0083(16) 0.0000(15) C75 0.058(2) 0.0355(16) 0.0384(16) 0.0032(13) -0.0080(18) -0.0002(17) C76 0.149(6) 0.050(2) 0.045(2) 0.0123(19) -0.018(3) -0.002(3) C81 0.101(5) 0.139(7) 0.084(5) 0.018(5) -0.022(4) 0.019(5) C82 0.147(8) 0.264(13) 0.105(6) 0.059(8) 0.006(6) -0.070(9) C83 0.099(5) 0.098(5) 0.098(5) 0.017(4) 0.016(4) 0.021(4) C84 0.158(9) 0.107(6) 0.233(12) -0.014(8) 0.007(9) 0.055(6) N1 0.0489(17) 0.0284(14) 0.0297(15) 0.0008(12) -0.0001(12) -0.0061(12) N2 0.0306(13) 0.0346(14) 0.0413(16) -0.0003(13) -0.0011(12) 0.0039(11) N3 0.0368(14) 0.0275(13) 0.0333(14) -0.0028(11) -0.0012(12) 0.0026(11) N4 0.0290(14) 0.0467(19) 0.0367(16) 0.0019(13) 0.0010(11) 0.0031(12) O1 0.0344(11) 0.0308(11) 0.0266(10) 0.0004(8) -0.0010(9) -0.0052(9) O2 0.0490(13) 0.0331(11) 0.0243(10) 0.0026(9) -0.0008(10) -0.0054(10) O3 0.0482(16) 0.0486(15) 0.0427(15) -0.0045(13) -0.0060(12) -0.0031(12) O4 0.0518(16) 0.0468(15) 0.0444(15) -0.0074(12) -0.0095(13) 0.0034(12) O5 0.0325(11) 0.0299(10) 0.0275(11) -0.0008(9) -0.0021(9) 0.0050(9) O6 0.0381(12) 0.0320(11) 0.0282(11) 0.0016(9) -0.0017(9) 0.0069(9) O7 0.0546(17) 0.0405(14) 0.0561(17) -0.0023(13) 0.0089(14) 0.0123(12) O8 0.0426(14) 0.0375(13) 0.0482(15) -0.0085(11) -0.0004(11) 0.0033(11) O9 0.0360(12) 0.0286(11) 0.0255(10) 0.0005(8) -0.0021(9) 0.0009(9) O10 0.0444(13) 0.0293(11) 0.0247(10) -0.0003(9) -0.0033(9) 0.0033(9) O11 0.0394(13) 0.0373(13) 0.0514(15) -0.0018(12) 0.0051(12) 0.0011(10) O12 0.0446(16) 0.0435(15) 0.0683(19) 0.0002(14) 0.0029(14) -0.0067(12) O13 0.0285(10) 0.0373(12) 0.0271(11) 0.0001(9) 0.0002(8) 0.0033(10) O14 0.0337(11) 0.0452(13) 0.0277(11) 0.0009(10) 0.0026(9) 0.0034(10) O15 0.0511(16) 0.0448(16) 0.0585(18) 0.0128(14) -0.0089(14) -0.0029(13) O16 0.0476(15) 0.0403(14) 0.0574(17) -0.0030(13) -0.0056(13) 0.0053(11) O17 0.0312(10) 0.0350(10) 0.0258(9) 0.0015(8) 0.0003(9) -0.0018(11) O18 0.0577(15) 0.0354(11) 0.0306(10) 0.0004(8) 0.0031(12) -0.0017(12) O20 0.105(3) 0.138(4) 0.088(3) -0.003(3) 0.009(3) 0.013(3) O21 0.099(4) 0.165(5) 0.088(3) 0.015(4) 0.007(3) 0.032(4) O19 0.0526(18) 0.059(3) 0.0300(11) 0.0104(14) -0.0046(12) -0.0017(16) C77 0.126(7) 0.110(9) 0.047(5) 0.026(5) -0.009(5) -0.038(6) C78 0.150(8) 0.122(9) 0.069(6) 0.051(6) -0.019(6) -0.033(7) C79 0.132(7) 0.147(9) 0.058(6) 0.041(6) -0.028(5) -0.012(7) C80 0.095(6) 0.152(9) 0.043(6) 0.028(6) -0.012(5) -0.025(6) O19' 0.0526(18) 0.059(3) 0.0300(11) 0.0104(14) -0.0046(12) -0.0017(16) C77' 0.126(7) 0.110(9) 0.047(5) 0.026(5) -0.009(5) -0.038(6) C78' 0.150(8) 0.122(9) 0.069(6) 0.051(6) -0.019(6) -0.033(7) C79' 0.132(7) 0.147(9) 0.058(6) 0.041(6) -0.028(5) -0.012(7) C80' 0.095(6) 0.152(9) 0.043(6) 0.028(6) -0.012(5) -0.025(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 O13 2.042(2) . ? Rh1 O1 2.041(2) . ? Rh1 O5 2.048(2) . ? Rh1 O9 2.064(2) . ? Rh1 Rh2 2.3843(10) . ? Rh1 O17 2.388(2) . ? Rh2 O10 2.011(2) . ? Rh2 O2 2.018(2) . ? Rh2 O14 2.025(2) . ? Rh2 O6 2.032(2) . ? Rh2 O19' 2.282(11) . ? Rh2 O19 2.290(10) . ? C1 O2 1.258(4) . ? C1 O1 1.265(4) . ? C1 C2 1.536(5) . ? C2 N1 1.474(5) . ? C2 C3 1.552(5) . ? C3 C4 1.534(7) . ? C3 C6 1.535(7) . ? C3 C5 1.546(6) . ? C7 O3 1.214(5) . ? C7 N1 1.408(5) . ? C7 C8 1.489(5) . ? C8 C13 1.384(6) . ? C8 C9 1.389(5) . ? C9 C10 1.394(6) . ? C10 C11 1.342(7) . ? C11 C12 1.425(6) . ? C12 C17 1.415(7) . ? C12 C13 1.438(5) . ? C13 C14 1.408(5) . ? C14 C15 1.365(6) . ? C14 C18 1.484(5) . ? C15 C16 1.414(6) . ? C16 C17 1.345(7) . ? C18 O4 1.223(4) . ? C18 N1 1.403(5) . ? C19 O6 1.259(4) . ? C19 O5 1.270(4) . ? C19 C20 1.539(5) . ? C20 N2 1.485(4) . ? C20 C21 1.558(5) . ? C21 C22 1.513(6) . ? C21 C24 1.540(6) . ? C21 C23 1.547(6) . ? C25 O7 1.217(4) . ? C25 N2 1.396(5) . ? C25 C26 1.495(5) . ? C26 C27 1.374(5) . ? C26 C31 1.404(5) . ? C27 C28 1.414(6) . ? C28 C29 1.361(8) . ? C29 C30 1.419(7) . ? C30 C35 1.419(7) . ? C30 C31 1.425(6) . ? C31 C32 1.409(6) . ? C32 C33 1.381(5) . ? C32 C36 1.483(5) . ? C33 C34 1.405(7) . ? C34 C35 1.340(8) . ? C36 O8 1.210(4) . ? C36 N2 1.405(4) . ? C37 O10 1.261(4) . ? C37 O9 1.266(4) . ? C37 C38 1.537(4) . ? C38 N3 1.485(4) . ? C38 C39 1.572(5) . ? C39 C42 1.517(6) . ? C39 C40 1.532(6) . ? C39 C41 1.551(6) . ? C43 O11 1.212(4) . ? C43 N3 1.403(5) . ? C43 C44 1.495(5) . ? C44 C45 1.383(6) . ? C44 C49 1.402(5) . ? C45 C46 1.398(6) . ? C46 C47 1.357(8) . ? C47 C48 1.394(7) . ? C48 C53 1.422(7) . ? C48 C49 1.432(5) . ? C49 C50 1.396(6) . ? C50 C51 1.384(6) . ? C50 C54 1.483(5) . ? C51 C52 1.405(7) . ? C52 C53 1.354(8) . ? C54 O12 1.219(5) . ? C54 N3 1.402(4) . ? C55 O14 1.257(4) . ? C55 O13 1.269(4) . ? C55 C56 1.524(4) . ? C56 N4 1.494(5) . ? C56 C57 1.564(5) . ? C57 C59 1.521(8) . ? C57 C58 1.532(7) . ? C57 C60 1.541(6) . ? C61 O15 1.217(4) . ? C61 N4 1.405(5) . ? C61 C62 1.481(5) . ? C62 C63 1.381(6) . ? C62 C67 1.413(5) . ? C63 C64 1.404(6) . ? C64 C65 1.372(7) . ? C65 C66 1.395(6) . ? C66 C67 1.429(5) . ? C66 C71 1.427(6) . ? C67 C68 1.399(6) . ? C68 C69 1.388(5) . ? C68 C72 1.468(5) . ? C69 C70 1.394(6) . ? C70 C71 1.354(7) . ? C72 O16 1.231(5) . ? C72 N4 1.401(5) . ? C73 O17 1.219(3) . ? C73 O18 1.335(3) . ? C73 C74 1.498(4) . ? C75 O18 1.445(4) . ? C75 C76 1.497(5) . ? C81 O20 1.207(9) . ? C81 O21 1.357(10) . ? C81 C82 1.505(11) . ? C83 O21 1.425(8) . ? C83 C84 1.458(11) . ? O19 C77 1.388(16) . ? O19 C80 1.450(14) . ? C77 C78 1.586(15) . ? C78 C79 1.611(18) . ? C79 C80 1.654(16) . ? O19' C77' 1.368(14) . ? O19' C80' 1.451(17) . ? C77' C78' 1.592(17) . ? C78' C79' 1.619(18) . ? C79' C80' 1.606(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 O13 Rh1 O1 89.13(9) . . ? O13 Rh1 O5 176.39(9) . . ? O1 Rh1 O5 91.03(9) . . ? O13 Rh1 O9 89.22(9) . . ? O1 Rh1 O9 174.51(8) . . ? O5 Rh1 O9 90.29(9) . . ? O13 Rh1 Rh2 88.03(6) . . ? O1 Rh1 Rh2 87.28(6) . . ? O5 Rh1 Rh2 88.38(6) . . ? O9 Rh1 Rh2 87.43(6) . . ? O13 Rh1 O17 93.42(8) . . ? O1 Rh1 O17 90.37(8) . . ? O5 Rh1 O17 90.18(8) . . ? O9 Rh1 O17 94.95(8) . . ? Rh2 Rh1 O17 177.22(5) . . ? O10 Rh2 O2 178.10(9) . . ? O10 Rh2 O14 89.88(10) . . ? O2 Rh2 O14 89.97(10) . . ? O10 Rh2 O6 89.36(10) . . ? O2 Rh2 O6 90.67(10) . . ? O14 Rh2 O6 176.30(9) . . ? O10 Rh2 O19' 89.0(7) . . ? O2 Rh2 O19' 92.9(7) . . ? O14 Rh2 O19' 91.9(9) . . ? O6 Rh2 O19' 91.7(9) . . ? O10 Rh2 O19 91.2(7) . . ? O2 Rh2 O19 90.7(7) . . ? O14 Rh2 O19 91.9(8) . . ? O6 Rh2 O19 91.7(8) . . ? O19' Rh2 O19 2.1(13) . . ? O10 Rh2 Rh1 89.05(6) . . ? O2 Rh2 Rh1 89.05(7) . . ? O14 Rh2 Rh1 88.38(6) . . ? O6 Rh2 Rh1 87.99(6) . . ? O19' Rh2 Rh1 178.1(6) . . ? O19 Rh2 Rh1 179.6(10) . . ? O2 C1 O1 126.7(3) . . ? O2 C1 C2 118.5(3) . . ? O1 C1 C2 114.8(3) . . ? N1 C2 C1 109.5(3) . . ? N1 C2 C3 114.3(3) . . ? C1 C2 C3 117.4(3) . . ? C4 C3 C6 110.6(4) . . ? C4 C3 C5 108.5(4) . . ? C6 C3 C5 106.9(4) . . ? C4 C3 C2 113.3(4) . . ? C6 C3 C2 108.9(4) . . ? C5 C3 C2 108.4(3) . . ? O3 C7 N1 120.6(3) . . ? O3 C7 C8 123.0(3) . . ? N1 C7 C8 116.4(3) . . ? C13 C8 C9 121.1(4) . . ? C13 C8 C7 120.2(3) . . ? C9 C8 C7 118.7(4) . . ? C8 C9 C10 119.7(4) . . ? C11 C10 C9 121.0(4) . . ? C10 C11 C12 121.1(4) . . ? C17 C12 C11 124.5(4) . . ? C17 C12 C13 117.6(4) . . ? C11 C12 C13 117.8(4) . . ? C8 C13 C14 122.1(4) . . ? C8 C13 C12 118.9(4) . . ? C14 C13 C12 119.0(4) . . ? C15 C14 C13 121.2(4) . . ? C15 C14 C18 120.1(4) . . ? C13 C14 C18 118.6(3) . . ? C14 C15 C16 119.5(5) . . ? C17 C16 C15 120.8(5) . . ? C16 C17 C12 121.8(4) . . ? O4 C18 N1 119.8(4) . . ? O4 C18 C14 122.1(4) . . ? N1 C18 C14 118.1(3) . . ? O6 C19 O5 126.2(3) . . ? O6 C19 C20 118.1(3) . . ? O5 C19 C20 115.6(3) . . ? N2 C20 C19 108.9(3) . . ? N2 C20 C21 114.4(3) . . ? C19 C20 C21 117.0(3) . . ? C22 C21 C24 110.2(4) . . ? C22 C21 C23 108.3(4) . . ? C24 C21 C23 108.2(3) . . ? C22 C21 C20 113.7(3) . . ? C24 C21 C20 107.5(3) . . ? C23 C21 C20 108.8(3) . . ? O7 C25 N2 121.1(3) . . ? O7 C25 C26 122.0(3) . . ? N2 C25 C26 117.0(3) . . ? C27 C26 C31 120.7(4) . . ? C27 C26 C25 119.1(4) . . ? C31 C26 C25 120.0(3) . . ? C26 C27 C28 120.2(4) . . ? C29 C28 C27 119.7(4) . . ? C28 C29 C30 121.9(4) . . ? C35 C30 C31 117.5(4) . . ? C35 C30 C29 124.8(4) . . ? C31 C30 C29 117.7(4) . . ? C26 C31 C32 120.9(3) . . ? C26 C31 C30 119.8(4) . . ? C32 C31 C30 119.3(4) . . ? C33 C32 C31 121.2(4) . . ? C33 C32 C36 118.7(4) . . ? C31 C32 C36 120.0(3) . . ? C32 C33 C34 118.5(5) . . ? C35 C34 C33 121.8(4) . . ? C34 C35 C30 121.6(4) . . ? O8 C36 N2 120.4(3) . . ? O8 C36 C32 122.4(3) . . ? N2 C36 C32 117.2(3) . . ? O10 C37 O9 126.8(3) . . ? O10 C37 C38 116.9(3) . . ? O9 C37 C38 116.2(3) . . ? N3 C38 C37 110.2(3) . . ? N3 C38 C39 112.9(3) . . ? C37 C38 C39 116.7(3) . . ? C42 C39 C40 110.6(4) . . ? C42 C39 C41 108.8(4) . . ? C40 C39 C41 107.0(4) . . ? C42 C39 C38 114.3(3) . . ? C40 C39 C38 108.2(3) . . ? C41 C39 C38 107.8(3) . . ? O11 C43 N3 120.5(3) . . ? O11 C43 C44 122.7(3) . . ? N3 C43 C44 116.8(3) . . ? C45 C44 C49 121.2(4) . . ? C45 C44 C43 119.1(4) . . ? C49 C44 C43 119.6(3) . . ? C44 C45 C46 119.3(5) . . ? C47 C46 C45 120.6(5) . . ? C46 C47 C48 121.8(4) . . ? C47 C48 C53 124.4(4) . . ? C47 C48 C49 118.5(4) . . ? C53 C48 C49 117.1(4) . . ? C50 C49 C44 121.4(3) . . ? C50 C49 C48 120.1(4) . . ? C44 C49 C48 118.5(4) . . ? C51 C50 C49 120.6(4) . . ? C51 C50 C54 119.1(4) . . ? C49 C50 C54 120.4(3) . . ? C50 C51 C52 119.8(5) . . ? C53 C52 C51 120.4(5) . . ? C52 C53 C48 122.0(4) . . ? O12 C54 N3 121.1(3) . . ? O12 C54 C50 122.3(3) . . ? N3 C54 C50 116.6(3) . . ? O14 C55 O13 126.6(3) . . ? O14 C55 C56 118.6(3) . . ? O13 C55 C56 114.5(3) . . ? N4 C56 C55 109.1(3) . . ? N4 C56 C57 113.9(3) . . ? C55 C56 C57 118.6(3) . . ? C59 C57 C58 110.6(4) . . ? C59 C57 C60 108.7(4) . . ? C58 C57 C60 107.8(4) . . ? C59 C57 C56 114.7(4) . . ? C58 C57 C56 107.2(3) . . ? C60 C57 C56 107.5(4) . . ? O15 C61 N4 120.5(3) . . ? O15 C61 C62 122.9(4) . . ? N4 C61 C62 116.7(3) . . ? C63 C62 C67 120.5(4) . . ? C63 C62 C61 119.7(4) . . ? C67 C62 C61 119.8(3) . . ? C62 C63 C64 120.2(4) . . ? C65 C64 C63 120.0(4) . . ? C64 C65 C66 121.7(4) . . ? C65 C66 C67 118.7(4) . . ? C65 C66 C71 123.8(4) . . ? C67 C66 C71 117.4(4) . . ? C68 C67 C62 120.8(3) . . ? C68 C67 C66 120.2(4) . . ? C62 C67 C66 118.9(4) . . ? C69 C68 C67 120.2(4) . . ? C69 C68 C72 119.1(4) . . ? C67 C68 C72 120.7(3) . . ? C68 C69 C70 119.6(4) . . ? C71 C70 C69 121.7(4) . . ? C70 C71 C66 120.8(4) . . ? O16 C72 N4 120.3(3) . . ? O16 C72 C68 122.7(3) . . ? N4 C72 C68 117.0(3) . . ? O17 C73 O18 122.0(3) . . ? O17 C73 C74 126.1(3) . . ? O18 C73 C74 111.9(3) . . ? O18 C75 C76 107.8(3) . . ? O20 C81 O21 123.1(8) . . ? O20 C81 C82 124.3(9) . . ? O21 C81 C82 112.6(8) . . ? O21 C83 C84 108.6(7) . . ? C18 N1 C7 123.4(3) . . ? C18 N1 C2 119.3(3) . . ? C7 N1 C2 117.2(3) . . ? C25 N2 C36 124.4(3) . . ? C25 N2 C20 117.3(3) . . ? C36 N2 C20 118.2(3) . . ? C54 N3 C43 124.3(3) . . ? C54 N3 C38 117.1(3) . . ? C43 N3 C38 118.4(3) . . ? C61 N4 C72 124.1(3) . . ? C61 N4 C56 117.4(3) . . ? C72 N4 C56 118.1(3) . . ? C1 O1 Rh1 118.8(2) . . ? C1 O2 Rh2 118.2(2) . . ? C19 O5 Rh1 117.8(2) . . ? C19 O6 Rh2 119.4(2) . . ? C37 O9 Rh1 117.7(2) . . ? C37 O10 Rh2 118.8(2) . . ? C55 O13 Rh1 118.1(2) . . ? C55 O14 Rh2 118.9(2) . . ? C73 O17 Rh1 129.13(19) . . ? C73 O18 C75 117.4(2) . . ? C81 O21 C83 115.0(6) . . ? C77 O19 C80 109.5(11) . . ? C77 O19 Rh2 119.5(15) . . ? C80 O19 Rh2 121.2(10) . . ? O19 C77 C78 101.0(12) . . ? C77 C78 C79 86.5(12) . . ? C80 C79 C78 91.5(11) . . ? O19 C80 C79 98.2(14) . . ? C77' O19' C80' 109.7(12) . . ? C77' O19' Rh2 125.6(12) . . ? C80' O19' Rh2 115.1(15) . . ? O19' C77' C78' 102.9(15) . . ? C77' C78' C79' 94.3(12) . . ? C80' C79' C78' 87.3(12) . . ? O19' C80' C79' 98.7(12) . . ? 