# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_d:\xray\yong029\1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H40 B2 F12 N14 Rh2' _chemical_formula_weight 1388.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.764(3) _cell_length_b 13.196(3) _cell_length_c 20.352(4) _cell_angle_alpha 83.78(3) _cell_angle_beta 72.12(3) _cell_angle_gamma 66.51(3) _cell_volume 2991.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1388 _exptl_absorpt_coefficient_mu 0.640 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9329 _exptl_absorpt_correction_T_max 0.9626 _exptl_absorpt_process_details 'SADABS, V2.3, Bruker(2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 32441 _diffrn_reflns_av_R_equivalents 0.0368 _diffrn_reflns_av_sigmaI/netI 0.0529 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.84 _reflns_number_total 12655 _reflns_number_gt 9312 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12655 _refine_ls_number_parameters 833 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0398 _refine_ls_wR_factor_ref 0.1116 _refine_ls_wR_factor_gt 0.1043 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _refine_ls_shift/su_max 0.064 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.33955(2) 0.27188(2) 0.300649(13) 0.01951(8) Uani 1 1 d . . . Rh2 Rh 0.48959(2) 0.36596(2) 0.244720(13) 0.02070(8) Uani 1 1 d . . . N13 N 0.2124(2) 0.1875(2) 0.34260(14) 0.0249(6) Uani 1 1 d . . . N14 N 0.6192(2) 0.4419(2) 0.19493(14) 0.0256(6) Uani 1 1 d . . . N5 N 0.2179(2) 0.3686(2) 0.25144(13) 0.0211(6) Uani 1 1 d . . . N6 N 0.3900(2) 0.1717(2) 0.21672(13) 0.0211(6) Uani 1 1 d . . . N8 N 0.5948(2) 0.2435(2) 0.17179(14) 0.0234(6) Uani 1 1 d . . . N2 N 0.4646(2) 0.1726(2) 0.34824(14) 0.0228(6) Uani 1 1 d . . . F10 F 0.0010(2) 0.31983(19) 0.63646(11) 0.0445(6) Uani 1 1 d . . . N7 N 0.4168(2) 0.4338(2) 0.16540(14) 0.0226(6) Uani 1 1 d . . . N4 N 0.2772(2) 0.3839(2) 0.37927(13) 0.0222(6) Uani 1 1 d . . . F9 F 0.3690(2) 0.91657(18) 0.29886(12) 0.0505(6) Uani 1 1 d . . . N3 N 0.3789(2) 0.4905(2) 0.31648(14) 0.0233(6) Uani 1 1 d . . . N1 N 0.5712(2) 0.2858(2) 0.31745(15) 0.0252(6) Uani 1 1 d . . . C45 C 0.2277(3) 0.3233(3) 0.19212(16) 0.0200(7) Uani 1 1 d . . . C44 C 0.1511(3) 0.3754(3) 0.15123(17) 0.0229(7) Uani 1 1 d . . . N9 N 0.0948(2) 0.3727(2) 0.04922(14) 0.0277(6) Uani 1 1 d . . . C50 C 0.3390(3) 0.1620(3) 0.11276(16) 0.0229(7) Uani 1 1 d . . . F12 F 0.4681(3) -0.2177(2) 0.48041(14) 0.0640(8) Uani 1 1 d . . . C46 C 0.3222(3) 0.2159(3) 0.17273(16) 0.0197(7) Uani 1 1 d . . . C32 C 0.4708(3) 0.3685(3) 0.10718(16) 0.0222(7) Uani 1 1 d . . . C27 C 0.6874(3) 0.1509(3) 0.17556(19) 0.0289(8) Uani 1 1 d . . . H27 H 0.7087 0.1355 0.2175 0.035 Uiso 1 1 calc R . . N10 N 0.2840(3) 0.1657(2) 0.00950(15) 0.0320(7) Uani 1 1 d . . . C31 C 0.5682(3) 0.2654(3) 0.11040(17) 0.0236(7) Uani 1 1 d . . . C7 C 0.3039(3) 0.4711(3) 0.37131(17) 0.0227(7) Uani 1 1 d . . . H7 H 0.2660 0.5242 0.4079 0.027 Uiso 1 1 calc R . . C52 C 0.1694(3) 0.3208(3) 0.08830(17) 0.0235(7) Uani 1 1 d . . . C34 C 0.2921(3) 0.5689(3) 0.10451(18) 0.0290(8) Uani 1 1 d . . . H34 H 0.2306 0.6397 0.1048 0.035 Uiso 1 1 calc R . . N11 N 0.4625(3) 0.3528(3) -0.07003(15) 0.0373(8) Uani 1 1 d . . . C8 C 0.2057(3) 0.3686(3) 0.44656(17) 0.0222(7) Uani 1 1 d . . . C37 C 0.4980(3) 0.3236(3) -0.01213(18) 0.0301(8) Uani 1 1 d . . . C51 C 0.2625(3) 0.2171(3) 0.06880(17) 0.0246(7) Uani 1 1 d . . . C13 C 0.0966(3) 0.3624(3) 0.45351(18) 0.0252(7) Uani 1 1 d . . . H13 H 0.0691 0.3704 0.4141 0.030 Uiso 1 1 calc R . . N12 N 0.6550(3) 0.1544(3) -0.06368(16) 0.0370(8) Uani 1 1 d . . . C20 C 0.5476(3) 0.2048(3) 0.35263(17) 0.0265(7) Uani 1 1 d . . . H20 H 0.5931 0.1667 0.3833 0.032 Uiso 1 1 calc R . . C49 C 0.4273(3) 0.0553(3) 0.09947(18) 0.0276(8) Uani 1 1 d . . . H49 H 0.4416 0.0152 0.0594 0.033 Uiso 1 1 calc R . . C48 C 0.4931(3) 0.0095(3) 0.14502(17) 0.0266(7) Uani 1 1 d . . . H48 H 0.5524 -0.0634 0.1372 0.032 Uiso 1 1 calc R . . C43 C 0.0595(3) 0.4782(3) 0.17447(17) 0.0263(7) Uani 1 1 d . . . H43 H 0.0057 0.5165 0.1482 0.032 Uiso 1 1 calc R . . C47 C 0.4729(3) 0.0699(3) 0.20274(17) 0.0241(7) Uani 1 1 d . . . H47 H 0.5201 0.0372 0.2334 0.029 Uiso 1 1 calc R . . C30 C 0.6302(3) 0.1934(3) 0.05388(18) 0.0269(8) Uani 1 1 d . . . C53 C 0.1145(3) 0.3190(3) -0.00746(18) 0.0325(8) Uani 1 1 d . . . H53 H 0.0627 0.3512 -0.0356 0.039 Uiso 1 1 calc R . . C22 C 0.5632(3) -0.0251(3) 0.36194(18) 0.0314(8) Uani 1 1 d . . . H22 H 0.6302 -0.0249 0.3250 0.038 Uiso 1 1 calc R . . C41 C 0.1289(3) 0.4661(3) 0.27267(17) 0.0244(7) Uani 1 1 d . . . H41 H 0.1205 0.4977 0.3147 0.029 Uiso 1 1 calc R . . C33 C 0.3305(3) 0.5317(3) 0.16272(17) 0.0242(7) Uani 1 1 d . . . H33 H 0.2934 0.5783 0.2026 0.029 Uiso 1 1 calc R . . C54 C 0.2086(3) 0.2168(3) -0.0275(2) 0.0381(9) Uani 1 1 d . . . H54 H 0.2190 0.1827 -0.0690 0.046 Uiso 1 1 calc R . . C5 C 0.2747(3) 0.6892(3) 0.31154(18) 0.0319(8) Uani 1 1 d . . . H5 H 0.2051 0.6771 0.3141 0.038 Uiso 1 1 calc R . . C9 C 0.2430(3) 0.3611(3) 0.50434(17) 0.0278(8) Uani 1 1 d . . . H9 H 0.3175 0.3653 0.4998 0.033 Uiso 1 1 calc R . . C21 C 0.4639(3) 0.0725(3) 0.38249(17) 0.0268(8) Uani 1 1 d . . . C56 C 0.6917(3) 0.4687(3) 0.1626(2) 0.0335(8) Uani 1 1 d . . . C35 C 0.3439(3) 0.5024(3) 0.04628(18) 0.0287(8) Uani 1 1 d . . . H35 H 0.3176 0.5259 0.0063 0.034 Uiso 1 1 calc R . . C29 C 0.7252(3) 0.0960(3) 0.0600(2) 0.0344(9) Uani 1 1 d . . . H29 H 0.7690 0.0446 0.0225 0.041 Uiso 1 1 calc R . . C42 C 0.0480(3) 0.5232(3) 0.23540(18) 0.0289(8) Uani 1 1 d . . . H42 H -0.0143 0.5924 0.2519 0.035 Uiso 1 1 calc R . . C36 C 0.4355(3) 0.4000(3) 0.04705(17) 0.0254(7) Uani 1 1 d . . . C11 C 0.0685(3) 0.3372(3) 0.57302(18) 0.0313(8) Uani 1 1 d . . . C4 C 0.3788(3) 0.6000(3) 0.31172(17) 0.0249(7) Uani 1 1 d . . . F11 F 0.8831(3) 0.4108(2) 0.39422(19) 0.0871(11) Uani 1 1 d . . . C3 C 0.4802(3) 0.6185(3) 0.30832(18) 0.0301(8) Uani 1 1 d . . . H3 H 0.5521 0.5578 0.3089 0.036 Uiso 1 1 calc R . . C2 C 0.4768(4) 0.7254(3) 0.30408(19) 0.0357(9) Uani 1 1 d . . . H2 H 0.5461 0.7386 0.3011 0.043 Uiso 1 1 calc R . . C28 C 0.7540(3) 0.0761(3) 0.1208(2) 0.0359(9) Uani 1 1 d . . . H28 H 0.8195 0.0112 0.1256 0.043 Uiso 1 1 calc R . . C12 C 0.0283(3) 0.3448(3) 0.51688(19) 0.0321(8) Uani 1 1 d . . . H12A H -0.0450 0.3381 0.5217 0.038 Uiso 1 1 calc R . . C38 C 0.5938(3) 0.2241(3) -0.00895(18) 0.0300(8) Uani 1 1 d . . . C26 C 0.3668(3) 0.0714(3) 0.43735(18) 0.0329(8) Uani 1 1 d . . . H26 H 0.2990 0.1380 0.4521 0.039 Uiso 1 1 calc R . . C10 C 0.1731(3) 0.3475(3) 0.56856(18) 0.0313(8) Uani 1 1 d . . . H10 H 0.1969 0.3453 0.6088 0.038 Uiso 1 1 calc R . . C17 C 0.6517(3) 0.3201(3) 0.33723(19) 0.0292(8) Uani 1 1 d . . . C16 C 0.6179(4) 0.3665(3) 0.4016(2) 0.0400(9) Uani 1 1 d . . . H16 H 0.5413 0.3774 0.4326 0.048 Uiso 1 1 calc R . . C55 C 0.7868(4) 0.5053(4) 0.1236(2) 0.0556(13) Uani 1 1 d . . . H55A H 0.7813 0.5687 0.1475 0.083 Uiso 1 1 calc R . . H55B H 0.7786 0.5270 0.0773 0.083 Uiso 1 1 calc R . . H55C H 0.8644 0.4448 0.1199 0.083 Uiso 1 1 calc R . . C58 C 0.1475(3) 0.1477(3) 0.3517(2) 0.0383(9) Uani 1 1 d . . . C57 C 0.0614(4) 0.0947(4) 0.3660(3) 0.0801(19) Uani 1 1 d . . . H57A H 0.0867 0.0287 0.3937 0.120 Uiso 1 1 calc R . . H57B H 0.0577 0.0734 0.3224 0.120 Uiso 1 1 calc R . . H57C H -0.0176 0.1465 0.3916 0.120 Uiso 1 1 calc R . . C6 C 0.2704(4) 0.7969(3) 0.3076(2) 0.0369(9) Uani 1 1 d . . . H6 H 0.1989 0.8583 0.3072 0.044 Uiso 1 1 calc R . . C40 C 0.5244(4) 0.2831(4) -0.1230(2) 0.0445(10) Uani 1 1 d . . . H40 H 0.5027 0.3003 -0.1647 0.053 Uiso 1 1 calc R . . C1 C 0.3722(4) 0.8111(3) 0.30426(19) 0.0369(9) Uani 1 1 d . . . C18 C 0.7619(3) 0.3057(3) 0.2917(2) 0.0379(9) Uani 1 1 d . . . H18 H 0.7841 0.2740 0.2473 0.046 Uiso 1 1 calc R . . C24 C 0.4677(4) -0.1213(3) 0.4482(2) 0.0438(11) Uani 1 1 d . . . C25 C 0.3688(4) -0.0267(3) 0.4705(2) 0.0441(10) Uani 1 1 d . . . H63 H 0.3029 -0.0281 0.5079 0.053 Uiso 1 1 calc R . . C39 C 0.6201(4) 0.1853(3) -0.1199(2) 0.0420(10) Uani 1 1 d . . . H39 H 0.6621 0.1390 -0.1599 0.050 Uiso 1 1 calc R . . C19 C 0.8403(4) 0.3371(4) 0.3102(3) 0.0510(12) Uani 1 1 d . . . H19 H 0.9161 0.3279 0.2789 0.061 Uiso 1 1 calc R . . C14 C 0.8060(4) 0.3814(4) 0.3743(3) 0.0563(13) Uani 1 1 d . . . C15 C 0.6974(4) 0.3973(4) 0.4210(3) 0.0526(12) Uani 1 1 d . . . H15 H 0.6764 0.4285 0.4654 0.063 Uiso 1 1 calc R . . B1 B 0.7918(4) -0.2259(4) 0.2149(3) 0.0433(11) Uani 1 1 d . . . C23 C 0.5647(4) -0.1234(3) 0.3955(2) 0.0426(10) Uani 1 1 d . . . H23 H 0.6321 -0.1906 0.3818 0.051 Uiso 1 1 calc R . . F5 F 0.9418(3) 0.0730(3) 0.2046(2) 0.0945(11) Uani 1 1 d . B . F6 F 0.9593(5) 0.2107(4) 0.1412(3) 0.164(2) Uani 1 1 d . B . F7 F 1.0782(4) 0.0484(4) 0.1016(3) 0.1538(19) Uani 1 1 d . B . B2 B 1.0321(6) 0.1003(5) 0.1630(4) 0.072(2) Uani 1 1 d . . . F4 F 0.8827(2) -0.2772(2) 0.16018(13) 0.0776(10) Uani 1 1 d . A . F1 F 0.7782(6) -0.2793(7) 0.2723(3) 0.089(3) Uani 0.701(9) 1 d P A 1 F2 F 0.8396(5) -0.1745(6) 0.2478(4) 0.146(4) Uani 0.701(9) 1 d P A 1 F3 F 0.6923(4) -0.1530(4) 0.2043(2) 0.0608(18) Uani 0.701(9) 1 d P A 1 F1' F 0.7674(16) -0.3142(14) 0.2457(14) 0.120(9) Uani 0.299(9) 1 d P A 2 F2' F 0.7483(13) -0.1127(8) 0.2106(6) 0.085(6) Uani 0.299(9) 1 d P A 2 F3' F 0.6987(10) -0.2424(14) 0.1864(6) 0.085(5) Uani 0.299(9) 1 d P A 2 F8 F 1.1220(9) -0.0043(12) 0.1988(7) 0.071(6) Uani 0.211(8) 1 d P B 1 F8' F 1.0902(5) 0.1320(7) 0.1891(3) 0.146(3) Uani 0.789(8) 1 d P B 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 0.02062(14) 0.01923(14) 0.02089(14) -0.00031(10) -0.00763(10) -0.00856(11) Rh2 0.01977(14) 0.02132(14) 0.02293(15) -0.00012(11) -0.00698(11) -0.00918(11) N13 0.0276(15) 0.0185(15) 0.0272(16) -0.0027(12) -0.0083(12) -0.0065(13) N14 0.0218(15) 0.0264(16) 0.0262(16) -0.0028(12) -0.0091(12) -0.0045(13) N5 0.0208(14) 0.0249(15) 0.0212(14) -0.0006(11) -0.0067(11) -0.0117(12) N6 0.0218(14) 0.0215(14) 0.0212(14) 0.0020(11) -0.0058(11) -0.0103(12) N8 0.0202(14) 0.0250(15) 0.0267(15) -0.0015(12) -0.0057(12) -0.0109(12) N2 0.0269(15) 0.0221(15) 0.0239(15) 0.0023(12) -0.0118(12) -0.0111(12) F10 0.0463(13) 0.0507(14) 0.0295(12) -0.0063(10) 0.0082(10) -0.0242(12) N7 0.0222(14) 0.0247(15) 0.0237(15) 0.0031(12) -0.0075(12) -0.0119(12) N4 0.0249(14) 0.0249(15) 0.0194(14) -0.0007(11) -0.0068(11) -0.0118(12) F9 0.0738(17) 0.0301(13) 0.0556(15) 0.0006(11) -0.0147(13) -0.0312(12) N3 0.0250(14) 0.0205(14) 0.0249(15) -0.0024(11) -0.0062(12) -0.0095(12) N1 0.0242(15) 0.0265(16) 0.0316(16) 0.0011(13) -0.0138(13) -0.0124(13) C45 0.0212(16) 0.0222(17) 0.0222(17) 0.0002(13) -0.0076(13) -0.0131(14) C44 0.0207(16) 0.0261(18) 0.0245(17) 0.0007(14) -0.0049(14) -0.0128(14) N9 0.0237(15) 0.0350(17) 0.0263(16) 0.0021(13) -0.0087(12) -0.0126(13) C50 0.0238(17) 0.0255(18) 0.0207(17) 0.0015(13) -0.0044(13) -0.0127(14) F12 0.104(2) 0.0381(15) 0.0688(18) 0.0280(13) -0.0473(17) -0.0369(15) C46 0.0190(16) 0.0187(16) 0.0239(17) 0.0019(13) -0.0076(13) -0.0091(13) C32 0.0229(17) 0.0236(18) 0.0231(17) 0.0028(14) -0.0061(14) -0.0132(14) C27 0.0262(18) 0.0272(19) 0.035(2) -0.0002(15) -0.0121(16) -0.0097(15) N10 0.0362(17) 0.0342(18) 0.0271(16) -0.0045(13) -0.0113(14) -0.0122(14) C31 0.0222(17) 0.0254(18) 0.0272(18) 0.0026(14) -0.0064(14) -0.0144(14) C7 0.0234(17) 0.0204(17) 0.0264(18) -0.0022(14) -0.0096(14) -0.0080(14) C52 0.0229(17) 0.0289(19) 0.0227(17) 0.0035(14) -0.0083(14) -0.0134(15) C34 0.0312(19) 0.0249(19) 0.036(2) 0.0060(15) -0.0131(16) -0.0146(16) N11 0.050(2) 0.043(2) 0.0266(17) 0.0063(15) -0.0156(15) -0.0249(17) C8 0.0232(17) 0.0174(16) 0.0239(17) -0.0009(13) -0.0052(14) -0.0068(14) C37 0.034(2) 0.035(2) 0.0275(19) 0.0022(16) -0.0053(16) -0.0233(17) C51 0.0265(18) 0.0273(18) 0.0256(18) 0.0006(14) -0.0077(14) -0.0158(15) C13 0.0216(17) 0.0263(18) 0.0274(18) -0.0058(14) -0.0085(14) -0.0064(14) N12 0.047(2) 0.0405(19) 0.0284(17) -0.0060(14) -0.0021(15) -0.0264(16) C20 0.0282(18) 0.0281(19) 0.0245(18) -0.0006(15) -0.0119(15) -0.0087(15) C49 0.0330(19) 0.0264(19) 0.0253(18) -0.0046(15) -0.0085(15) -0.0121(16) C48 0.0282(18) 0.0200(17) 0.0302(19) -0.0006(14) -0.0069(15) -0.0089(15) C43 0.0222(17) 0.0289(19) 0.0295(19) 0.0025(15) -0.0126(15) -0.0083(15) C47 0.0254(17) 0.0182(17) 0.0287(18) 0.0005(14) -0.0085(14) -0.0079(14) C30 0.0273(18) 0.0258(19) 0.0286(19) -0.0022(15) -0.0034(15) -0.0138(15) C53 0.032(2) 0.045(2) 0.029(2) 0.0054(17) -0.0150(16) -0.0207(18) C22 0.040(2) 0.0270(19) 0.0272(19) -0.0001(15) -0.0163(16) -0.0082(16) C41 0.0208(16) 0.0261(18) 0.0256(18) -0.0032(14) -0.0067(14) -0.0076(14) C33 0.0250(17) 0.0237(18) 0.0254(18) 0.0040(14) -0.0072(14) -0.0118(15) C54 0.044(2) 0.042(2) 0.032(2) -0.0022(17) -0.0182(18) -0.0142(19) C5 0.0304(19) 0.030(2) 0.035(2) -0.0038(16) -0.0036(16) -0.0146(16) C9 0.0271(18) 0.032(2) 0.0281(19) -0.0022(15) -0.0102(15) -0.0126(16) C21 0.038(2) 0.0232(18) 0.0248(18) 0.0006(14) -0.0175(16) -0.0117(16) C56 0.031(2) 0.037(2) 0.038(2) 0.0009(17) -0.0148(17) -0.0149(17) C35 0.0310(19) 0.033(2) 0.0265(19) 0.0077(15) -0.0115(15) -0.0161(16) C29 0.0287(19) 0.029(2) 0.041(2) -0.0106(17) -0.0023(17) -0.0099(16) C42 0.0259(18) 0.0233(18) 0.033(2) -0.0016(15) -0.0087(15) -0.0043(15) C36 0.0267(18) 0.0294(19) 0.0253(18) 0.0021(15) -0.0070(14) -0.0169(15) C11 0.0309(19) 0.029(2) 0.0268(19) -0.0032(15) 0.0018(15) -0.0111(16) C4 0.0304(18) 0.0248(18) 0.0236(18) -0.0027(14) -0.0069(14) -0.0147(15) F11 0.0657(19) 0.068(2) 0.162(3) -0.018(2) -0.073(2) -0.0258(16) C3 0.0336(19) 0.031(2) 0.0292(19) -0.0041(15) -0.0083(16) -0.0155(16) C2 0.044(2) 0.042(2) 0.032(2) -0.0034(17) -0.0070(17) -0.030(2) C28 0.0281(19) 0.031(2) 0.044(2) -0.0045(17) -0.0086(17) -0.0060(16) C12 0.0233(18) 0.032(2) 0.040(2) -0.0081(17) -0.0020(16) -0.0128(16) C38 0.034(2) 0.032(2) 0.0263(19) -0.0041(15) -0.0010(15) -0.0192(17) C26 0.037(2) 0.031(2) 0.031(2) 0.0020(16) -0.0116(17) -0.0137(17) C10 0.036(2) 0.032(2) 0.0244(18) -0.0012(15) -0.0084(16) -0.0105(17) C17 0.0278(18) 0.0254(19) 0.043(2) 0.0065(16) -0.0220(17) -0.0112(15) C16 0.042(2) 0.040(2) 0.046(2) 0.0002(19) -0.024(2) -0.0160(19) C55 0.048(3) 0.084(4) 0.055(3) 0.012(3) -0.014(2) -0.049(3) C58 0.033(2) 