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 O13 Rh1 Rh2 O10 -89.63(9) . . . . ? O1 Rh1 Rh2 O10 -178.85(10) . . . . ? O5 Rh1 Rh2 O10 90.04(9) . . . . ? O9 Rh1 Rh2 O10 -0.32(9) . . . . ? O17 Rh1 Rh2 O10 148.8(11) . . . . ? O13 Rh1 Rh2 O2 90.28(10) . . . . ? O1 Rh1 Rh2 O2 1.06(9) . . . . ? O5 Rh1 Rh2 O2 -90.05(10) . . . . ? O9 Rh1 Rh2 O2 179.59(10) . . . . ? O17 Rh1 Rh2 O2 -31.3(11) . . . . ? O13 Rh1 Rh2 O14 0.28(9) . . . . ? O1 Rh1 Rh2 O14 -88.94(10) . . . . ? O5 Rh1 Rh2 O14 179.95(10) . . . . ? O9 Rh1 Rh2 O14 89.59(10) . . . . ? O17 Rh1 Rh2 O14 -121.3(11) . . . . ? O13 Rh1 Rh2 O6 -179.02(9) . . . . ? O1 Rh1 Rh2 O6 91.76(9) . . . . ? O5 Rh1 Rh2 O6 0.65(9) . . . . ? O9 Rh1 Rh2 O6 -89.71(9) . . . . ? O17 Rh1 Rh2 O6 59.4(11) . . . . ? O13 Rh1 Rh2 O19' -98(29) . . . . ? O1 Rh1 Rh2 O19' 172(29) . . . . ? O5 Rh1 Rh2 O19' 81(29) . . . . ? O9 Rh1 Rh2 O19' -9(29) . . . . ? O17 Rh1 Rh2 O19' 140(29) . . . . ? O13 Rh1 Rh2 O19 142(85) . . . . ? O1 Rh1 Rh2 O19 53(84) . . . . ? O5 Rh1 Rh2 O19 -38(84) . . . . ? O9 Rh1 Rh2 O19 -129(84) . . . . ? O17 Rh1 Rh2 O19 21(84) . . . . ? O2 C1 C2 N1 -132.9(3) . . . . ? O1 C1 C2 N1 49.6(4) . . . . ? O2 C1 C2 C3 -0.4(5) . . . . ? O1 C1 C2 C3 -178.0(3) . . . . ? N1 C2 C3 C4 67.5(4) . . . . ? C1 C2 C3 C4 -62.8(5) . . . . ? N1 C2 C3 C6 -168.9(3) . . . . ? C1 C2 C3 C6 60.8(5) . . . . ? N1 C2 C3 C5 -53.0(5) . . . . ? C1 C2 C3 C5 176.7(4) . . . . ? O3 C7 C8 C13 172.6(4) . . . . ? N1 C7 C8 C13 -10.0(5) . . . . ? O3 C7 C8 C9 -9.9(5) . . . . ? N1 C7 C8 C9 167.5(3) . . . . ? C13 C8 C9 C10 2.2(6) . . . . ? C7 C8 C9 C10 -175.2(3) . . . . ? C8 C9 C10 C11 -4.8(6) . . . . ? C9 C10 C11 C12 1.5(7) . . . . ? C10 C11 C12 C17 -179.2(4) . . . . ? C10 C11 C12 C13 4.0(6) . . . . ? C9 C8 C13 C14 -176.4(3) . . . . ? C7 C8 C13 C14 1.0(6) . . . . ? C9 C8 C13 C12 3.3(6) . . . . ? C7 C8 C13 C12 -179.2(3) . . . . ? C17 C12 C13 C8 176.7(4) . . . . ? C11 C12 C13 C8 -6.3(5) . . . . ? C17 C12 C13 C14 -3.6(5) . . . . ? C11 C12 C13 C14 173.4(3) . . . . ? C8 C13 C14 C15 -178.1(4) . . . . ? C12 C13 C14 C15 2.2(6) . . . . ? C8 C13 C14 C18 5.2(6) . . . . ? C12 C13 C14 C18 -174.5(3) . . . . ? C13 C14 C15 C16 0.4(6) . . . . ? C18 C14 C15 C16 177.1(4) . . . . ? C14 C15 C16 C17 -1.6(7) . . . . ? C15 C16 C17 C12 0.0(7) . . . . ? C11 C12 C17 C16 -174.2(4) . . . . ? C13 C12 C17 C16 2.5(6) . . . . ? C15 C14 C18 O4 0.7(6) . . . . ? C13 C14 C18 O4 177.4(3) . . . . ? C15 C14 C18 N1 -179.1(4) . . . . ? C13 C14 C18 N1 -2.4(5) . . . . ? O6 C19 C20 N2 -137.7(3) . . . . ? O5 C19 C20 N2 46.4(4) . . . . ? O6 C19 C20 C21 -6.1(4) . . . . ? O5 C19 C20 C21 178.1(3) . . . . ? N2 C20 C21 C22 71.0(4) . . . . ? C19 C20 C21 C22 -58.2(4) . . . . ? N2 C20 C21 C24 -166.8(3) . . . . ? C19 C20 C21 C24 64.1(4) . . . . ? N2 C20 C21 C23 -49.8(4) . . . . ? C19 C20 C21 C23 -178.9(3) . . . . ? O7 C25 C26 C27 -2.5(5) . . . . ? N2 C25 C26 C27 178.6(3) . . . . ? O7 C25 C26 C31 172.5(4) . . . . ? N2 C25 C26 C31 -6.3(5) . . . . ? C31 C26 C27 C28 -1.0(5) . . . . ? C25 C26 C27 C28 174.0(3) . . . . ? C26 C27 C28 C29 0.1(6) . . . . ? C27 C28 C29 C30 0.7(6) . . . . ? C28 C29 C30 C35 -178.8(4) . . . . ? C28 C29 C30 C31 -0.5(6) . . . . ? C27 C26 C31 C32 178.9(3) . . . . ? C25 C26 C31 C32 4.0(5) . . . . ? C27 C26 C31 C30 1.2(5) . . . . ? C25 C26 C31 C30 -173.8(3) . . . . ? C35 C30 C31 C26 178.0(4) . . . . ? C29 C30 C31 C26 -0.4(5) . . . . ? C35 C30 C31 C32 0.1(5) . . . . ? C29 C30 C31 C32 -178.2(4) . . . . ? C26 C31 C32 C33 -177.5(4) . . . . ? C30 C31 C32 C33 0.3(6) . . . . ? C26 C31 C32 C36 2.6(5) . . . . ? C30 C31 C32 C36 -179.6(3) . . . . ? C31 C32 C33 C34 -0.1(6) . . . . ? C36 C32 C33 C34 179.8(4) . . . . ? C32 C33 C34 C35 -0.6(8) . . . . ? C33 C34 C35 C30 1.1(8) . . . . ? C31 C30 C35 C34 -0.9(7) . . . . ? C29 C30 C35 C34 177.4(5) . . . . ? C33 C32 C36 O8 -4.9(6) . . . . ? C31 C32 C36 O8 175.0(3) . . . . ? C33 C32 C36 N2 173.4(3) . . . . ? C31 C32 C36 N2 -6.7(5) . . . . ? O10 C37 C38 N3 -134.0(3) . . . . ? O9 C37 C38 N3 50.0(4) . . . . ? O10 C37 C38 C39 -3.5(4) . . . . ? O9 C37 C38 C39 -179.5(3) . . . . ? N3 C38 C39 C42 69.4(4) . . . . ? C37 C38 C39 C42 -59.8(4) . . . . ? N3 C38 C39 C40 -166.9(3) . . . . ? C37 C38 C39 C40 63.9(4) . . . . ? N3 C38 C39 C41 -51.6(4) . . . . ? C37 C38 C39 C41 179.2(3) . . . . ? O11 C43 C44 C45 -0.2(5) . . . . ? N3 C43 C44 C45 -179.7(3) . . . . ? O11 C43 C44 C49 179.5(3) . . . . ? N3 C43 C44 C49 -0.1(5) . . . . ? C49 C44 C45 C46 -2.4(6) . . . . ? C43 C44 C45 C46 177.2(4) . . . . ? C44 C45 C46 C47 0.1(7) . . . . ? C45 C46 C47 C48 1.8(8) . . . . ? C46 C47 C48 C53 178.0(4) . . . . ? C46 C47 C48 C49 -1.3(7) . . . . ? C45 C44 C49 C50 -176.0(4) . . . . ? C43 C44 C49 C50 4.4(5) . . . . ? C45 C44 C49 C48 2.8(5) . . . . ? C43 C44 C49 C48 -176.8(3) . . . . ? C47 C48 C49 C50 177.8(4) . . . . ? C53 C48 C49 C50 -1.5(5) . . . . ? C47 C48 C49 C44 -1.0(5) . . . . ? C53 C48 C49 C44 179.6(3) . . . . ? C44 C49 C50 C51 179.5(3) . . . . ? C48 C49 C50 C51 0.7(6) . . . . ? C44 C49 C50 C54 -1.0(5) . . . . ? C48 C49 C50 C54 -179.8(3) . . . . ? C49 C50 C51 C52 1.1(6) . . . . ? C54 C50 C51 C52 -178.4(4) . . . . ? C50 C51 C52 C53 -2.0(7) . . . . ? C51 C52 C53 C48 1.1(8) . . . . ? C47 C48 C53 C52 -178.7(5) . . . . ? C49 C48 C53 C52 0.6(6) . . . . ? C51 C50 C54 O12 -6.1(6) . . . . ? C49 C50 C54 O12 174.4(4) . . . . ? C51 C50 C54 N3 172.9(3) . . . . ? C49 C50 C54 N3 -6.6(5) . . . . ? O14 C55 C56 N4 -137.9(3) . . . . ? O13 C55 C56 N4 47.6(4) . . . . ? O14 C55 C56 C57 -5.4(5) . . . . ? O13 C55 C56 C57 -179.8(3) . . . . ? N4 C56 C57 C59 70.9(5) . . . . ? C55 C56 C57 C59 -59.5(5) . . . . ? N4 C56 C57 C58 -165.8(4) . . . . ? C55 C56 C57 C58 63.8(5) . . . . ? N4 C56 C57 C60 -50.2(5) . . . . ? C55 C56 C57 C60 179.5(4) . . . . ? O15 C61 C62 C63 6.4(6) . . . . ? N4 C61 C62 C63 -173.7(3) . . . . ? O15 C61 C62 C67 -171.5(4) . . . . ? N4 C61 C62 C67 8.3(5) . . . . ? C67 C62 C63 C64 0.7(6) . . . . ? C61 C62 C63 C64 -177.2(4) . . . . ? C62 C63 C64 C65 1.1(7) . . . . ? C63 C64 C65 C66 -0.9(7) . . . . ? C64 C65 C66 C67 -1.1(6) . . . . ? C64 C65 C66 C71 177.2(4) . . . . ? C63 C62 C67 C68 -178.9(4) . . . . ? C61 C62 C67 C68 -1.0(5) . . . . ? C63 C62 C67 C66 -2.6(5) . . . . ? C61 C62 C67 C66 175.3(3) . . . . ? C65 C66 C67 C68 179.1(3) . . . . ? C71 C66 C67 C68 0.8(5) . . . . ? C65 C66 C67 C62 2.8(5) . . . . ? C71 C66 C67 C62 -175.6(3) . . . . ? C62 C67 C68 C69 176.3(3) . . . . ? C66 C67 C68 C69 0.0(5) . . . . ? C62 C67 C68 C72 -2.8(5) . . . . ? C66 C67 C68 C72 -179.1(3) . . . . ? C67 C68 C69 C70 -0.3(5) . . . . ? C72 C68 C69 C70 178.8(3) . . . . ? C68 C69 C70 C71 -0.3(6) . . . . ? C69 C70 C71 C66 1.1(6) . . . . ? C65 C66 C71 C70 -179.6(4) . . . . ? C67 C66 C71 C70 -1.3(6) . . . . ? C69 C68 C72 O16 1.3(5) . . . . ? C67 C68 C72 O16 -179.6(3) . . . . ? C69 C68 C72 N4 -179.9(3) . . . . ? C67 C68 C72 N4 -0.8(5) . . . . ? O4 C18 N1 C7 173.0(3) . . . . ? C14 C18 N1 C7 -7.2(5) . . . . ? O4 C18 N1 C2 -2.2(5) . . . . ? C14 C18 N1 C2 177.5(3) . . . . ? O3 C7 N1 C18 -169.4(3) . . . . ? C8 C7 N1 C18 13.1(5) . . . . ? O3 C7 N1 C2 6.0(5) . . . . ? C8 C7 N1 C2 -171.5(3) . . . . ? C1 C2 N1 C18 45.7(4) . . . . ? C3 C2 N1 C18 -88.3(4) . . . . ? C1 C2 N1 C7 -129.9(3) . . . . ? C3 C2 N1 C7 96.1(4) . . . . ? O7 C25 N2 C36 -176.8(3) . . . . ? C26 C25 N2 C36 2.0(5) . . . . ? O7 C25 N2 C20 -1.7(5) . . . . ? C26 C25 N2 C20 177.2(3) . . . . ? O8 C36 N2 C25 -177.4(3) . . . . ? C32 C36 N2 C25 4.3(5) . . . . ? O8 C36 N2 C20 7.5(5) . . . . ? C32 C36 N2 C20 -170.8(3) . . . . ? C19 C20 N2 C25 -133.4(3) . . . . ? C21 C20 N2 C25 93.6(4) . . . . ? C19 C20 N2 C36 42.1(4) . . . . ? C21 C20 N2 C36 -90.9(4) . . . . ? O12 C54 N3 C43 -169.6(3) . . . . ? C50 C54 N3 C43 11.4(5) . . . . ? O12 C54 N3 C38 6.4(5) . . . . ? C50 C54 N3 C38 -172.7(3) . . . . ? O11 C43 N3 C54 172.3(3) . . . . ? C44 C43 N3 C54 -8.1(5) . . . . ? O11 C43 N3 C38 -3.6(5) . . . . ? C44 C43 N3 C38 176.0(3) . . . . ? C37 C38 N3 C54 -130.3(3) . . . . ? C39 C38 N3 C54 97.2(4) . . . . ? C37 C38 N3 C43 45.9(4) . . . . ? C39 C38 N3 C43 -86.6(4) . . . . ? O15 C61 N4 C72 167.2(3) . . . . ? C62 C61 N4 C72 -12.6(5) . . . . ? O15 C61 N4 C56 -4.7(5) . . . . ? C62 C61 N4 C56 175.5(3) . . . . ? O16 C72 N4 C61 -172.2(3) . . . . ? C68 C72 N4 C61 8.9(5) . . . . ? O16 C72 N4 C56 -0.3(5) . . . . ? C68 C72 N4 C56 -179.2(3) . . . . ? C55 C56 N4 C61 51.1(4) . . . . ? C57 C56 N4 C61 -83.9(4) . . . . ? C55 C56 N4 C72 -121.3(3) . . . . ? C57 C56 N4 C72 103.7(4) . . . . ? O2 C1 O1 Rh1 2.8(5) . . . . ? C2 C1 O1 Rh1 -179.9(2) . . . . ? O13 Rh1 O1 C1 -90.3(2) . . . . ? O5 Rh1 O1 C1 86.1(2) . . . . ? O9 Rh1 O1 C1 -17.7(11) . . . . ? Rh2 Rh1 O1 C1 -2.2(2) . . . . ? O17 Rh1 O1 C1 176.3(2) . . . . ? O1 C1 O2 Rh2 -1.5(5) . . . . ? C2 C1 O2 Rh2 -178.8(2) . . . . ? O10 Rh2 O2 C1 3(3) . . . . ? O14 Rh2 O2 C1 88.1(3) . . . . ? O6 Rh2 O2 C1 -88.2(3) . . . . ? O19' Rh2 O2 C1 -180.0(9) . . . . ? O19 Rh2 O2 C1 -180.0(9) . . . . ? Rh1 Rh2 O2 C1 -0.3(2) . . . . ? O6 C19 O5 Rh1 6.5(4) . . . . ? C20 C19 O5 Rh1 -178.1(2) . . . . ? O13 Rh1 O5 C19 1.7(15) . . . . ? O1 Rh1 O5 C19 -90.8(2) . . . . ? O9 Rh1 O5 C19 83.9(2) . . . . ? Rh2 Rh1 O5 C19 -3.5(2) . . . . ? O17 Rh1 O5 C19 178.9(2) . . . . ? O5 C19 O6 Rh2 -5.8(4) . . . . ? C20 C19 O6 Rh2 178.9(2) . . . . ? O10 Rh2 O6 C19 -87.0(2) . . . . ? O2 Rh2 O6 C19 91.1(2) . . . . ? O14 Rh2 O6 C19 -8.9(16) . . . . ? O19' Rh2 O6 C19 -176.0(7) . . . . ? O19 Rh2 O6 C19 -178.2(7) . . . . ? Rh1 Rh2 O6 C19 2.1(2) . . . . ? O10 C37 O9 Rh1 3.8(4) . . . . ? C38 C37 O9 Rh1 179.4(2) . . . . ? O13 Rh1 O9 C37 86.7(2) . . . . ? O1 Rh1 O9 C37 14.1(11) . . . . ? O5 Rh1 O9 C37 -89.8(2) . . . . ? Rh2 Rh1 O9 C37 -1.4(2) . . . . ? O17 Rh1 O9 C37 -180.0(2) . . . . ? O9 C37 O10 Rh2 -4.2(4) . . . . ? C38 C37 O10 Rh2 -179.7(2) . . . . ? O2 Rh2 O10 C37 -1(3) . . . . ? O14 Rh2 O10 C37 -86.2(2) . . . . ? O6 Rh2 O10 C37 90.2(2) . . . . ? O19' Rh2 O10 C37 -178.1(9) . . . . ? O19 Rh2 O10 C37 -178.1(8) . . . . ? Rh1 Rh2 O10 C37 2.2(2) . . . . ? O14 C55 O13 Rh1 1.8(5) . . . . ? C56 C55 O13 Rh1 175.8(2) . . . . ? O1 Rh1 O13 C55 86.2(2) . . . . ? O5 Rh1 O13 C55 -6.3(16) . . . . ? O9 Rh1 O13 C55 -88.5(2) . . . . ? Rh2 Rh1 O13 C55 -1.1(2) . . . . ? O17 Rh1 O13 C55 176.6(2) . . . . ? O13 C55 O14 Rh2 -1.5(5) . . . . ? C56 C55 O14 Rh2 -175.2(2) . . . . ? O10 Rh2 O14 C55 89.5(2) . . . . ? O2 Rh2 O14 C55 -88.6(3) . . . . ? O6 Rh2 O14 C55 11.4(16) . . . . ? O19' Rh2 O14 C55 178.5(7) . . . . ? O19 Rh2 O14 C55 -179.4(7) . . . . ? Rh1 Rh2 O14 C55 0.4(2) . . . . ? O18 C73 O17 Rh1 173.3(2) . . . . ? C74 C73 O17 Rh1 -5.7(5) . . . . ? O13 Rh1 O17 C73 -113.5(3) . . . . ? O1 Rh1 O17 C73 -24.3(3) . . . . ? O5 Rh1 O17 C73 66.7(3) . . . . ? O9 Rh1 O17 C73 157.0(3) . . . . ? Rh2 Rh1 O17 C73 8.0(13) . . . . ? O17 C73 O18 C75 -2.2(5) . . . . ? C74 C73 O18 C75 177.0(3) . . . . ? C76 C75 O18 C73 -171.3(4) . . . . ? O20 C81 O21 C83 3.7(10) . . . . ? C82 C81 O21 C83 -178.0(7) . . . . ? C84 C83 O21 C81 -165.5(7) . . . . ? O10 Rh2 O19 C77 180(2) . . . . ? O2 Rh2 O19 C77 0(2) . . . . ? O14 Rh2 O19 C77 90(2) . . . . ? O6 Rh2 O19 C77 -91(2) . . . . ? O19' Rh2 O19 C77 -180(100) . . . . ? Rh1 Rh2 O19 C77 -52(84) . . . . ? O10 Rh2 O19 C80 -38(2) . . . . ? O2 Rh2 O19 C80 142(2) . . . . ? O14 Rh2 O19 C80 -128(2) . . . . ? O6 Rh2 O19 C80 52(2) . . . . ? O19' Rh2 O19 C80 -37(45) . . . . ? Rh1 Rh2 O19 C80 90(84) . . . . ? C80 O19 C77 C78 33(3) . . . . ? Rh2 O19 C77 C78 179.6(17) . . . . ? O19 C77 C78 C79 -63(2) . . . . ? C77 C78 C79 C80 64.0(14) . . . . ? C77 O19 C80 C79 11(3) . . . . ? Rh2 O19 C80 C79 -134.5(19) . . . . ? C78 C79 C80 O19 -49.8(19) . . . . ? O10 Rh2 O19' C77' 150(3) . . . . ? O2 Rh2 O19' C77' -30(3) . . . . ? O14 Rh2 O19' C77' 60(3) . . . . ? O6 Rh2 O19' C77' -120(3) . . . . ? O19 Rh2 O19' C77' -29(45) . . . . ? Rh1 Rh2 O19' C77' 159(26) . . . . ? O10 Rh2 O19' C80' -67(2) . . . . ? O2 Rh2 O19' C80' 113(2) . . . . ? O14 Rh2 O19' C80' -157(2) . . . . ? O6 Rh2 O19' C80' 22(2) . . . . ? O19 Rh2 O19' C80' 113(49) . . . . ? Rh1 Rh2 O19' C80' -58(31) . . . . ? C80' O19' C77' C78' -5(3) . . . . ? Rh2 O19' C77' C78' 139(2) . . . . ? O19' C77' C78' C79' 45(2) . . . . ? C77' C78' C79' C80' -60.1(17) . . . . ? C77' O19' C80' C79' -36(3) . . . . ? Rh2 O19' C80' C79' 175.2(18) . . . . ? C78' C79' C80' O19' 60(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.048 _refine_diff_density_min -0.400 _refine_diff_density_rms 0.075 # Attachment 'joef097as.cif' data_joef097as _database_code_depnum_ccdc_archive 'CCDC 761721' #TrackingRef 'joef097as.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H71 Cu2 N7 O17' _chemical_formula_weight 1337.36 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 25.068(4) _cell_length_b 26.409(4) _cell_length_c 10.1657(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6730.0(17) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 998 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 26.82 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.320 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2792 _exptl_absorpt_coefficient_mu 0.703 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8472 _exptl_absorpt_correction_T_max 0.9129 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 85763 _diffrn_reflns_av_R_equivalents 0.0523 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 28.28 _reflns_number_total 16721 _reflns_number_gt 14450 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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^)+(0.0572P)^2^+0.2160P] 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: 7550 Friedel pairs' _refine_ls_abs_structure_Flack -0.010(8) _refine_ls_number_reflns 16721 _refine_ls_number_parameters 782 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0550 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1143 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.011 _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 Cu1 Cu 0.319529(13) 0.328683(12) 0.78133(3) 0.03283(8) Uani 1 1 d . A . Cu2 Cu 0.340309(13) 0.342379(12) 1.03365(3) 0.03128(8) Uani 1 1 d . . . N1 N 0.40363(10) 0.17454(9) 0.8011(3) 0.0429(6) Uani 1 1 d . . . N2 N 0.16416(11) 0.25647(10) 0.9175(3) 0.0466(6) Uani 1 1 d . . . N3 N 0.24308(9) 0.48324(8) 0.7685(2) 0.0357(5) Uani 1 1 d . . . N4 N 0.47955(9) 0.40403(9) 0.7041(2) 0.0386(5) Uani 1 1 d . . . O1 O 0.34060(9) 0.25780(7) 0.80010(19) 0.0399(4) Uani 1 1 d . . . O2 O 0.35764(9) 0.26921(7) 1.0144(2) 0.0402(5) Uani 1 1 d . . . O3 O 0.35381(11) 0.10603(9) 0.7336(3) 0.0680(7) Uani 1 1 d . . . O4 O 0.46207(9) 0.24292(8) 0.8002(3) 0.0540(6) Uani 1 1 d . . . O5 O 0.24883(8) 0.31238(8) 0.8510(2) 0.0424(5) Uani 1 1 d . . . O6 O 0.26539(8) 0.32594(8) 1.06546(19) 0.0410(5) Uani 1 1 d . . . O7 O 0.09562(10) 0.28997(12) 0.7942(3) 0.0765(9) Uani 1 1 d . . . O8 O 0.23760(11) 0.20765(8) 0.9775(3) 0.0570(6) Uani 1 1 d . . . O9 O 0.30099(8) 0.40018(7) 0.7843(2) 0.0388(4) Uani 1 1 d . . . O10 O 0.31815(9) 0.41290(7) 0.99873(18) 0.0389(4) Uani 1 1 d . . . O11 O 0.28401(10) 0.53524(9) 0.6155(2) 0.0563(6) Uani 1 1 d . . . O12 O 0.18652(10) 0.42395(9) 0.8610(2) 0.0541(6) Uani 1 1 d . . . O13 O 0.39469(8) 0.34715(8) 0.76232(19) 0.0392(4) Uani 1 1 d . . . O14 O 0.41329(8) 0.35812(7) 0.9762(2) 0.0380(4) Uani 1 1 d . . . O15 O 0.51646(10) 0.35203(10) 0.5458(3) 0.0604(6) Uani 1 1 d . . . O16 O 0.42331(9) 0.46354(8) 0.8008(2) 0.0466(5) Uani 1 1 d . . . C1 C 0.35622(11) 0.24337(11) 0.9115(3) 0.0360(6) Uani 1 1 d . . . C2 C 0.37225(13) 0.18692(11) 0.9196(3) 0.0386(6) Uani 1 1 d . . . H2A H 0.3383 0.1673 0.9116 0.046 Uiso 1 1 calc R . . C3 C 0.44502(12) 0.20466(12) 0.7508(3) 0.0437(7) Uani 1 1 d . . . C4 C 0.46269(14) 0.17889(13) 0.6277(3) 0.0498(8) Uani 1 1 d . . . C5 C 0.50303(15) 0.19054(15) 0.5419(4) 0.0621(10) Uani 1 1 d . . . H5A H 0.5249 0.2194 0.5559 0.074 Uiso 1 1 calc R . . C6 C 0.51106(17) 0.15954(19) 0.4354(4) 0.0703(12) Uani 1 1 d . . . H6A H 0.5387 0.1669 0.3744 0.084 Uiso 1 1 calc R . . C7 C 0.4789(2) 0.1175(2) 0.4169(4) 0.0811(15) Uani 1 1 d . . . H7A H 0.4854 0.0961 0.3433 0.097 Uiso 1 1 calc R . . C8 C 0.4378(2) 0.10549(17) 0.5019(4) 0.0710(11) Uani 1 1 d . . . H8A H 0.4155 0.0769 0.4872 0.085 Uiso 1 1 calc R . . C9 C 0.43054(16) 0.13679(13) 0.6090(3) 0.0524(8) Uani 1 1 d . . . C10 C 0.39046(15) 0.13498(12) 0.7175(4) 0.0508(8) Uani 1 1 d . . . C11 C 0.39901(14) 0.16833(12) 1.0483(3) 0.0495(7) Uani 1 1 d . . . C12 C 0.44979(16) 0.19676(16) 1.0826(4) 0.0643(10) Uani 1 1 d . . . H12A H 0.4418 0.2329 1.0918 0.096 Uiso 1 1 calc R . . H12B H 0.4761 0.1919 1.0125 0.096 Uiso 1 1 calc R . . H12C H 0.4642 0.1838 1.1657 0.096 Uiso 1 1 calc R . . C13 C 0.4114(2) 0.11067(14) 1.0297(5) 0.0795(13) Uani 1 1 d . . . H13A H 0.4246 0.0965 1.1126 0.119 Uiso 1 1 calc R . . H13B H 0.4385 0.1065 0.9612 0.119 Uiso 1 1 calc R . . H13C H 0.3787 0.0929 1.0036 0.119 Uiso 1 1 calc R . . C14 C 0.35813(16) 0.17297(14) 1.1607(3) 0.0599(9) Uani 1 1 d . . . H14A H 0.3486 0.2087 1.1731 0.090 Uiso 1 1 calc R . . H14B H 0.3737 0.1597 1.2421 0.090 Uiso 1 1 calc R . . H14C H 0.3261 0.1536 1.1385 0.090 Uiso 1 1 calc R . . C15 C 0.23582(12) 0.31417(10) 0.9708(3) 0.0393(6) Uani 1 1 d . . . C16 C 0.17672(13) 0.30225(13) 0.9940(3) 0.0477(7) Uani 1 1 d . . . H16A H 0.1568 0.3302 0.9493 0.057 Uiso 1 1 calc R . . C17 C 0.12751(13) 0.25703(15) 0.8140(4) 0.0537(8) Uani 1 1 d . . . C18 C 0.13771(13) 0.20984(13) 0.7375(4) 0.0511(8) Uani 1 1 d . . . C19 C 0.11198(16) 0.19048(17) 0.6282(4) 0.0654(10) Uani 1 1 d . . . H19A H 0.0811 0.2064 0.5929 0.078 Uiso 1 1 calc R . . C20 C 0.13285(19) 0.14718(18) 0.5725(4) 0.0754(13) Uani 1 1 d . . . H20A H 0.1164 0.1334 0.4963 0.090 Uiso 1 1 calc R . . C21 C 0.17726(19) 0.12339(16) 0.6250(4) 0.0696(11) Uani 1 1 d . . . H21A H 0.1904 0.0933 0.5851 0.084 Uiso 1 1 calc R . . C22 C 0.20285(17) 0.14285(13) 0.7351(4) 0.0585(9) Uani 1 1 d . . . H22A H 0.2336 0.1269 0.7710 0.070 Uiso 1 1 calc R . . C23 C 0.18170(14) 0.18647(12) 0.7906(3) 0.0469(7) Uani 1 1 d . . . C24 C 0.19994(14) 0.21555(12) 0.9062(3) 0.0462(7) Uani 1 1 d . . . C25 C 0.15535(16) 0.30169(18) 1.1367(4) 0.0676(11) Uani 1 1 d . . . C26 C 0.16359(17) 0.35441(18) 1.1980(4) 0.0791(13) Uani 1 1 d . . . H26A H 0.2016 0.3597 1.2159 0.119 Uiso 1 1 calc R . . H26B H 0.1435 0.3567 1.2805 0.119 Uiso 1 1 calc R . . H26C H 0.1509 0.3804 1.1368 0.119 Uiso 1 1 calc R . . C27 C 0.1811(2) 0.26152(19) 1.2204(4) 0.0913(16) Uani 1 1 d . . . H27A H 0.2199 0.2646 1.2145 0.137 Uiso 1 1 calc R . . H27B H 0.1701 0.2280 1.1891 0.137 Uiso 1 1 calc R . . H27C H 0.1699 0.2658 1.3121 0.137 Uiso 1 1 calc R . . C28 C 0.09430(19) 0.2927(3) 1.1273(6) 0.117(3) Uani 1 1 d . . . H28A H 0.0875 0.2597 1.0867 0.176 Uiso 1 1 calc R . . H28B H 0.0781 0.3194 1.0737 0.176 Uiso 1 1 calc R . . H28C H 0.0788 0.2934 1.2158 0.176 Uiso 1 1 calc R . . C29 C 0.30289(11) 0.42671(11) 0.8864(3) 0.0365(6) Uani 1 1 d . . . C30 C 0.28648(11) 0.48245(10) 0.8656(3) 0.0367(6) Uani 1 1 d . . . H30A H 0.3175 0.4980 0.8187 0.044 Uiso 1 1 calc R . . C31 C 0.24786(13) 0.50808(11) 0.6473(3) 0.0429(7) Uani 1 1 d . . . C32 C 0.19904(14) 0.49404(12) 0.5703(3) 0.0465(7) Uani 1 1 d . . . C33 C 0.18235(17) 0.50831(14) 0.4475(3) 0.0599(9) Uani 1 1 d . . . H33A H 0.2022 0.5320 0.3970 0.072 Uiso 1 1 calc R . . C34 C 0.1362(2) 0.48744(17) 0.3995(4) 0.0732(12) Uani 1 1 d . . . H34A H 0.1239 0.4969 0.3147 0.088 Uiso 1 1 calc R . . C35 C 0.10765(19) 0.45328(18) 0.4717(5) 0.0793(13) Uani 1 1 d . . . H35A H 0.0759 0.4393 0.4355 0.095 Uiso 1 1 calc R . . C36 C 0.12369(17) 0.43834(16) 0.5966(4) 0.0674(11) Uani 1 1 d . . . H36A H 0.1037 0.4147 0.6467 0.081 Uiso 1 1 calc R . . C37 C 0.17011(13) 0.45954(12) 0.6444(3) 0.0459(7) Uani 1 1 d . . . C38 C 0.19839(12) 0.45145(12) 0.7722(3) 0.0444(7) Uani 1 1 d . . . C39 C 0.27714(15) 0.51704(12) 0.9847(3) 0.0502(8) Uani 1 1 d . . . C40 C 0.23258(18) 0.49806(19) 1.0746(4) 0.0730(12) Uani 1 1 d . . . H40A H 0.2406 0.4635 1.1032 0.110 Uiso 1 1 calc R . . H40B H 0.1987 0.4983 1.0266 0.110 Uiso 1 1 calc R . . H40C H 0.2298 0.5202 1.1517 0.110 Uiso 1 1 calc R . . C41 C 0.26345(19) 0.57010(14) 0.9322(4) 0.0710(12) Uani 1 1 d . . . H41A H 0.2911 0.5810 0.8702 0.106 Uiso 1 1 calc R . . H41B H 0.2617 0.5940 1.0058 0.106 Uiso 1 1 calc R . . H41C H 0.2289 0.5691 0.8874 0.106 Uiso 1 1 calc R . . C42 C 0.32932(16) 0.52149(14) 1.0631(4) 0.0646(11) Uani 1 1 d . . . H42A H 0.3587 0.5294 1.0030 0.097 Uiso 1 1 calc R . . H42B H 0.3366 0.4894 1.1079 0.097 Uiso 1 1 calc R . . H42C H 0.3259 0.5486 1.1285 0.097 Uiso 1 1 calc R . . C43 C 0.42519(12) 0.35725(10) 0.8568(3) 0.0354(6) Uani 1 1 d . . . C44 C 0.48324(11) 0.36741(11) 0.8136(3) 0.0358(6) Uani 1 1 d . . . H44A H 0.4954 0.3351 0.7720 0.043 Uiso 1 1 calc R . . C45 C 0.49148(13) 0.38942(13) 0.5748(3) 0.0464(7) Uani 1 1 d . . . C46 C 0.46618(13) 0.42734(14) 0.4876(3) 0.0500(8) Uani 1 1 d . . . C47 C 0.46542(18) 0.43077(19) 0.3517(4) 0.0715(12) Uani 1 1 d . . . H47A H 0.4850 0.4078 0.2984 0.086 Uiso 1 1 calc R . . C48 C 0.4351(2) 0.4689(2) 0.2965(4) 0.0862(15) Uani 1 1 d . . . H48A H 0.4336 0.4720 0.2035 0.103 Uiso 1 1 calc R . . C49 C 0.40719(19) 0.50237(19) 0.3730(4) 0.0778(13) Uani 1 1 d . . . H49A H 0.3870 0.5283 0.3317 0.093 Uiso 1 1 calc R . . C50 C 0.40771(16) 0.49941(14) 0.5096(4) 0.0572(9) Uani 1 1 d . . . H50A H 0.3884 0.5227 0.5626 0.069 Uiso 1 1 calc R . . C51 C 0.43763(13) 0.46114(12) 0.5641(3) 0.0443(7) Uani 1 1 d . . . C52 C 0.44409(12) 0.44586(11) 0.7047(3) 0.0394(6) Uani 1 1 d . . . C53 C 0.52608(12) 0.37973(11) 0.9176(3) 0.0409(7) Uani 1 1 d . . . C54 C 0.52782(14) 0.33677(13) 1.0179(4) 0.0536(8) Uani 1 1 d . . . H54A H 0.5592 0.3408 1.0744 0.080 Uiso 1 1 calc R . . H54B H 0.5300 0.3043 0.9717 0.080 Uiso 1 1 calc R . . H54C H 0.4954 0.3376 1.0718 0.080 Uiso 1 1 calc R . . C55 C 0.57979(13) 0.38206(16) 0.8450(4) 0.0610(10) Uani 1 1 d . . . H55A H 0.6085 0.3882 0.9085 0.092 Uiso 1 1 calc R . . H55B H 0.5790 0.4096 0.7805 0.092 Uiso 1 1 calc R . . H55C H 0.5861 0.3499 0.7997 0.092 Uiso 1 1 calc R . . C56 C 0.51657(14) 0.42957(12) 0.9877(3) 0.0475(7) Uani 1 1 d . . . H56A H 0.5433 0.4339 1.0571 0.071 Uiso 1 1 calc R . . H56B H 0.4808 0.4295 1.0268 0.071 Uiso 1 1 calc R . . H56C H 0.5194 0.4575 0.9245 0.071 Uiso 1 1 calc R . . N5 N 0.36505(13) 0.33597(13) 1.2412(3) 0.0608(8) Uani 1 1 d . . . C57 C 0.38587(17) 0.31542(16) 1.3242(4) 0.0602(10) Uani 1 1 d . . . C58 C 0.4123(2) 0.2879(2) 1.4313(5) 0.0983(17) Uani 1 1 d . . . H58A H 0.3932 0.2562 1.4485 0.147 Uiso 1 1 calc R . . H58B H 0.4123 0.3088 1.5109 0.147 Uiso 1 1 calc R . . H58C H 0.4492 0.2803 1.4060 0.147 Uiso 1 1 calc R . . O17 O 0.30042(11) 0.31934(11) 0.5743(2) 0.0605(7) Uani 1 1 d D . . H17 H 0.2875(17) 0.2879(16) 0.561(4) 0.073 Uiso 1 1 d . . . C59 C 0.2541(7) 0.3445(11) 0.518(2) 0.084(6) Uani 0.582(7) 1 d PD A 1 H59A H 0.2272 0.3532 0.5858 0.101 Uiso 0.582(7) 1 calc PR A 1 H59B H 0.2373 0.3243 0.4475 0.101 Uiso 0.582(7) 1 calc PR A 1 C60 C 0.2889(5) 0.4022(3) 0.4522(8) 0.110(3) Uani 0.582(7) 1 d PD A 1 H60A H 0.2624 0.4263 0.4191 0.165 Uiso 0.582(7) 1 calc PR A 1 H60B H 0.3128 0.3923 0.3804 0.165 Uiso 0.582(7) 1 calc PR A 1 H60C H 0.3097 0.4181 0.5226 0.165 Uiso 0.582(7) 1 calc PR A 1 C59' C 0.2677(10) 0.3527(16) 0.493(3) 0.084(6) Uani 0.418(7) 1 d PD A 2 H59C H 0.2730 0.3472 0.3977 0.101 Uiso 0.418(7) 1 calc PR A 2 H59D H 0.2724 0.3890 0.5151 0.101 Uiso 0.418(7) 1 calc PR A 2 C60' C 0.2017(6) 0.3257(5) 0.5558(11) 0.110(3) Uani 0.418(7) 1 d PD A 2 