0.026(2) 0.051(3) -0.0045(18) -0.0039(18) -0.0122(17) C57 0.047(3) 0.044(3) 0.145(6) -0.004(3) -0.006(3) -0.029(2) C6 0.042(2) 0.025(2) 0.042(2) -0.0013(17) -0.0119(18) -0.0112(17) C40 0.067(3) 0.051(3) 0.029(2) 0.0005(19) -0.017(2) -0.034(2) C1 0.058(3) 0.026(2) 0.031(2) -0.0001(16) -0.0062(19) -0.025(2) C18 0.028(2) 0.036(2) 0.052(3) 0.0005(19) -0.0167(18) -0.0119(17) C24 0.076(3) 0.027(2) 0.045(2) 0.0180(18) -0.039(2) -0.025(2) C25 0.056(3) 0.045(3) 0.040(2) 0.0130(19) -0.017(2) -0.028(2) C39 0.061(3) 0.045(3) 0.026(2) -0.0073(18) -0.0035(19) -0.031(2) C19 0.034(2) 0.045(3) 0.085(4) 0.008(2) -0.031(2) -0.018(2) C14 0.047(3) 0.042(3) 0.101(4) -0.003(3) -0.050(3) -0.017(2) C15 0.063(3) 0.044(3) 0.068(3) -0.007(2) -0.044(3) -0.019(2) B1 0.041(3) 0.037(3) 0.042(3) -0.004(2) -0.010(2) -0.005(2) C23 0.065(3) 0.025(2) 0.040(2) 0.0005(17) -0.028(2) -0.010(2) F5 0.067(2) 0.081(2) 0.134(3) 0.012(2) -0.015(2) -0.0404(19) F6 0.193(5) 0.105(4) 0.140(4) -0.015(3) 0.034(4) -0.059(4) F7 0.113(3) 0.134(4) 0.146(4) -0.049(3) 0.012(3) -0.002(3) B2 0.059(4) 0.051(4) 0.094(5) -0.023(4) 0.019(4) -0.034(3) F4 0.0671(18) 0.080(2) 0.0345(14) -0.0003(14) -0.0145(13) 0.0232(16) F1 0.054(4) 0.109(6) 0.036(3) 0.035(3) -0.002(2) 0.022(4) F2 0.094(4) 0.138(6) 0.225(8) -0.105(6) -0.061(5) -0.026(4) F3 0.045(3) 0.056(4) 0.049(2) 0.005(2) -0.018(2) 0.015(2) F1' 0.048(7) 0.047(8) 0.26(3) 0.033(13) -0.042(14) -0.022(6) F2' 0.101(13) 0.026(5) 0.081(8) 0.016(5) 0.012(8) -0.008(6) F3' 0.069(8) 0.140(14) 0.073(8) 0.027(8) -0.028(6) -0.066(9) F8 0.019(6) 0.072(11) 0.095(12) -0.015(8) -0.014(6) 0.011(6) F8' 0.145(5) 0.278(10) 0.111(4) 0.059(5) -0.054(4) -0.179(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 N5 2.035(3) . ? Rh1 N4 2.043(3) . ? Rh1 N2 2.052(3) . ? Rh1 N6 2.053(3) . ? Rh1 N13 2.233(3) . ? Rh1 Rh2 2.5989(8) . ? Rh2 N1 2.031(3) . ? Rh2 N8 2.045(3) . ? Rh2 N7 2.053(3) . ? Rh2 N3 2.057(3) . ? Rh2 N14 2.199(3) . ? N13 C58 1.108(4) . ? N14 C56 1.119(4) . ? N5 C41 1.336(4) . ? N5 C45 1.355(4) . ? N6 C47 1.331(4) . ? N6 C46 1.361(4) . ? N8 C27 1.335(4) . ? N8 C31 1.365(4) . ? N2 C20 1.317(4) . ? N2 C21 1.426(4) . ? F10 C11 1.368(4) . ? N7 C33 1.331(4) . ? N7 C32 1.367(4) . ? N4 C7 1.306(4) . ? N4 C8 1.438(4) . ? F9 C1 1.370(4) . ? N3 C7 1.306(4) . ? N3 C4 1.438(4) . ? N1 C20 1.306(4) . ? N1 C17 1.444(4) . ? C45 C44 1.400(4) . ? C45 C46 1.444(4) . ? C44 C43 1.402(5) . ? C44 C52 1.448(5) . ? N9 C53 1.324(4) . ? N9 C52 1.355(4) . ? C50 C46 1.396(4) . ? C50 C49 1.398(5) . ? C50 C51 1.453(5) . ? F12 C24 1.366(4) . ? C32 C36 1.397(4) . ? C32 C31 1.443(5) . ? C27 C28 1.388(5) . ? N10 C54 1.328(5) . ? N10 C51 1.348(4) . ? C31 C30 1.390(5) . ? C52 C51 1.405(5) . ? C34 C35 1.376(5) . ? C34 C33 1.387(5) . ? N11 C40 1.321(5) . ? N11 C37 1.354(4) . ? C8 C9 1.379(5) . ? C8 C13 1.390(4) . ? C37 C38 1.405(5) . ? C37 C36 1.461(5) . ? C13 C12 1.372(5) . ? N12 C39 1.320(5) . ? N12 C38 1.347(4) . ? C49 C48 1.372(5) . ? C48 C47 1.391(5) . ? C43 C42 1.375(5) . ? C30 C29 1.397(5) . ? C30 C38 1.455(5) . ? C53 C54 1.399(5) . ? C22 C21 1.389(5) . ? C22 C23 1.396(5) . ? C41 C42 1.396(5) . ? C5 C4 1.381(5) . ? C5 C6 1.393(5) . ? C9 C10 1.377(5) . ? C21 C26 1.395(5) . ? C56 C55 1.459(5) . ? C35 C36 1.393(5) . ? C29 C28 1.367(5) . ? C11 C12 1.368(5) . ? C11 C10 1.370(5) . ? C4 C3 1.390(5) . ? F11 C14 1.366(4) . ? C3 C2 1.388(5) . ? C2 C1 1.362(6) . ? C26 C25 1.388(5) . ? C17 C16 1.376(5) . ? C17 C18 1.378(5) . ? C16 C15 1.400(5) . ? C58 C57 1.467(6) . ? C6 C1 1.366(5) . ? C40 C39 1.390(6) . ? C18 C19 1.382(5) . ? C24 C23 1.359(6) . ? C24 C25 1.369(6) . ? C19 C14 1.360(7) . ? C14 C15 1.368(7) . ? B1 F1 1.300(7) . ? B1 F3 1.317(6) . ? B1 F4 1.337(5) . ? B1 F1' 1.364(17) . ? B1 F2' 1.373(10) . ? B1 F2 1.399(7) . ? B1 F3' 1.566(12) . ? F5 B2 1.358(6) . ? F6 B2 1.489(8) . ? F7 B2 1.338(7) . ? B2 F8' 1.242(8) . ? B2 F8 1.670(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 N5 Rh1 N4 93.53(11) . . ? N5 Rh1 N2 178.74(11) . . ? N4 Rh1 N2 87.63(11) . . ? N5 Rh1 N6 80.47(11) . . ? N4 Rh1 N6 173.96(10) . . ? N2 Rh1 N6 98.37(11) . . ? N5 Rh1 N13 84.47(10) . . ? N4 Rh1 N13 98.24(10) . . ? N2 Rh1 N13 95.86(10) . . ? N6 Rh1 N13 81.96(10) . . ? N5 Rh1 Rh2 94.13(8) . . ? N4 Rh1 Rh2 84.85(8) . . ? N2 Rh1 Rh2 85.47(8) . . ? N6 Rh1 Rh2 94.83(8) . . ? N13 Rh1 Rh2 176.67(7) . . ? N1 Rh2 N8 93.87(11) . . ? N1 Rh2 N7 174.58(11) . . ? N8 Rh2 N7 80.74(11) . . ? N1 Rh2 N3 87.92(11) . . ? N8 Rh2 N3 177.96(10) . . ? N7 Rh2 N3 97.47(11) . . ? N1 Rh2 N14 95.31(11) . . ? N8 Rh2 N14 84.61(10) . . ? N7 Rh2 N14 84.79(10) . . ? N3 Rh2 N14 96.23(11) . . ? N1 Rh2 Rh1 85.01(8) . . ? N8 Rh2 Rh1 93.71(8) . . ? N7 Rh2 Rh1 94.73(7) . . ? N3 Rh2 Rh1 85.44(8) . . ? N14 Rh2 Rh1 178.31(7) . . ? C58 N13 Rh1 167.4(3) . . ? C56 N14 Rh2 169.9(3) . . ? C41 N5 C45 118.3(3) . . ? C41 N5 Rh1 127.7(2) . . ? C45 N5 Rh1 114.0(2) . . ? C47 N6 C46 117.6(3) . . ? C47 N6 Rh1 129.0(2) . . ? C46 N6 Rh1 113.3(2) . . ? C27 N8 C31 117.5(3) . . ? C27 N8 Rh2 128.8(2) . . ? C31 N8 Rh2 113.6(2) . . ? C20 N2 C21 115.9(3) . . ? C20 N2 Rh1 119.4(2) . . ? C21 N2 Rh1 124.5(2) . . ? C33 N7 C32 117.7(3) . . ? C33 N7 Rh2 129.2(2) . . ? C32 N7 Rh2 113.0(2) . . ? C7 N4 C8 116.8(3) . . ? C7 N4 Rh1 121.4(2) . . ? C8 N4 Rh1 121.8(2) . . ? C7 N3 C4 116.0(3) . . ? C7 N3 Rh2 119.5(2) . . ? C4 N3 Rh2 124.5(2) . . ? C20 N1 C17 115.8(3) . . ? C20 N1 Rh2 121.8(2) . . ? C17 N1 Rh2 122.2(2) . . ? N5 C45 C44 123.0(3) . . ? N5 C45 C46 116.3(3) . . ? C44 C45 C46 120.8(3) . . ? C45 C44 C43 117.4(3) . . ? C45 C44 C52 119.0(3) . . ? C43 C44 C52 123.6(3) . . ? C53 N9 C52 115.8(3) . . ? C46 C50 C49 117.5(3) . . ? C46 C50 C51 119.0(3) . . ? C49 C50 C51 123.5(3) . . ? N6 C46 C50 123.4(3) . . ? N6 C46 C45 116.0(3) . . ? C50 C46 C45 120.6(3) . . ? N7 C32 C36 122.1(3) . . ? N7 C32 C31 116.6(3) . . ? C36 C32 C31 121.3(3) . . ? N8 C27 C28 122.7(3) . . ? C54 N10 C51 115.8(3) . . ? N8 C31 C30 122.6(3) . . ? N8 C31 C32 116.1(3) . . ? C30 C31 C32 121.3(3) . . ? N4 C7 N3 124.6(3) . . ? N9 C52 C51 121.6(3) . . ? N9 C52 C44 118.1(3) . . ? C51 C52 C44 120.3(3) . . ? C35 C34 C33 119.4(3) . . ? C40 N11 C37 115.9(4) . . ? C9 C8 C13 119.5(3) . . ? C9 C8 N4 121.1(3) . . ? C13 C8 N4 119.4(3) . . ? N11 C37 C38 121.5(3) . . ? N11 C37 C36 118.1(3) . . ? C38 C37 C36 120.4(3) . . ? N10 C51 C52 121.7(3) . . ? N10 C51 C50 117.9(3) . . ? C52 C51 C50 120.3(3) . . ? C12 C13 C8 120.5(3) . . ? C39 N12 C38 116.2(4) . . ? N1 C20 N2 124.1(3) . . ? C48 C49 C50 119.1(3) . . ? C49 C48 C47 119.9(3) . . ? C42 C43 C44 119.7(3) . . ? N6 C47 C48 122.5(3) . . ? C31 C30 C29 118.4(3) . . ? C31 C30 C38 118.2(3) . . ? C29 C30 C38 123.4(3) . . ? N9 C53 C54 122.6(3) . . ? C21 C22 C23 120.1(4) . . ? N5 C41 C42 122.5(3) . . ? N7 C33 C34 123.2(3) . . ? N10 C54 C53 122.4(3) . . ? C4 C5 C6 121.0(3) . . ? C10 C9 C8 120.5(3) . . ? C22 C21 C26 119.4(3) . . ? C22 C21 N2 119.3(3) . . ? C26 C21 N2 121.3(3) . . ? N14 C56 C55 177.1(4) . . ? C34 C35 C36 118.9(3) . . ? C28 C29 C30 118.9(3) . . ? C43 C42 C41 119.2(3) . . ? C35 C36 C32 118.6(3) . . ? C35 C36 C37 123.5(3) . . ? C32 C36 C37 117.9(3) . . ? C12 C11 F10 118.8(3) . . ? C12 C11 C10 122.7(3) . . ? F10 C11 C10 118.5(3) . . ? C5 C4 C3 119.2(3) . . ? C5 C4 N3 119.1(3) . . ? C3 C4 N3 121.7(3) . . ? C2 C3 C4 120.2(4) . . ? C1 C2 C3 118.7(3) . . ? C29 C28 C27 119.8(3) . . ? C11 C12 C13 118.3(3) . . ? N12 C38 C37 121.3(3) . . ? N12 C38 C30 117.9(3) . . ? C37 C38 C30 120.8(3) . . ? C25 C26 C21 120.3(4) . . ? C11 C10 C9 118.4(3) . . ? C16 C17 C18 120.5(3) . . ? C16 C17 N1 119.7(3) . . ? C18 C17 N1 119.8(3) . . ? C17 C16 C15 119.4(4) . . ? N13 C58 C57 178.2(5) . . ? C1 C6 C5 117.8(4) . . ? N11 C40 C39 122.5(4) . . ? C2 C1 C6 123.1(3) . . ? C2 C1 F9 118.9(3) . . ? C6 C1 F9 118.0(4) . . ? C17 C18 C19 120.4(4) . . ? C23 C24 F12 118.8(4) . . ? C23 C24 C25 123.0(4) . . ? F12 C24 C25 118.1(4) . . ? C24 C25 C26 118.5(4) . . ? N12 C39 C40 122.6(4) . . ? C14 C19 C18 118.3(4) . . ? C19 C14 F11 119.3(5) . . ? C19 C14 C15 123.1(4) . . ? F11 C14 C15 117.7(5) . . ? C14 C15 C16 118.3(4) . . ? F1 B1 F3 115.0(5) . . ? F1 B1 F4 118.5(5) . . ? F3 B1 F4 118.6(4) . . ? F1 B1 F1' 35.8(10) . . ? F3 B1 F1' 106.8(9) . . ? F4 B1 F1' 99.5(11) . . ? F1 B1 F2' 124.2(7) . . ? F3 B1 F2' 47.7(7) . . ? F4 B1 F2' 113.5(6) . . ? F1' B1 F2' 145.0(11) . . ? F1 B1 F2 83.7(7) . . ? F3 B1 F2 109.8(5) . . ? F4 B1 F2 103.9(5) . . ? F1' B1 F2 118.5(12) . . ? F2' B1 F2 65.4(8) . . ? F1 B1 F3' 99.8(7) . . ? F3 B1 F3' 49.9(6) . . ? F4 B1 F3' 92.7(6) . . ? F1' B1 F3' 70.2(11) . . ? F2' B1 F3' 96.3(10) . . ? F2 B1 F3' 159.0(7) . . ? C24 C23 C22 118.7(4) . . ? F8' B2 F7 122.9(6) . . ? F8' B2 F5 119.6(7) . . ? F7 B2 F5 111.9(5) . . ? F8' B2 F6 97.2(6) . . ? F7 B2 F6 98.1(6) . . ? F5 B2 F6 98.5(5) . . ? F8' B2 F8 68.8(7) . . ? F7 B2 F8 92.6(6) . . ? F5 B2 F8 86.3(6) . . ? F6 B2 F8 165.6(8) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.84 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.124 _refine_diff_density_min -0.786 _refine_diff_density_rms 0.139 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 _platon_squeeze_void_content 1 0.000 0.000 -0.009 367 112 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 937902' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_d:\xray\yong06~1\work\2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H44 B2 F12 N14 Rh2' _chemical_formula_weight 1488.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.104(3) _cell_length_b 13.114(3) _cell_length_c 22.820(5) _cell_angle_alpha 73.63(3) _cell_angle_beta 86.21(3) _cell_angle_gamma 66.42(3) _cell_volume 3443.5(12) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.436 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1492 _exptl_absorpt_coefficient_mu 0.562 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9205 _exptl_absorpt_correction_T_max 0.9779 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 22410 _diffrn_reflns_av_R_equivalents 0.0364 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 24.71 _reflns_number_total 11489 _reflns_number_gt 8562 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1094P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11489 _refine_ls_number_parameters 867 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0752 _refine_ls_R_factor_gt 0.0560 _refine_ls_wR_factor_ref 0.1720 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.72664(3) 0.84313(3) 0.319743(17) 0.01801(14) Uani 1 1 d . . . Rh2 Rh 0.62503(3) 0.74699(3) 0.271994(17) 0.01900(14) Uani 1 1 d . . . N13 N 0.8125(4) 0.9257(4) 0.35885(18) 0.0227(10) Uani 1 1 d . . . N14 N 0.5482(4) 0.6563(4) 0.2298(2) 0.0303(11) Uani 1 1 d . . . N3 N 0.6139(4) 0.8445(4) 0.38608(18) 0.0218(10) Uani 1 1 d . . . N6 N 0.8298(4) 0.8563(4) 0.24872(19) 0.0214(10) Uani 1 1 d . . . N8 N 0.7467(4) 0.7027(4) 0.21095(19) 0.0249(10) Uani 1 1 d . . . N5 N 0.6319(4) 1.0084(4) 0.26816(19) 0.0218(10) Uani 1 1 d . . . N1 N 0.8248(4) 0.6767(4) 0.36882(19) 0.0239(10) Uani 1 1 d . . . F11 F 0.6624(3) 0.8976(3) 0.61456(14) 0.0414(9) Uani 1 1 d . . . N7 N 0.5558(4) 0.8884(4) 0.19688(19) 0.0229(10) Uani 1 1 d . . . N2 N 0.7064(4) 0.6011(4) 0.3422(2) 0.0242(10) Uani 1 1 d . . . N4 N 0.5004(4) 0.8006(4) 0.33046(19) 0.0229(10) Uani 1 1 d . . . F12 F 0.0650(3) 0.8342(4) 0.31950(18) 0.0574(11) Uani 1 1 d . . . F9 F 1.2412(3) 0.5450(4) 0.48011(18) 0.0581(11) Uani 1 1 d . . . N10 N 0.8452(4) 1.1214(4) 0.0570(2) 0.0276(11) Uani 1 1 d . . . C36 C 0.7867(4) 0.9615(5) 0.2048(2) 0.0224(11) Uani 1 1 d . . . C54 C 0.6201(4) 0.8836(5) 0.1473(2) 0.0224(11) Uani 1 1 d . . . C20 C 0.5225(4) 0.8285(4) 0.3784(2) 0.0218(11) Uani 1 1 d . . . H20 H 0.4696 0.8375 0.4091 0.026 Uiso 1 1 calc R . . C18 C 0.6293(4) 0.8565(4) 0.4453(2) 0.0216(11) Uani 1 1 d . . . C53 C 0.7242(5) 0.7828(4) 0.1553(2) 0.0219(11) Uani 1 1 d . . . F4 F 1.2594(5) 0.4200(4) 0.20492(18) 0.0860(18) Uani 1 1 d . . . C37 C 0.8437(4) 0.9894(5) 0.1524(2) 0.0220(11) Uani 1 1 d . . . C31 C 0.5368(4) 1.0846(5) 0.2821(2) 0.0240(12) Uani 1 1 d . . . H31 H 0.5043 1.0615 0.3193 0.029 Uiso 1 1 calc R . . C34 C 0.6298(5) 1.1547(5) 0.1737(2) 0.0264(12) Uani 1 1 d . . . N12 N 0.8367(4) 0.8464(5) 0.0038(2) 0.0360(12) Uani 1 1 d . . . C35 C 0.6798(4) 1.0449(4) 0.2147(2) 0.0210(11) Uani 1 1 d . . . N11 N 0.6379(4) 1.0488(4) -0.0090(2) 0.0366(12) Uani 1 1 d . . . C17 C 0.6415(4) 0.7666(5) 0.4979(2) 0.0260(12) Uani 1 1 d . . . H17 H 0.6425 0.6955 0.4947 0.031 Uiso 1 1 calc R . . C38 C 0.9505(5) 0.9062(5) 0.1468(2) 0.0264(12) Uani 1 1 d . . . H38 H 0.9917 0.9209 0.1119 0.032 Uiso 1 1 calc R . . C42 C 0.7914(4) 1.1011(5) 0.1071(2) 0.0219(11) Uani 1 1 d . . . C26 C 0.3670(5) 0.7139(5) 0.3245(2) 0.0303(13) Uani 1 1 d . . . H26 H 0.4274 0.6424 0.3255 0.036 Uiso 1 1 calc R . . C40 C 0.9316(4) 0.7816(5) 0.2420(2) 0.0224(11) Uani 1 1 d . . . H40 H 0.9630 0.7097 0.2726 0.027 Uiso 1 1 calc R . . C56 C 0.4225(5) 1.0679(5) 0.1371(3) 0.0331(14) Uani 1 1 d . . . H56 H 0.3526 1.1310 0.1349 0.040 Uiso 1 1 calc R . . C52 C 0.7963(5) 0.7676(5) 0.1068(2) 0.0261(12) Uani 1 1 d . . . C21 C 0.3882(5) 0.8096(5) 0.3253(2) 0.0253(12) Uani 1 1 d . . . C19 C 0.6313(5) 0.9599(5) 0.4499(2) 0.0266(12) Uani 1 1 d . . . H19 H 0.6236 1.0211 0.4140 0.032 Uiso 1 1 calc R . . C60 C 0.7664(5) 0.8602(5) 0.0490(2) 0.0315(14) Uani 1 1 d . . . N9 N 0.6358(4) 1.2858(4) 0.0768(2) 0.0421(13) Uani 1 1 d . . . C57 C 0.4870(5) 1.0668(5) 0.0872(3) 0.0348(14) Uani 1 1 d . . . H57 H 0.4633 1.1284 0.0506 0.042 Uiso 1 1 calc R . . C49 C 0.8397(5) 0.6045(5) 0.2187(3) 0.0290(13) Uani 1 1 d . . . H49 H 0.8553 0.5473 0.2571 0.035 Uiso 1 1 calc R . . C33 C 0.5280(5) 1.2324(5) 0.1893(3) 0.0331(14) Uani 1 1 d . . . H33 H 0.4909 1.3079 0.1626 0.040 Uiso 1 1 calc R . . C14 C 0.6445(4) 0.9731(5) 0.5069(2) 0.0263(12) Uani 1 1 d . . . H14 H 0.6471 1.0425 0.5104 0.032 Uiso 1 1 calc R . . C43 C 0.7962(5) 1.2263(5) 0.0155(2) 0.0312(13) Uani 1 1 d . . . C41 C 0.6850(5) 1.1842(5) 0.1168(2) 0.0278(12) Uani 1 1 d . . . C55 C 0.4578(5) 0.9786(5) 0.1905(2) 0.0263(12) Uani 1 1 d . . . H55 H 0.4105 0.9815 0.2239 0.032 Uiso 1 1 calc R . . C39 C 0.9937(5) 0.8046(5) 0.1921(2) 0.0283(13) Uani 1 1 d . . . H39 H 