H60D H 0.1756 0.3253 0.4840 0.165 Uiso 0.418(7) 1 calc PR A 2 H60E H 0.1883 0.3468 0.6278 0.165 Uiso 0.418(7) 1 calc PR A 2 H60F H 0.2074 0.2911 0.5877 0.165 Uiso 0.418(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.03322(16) 0.03411(16) 0.03117(15) -0.00324(13) -0.00332(13) 0.00200(13) Cu2 0.03123(16) 0.03190(15) 0.03072(15) -0.00146(12) -0.00278(13) -0.00046(13) N1 0.0439(14) 0.0327(12) 0.0521(15) -0.0035(11) 0.0028(11) 0.0019(11) N2 0.0349(14) 0.0492(15) 0.0556(15) -0.0084(12) -0.0030(12) -0.0108(12) N3 0.0329(12) 0.0350(11) 0.0392(12) 0.0064(10) -0.0012(10) 0.0006(9) N4 0.0338(12) 0.0376(12) 0.0443(13) -0.0007(10) 0.0042(10) 0.0009(10) O1 0.0418(11) 0.0349(10) 0.0431(11) -0.0054(8) -0.0024(9) 0.0022(9) O2 0.0449(12) 0.0320(10) 0.0437(11) -0.0032(8) -0.0036(9) -0.0010(8) O3 0.0802(19) 0.0516(14) 0.0723(17) -0.0180(13) 0.0128(14) -0.0207(13) O4 0.0419(12) 0.0389(12) 0.0811(17) 0.0023(12) -0.0018(12) -0.0043(9) O5 0.0348(11) 0.0419(11) 0.0503(12) -0.0035(9) -0.0022(9) -0.0010(9) O6 0.0310(10) 0.0454(11) 0.0466(11) -0.0064(9) -0.0028(8) -0.0047(9) O7 0.0434(14) 0.088(2) 0.098(2) -0.0281(18) -0.0212(15) 0.0161(14) O8 0.0648(16) 0.0459(12) 0.0604(14) 0.0009(11) -0.0217(13) -0.0044(11) O9 0.0467(11) 0.0341(10) 0.0356(9) 0.0014(8) -0.0006(9) 0.0064(8) O10 0.0417(11) 0.0361(10) 0.0390(10) 0.0019(8) -0.0033(9) 0.0019(9) O11 0.0526(15) 0.0532(14) 0.0631(15) 0.0200(12) -0.0004(12) -0.0079(11) O12 0.0486(13) 0.0600(14) 0.0537(13) 0.0184(11) 0.0002(11) -0.0083(11) O13 0.0346(10) 0.0426(11) 0.0402(10) -0.0028(9) -0.0002(8) -0.0006(9) O14 0.0342(10) 0.0406(10) 0.0391(10) 0.0004(9) -0.0016(8) -0.0033(8) O15 0.0577(15) 0.0659(15) 0.0578(14) -0.0066(12) 0.0154(12) 0.0178(12) O16 0.0496(13) 0.0427(12) 0.0475(12) -0.0059(10) 0.0040(10) 0.0081(10) C1 0.0313(14) 0.0331(14) 0.0437(14) 0.0005(12) -0.0008(11) 0.0000(11) C2 0.0412(16) 0.0313(14) 0.0434(15) -0.0022(11) 0.0030(12) -0.0004(12) C3 0.0377(16) 0.0381(15) 0.0553(19) 0.0061(13) -0.0011(13) 0.0049(13) C4 0.0488(18) 0.0485(18) 0.0521(18) 0.0079(15) 0.0026(15) 0.0115(15) C5 0.052(2) 0.070(2) 0.064(2) 0.021(2) 0.0070(19) 0.0165(18) C6 0.060(2) 0.095(3) 0.055(2) 0.021(2) 0.0135(18) 0.028(2) C7 0.099(4) 0.097(4) 0.048(2) -0.001(2) 0.006(2) 0.036(3) C8 0.093(3) 0.065(2) 0.055(2) -0.0077(18) 0.011(2) 0.008(2) C9 0.061(2) 0.0456(18) 0.0510(19) -0.0019(15) 0.0053(16) 0.0072(16) C10 0.063(2) 0.0360(15) 0.0538(18) -0.0036(15) 0.0053(17) -0.0016(14) C11 0.057(2) 0.0422(16) 0.0491(17) 0.0050(14) -0.0002(15) 0.0105(15) C12 0.049(2) 0.084(3) 0.060(2) 0.011(2) -0.0155(17) 0.0055(19) C13 0.112(4) 0.047(2) 0.079(3) 0.010(2) -0.007(3) 0.029(2) C14 0.078(3) 0.0515(19) 0.0506(18) 0.0059(16) 0.0022(17) -0.0024(18) C15 0.0333(14) 0.0341(14) 0.0505(16) -0.0043(13) -0.0003(13) -0.0007(11) C16 0.0335(15) 0.0496(17) 0.060(2) -0.0145(14) -0.0003(14) -0.0033(13) C17 0.0325(16) 0.066(2) 0.062(2) -0.0093(17) -0.0037(14) -0.0087(16) C18 0.0389(17) 0.057(2) 0.057(2) -0.0085(16) -0.0001(15) -0.0126(15) C19 0.053(2) 0.077(3) 0.066(2) -0.017(2) -0.0131(19) -0.0106(19) C20 0.069(3) 0.085(3) 0.072(3) -0.029(2) -0.008(2) -0.017(2) C21 0.079(3) 0.057(2) 0.072(3) -0.0183(19) -0.001(2) -0.008(2) C22 0.073(2) 0.0442(18) 0.058(2) 0.0001(15) -0.0045(18) -0.0063(16) C23 0.0470(17) 0.0453(16) 0.0485(16) 0.0023(14) -0.0021(15) -0.0123(14) C24 0.0473(19) 0.0405(16) 0.0507(17) 0.0018(14) -0.0023(15) -0.0125(14) C25 0.047(2) 0.095(3) 0.060(2) -0.025(2) 0.0173(18) -0.028(2) C26 0.050(2) 0.104(3) 0.083(3) -0.047(3) 0.009(2) -0.009(2) C27 0.125(4) 0.093(3) 0.055(2) -0.007(2) 0.017(3) -0.049(3) C28 0.057(3) 0.189(7) 0.106(4) -0.067(4) 0.034(3) -0.052(4) C29 0.0324(15) 0.0344(14) 0.0428(15) 0.0014(11) 0.0002(11) 0.0005(11) C30 0.0338(14) 0.0336(14) 0.0427(14) 0.0023(11) -0.0032(12) 0.0022(11) C31 0.0453(17) 0.0372(15) 0.0461(16) 0.0068(13) 0.0017(13) 0.0047(13) C32 0.0482(18) 0.0421(16) 0.0490(18) 0.0048(13) -0.0025(14) 0.0075(14) C33 0.073(2) 0.059(2) 0.0478(18) 0.0138(16) -0.0077(18) 0.0082(19) C34 0.088(3) 0.076(3) 0.055(2) 0.006(2) -0.026(2) -0.001(2) C35 0.071(3) 0.089(3) 0.077(3) 0.001(3) -0.034(2) -0.012(2) C36 0.058(2) 0.071(3) 0.072(3) 0.008(2) -0.012(2) -0.016(2) C37 0.0424(18) 0.0468(17) 0.0485(16) 0.0033(13) -0.0077(13) 0.0008(13) C38 0.0406(16) 0.0459(16) 0.0466(16) 0.0060(14) -0.0032(14) 0.0002(13) C39 0.055(2) 0.0424(16) 0.0527(19) -0.0091(14) -0.0118(15) 0.0141(15) C40 0.073(3) 0.087(3) 0.060(2) -0.017(2) 0.009(2) 0.020(2) C41 0.094(3) 0.0432(19) 0.075(3) -0.0108(18) -0.024(2) 0.024(2) C42 0.071(3) 0.0455(18) 0.078(3) -0.0107(17) -0.028(2) 0.0115(17) C43 0.0369(15) 0.0258(12) 0.0435(15) 0.0023(11) 0.0005(12) 0.0043(11) C44 0.0326(14) 0.0346(13) 0.0402(14) -0.0030(11) 0.0052(11) 0.0031(11) C45 0.0370(17) 0.0547(19) 0.0475(17) -0.0037(14) 0.0127(13) 0.0020(14) C46 0.0393(17) 0.062(2) 0.0485(18) 0.0054(15) 0.0081(14) 0.0012(15) C47 0.073(3) 0.096(3) 0.046(2) 0.007(2) 0.0157(19) 0.015(2) C48 0.093(4) 0.113(4) 0.052(2) 0.016(2) 0.018(2) 0.033(3) C49 0.087(3) 0.083(3) 0.063(2) 0.021(2) -0.001(2) 0.024(3) C50 0.058(2) 0.057(2) 0.058(2) 0.0092(17) -0.0003(16) 0.0085(17) C51 0.0374(16) 0.0433(16) 0.0521(18) 0.0045(13) 0.0032(13) -0.0014(13) C52 0.0356(15) 0.0354(14) 0.0472(16) -0.0027(13) 0.0023(13) -0.0030(11) C53 0.0335(15) 0.0376(15) 0.0515(17) -0.0028(13) 0.0001(12) 0.0007(12) C54 0.0495(19) 0.0469(18) 0.064(2) 0.0041(16) -0.0152(15) 0.0045(15) C55 0.0336(17) 0.073(2) 0.076(3) -0.008(2) 0.0026(17) 0.0000(16) C56 0.0460(18) 0.0433(16) 0.0532(18) -0.0085(14) -0.0040(14) -0.0026(14) N5 0.0608(18) 0.083(2) 0.0388(14) 0.0016(15) -0.0052(13) -0.0171(17) C57 0.066(2) 0.068(2) 0.0465(18) -0.0024(17) -0.0057(17) -0.0016(19) C58 0.099(4) 0.118(4) 0.077(3) 0.021(3) -0.027(3) 0.018(3) O17 0.0702(17) 0.0692(17) 0.0422(12) -0.0096(12) -0.0149(11) 0.0091(14) C59 0.096(11) 0.105(9) 0.051(8) 0.000(6) -0.021(7) 0.017(10) C60 0.173(9) 0.098(5) 0.059(4) -0.011(4) -0.008(5) 0.058(6) C59' 0.096(11) 0.105(9) 0.051(8) 0.000(6) -0.021(7) 0.017(10) C60' 0.173(9) 0.098(5) 0.059(4) -0.011(4) -0.008(5) 0.058(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 Cu1 O9 1.9448(19) . ? Cu1 O1 1.9545(19) . ? Cu1 O13 1.956(2) . ? Cu1 O5 1.957(2) . ? Cu1 O17 2.173(2) . ? Cu1 Cu2 2.6422(6) . ? Cu2 O6 1.955(2) . ? Cu2 O14 1.965(2) . ? Cu2 O10 1.976(2) . ? Cu2 O2 1.9902(19) . ? Cu2 N5 2.205(3) . ? N1 C10 1.387(4) . ? N1 C3 1.404(4) . ? N1 C2 1.475(4) . ? N2 C17 1.397(4) . ? N2 C24 1.409(4) . ? N2 C16 1.471(4) . ? N3 C38 1.400(4) . ? N3 C31 1.401(4) . ? N3 C30 1.469(4) . ? N4 C45 1.403(4) . ? N4 C52 1.418(4) . ? N4 C44 1.478(4) . ? O1 C1 1.257(3) . ? O2 C1 1.249(3) . ? O3 C10 1.206(4) . ? O4 C3 1.207(4) . ? O5 C15 1.261(4) . ? O6 C15 1.254(4) . ? O7 C17 1.199(4) . ? O8 C24 1.208(4) . ? O9 C29 1.253(3) . ? O10 C29 1.259(3) . ? O11 C31 1.200(4) . ? O12 C38 1.196(4) . ? O13 C43 1.257(3) . ? O14 C43 1.250(3) . ? O15 C45 1.206(4) . ? O16 C52 1.202(4) . ? C1 C2 1.546(4) . ? C2 C11 1.551(4) . ? C3 C4 1.492(5) . ? C4 C5 1.370(5) . ? C4 C9 1.386(5) . ? C5 C6 1.372(6) . ? C6 C7 1.385(7) . ? C7 C8 1.382(6) . ? C8 C9 1.379(5) . ? C9 C10 1.492(5) . ? C11 C12 1.518(5) . ? C11 C14 1.539(5) . ? C11 C13 1.565(5) . ? C15 C16 1.533(4) . ? C16 C25 1.547(5) . ? C17 C18 1.491(5) . ? C18 C23 1.374(5) . ? C18 C19 1.382(5) . ? C19 C20 1.379(6) . ? C20 C21 1.385(6) . ? C21 C22 1.389(5) . ? C22 C23 1.388(5) . ? C23 C24 1.477(5) . ? C25 C27 1.505(7) . ? C25 C26 1.539(6) . ? C25 C28 1.552(6) . ? C29 C30 1.543(4) . ? C30 C39 1.535(4) . ? C31 C32 1.499(5) . ? C32 C33 1.369(5) . ? C32 C37 1.387(5) . ? C33 C34 1.372(6) . ? C34 C35 1.365(6) . ? C35 C36 1.389(6) . ? C36 C37 1.380(5) . ? C37 C38 1.495(4) . ? C39 C40 1.528(6) . ? C39 C42 1.536(5) . ? C39 C41 1.538(5) . ? C43 C44 1.543(4) . ? C44 C53 1.541(4) . ? C45 C46 1.480(5) . ? C46 C51 1.383(5) . ? C46 C47 1.385(5) . ? C47 C48 1.380(6) . ? C48 C49 1.370(6) . ? C49 C50 1.391(6) . ? C50 C51 1.375(5) . ? C51 C52 1.493(4) . ? C53 C56 1.516(4) . ? C53 C54 1.526(4) . ? C53 C55 1.537(4) . ? N5 C57 1.131(5) . ? C57 C58 1.467(6) . ? O17 C59 1.454(10) . ? O17 C59' 1.460(14) . ? C59 C60 1.88(3) . ? C59' C60' 1.91(3) . ? 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 O9 Cu1 O1 173.24(9) . . ? O9 Cu1 O13 89.41(9) . . ? O1 Cu1 O13 89.32(9) . . ? O9 Cu1 O5 89.52(9) . . ? O1 Cu1 O5 89.93(9) . . ? O13 Cu1 O5 164.41(9) . . ? O9 Cu1 O17 94.16(10) . . ? O1 Cu1 O17 92.60(10) . . ? O13 Cu1 O17 98.34(10) . . ? O5 Cu1 O17 97.25(10) . . ? O9 Cu1 Cu2 84.22(6) . . ? O1 Cu1 Cu2 89.03(6) . . ? O13 Cu1 Cu2 82.64(6) . . ? O5 Cu1 Cu2 81.78(7) . . ? O17 Cu1 Cu2 178.11(8) . . ? O6 Cu2 O14 172.23(8) . . ? O6 Cu2 O10 88.22(9) . . ? O14 Cu2 O10 90.51(9) . . ? O6 Cu2 O2 90.59(9) . . ? O14 Cu2 O2 88.45(9) . . ? O10 Cu2 O2 163.53(8) . . ? O6 Cu2 N5 95.45(10) . . ? O14 Cu2 N5 92.21(10) . . ? O10 Cu2 N5 108.86(11) . . ? O2 Cu2 N5 87.60(11) . . ? O6 Cu2 Cu1 86.60(6) . . ? O14 Cu2 Cu1 85.64(6) . . ? O10 Cu2 Cu1 84.21(6) . . ? O2 Cu2 Cu1 79.32(6) . . ? N5 Cu2 Cu1 166.79(10) . . ? C10 N1 C3 112.3(3) . . ? C10 N1 C2 122.7(3) . . ? C3 N1 C2 124.5(3) . . ? C17 N2 C24 111.4(3) . . ? C17 N2 C16 122.0(3) . . ? C24 N2 C16 122.5(3) . . ? C38 N3 C31 111.8(2) . . ? C38 N3 C30 124.5(2) . . ? C31 N3 C30 122.3(2) . . ? C45 N4 C52 110.6(3) . . ? C45 N4 C44 120.9(2) . . ? C52 N4 C44 123.1(2) . . ? C1 O1 Cu1 117.53(17) . . ? C1 O2 Cu2 127.33(18) . . ? C15 O5 Cu1 125.13(19) . . ? C15 O6 Cu2 119.75(19) . . ? C29 O9 Cu1 123.13(18) . . ? C29 O10 Cu2 121.45(18) . . ? C43 O13 Cu1 124.32(19) . . ? C43 O14 Cu2 120.46(19) . . ? O2 C1 O1 126.7(3) . . ? O2 C1 C2 118.4(2) . . ? O1 C1 C2 114.9(2) . . ? N1 C2 C1 108.0(2) . . ? N1 C2 C11 112.8(2) . . ? C1 C2 C11 117.6(2) . . ? O4 C3 N1 125.7(3) . . ? O4 C3 C4 128.8(3) . . ? N1 C3 C4 105.5(3) . . ? C5 C4 C9 121.5(4) . . ? C5 C4 C3 130.6(4) . . ? C9 C4 C3 107.9(3) . . ? C6 C5 C4 118.4(4) . . ? C5 C6 C7 120.1(4) . . ? C8 C7 C6 122.2(4) . . ? C9 C8 C7 117.1(4) . . ? C8 C9 C4 120.8(4) . . ? C8 C9 C10 130.8(4) . . ? C4 C9 C10 108.4(3) . . ? O3 C10 N1 125.1(3) . . ? O3 C10 C9 129.3(3) . . ? N1 C10 C9 105.6(3) . . ? C12 C11 C14 110.4(3) . . ? C12 C11 C2 113.6(3) . . ? C14 C11 C2 108.2(3) . . ? C12 C11 C13 110.0(3) . . ? C14 C11 C13 107.4(3) . . ? C2 C11 C13 107.0(3) . . ? O6 C15 O5 126.7(3) . . ? O6 C15 C16 120.3(3) . . ? O5 C15 C16 113.0(3) . . ? N2 C16 C15 107.1(2) . . ? N2 C16 C25 114.4(3) . . ? C15 C16 C25 118.7(3) . . ? O7 C17 N2 124.9(3) . . ? O7 C17 C18 129.3(3) . . ? N2 C17 C18 105.7(3) . . ? C23 C18 C19 121.6(4) . . ? C23 C18 C17 107.9(3) . . ? C19 C18 C17 130.4(4) . . ? C20 C19 C18 117.4(4) . . ? C19 C20 C21 121.5(4) . . ? C20 C21 C22 120.9(4) . . ? C23 C22 C21 117.3(4) . . ? C18 C23 C22 121.3(3) . . ? C18 C23 C24 109.1(3) . . ? C22 C23 C24 129.5(3) . . ? O8 C24 N2 125.5(3) . . ? O8 C24 C23 129.0(3) . . ? N2 C24 C23 105.5(3) . . ? C27 C25 C26 110.6(4) . . ? C27 C25 C16 112.9(4) . . ? C26 C25 C16 109.0(3) . . ? C27 C25 C28 110.4(4) . . ? C26 C25 C28 107.2(4) . . ? C16 C25 C28 106.6(3) . . ? O9 C29 O10 127.0(3) . . ? O9 C29 C30 114.2(2) . . ? O10 C29 C30 118.8(2) . . ? N3 C30 C39 114.1(2) . . ? N3 C30 C29 107.6(2) . . ? C39 C30 C29 120.0(2) . . ? O11 C31 N3 125.6(3) . . ? O11 C31 C32 128.6(3) . . ? N3 C31 C32 105.9(3) . . ? C33 C32 C37 121.1(3) . . ? C33 C32 C31 131.1(3) . . ? C37 C32 C31 107.8(3) . . ? C32 C33 C34 118.1(4) . . ? C35 C34 C33 121.1(4) . . ? C34 C35 C36 121.8(4) . . ? C37 C36 C35 116.8(4) . . ? C36 C37 C32 121.1(3) . . ? C36 C37 C38 130.4(3) . . ? C32 C37 C38 108.5(3) . . ? O12 C38 N3 125.6(3) . . ? O12 C38 C37 128.6(3) . . ? N3 C38 C37 105.7(3) . . ? C40 C39 C30 112.8(3) . . ? C40 C39 C42 109.7(3) . . ? C30 C39 C42 109.0(3) . . ? C40 C39 C41 110.1(3) . . ? C30 C39 C41 107.6(3) . . ? C42 C39 C41 107.5(3) . . ? O14 C43 O13 126.9(3) . . ? O14 C43 C44 119.9(3) . . ? O13 C43 C44 113.2(2) . . ? N4 C44 C53 115.0(2) . . ? N4 C44 C43 105.6(2) . . ? C53 C44 C43 119.9(2) . . ? O15 C45 N4 124.4(3) . . ? O15 C45 C46 129.1(3) . . ? N4 C45 C46 106.5(3) . . ? C51 C46 C47 120.8(4) . . ? C51 C46 C45 108.8(3) . . ? C47 C46 C45 130.4(4) . . ? C48 C47 C46 117.4(4) . . ? C49 C48 C47 121.4(4) . . ? C48 C49 C50 121.7(4) . . ? C51 C50 C49 116.6(4) . . ? C50 C51 C46 122.0(3) . . ? C50 C51 C52 130.0(3) . . ? C46 C51 C52 107.9(3) . . ? O16 C52 N4 125.3(3) . . ? O16 C52 C51 128.8(3) . . ? N4 C52 C51 105.9(3) . . ? C56 C53 C54 109.6(3) . . ? C56 C53 C55 109.2(3) . . ? C54 C53 C55 109.0(3) . . ? C56 C53 C44 113.3(2) . . ? C54 C53 C44 108.7(2) . . ? C55 C53 C44 106.8(3) . . ? C57 N5 Cu2 151.7(3) . . ? N5 C57 C58 179.0(5) . . ? C59 O17 C59' 18.8(19) . . ? C59 O17 Cu1 120.3(11) . . ? C59' O17 Cu1 127.1(17) . . ? O17 C59 C60 98.1(13) . . ? O17 C59' C60' 94.1(16) . . ? 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 O9 Cu1 Cu2 O6 88.70(9) . . . . ? O1 Cu1 Cu2 O6 -91.71(9) . . . . ? O13 Cu1 Cu2 O6 178.85(9) . . . . ? O5 Cu1 Cu2 O6 -1.65(9) . . . . ? O17 Cu1 Cu2 O6 58(3) . . . . ? O9 Cu1 Cu2 O14 -90.81(9) . . . . ? O1 Cu1 Cu2 O14 88.77(9) . . . . ? O13 Cu1 Cu2 O14 -0.66(9) . . . . ? O5 Cu1 Cu2 O14 178.84(9) . . . . ? O17 Cu1 Cu2 O14 -122(3) . . . . ? O9 Cu1 Cu2 O10 0.15(9) . . . . ? O1 Cu1 Cu2 O10 179.73(9) . . . . ? O13 Cu1 Cu2 O10 90.30(9) . . . . ? O5 Cu1 Cu2 O10 -90.20(9) . . . . ? O17 Cu1 Cu2 O10 -31(3) . . . . ? O9 Cu1 Cu2 O2 179.95(9) . . . . ? O1 Cu1 Cu2 O2 -0.47(9) . . . . ? O13 Cu1 Cu2 O2 -89.90(9) . . . . ? O5 Cu1 Cu2 O2 89.60(9) . . . . ? O17 Cu1 Cu2 O2 149(3) . . . . ? O9 Cu1 Cu2 N5 -171.9(4) . . . . ? O1 Cu1 Cu2 N5 7.7(4) . . . . ? O13 Cu1 Cu2 N5 -81.7(4) . . . . ? O5 Cu1 Cu2 N5 97.8(4) . . . . ? O17 Cu1 Cu2 N5 157(3) . . . . ? O9 Cu1 O1 C1 2.4(9) . . . . ? O13 Cu1 O1 C1 81.6(2) . . . . ? O5 Cu1 O1 C1 -82.9(2) . . . . ? O17 Cu1 O1 C1 179.9(2) . . . . ? Cu2 Cu1 O1 C1 -1.1(2) . . . . ? O6 Cu2 O2 C1 88.8(2) . . . . ? O14 Cu2 O2 C1 -83.5(2) . . . . ? O10 Cu2 O2 C1 3.1(5) . . . . ? N5 Cu2 O2 C1 -175.8(3) . . . . ? Cu1 Cu2 O2 C1 2.4(2) . . . . ? O9 Cu1 O5 C15 -82.4(2) . . . . ? O1 Cu1 O5 C15 90.9(2) . . . . ? O13 Cu1 O5 C15 3.7(5) . . . . ? O17 Cu1 O5 C15 -176.5(2) . . . . ? Cu2 Cu1 O5 C15 1.8(2) . . . . ? O14 Cu2 O6 C15 5.6(8) . . . . ? O10 Cu2 O6 C15 86.4(2) . . . . ? O2 Cu2 O6 C15 -77.2(2) . . . . ? N5 Cu2 O6 C15 -164.9(2) . . . . ? Cu1 Cu2 O6 C15 2.1(2) . . . . ? O1 Cu1 O9 C29 -4.8(9) . . . . ? O13 Cu1 O9 C29 -83.9(2) . . . . ? O5 Cu1 O9 C29 80.5(2) . . . . ? O17 Cu1 O9 C29 177.8(2) . . . . ? Cu2 Cu1 O9 C29 -1.3(2) . . . . ? O6 Cu2 O10 C29 -85.9(2) . . . . ? O14 Cu2 O10 C29 86.5(2) . . . . ? O2 Cu2 O10 C29 0.2(5) . . . . ? N5 Cu2 O10 C29 179.0(2) . . . . ? Cu1 Cu2 O10 C29 0.9(2) . . . . ? O9 Cu1 O13 C43 85.4(2) . . . . ? O1 Cu1 O13 C43 -88.0(2) . . . . ? O5 Cu1 O13 C43 -0.7(5) . . . . ? O17 Cu1 O13 C43 179.5(2) . . . . ? Cu2 Cu1 O13 C43 1.1(2) . . . . ? O6 Cu2 O14 C43 -3.1(8) . . . . ? O10 Cu2 O14 C43 -83.7(2) . . . . ? O2 Cu2 O14 C43 79.9(2) . . . . ? N5 Cu2 O14 C43 167.4(2) . . . . ? Cu1 Cu2 O14 C43 0.46(19) . . . . ? Cu2 O2 C1 O1 -4.3(4) . . . . ? Cu2 O2 C1 C2 179.13(19) . . . . ? Cu1 O1 C1 O2 3.3(4) . . . . ? Cu1 O1 C1 C2 179.97(18) . . . . ? C10 N1 C2 C1 -125.5(3) . . . . ? C3 N1 C2 C1 45.6(4) . . . . ? C10 N1 C2 C11 102.8(3) . . . . ? C3 N1 C2 C11 -86.0(3) . . . . ? O2 C1 C2 N1 -140.2(3) . . . . ? O1 C1 C2 N1 42.9(3) . . . . ? O2 C1 C2 C11 -11.1(4) . . . . ? O1 C1 C2 C11 171.9(3) . . . . ? C10 N1 C3 O4 175.7(3) . . . . ? C2 N1 C3 O4 3.8(5) . . . . ? C10 N1 C3 C4 -5.0(3) . . . . ? C2 N1 C3 C4 -176.9(3) . . . . ? O4 C3 C4 C5 2.2(6) . . . . ? N1 C3 C4 C5 -177.1(3) . . . . ? O4 C3 C4 C9 -178.7(3) . . . . ? N1 C3 C4 C9 2.0(3) . . . . ? C9 C4 C5 C6 0.3(5) . . . . ? C3 C4 C5 C6 179.3(3) . . . . ? C4 C5 C6 C7 -0.3(6) . . . . ? C5 C6 C7 C8 0.9(6) . . . . ? C6 C7 C8 C9 -1.4(6) . . . . ? C7 C8 C9 C4 1.3(6) . . . . ? C7 C8 C9 C10 179.6(4) . . . . ? C5 C4 C9 C8 -0.8(5) . . . . ? C3 C4 C9 C8 180.0(3) . . . . ? C5 C4 C9 C10 -179.4(3) . . . . ? C3 C4 C9 C10 1.4(4) . . . . ? C3 N1 C10 O3 -174.4(3) . . . . ? C2 N1 C10 O3 -2.2(5) . . . . ? C3 N1 C10 C9 5.8(4) . . . . ? C2 N1 C10 C9 177.9(3) . . . . ? C8 C9 C10 O3 -2.6(7) . . . . ? C4 C9 C10 O3 175.8(4) . . . . ? C8 C9 C10 N1 177.3(4) . . . . ? C4 C9 C10 N1 -4.3(4) . . . . ? N1 C2 C11 C12 68.8(4) . . . . ? C1 C2 C11 C12 -57.9(4) . . . . ? N1 C2 C11 C14 -168.2(3) . . . . ? C1 C2 C11 C14 65.0(4) . . . . ? N1 C2 C11 C13 -52.8(4) . . . . ? C1 C2 C11 C13 -179.5(3) . . . . ? Cu2 O6 C15 O5 -1.4(4) . . . . ? Cu2 O6 C15 C16 -178.7(2) . . . . ? Cu1 O5 C15 O6 -0.9(4) . . . . ? Cu1 O5 C15 C16 176.64(18) . . . . ? C17 N2 C16 C15 -116.5(3) . . . . ? C24 N2 C16 C15 38.8(4) . . . . ? C17 N2 C16 C25 109.6(4) . . . . ? C24 N2 C16 C25 -95.0(4) . . . . ? O6 C15 C16 N2 -135.4(3) . . . . ? O5 C15 C16 N2 47.0(4) . . . . ? O6 C15 C16 C25 -3.9(5) . . . . ? O5 C15 C16 C25 178.5(3) . . . . ? C24 N2 C17 O7 -173.7(4) . . . . ? C16 N2 C17 O7 -15.9(5) . . . . ? C24 N2 C17 C18 5.6(4) . . . . ? C16 N2 C17 C18 163.3(3) . . . . ? O7 C17 C18 C23 174.0(4) . . . . ? N2 C17 C18 C23 -5.2(4) . . . . ? O7 C17 C18 C19 -3.2(7) . . . . ? N2 C17 C18 C19 177.6(4) . . . . ? C23 C18 C19 C20 -1.3(6) . . . . ? C17 C18 C19 C20 175.6(4) . . . . ? C18 C19 C20 C21 1.1(7) . . . . ? C19 C20 C21 C22 -0.9(7) . . . . ? C20 C21 C22 C23 0.7(6) . . . . ? C19 C18 C23 C22 1.3(5) . . . . ? C17 C18 C23 C22 -176.3(3) . . . . ? C19 C18 C23 C24 -179.6(3) . . . . ? C17 C18 C23 C24 2.9(4) . . . . ? C21 C22 C23 C18 -0.9(5) . . . . ? C21 C22 C23 C24 -179.9(3) . . . . ? C17 N2 C24 O8 175.3(3) . . . . ? C16 N2 C24 O8 17.7(5) . . . . ? C17 N2 C24 C23 -3.8(4) . . . . ? C16 N2 C24 C23 -161.5(3) . . . . ? C18 C23 C24 O8 -178.7(3) . . . . ? C22 C23 C24 O8 0.4(6) . . . . ? C18 C23 C24 N2 0.4(4) . . . . ? C22 C23 C24 N2 179.5(3) . . . . ? N2 C16 C25 C27 65.4(4) . . . . ? C15 C16 C25 C27 -62.8(4) . . . . ? N2 C16 C25 C26 -171.4(3) . . . . ? C15 C16 C25 C26 60.4(5) . . . . ? N2 C16 C25 C28 -56.1(5) . . . . ? C15 C16 C25 C28 175.8(4) . . . . ? Cu1 O9 C29 O10 2.5(4) . . . . ? Cu1 O9 C29 C30 179.94(18) . . . . ? Cu2 O10 C29 O9 -2.3(4) . . . . ? Cu2 O10 C29 C30 -179.60(19) . . . . ? C38 N3 C30 C39 -88.7(4) . . . . ? C31 N3 C30 C39 105.8(3) . . . . ? C38 N3 C30 C29 47.2(4) . . . . ? C31 N3 C30 C29 -118.3(3) . . . . ? O9 C29 C30 N3 36.3(3) . . . . ? O10 C29 C30 N3 -146.1(3) . . . . ? O9 C29 C30 C39 169.0(3) . . . . ? O10 C29 C30 C39 -13.3(4) . . . . ? C38 N3 C31 O11 -175.7(3) . . . . ? C30 N3 C31 O11 -8.5(5) . . . . ? C38 N3 C31 C32 5.0(3) . . . . ? C30 N3 C31 C32 172.2(2) . . . . ? O11 C31 C32 C33 -1.0(6) . . . . ? N3 C31 C32 C33 178.3(4) . . . . ? O11 C31 C32 C37 176.8(4) . . . . ? N3 C31 C32 C37 -4.0(3) . . . . ? C37 C32 C33 C34 -0.1(5) . . . . ? C31 C32 C33 C34 177.4(4) . . . . ? C32 C33 C34 C35 -0.2(7) . . . . ? C33 C34 C35 C36 0.4(8) . . . . ? C34 C35 C36 C37 -0.3(7) . . . . ? C35 C36 C37 C32 -0.1(6) . . . . ? C35 C36 C37 C38 -179.3(4) . . . . ? C33 C32 C37 C36 0.2(5) . . . . ? C31 C32 C37 C36 -177.8(3) . . . . ? C33 C32 C37 C38 179.6(3) . . . . ? C31 C32 C37 C38 1.6(4) . . . . ? C31 N3 C38 O12 175.9(3) . . . . ? C30 N3 C38 O12 9.1(5) . . . . ? C31 N3 C38 C37 -4.1(3) . . . . ? C30 N3 C38 C37 -170.9(3) . . . . ? C36 C37 C38 O12 0.7(6) . . . . ? C32 C37 C38 O12 -178.6(4) . . . . ? C36 C37 C38 N3 -179.3(4) . . . . ? C32 C37 C38 N3 1.4(4) . . . . ? N3 C30 C39 C40 69.6(4) . . . . ? C29 C30 C39 C40 -60.4(4) . . . . ? N3 C30 C39 C42 -168.3(3) . . . . ? C29 C30 C39 C42 61.8(4) . . . . ? N3 C30 C39 C41 -52.1(4) . . . . ? C29 C30 C39 C41 178.0(3) . . . . ? Cu2 O14 C43 O13 0.3(4) . . . . ? Cu2 O14 C43 C44 -177.33(17) . . . . ? Cu1 O13 C43 O14 -1.2(4) . . . . ? Cu1 O13 C43 C44 176.53(17) . . . . ? C45 N4 C44 C53 115.6(3) . . . . ? C52 N4 C44 C53 -92.9(3) . . . . ? C45 N4 C44 C43 -109.9(3) . . . . ? C52 N4 C44 C43 41.6(3) . . . . ? O14 C43 C44 N4 -133.1(3) . . . . ? O13 C43 C44 N4 49.0(3) . . . . ? O14 C43 C44 C53 -1.3(4) . . . . ? O13 C43 C44 C53 -179.2(2) . . . . ? C52 N4 C45 O15 -172.5(3) . . . . ? C44 N4 C45 O15 -17.8(5) . . . . ? C52 N4 C45 C46 5.7(3) . . . . ? C44 N4 C45 C46 160.4(3) . . . . ? O15 C45 C46 C51 174.5(4) . . . . ? N4 C45 C46 C51 -3.6(4) . . . . ? O15 C45 C46 C47 -1.7(7) . . . . ? N4 C45 C46 C47 -179.8(4) . . . . ? C51 C46 C47 C48 -0.2(7) . . . . ? C45 C46 C47 C48 175.6(4) . . . . ? C46 C47 C48 C49 0.6(8) . . . . ? C47 C48 C49 C50 -0.5(9) . . . . ? C48 C49 C50 C51 0.0(8) . . . . ? C49 C50 C51 C46 0.4(6) . . . . ? C49 C50 C51 C52 -176.1(4) . . . . ? C47 C46 C51 C50 -0.3(6) . . . . ? C45 C46 C51 C50 -176.9(3) . . . . ? C47 C46 C51 C52 176.9(4) . . . . ? C45 C46 C51 C52 0.3(4) . . . . ? C45 N4 C52 O16 173.0(3) . . . . ? C44 N4 C52 O16 18.9(4) . . . . ? C45 N4 C52 C51 -5.5(3) . . . . ? C44 N4 C52 C51 -159.5(3) . . . . ? C50 C51 C52 O16 1.6(6) . . . . ? C46 C51 C52 O16 -175.3(3) . . . . ? C50 C51 C52 N4 180.0(4) . . . . ? C46 C51 C52 N4 3.1(3) . . . . ? N4 C44 C53 C56 62.0(3) . . . . ? C43 C44 C53 C56 -65.6(3) . . . . ? N4 C44 C53 C54 -175.8(2) . . . . ? C43 C44 C53 C54 56.6(3) . . . . ? N4 C44 C53 C55 -58.3(3) . . . . ? C43 C44 C53 C55 174.1(3) . . . . ? O6 Cu2 N5 C57 105.9(7) . . . . ? O14 Cu2 N5 C57 -72.8(7) . . . . ? O10 Cu2 N5 C57 -164.1(7) . . . . ? O2 Cu2 N5 C57 15.6(7) . . . . ? Cu1 Cu2 N5 C57 7.5(10) . . . . ? Cu2 N5 C57 C58 -51(30) . . . . ? O9 Cu1 O17 C59 -39.4(12) . . . . ? O1 Cu1 O17 C59 140.9(12) . . . . ? O13 Cu1 O17 C59 -129.4(12) . . . . ? O5 Cu1 O17 C59 50.6(12) . . . . ? Cu2 Cu1 O17 C59 -9(3) . . . . ? O9 Cu1 O17 C59' -18.3(18) . . . . ? O1 Cu1 O17 C59' 162.0(18) . . . . ? O13 Cu1 O17 C59' -108.3(18) . . . . ? O5 Cu1 O17 C59' 71.8(18) . . . . ? Cu2 Cu1 O17 C59' 13(3) . . . . ? C59' O17 C59 C60 -21(9) . . . . ? Cu1 O17 C59 C60 95.4(9) . . . . ? C59 O17 C59' C60' -5(8) . . . . ? Cu1 O17 C59' C60' -80(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.728 _refine_diff_density_min -0.296 _refine_diff_density_rms 0.058 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 0.000 -0.007 260.7 27.3 2 0.000 0.500 0.003 261.1 28.2 3 0.353 0.068 0.260 8.3 -0.2 4 0.274 0.175 0.428 88.9 17.5 5 0.508 0.273 0.250 6.7 0.1 6 0.492 0.727 0.250 6.7 0.1 7 0.725 0.826 0.426 89.8 18.0 8 0.645 0.934 0.253 7.8 -0.2 9 0.775 0.326 0.573 88.9 18.1 10 0.225 0.674 0.573 89.5 17.7 11 0.855 0.434 0.746 7.6 -0.2 12 0.145 0.566 0.746 8.4 -0.3 13 0.008 0.227 0.750 6.7 0.1 14 0.992 0.773 0.750 6.7 0.0 _platon_squeeze_details ; Void space analysis consistent with initial solutions displaying two severely disordered acetonitrile solvent molecules per compound molecule. PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13 ; # Attachment 'joef099a.cif' data_joef099a _database_code_depnum_ccdc_archive 'CCDC 770533' #TrackingRef 'joef099a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H63 N9 O16 Rh2' _chemical_formula_weight 1588.19 _chemical_absolute_configuration syn 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' 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 P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.649(4) _cell_length_b 24.398(7) _cell_length_c 12.670(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.947(4) _cell_angle_gamma 90.00 _cell_volume 3719.9(18) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 997 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 25.53 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1624 _exptl_absorpt_coefficient_mu 0.517 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8812 _exptl_absorpt_correction_T_max 0.9159 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; Data collection is performed with four batch runs at \f = 0.00 \% (600 frames), at \f = 90.00 \% (600 frames), at \f = 180 \% (600 frames) and at \f = 270 \% (600 frames). Frame width = 0.30 \& in \w. Data is merged, corrected for decay, and treated with multi-scan absorption corrections. ; _diffrn_ambient_temperature 200(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 'Bruker AXS APEX diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 836.6 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 1 _diffrn_reflns_number 51127 _diffrn_reflns_av_R_equivalents 0.0403 _diffrn_reflns_av_sigmaI/netI 0.0450 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.34 _reflns_number_total 18446 _reflns_number_gt 16477 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 2002)' _computing_cell_refinement 'SAINT (Bruker, 2002)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2001)' _computing_publication_material 'SHELXTL (Sheldrick, 2001)' _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. Three acetonitrile solvent molecules refined with SAME & SIMU constraints with isotropic parameters because of unresolvable disorder. ; _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^)+(0.0835P)^2^+2.5054P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881: 8987 Friedel pairs' _refine_ls_abs_structure_Flack 0.03(2) _refine_ls_number_reflns 18446 _refine_ls_number_parameters 903 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0525 _refine_ls_wR_factor_ref 0.1444 _refine_ls_wR_factor_gt 0.1383 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.010 _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 0.46348(3) 0.032044(12) 0.30318(3) 0.03192(9) Uani 1 1 d . . . Rh2 Rh 0.55053(3) -0.031232(12) 0.21100(3) 0.03271(9) Uani 1 1 d . . . N1 N 0.1252(3) -0.07183(18) 0.1272(4) 0.0437(9) Uani 1 1 d . . . N2 N 0.5036(4) -0.10526(18) 0.5807(4) 0.0474(10) Uani 1 1 d . . . N3 N 0.8531(3) 0.09240(19) 0.2750(4) 0.0430(9) Uani 1 1 d . . . N4 N 0.3931(3) 0.07598(18) -0.1198(3) 0.0421(9) Uani 1 1 d . . . N5 N 0.3844(3) 0.09270(18) 0.3883(3) 0.0339(8) Uani 1 1 d . . . N6 N 0.6333(4) -0.0889(2) 0.1231(4) 0.0427(10) Uani 1 1 d . . . O1 O 0.3231(3) -0.01266(15) 0.2461(3) 0.0386(8) Uani 1 1 d . . . O2 O 0.4085(3) -0.07596(15) 0.1707(3) 0.0399(8) Uani 1 1 d . . . O3 O 0.0514(4) -0.0621(2) 0.2710(4) 0.0648(11) Uani 1 1 d . . . O4 O 0.1436(4) -0.0745(3) -0.0499(4) 0.0801(14) Uani 1 1 d . . . O5 O 0.5084(3) -0.01964(15) 0.4376(3) 0.0390(8) Uani 1 1 d . . . O6 O 0.6005(3) -0.07495(15) 0.3546(3) 0.0372(7) Uani 1 1 d . . . O7 O 0.5883(6) -0.0775(3) 0.7555(4) 0.098(2) Uani 1 1 d . . . O8 O 0.3683(4) -0.1409(2) 0.4242(5) 0.0790(14) Uani 1 1 d . . . O9 O 0.6087(3) 0.07379(15) 0.3541(3) 0.0397(8) Uani 1 1 d . . . O10 O 0.6895(3) 0.01846(15) 0.2590(3) 0.0388(8) Uani 1 1 d . . . O11 O 1.0179(4) 0.0713(2) 0.4069(4) 0.0703(12) Uani 1 1 d . . . O12 O 0.7237(3) 0.12087(19) 0.1114(4) 0.0633(11) Uani 1 1 d . . . O13 O 0.4271(3) 0.07954(14) 0.1647(3) 0.0378(7) Uani 1 1 d . . . O14 O 0.4963(3) 0.01594(15) 0.0725(3) 0.0416(8) Uani 1 1 d . . . O15 O 0.5475(3) 0.07770(18) -0.1805(3) 0.0571(10) Uani 1 1 d . . . O16 O 0.2224(4) 0.0569(2) -0.1010(4) 0.0751(14) Uani 1 1 d . . . C1 C 0.3288(4) -0.0586(2) 0.2025(4) 0.0380(11) Uani 1 1 d . . . C2 C 0.2304(4) -0.0971(2) 0.1899(4) 0.0423(11) Uani 1 1 d . . . H2A H 0.2261 -0.1036 0.2664 0.051 Uiso 1 1 calc R . . C3 C 0.0428(4) -0.0589(2) 0.1743(5) 0.0499(13) Uani 1 1 d . . . C4 C -0.0535(5) -0.0406(2) 0.0815(6) 0.0585(15) Uani 1 1 d . . . C5 C -0.1570(5) -0.0231(3) 0.0828(8) 0.082(2) Uani 1 1 d . . . H5A H -0.1775 -0.0217 0.1489 0.098 Uiso 1 1 calc R . . C6 C -0.2309(7) -0.0074(4) -0.0230(12) 0.107(4) Uani 1 1 d . . . H6A H -0.3012 0.0079 -0.0271 0.129 Uiso 1 1 calc R . . C7 C -0.2022(9) -0.0139(5) -0.1211(11) 0.122(5) Uani 1 1 d . . . H7A H -0.2562 -0.0061 -0.1903 0.147 Uiso 1 1 calc R . . C8 C -0.1036(7) -0.0305(4) -0.1200(8) 0.098(3) Uani 1 1 d . . . H8A H -0.0835 -0.0326 -0.1862 0.118 Uiso 1 1 calc R . . C9 C -0.0272(5) -0.0453(3) -0.0152(6) 0.0641(16) Uani 1 1 d . . . C10 C 0.0875(5) -0.0644(3) 0.0124(5) 0.0550(13) Uani 1 1 d . . . C11 C 0.2471(5) -0.1538(3) 0.1434(6) 0.0557(15) Uani 1 1 d . . . H11A H 0.2587 -0.1487 0.0702 0.067 Uiso 1 1 calc R . . H11B H 0.3151 -0.1708 0.1937 0.067 Uiso 1 1 calc R . . C12 C 0.1039(11) -0.2010(4) 0.2125(9) 0.120(4) Uani 1 1 d . . . H12A H 0.1299 -0.1817 0.2807 0.144 Uiso 1 1 calc R . . C13 C 0.0158(13) -0.2392(6) 0.1947(11) 0.145(6) Uani 1 1 d . . . H13A H -0.0146 -0.2471 0.2528 0.174 Uiso 1 1 calc R . . C14 C -0.0248(8) -0.2641(4) 0.0963(10) 0.096(3) Uani 1 1 d . . . H14A H -0.0876 -0.2874 0.0844 0.115 Uiso 1 1 calc R . . C15 C 0.0192(7) -0.2576(3) 0.0154(7) 0.078(2) Uani 1 1 d . . . H15A H -0.0071 -0.2779 -0.0517 0.094 Uiso 1 1 calc R . . C16 C 0.1043(6) -0.2205(3) 0.0313(7) 0.074(2) Uani 1 1 d . . . H16A H 0.1329 -0.2137 -0.0286 0.089 Uiso 1 1 calc R . . C17 C 0.1510(5) -0.1922(3) 0.1303(6) 0.0539(14) Uani 1 1 d . . . C18 C 0.5643(4) -0.0623(2) 0.4319(4) 0.0358(10) Uani 1 1 d . . . C19 C 0.5932(4) -0.1004(2) 0.5328(4) 0.0408(10) Uani 1 1 d . . . H19A H 0.6573 -0.0834 0.5906 0.049 Uiso 1 1 calc R . . C20 C 0.5103(8) -0.0948(3) 0.6902(5) 0.072(2) Uani 1 1 d . . . C21 C 0.4009(10) -0.1125(3) 0.6983(9) 0.099(4) Uani 1 1 d . . . C22 C 0.3615(18) -0.1069(5) 0.7941(12) 0.210(10) Uani 1 1 d . . . H22A H 0.4078 -0.0916 0.8616 0.252 Uiso 1 1 calc R . . C23 C 0.263(2) -0.1230(7) 0.7852(19) 0.232(16) Uani 1 1 d . . . H23A H 0.2367 -0.1216 0.8477 0.279 Uiso 1 1 calc R . . C24 C 0.198(2) -0.1417(8) 0.690(3) 0.266(19) Uani 1 1 d . . . H24A H 0.1240 -0.1513 0.6860 0.319 Uiso 1 1 calc R . . C25 C 0.2277(10) -0.1485(5) 0.5951(15) 0.146(6) Uani 1 1 d . . . H25A H 0.1774 -0.1635 0.5296 0.176 Uiso 1 1 calc R . . C26 C 0.3344(8) -0.1326(3) 0.5987(10) 0.088(3) Uani 1 1 d . . . C27 C 0.3975(6) -0.1282(2) 0.5214(7) 0.0630(17) Uani 1 1 d . . . C28 C 0.6315(5) -0.1575(3) 0.5079(5) 0.0514(14) Uani 1 1 d . . . H28A H 0.5701 -0.1759 0.4510 0.062 Uiso 1 1 calc R . . H28B H 0.6948 -0.1536 0.4780 0.062 Uiso 1 1 calc R . . C29 C 0.7604(6) -0.1808(3) 0.7003(6) 0.0659(17) Uani 1 1 d . . . H29A H 0.8053 -0.1505 0.6948 0.079 Uiso 1 1 calc R . . C30 C 0.7895(7) -0.2114(3) 0.7936(6) 0.078(2) Uani 1 1 d . . . H30A H 0.8540 -0.2019 0.8526 0.094 Uiso 1 1 calc R . . C31 C 0.7294(10) -0.2549(4) 0.8047(7) 0.096(3) Uani 1 1 d . . . H31A H 0.7536 -0.2770 0.8694 0.115 Uiso 1 1 calc R . . C32 C 0.6329(8) -0.2678(3) 0.7229(7) 0.080(2) Uani 1 1 d . . . H32A H 0.5881 -0.2976 0.7321 0.096 Uiso 1 1 calc R . . C33 C 0.6010(8) -0.2358(3) 0.6241(6) 0.077(2) Uani 1 1 d . . . H33A H 0.5347 -0.2443 0.5663 0.092 Uiso 1 1 calc R . . C34 C 0.6668(6) -0.1926(2) 0.6127(5) 0.0562(15) Uani 1 1 d . . . C35 C 0.6853(4) 0.0600(2) 0.3171(4) 0.0378(10) Uani 1 1 d . . . C36 C 0.7877(4) 0.0982(3) 0.3485(5) 0.0487(12) Uani 1 1 d . . . H36A H 0.8359 0.0859 0.4231 0.058 Uiso 1 1 calc R . . C37 C 0.9679(4) 0.0811(3) 0.3133(5) 0.0477(13) Uani 1 1 d . . . C38 C 1.0057(4) 0.0860(2) 0.2151(5) 0.0472(11) Uani 1 1 d . . . C39 C 1.1104(5) 0.0747(3) 0.2047(6) 0.0636(16) Uani 1 1 d . . . H39A H 1.1706 0.0639 0.2670 0.076 Uiso 1 1 calc R . . C40 C 1.1237(6) 0.0798(3) 0.1023(7) 0.0691(19) Uani 1 1 d . . . H40A H 1.1934 0.0715 0.0923 0.083 Uiso 1 1 calc R . . C41 C 1.0365(7) 0.0968(3) 0.0136(7) 0.078(2) Uani 1 1 d . . . H41A H 1.0493 0.1024 -0.0556 0.094 Uiso 1 1 calc R . . C42 C 0.9287(6) 0.1063(3) 0.0206(6) 0.0669(17) Uani 1 1 d . . . H42A H 0.8677 0.1154 -0.0424 0.080 Uiso 1 1 calc R . . C43 C 0.9182(5) 0.1013(2) 0.1258(5) 0.0512(12) Uani 1 1 d . . . C44 C 0.8191(4) 0.1073(2) 0.1640(5) 0.0504(12) Uani 1 1 d . . . C45 C 0.7589(6) 0.1578(3) 0.3617(8) 0.076(2) Uani 1 1 d . . . H45A H 0.7017 0.1703 0.2934 0.091 Uiso 1 1 calc R . . H45B H 0.7277 0.1611 0.4242 0.091 Uiso 1 1 calc R . . C46 C 0.9309(10) 0.1986(5) 0.4917(10) 0.128(5) Uani 1 1 d . . . H46A H 0.9125 0.1808 0.5504 0.153 Uiso 1 1 calc R . . C47 C 1.0265(10) 0.2294(5) 0.5123(12) 0.132(5) Uani 1 1 d . . . H47A H 1.0727 0.2332 0.5869 0.158 Uiso 1 1 calc R . . C48 C 1.0584(8) 0.2553(5) 0.4285(10) 0.109(4) Uani 1 1 d . . . H48A H 1.1253 0.2758 0.4443 0.131 Uiso 1 1 calc R . . C49 C 0.9899(10) 0.2497(5) 0.3248(12) 0.115(4) Uani 1 1 d . . . H49A H 1.0101 0.2661 0.2657 0.139 Uiso 1 1 calc R . . C50 C 0.8866(7) 0.2199(4) 0.2991(9) 0.087(3) Uani 1 1 d . . . H50A H 0.8372 0.2182 0.2255 0.105 Uiso 1 1 calc R . . C51 C 0.8626(7) 0.1942(4) 0.3840(8) 0.084(3) Uani 1 1 d . . . C52 C 0.4540(4) 0.0620(2) 0.0823(4) 0.0342(10) Uani 1 1 d . . . C53 C 0.4440(4) 0.1023(2) -0.0127(4) 0.0403(10) Uani 1 1 d . . . H53A H 0.5213 0.1127 -0.0098 0.048 Uiso 1 1 calc R . . C54 C 0.4513(4) 0.0655(2) -0.1956(4) 0.0419(11) Uani 1 1 d . . . C55 C 0.3701(4) 0.0391(2) -0.2917(4) 0.0428(10) Uani 1 1 d . . . C56 C 0.3797(5) 0.0221(2) -0.3910(4) 0.0526(13) Uani 1 1 d . . . H56A H 0.4479 0.0258 -0.4072 0.063 Uiso 1 1 calc R . . C57 C 0.2876(6) -0.0005(3) -0.4672(5) 0.0606(15) Uani 1 1 d . . . H57A H 0.2923 -0.0116 -0.5375 0.073 Uiso 1 1 calc R . . C58 C 0.1902(6) -0.0074(3) -0.4444(5) 0.0642(16) Uani 1 1 d . . . H58A H 0.1282 -0.0231 -0.4988 0.077 Uiso 1 1 calc R . . C59 C 0.1801(6) 0.0083(3) -0.3423(5) 0.0707(18) Uani 1 1 d . . . H59A H 0.1134 0.0023 -0.3244 0.085 Uiso 1 1 calc R . . C60 C 0.2710(4) 0.0329(3) -0.2687(4) 0.0511(11) Uani 1 1 d . . . C61 C 0.2866(5) 0.0549(3) -0.1546(4) 0.0516(13) Uani 1 1 d . . . C62 C 0.3841(5) 0.1551(2) -0.0003(5) 0.0486(13) Uani 1 1 d . . . H62A H 0.3037 0.1473 -0.0172 0.058 Uiso 1 1 calc R . . H62B H 0.4122 0.1676 0.0778 0.058 Uiso 1 1 calc R . . C63 C 0.3310(7) 0.2102(3) -0.1779(6) 0.0714(18) Uani 1 1 d . . . H63A H 0.2693 0.1866 -0.2070 0.086 Uiso 1 1 calc R . . C64 C 0.3476(10) 0.2532(4) -0.2431(7) 0.093(3) Uani 1 1 d . . . H64A H 0.2970 0.2588 -0.3152 0.111 Uiso 1 1 calc R . . C65 C 0.4350(9) 0.2868(3) -0.2043(8) 0.086(3) Uani 1 1 d . . . H65A H 0.4474 0.3152 -0.2503 0.103 Uiso 1 1 calc R . . C66 C 0.5077(8) 0.2805(4) -0.0976(9) 0.095(3) Uani 1 1 d . . . H66A H 0.5678 0.3050 -0.0681 0.114 Uiso 1 1 calc R . . C67 C 0.4883(7) 0.2361(4) -0.0352(7) 0.085(2) Uani 1 1 d . . . H67A H 0.5381 0.2300 0.0371 0.102 Uiso 1 1 calc R . . C68 C 0.3991(5) 0.2012(2) -0.0756(5) 0.0505(13) Uani 1 1 d . . . C69 C 0.3383(5) 0.1199(2) 0.4302(5) 0.0481(13) Uani 1 1 d . . . C70 C 0.2748(9) 0.1526(4) 0.4839(9) 0.094(3) Uani 1 1 d . . . H70A H 0.2460 0.1851 0.4389 0.141 Uiso 1 1 calc R . . H70B H 0.3226 0.1639 0.5573 0.141 Uiso 1 1 calc R . . H70C H 0.2126 0.1309 0.4921 0.141 Uiso 1 1 calc R . . C71 C 0.6636(6) -0.1169(3) 0.0705(5) 0.0564(15) Uani 1 1 d . . . C72 C 0.7102(9) -0.1526(3) 0.0020(8) 0.093(3) Uani 1 1 d . . . H72A H 0.7845 -0.1648 0.0460 0.139 Uiso 1 1 calc R . . H72B H 0.7152 -0.1321 -0.0628 0.139 Uiso 1 1 calc R . . H72C H 0.6618 -0.1845 -0.0226 0.139 Uiso 1 1 calc R . . N7 N 0.8545(12) -0.0484(6) 0.5803(11) 0.166(5) Uiso 1 1 d DU . . C73 C 0.8723(10) -0.0629(5) 0.4966(10) 0.113(3) Uiso 1 1 d DU . . C74 C 0.8726(11) -0.0871(6) 0.3986(10) 0.140(5) Uiso 1 1 d DU . . H74A H 0.9405 -0.0769 0.3818 0.209 Uiso 1 1 calc R . . H74B H 0.8076 -0.0746 0.3386 0.209 Uiso 1 1 calc R . . H74C H 0.8696 -0.1270 0.4057 0.209 Uiso 1 1 calc R . . N8 N -0.117(2) 0.0975(11) -0.314(2) 0.298(11) Uiso 1 1 d DU . . C75 C -0.218(3) 0.096(2) -0.315(4) 0.54(3) Uiso 1 1 d DU . . C76 C -0.3017(17) 0.0630(9) -0.3831(17) 0.220(9) Uiso 1 1 d DU . . H76A H -0.3683 0.0654 -0.3594 0.331 Uiso 1 1 calc R . . H76B H -0.2760 0.0249 -0.3775 0.331 Uiso 1 1 calc R . . H76C H -0.3194 