1.0665 0.7493 0.1895 0.034 Uiso 1 1 calc R . . C8 C 0.6719(5) 0.5069(5) 0.3599(2) 0.0276(12) Uani 1 1 d . . . C5 C 0.9418(5) 0.6881(5) 0.4458(2) 0.0309(13) Uani 1 1 d . . . H5 H 0.8777 0.7421 0.4587 0.037 Uiso 1 1 calc R . . C58 C 0.5901(5) 0.9706(5) 0.0923(2) 0.0260(12) Uani 1 1 d . . . C59 C 0.6653(5) 0.9616(5) 0.0421(2) 0.0301(13) Uani 1 1 d . . . F10 F 0.5781(5) 0.2312(4) 0.4128(3) 0.0956(18) Uani 1 1 d . . . C7 C 0.7915(5) 0.5913(5) 0.3742(2) 0.0256(12) Uani 1 1 d . . . H7 H 0.8316 0.5188 0.4028 0.031 Uiso 1 1 calc R . . C51 C 0.8927(5) 0.6644(5) 0.1172(3) 0.0338(14) Uani 1 1 d . . . H51 H 0.9431 0.6509 0.0856 0.041 Uiso 1 1 calc R . . C15 C 0.6536(5) 0.8840(5) 0.5579(2) 0.0313(14) Uani 1 1 d . . . C3 C 0.9308(4) 0.6423(5) 0.3993(2) 0.0256(12) Uani 1 1 d . . . C50 C 0.9137(5) 0.5839(5) 0.1726(3) 0.0366(15) Uani 1 1 d . . . H50 H 0.9786 0.5138 0.1797 0.044 Uiso 1 1 calc R . . C22 C 0.2981(5) 0.9133(5) 0.3234(3) 0.0324(14) Uani 1 1 d . . . H22 H 0.3119 0.9791 0.3234 0.039 Uiso 1 1 calc R . . C4 C 1.0261(5) 0.5605(5) 0.3818(3) 0.0315(13) Uani 1 1 d . . . H4 H 1.0196 0.5273 0.3510 0.038 Uiso 1 1 calc R . . F1 F 1.2890(5) 0.4064(5) 0.30273(18) 0.110(2) Uani 1 1 d . . . C24 C 0.1726(5) 0.8268(7) 0.3215(3) 0.0415(17) Uani 1 1 d . . . C25 C 0.2579(5) 0.7225(6) 0.3222(3) 0.0370(15) Uani 1 1 d . . . H25 H 0.2428 0.6580 0.3211 0.044 Uiso 1 1 calc R . . C63 C 0.8779(7) 0.9212(7) -0.0996(3) 0.0490(19) Uani 1 1 d . . . H63 H 0.9443 0.8535 -0.0964 0.059 Uiso 1 1 calc R . . C23 C 0.1896(5) 0.9234(6) 0.3215(3) 0.0365(15) Uani 1 1 d . . . H23 H 0.1287 0.9947 0.3203 0.044 Uiso 1 1 calc R . . C16 C 0.6523(5) 0.7803(5) 0.5555(2) 0.0325(14) Uani 1 1 d . . . H16 H 0.6586 0.7203 0.5918 0.039 Uiso 1 1 calc R . . C32 C 0.4832(5) 1.1972(5) 0.2440(2) 0.0290(13) Uani 1 1 d . . . H32 H 0.4161 1.2494 0.2557 0.035 Uiso 1 1 calc R . . C13 C 0.6075(6) 0.4949(6) 0.4095(3) 0.0450(17) Uani 1 1 d . . . H13 H 0.5845 0.5516 0.4315 0.054 Uiso 1 1 calc R . . C1 C 1.1379(5) 0.5758(6) 0.4541(3) 0.0387(15) Uani 1 1 d . . . C61 C 0.8076(6) 0.9334(7) -0.0488(3) 0.0453(18) Uani 1 1 d . . . C66 C 0.7492(8) 1.1142(9) -0.1585(3) 0.068(3) Uani 1 1 d . . . H66 H 0.7311 1.1746 -0.1958 0.081 Uiso 1 1 calc R . . C46 C 0.8529(6) 1.2553(6) -0.0388(3) 0.0399(15) Uani 1 1 d . . . H46 H 0.9231 1.2006 -0.0457 0.048 Uiso 1 1 calc R . . C9 C 0.7018(6) 0.4252(6) 0.3273(3) 0.0455(17) Uani 1 1 d . . . H9 H 0.7445 0.4330 0.2923 0.055 Uiso 1 1 calc R . . C62 C 0.7083(6) 1.0361(6) -0.0544(3) 0.0414(16) Uani 1 1 d . . . F3 F 1.1253(5) 0.5304(6) 0.2530(3) 0.139(3) Uani 1 1 d . . . C6 C 1.0455(5) 0.6551(6) 0.4732(3) 0.0392(15) Uani 1 1 d . . . H6 H 1.0532 0.6865 0.5047 0.047 Uiso 1 1 calc R . . C64 C 0.6825(7) 1.1274(7) -0.1106(3) 0.059(2) Uani 1 1 d . . . H64 H 0.6185 1.1974 -0.1143 0.071 Uiso 1 1 calc R . . C44 C 0.6924(5) 1.3084(6) 0.0254(3) 0.0440(17) Uani 1 1 d . . . C2 C 1.1308(5) 0.5280(6) 0.4097(3) 0.0409(16) Uani 1 1 d . . . H2 H 1.1957 0.4733 0.3978 0.049 Uiso 1 1 calc R . . C47 C 0.8064(6) 1.3604(6) -0.0802(3) 0.0457(17) Uani 1 1 d . . . H47 H 0.8442 1.3782 -0.1161 0.055 Uiso 1 1 calc R . . C11 C 0.6091(7) 0.3219(6) 0.3957(4) 0.060(2) Uani 1 1 d . . . F2 F 1.2618(8) 0.5694(7) 0.2266(3) 0.146(3) Uani 1 1 d . . . C48 C 0.7033(7) 1.4435(8) -0.0709(4) 0.077(3) Uani 1 1 d . . . H48 H 0.6715 1.5165 -0.1007 0.092 Uiso 1 1 calc R . . C12 C 0.5751(7) 0.4017(6) 0.4285(3) 0.057(2) Uani 1 1 d . . . H12 H 0.5311 0.3939 0.4629 0.069 Uiso 1 1 calc R . . B1 B 1.2336(8) 0.4711(7) 0.2504(4) 0.056(2) Uani 1 1 d . . . C45 C 0.6492(7) 1.4196(8) -0.0194(4) 0.081(3) Uani 1 1 d . . . H45 H 0.5812 1.4777 -0.0128 0.098 Uiso 1 1 calc R . . C28 C 0.8555(5) 0.9724(6) 0.3753(3) 0.0362(15) Uani 1 1 d . . . C10 C 0.6698(7) 0.3317(6) 0.3453(4) 0.065(2) Uani 1 1 d . . . H10 H 0.6900 0.2762 0.3229 0.078 Uiso 1 1 calc R . . C30 C 0.5364(7) 0.5953(7) 0.2078(4) 0.062(2) Uani 1 1 d . . . C27 C 0.9126(8) 1.0260(10) 0.4025(5) 0.101(4) Uani 1 1 d . . . H27A H 0.8595 1.0766 0.4249 0.151 Uiso 1 1 calc R . . H27B H 0.9424 1.0718 0.3701 0.151 Uiso 1 1 calc R . . H27C H 0.9739 0.9653 0.4307 0.151 Uiso 1 1 calc R . . C29 C 0.5258(14) 0.5077(12) 0.1817(7) 0.164(7) Uani 1 1 d . . . H29A H 0.5931 0.4359 0.1932 0.246 Uiso 1 1 calc R . . H29B H 0.5167 0.5376 0.1370 0.246 Uiso 1 1 calc R . . H29C H 0.4607 0.4921 0.1976 0.246 Uiso 1 1 calc R . . C65 C 0.8469(8) 1.0095(9) -0.1529(3) 0.068(3) Uani 1 1 d . . . H65 H 0.8915 1.0010 -0.1872 0.081 Uiso 1 1 calc R . . F5 F 0.8750(7) 0.3436(5) 0.2205(3) 0.123(3) Uani 1 1 d . . . F7 F 0.8962(7) 0.2302(7) 0.1591(4) 0.148(3) Uani 1 1 d . . . F8 F 0.7828(8) 0.2291(9) 0.2308(4) 0.173(4) Uani 1 1 d . . . B2 B 0.8810(11) 0.2423(11) 0.2169(5) 0.074(3) Uani 1 1 d . . . F6 F 0.9483(9) 0.1647(8) 0.2612(6) 0.255(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0186(2) 0.0211(2) 0.0176(2) -0.00844(17) 0.00321(16) -0.00949(18) Rh2 0.0225(3) 0.0220(2) 0.0169(2) -0.00913(17) 0.00362(16) -0.01126(19) N13 0.017(2) 0.031(3) 0.017(2) -0.010(2) 0.0079(17) -0.007(2) N14 0.034(3) 0.038(3) 0.021(2) -0.014(2) 0.008(2) -0.014(2) N3 0.024(2) 0.030(3) 0.018(2) -0.0121(19) 0.0017(17) -0.013(2) N6 0.024(2) 0.022(2) 0.024(2) -0.0094(19) 0.0005(18) -0.013(2) N8 0.027(3) 0.028(3) 0.027(2) -0.016(2) 0.0075(19) -0.013(2) N5 0.025(2) 0.027(2) 0.022(2) -0.0141(19) 0.0056(18) -0.014(2) N1 0.024(2) 0.030(3) 0.021(2) -0.0073(19) 0.0028(18) -0.014(2) F11 0.045(2) 0.057(2) 0.0311(18) -0.0285(17) 0.0009(15) -0.0180(19) N7 0.025(3) 0.027(3) 0.026(2) -0.013(2) 0.0000(18) -0.015(2) N2 0.028(3) 0.021(2) 0.027(2) -0.0076(19) 0.0028(19) -0.012(2) N4 0.022(2) 0.029(3) 0.021(2) -0.009(2) 0.0000(18) -0.013(2) F12 0.031(2) 0.101(3) 0.058(2) -0.030(2) 0.0103(18) -0.040(2) F9 0.033(2) 0.072(3) 0.056(2) -0.001(2) -0.0186(18) -0.015(2) N10 0.034(3) 0.031(3) 0.024(2) -0.012(2) 0.006(2) -0.018(2) C36 0.029(3) 0.026(3) 0.021(3) -0.009(2) 0.001(2) -0.017(2) C54 0.024(3) 0.030(3) 0.021(3) -0.013(2) 0.001(2) -0.015(2) C20 0.022(3) 0.023(3) 0.023(3) -0.011(2) 0.004(2) -0.010(2) C18 0.021(3) 0.026(3) 0.021(3) -0.014(2) 0.005(2) -0.008(2) C53 0.033(3) 0.022(3) 0.017(3) -0.010(2) 0.001(2) -0.014(2) F4 0.119(4) 0.048(3) 0.036(2) -0.006(2) 0.012(2) 0.017(3) C37 0.022(3) 0.028(3) 0.022(3) -0.011(2) 0.004(2) -0.015(2) C31 0.019(3) 0.031(3) 0.030(3) -0.018(2) 0.012(2) -0.013(2) C34 0.027(3) 0.031(3) 0.025(3) -0.011(2) 0.002(2) -0.014(3) N12 0.051(3) 0.053(3) 0.024(3) -0.018(2) 0.015(2) -0.037(3) C35 0.021(3) 0.024(3) 0.026(3) -0.013(2) 0.003(2) -0.013(2) N11 0.049(3) 0.046(3) 0.024(3) -0.003(2) -0.004(2) -0.032(3) C17 0.027(3) 0.027(3) 0.025(3) -0.013(2) 0.001(2) -0.008(2) C38 0.032(3) 0.026(3) 0.025(3) -0.011(2) 0.012(2) -0.013(3) C42 0.028(3) 0.027(3) 0.021(3) -0.011(2) 0.006(2) -0.018(2) C26 0.036(3) 0.042(4) 0.023(3) -0.014(3) 0.008(2) -0.023(3) C40 0.021(3) 0.023(3) 0.025(3) -0.007(2) 0.006(2) -0.011(2) C56 0.026(3) 0.033(3) 0.041(4) -0.010(3) -0.004(3) -0.012(3) C52 0.034(3) 0.029(3) 0.024(3) -0.016(2) 0.007(2) -0.017(3) C21 0.027(3) 0.039(3) 0.020(3) -0.012(2) 0.007(2) -0.021(3) C19 0.027(3) 0.034(3) 0.024(3) -0.010(2) 0.004(2) -0.016(3) C60 0.044(4) 0.041(4) 0.027(3) -0.018(3) 0.009(3) -0.031(3) N9 0.034(3) 0.037(3) 0.035(3) 0.006(2) 0.004(2) -0.004(2) C57 0.038(4) 0.033(3) 0.030(3) 0.002(3) -0.015(3) -0.016(3) C49 0.032(3) 0.025(3) 0.030(3) -0.010(2) 0.008(2) -0.011(3) C33 0.034(3) 0.019(3) 0.036(3) -0.007(2) 0.001(3) -0.001(3) C14 0.026(3) 0.033(3) 0.030(3) -0.020(3) 0.008(2) -0.015(3) C43 0.041(4) 0.033(3) 0.024(3) -0.007(3) 0.001(2) -0.019(3) C41 0.033(3) 0.028(3) 0.027(3) -0.004(2) -0.001(2) -0.018(3) C55 0.024(3) 0.031(3) 0.025(3) -0.010(2) 0.002(2) -0.011(3) C39 0.022(3) 0.029(3) 0.034(3) -0.014(3) 0.006(2) -0.006(2) C8 0.032(3) 0.023(3) 0.027(3) -0.004(2) 0.001(2) -0.012(3) C5 0.033(3) 0.035(3) 0.022(3) -0.007(2) 0.003(2) -0.011(3) C58 0.033(3) 0.032(3) 0.018(3) -0.006(2) -0.003(2) -0.019(3) C59 0.036(3) 0.037(3) 0.026(3) -0.013(3) 0.001(2) -0.020(3) F10 0.101(4) 0.051(3) 0.151(5) -0.017(3) 0.038(4) -0.059(3) C7 0.030(3) 0.025(3) 0.020(3) -0.006(2) 0.007(2) -0.010(3) C51 0.041(4) 0.032(3) 0.040(3) -0.023(3) 0.022(3) -0.021(3) C15 0.032(3) 0.045(4) 0.024(3) -0.022(3) 0.001(2) -0.014(3) C3 0.022(3) 0.026(3) 0.023(3) 0.001(2) 0.000(2) -0.008(2) C50 0.034(4) 0.029(3) 0.047(4) -0.018(3) 0.016(3) -0.010(3) C22 0.031(3) 0.042(4) 0.034(3) -0.021(3) 0.005(2) -0.018(3) C4 0.030(3) 0.033(3) 0.028(3) -0.006(3) 0.002(2) -0.011(3) F1 0.109(4) 0.102(4) 0.026(2) -0.004(2) 0.003(2) 0.044(3) C24 0.026(3) 0.080(5) 0.026(3) -0.018(3) 0.004(2) -0.028(4) C25 0.044(4) 0.056(4) 0.029(3) -0.019(3) 0.010(3) -0.035(4) C63 0.068(5) 0.081(5) 0.026(3) -0.023(3) 0.017(3) -0.055(4) C23 0.027(3) 0.057(4) 0.036(3) -0.021(3) 0.007(3) -0.022(3) C16 0.036(3) 0.036(3) 0.018(3) -0.005(2) 0.002(2) -0.007(3) C32 0.025(3) 0.024(3) 0.032(3) -0.010(2) 0.007(2) -0.004(2) C13 0.062(5) 0.042(4) 0.039(4) -0.014(3) 0.016(3) -0.029(4) C1 0.026(3) 0.043(4) 0.036(3) 0.007(3) -0.010(3) -0.013(3) C61 0.069(5) 0.078(5) 0.025(3) -0.026(3) 0.015(3) -0.060(5) C66 0.090(7) 0.112(8) 0.028(4) -0.002(4) -0.002(4) -0.077(6) C46 0.055(4) 0.043(4) 0.025(3) -0.012(3) 0.012(3) -0.023(3) C9 0.052(4) 0.038(4) 0.063(4) -0.026(3) 0.025(3) -0.030(3) C62 0.058(5) 0.061(5) 0.021(3) -0.005(3) 0.000(3) -0.043(4) F3 0.092(5) 0.150(6) 0.082(4) -0.038(4) 0.009(3) 0.048(4) C6 0.038(4) 0.046(4) 0.032(3) -0.007(3) -0.010(3) -0.016(3) C64 0.087(6) 0.081(6) 0.023(3) -0.001(4) -0.006(4) -0.056(5) C44 0.033(4) 0.048(4) 0.034(3) 0.006(3) 0.006(3) -0.011(3) C2 0.027(3) 0.040(4) 0.041(4) -0.001(3) 0.001(3) -0.005(3) C47 0.058(5) 0.051(4) 0.027(3) -0.004(3) 0.007(3) -0.026(4) C11 0.062(5) 0.031(4) 0.090(6) -0.001(4) 0.010(4) -0.032(4) F2 0.214(9) 0.140(7) 0.099(5) -0.026(5) -0.024(5) -0.086(6) C48 0.046(5) 0.075(6) 0.053(5) 0.035(4) 0.007(4) -0.005(4) C12 0.074(6) 0.053(5) 0.057(5) -0.007(4) 0.024(4) -0.045(4) B1 0.059(6) 0.032(4) 0.066(6) -0.017(4) 0.012(5) -0.006(4) C45 0.049(5) 0.070(6) 0.064(5) 0.029(4) 0.019(4) 0.005(4) C28 0.029(3) 0.052(4) 0.042(4) -0.028(3) 0.009(3) -0.021(3) C10 0.076(6) 0.037(4) 0.101(7) -0.036(4) 0.028(5) -0.035(4) C30 0.092(6) 0.067(5) 0.060(5) -0.031(4) -0.003(4) -0.055(5) C27 0.077(7) 0.148(10) 0.160(10) -0.120(9) 0.038(6) -0.080(7) C29 0.216(17) 0.179(14) 0.215(15) -0.144(13) 0.036(13) -0.140(13) C65 0.106(7) 0.128(8) 0.020(4) -0.022(4) 0.017(4) -0.099(7) F5 0.214(8) 0.084(4) 0.103(4) -0.057(4) 0.062(5) -0.077(5) F7 0.167(7) 0.180(8) 0.162(7) -0.127(6) 0.067(6) -0.089(6) F8 0.175(8) 0.279(11) 0.169(7) -0.138(8) 0.030(6) -0.147(8) B2 0.078(8) 0.081(8) 0.079(7) -0.044(6) 0.011(6) -0.035(7) F6 0.228(11) 0.126(7) 0.366(16) 0.012(9) -0.191(12) -0.048(7) _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 N3 2.042(4) . ? Rh1 N6 2.055(4) . ? Rh1 N5 2.056(5) . ? Rh1 N1 2.059(5) . ? Rh1 N13 2.210(5) . ? Rh1 Rh2 2.6188(8) . ? Rh2 N2 2.057(4) . ? Rh2 N8 2.059(4) . ? Rh2 N4 2.065(4) . ? Rh2 N7 2.066(5) . ? Rh2 N14 2.255(5) . ? N13 C28 1.127(7) . ? N14 C30 1.119(8) . ? N3 C20 1.327(7) . ? N3 C18 1.440(6) . ? N6 C40 1.333(7) . ? N6 C36 1.379(7) . ? N8 C49 1.349(7) . ? N8 C53 1.361(7) . ? N5 C31 1.335(7) . ? N5 C35 1.386(6) . ? N1 C7 1.329(7) . ? N1 C3 1.438(7) . ? F11 C15 1.371(6) . ? N7 C55 1.335(7) . ? N7 C54 1.367(7) . ? N2 C7 1.316(7) . ? N2 C8 1.427(7) . ? N4 C20 1.330(6) . ? N4 C21 1.438(7) . ? F12 C24 1.376(7) . ? F9 C1 1.371(7) . ? N10 C42 1.322(6) . ? N10 C43 1.356(7) . ? C36 C37 1.405(7) . ? C36 C35 1.443(7) . ? C54 C58 1.389(7) . ? C54 C53 1.448(7) . ? C18 C17 1.390(7) . ? C18 C19 1.399(7) . ? C53 C52 1.412(7) . ? F4 B1 1.343(10) . ? C37 C38 1.414(7) . ? C37 C42 1.456(7) . ? C31 C32 1.399(8) . ? C34 C35 1.395(8) . ? C34 C33 1.414(8) . ? C34 C41 1.474(8) . ? N12 C60 1.339(7) . ? N12 C61 1.353(8) . ? N11 C59 1.331(7) . ? N11 C62 1.342(8) . ? C17 C16 1.400(7) . ? C38 C39 1.366(8) . ? C42 C41 1.437(8) . ? C26 C25 1.392(8) . ? C26 C21 1.394(8) . ? C40 C39 1.388(7) . ? C56 C57 1.371(8) . ? C56 C55 1.381(8) . ? C52 C51 1.406(8) . ? C52 C60 1.466(8) . ? C21 C22 1.390(8) . ? C19 C14 1.390(7) . ? C60 C59 1.432(8) . ? N9 C41 1.315(7) . ? N9 C44 1.371(8) . ? C57 C58 1.416(8) . ? C49 C50 1.392(8) . ? C33 C32 1.382(8) . ? C14 C15 1.368(8) . ? C43 C44 1.409(9) . ? C43 C46 1.440(8) . ? C8 C13 1.378(8) . ? C8 C9 1.389(8) . ? C5 C6 1.384(8) . ? C5 C3 1.399(8) . ? C58 C59 1.459(8) . ? F10 C11 1.356(7) . ? C51 C50 1.359(8) . ? C15 C16 1.384(8) . ? C3 C4 1.405(8) . ? C22 C23 1.378(8) . ? C4 C2 1.401(8) . ? F1 B1 1.313(10) . ? C24 C23 1.372(9) . ? C24 C25 1.374(9) . ? C63 C65 1.372(10) . ? C63 C61 1.437(9) . ? C13 C12 1.398(9) . ? C1 C2 1.358(9) . ? C1 C6 1.385(9) . ? C61 C62 1.429(10) . ? C66 C64 1.360(11) . ? C66 C65 1.435(13) . ? C46 C47 1.353(9) . ? C9 C10 1.397(9) . ? C62 C64 1.435(9) . ? F3 B1 1.325(11) . ? C44 C45 1.439(9) . ? C47 C48 1.404(10) . ? C11 C10 1.359(11) . ? C11 C12 1.370(11) . ? F2 B1 1.432(11) . ? C48 C45 1.358(10) . ? C28 C27 1.472(10) . ? C30 C29 1.490(11) . ? F5 B2 1.324(12) . ? F7 B2 1.363(12) . ? F8 B2 1.371(13) . ? B2 F6 1.287(14) . ? 