0.0754 -0.4602 0.331 Uiso 1 1 calc R . . N9 N 0.555(2) 0.1924(11) -0.3827(19) 0.282(10) Uiso 1 1 d DU . . C77 C 0.650(2) 0.1924(12) -0.318(2) 0.253(11) Uiso 1 1 d DU . . C78 C 0.6940(19) 0.1870(10) -0.2049(19) 0.241(10) Uiso 1 1 d DU . . H78A H 0.7745 0.1927 -0.1829 0.362 Uiso 1 1 calc R . . H78B H 0.6782 0.1502 -0.1828 0.362 Uiso 1 1 calc R . . H78C H 0.6604 0.2143 -0.1683 0.362 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 0.03564(16) 0.03482(19) 0.03146(15) 0.00011(14) 0.01939(12) 0.00156(14) Rh2 0.03635(16) 0.03611(19) 0.03132(15) -0.00044(14) 0.01874(13) 0.00261(14) N1 0.036(2) 0.048(2) 0.054(2) -0.0022(19) 0.0245(18) -0.0034(17) N2 0.064(3) 0.046(2) 0.043(2) 0.0037(18) 0.032(2) 0.006(2) N3 0.0361(19) 0.050(2) 0.049(2) -0.0030(19) 0.0224(17) -0.0082(18) N4 0.047(2) 0.048(2) 0.040(2) 0.0067(17) 0.0254(18) 0.0020(18) N5 0.0341(18) 0.035(2) 0.045(2) 0.0003(17) 0.0298(17) -0.0044(16) N6 0.046(2) 0.043(3) 0.046(2) -0.0045(19) 0.0246(19) -0.0008(19) O1 0.0345(16) 0.0422(19) 0.0453(18) -0.0042(15) 0.0214(14) 0.0012(13) O2 0.0400(17) 0.0406(19) 0.0427(18) -0.0041(15) 0.0182(15) 0.0014(15) O3 0.057(2) 0.085(3) 0.068(3) -0.001(2) 0.042(2) -0.006(2) O4 0.081(3) 0.112(4) 0.057(3) 0.005(3) 0.035(2) 0.010(3) O5 0.0467(18) 0.044(2) 0.0334(15) 0.0018(13) 0.0231(14) 0.0080(15) O6 0.0359(16) 0.0428(19) 0.0384(17) 0.0026(14) 0.0197(14) 0.0057(14) O7 0.139(5) 0.099(5) 0.050(3) -0.020(3) 0.022(3) 0.009(4) O8 0.070(3) 0.068(3) 0.093(4) -0.014(3) 0.017(3) -0.004(2) O9 0.0380(17) 0.046(2) 0.0438(18) -0.0099(15) 0.0248(15) -0.0044(15) O10 0.0361(16) 0.043(2) 0.0463(18) -0.0067(14) 0.0260(14) -0.0052(13) O11 0.053(2) 0.099(4) 0.060(3) 0.007(2) 0.018(2) 0.007(2) O12 0.043(2) 0.070(3) 0.076(3) 0.009(2) 0.018(2) 0.0067(19) O13 0.0488(19) 0.0400(19) 0.0343(16) 0.0030(13) 0.0268(14) 0.0063(14) O14 0.057(2) 0.042(2) 0.0333(16) 0.0051(13) 0.0250(16) 0.0087(16) O15 0.051(2) 0.072(3) 0.063(2) -0.005(2) 0.0390(19) -0.0026(19) O16 0.054(2) 0.124(4) 0.065(3) -0.012(3) 0.043(2) -0.010(2) C1 0.033(2) 0.045(3) 0.037(2) 0.004(2) 0.0138(19) 0.003(2) C2 0.040(2) 0.041(3) 0.046(3) 0.000(2) 0.013(2) -0.001(2) C3 0.042(3) 0.045(3) 0.066(3) -0.008(3) 0.021(2) -0.011(2) C4 0.041(3) 0.045(3) 0.094(4) 0.001(3) 0.026(3) -0.007(2) C5 0.041(3) 0.050(4) 0.149(7) 0.005(4) 0.023(4) -0.005(3) C6 0.047(4) 0.063(5) 0.189(12) 0.015(6) 0.003(6) -0.002(3) C7 0.079(7) 0.100(8) 0.140(10) 0.039(7) -0.036(6) -0.014(5) C8 0.073(5) 0.110(7) 0.094(6) 0.034(6) 0.001(4) -0.008(5) C9 0.049(3) 0.062(4) 0.073(4) 0.012(3) 0.007(3) -0.009(3) C10 0.051(3) 0.065(4) 0.050(3) 0.001(3) 0.017(2) -0.003(3) C11 0.045(3) 0.043(3) 0.074(4) -0.008(3) 0.010(3) -0.002(2) C12 0.199(12) 0.085(6) 0.104(7) -0.023(5) 0.086(8) -0.073(8) C13 0.210(13) 0.121(10) 0.166(11) -0.030(8) 0.149(11) -0.085(10) C14 0.069(5) 0.082(6) 0.147(9) -0.021(6) 0.048(6) -0.025(4) C15 0.079(5) 0.054(4) 0.088(5) 0.002(4) 0.006(4) -0.012(3) C16 0.068(4) 0.054(4) 0.081(5) 0.012(3) -0.003(4) -0.011(3) C17 0.052(3) 0.038(3) 0.073(4) -0.003(3) 0.021(3) 0.002(2) C18 0.035(2) 0.043(3) 0.033(2) 0.0018(19) 0.0155(18) -0.0015(19) C19 0.044(2) 0.046(3) 0.037(2) 0.003(2) 0.019(2) 0.008(2) C20 0.134(7) 0.050(3) 0.047(3) 0.012(3) 0.050(4) 0.029(4) C21 0.158(9) 0.061(4) 0.134(8) 0.046(5) 0.128(8) 0.038(5) C22 0.43(3) 0.111(8) 0.213(14) 0.093(9) 0.290(19) 0.126(13) C23 0.43(4) 0.110(11) 0.31(3) 0.114(14) 0.34(3) 0.131(17) C24 0.34(3) 0.127(14) 0.51(5) 0.10(2) 0.39(4) 0.054(16) C25 0.117(8) 0.081(6) 0.282(18) 0.026(9) 0.121(11) 0.005(6) C26 0.103(6) 0.056(4) 0.137(8) 0.022(5) 0.084(6) 0.012(4) C27 0.061(4) 0.043(3) 0.100(5) 0.016(3) 0.047(4) 0.009(3) C28 0.061(3) 0.055(3) 0.046(3) 0.010(2) 0.029(3) 0.017(3) C29 0.058(4) 0.077(4) 0.065(4) 0.018(3) 0.024(3) 0.020(3) C30 0.081(5) 0.089(5) 0.070(4) 0.028(4) 0.030(4) 0.036(4) C31 0.154(9) 0.076(5) 0.064(5) 0.028(4) 0.043(5) 0.043(6) C32 0.130(7) 0.056(4) 0.076(5) 0.009(3) 0.063(5) -0.011(4) C33 0.124(6) 0.056(4) 0.063(4) 0.006(3) 0.046(4) 0.017(4) C34 0.081(4) 0.042(3) 0.060(3) 0.009(2) 0.044(3) 0.018(3) C35 0.037(2) 0.049(3) 0.034(2) -0.004(2) 0.0196(19) -0.002(2) C36 0.038(2) 0.054(3) 0.062(3) -0.012(3) 0.026(2) -0.008(2) C37 0.036(2) 0.054(3) 0.055(3) -0.006(2) 0.015(2) -0.005(2) C38 0.043(3) 0.046(3) 0.059(3) -0.001(2) 0.027(2) -0.004(2) C39 0.043(3) 0.057(3) 0.098(5) -0.008(3) 0.032(3) 0.002(2) C40 0.058(3) 0.081(5) 0.094(5) 0.007(4) 0.060(4) 0.005(3) C41 0.099(5) 0.071(4) 0.096(5) 0.022(4) 0.075(5) 0.009(4) C42 0.080(4) 0.067(4) 0.065(4) 0.014(3) 0.040(3) -0.001(3) C43 0.051(3) 0.044(3) 0.068(3) 0.003(2) 0.034(3) -0.006(2) C44 0.044(3) 0.048(3) 0.060(3) 0.006(2) 0.016(2) -0.004(2) C45 0.066(4) 0.058(4) 0.131(7) -0.043(4) 0.070(4) -0.024(3) C46 0.134(9) 0.157(10) 0.120(8) -0.076(8) 0.080(7) -0.092(8) C47 0.121(9) 0.132(9) 0.166(12) -0.069(9) 0.078(9) -0.056(8) C48 0.079(6) 0.125(8) 0.132(9) -0.034(7) 0.046(6) -0.041(6) C49 0.122(8) 0.081(7) 0.165(11) -0.015(7) 0.075(8) -0.035(6) C50 0.081(5) 0.070(5) 0.133(8) -0.017(5) 0.065(5) -0.024(4) C51 0.091(5) 0.066(5) 0.113(7) -0.035(5) 0.058(5) -0.028(4) C52 0.037(2) 0.039(3) 0.028(2) -0.0015(18) 0.0134(18) 0.0019(19) C53 0.052(3) 0.041(3) 0.035(2) 0.0050(19) 0.024(2) 0.003(2) C54 0.051(3) 0.043(3) 0.038(2) 0.0079(19) 0.023(2) 0.015(2) C55 0.053(3) 0.043(3) 0.042(2) 0.009(2) 0.029(2) 0.007(2) C56 0.073(3) 0.051(3) 0.044(3) 0.003(2) 0.032(3) 0.011(3) C57 0.088(4) 0.061(4) 0.036(3) 0.002(2) 0.023(3) 0.009(3) C58 0.074(4) 0.065(4) 0.050(3) 0.000(3) 0.014(3) -0.008(3) C59 0.073(4) 0.086(5) 0.053(3) 0.003(3) 0.019(3) 0.003(4) C60 0.057(3) 0.060(3) 0.040(2) 0.006(3) 0.020(2) 0.008(3) C61 0.054(3) 0.070(4) 0.039(2) 0.003(2) 0.026(2) 0.014(3) C62 0.070(4) 0.045(3) 0.044(3) 0.006(2) 0.036(3) 0.011(3) C63 0.093(5) 0.057(4) 0.062(4) 0.012(3) 0.020(4) 0.004(3) C64 0.157(9) 0.069(5) 0.064(5) 0.019(4) 0.052(5) 0.023(6) C65 0.146(8) 0.052(4) 0.095(6) 0.023(4) 0.088(6) 0.019(5) C66 0.105(6) 0.074(5) 0.125(8) 0.021(5) 0.062(6) -0.011(5) C67 0.079(5) 0.093(6) 0.081(5) 0.021(4) 0.021(4) -0.021(4) C68 0.069(3) 0.041(3) 0.053(3) 0.012(2) 0.036(3) 0.010(3) C69 0.055(3) 0.045(3) 0.056(3) 0.001(2) 0.033(3) -0.002(2) C70 0.129(8) 0.069(5) 0.114(7) -0.018(5) 0.082(7) -0.003(5) C71 0.083(4) 0.042(3) 0.057(3) -0.012(3) 0.042(3) -0.002(3) C72 0.159(8) 0.053(4) 0.103(6) -0.011(4) 0.095(6) 0.028(5) _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 2.018(4) . ? Rh1 O9 2.025(3) . ? Rh1 O13 2.033(3) . ? Rh1 O5 2.054(3) . ? Rh1 N5 2.241(4) . ? Rh1 Rh2 2.3985(5) . ? Rh2 O14 2.033(3) . ? Rh2 O2 2.028(4) . ? Rh2 O6 2.035(3) . ? Rh2 O10 2.066(3) . ? Rh2 N6 2.244(4) . ? N1 C3 1.388(7) . ? N1 C10 1.396(7) . ? N1 C2 1.459(7) . ? N2 C20 1.387(7) . ? N2 C19 1.447(6) . ? N2 C27 1.434(9) . ? N3 C44 1.387(7) . ? N3 C37 1.409(7) . ? N3 C36 1.431(6) . ? N4 C61 1.381(7) . ? N4 C54 1.402(6) . ? N4 C53 1.459(6) . ? N5 C69 1.119(7) . ? N6 C71 1.102(7) . ? O1 C1 1.261(6) . ? O2 C1 1.268(6) . ? O3 C3 1.198(8) . ? O4 C10 1.237(7) . ? O5 C18 1.272(6) . ? O6 C18 1.241(6) . ? O7 C20 1.154(10) . ? O8 C27 1.213(9) . ? O9 C35 1.246(6) . ? O10 C35 1.262(6) . ? O11 C37 1.185(7) . ? O12 C44 1.231(7) . ? O13 C52 1.268(6) . ? O14 C52 1.268(6) . ? O15 C54 1.209(6) . ? O16 C61 1.210(6) . ? C1 C2 1.528(7) . ? C2 C11 1.545(8) . ? C3 C4 1.478(9) . ? C4 C9 1.370(10) . ? C4 C5 1.382(9) . ? C5 C6 1.430(14) . ? C6 C7 1.408(16) . ? C7 C8 1.307(16) . ? C8 C9 1.426(10) . ? C9 C10 1.461(9) . ? C11 C17 1.503(9) . ? C12 C17 1.366(11) . ? C12 C13 1.415(14) . ? C13 C14 1.340(15) . ? C14 C15 1.318(13) . ? C15 C16 1.374(10) . ? C16 C17 1.394(10) . ? C18 C19 1.532(7) . ? C19 C28 1.537(8) . ? C20 C21 1.483(13) . ? C21 C26 1.372(14) . ? C21 C22 1.454(10) . ? C22 C23 1.28(3) . ? C23 C24 1.32(4) . ? C24 C25 1.37(2) . ? C25 C26 1.392(13) . ? C26 C27 1.445(10) . ? C28 C34 1.527(8) . ? C29 C30 1.350(9) . ? C29 C34 1.380(10) . ? C30 C31 1.338(13) . ? C31 C32 1.372(13) . ? C32 C33 1.423(10) . ? C33 C34 1.378(10) . ? C35 C36 1.545(7) . ? C36 C45 1.522(9) . ? C37 C38 1.468(8) . ? C38 C43 1.369(8) . ? C38 C39 1.399(7) . ? C39 C40 1.363(10) . ? C40 C41 1.374(11) . ? C41 C42 1.412(10) . ? C42 C43 1.384(8) . ? C43 C44 1.484(7) . ? C45 C51 1.537(10) . ? C46 C51 1.376(14) . ? C46 C47 1.379(14) . ? C47 C48 1.399(16) . ? C48 C49 1.340(15) . ? C49 C50 1.443(13) . ? C50 C51 1.357(12) . ? C52 C53 1.528(7) . ? C53 C62 1.527(7) . ? C54 C55 1.478(8) . ? C55 C56 1.365(7) . ? C55 C60 1.381(7) . ? C56 C57 1.379(9) . ? C57 C58 1.361(10) . ? C58 C59 1.392(9) . ? C59 C60 1.375(9) . ? C60 C61 1.497(7) . ? C62 C68 1.523(7) . ? C63 C68 1.335(9) . ? C63 C64 1.390(11) . ? C64 C65 1.341(14) . ? C65 C66 1.389(14) . ? C66 C67 1.405(11) . ? C67 C68 1.381(10) . ? C69 C70 1.443(10) . ? C71 C72 1.474(8) . ? N7 C73 1.204(14) . ? C73 C74 1.375(14) . ? N8 C75 1.28(2) . ? C75 C76 1.40(2) . ? N9 C77 1.222(19) . ? C77 C78 1.380(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 O9 176.19(14) . . ? O1 Rh1 O13 93.35(15) . . ? O9 Rh1 O13 86.00(15) . . ? O1 Rh1 O5 87.34(15) . . ? O9 Rh1 O5 93.01(15) . . ? O13 Rh1 O5 175.33(13) . . ? O1 Rh1 N5 93.18(14) . . ? O9 Rh1 N5 90.59(14) . . ? O13 Rh1 N5 91.32(14) . . ? O5 Rh1 N5 93.25(14) . . ? O1 Rh1 Rh2 87.87(10) . . ? O9 Rh1 Rh2 88.35(10) . . ? O13 Rh1 Rh2 87.85(9) . . ? O5 Rh1 Rh2 87.56(9) . . ? N5 Rh1 Rh2 178.70(10) . . ? O14 Rh2 O2 92.89(15) . . ? O14 Rh2 O6 176.40(14) . . ? O2 Rh2 O6 87.15(14) . . ? O14 Rh2 O10 87.25(16) . . ? O2 Rh2 O10 175.42(14) . . ? O6 Rh2 O10 92.43(14) . . ? O14 Rh2 N6 90.66(16) . . ? O2 Rh2 N6 92.88(15) . . ? O6 Rh2 N6 92.94(16) . . ? O10 Rh2 N6 91.70(15) . . ? O14 Rh2 Rh1 88.42(10) . . ? O2 Rh2 Rh1 87.98(10) . . ? O6 Rh2 Rh1 87.98(10) . . ? O10 Rh2 Rh1 87.44(9) . . ? N6 Rh2 Rh1 178.77(12) . . ? C3 N1 C10 111.0(5) . . ? C3 N1 C2 122.8(5) . . ? C10 N1 C2 125.7(4) . . ? C20 N2 C19 126.2(6) . . ? C20 N2 C27 110.8(6) . . ? C19 N2 C27 122.6(5) . . ? C44 N3 C37 111.4(4) . . ? C44 N3 C36 125.0(5) . . ? C37 N3 C36 122.4(5) . . ? C61 N4 C54 112.3(4) . . ? C61 N4 C53 124.6(4) . . ? C54 N4 C53 122.9(4) . . ? C69 N5 Rh1 174.4(4) . . ? C71 N6 Rh2 172.3(5) . . ? C1 O1 Rh1 118.3(3) . . ? C1 O2 Rh2 118.0(3) . . ? C18 O5 Rh1 118.1(3) . . ? C18 O6 Rh2 119.1(3) . . ? C35 O9 Rh1 118.6(3) . . ? C35 O10 Rh2 117.3(3) . . ? C52 O13 Rh1 118.1(3) . . ? C52 O14 Rh2 117.3(3) . . ? O2 C1 O1 126.5(5) . . ? O2 C1 C2 117.6(5) . . ? O1 C1 C2 115.9(4) . . ? N1 C2 C1 112.0(4) . . ? N1 C2 C11 112.3(4) . . ? C1 C2 C11 112.8(5) . . ? O3 C3 N1 125.5(6) . . ? O3 C3 C4 128.8(6) . . ? N1 C3 C4 105.7(5) . . ? C9 C4 C5 121.9(7) . . ? C9 C4 C3 108.6(5) . . ? C5 C4 C3 129.4(7) . . ? C4 C5 C6 114.8(9) . . ? C7 C6 C5 121.7(8) . . ? C8 C7 C6 122.0(9) . . ? C7 C8 C9 117.3(10) . . ? C4 C9 C8 122.0(7) . . ? C4 C9 C10 108.0(5) . . ? C8 C9 C10 129.9(7) . . ? O4 C10 N1 124.1(6) . . ? O4 C10 C9 129.2(6) . . ? N1 C10 C9 106.6(5) . . ? C17 C11 C2 113.6(5) . . ? C17 C12 C13 119.3(9) . . ? C14 C13 C12 120.2(9) . . ? C15 C14 C13 122.5(8) . . ? C14 C15 C16 117.7(9) . . ? C15 C16 C17 123.6(8) . . ? C12 C17 C16 116.4(7) . . ? C12 C17 C11 122.8(7) . . ? C16 C17 C11 120.7(7) . . ? O6 C18 O5 126.5(5) . . ? O6 C18 C19 117.1(4) . . ? O5 C18 C19 116.3(4) . . ? N2 C19 C18 112.5(4) . . ? N2 C19 C28 110.4(5) . . ? C18 C19 C28 112.9(4) . . ? O7 C20 N2 124.0(8) . . ? O7 C20 C21 131.8(7) . . ? N2 C20 C21 104.2(8) . . ? C26 C21 C22 122.0(12) . . ? C26 C21 C20 111.1(6) . . ? C22 C21 C20 126.7(13) . . ? C23 C22 C21 118.2(19) . . ? C22 C23 C24 120.3(13) . . ? C23 C24 C25 126(2) . . ? C26 C25 C24 117.5(19) . . ? C25 C26 C21 116.3(11) . . ? C25 C26 C27 136.9(13) . . ? C21 C26 C27 106.7(7) . . ? O8 C27 N2 125.1(6) . . ? O8 C27 C26 127.7(8) . . ? N2 C27 C26 107.2(7) . . ? C34 C28 C19 110.9(5) . . ? C30 C29 C34 121.6(7) . . ? C29 C30 C31 121.3(8) . . ? C32 C31 C30 120.4(7) . . ? C31 C32 C33 118.9(8) . . ? C34 C33 C32 119.6(8) . . ? C33 C34 C29 118.1(6) . . ? C33 C34 C28 119.8(7) . . ? C29 C34 C28 122.0(6) . . ? O9 C35 O10 127.8(5) . . ? O9 C35 C36 115.3(4) . . ? O10 C35 C36 116.9(4) . . ? N3 C36 C45 111.9(5) . . ? N3 C36 C35 112.3(4) . . ? C45 C36 C35 113.2(5) . . ? O11 C37 N3 124.0(5) . . ? O11 C37 C38 130.7(5) . . ? N3 C37 C38 105.2(5) . . ? C43 C38 C39 121.5(6) . . ? C43 C38 C37 109.4(5) . . ? C39 C38 C37 129.0(6) . . ? C40 C39 C38 118.0(6) . . ? C39 C40 C41 120.2(6) . . ? C40 C41 C42 123.0(6) . . ? C43 C42 C41 115.3(7) . . ? C38 C43 C42 121.8(5) . . ? C38 C43 C44 107.8(5) . . ? C42 C43 C44 130.3(6) . . ? O12 C44 N3 124.4(5) . . ? O12 C44 C43 129.6(6) . . ? N3 C44 C43 106.0(4) . . ? C51 C45 C36 110.6(6) . . ? C51 C46 C47 118.4(11) . . ? C46 C47 C48 123.0(12) . . ? C49 C48 C47 116.6(10) . . ? C48 C49 C50 122.6(11) . . ? C51 C50 C49 117.5(10) . . ? C50 C51 C46 121.7(8) . . ? C50 C51 C45 120.5(9) . . ? C46 C51 C45 117.8(8) . . ? O13 C52 O14 127.4(5) . . ? O13 C52 C53 117.0(4) . . ? O14 C52 C53 115.4(4) . . ? N4 C53 C52 110.8(4) . . ? N4 C53 C62 112.1(4) . . ? C52 C53 C62 112.6(4) . . ? O15 C54 N4 124.2(5) . . ? O15 C54 C55 130.4(4) . . ? N4 C54 C55 105.4(4) . . ? C56 C55 C60 120.4(5) . . ? C56 C55 C54 130.9(5) . . ? C60 C55 C54 108.6(4) . . ? C55 C56 C57 118.1(5) . . ? C58 C57 C56 121.7(5) . . ? C57 C58 C59 120.8(6) . . ? C60 C59 C58 117.0(6) . . ? C59 C60 C55 121.9(5) . . ? C59 C60 C61 130.2(5) . . ? C55 C60 C61 107.8(5) . . ? O16 C61 N4 124.3(5) . . ? O16 C61 C60 130.1(6) . . ? N4 C61 C60 105.5(4) . . ? C68 C62 C53 113.3(4) . . ? C68 C63 C64 122.1(8) . . ? C65 C64 C63 120.0(9) . . ? C64 C65 C66 120.9(7) . . ? C67 C66 C65 117.0(9) . . ? C68 C67 C66 122.1(8) . . ? C63 C68 C67 117.8(6) . . ? C63 C68 C62 124.3(6) . . ? C67 C68 C62 117.9(6) . . ? N5 C69 C70 176.9(7) . . ? N6 C71 C72 176.7(8) . . ? N7 C73 C74 167.1(15) . . ? N8 C75 C76 126(3) . . ? N9 C77 C78 134(3) . . ? 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 O1 Rh1 Rh2 O14 88.29(15) . . . . ? O9 Rh1 Rh2 O14 -91.20(16) . . . . ? O13 Rh1 Rh2 O14 -5.14(15) . . . . ? O5 Rh1 Rh2 O14 175.72(17) . . . . ? N5 Rh1 Rh2 O14 -56(5) . . . . ? O1 Rh1 Rh2 O2 -4.65(14) . . . . ? O9 Rh1 Rh2 O2 175.85(16) . . . . ? O13 Rh1 Rh2 O2 -98.09(14) . . . . ? O5 Rh1 Rh2 O2 82.77(14) . . . . ? N5 Rh1 Rh2 O2 -149(5) . . . . ? O1 Rh1 Rh2 O6 -91.87(15) . . . . ? O9 Rh1 Rh2 O6 88.64(14) . . . . ? O13 Rh1 Rh2 O6 174.70(15) . . . . ? O5 Rh1 Rh2 O6 -4.44(14) . . . . ? N5 Rh1 Rh2 O6 124(5) . . . . ? O1 Rh1 Rh2 O10 175.60(16) . . . . ? O9 Rh1 Rh2 O10 -3.89(14) . . . . ? O13 Rh1 Rh2 O10 82.17(15) . . . . ? O5 Rh1 Rh2 O10 -96.97(14) . . . . ? N5 Rh1 Rh2 O10 31(5) . . . . ? O1 Rh1 Rh2 N6 130(6) . . . . ? O9 Rh1 Rh2 N6 -49(6) . . . . ? O13 Rh1 Rh2 N6 37(6) . . . . ? O5 Rh1 Rh2 N6 -143(6) . . . . ? N5 Rh1 Rh2 N6 -14(7) . . . . ? O1 Rh1 N5 C69 17(5) . . . . ? O9 Rh1 N5 C69 -163(5) . . . . ? O13 Rh1 N5 C69 111(5) . . . . ? O5 Rh1 N5 C69 -70(5) . . . . ? Rh2 Rh1 N5 C69 161(4) . . . . ? O14 Rh2 N6 C71 -45(4) . . . . ? O2 Rh2 N6 C71 48(4) . . . . ? O6 Rh2 N6 C71 135(4) . . . . ? O10 Rh2 N6 C71 -132(4) . . . . ? Rh1 Rh2 N6 C71 -86(7) . . . . ? O9 Rh1 O1 C1 18(3) . . . . ? O13 Rh1 O1 C1 98.4(4) . . . . ? O5 Rh1 O1 C1 -76.9(3) . . . . ? N5 Rh1 O1 C1 -170.1(3) . . . . ? Rh2 Rh1 O1 C1 10.7(3) . . . . ? O14 Rh2 O2 C1 -88.2(4) . . . . ? O6 Rh2 O2 C1 88.2(4) . . . . ? O10 Rh2 O2 C1 3(2) . . . . ? N6 Rh2 O2 C1 -179.0(4) . . . . ? Rh1 Rh2 O2 C1 0.2(3) . . . . ? O1 Rh1 O5 C18 90.2(4) . . . . ? O9 Rh1 O5 C18 -86.0(4) . . . . ? O13 Rh1 O5 C18 -8(2) . . . . ? N5 Rh1 O5 C18 -176.8(4) . . . . ? Rh2 Rh1 O5 C18 2.2(3) . . . . ? O14 Rh2 O6 C18 11(3) . . . . ? O2 Rh2 O6 C18 -79.7(4) . . . . ? O10 Rh2 O6 C18 95.8(4) . . . . ? N6 Rh2 O6 C18 -172.4(4) . . . . ? Rh1 Rh2 O6 C18 8.4(4) . . . . ? O1 Rh1 O9 C35 0(3) . . . . ? O13 Rh1 O9 C35 -80.7(4) . . . . ? O5 Rh1 O9 C35 94.7(4) . . . . ? N5 Rh1 O9 C35 -172.0(4) . . . . ? Rh2 Rh1 O9 C35 7.3(4) . . . . ? O14 Rh2 O10 C35 90.5(4) . . . . ? O2 Rh2 O10 C35 -1(2) . . . . ? O6 Rh2 O10 C35 -86.0(4) . . . . ? N6 Rh2 O10 C35 -179.0(4) . . . . ? Rh1 Rh2 O10 C35 1.9(3) . . . . ? O1 Rh1 O13 C52 -85.1(4) . . . . ? O9 Rh1 O13 C52 91.1(4) . . . . ? O5 Rh1 O13 C52 13(2) . . . . ? N5 Rh1 O13 C52 -178.4(4) . . . . ? Rh2 Rh1 O13 C52 2.6(3) . . . . ? O2 Rh2 O14 C52 97.1(4) . . . . ? O6 Rh2 O14 C52 7(3) . . . . ? O10 Rh2 O14 C52 -78.3(4) . . . . ? N6 Rh2 O14 C52 -170.0(4) . . . . ? Rh1 Rh2 O14 C52 9.2(3) . . . . ? Rh2 O2 C1 O1 8.9(7) . . . . ? Rh2 O2 C1 C2 -169.5(3) . . . . ? Rh1 O1 C1 O2 -14.6(7) . . . . ? Rh1 O1 C1 C2 163.9(3) . . . . ? C3 N1 C2 C1 -113.4(5) . . . . ? C10 N1 C2 C1 75.9(6) . . . . ? C3 N1 C2 C11 118.5(6) . . . . ? C10 N1 C2 C11 -52.2(7) . . . . ? O2 C1 C2 N1 -125.3(5) . . . . ? O1 C1 C2 N1 56.1(6) . . . . ? O2 C1 C2 C11 2.5(7) . . . . ? O1 C1 C2 C11 -176.1(5) . . . . ? C10 N1 C3 O3 179.0(6) . . . . ? C2 N1 C3 O3 7.0(9) . . . . ? C10 N1 C3 C4 -1.5(6) . . . . ? C2 N1 C3 C4 -173.4(4) . . . . ? O3 C3 C4 C9 -178.2(6) . . . . ? N1 C3 C4 C9 2.3(6) . . . . ? O3 C3 C4 C5 -0.4(10) . . . . ? N1 C3 C4 C5 -179.9(6) . . . . ? C9 C4 C5 C6 -3.5(9) . . . . ? C3 C4 C5 C6 179.0(6) . . . . ? C4 C5 C6 C7 5.1(12) . . . . ? C5 C6 C7 C8 -5.7(16) . . . . ? C6 C7 C8 C9 4.0(16) . . . . ? C5 C4 C9 C8 2.3(10) . . . . ? C3 C4 C9 C8 -179.8(7) . . . . ? C5 C4 C9 C10 179.8(6) . . . . ? C3 C4 C9 C10 -2.3(7) . . . . ? C7 C8 C9 C4 -2.4(13) . . . . ? C7 C8 C9 C10 -179.3(8) . . . . ? C3 N1 C10 O4 -177.9(6) . . . . ? C2 N1 C10 O4 -6.2(10) . . . . ? C3 N1 C10 C9 0.1(7) . . . . ? C2 N1 C10 C9 171.8(5) . . . . ? C4 C9 C10 O4 179.3(7) . . . . ? C8 C9 C10 O4 -3.5(13) . . . . ? C4 C9 C10 N1 1.4(7) . . . . ? C8 C9 C10 N1 178.6(8) . . . . ? N1 C2 C11 C17 -52.3(7) . . . . ? C1 C2 C11 C17 -180.0(5) . . . . ? C17 C12 C13 C14 -4(2) . . . . ? C12 C13 C14 C15 5(2) . . . . ? C13 C14 C15 C16 -5.0(17) . . . . ? C14 C15 C16 C17 4.3(12) . . . . ? C13 C12 C17 C16 2.7(16) . . . . ? C13 C12 C17 C11 -178.0(11) . . . . ? C15 C16 C17 C12 -3.2(12) . . . . ? C15 C16 C17 C11 177.6(7) . . . . ? C2 C11 C17 C12 -48.6(11) . . . . ? C2 C11 C17 C16 130.6(6) . . . . ? Rh2 O6 C18 O5 -9.6(7) . . . . ? Rh2 O6 C18 C19 172.9(3) . . . . ? Rh1 O5 C18 O6 4.1(7) . . . . ? Rh1 O5 C18 C19 -178.3(3) . . . . ? C20 N2 C19 C18 -124.5(6) . . . . ? C27 N2 C19 C18 63.2(6) . . . . ? C20 N2 C19 C28 108.4(6) . . . . ? C27 N2 C19 C28 -64.0(6) . . . . ? O6 C18 C19 N2 -143.8(5) . . . . ? O5 C18 C19 N2 38.4(6) . . . . ? O6 C18 C19 C28 -18.0(7) . . . . ? O5 C18 C19 C28 164.3(5) . . . . ? C19 N2 C20 O7 5.0(10) . . . . ? C27 N2 C20 O7 178.1(7) . . . . ? C19 N2 C20 C21 -173.2(5) . . . . ? C27 N2 C20 C21 -0.1(6) . . . . ? O7 C20 C21 C26 -177.5(8) . . . . ? N2 C20 C21 C26 0.5(8) . . . . ? O7 C20 C21 C22 6.5(13) . . . . ? N2 C20 C21 C22 -175.6(7) . . . . ? C26 C21 C22 C23 2.3(15) . . . . ? C20 C21 C22 C23 178.0(10) . . . . ? C21 C22 C23 C24 -3(2) . . . . ? C22 C23 C24 C25 3(3) . . . . ? C23 C24 C25 C26 -2(3) . . . . ? C24 C25 C26 C21 1.3(16) . . . . ? C24 C25 C26 C27 -174.5(12) . . . . ? C22 C21 C26 C25 -1.4(12) . . . . ? C20 C21 C26 C25 -177.6(7) . . . . ? C22 C21 C26 C27 175.6(7) . . . . ? C20 C21 C26 C27 -0.7(8) . . . . ? C20 N2 C27 O8 179.4(6) . . . . ? C19 N2 C27 O8 -7.3(9) . . . . ? C20 N2 C27 C26 -0.2(7) . . . . ? C19 N2 C27 C26 173.1(5) . . . . ? C25 C26 C27 O8 -3.0(15) . . . . ? C21 C26 C27 O8 -179.0(7) . . . . ? C25 C26 C27 N2 176.6(10) . . . . ? C21 C26 C27 N2 0.5(7) . . . . ? N2 C19 C28 C34 -56.9(7) . . . . ? C18 C19 C28 C34 176.1(5) . . . . ? C34 C29 C30 C31 0.7(11) . . . . ? C29 C30 C31 C32 -3.3(13) . . . . ? C30 C31 C32 C33 3.1(13) . . . . ? C31 C32 C33 C34 -0.4(11) . . . . ? C32 C33 C34 C29 -2.0(10) . . . . ? C32 C33 C34 C28 -178.7(6) . . . . ? C30 C29 C34 C33 2.0(10) . . . . ? C30 C29 C34 C28 178.5(6) . . . . ? C19 C28 C34 C33 108.4(7) . . . . ? C19 C28 C34 C29 -68.1(7) . . . . ? Rh1 O9 C35 O10 -8.4(7) . . . . ? Rh1 O9 C35 C36 172.8(3) . . . . ? Rh2 O10 C35 O9 3.6(7) . . . . ? Rh2 O10 C35 C36 -177.6(4) . . . . ? C44 N3 C36 C45 -61.5(7) . . . . ? C37 N3 C36 C45 105.2(7) . . . . ? C44 N3 C36 C35 67.1(7) . . . . ? C37 N3 C36 C35 -126.2(6) . . . . ? O9 C35 C36 N3 -159.3(5) . . . . ? O10 C35 C36 N3 21.8(7) . . . . ? O9 C35 C36 C45 -31.4(8) . . . . ? O10 C35 C36 C45 149.7(6) . . . . ? C44 N3 C37 O11 174.6(6) . . . . ? C36 N3 C37 O11 6.2(9) . . . . ? C44 N3 C37 C38 -4.1(6) . . . . ? C36 N3 C37 C38 -172.4(5) . . . . ? O11 C37 C38 C43 -176.3(7) . . . . ? N3 C37 C38 C43 2.2(6) . . . . ? O11 C37 C38 C39 7.0(11) . . . . ? N3 C37 C38 C39 -174.4(6) . . . . ? C43 C38 C39 C40 0.4(9) . . . . ? C37 C38 C39 C40 176.7(6) . . . . ? C38 C39 C40 C41 1.6(10) . . . . ? C39 C40 C41 C42 -4.3(12) . . . . ? C40 C41 C42 C43 4.7(11) . . . . ? C39 C38 C43 C42 0.3(9) . . . . ? C37 C38 C43 C42 -176.7(6) . . . . ? C39 C38 C43 C44 177.2(5) . . . . ? C37 C38 C43 C44 0.2(6) . . . . ? C41 C42 C43 C38 -2.7(9) . . . . ? C41 C42 C43 C44 -178.8(6) . . . . ? C37 N3 C44 O12 -177.6(6) . . . . ? C36 N3 C44 O12 -9.6(9) . . . . ? C37 N3 C44 C43 4.2(6) . . . . ? C36 N3 C44 C43 172.2(5) . . . . ? C38 C43 C44 O12 179.3(6) . . . . ? C42 C43 C44 O12 -4.2(11) . . . . ? C38 C43 C44 N3 -2.7(6) . . . . ? C42 C43 C44 N3 173.9(6) . . . . ? N3 C36 C45 C51 -47.5(9) . . . . ? C35 C36 C45 C51 -175.6(6) . . . . ? C51 C46 C47 C48 -2(2) . . . . ? C46 C47 C48 C49 1(2) . . . . ? C47 C48 C49 C50 1.5(19) . . . . ? C48 C49 C50 C51 -3.7(18) . . . . ? C49 C50 C51 C46 3.3(15) . . . . ? C49 C50 C51 C45 -175.1(8) . . . . ? C47 C46 C51 C50 -0.8(17) . . . . ? C47 C46 C51 C45 177.6(10) . . . . ? C36 C45 C51 C50 93.9(10) . . . . ? C36 C45 C51 C46 -84.5(10) . . . . ? Rh1 O13 C52 O14 4.4(7) . . . . ? Rh1 O13 C52 C53 -169.8(3) . . . . ? Rh2 O14 C52 O13 -10.5(7) . . . . ? Rh2 O14 C52 C53 163.8(3) . . . . ? C61 N4 C53 C52 62.7(6) . . . . ? C54 N4 C53 C52 -112.2(5) . . . . ? C61 N4 C53 C62 -64.1(6) . . . . ? C54 N4 C53 C62 121.0(5) . . . . ? O13 C52 C53 N4 -136.1(4) . . . . ? O14 C52 C53 N4 49.0(6) . . . . ? O13 C52 C53 C62 -9.6(7) . . . . ? O14 C52 C53 C62 175.5(5) . . . . ? C61 N4 C54 O15 -176.3(5) . . . . ? C53 N4 C54 O15 -0.9(8) . . . . ? C61 N4 C54 C55 4.8(6) . . . . ? C53 N4 C54 C55 -179.8(4) . . . . ? O15 C54 C55 C56 -1.7(10) . . . . ? N4 C54 C55 C56 177.1(5) . . . . ? O15 C54 C55 C60 178.9(6) . . . . ? N4 C54 C55 C60 -2.3(6) . . . . ? C60 C55 C56 C57 0.8(8) . . . . ? C54 C55 C56 C57 -178.5(5) . . . . ? C55 C56 C57 C58 -1.7(9) . . . . ? C56 C57 C58 C59 0.0(10) . . . . ? C57 C58 C59 C60 2.6(10) . . . . ? C58 C59 C60 C55 -3.5(10) . . . . ? C58 C59 C60 C61 179.0(6) . . . . ? C56 C55 C60 C59 1.9(9) . . . . ? C54 C55 C60 C59 -178.6(6) . . . . ? C56 C55 C60 C61 179.8(5) . . . . ? C54 C55 C60 C61 -0.7(6) . . . . ? C54 N4 C61 O16 176.9(6) . . . . ? C53 N4 C61 O16 1.6(9) . . . . ? C54 N4 C61 C60 -5.2(6) . . . . ? C53 N4 C61 C60 179.5(5) . . . . ? C59 C60 C61 O16 -1.1(12) . . . . ? C55 C60 C61 O16 -178.8(7) . . . . ? C59 C60 C61 N4 -178.8(7) . . . . ? C55 C60 C61 N4 3.5(6) . . . . ? N4 C53 C62 C68 -69.1(6) . . . . ? C52 C53 C62 C68 165.1(5) . . . . ? C68 C63 C64 C65 0.8(13) . . . . ? C63 C64 C65 C66 -2.3(13) . . . . ? C64 C65 C66 C67 2.9(13) . . . . ? C65 C66 C67 C68 -2.1(14) . . . . ? C64 C63 C68 C67 0.0(11) . . . . ? C64 C63 C68 C62 179.3(7) . . . . ? C66 C67 C68 C63 0.7(12) . . . . ? C66 C67 C68 C62 -178.6(7) . . . . ? C53 C62 C68 C63 90.7(8) . . . . ? C53 C62 C68 C67 -90.0(7) . . . . ? Rh1 N5 C69 C70 6(18) . . . . ? Rh2 N6 C71 C72 135(12) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.198 _refine_diff_density_min -0.557 _refine_diff_density_rms 0.088