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 N3 Rh1 N6 174.80(17) . . ? N3 Rh1 N5 93.93(17) . . ? N6 Rh1 N5 80.88(17) . . ? N3 Rh1 N1 87.97(17) . . ? N6 Rh1 N1 97.22(17) . . ? N5 Rh1 N1 178.03(16) . . ? N3 Rh1 N13 95.46(15) . . ? N6 Rh1 N13 84.56(15) . . ? N5 Rh1 N13 85.43(16) . . ? N1 Rh1 N13 94.92(17) . . ? N3 Rh1 Rh2 85.08(12) . . ? N6 Rh1 Rh2 94.85(11) . . ? N5 Rh1 Rh2 94.04(12) . . ? N1 Rh1 Rh2 85.60(12) . . ? N13 Rh1 Rh2 179.26(11) . . ? N2 Rh2 N8 94.44(18) . . ? N2 Rh2 N4 88.38(17) . . ? N8 Rh2 N4 176.94(17) . . ? N2 Rh2 N7 174.79(17) . . ? N8 Rh2 N7 80.36(18) . . ? N4 Rh2 N7 96.81(17) . . ? N2 Rh2 N14 93.34(17) . . ? N8 Rh2 N14 83.58(16) . . ? N4 Rh2 N14 97.45(16) . . ? N7 Rh2 N14 86.46(17) . . ? N2 Rh2 Rh1 84.97(12) . . ? N8 Rh2 Rh1 93.36(12) . . ? N4 Rh2 Rh1 85.71(12) . . ? N7 Rh2 Rh1 94.93(11) . . ? N14 Rh2 Rh1 176.39(12) . . ? C28 N13 Rh1 175.7(5) . . ? C30 N14 Rh2 163.1(6) . . ? C20 N3 C18 114.8(4) . . ? C20 N3 Rh1 121.7(3) . . ? C18 N3 Rh1 123.5(3) . . ? C40 N6 C36 117.8(4) . . ? C40 N6 Rh1 129.2(4) . . ? C36 N6 Rh1 112.8(3) . . ? C49 N8 C53 118.1(4) . . ? C49 N8 Rh2 128.4(4) . . ? C53 N8 Rh2 113.5(3) . . ? C31 N5 C35 118.0(5) . . ? C31 N5 Rh1 128.1(4) . . ? C35 N5 Rh1 113.7(3) . . ? C7 N1 C3 114.8(5) . . ? C7 N1 Rh1 120.2(4) . . ? C3 N1 Rh1 125.0(3) . . ? C55 N7 C54 117.6(5) . . ? C55 N7 Rh2 129.0(4) . . ? C54 N7 Rh2 113.4(3) . . ? C7 N2 C8 116.5(5) . . ? C7 N2 Rh2 121.5(4) . . ? C8 N2 Rh2 121.9(4) . . ? C20 N4 C21 114.6(4) . . ? C20 N4 Rh2 119.4(3) . . ? C21 N4 Rh2 125.9(3) . . ? C42 N10 C43 116.7(5) . . ? N6 C36 C37 122.4(5) . . ? N6 C36 C35 117.4(4) . . ? C37 C36 C35 120.2(5) . . ? N7 C54 C58 122.9(5) . . ? N7 C54 C53 116.1(5) . . ? C58 C54 C53 121.0(5) . . ? N3 C20 N4 124.1(5) . . ? C17 C18 C19 119.9(5) . . ? C17 C18 N3 120.6(5) . . ? C19 C18 N3 119.6(5) . . ? N8 C53 C52 122.2(5) . . ? N8 C53 C54 116.7(4) . . ? C52 C53 C54 121.0(5) . . ? C36 C37 C38 117.5(5) . . ? C36 C37 C42 119.2(5) . . ? C38 C37 C42 123.3(5) . . ? N5 C31 C32 122.4(5) . . ? C35 C34 C33 117.6(5) . . ? C35 C34 C41 119.0(5) . . ? C33 C34 C41 123.4(5) . . ? C60 N12 C61 116.6(6) . . ? N5 C35 C34 122.8(5) . . ? N5 C35 C36 115.2(5) . . ? C34 C35 C36 122.0(5) . . ? C59 N11 C62 116.9(6) . . ? C18 C17 C16 120.2(5) . . ? C39 C38 C37 119.2(5) . . ? N10 C42 C41 122.0(5) . . ? N10 C42 C37 117.3(5) . . ? C41 C42 C37 120.7(4) . . ? C25 C26 C21 120.4(6) . . ? N6 C40 C39 122.7(5) . . ? C57 C56 C55 120.9(6) . . ? C51 C52 C53 117.6(5) . . ? C51 C52 C60 124.2(5) . . ? C53 C52 C60 118.3(5) . . ? C22 C21 C26 118.6(5) . . ? C22 C21 N4 120.4(5) . . ? C26 C21 N4 120.9(5) . . ? C14 C19 C18 120.1(5) . . ? N12 C60 C59 121.8(5) . . ? N12 C60 C52 117.8(6) . . ? C59 C60 C52 120.4(5) . . ? C41 N9 C44 116.2(5) . . ? C56 C57 C58 117.8(5) . . ? N8 C49 C50 122.5(5) . . ? C32 C33 C34 119.2(5) . . ? C15 C14 C19 118.7(5) . . ? N10 C43 C44 121.3(5) . . ? N10 C43 C46 119.3(6) . . ? C44 C43 C46 119.4(5) . . ? N9 C41 C42 122.0(5) . . ? N9 C41 C34 119.2(5) . . ? C42 C41 C34 118.8(5) . . ? N7 C55 C56 122.5(5) . . ? C38 C39 C40 120.3(5) . . ? C13 C8 C9 118.3(5) . . ? C13 C8 N2 120.9(5) . . ? C9 C8 N2 120.8(5) . . ? C6 C5 C3 120.4(6) . . ? C54 C58 C57 118.3(5) . . ? C54 C58 C59 119.7(5) . . ? C57 C58 C59 122.0(5) . . ? N11 C59 C60 121.7(5) . . ? N11 C59 C58 118.8(5) . . ? C60 C59 C58 119.5(5) . . ? N2 C7 N1 123.9(5) . . ? C50 C51 C52 119.9(5) . . ? C14 C15 F11 119.3(5) . . ? C14 C15 C16 123.1(5) . . ? F11 C15 C16 117.6(5) . . ? C5 C3 C4 119.0(5) . . ? C5 C3 N1 121.9(5) . . ? C4 C3 N1 119.1(5) . . ? C51 C50 C49 119.7(6) . . ? C23 C22 C21 122.0(6) . . ? C2 C4 C3 120.1(6) . . ? C23 C24 C25 123.2(6) . . ? C23 C24 F12 118.9(6) . . ? C25 C24 F12 117.9(6) . . ? C24 C25 C26 118.3(6) . . ? C65 C63 C61 118.4(8) . . ? C24 C23 C22 117.5(6) . . ? C15 C16 C17 118.0(5) . . ? C33 C32 C31 119.9(5) . . ? C8 C13 C12 121.7(6) . . ? C2 C1 F9 118.3(6) . . ? C2 C1 C6 122.5(6) . . ? F9 C1 C6 119.2(6) . . ? N12 C61 C62 121.0(5) . . ? N12 C61 C63 118.9(7) . . ? C62 C61 C63 120.1(6) . . ? C64 C66 C65 120.2(8) . . ? C47 C46 C43 120.2(6) . . ? C8 C9 C10 120.8(6) . . ? N11 C62 C61 121.9(6) . . ? N11 C62 C64 119.1(7) . . ? C61 C62 C64 119.0(6) . . ? C5 C6 C1 119.0(6) . . ? C66 C64 C62 120.3(9) . . ? N9 C44 C43 121.7(5) . . ? N9 C44 C45 120.6(6) . . ? C43 C44 C45 117.6(6) . . ? C1 C2 C4 118.9(6) . . ? C46 C47 C48 121.2(6) . . ? F10 C11 C10 118.3(7) . . ? F10 C11 C12 118.9(7) . . ? C10 C11 C12 122.8(6) . . ? C45 C48 C47 119.9(7) . . ? C11 C12 C13 117.7(7) . . ? F1 B1 F3 116.4(8) . . ? F1 B1 F4 114.6(7) . . ? F3 B1 F4 113.8(9) . . ? F1 B1 F2 110.5(9) . . ? F3 B1 F2 96.5(7) . . ? F4 B1 F2 102.4(7) . . ? C48 C45 C44 121.6(8) . . ? N13 C28 C27 174.6(8) . . ? C11 C10 C9 118.7(7) . . ? N14 C30 C29 176.3(11) . . ? C63 C65 C66 122.0(7) . . ? F6 B2 F5 106.4(10) . . ? F6 B2 F7 119.5(12) . . ? F5 B2 F7 113.3(10) . . ? F6 B2 F8 102.5(11) . . ? F5 B2 F8 111.8(10) . . ? F7 B2 F8 102.8(9) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 1.672 _refine_diff_density_min -1.678 _refine_diff_density_rms 0.210 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 _platon_squeeze_void_content 1 0.000 0.152 0.348 707 257 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 937903' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_d:\xray\yong033\1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H54 B2 F12 N16 Rh2' _chemical_formula_weight 1670.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.698(3) _cell_length_b 26.636(5) _cell_length_c 23.354(7) _cell_angle_alpha 90.00 _cell_angle_beta 123.59(2) _cell_angle_gamma 90.00 _cell_volume 7616(3) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.457 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3368 _exptl_absorpt_coefficient_mu 0.518 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9264 _exptl_absorpt_correction_T_max 0.9796 _exptl_absorpt_process_details 'SADABS, V2.3 Bruker (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 63251 _diffrn_reflns_av_R_equivalents 0.0960 _diffrn_reflns_av_sigmaI/netI 0.0817 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 24.07 _reflns_number_total 11719 _reflns_number_gt 8215 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0931P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11719 _refine_ls_number_parameters 995 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0871 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1709 _refine_ls_wR_factor_gt 0.1578 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _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 -0.31651(4) -0.142711(17) 0.18598(2) 0.03184(16) Uani 1 1 d . . . Rh2 Rh -0.18276(4) -0.156191(18) 0.14664(2) 0.03373(16) Uani 1 1 d . . . N1 N -0.2334(4) -0.22938(18) 0.1317(2) 0.0370(12) Uani 1 1 d . . . N2 N -0.3839(4) -0.20974(18) 0.1367(2) 0.0391(12) Uani 1 1 d . . . N3 N -0.3179(4) -0.13967(18) 0.0500(2) 0.0368(12) Uani 1 1 d . . . N4 N -0.4144(4) -0.10643(17) 0.0937(2) 0.0331(11) Uani 1 1 d . . . N5 N -0.2179(4) -0.17694(18) 0.2797(2) 0.0337(11) Uani 1 1 d . . . N6 N -0.2338(3) -0.08061(17) 0.2448(2) 0.0313(11) Uani 1 1 d . . . N7 N -0.0473(4) -0.16483(19) 0.2448(2) 0.0365(12) Uani 1 1 d . . . N8 N -0.1263(4) -0.08384(18) 0.1655(2) 0.0319(11) Uani 1 1 d . . . N9 N 0.0648(4) -0.14058(19) 0.5136(2) 0.0421(13) Uani 1 1 d . . . N10 N 0.0673(4) -0.03933(18) 0.4739(2) 0.0352(12) Uani 1 1 d . . . N11 N 0.2427(4) -0.0665(2) 0.4307(3) 0.0462(14) Uani 1 1 d . . . N12 N 0.1706(4) 0.0178(2) 0.3402(3) 0.0482(14) Uani 1 1 d . . . N13 N -0.0610(4) -0.1683(2) 0.1185(3) 0.0477(14) Uani 1 1 d . . . N14 N -0.4319(4) -0.12861(19) 0.2163(2) 0.0393(12) Uani 1 1 d . . . C1 C -0.7064(6) -0.2502(3) 0.0604(6) 0.081(3) Uani 1 1 d . . . C2 C -0.6753(7) -0.2438(3) 0.0159(5) 0.087(3) Uani 1 1 d . . . H2 H -0.7262 -0.2480 -0.0321 0.104 Uiso 1 1 calc R . . C3 C -0.5679(6) -0.2309(3) 0.0419(4) 0.060(2) Uani 1 1 d . . . H3 H -0.5447 -0.2269 0.0113 0.072 Uiso 1 1 calc R . . C4 C -0.4944(5) -0.2239(2) 0.1111(3) 0.0434(16) Uani 1 1 d . . . C5 C -0.5278(5) -0.2319(2) 0.1561(4) 0.0499(17) Uani 1 1 d . . . H5 H -0.4769 -0.2283 0.2043 0.060 Uiso 1 1 calc R . . C6 C -0.6355(6) -0.2451(3) 0.1304(5) 0.066(2) Uani 1 1 d . . . H6 H -0.6594 -0.2505 0.1603 0.079 Uiso 1 1 calc R . . C7 C -0.3288(5) -0.2404(2) 0.1228(3) 0.0376(15) Uani 1 1 d . . . H7 H -0.3590 -0.2727 0.1051 0.045 Uiso 1 1 calc R . . C8 C -0.1447(5) -0.3109(3) 0.1748(4) 0.0531(18) Uani 1 1 d . . . H8 H -0.1625 -0.3095 0.2081 0.064 Uiso 1 1 calc R . . C9 C -0.1758(5) -0.2717(2) 0.1291(3) 0.0446(16) Uani 1 1 d . . . C10 C -0.1488(7) -0.2743(3) 0.0808(4) 0.070(2) Uani 1 1 d . . . H1 H -0.1692 -0.2478 0.0488 0.084 Uiso 1 1 calc R . . C11 C -0.0914(8) -0.3160(3) 0.0787(5) 0.092(3) Uani 1 1 d . . . H4 H -0.0729 -0.3183 0.0458 0.111 Uiso 1 1 calc R . . C12 C -0.0636(8) -0.3531(3) 0.1265(6) 0.084(3) Uani 1 1 d . . . C13 C -0.0881(6) -0.3528(3) 0.1740(5) 0.067(2) Uani 1 1 d . . . H13 H -0.0680 -0.3797 0.2055 0.080 Uiso 1 1 calc R . . C14 C -0.5980(5) 0.0041(2) 0.0524(3) 0.0412(15) Uani 1 1 d . . . H14 H -0.5973 0.0395 0.0478 0.049 Uiso 1 1 calc R . . C15 C -0.5085(5) -0.0250(2) 0.0679(3) 0.0363(14) Uani 1 1 d . . . H15 H -0.4463 -0.0095 0.0730 0.044 Uiso 1 1 calc R . . C16 C -0.5094(5) -0.0766(2) 0.0760(3) 0.0356(14) Uani 1 1 d . . . C17 C -0.6036(5) -0.0996(2) 0.0668(3) 0.0448(16) Uani 1 1 d . . . H17 H -0.6050 -0.1348 0.0727 0.054 Uiso 1 1 calc R . . C18 C -0.6924(5) -0.0708(3) 0.0494(3) 0.0512(18) Uani 1 1 d . . . H18 H -0.7572 -0.0859 0.0411 0.061 Uiso 1 1 calc R . . C19 C -0.6867(5) -0.0196(3) 0.0441(3) 0.0454(17) Uani 1 1 d . . . C20 C -0.4046(5) -0.1168(2) 0.0421(3) 0.0353(14) Uani 1 1 d . . . H20 H -0.4624 -0.1074 -0.0030 0.042 Uiso 1 1 calc R . . C21 C -0.3295(5) -0.1536(2) -0.0133(3) 0.0384(15) Uani 1 1 d . . . C22 C -0.2534(6) -0.1392(2) -0.0271(3) 0.0441(16) Uani 1 1 d . . . H22 H -0.1915 -0.1204 0.0062 0.053 Uiso 1 1 calc R . . C23 C -0.2652(7) -0.1517(3) -0.0881(4) 0.059(2) Uani 1 1 d . . . H23 H -0.2123 -0.1420 -0.0973 0.071 Uiso 1 1 calc R . . C24 C -0.3575(7) -0.1789(3) -0.1358(4) 0.065(2) Uani 1 1 d . . . C25 C -0.4341(7) -0.1942(3) -0.1241(3) 0.061(2) Uani 1 1 d . . . H25 H -0.4957 -0.2131 -0.1577 0.073 Uiso 1 1 calc R . . C26 C -0.4201(5) -0.1817(2) -0.0619(3) 0.0464(17) Uani 1 1 d . . . H26 H -0.4723 -0.1923 -0.0525 0.056 Uiso 1 1 calc R . . C27 C -0.5841(6) -0.1053(3) 0.2359(4) 0.079(3) Uani 1 1 d . . . H27A H -0.6447 -0.0898 0.1939 0.119 Uiso 1 1 calc R . . H27B H -0.5555 -0.0815 0.2742 0.119 Uiso 1 1 calc R . . H27C H -0.6102 -0.1356 0.2465 0.119 Uiso 1 1 calc R . . C28 C -0.4977(5) -0.1189(3) 0.2259(3) 0.0478(17) Uani 1 1 d . . . C29 C 0.1045(8) -0.1826(5) 0.1083(6) 0.136(5) Uani 1 1 d . . . H29A H 0.1145 -0.2187 0.1058 0.204 Uiso 1 1 calc R . . H29B H 0.1709 -0.1684 0.1484 0.204 Uiso 1 1 calc R . . H29C H 0.0901 -0.1662 0.0665 0.204 Uiso 1 1 calc R . . C30 C 0.0123(6) -0.1743(3) 0.1147(4) 0.063(2) Uani 1 1 d . . . C31 C -0.2176(5) -0.2252(2) 0.2945(3) 0.0370(14) Uani 1 1 d . . . H31 H -0.2659 -0.2477 0.2588 0.044 Uiso 1 1 calc R . . C32 C -0.1476(5) -0.2441(2) 0.3618(3) 0.0415(15) Uani 1 1 d . . . H32 H -0.1491 -0.2787 0.3712 0.050 Uiso 1 1 calc R . . C33 C -0.0784(5) -0.2123(2) 0.4128(3) 0.0406(15) Uani 1 1 d . . . H33 H -0.0292 -0.2248 0.4580 0.049 Uiso 1 1 calc R . . C34 C -0.0792(4) -0.1607(2) 0.3990(3) 0.0326(14) Uani 1 1 d . . . C35 C -0.1509(5) -0.1446(2) 0.3315(3) 0.0318(14) Uani 1 1 d . . . C36 C -0.1569(4) -0.0922(2) 0.3128(3) 0.0307(13) Uani 1 1 d . . . C37 C -0.0879(4) -0.0563(2) 0.3603(3) 0.0280(13) Uani 1 1 d . . . C38 C -0.0990(4) -0.0068(2) 0.3396(3) 0.0326(14) Uani 1 1 d . . . H38 H -0.0522 0.0184 0.3711 0.039 Uiso 1 1 calc R . . C39 C -0.1798(5) 0.0058(2) 0.2715(3) 0.0355(14) Uani 1 1 d . . . H39 H -0.1897 0.0397 0.2563 0.043 Uiso 1 1 calc R . . C40 C -0.2451(5) -0.0320(2) 0.2269(3) 0.0346(14) Uani 1 1 d . . . H40 H -0.3007 -0.0231 0.1810 0.042 Uiso 1 1 calc R . . C41 C -0.0036(4) -0.1243(2) 0.4510(3) 0.0339(14) Uani 1 1 d . . . C42 C -0.0051(4) -0.0725(2) 0.4313(3) 0.0313(13) Uani 1 1 d . . . C43 C 0.1416(5) -0.1063(2) 0.5600(3) 0.0368(15) Uani 1 1 d . . . C44 C 0.1450(4) -0.0561(2) 0.5394(3) 0.0349(14) Uani 1 1 d . . . C45 C 0.2272(5) -0.0233(2) 0.5849(3) 0.0381(15) Uani 1 1 d . . . H45 H 0.2298 0.0098 0.5706 0.046 Uiso 1 1 calc R . . C46 C 0.2192(5) -0.1226(3) 0.6273(3) 0.0493(17) Uani 1 1 d . . . H46 H 0.2157 -0.1556 0.6413 0.059 Uiso 1 1 calc R . . C47 C 0.3021(5) -0.0895(3) 0.6736(3) 0.0422(16) Uani 1 1 d . . . C48 C 0.3068(5) -0.0392(3) 0.6523(3) 0.0428(16) Uani 1 1 d . . . C49 C 0.3923(5) -0.0063(3) 0.7006(3) 0.0470(17) Uani 1 1 d . . . H49 H 0.3977 0.0268 0.6874 0.056 Uiso 1 1 calc R . . C50 C 0.4659(5) -0.0228(3) 0.7657(3) 0.0558(19) Uani 1 1 d . . . H50 H 0.5222 -0.0007 0.7975 0.067 Uiso 1 1 calc R . . C51 C 0.4615(6) -0.0717(3) 0.7878(3) 0.058(2) Uani 1 1 d . . . H51 H 0.5135 -0.0817 0.8339 0.070 Uiso 1 1 calc R . . C52 C 0.3822(5) -0.1048(3) 0.7426(3) 0.0523(18) Uani 1 1 d . . . H52 H 0.3804 -0.1379 0.7572 0.063 Uiso 1 1 calc R . . C53 C -0.1648(5) -0.0442(2) 0.1233(3) 0.0368(14) Uani 1 1 d . . . H53 H -0.2311 -0.0480 0.0795 0.044 Uiso 1 1 calc R . . C54 C -0.1133(5) 0.0026(2) 0.1398(3) 0.0431(16) Uani 1 1 d . . . H54 H -0.1432 0.0294 0.1076 0.052 Uiso 1 1 calc R . . C55 C -0.0187(5) 0.0092(2) 0.2033(3) 0.0402(15) Uani 1 1 d . . . H55 H 0.0181 0.0406 0.2154 0.048 Uiso 1 1 calc R . . C56 C 0.0231(5) -0.0307(2) 0.2502(3) 0.0383(15) Uani 1 1 d . . . C57 C -0.0304(4) -0.0768(2) 0.2289(3) 0.0338(14) Uani 1 1 d . . . C58 C 0.0103(5) -0.1209(2) 0.2728(3) 0.0362(14) Uani 1 1 d . . . C59 C -0.0078(5) -0.2055(3) 0.2835(3) 0.0421(16) Uani 1 1 d . . . H59 H -0.0452 -0.2363 0.2645 0.051 Uiso 1 1 calc R . . C60 C 0.0847(5) -0.2060(3) 0.3500(3) 0.0480(17) Uani 1 1 d . . . H60 H 0.1087 -0.2365 0.3754 0.058 Uiso 1 1 calc R . . C61 C 0.1410(5) -0.1625(3) 0.3790(3) 0.0443(16) Uani 1 1 d . . . H61 H 0.2039 -0.1622 0.4247 0.053 Uiso 1 1 calc R . . C62 C 0.1041(5) -0.1179(2) 0.3397(3) 0.0410(15) Uani 1 1 d . . . C63 C 0.1590(5) -0.0688(2) 0.3661(3) 0.0399(15) Uani 1 1 d . . . C64 C 0.1212(5) -0.0264(2) 0.3206(3) 0.0375(15) Uani 1 1 d . . . C65 C 0.2946(5) -0.0205(3) 0.4522(3) 0.0468(17) Uani 1 1 d . . . C66 C 0.2599(5) 0.0213(3) 0.4070(3) 0.0498(18) Uani 1 1 d . . . C67 C 0.3178(5) 0.0669(3) 0.4295(4) 0.0531(18) Uani 1 1 d . . . H67 H 0.2938 0.0947 0.3990 0.064 Uiso 1 1 calc R . . C68 C 0.3876(5) -0.0160(3) 0.5197(3) 0.0549(19) Uani 1 1 d . . . H68 H 0.4110 -0.0436 0.5505 0.066 Uiso 1 1 calc R . . C69 C 0.4457(5) 0.0293(3) 0.5415(4) 0.056(2) Uani 1 1 d . . . C70 C 0.4111(6) 0.0717(3) 0.4968(4) 0.066(2) Uani 1 1 d . . . C71 C 0.4751(6) 0.1167(3) 0.5204(5) 0.077(3) Uani 1 1 d . . . H71 H 0.4534 0.1446 0.4903 0.092 Uiso 1 1 calc R . . C72 C 0.5657(7) 0.1201(4) 0.5845(5) 0.086(3) Uani 1 1 d . . . H72 H 0.6062 0.1505 0.5998 0.103 Uiso 1 1 calc R . . C73 C 0.6007(6) 0.0771(4) 0.6299(5) 0.081(3) Uani 1 1 d . . . H73 H 0.6652 0.0796 0.6748 0.097 Uiso 1 1 calc R . . C74 C 0.5437(5) 0.0330(3) 0.6100(4) 0.065(2) Uani 1 1 d . . . H74 H 0.5680 0.0053 0.6406 0.078 Uiso 1 1 calc R . . N15 N -0.2796(7) -0.1014(3) 0.4062(4) 0.087(2) Uani 1 1 d . . . C75 C -0.3595(8) -0.1876(3) 0.4022(6) 0.121(4) Uani 1 1 d . . . H75A H -0.4344 -0.1893 0.3614 0.181 Uiso 1 1 calc R . . H75B H -0.3601 -0.1933 0.4434 0.181 Uiso 1 1 calc R . . H75C H -0.3150 -0.2135 0.3991 0.181 Uiso 1 1 calc R . . C76 C -0.3146(7) -0.1393(4) 0.4059(5) 0.074(2) Uani 1 1 d . . . N16 N 0.3368(5) -0.4255(3) 0.3875(3) 0.0693(18) Uani 1 1 d . . . C77 C 0.2133(9) -0.3488(3) 0.3409(6) 0.116(4) Uani 1 1 d . . . H77A H 0.1501 -0.3566 0.2947 0.174 Uiso 1 1 calc R . . H77B H 0.2528 -0.3201 0.3385 0.174 Uiso 1 1 calc R . . H77C H 0.1882 -0.3405 0.3709 0.174 Uiso 1 1 calc R . . C78 C 0.2844(6) -0.3915(3) 0.3681(4) 0.0516(18) Uani 1 1 d . . . F12 F -0.7756(3) 0.00965(15) 0.0290(2) 0.0633(11) Uani 1 1 d . . . F11 F -0.3703(4) -0.1917(2) -0.1973(2) 0.0925(16) Uani 1 1 d . . . F8 F 0.3422(4) 0.7571(2) 0.3550(3) 0.1031(17) Uani 1 1 d . . . F10 F -0.8121(3) -0.2630(2) 0.0349(3) 0.115(2) Uani 1 1 d . . . F9 F -0.0052(5) -0.39343(17) 0.1255(4) 0.129(2) Uani 1 1 d . . . F6 F 0.3797(5) 0.7864(2) 0.2800(3) 0.127(2) Uani 1 1 d . . . F3 F 0.0281(7) 0.1463(3) 0.0639(4) 0.155(3) Uani 1 1 d . . . F7 F 0.2303(5) 0.8123(3) 0.2706(3) 0.134(2) Uani 1 1 d . . . F1 F -0.0622(7) 0.1004(3) 0.0979(5) 0.206(4) Uani 1 1 d . . . F5 F 0.2482(8) 0.7321(3) 0.2445(3) 0.181(4) Uani 1 1 d . . . B1 B -0.0231(9) 0.1412(4) 0.0952(7) 0.082(3) Uani 1 1 d . . . B2 B 0.2972(10) 0.7716(4) 0.2877(7) 0.082(3) Uani 1 1 d . . . F2 F 0.0552(10) 0.1504(5) 0.1590(5) 0.264(7) Uani 1 1 d . . . F4 F -0.0901(10) 0.1767(4) 0.0739(8) 0.302(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0265(3) 0.0372(3) 0.0266(3) -0.0006(2) 0.0115(2) 0.0016(2) Rh2 0.0297(3) 0.0398(3) 0.0277(3) 0.0000(2) 0.0133(2) 0.0053(2) N1 0.034(3) 0.040(3) 0.030(3) 0.000(2) 0.014(2) 0.008(2) N2 0.026(3) 0.044(3) 0.040(3) 0.001(2) 0.014(3) 0.000(2) N3 0.034(3) 0.038(3) 0.026(3) -0.004(2) 0.009(2) 0.005(2) N4 0.026(3) 0.038(3) 0.029(3) 0.000(2) 0.012(2) 0.007(2) N5 0.030(3) 0.036(3) 0.036(3) 0.001(2) 0.019(2) 0.002(2) N6 0.026(3) 0.040(3) 0.026(3) 0.004(2) 0.013(2) 0.009(2) N7 0.035(3) 0.047(3) 0.031(3) 0.005(2) 0.020(2) 0.011(3) N8 0.025(3) 0.041(3) 0.031(3) -0.004(2) 0.016(2) 0.004(2) N9 0.041(3) 0.049(3) 0.031(3) 0.004(2) 0.017(3) 0.002(3) N10 0.036(3) 0.045(3) 0.026(3) -0.001(2) 0.017(2) -0.002(2) N11 0.033(3) 0.068(4) 0.037(3) -0.009(3) 0.019(3) 0.001(3) N12 0.036(3) 0.056(4) 0.050(4) -0.014(3) 0.023(3) 0.000(3) N13 0.044(3) 0.058(4) 0.038(3) 0.005(3) 0.020(3) 0.016(3) N14 0.029(3) 0.044(3) 0.034(3) -0.001(2) 0.011(3) -0.002(2) C1 0.026(4) 0.065(6) 0.116(8) -0.004(5) 0.018(5) -0.022(4) C2 0.044(5) 0.094(7) 0.066(6) 0.013(5) -0.005(5) -0.028(5) C3 0.052(5) 0.059(5) 0.043(4) 0.000(4) 0.009(4) -0.010(4) C4 0.032(4) 0.037(4) 0.043(4) -0.004(3) 0.010(3) -0.002(3) C5 0.038(4) 0.045(4) 0.055(4) -0.006(3) 0.019(4) 0.000(3) C6 0.052(5) 0.052(5) 0.096(7) -0.006(4) 0.042(5) -0.010(4) C7 0.042(4) 0.034(3) 0.030(3) -0.003(3) 0.016(3) 0.005(3) C8 0.048(4) 0.049(4) 0.057(5) -0.003(4) 0.026(4) 0.006(3) C9 0.050(4) 0.041(4) 0.048(4) -0.002(3) 0.030(4) 0.005(3) C10 0.113(7) 0.045(4) 0.078(5) 0.001(4) 0.070(5) 0.015(4) C11 0.160(9) 0.049(5) 0.132(8) -0.001(5) 0.121(8) 0.018(6) C12 0.104(7) 0.041(5) 0.142(9) -0.003(5) 0.089(7) 0.018(5) C13 0.063(5) 0.051(5) 0.091(6) 0.014(4) 0.045(5) 0.012(4) C14 0.048(4) 0.045(4) 0.031(3) 0.005(3) 0.022(3) 0.010(3) C15 0.031(3) 0.045(4) 0.025(3) -0.001(3) 0.011(3) 0.000(3) C16 0.030(3) 0.038(4) 0.033(3) -0.002(3) 0.014(3) 0.005(3) C17 0.037(4) 0.044(4) 0.042(4) 0.005(3) 0.015(3) 0.004(3) C18 0.033(4) 0.058(5) 0.056(4) 0.012(4) 0.021(3) 0.009(3) C19 0.034(4) 0.062(5) 0.039(4) 0.013(3) 0.020(3) 0.022(3) C20 0.035(4) 0.038(4) 0.027(3) 0.002(3) 0.013(3) 0.001(3) C21 0.044(4) 0.034(3) 0.028(3) 0.000(3) 0.014(3) 0.010(3) C22 0.050(4) 0.048(4) 0.035(4) 0.004(3) 0.024(3) 0.012(3) C23 0.066(5) 0.072(5) 0.041(4) 0.015(4) 0.031(4) 0.033(4) C24 0.079(6) 0.069(5) 0.036(4) -0.001(4) 0.024(5) 0.032(5) C25 0.065(5) 0.062(5) 0.032(4) -0.008(3) 0.013(4) 0.016(4) C26 0.052(4) 0.046(4) 0.033(4) -0.003(3) 0.018(3) 0.008(3) C27 0.052(5) 0.116(7) 0.092(6) -0.017(5) 0.054(5) -0.008(5) C28 0.036(4) 0.054(4) 0.047(4) -0.009(3) 0.020(4) -0.003(3) C29 0.094(7) 0.229(14) 0.126(9) 0.034(9) 0.087(8) 0.070(9) C30 0.054(5) 0.097(6) 0.044(4) 0.009(4) 0.030(4) 0.026(4) C31 0.032(3) 0.041(4) 0.038(4) 0.000(3) 0.020(3) 0.000(3) C32 0.035(4) 0.041(4) 0.043(4) 0.004(3) 0.017(3) -0.001(3) C33 0.033(4) 0.050(4) 0.035(4) 0.010(3) 0.016(3) 0.005(3) C34 0.027(3) 0.042(4) 0.028(3) 0.003(3) 0.014(3) 0.002(3) C35 0.030(3) 0.037(4) 0.030(3) -0.001(3) 0.017(3) 0.003(3) C36 0.025(3) 0.039(4) 0.031(3) -0.002(3) 0.017(3) 0.000(3) C37 0.025(3) 0.039(4) 0.023(3) -0.001(3) 0.016(3) 0.005(3) C38 0.031(3) 0.038(4) 0.027(3) -0.003(3) 0.015(3) -0.001(3) C39 0.040(4) 0.036(3) 0.036(4) -0.001(3) 0.024(3) 0.001(3) C40 0.029(3) 0.040(4) 0.035(3) 0.003(3) 0.018(3) 0.009(3) C41 0.028(3) 0.045(4) 0.029(3) 0.003(3) 0.016(3) 0.004(3) C42 0.025(3) 0.041(4) 0.035(3) 0.000(3) 0.021(3) 0.001(3) C43 0.037(4) 0.043(4) 0.029(3) -0.003(3) 0.017(3) 0.002(3) C44 0.030(3) 0.048(4) 0.025(3) -0.002(3) 0.014(3) 0.001(3) C45 0.037(4) 0.048(4) 0.033(4) -0.005(3) 0.022(3) 0.000(3) C46 0.049(4) 0.057(4) 0.032(4) 0.003(3) 0.016(3) 0.004(3) C47 0.037(4) 0.060(4) 0.028(3) -0.006(3) 0.017(3) 0.005(3) C48 0.038(4) 0.061(4) 0.028(3) -0.010(3) 0.018(3) 0.003(3) C49 0.038(4) 0.058(4) 0.041(4) -0.008(3) 0.020(3) -0.001(3) C50 0.043(4) 0.075(5) 0.039(4) -0.015(4) 0.016(4) 0.002(4) C51 0.054(5) 0.063(5) 0.037(4) 0.001(4) 0.012(4) 0.014(4) C52 0.053(4) 0.057(4) 0.030(4) -0.001(3) 0.012(3) 0.009(4) C53 0.037(4) 0.042(4) 0.034(3) 0.001(3) 0.021(3) 0.004(3) C54 0.042(4) 0.052(4) 0.038(4) 0.005(3) 0.024(3) 0.007(3) C55 0.046(4) 0.041(4) 0.042(4) -0.002(3) 0.030(4) 0.001(3) C56 0.031(3) 0.050(4) 0.036(4) 0.000(3) 0.020(3) 0.004(3) C57 0.023(3) 0.049(4) 0.029(3) -0.002(3) 0.014(3) 0.003(3) C58 0.028(3) 0.046(4) 0.033(3) -0.001(3) 0.016(3) 0.001(3) C59 0.035(4) 0.053(4) 0.035(4) 0.005(3) 0.017(3) 0.011(3) C60 0.041(4) 0.054(4) 0.040(4) 0.004(3) 0.017(4) 0.005(3) C61 0.026(3) 0.065(5) 0.026(3) 0.007(3) 0.004(3) 0.011(3) C62 0.032(4) 0.055(4) 0.034(4) 0.001(3) 0.017(3) 0.005(3) C63 0.030(3) 0.060(4) 0.034(4) -0.003(3) 0.020(3) 0.004(3) C64 0.026(3) 0.055(4) 0.032(3) -0.008(3) 0.016(3) -0.003(3) C65 0.034(4) 0.072(5) 0.038(4) -0.014(4) 0.023(3) -0.002(3) C66 0.036(4) 0.072(5) 0.043(4) -0.014(4) 0.023(4) 0.001(4) C67 0.027(4) 0.059(5) 0.061(5) -0.018(4) 0.017(4) -0.007(3) C68 0.034(4) 0.095(6) 0.040(4) -0.014(4) 0.023(3) 0.001(4) C69 0.028(4) 0.089(6) 0.053(5) -0.032(4) 0.023(4) -0.004(4) C70 0.040(4) 0.085(6) 0.072(6) -0.034(5) 0.030(4) 0.001(4) C71 0.044(5) 0.087(6) 0.091(6) -0.043(5) 0.033(5) -0.008(4) C72 0.048(5) 0.116(8) 0.088(7) -0.058(7) 0.034(5) -0.017(5) C73 0.038(5) 0.140(9) 0.064(6) -0.047(6) 0.028(4) -0.008(6) C74 0.039(4) 0.114(7) 0.044(4) -0.031(4) 0.024(4) -0.013(4) N15 0.106(6) 0.073(5) 0.107(6) -0.007(5) 0.076(5) -0.002(5) C75 0.103(8) 0.069(7) 0.213(13) -0.038(7) 0.101(9) -0.026(6) C76 0.066(6) 0.067(6) 0.094(7) -0.015(5) 0.048(5) 0.000(5) N16 0.069(5) 0.077(5) 0.055(4) 0.000(4) 0.030(4) 0.011(4) C77 0.103(8) 0.068(7) 0.187(12) 0.023(7) 0.086(9) 0.021(6) C78 0.046(4) 0.060(5) 0.051(5) -0.013(4) 0.028(4) -0.012(4) F12 0.054(2) 0.077(3) 0.067(3) 0.020(2) 0.038(2) 0.027(2) F11 0.105(4) 0.132(4) 0.037(2) -0.011(3) 0.037(3) 0.041(3) F8 0.111(4) 0.112(4) 0.082(4) -0.010(3) 0.051(3) -0.030(3) F10 0.042(3) 0.101(4) 0.157(5) 0.006(4) 0.027(3) -0.024(3) F9 0.169(5) 0.052(3) 0.250(8) 0.013(4) 0.169(6) 0.034(3) F6 0.131(5) 0.131(5) 0.152(6) 0.030(4) 0.099(5) 0.007(4) F3 0.205(8) 0.160(7) 0.169(7) -0.027(5) 0.146(7) -0.036(5) F7 0.103(4) 0.200(7) 0.091(4) 0.001(4) 0.047(4) 0.054(5) F1 0.203(8) 0.128(6) 0.230(9) 0.040(6) 0.084(7) -0.095(6) F5 0.290(10) 0.129(5) 0.091(4) -0.038(4) 0.085(6) -0.096(6) B1 0.051(6) 0.083(8) 0.109(10) 0.015(7) 0.044(7) -0.005(6) B2 0.072(8) 0.079(8) 0.095(9) -0.007(7) 0.046(7) -0.019(6) F2 0.263(12) 0.356(16) 0.106(7) -0.015(8) 0.060(8) -0.146(11) F4 0.278(12) 0.193(9) 0.59(2) 0.216(12) 0.339(16) 0.154(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 N5 2.052(5) . ? Rh1 N4 2.053(5) . ? Rh1 N2 2.057(5) . ? Rh1 N6 2.063(5) . ? Rh1 N14 2.202(6) . ? Rh1 Rh2 2.6146(8) . ? Rh2 N1 2.047(5) . ? Rh2 N8 2.048(5) . ? Rh2 N7 2.054(5) . ? Rh2 N3 2.067(5) . ? Rh2 N13 2.245(6) . ? N1 C7 1.331(7) . ? N1 C9 1.432(7) . ? N2 C7 1.312(7) . ? N2 C4 1.437(7) . ? N3 C20 1.330(7) . ? N3 C21 1.439(7) . ? N4 C20 1.320(7) . ? N4 C16 1.453(7) . ? N5 C31 1.332(7) . ? N5 C35 1.363(7) . ? N6 C40 1.343(7) . ? N6 C36 1.381(7) . ? N7 C59 1.321(7) . ? N7 C58 1.379(7) . ? N8 C53 1.339(7) . ? N8 C57 1.380(7) . ? N9 C41 1.308(7) . ? N9 C43 1.389(7) . ? N10 C42 1.316(7) . ? N10 C44 1.382(7) . ? N11 C63 1.318(7) . ? N11 C65 1.382(8) . ? N12 C64 1.325(8) . ? N12 C66 1.378(8) . ? N13 C30 1.139(8) . ? N14 C28 1.136(8) . ? C1 C2 1.358(13) . ? C1 F10 1.365(8) . ? C1 C6 1.375(12) . ? C2 C3 1.385(10) . ? C3 C4 1.372(9) . ? C4 C5 1.401(9) . ? C5 C6 1.393(9) . ? C8 C9 1.378(9) . ? C8 C13 1.397(9) . ? C9 C10 1.389(9) . ? C10 C11 1.411(10) . ? C11 C12 1.372(12) . ? C12 C13 1.343(12) . ? C12 F9 1.384(8) . ? C14 C19 1.362(9) . ? C14 C15 1.393(8) . ? C15 C16 1.387(8) . ? C16 C17 1.418(8) . ? C17 C18 1.369(8) . ? C18 C19 1.376(9) . ? C19 F12 1.388(7) . ? C21 C22 1.378(9) . ? C21 C26 1.396(8) . ? C22 C23 1.377(9) . ? C23 C24 1.391(11) . ? C24 C25 1.359(11) . ? C24 F11 1.384(8) . ? C25 C26 1.391(9) . ? C27 C28 1.459(10) . ? C29 C30 1.461(11) . ? C31 C32 1.411(8) . ? C32 C33 1.352(8) . ? C33 C34 1.411(8) . ? C34 C35 1.393(8) . ? C34 C41 1.468(8) . ? C35 C36 1.450(8) . ? C36 C37 1.390(7) . ? C37 C38 1.384(8) . ? C37 C42 1.478(7) . ? C38 C39 1.400(8) . ? C39 C40 1.385(8) . ? C41 C42 1.451(8) . ? C43 C46 1.405(8) . ? C43 C44 1.433(8) . ? C44 C45 1.389(8) . ? C45 C48 1.411(8) . ? C46 C47 1.405(9) . ? C47 C52 1.431(8) . ? C47 C48 1.444(9) . ? C48 C49 1.434(8) . ? C49 C50 1.362(9) . ? C50 C51 1.417(10) . ? C51 C52 1.374(9) . ? C53 C54 1.397(8) . ? C54 C55 1.371(8) . ? C55 C56 1.402(8) . ? C56 C57 1.393(8) . ? C56 C64 1.474(8) . ? C57 C58 1.453(8) . ? C58 C62 1.401(8) . ? C59 C60 1.389(8) . ? C60 C61 1.367(9) . ? C61 C62 1.413(8) . ? C62 C63 1.479(9) . ? C63 C64 1.437(8) . ? C65 C68 1.409(9) . ? C65 C66 1.422(9) . ? C66 C67 1.408(9) . ? C67 C70 1.407(9) . ? C68 C69 1.401(10) . ? C69 C70 1.428(11) . ? C69 C74 1.447(9) . ? C70 C71 1.431(11) . ? C71 C72 1.348(11) . ? C72 C73 1.446(13) . ? C73 C74 1.367(12) . ? N15 C76 1.131(10) . ? C75 C76 1.427(12) . ? N16 C78 1.111(9) . ? C77 C78 1.432(11) . ? F8 B2 1.381(13) . ? F6 B2 1.378(12) . ? F3 B1 1.314(13) . ? F7 B2 1.366(13) . ? F1 B1 1.248(11) . ? F5 B2 1.356(12) . ? B1 F4 1.253(12) . ? B1 F2 1.306(14) . ? 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 N5 Rh1 N4 178.26(19) . . ? N5 Rh1 N2 92.75(19) . . ? N4 Rh1 N2 88.90(18) . . ? N5 Rh1 N6 80.65(18) . . ? N4 Rh1 N6 97.72(18) . . ? N2 Rh1 N6 173.05(18) . . ? N5 Rh1 N14 87.02(18) . . ? N4 Rh1 N14 92.27(18) . . ? N2 Rh1 N14 96.29(19) . . ? N6 Rh1 N14 85.62(17) . . ? N5 Rh1 Rh2 95.11(13) . . ? N4 Rh1 Rh2 85.57(13) . . ? N2 Rh1 Rh2 84.68(14) . . ? N6 Rh1 Rh2 93.66(12) . . ? N14 Rh1 Rh2 177.62(13) . . ? N1 Rh2 N8 177.56(18) . . ? N1 Rh2 N7 96.89(19) . . ? N8 Rh2 N7 80.68(19) . . ? N1 Rh2 N3 88.71(18) . . ? N8 Rh2 N3 93.73(18) . . ? N7 Rh2 N3 174.10(19) . . ? N1 Rh2 N13 95.0(2) . . ? N8 Rh2 N13 84.47(19) . . ? N7 Rh2 N13 82.69(18) . . ? N3 Rh2 N13 98.70(19) . . ? N1 Rh2 Rh1 85.27(14) . . ? N8 Rh2 Rh1 95.13(12) . . ? N7 Rh2 Rh1 94.39(13) . . ? N3 Rh2 Rh1 84.21(14) . . ? N13 Rh2 Rh1 177.09(13) . . ? C7 N1 C9 114.6(5) . . ? C7 N1 Rh2 119.3(4) . . ? C9 N1 Rh2 126.1(4) . . ? C7 N2 C4 116.4(5) . . ? C7 N2 Rh1 120.5(4) . . ? C4 N2 Rh1 123.0(4) . . ? C20 N3 C21 114.6(5) . . ? C20 N3 Rh2 121.2(4) . . ? C21 N3 Rh2 124.2(4) . . ? C20 N4 C16 115.2(5) . . ? C20 N4 Rh1 119.5(4) . . ? C16 N4 Rh1 124.2(4) . . ? C31 N5 C35 118.8(5) . . ? C31 N5 Rh1 127.3(4) . . ? C35 N5 Rh1 113.8(4) . . ? C40 N6 C36 117.2(5) . . ? C40 N6 Rh1 129.8(4) . . ? C36 N6 Rh1 113.1(4) . . ? C59 N7 C58 116.7(5) . . ? C59 N7 Rh2 130.0(4) . . ? C58 N7 Rh2 113.4(4) . . ? C53 N8 C57 116.6(5) . . ? C53 N8 Rh2 128.9(4) . . ? C57 N8 Rh2 114.2(4) . . ? C41 N9 C43 116.4(5) . . ? C42 N10 C44 116.6(5) . . ? C63 N11 C65 115.9(6) . . ? C64 N12 C66 116.7(6) . . ? C30 N13 Rh2 169.6(5) . . ? C28 N14 Rh1 173.2(5) . . ? C2 C1 F10 118.8(9) . . ? C2 C1 C6 122.9(7) . . ? F10 C1 C6 118.3(10) . . ? C1 C2 C3 118.7(8) . . ? C4 C3 C2 120.8(8) . . ? C3 C4 C5 119.4(6) . . ? C3 C4 N2 119.8(6) . . ? C5 C4 N2 120.8(6) . . ? C6 C5 C4 120.1(7) . . ? C1 C6 C5 118.1(8) . . ? N2 C7 N1 124.4(6) . . ? C9 C8 C13 122.7(7) . . ? C8 C9 C10 118.0(6) . . ? C8 C9 N1 121.0(6) . . ? C10 C9 N1 121.0(6) . . ? C9 C10 C11 120.8(7) . . ? C12 C11 C10 116.9(8) . . ? C13 C12 C11 124.9(7) . . ? C13 C12 F9 118.1(8) . . ? C11 C12 F9 117.0(8) . . ? C12 C13 C8 116.7(7) . . ? C19 C14 C15 118.1(6) . . ? C16 C15 C14 120.6(6) . . ? C15 C16 C17 119.2(5) . . ? C15 C16 N4 120.1(5) . . ? C17 C16 N4 120.7(5) . . ? C18 C17 C16 119.6(6) . . ? C17 C18 C19 119.2(6) . . ? C14 C19 C18 123.2(6) . . ? C14 C19 F12 117.9(6) . . ? C18 C19 F12 118.9(6) . . ? N4 C20 N3 123.3(5) . . ? C22 C21 C26 119.4(6) . . ? C22 C21 N3 121.2(5) . . ? C26 C21 N3 119.4(6) . . ? C23 C22 C21 121.4(7) . . ? C22 C23 C24 117.5(8) . . ? C25 C24 F11 118.8(8) . . ? C25 C24 C23 123.0(7) . . ? F11 C24 C23 118.2(8) . . ? C24 C25 C26 118.5(7) . . ? C25 C26 C21 120.1(7) . . ? N14 C28 C27 178.0(8) . . ? N13 C30 C29 178.6(10) . . ? N5 C31 C32 121.9(6) . . ? C33 C32 C31 119.2(6) . . ? C32 C33 C34 120.1(6) . . ? C35 C34 C33 117.7(5) . . ? C35 C34 C41 119.0(5) . . ? C33 C34 C41 123.2(5) . . ? N5 C35 C34 122.2(5) . . ? N5 C35 C36 116.5(5) . . ? C34 C35 C36 121.3(5) . . ? N6 C36 C37 122.4(5) . . ? N6 C36 C35 115.9(5) . . ? C37 C36 C35 121.7(5) . . ? C38 C37 C36 119.0(5) . . ? C38 C37 C42 122.5(5) . . ? C36 C37 C42 118.6(5) . . ? C37 C38 C39 119.2(5) . . ? C40 C39 C38 118.7(5) . . ? N6 C40 C39 123.5(5) . . ? N9 C41 C42 122.5(5) . . ? N9 C41 C34 117.9(5) . . ? C42 C41 C34 119.6(5) . . ? N10 C42 C41 122.4(5) . . ? N10 C42 C37 118.1(5) . . ? C41 C42 C37 119.5(5) . . ? N9 C43 C46 118.4(6) . . ? N9 C43 C44 121.1(5) . . ? C46 C43 C44 120.5(6) . . ? N10 C44 C45 118.7(5) . . ? N10 C44 C43 120.8(5) . . ? C45 C44 C43 120.5(5) . . ? C44 C45 C48 119.9(6) . . ? C47 C46 C43 119.3(6) . . ? C46 C47 C52 120.7(6) . . ? C46 C47 C48 120.2(6) . . ? C52 C47 C48 119.1(6) . . ? C45 C48 C49 121.3(6) . . ? C45 C48 C47 119.7(6) . . ? C49 C48 C47 119.0(6) . . ? C50 C49 C48 119.3(7) . . ? C49 C50 C51 122.4(7) . . ? C52 C51 C50 120.0(6) . . ? C51 C52 C47 120.1(7) . . ? N8 C53 C54 123.8(6) . . ? C55 C54 C53 118.9(6) . . ? C54 C55 C56 119.4(6) . . ? C57 C56 C55 118.2(5) . . ? C57 C56 C64 118.6(6) . . ? C55 C56 C64 123.2(6) . . ? N8 C57 C56 122.8(5) . . ? N8 C57 C58 115.2(5) . . ? C56 C57 C58 122.0(5) . . ? N7 C58 C62 123.1(6) . . ? N7 C58 C57 116.4(5) . . ? C62 C58 C57 120.5(6) . . ? N7 C59 C60 124.2(6) . . ? C61 C60 C59 119.6(6) . . ? C60 C61 C62 118.9(6) . . ? C58 C62 C61 117.5(6) . . ? C58 C62 C63 119.3(6) . . ? C61 C62 C63 123.2(6) . . ? N11 C63 C64 122.9(6) . . ? N11 C63 C62 117.9(6) . . ? C64 C63 C62 119.2(5) . . ? N12 C64 C63 121.9(5) . . ? N12 C64 C56 117.8(6) . . ? C63 C64 C56 120.2(6) . . ? N11 C65 C68 118.8(7) . . ? N11 C65 C66 121.6(6) . . ? C68 C65 C66 119.4(7) . . ? N12 C66 C67 118.8(7) . . ? N12 C66 C65 120.9(6) . . ? C67 C66 C65 120.3(6) . . ? C70 C67 C66 120.7(7) . . ? C69 C68 C65 120.0(7) . . ? C68 C69 C70 121.1(6) . . ? C68 C69 C74 119.6(8) . . ? C70 C69 C74 119.3(7) . . ? C67 C70 C69 118.5(7) . . ? C67 C70 C71 122.2(9) . . ? C69 C70 C71 119.2(7) . . ? C72 C71 C70 121.3(10) . . ? C71 C72 C73 119.5(9) . . ? C74 C73 C72 121.9(8) . . ? C73 C74 C69 118.8(9) . . ? N15 C76 C75 176.9(11) . . ? N16 C78 C77 177.7(9) . . ? F1 B1 F4 113.2(10) . . ? F1 B1 F2 104.2(11) . . ? F4 B1 F2 108.4(14) . . ? F1 B1 F3 122.6(13) . . ? F4 B1 F3 105.6(11) . . ? F2 B1 F3 101.6(9) . . ? F5 B2 F7 113.5(10) . . ? F5 B2 F6 105.6(10) . . ? F7 B2 F6 106.1(9) . . ? F5 B2 F8 110.7(9) . . ? F7 B2 F8 111.5(10) . . ? F6 B2 F8 109.0(9) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 24.07 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.840 _refine_diff_density_min -0.848 _refine_diff_density_rms 0.129 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 _platon_squeeze_void_content 1 0.000 0.000 0.000 410 163 ' ' 2 0.000 0.500 0.500 410 163 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 937904' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_d:\xray\yong011b\mono1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H53 B2 F8 N13 Rh2' _chemical_formula_weight 1431.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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 ? _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 50.745(10) _cell_length_b 19.810(4) _cell_length_c 13.614(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.70(3) _cell_angle_gamma 90.00 _cell_volume 13490(5) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description PLATE _exptl_crystal_colour RED _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5792 _exptl_absorpt_coefficient_mu 0.562 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9460 _exptl_absorpt_correction_T_max 0.9779 _exptl_absorpt_process_details 'SADABS V2.3 (Bruker, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 63553 _diffrn_reflns_av_R_equivalents 0.0737 _diffrn_reflns_av_sigmaI/netI 0.0580 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 60 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 25.01 _reflns_number_total 11892 _reflns_number_gt 7329 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1064P)^2^+23.9212P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11892 _refine_ls_number_parameters 843 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0579 _refine_ls_wR_factor_ref 0.1962 _refine_ls_wR_factor_gt 0.1589 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.144617(10) 0.22836(3) 0.07635(4) 0.05020(18) Uani 1 1 d . . . Rh2 Rh 0.140037(10) 0.24254(3) 0.26237(4) 0.04941(18) Uani 1 1 d . . . N1 N 0.13348(12) 0.2527(3) 0.4142(4) 0.0556(15) Uani 1 1 d . . . N4 N 0.10947(10) 0.2714(3) 0.0110(4) 0.0574(14) Uani 1 1 d . . . N9 N 0.17835(10) 0.1780(3) 0.1318(4) 0.0515(13) Uani 1 1 d . . . N7 N 0.16531(10) 0.3159(3) 0.0944(4) 0.0526(13) Uani 1 1 d . . . N6 N 0.17013(10) 0.3117(3) 0.2670(4) 0.0517(13) Uani 1 1 d . . . N8 N 0.16894(10) 0.1698(3) 0.2918(4) 0.0502(12) Uani 1 1 d . . . N3 N 0.10804(10) 0.1789(3) 0.2492(4) 0.0570(14) Uani 1 1 d . . . C9 C 0.17626(12) 0.1340(3) 0.3848(5) 0.0495(15) Uani 1 1 d . . . N5 N 0.12214(11) 0.1427(3) 0.0459(4) 0.0565(14) Uani 1 1 d . . . N2 N 0.10965(11) 0.3122(3) 0.2290(4) 0.0608(14) Uani 1 1 d . . . C23 C 0.17646(13) 0.3360(3) 0.1835(5) 0.0532(16) Uani 1 1 d . . . H23 H 0.1899 0.3699 0.1883 0.064 Uiso 1 1 calc R . . C8 C 0.18360(13) 0.1556(3) 0.2238(5) 0.0516(15) Uani 1 1 d . . . H8 H 0.1988 0.1277 0.2421 0.062 Uiso 1 1 calc R . . C53 C 0.08957(13) 0.2250(3) -0.0146(5) 0.0570(17) Uani 1 1 d . . . C54 C 0.09627(13) 0.1560(3) 0.0050(5) 0.0567(17) Uani 1 1 d . . . C58 C 0.07784(14) 0.1036(4) -0.0193(5) 0.0653(19) Uani 1 1 d . . . C25 C 0.18865(12) 0.3267(3) 0.3545(5) 0.0496(15) Uani 1 1 d . . . C7 C 0.19765(13) 0.1680(3) 0.0688(5) 0.0522(15) Uani 1 1 d . . . C55 C 0.12969(15) 0.0784(4) 0.0598(5) 0.0667(19) Uani 1 1 d . . . H55 H 0.1477 0.0689 0.0891 0.080 Uiso 1 1 calc R . . N11 N 0.01835(13) 0.2130(4) -0.1097(5) 0.0797(19) Uani 1 1 d . . . C49 C 0.10412(14) 0.3361(4) -0.0100(5) 0.067(2) Uani 1 1 d . . . H49 H 0.1180 0.3683 0.0068 0.081 Uiso 1 1 calc R . . C2 C 0.20728(16) 0.1458(4) -0.0940(5) 0.071(2) Uani 1 1 d . . . H2 H 0.2013 0.1360 -0.1624 0.085 Uiso 1 1 calc R . . C6 C 0.22447(14) 0.1729(4) 0.1023(6) 0.075(2) Uani 1 1 d . . . H6 H 0.2308 0.1834 0.1702 0.090 Uiso 1 1 calc R . . C21 C 0.17010(13) 0.3547(3) 0.0114(5) 0.0552(16) Uani 1 1 d . . . C52 C 0.06381(14) 0.2444(4) -0.0580(5) 0.0660(19) Uani 1 1 d . . . C5 C 0.18889(14) 0.1547(3) -0.0318(5) 0.0582(17) Uani 1 1 d . . . H5 H 0.1703 0.1518 -0.0573 0.070 Uiso 1 1 calc R . . C11 C 0.17601(13) 0.0648(3) 0.3857(5) 0.0592(17) Uani 1 1 d . . . H11 H 0.1697 0.0406 0.3261 0.071 Uiso 1 1 calc R . . C22 C 0.17192(17) 0.3248(4) -0.0768(5) 0.079(2) Uani 1 1 d . . . H22 H 0.1699 0.2772 -0.0832 0.095 Uiso 1 1 calc R . . C59 C 0.05012(16) 0.1240(4) -0.0589(5) 0.074(2) Uani 1 1 d . . . C60 C 0.04326(15) 0.1933(4) -0.0769(5) 0.070(2) Uani 1 1 d . . . C68 C 0.1301(3) 0.2664(5) 0.5981(7) 0.123(4) Uani 1 1 d . . . H68A H 0.1280 0.3144 0.6123 0.185 Uiso 1 1 calc R . . H68B H 0.1463 0.2491 0.6400 0.185 Uiso 1 1 calc R . . H68C H 0.1145 0.2413 0.6123 0.185 Uiso 1 1 calc R . . C10 C 0.18513(13) 0.1685(3) 0.4724(5) 0.0564(16) Uani 1 1 d . . . H10 H 0.1853 0.2165 0.4730 0.068 Uiso 1 1 calc R . . C24 C 0.21539(13) 0.3119(4) 0.3603(5) 0.0665(19) Uani 1 1 d . . . H24 H 0.2213 0.2907 0.3054 0.080 Uiso 1 1 calc R . . C26 C 0.17988(14) 0.3559(3) 0.4359(5) 0.0590(17) Uani 1 1 d . . . H26 H 0.1615 0.3664 0.4339 0.071 Uiso 1 1 calc R . . C56 C 0.11232(17) 0.0247(4) 0.0332(6) 0.076(2) Uani 1 1 d . . . H56 H 0.1185 -0.0205 0.0407 0.091 Uiso 1 1 calc R . . C12 C 0.19384(15) 0.1326(4) 0.5596(5) 0.0669(19) Uani 1 1 d . . . H12 H 0.1999 0.1566 0.6196 0.080 Uiso 1 1 calc R . . C13 C 0.18484(15) 0.0305(4) 0.4724(6) 0.072(2) Uani 1 1 d . . . H13 H 0.1848 -0.0175 0.4712 0.087 Uiso 1 1 calc R . . C27 C 0.19875(17) 0.3696(4) 0.5210(6) 0.077(2) Uani 1 1 d . . . H27 H 0.1930 0.3892 0.5774 0.093 Uiso 1 1 calc R . . C20 C 0.1718(2) 0.4226(4) 0.0145(6) 0.097(3) Uani 1 1 d . . . H20 H 0.1689 0.4456 0.0731 0.117 Uiso 1 1 calc R . . C18 C 0.1766(2) 0.3622(4) -0.1569(6) 0.104(3) Uani 1 1 d . . . H18 H 0.1779 0.3398 -0.2177 0.125 Uiso 1 1 calc R . . C4 C 0.24229(16) 0.1629(5) 0.0392(7) 0.090(3) Uani 1 1 d . . . H4 H 0.2609 0.1644 0.0648 0.109 Uiso 1 1 calc R . . C3 C 0.23410(18) 0.1508(5) -0.0593(7) 0.088(3) Uani 1 1 d . . . C28 C 0.22549(18) 0.3552(5) 0.5250(6) 0.092(3) Uani 1 1 d . . . C29 C 0.23354(16) 0.3272(5) 0.4433(6) 0.091(3) Uani 1 1 d . . . H29 H 0.2520 0.3182 0.4443 0.109 Uiso 1 1 calc R . . C14 C 0.19383(16) 0.0629(4) 0.5611(5) 0.069(2) Uani 1 1 d . . . C17 C 0.1795(2) 0.4297(5) -0.1520(6) 0.103(3) Uani 1 1 d . . . C16 C 0.1842(3) 0.4717(5) -0.2419(8) 0.196(8) Uani 1 1 d . . . H16A H 0.2020 0.4619 -0.2570 0.295 Uiso 1 1 calc R . . H16B H 0.1830 0.5198 -0.2266 0.295 Uiso 1 1 calc R . . H16C H 0.1707 0.4603 -0.2997 0.295 Uiso 1 1 calc R . . C19 C 0.1774(3) 0.4593(4) -0.0642(7) 0.127(4) Uani 1 1 d . . . H19 H 0.1800 0.5067 -0.0571 0.152 Uiso 1 1 calc R . . C15 C 0.2038(2) 0.0248(4) 0.6561(6) 0.118(4) Uani 1 1 d . . . H15A H 0.1971 0.0467 0.7117 0.177 Uiso 1 1 calc R . . H15B H 0.2233 0.0249 0.6688 0.177 Uiso 1 1 calc R . . H15C H 0.1972 -0.0218 0.6495 0.177 Uiso 1 1 calc R . . C1 C 0.2544(2) 0.1402(6) -0.1304(8) 0.140(4) Uani 1 1 d . . . H1A H 0.2593 0.1840 -0.1555 0.209 Uiso 1 1 calc R . . H1B H 0.2464 0.1118 -0.1865 0.209 Uiso 1 1 calc R . . H1C H 0.2705 0.1181 -0.0944 0.209 Uiso 1 1 calc R . . C30 C 0.2453(2) 0.3711(8) 0.6183(8) 0.168(6) Uani 1 1 d . . . H30A H 0.2443 0.4192 0.6342 0.252 Uiso 1 1 calc R . . H30B H 0.2635 0.3604 0.6072 0.252 Uiso 1 1 calc R . . H30C H 0.2411 0.3441 0.6739 0.252 Uiso 1 1 calc R . . C36 C 0.08454(13) 0.2116(4) 0.2199(5) 0.0603(17) Uani 1 1 d . . . C35 C 0.08535(13) 0.2841(4) 0.2103(5) 0.0610(18) Uani 1 1 d . . . C40 C 0.06025(13) 0.1758(4) 0.2023(5) 0.067(2) Uani 1 1 d . . . C31 C 0.11180(17) 0.3785(4) 0.2290(6) 0.078(2) Uani 1 1 d . . . H31 H 0.1290 0.3987 0.2443 0.094 Uiso 1 1 calc R . . C37 C 0.10799(14) 0.1128(4) 0.2666(5) 0.0639(18) Uani 1 1 d . . . H37 H 0.1245 0.0902 0.2885 0.077 Uiso 1 1 calc R . . N12 N 0.01450(15) 0.3231(5) 0.1354(5) 0.104(3) Uani 1 1 d . . . N13 N 0.01304(13) 0.1800(4) 0.1424(5) 0.095(2) Uani 1 1 d . . . C57 C 0.08629(17) 0.0383(4) -0.0040(6) 0.075(2) Uani 1 1 d . . . H57 H 0.0739 0.0023 -0.0194 0.090 Uiso 1 1 calc R . . C34 C 0.06192(15) 0.3218(5) 0.1864(6) 0.074(2) Uani 1 1 d . . . N10 N 0.03134(15) 0.0756(4) -0.0740(5) 0.094(2) Uani 1 1 d . . . C42 C 0.03652(15) 0.2866(5) 0.1621(6) 0.084(2) Uani 1 1 d . . . C41 C 0.03554(14) 0.2145(5) 0.1680(5) 0.077(2) Uani 1 1 d . . . C39 C 0.06065(16) 0.1074(5) 0.2210(6) 0.079(2) Uani 1 1 d . . . H39 H 0.0445 0.0822 0.2114 0.095 Uiso 1 1 calc R . . C38 C 0.08444(16) 0.0762(4) 0.2536(6) 0.075(2) Uani 1 1 d . . . H38 H 0.0849 0.0292 0.2673 0.090 Uiso 1 1 calc R . . C51 C 0.05889(16) 0.3123(4) -0.0774(6) 0.080(2) Uani 1 1 d . . . H51 H 0.0414 0.3266 -0.1059 0.096 Uiso 1 1 calc R . . C50 C 0.07884(15) 0.3588(4) -0.0559(6) 0.079(2) Uani 1 1 d . . . H50 H 0.0757 0.4052 -0.0716 0.095 Uiso 1 1 calc R . . C67 C 0.13250(17) 0.2575(4) 0.4866(9) 0.083(3) Uani 1 1 d . . . C62 C -0.00055(17) 0.1652(6) -0.1263(6) 0.086(3) Uani 1 1 d . . . C43 C -0.00868(19) 0.2887(7) 0.1105(7) 0.107(4) Uani 1 1 d . . . C44 C -0.00929(17) 0.2178(7) 0.1129(6) 0.103(4) Uani 1 1 d . . . C45 C -0.03339(17) 0.1819(7) 0.0852(7) 0.118(4) Uani 1 1 d . . . H45 H -0.0337 0.1339 0.0864 0.142 Uiso 1 1 calc R . . C33 C 0.06467(19) 0.3910(5) 0.1858(7) 0.096(3) Uani 1 1 d . . . H33 H 0.0493 0.4189 0.1706 0.115 Uiso 1 1 calc R . . C61 C 0.00595(18) 0.0973(6) -0.1072(7) 0.098(3) Uani 1 1 d . . . C32 C 0.0892(2) 0.4193(5) 0.2068(7) 0.094(3) Uani 1 1 d . . . H32 H 0.0910 0.4670 0.2065 0.113 Uiso 1 1 calc R . . C66 C -0.02677(17) 0.1851(6) -0.1602(6) 0.103(3) Uani 1 1 d . . . H66 H -0.0310 0.2313 -0.1735 0.123 Uiso 1 1 calc R . . C65 C -0.0463(2) 0.1370(8) -0.1741(8) 0.127(4) Uani 1 1 d . . . H65 H -0.0642 0.1499 -0.1988 0.152 Uiso 1 1 calc R . . C48 C -0.0330(2) 0.3226(8) 0.0822(8) 0.139(5) Uani 1 1 d . . . H48 H -0.0331 0.3706 0.0816 0.166 Uiso 1 1 calc R . . C64 C -0.0404(2) 0.0696(8) -0.1530(10) 0.142(5) Uani 1 1 d . . . H64 H -0.0544 0.0372 -0.1627 0.171 Uiso 1 1 calc R . . C63 C -0.0152(2) 0.0494(6) -0.1190(8) 0.134(4) Uani 1 1 d . . . H63 H -0.0116 0.0033 -0.1030 0.161 Uiso 1 1 calc R . . C46 C -0.0569(2) 0.2190(10) 0.0560(9) 0.151(6) Uani 1 1 d . . . H46 H -0.0734 0.1963 0.0362 0.181 Uiso 1 1 calc R . . C47 C -0.0559(2) 0.2895(10) 0.0561(10) 0.158(7) Uani 1 1 d . . . H47 H -0.0720 0.3143 0.0372 0.190 Uiso 1 1 calc R . . B2 B 0.1236(3) 0.1077(6) 0.7503(10) 0.159(8) Uani 1 1 d D . . B1 B 0.1042(5) 0.4464(9) 0.5149(14) 0.43(4) Uani 1 1 d D . . F6 F 0.11129(14) 0.1160(4) 0.6574(5) 0.162(3) Uani 1 1 d D . . F1 F 0.1137(3) 0.4023(6) 0.4605(9) 0.272(6) Uani 1 1 d D . . F2 F 0.1199(3) 0.4913(10) 0.5631(14) 0.407(12) Uani 1 1 d D . . F4 F 0.0965(4) 0.4212(7) 0.5926(12) 0.352(9) Uani 1 1 d D . . F3 F 0.0878(6) 0.4789(10) 0.4449(15) 0.60(2) Uani 1 1 d D . . F5 F 0.14830(19) 0.0971(10) 0.7447(8) 0.394(12) Uani 1 1 d D . . F7 F 0.1243(3) 0.1620(5) 0.8074(7) 0.244(5) Uani 1 1 d D . . F8 F 0.1129(4) 0.0588(7) 0.7909(9) 0.355(10) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0464(3) 0.0546(3) 0.0475(3) -0.0010(2) 0.0022(2) -0.0041(2) Rh2 0.0429(3) 0.0545(3) 0.0514(3) -0.0023(2) 0.0098(2) -0.0024(2) N1 0.068(4) 0.062(4) 0.036(3) -0.011(3) 0.009(3) -0.008(3) N4 0.048(3) 0.060(4) 0.060(3) 0.007(3) -0.001(3) -0.004(3) N9 0.047(3) 0.059(3) 0.048(3) 0.000(3) 0.008(2) 0.000(2) N7 0.053(3) 0.054(3) 0.050(3) 0.001(3) 0.008(3) -0.008(2) N6 0.053(3) 0.054(3) 0.048(3) -0.002(2) 0.007(2) -0.008(2) N8 0.050(3) 0.054(3) 0.047(3) 0.000(2) 0.010(2) -0.001(2) N3 0.046(3) 0.066(4) 0.059(3) 0.000(3) 0.011(3) -0.003(3) C9 0.047(4) 0.052(4) 0.051(4) 0.004(3) 0.015(3) 0.000(3) N5 0.056(3) 0.062(4) 0.048(3) -0.003(3) -0.001(3) -0.004(3) N2 0.057(4) 0.060(4) 0.065(4) -0.002(3) 0.010(3) 0.003(3) C23 0.055(4) 0.051(4) 0.053(4) -0.005(3) 0.008(3) -0.006(3) C8 0.052(4) 0.050(4) 0.054(4) 0.001(3) 0.014(3) -0.002(3) C53 0.051(4) 0.067(5) 0.051(4) 0.005(3) 0.003(3) -0.008(3) C54 0.057(4) 0.065(5) 0.048(4) -0.005(3) 0.008(3) -0.018(3) C58 0.063(5) 0.081(6) 0.051(4) -0.004(4) 0.008(3) -0.020(4) C25 0.048(4) 0.050(4) 0.050(4) 0.003(3) 0.007(3) -0.007(3) C7 0.055(4) 0.052(4) 0.051(4) 0.001(3) 0.014(3) 0.002(3) C55 0.071(5) 0.066(5) 0.063(5) -0.002(4) 0.010(4) -0.002(4) N11 0.058(4) 0.116(5) 0.063(4) 0.015(4) 0.002(3) -0.017(4) C49 0.064(5) 0.058(5) 0.075(5) 0.011(4) -0.002(4) -0.012(4) C2 0.084(6) 0.080(5) 0.052(4) -0.013(4) 0.020(4) -0.019(4) C6 0.055(5) 0.108(6) 0.061(5) -0.010(4) 0.011(4) -0.014(4) C21 0.063(4) 0.050(4) 0.051(4) 0.000(3) 0.006(3) -0.003(3) C52 0.055(4) 0.081(5) 0.058(4) 0.012(4) -0.001(3) -0.011(4) C5 0.060(4) 0.065(4) 0.051(4) -0.003(3) 0.011(3) 0.001(3) C11 0.070(5) 0.053(4) 0.056(4) -0.005(3) 0.015(3) -0.004(3) C22 0.118(7) 0.066(5) 0.055(5) -0.006(4) 0.015(4) -0.002(5) C59 0.070(5) 0.093(6) 0.055(4) -0.002(4) 0.002(4) -0.028(4) C60 0.057(5) 0.100(6) 0.050(4) 0.010(4) 0.003(3) -0.016(4) C68 0.179(12) 0.131(9) 0.068(6) -0.001(6) 0.045(7) -0.004(8) C10 0.061(4) 0.053(4) 0.056(4) 0.000(3) 0.014(3) -0.005(3) C24 0.053(4) 0.083(5) 0.063(5) -0.005(4) 0.006(4) 0.002(4) C26 0.064(4) 0.051(4) 0.059(4) -0.003(3) 0.002(3) -0.002(3) C56 0.092(6) 0.060(5) 0.074(5) -0.005(4) 0.009(4) -0.016(4) C12 0.078(5) 0.072(5) 0.049(4) -0.003(4) 0.007(4) -0.007(4) C13 0.096(6) 0.049(4) 0.075(5) 0.001(4) 0.025(4) -0.004(4) C27 0.091(6) 0.076(5) 0.060(5) -0.015(4) 0.003(4) -0.001(4) C20 0.182(10) 0.061(5) 0.052(5) 0.001(4) 0.030(5) 0.006(6) C18 0.191(11) 0.071(6) 0.056(5) 0.004(4) 0.039(6) 0.009(6) C4 0.051(5) 0.148(8) 0.076(6) -0.006(5) 0.020(4) -0.006(5) C3 0.077(6) 0.108(7) 0.090(6) -0.013(5) 0.042(5) -0.008(5) C28 0.077(6) 0.116(7) 0.071(6) -0.006(5) -0.023(5) -0.004(5) C29 0.058(5) 0.140(8) 0.071(6) -0.009(5) 0.003(4) 0.005(5) C14 0.090(6) 0.057(5) 0.061(5) 0.015(4) 0.016(4) 0.004(4) C17 0.178(10) 0.072(6) 0.062(5) 0.014(4) 0.025(6) 0.004(6) C16 0.43(2) 0.094(8) 0.088(8) 0.021(6) 0.100(11) -0.038(11) C19 0.258(14) 0.056(5) 0.074(6) 0.005(5) 0.047(7) -0.024(7) C15 0.192(11) 0.079(6) 0.079(6) 0.029(5) 0.009(6) 0.012(7) C1 0.115(9) 0.194(12) 0.128(9) -0.033(8) 0.074(7) -0.016(8) C30 0.115(9) 0.274(17) 0.094(8) -0.049(9) -0.042(7) 0.003(10) C36 0.048(4) 0.080(5) 0.054(4) 0.000(3) 0.013(3) -0.003(4) C35 0.048(4) 0.079(5) 0.060(4) -0.001(4) 0.017(3) 0.007(4) C40 0.044(4) 0.096(6) 0.061(5) 0.001(4) 0.008(3) -0.006(4) C31 0.078(5) 0.070(5) 0.086(6) -0.003(4) 0.013(4) 0.017(4) C37 0.055(4) 0.067(5) 0.068(5) -0.002(4) 0.008(3) -0.014(3) N12 0.057(5) 0.170(8) 0.086(5) 0.018(5) 0.013(4) 0.032(5) N13 0.053(4) 0.166(8) 0.069(4) 0.005(4) 0.020(3) -0.017(5) C57 0.085(6) 0.063(5) 0.075(5) -0.007(4) 0.006(4) -0.028(4) C34 0.060(5) 0.093(6) 0.070(5) 0.005(4) 0.014(4) 0.016(4) N10 0.084(5) 0.108(6) 0.085(5) -0.002(4) -0.002(4) -0.045(4) C42 0.047(5) 0.131(8) 0.075(5) 0.008(5) 0.011(4) 0.011(5) C41 0.048(5) 0.133(8) 0.053(4) 0.000(5) 0.017(3) -0.011(5) C39 0.061(5) 0.109(7) 0.067(5) -0.006(5) 0.010(4) -0.031(5) C38 0.071(5) 0.073(5) 0.084(6) -0.003(4) 0.017(4) -0.020(4) C51 0.060(5) 0.087(6) 0.087(6) 0.017(5) -0.007(4) 0.000(4) C50 0.063(5) 0.075(5) 0.095(6) 0.017(4) 0.002(4) 0.003(4) C67 0.064(5) 0.060(5) 0.127(9) 0.000(5) 0.017(6) -0.006(4) C62 0.066(6) 0.121(8) 0.068(5) 0.002(5) 0.002(4) -0.032(5) C43 0.054(6) 0.185(12) 0.082(6) 0.016(7) 0.010(5) 0.027(7) C44 0.045(5) 0.208(13) 0.058(5) 0.009(7) 0.014(4) 0.009(7) C45 0.045(5) 0.226(13) 0.084(6) 0.014(7) 0.011(5) -0.013(6) C33 0.076(6) 0.101(8) 0.112(7) 0.007(6) 0.022(5) 0.027(5) C61 0.069(6) 0.137(9) 0.082(6) 0.002(6) -0.007(5) -0.050(6) C32 0.107(8) 0.078(6) 0.098(7) -0.002(5) 0.019(6) 0.020(6) C66 0.061(6) 0.165(10) 0.078(6) 0.008(6) -0.003(5) -0.034(6) C65 0.080(7) 0.203(14) 0.088(7) 0.013(8) -0.014(6) -0.035(9) C48 0.068(7) 0.239(15) 0.109(8) 0.026(9) 0.017(6) 0.031(8) C64 0.079(8) 0.180(13) 0.156(11) 0.016(10) -0.014(7) -0.054(8) C63 0.097(8) 0.156(11) 0.136(9) 0.019(8) -0.018(7) -0.045(8) C46 0.062(7) 0.31(2) 0.086(8) 0.035(12) 0.015(6) -0.019(11) C47 0.049(7) 0.30(2) 0.122(10) 0.043(14) 0.005(6) 0.000(11) B2 0.23(2) 0.076(9) 0.134(13) -0.004(9) -0.086(14) 0.053(11) B1 0.95(12) 0.23(3) 0.20(3) -0.13(2) 0.31(5) -0.35(5) F6 0.180(7) 0.162(6) 0.122(5) -0.023(4) -0.034(5) 0.045(5) F1 0.376(16) 0.227(11) 0.232(11) -0.002(9) 0.111(11) 0.135(11) F2 0.347(18) 0.48(3) 0.45(3) -0.21(2) 0.220(18) -0.229(19) F4 0.44(2) 0.251(14) 0.43(2) -0.096(14) 0.26(2) -0.116(15) F3 1.01(7) 0.30(2) 0.45(3) -0.02(2) 0.03(4) 0.30(3) F5 0.144(8) 0.81(4) 0.215(11) 0.002(17) -0.004(8) 0.190(15) F7 0.364(16) 0.196(10) 0.159(8) -0.014(7) 0.004(8) 0.020(10) F8 0.57(3) 0.263(14) 0.232(12) 0.037(10) 0.067(14) -0.193(17) _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 N9 2.015(5) . ? Rh1 N7 2.021(5) . ? Rh1 N4 2.041(5) . ? Rh1 N5 2.048(5) . ? Rh1 Rh2 2.5971(9) . ? Rh2 N3 2.040(5) . ? Rh2 N6 2.044(5) . ? Rh2 N8 2.048(5) . ? Rh2 N2 2.062(5) . ? Rh2 N1 2.158(6) . ? N1 C67 0.999(11) . ? N4 C49 1.330(8) . ? N4 C53 1.367(8) . ? N9 C8 1.313(8) . ? N9 C7 1.420(8) . ? N7 C23 1.310(7) . ? N7 C21 1.421(8) . ? N6 C23 1.323(8) . ? N6 C25 1.419(7) . ? N8 C8 1.312(7) . ? N8 C9 1.444(8) . ? N3 C37 1.331(8) . ? N3 C36 1.356(8) . ? C9 C11 1.370(8) . ? C9 C10 1.383(8) . ? N5 C55 1.334(8) . ? N5 C54 1.362(8) . ? N2 C31 1.317(9) . ? N2 C35 1.338(8) . ? C53 C52 1.395(9) . ? C53 C54 1.422(9) . ? C54 C58 1.398(9) . ? C58 C57 1.369(10) . ? C58 C59 1.475(10) . ? C25 C24 1.377(9) . ? C25 C26 1.388(9) . ? C7 C6 1.364(9) . ? C7 C5 1.392(9) . ? C55 C56 1.389(10) . ? N11 C60 1.326(9) . ? N11 C62 1.340(10) . ? C49 C50 1.403(9) . ? C2 C3 1.367(11) . ? C2 C5 1.373(9) . ? C6 C4 1.362(10) . ? C21 C20 1.348(10) . ? C21 C22 1.356(9) . ? C52 C51 1.386(10) . ? C52 C60 1.445(10) . ? C11 C13 1.371(9) . ? C22 C18 1.373(10) . ? C59 N10 1.344(9) . ? C59 C60 1.426(11) . ? C68 C67 1.553(14) . ? C10 C12 1.391(9) . ? C24 C29 1.366(10) . ? C26 C27 1.400(9) . ? C56 C57 1.359(10) . ? C12 C14 1.381(9) . ? C13 C14 1.376(10) . ? C27 C28 1.379(11) . ? C20 C19 1.364(11) . ? C18 C17 1.345(11) . ? C4 C3 1.356(11) . ? C3 C1 1.544(11) . ? C28 C29 1.365(12) . ? C28 C30 1.516(11) . ? C14 C15 1.509(10) . ? C17 C19 1.351(11) . ? C17 C16 1.532(11) . ? C36 C40 1.407(9) . ? C36 C35 1.444(10) . ? C35 C34 1.395(9) . ? C40 C39 1.379(11) . ? C40 C41 1.477(10) . ? C31 C32 1.396(11) . ? C37 C38 1.383(9) . ? N12 C42 1.329(10) . ? N12 C43 1.352(13) . ? N13 C41 1.326(10) . ? N13 C44 1.362(12) . ? C34 C33 1.379(12) . ? C34 C42 1.453(11) . ? N10 C61 1.361(11) . ? C42 C41 1.433(12) . ? C39 C38 1.361(10) . ? C51 C50 1.364(10) . ? C62 C66 1.390(12) . ? C62 C61 1.400(13) . ? C43 C48 1.400(13) . ? C43 C44 1.404(16) . ? C44 C45 1.411(13) . ? C45 C46 1.399(16) . ? C33 C32 1.350(12) . ? C61 C63 1.420(12) . ? C66 C65 1.364(13) . ? C65 C64 1.387(16) . ? C48 C47 1.333(17) . ? C64 C63 1.347(15) . ? C46 C47 1.40(2) . ? B2 F8 1.281(14) . ? B2 F5 1.287(14) . ? B2 F7 1.322(12) . ? B2 F6 1.323(11) . ? B1 F1 1.288(16) . ? B1 F4 1.290(15) . ? B1 F2 1.295(16) . ? B1 F3 1.323(18) . ? 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 N9 Rh1 N7 89.3(2) . . ? N9 Rh1 N4 174.3(2) . . ? N7 Rh1 N4 95.3(2) . . ? N9 Rh1 N5 94.3(2) . . ? N7 Rh1 N5 175.0(2) . . ? N4 Rh1 N5 80.9(2) . . ? N9 Rh1 Rh2 84.17(15) . . ? N7 Rh1 Rh2 85.31(14) . . ? N4 Rh1 Rh2 99.49(16) . . ? N5 Rh1 Rh2 98.55(15) . . ? N3 Rh2 N6 175.1(2) . . ? N3 Rh2 N8 96.6(2) . . ? N6 Rh2 N8 87.7(2) . . ? N3 Rh2 N2 80.8(2) . . ? N6 Rh2 N2 94.9(2) . . ? N8 Rh2 N2 177.1(2) . . ? N3 Rh2 N1 83.9(2) . . ? N6 Rh2 N1 98.2(2) . . ? N8 Rh2 N1 95.7(2) . . ? N2 Rh2 N1 85.3(2) . . ? N3 Rh2 Rh1 92.76(15) . . ? N6 Rh2 Rh1 85.03(14) . . ? N8 Rh2 Rh1 86.34(14) . . ? N2 Rh2 Rh1 92.51(15) . . ? N1 Rh2 Rh1 176.23(16) . . ? C67 N1 Rh2 174.1(8) . . ? C49 N4 C53 118.6(6) . . ? C49 N4 Rh1 128.9(5) . . ? C53 N4 Rh1 112.5(4) . . ? C8 N9 C7 118.6(5) . . ? C8 N9 Rh1 123.2(4) . . ? C7 N9 Rh1 118.2(4) . . ? C23 N7 C21 117.8(5) . . ? C23 N7 Rh1 120.5(4) . . ? C21 N7 Rh1 121.5(4) . . ? C23 N6 C25 115.0(5) . . ? C23 N6 Rh2 120.4(4) . . ? C25 N6 Rh2 123.5(4) . . ? C8 N8 C9 114.9(5) . . ? C8 N8 Rh2 119.0(4) . . ? C9 N8 Rh2 126.0(4) . . ? C37 N3 C36 119.6(6) . . ? C37 N3 Rh2 128.2(5) . . ? C36 N3 Rh2 112.2(5) . . ? C11 C9 C10 119.3(6) . . ? C11 C9 N8 119.8(6) . . ? C10 C9 N8 120.7(6) . . ? C55 N5 C54 118.5(6) . . ? C55 N5 Rh1 128.7(5) . . ? C54 N5 Rh1 112.8(4) . . ? C31 N2 C35 119.2(6) . . ? C31 N2 Rh2 127.5(5) . . ? C35 N2 Rh2 113.2(5) . . ? N7 C23 N6 123.7(6) . . ? N8 C8 N9 123.6(6) . . ? N4 C53 C52 121.4(6) . . ? N4 C53 C54 117.2(6) . . ? C52 C53 C54 121.4(6) . . ? N5 C54 C58 120.9(7) . . ? N5 C54 C53 116.5(6) . . ? C58 C54 C53 122.6(7) . . ? C57 C58 C54 119.0(7) . . ? C57 C58 C59 124.7(7) . . ? C54 C58 C59 116.2(7) . . ? C24 C25 C26 119.2(6) . . ? C24 C25 N6 120.7(6) . . ? C26 C25 N6 120.1(6) . . ? C6 C7 C5 118.5(6) . . ? C6 C7 N9 122.6(6) . . ? C5 C7 N9 118.8(6) . . ? N5 C55 C56 122.6(7) . . ? C60 N11 C62 117.6(8) . . ? N4 C49 C50 122.9(7) . . ? C3 C2 C5 121.2(7) . . ? C4 C6 C7 120.7(7) . . ? C20 C21 C22 116.8(7) . . ? C20 C21 N7 122.2(6) . . ? C22 C21 N7 120.9(6) . . ? C51 C52 C53 118.3(7) . . ? C51 C52 C60 123.0(7) . . ? C53 C52 C60 118.6(7) . . ? C2 C5 C7 119.6(7) . . ? C9 C11 C13 120.1(6) . . ? C21 C22 C18 121.0(8) . . ? N10 C59 C60 121.0(8) . . ? N10 C59 C58 117.9(8) . . ? C60 C59 C58 121.1(7) . . ? N11 C60 C59 122.2(7) . . ? N11 C60 C52 118.1(8) . . ? C59 C60 C52 119.7(7) . . ? C9 C10 C12 119.5(6) . . ? C29 C24 C25 121.4(7) . . ? C25 C26 C27 118.4(7) . . ? C57 C56 C55 118.7(7) . . ? C14 C12 C10 121.5(7) . . ? C11 C13 C14 122.4(7) . . ? C28 C27 C26 121.6(7) . . ? C21 C20 C19 121.8(8) . . ? C17 C18 C22 121.9(8) . . ? C3 C4 C6 121.6(7) . . ? C4 C3 C2 118.4(7) . . ? C4 C3 C1 121.2(8) . . ? C2 C3 C1 120.3(9) . . ? C29 C28 C27 118.7(7) . . ? C29 C28 C30 121.3(9) . . ? C27 C28 C30 120.0(9) . . ? C28 C29 C24 120.7(8) . . ? C13 C14 C12 117.1(6) . . ? C13 C14 C15 122.2(7) . . ? C12 C14 C15 120.8(7) . . ? C18 C17 C19 116.8(8) . . ? C18 C17 C16 122.0(9) . . ? C19 C17 C16 121.2(9) . . ? C17 C19 C20 121.5(8) . . ? N3 C36 C40 120.8(7) . . ? N3 C36 C35 117.7(6) . . ? C40 C36 C35 121.5(7) . . ? N2 C35 C34 122.9(7) . . ? N2 C35 C36 115.9(6) . . ? C34 C35 C36 121.2(7) . . ? C39 C40 C36 118.6(7) . . ? C39 C40 C41 123.6(7) . . ? C36 C40 C41 117.8(8) . . ? N2 C31 C32 120.8(8) . . ? N3 C37 C38 121.3(7) . . ? C42 N12 C43 116.8(10) . . ? C41 N13 C44 115.4(9) . . ? C56 C57 C58 120.2(7) . . ? C33 C34 C35 116.8(8) . . ? C33 C34 C42 124.2(8) . . ? C35 C34 C42 119.0(8) . . ? C59 N10 C61 115.6(8) . . ? N12 C42 C41 121.5(8) . . ? N12 C42 C34 118.4(9) . . ? C41 C42 C34 120.2(7) . . ? N13 C41 C42 122.4(8) . . ? N13 C41 C40 117.6(9) . . ? C42 C41 C40 120.0(7) . . ? C38 C39 C40 119.4(7) . . ? C39 C38 C37 120.3(8) . . ? C50 C51 C52 120.8(7) . . ? C51 C50 C49 117.9(7) . . ? N1 C67 C68 178.1(11) . . ? N11 C62 C66 118.2(10) . . ? N11 C62 C61 120.6(8) . . ? C66 C62 C61 121.1(9) . . ? N12 C43 C48 121.0(13) . . ? N12 C43 C44 121.3(9) . . ? C48 C43 C44 117.7(12) . . ? N13 C44 C43 122.5(9) . . ? N13 C44 C45 116.2(12) . . ? C43 C44 C45 121.3(10) . . ? C46 C45 C44 118.0(13) . . ? C32 C33 C34 120.2(8) . . ? N10 C61 C62 123.1(8) . . ? N10 C61 C63 118.8(11) . . ? C62 C61 C63 118.1(10) . . ? C33 C32 C31 120.0(9) . . ? C65 C66 C62 118.6(11) . . ? C66 C65 C64 121.3(11) . . ? C47 C48 C43 121.8(15) . . ? C63 C64 C65 120.9(11) . . ? C64 C63 C61 119.8(12) . . ? C47 C46 C45 119.9(13) . . ? C48 C47 C46 121.3(14) . . ? F8 B2 F5 113.0(12) . . ? F8 B2 F7 109.5(13) . . ? F5 B2 F7 103.6(14) . . ? F8 B2 F6 109.8(13) . . ? F5 B2 F6 105.7(13) . . ? F7 B2 F6 115.1(10) . . ? F1 B1 F4 113.7(15) . . ? F1 B1 F2 120.2(19) . . ? F4 B1 F2 95.5(15) . . ? F1 B1 F3 99.6(16) . . ? F4 B1 F3 123(2) . . ? F2 B1 F3 106.8(16) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.950 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.099 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 _platon_squeeze_void_content 1 0.000 0.500 -0.012 661 79 ' ' 2 0.242 0.497 -0.048 27 2 ' ' 3 0.258 0.003 0.047 27 2 ' ' 4 0.500 0.000 0.005 661 79 ' ' 5 0.742 -0.003 -0.048 27 2 ' ' 6 0.758 0.503 0.047 27 2 ' ' 7 0.213 0.741 0.239 18 1 ' ' 8 0.713 0.241 0.239 18 1 ' ' 9 0.287 0.241 0.261 18 1 ' ' 10 0.787 0.741 0.261 18 1 ' ' 11 0.000 0.063 0.250 7 1 ' ' 12 0.500 0.563 0.250 7 1 ' ' 13 0.242 0.503 0.452 27 2 ' ' 14 0.742 1.003 0.452 27 2 ' ' 15 0.258 -0.003 0.547 27 2 ' ' 16 0.758 0.497 0.547 27 2 ' ' 17 0.213 0.259 0.739 18 1 ' ' 18 0.713 0.759 0.739 18 1 ' ' 19 0.287 0.759 0.761 18 1 ' ' 20 0.787 0.259 0.761 18 1 ' ' 21 0.000 0.938 0.750 7 1 ' ' 22 0.500 0.438 0.750 7 1 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 937905' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_2 _vrf_PLAT029 ; PROBLEM: diffrn_measured_fraction_theta_full Low ....... 0.939 RESPONSE: The data was collected at synchrotron ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H63 B Cl F4 N15 Rh2' _chemical_formula_weight 1562.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0000 0.0010 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0040 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.0550 0.0530 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -0.3410 2.3820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.056(2) _cell_length_b 19.244(4) _cell_length_c 19.431(4) _cell_angle_alpha 97.18(3) _cell_angle_beta 94.07(3) _cell_angle_gamma 102.62(3) _cell_volume 3622.0(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_F_000 1592 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.040 _exptl_crystal_size_min 0.010 _exptl_absorpt_coefficient_mu 0.630 _shelx_estimated_absorpt_T_min 0.969 _shelx_estimated_absorpt_T_max 0.994 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.41328 _diffrn_radiation_type ? _diffrn_source ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 95222 _diffrn_reflns_av_unetI/netI 0.0660 _diffrn_reflns_av_R_equivalents 0.0482 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 0.617 _diffrn_reflns_theta_max 20.243 _diffrn_reflns_theta_full 14.357 _diffrn_measured_fraction_theta_max 0.870 _diffrn_measured_fraction_theta_full 0.939 _diffrn_reflns_Laue_measured_fraction_max 0.870 _diffrn_reflns_Laue_measured_fraction_full 0.939 _diffrn_reflns_point_group_measured_fraction_max 0.870 _diffrn_reflns_point_group_measured_fraction_full 0.939 _reflns_number_total 30986 _reflns_number_gt 21988 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2013 (Sheldrick, 2013)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; ? ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 30986 _refine_ls_number_parameters 935 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0501 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1547 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 0.093 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Rh1 Rh 0.28053(2) 0.25981(2) 0.62861(2) 0.01414(4) Uani 1 1 d . . . . . Rh2 Rh 0.48093(2) 0.33663(2) 0.71505(2) 0.01505(4) Uani 1 1 d . . . . . Cl1 Cl 0.07368(6) 0.18606(4) 0.55805(3) 0.02345(12) Uani 1 1 d . . . . . N7 N 0.1789(2) 0.22611(11) 0.70940(10) 0.0154(3) Uani 1 1 d . . . . . N6 N 0.6140(2) 0.27364(11) 0.69166(10) 0.0161(4) Uani 1 1 d . . . . . N3 N 0.4038(2) 0.29584(11) 0.55277(10) 0.0178(4) Uani 1 1 d . . . . . N5 N 0.4619(2) 0.27759(11) 0.79632(10) 0.0166(4) Uani 1 1 d . . . . . N8 N 0.3417(2) 0.16578(10) 0.63323(10) 0.0151(3) Uani 1 1 d . . . . . N2 N 0.3449(2) 0.39828(11) 0.74005(11) 0.0188(4) Uani 1 1 d . . . . . N4 N 0.5187(2) 0.39287(11) 0.63427(11) 0.0179(4) Uani 1 1 d . . . . . F4 F 0.90523(18) 0.36489(10) 0.77748(9) 0.0302(4) Uani 1 1 d . . . . . N1 N 0.2099(2) 0.35334(11) 0.63448(10) 0.0170(4) Uani 1 1 d . . . . . C35 C 0.2035(2) 0.16417(12) 0.72781(12) 0.0153(4) Uani 1 1 d . . . . . N9 N 0.1462(2) 0.04765(12) 0.86115(11) 0.0205(4) Uani 1 1 d . . . . . C20 C 0.4210(3) 0.26076(14) 0.48637(12) 0.0195(4) Uani 1 1 d . . . . . C23 C 0.4816(3) 0.36202(13) 0.56973(12) 0.0188(4) Uani 1 1 d . . . . . H23 H 0.5117 0.3883 0.5332 0.023 Uiso 1 1 calc R U . . . C42 C 0.1877(2) 0.07016(13) 0.80365(12) 0.0169(4) Uani 1 1 d . . . . . C58 C 0.5343(2) 0.22568(13) 0.79191(12) 0.0169(4) Uani 1 1 d . . . . . C36 C 0.2916(2) 0.13020(12) 0.68631(12) 0.0156(4) Uani 1 1 d . . . . . C31 C 0.0943(2) 0.25834(13) 0.74509(12) 0.0175(4) Uani 1 1 d . . . . . H31 H 0.0731 0.3005 0.7310 0.021 Uiso 1 1 calc R U . . . N10 N 0.3090(3) -0.02308(12) 0.77631(11) 0.0228(4) Uani 1 1 d . . . . . C54 C 0.7811(3) 0.22886(14) 0.62825(13) 0.0210(5) Uani 1 1 d . . . . . H54 H 0.8379 0.2325 0.5912 0.025 Uiso 1 1 calc R U . . . N12 N 0.7622(2) 0.06986(12) 0.76017(12) 0.0221(4) Uani 1 1 d . . . . . C32 C 0.0366(3) 0.23155(14) 0.80237(13) 0.0197(4) Uani 1 1 d . . . . . H32 H -0.0221 0.2557 0.8273 0.024 Uiso 1 1 calc R U . . . C55 C 0.7820(3) 0.17696(14) 0.67003(14) 0.0214(5) Uani 1 1 d . . . . . H55 H 0.8383 0.1437 0.6619 0.026 Uiso 1 1 calc R U . . . C37 C 0.3229(2) 0.06619(13) 0.69996(12) 0.0172(4) Uani 1 1 d . . . . . C8 C 0.2483(3) 0.40142(13) 0.69131(13) 0.0184(4) Uani 1 1 d . . . . . H8 H 0.2041 0.4403 0.6975 0.022 Uiso 1 1 calc R U . . . C5 C 0.1093(3) 0.36713(13) 0.58563(12) 0.0181(4) Uani 1 1 d . . . . . C41 C 0.2723(3) 0.03462(13) 0.76101(12) 0.0177(4) Uani 1 1 d . . . . . C40 C 0.4211(2) 0.13498(13) 0.59189(12) 0.0170(4) Uani 1 1 d . . . . . H40 H 0.4572 0.1589 0.5550 0.020 Uiso 1 1 calc R U . . . C62 C 0.5328(3) 0.17752(14) 0.84003(12) 0.0190(4) Uani 1 1 d . . . . . F3 F 0.8277(2) 0.32155(11) 0.87446(10) 0.0424(5) Uani 1 1 d . . . . . C33 C 0.0651(3) 0.17024(13) 0.82253(13) 0.0192(4) Uani 1 1 d . . . . . H33 H 0.0279 0.1520 0.8620 0.023 Uiso 1 1 calc R U . . . C34 C 0.1496(2) 0.13474(13) 0.78416(12) 0.0164(4) Uani 1 1 d . . . . . C57 C 0.6180(2) 0.22323(13) 0.73431(12) 0.0175(4) Uani 1 1 d . . . . . C19 C 0.5486(3) 0.27656(14) 0.45995(13) 0.0221(5) Uani 1 1 d . . . . . H19 H 0.6237 0.3095 0.4872 0.026 Uiso 1 1 calc R U . . . C56 C 0.6986(2) 0.17333(13) 0.72530(13) 0.0182(4) Uani 1 1 d . . . . . N11 N 0.5928(3) 0.07140(14) 0.87051(12) 0.0279(5) Uani 1 1 d . . . . . C44 C 0.1840(3) -0.01224(14) 0.87863(13) 0.0216(5) Uani 1 1 d . . . . . C38 C 0.4048(3) 0.03518(13) 0.65600(12) 0.0186(4) Uani 1 1 d . . . . . H38 H 0.4277 -0.0088 0.6636 0.022 Uiso 1 1 calc R U . . . C63 C 0.6068(3) 0.12069(14) 0.82888(13) 0.0215(5) Uani 1 1 d . . . . . C64 C 0.6922(3) 0.11935(14) 0.77188(13) 0.0194(4) Uani 1 1 d . . . . . C4 C -0.0039(3) 0.39144(14) 0.60820(14) 0.0216(5) Uani 1 1 d . . . . . H4 H -0.0191 0.3946 0.6561 0.026 Uiso 1 1 calc R U . . . C39 C 0.4522(3) 0.07000(13) 0.60089(13) 0.0202(5) Uani 1 1 d . . . . . H39 H 0.5058 0.0492 0.5695 0.024 Uiso 1 1 calc R U . . . C60 C 0.3896(3) 0.24105(15) 0.90355(13) 0.0230(5) Uani 1 1 d . . . . . H60 H 0.3410 0.2487 0.9429 0.028 Uiso 1 1 calc R U . . . C59 C 0.3921(3) 0.28512(14) 0.85194(12) 0.0194(4) Uani 1 1 d . . . . . H59 H 0.3425 0.3219 0.8563 0.023 Uiso 1 1 calc R U . . . C53 C 0.6964(2) 0.27616(14) 0.64035(13) 0.0195(4) Uani 1 1 d . . . . . H53 H 0.6968 0.3120 0.6109 0.023 Uiso 1 1 calc R U . . . C61 C 0.4581(3) 0.18632(15) 0.89724(13) 0.0233(5) Uani 1 1 d . . . . . H61 H 0.4547 0.1549 0.9314 0.028 Uiso 1 1 calc R U . . . C43 C 0.2656(3) -0.04841(14) 0.83560(13) 0.0226(5) Uani 1 1 d . . . . . C30 C 0.5858(3) 0.46677(13) 0.64703(13) 0.0196(5) Uani 1 1 d . . . . . F2 F 0.9200(2) 0.44153(12) 0.87795(13) 0.0551(7) Uani 1 1 d . . . . . C9 C 0.3581(3) 0.44628(14) 0.80326(13) 0.0203(5) Uani 1 1 d . . . . . C3 C -0.0944(3) 0.41102(15) 0.56062(15) 0.0247(5) Uani 1 1 d . . . . . H3 H -0.1697 0.4284 0.5769 0.030 Uiso 1 1 calc R U . . . C68 C 0.8266(3) -0.03393(16) 0.79391(16) 0.0274(5) Uani 1 1 d . . . . . H68 H 0.8845 -0.0338 0.7573 0.033 Uiso 1 1 calc R U . . . F1 F 0.71279(18) 0.38981(11) 0.81873(10) 0.0345(4) Uani 1 1 d . . . . . C65 C 0.7524(3) 0.01907(15) 0.80392(14) 0.0244(5) Uani 1 1 d . . . . . C10 C 0.2435(3) 0.45965(15) 0.83377(15) 0.0268(6) Uani 1 1 d . . . . . H10 H 0.1543 0.4356 0.8130 0.032 Uiso 1 1 calc R U . . . C17 C 0.4634(3) 0.19311(17) 0.35431(15) 0.0309(6) Uani 1 1 d . . . . . C7 C 0.0330(3) 0.37894(16) 0.46778(15) 0.0275(5) Uani 1 1 d . . . . . H7 H 0.0456 0.3737 0.4196 0.033 Uiso 1 1 calc R U . . . C2 C -0.0772(3) 0.40578(14) 0.48996(15) 0.0250(5) Uani 1 1 d . . . . . C18 C 0.5662(3) 0.24444(16) 0.39419(15) 0.0273(6) Uani 1 1 d . . . . . H18 H 0.6519 0.2584 0.3762 0.033 Uiso 1 1 calc R U . . . C6 C 0.1251(3) 0.35955(15) 0.51484(13) 0.0233(5) Uani 1 1 d . . . . . H6 H 0.1991 0.3411 0.4984 0.028 Uiso 1 1 calc R U . . . C29 C 0.7007(3) 0.48892(15) 0.69572(15) 0.0282(6) Uani 1 1 d . . . . . H29 H 0.7332 0.4549 0.7197 0.034 Uiso 1 1 calc R U . . . C66 C 0.6646(3) 0.01926(16) 0.85909(15) 0.0287(6) Uani 1 1 d . . . . . C21 C 0.3158(3) 0.20865(16) 0.44666(14) 0.0252(5) Uani 1 1 d . . . . . H21 H 0.2288 0.1959 0.4638 0.030 Uiso 1 1 calc R U . . . C1 C -0.1717(3) 0.43001(17) 0.43898(17) 0.0320(6) Uani 1 1 d . . . . . H1A H -0.2378 0.3879 0.4135 0.048 Uiso 1 1 calc R U . . . H1B H -0.1179 0.4557 0.4059 0.048 Uiso 1 1 calc R U . . . H1C H -0.2207 0.4621 0.4644 0.048 Uiso 1 1 calc R U . . . C46 C 0.3014(3) -0.10965(16) 0.85531(15) 0.0296(6) Uani 1 1 d . . . . . H46 H 0.3577 -0.1330 0.8278 0.036 Uiso 1 1 calc R U . . . C11 C 0.2595(3) 0.50845(17) 0.89494(16) 0.0311(6) Uani 1 1 d . . . . . H11 H 0.1804 0.5185 0.9143 0.037 Uiso 1 1 calc R U . . . C45 C 0.1420(3) -0.03849(16) 0.93899(14) 0.0287(6) Uani 1 1 d . . . . . H45 H 0.0911 -0.0132 0.9682 0.034 Uiso 1 1 calc R U . . . B1 B 0.8423(3) 0.38021(16) 0.83765(16) 0.0223(5) Uani 1 1 d . . . . . C14 C 0.4879(3) 0.47907(18) 0.83737(16) 0.0319(7) Uani 1 1 d . . . . . H14 H 0.5675 0.4696 0.8181 0.038 Uiso 1 1 calc R U . . . C70 C 0.8170(4) -0.08716(17) 0.83689(17) 0.0336(7) Uani 1 1 d . . . . . C22 C 0.3379(3) 0.17540(17) 0.38220(15) 0.0302(6) Uani 1 1 d . . . . . H22 H 0.2655 0.1395 0.3562 0.036 Uiso 1 1 calc R U . . . C47 C 0.2563(3) -0.13728(15) 0.91451(15) 0.0273(6) Uani 1 1 d . . . . . C48 C 0.1730(3) -0.10093(16) 0.95728(14) 0.0280(6) Uani 1 1 d . . . . . C24 C 0.5393(3) 0.51728(15) 0.61146(16) 0.0288(6) Uani 1 1 d . . . . . H24 H 0.4609 0.5027 0.5783 0.035 Uiso 1 1 calc R U . . . C50 C 0.2886(4) -0.20059(16) 0.93480(16) 0.0332(7) Uani 1 1 d . . . . . H50 H 0.3458 -0.2243 0.9083 0.040 Uiso 1 1 calc R U . . . C12 C 0.3876(3) 0.54246(18) 0.92805(16) 0.0346(7) Uani 1 1 d . . . . . C49 C 0.1230(4) -0.13158(18) 1.01593(17) 0.0362(7) Uani 1 1 d . . . . . H49 H 0.0671 -0.1086 1.0441 0.043 Uiso 1 1 calc R U . . . C13 C 0.5004(4) 0.5253(2) 0.89909(18) 0.0404(8) Uani 1 1 d . . . . . H13 H 0.5891 0.5460 0.9224 0.048 Uiso 1 1 calc R U . . . C28 C 0.7674(4) 0.56111(17) 0.70884(18) 0.0400(8) Uani 1 1 d . . . . . H28 H 0.8441 0.5761 0.7431 0.048 Uiso 1 1 calc R U . . . C16 C 0.4864(4) 0.1577(2) 0.28439(17) 0.0438(9) Uani 1 1 d . . . . . H16A H 0.4170 0.1638 0.2490 0.066 Uiso 1 1 calc R U . . . H16B H 0.4794 0.1063 0.2857 0.066 Uiso 1 1 calc R U . . . H16C H 0.5778 0.1799 0.2727 0.066 Uiso 1 1 calc R U . . . C15 C 0.4048(4) 0.5966(2) 0.9936(2) 0.0514(11) Uani 1 1 d . . . . . H15A H 0.4305 0.6455 0.9817 0.077 Uiso 1 1 calc R U . . . H15B H 0.4767 0.5889 1.0266 0.077 Uiso 1 1 calc R U . . . H15C H 0.3183 0.5905 1.0150 0.077 Uiso 1 1 calc R U . . . C26 C 0.7253(4) 0.61200(16) 0.67341(17) 0.0397(8) Uani 1 1 d . . . . . C25 C 0.6095(4) 0.58893(17) 0.62531(17) 0.0390(8) Uani 1 1 d . . . . . H25 H 0.5777 0.6232 0.6013 0.047 Uiso 1 1 calc R U . . . C71 C 0.8893(4) -0.14328(18) 0.82619(19) 0.0379(7) Uani 1 1 d . . . . . H71 H 0.9439 -0.1452 0.7884 0.046 Uiso 1 1 calc R U . . . C51 C 0.2387(4) -0.22792(17) 0.99180(16) 0.0327(6) Uani 1 1 d . . . . . H51 H 0.2609 -0.2705 1.0043 0.039 Uiso 1 1 calc R U . . . C52 C 0.1536(4) -0.19304(17) 1.03251(16) 0.0334(7) Uani 1 1 d . . . . . H52 H 0.1179 -0.2129 1.0716 0.040 Uiso 1 1 calc R U . . . C76 C 0.0631(4) 0.0121(2) 0.3985(2) 0.0477(9) Uani 1 1 d . . . . . C67 C 0.6571(5) -0.03325(19) 0.90260(18) 0.0436(9) Uani 1 1 d . . . . . H67 H 0.6006 -0.0330 0.9398 0.052 Uiso 1 1 calc R U . . . C69 C 0.7309(5) -0.0859(2) 0.89235(18) 0.0458(9) Uani 1 1 d . . . . . C75 C 0.1531(5) 0.0041(3) 0.4528(3) 0.0696(14) Uani 1 1 d . . . . . H75A H 0.2469 0.0154 0.4397 0.104 Uiso 1 1 calc R U . . . H75B H 0.1299 -0.0456 0.4626 0.104 Uiso 1 1 calc R U . . . H75C H 0.1461 0.0369 0.4945 0.104 Uiso 1 1 calc R U . . . C27 C 0.7980(6) 0.69037(19) 0.6886(2) 0.0662(15) Uani 1 1 d . . . . . H27A H 0.7323 0.7193 0.7017 0.099 Uiso 1 1 calc R U . . . H27B H 0.8386 0.7055 0.6469 0.099 Uiso 1 1 calc R U . . . H27C H 0.8703 0.6973 0.7270 0.099 Uiso 1 1 calc R U . . . C73 C 0.8807(6) -0.1936(2) 0.8693(2) 0.0615(13) Uani 1 1 d . . . . . H73 H 0.9281 -0.2310 0.8613 0.074 Uiso 1 1 calc R U . . . C72 C 0.7288(8) -0.1394(3) 0.9366(3) 0.090(2) Uani 1 1 d . . . . . H72 H 0.6745 -0.1392 0.9747 0.108 Uiso 1 1 calc R U . . . C74 C 0.8011(8) -0.1907(3) 0.9264(3) 0.106(3) Uani 1 1 d . . . . . H74 H 0.7986 -0.2251 0.9577 0.127 Uiso 1 1 calc R U . . . N15 N 0.1886(4) 0.3316(2) 0.9738(2) 0.0577(10) Uani 1 1 d . . . . . N14 N -0.0077(4) 0.0215(2) 0.35299(19) 0.0579(10) Uani 1 1 d . . . . . C77 C -0.1458(5) 0.1672(3) 0.4009(3) 0.0661(13) Uani 1 1 d . . . . . H77A H -0.1891 0.1752 0.3567 0.099 Uiso 1 1 calc R U . . . H77B H -0.0824 0.1359 0.3915 0.099 Uiso 1 1 calc R U . . . H77C H -0.0953 0.2134 0.4270 0.099 Uiso 1 1 calc R U . . . N13 N -0.3353(5) 0.1058(2) 0.4740(2) 0.0597(10) Uani 1 1 d . . . . . C78 C -0.2523(5) 0.1327(2) 0.4424(2) 0.0515(10) Uani 1 1 d . . . . . C84 C 0.1208(4) 0.36472(18) 0.9990(2) 0.0392(7) Uani 1 1 d . . . . . C83 C 0.0296(5) 0.4055(3) 1.0310(3) 0.0642(13) Uani 1 1 d . . . . . H83A H -0.0408 0.4101 0.9954 0.096 Uiso 1 1 calc R U . . . H83B H 0.0824 0.4535 1.0519 0.096 Uiso 1 1 calc R U . . . H83C H -0.0142 0.3804 1.0673 0.096 Uiso 1 1 calc R U . . . 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 0.01430(8) 0.01655(8) 0.01386(7) 0.00486(6) 0.00564(5) 0.00565(6) Rh2 0.01538(8) 0.01746(8) 0.01433(7) 0.00402(6) 0.00529(6) 0.00591(6) Cl1 0.0197(3) 0.0290(3) 0.0235(3) 0.0060(2) 0.0062(2) 0.0070(2) N7 0.0144(8) 0.0178(8) 0.0161(8) 0.0040(7) 0.0048(7) 0.0063(7) N6 0.0154(8) 0.0187(9) 0.0156(8) 0.0037(7) 0.0041(7) 0.0057(7) N3 0.0182(9) 0.0210(9) 0.0157(8) 0.0044(7) 0.0062(7) 0.0053(7) N5 0.0169(9) 0.0192(9) 0.0149(8) 0.0039(7) 0.0040(7) 0.0053(7) N8 0.0152(8) 0.0166(8) 0.0152(8) 0.0040(7) 0.0055(7) 0.0049(7) N2 0.0211(9) 0.0193(9) 0.0176(9) 0.0014(7) 0.0055(7) 0.0080(8) N4 0.0203(9) 0.0192(9) 0.0169(8) 0.0052(7) 0.0074(7) 0.0067(8) F4 0.0303(9) 0.0354(9) 0.0291(8) 0.0062(7) 0.0112(7) 0.0128(7) N1 0.0184(9) 0.0183(9) 0.0173(8) 0.0071(7) 0.0048(7) 0.0074(7) C35 0.0164(9) 0.0172(9) 0.0146(9) 0.0044(7) 0.0046(7) 0.0070(8) N9 0.0260(10) 0.0213(9) 0.0192(9) 0.0079(8) 0.0105(8) 0.0106(8) C20 0.0222(11) 0.0217(11) 0.0168(10) 0.0057(8) 0.0079(8) 0.0061(9) C23 0.0205(11) 0.0215(10) 0.0178(10) 0.0074(8) 0.0078(8) 0.0077(9) C42 0.0205(10) 0.0181(10) 0.0149(9) 0.0052(8) 0.0066(8) 0.0073(8) C58 0.0170(10) 0.0187(10) 0.0162(9) 0.0038(8) 0.0037(8) 0.0052(8) C36 0.0149(9) 0.0181(9) 0.0151(9) 0.0026(7) 0.0055(7) 0.0050(8) C31 0.0170(10) 0.0198(10) 0.0185(10) 0.0050(8) 0.0057(8) 0.0079(8) N10 0.0326(12) 0.0217(10) 0.0204(9) 0.0083(8) 0.0131(9) 0.0137(9) C54 0.0181(10) 0.0256(12) 0.0212(11) 0.0034(9) 0.0081(8) 0.0074(9) N12 0.0206(10) 0.0212(10) 0.0263(10) 0.0045(8) 0.0022(8) 0.0080(8) C32 0.0199(11) 0.0239(11) 0.0200(10) 0.0070(9) 0.0101(9) 0.0104(9) C55 0.0167(10) 0.0249(11) 0.0243(11) 0.0024(9) 0.0056(9) 0.0078(9) C37 0.0204(10) 0.0183(10) 0.0154(9) 0.0041(8) 0.0071(8) 0.0074(8) C8 0.0197(10) 0.0183(10) 0.0208(10) 0.0065(8) 0.0084(8) 0.0082(8) C5 0.0199(10) 0.0186(10) 0.0189(10) 0.0085(8) 0.0057(8) 0.0069(9) C41 0.0202(10) 0.0199(10) 0.0155(9) 0.0052(8) 0.0072(8) 0.0073(9) C40 0.0183(10) 0.0193(10) 0.0153(9) 0.0029(8) 0.0069(8) 0.0061(8) C62 0.0204(11) 0.0236(11) 0.0149(9) 0.0038(8) 0.0032(8) 0.0080(9) F3 0.0616(13) 0.0438(11) 0.0373(10) 0.0205(9) 0.0221(10) 0.0317(10) C33 0.0214(11) 0.0225(11) 0.0177(10) 0.0069(8) 0.0104(8) 0.0086(9) C34 0.0180(10) 0.0182(10) 0.0156(9) 0.0042(8) 0.0059(8) 0.0073(8) C57 0.0142(9) 0.0226(10) 0.0171(10) 0.0042(8) 0.0042(8) 0.0053(8) C19 0.0200(11) 0.0257(12) 0.0208(11) 0.0030(9) 0.0077(9) 0.0041(9) C56 0.0156(10) 0.0215(10) 0.0185(10) 0.0026(8) 0.0033(8) 0.0060(8) N11 0.0385(13) 0.0302(12) 0.0205(10) 0.0086(9) 0.0077(9) 0.0156(11) C44 0.0269(12) 0.0228(11) 0.0204(11) 0.0077(9) 0.0117(9) 0.0114(10) C38 0.0225(11) 0.0195(10) 0.0166(9) 0.0037(8) 0.0073(8) 0.0083(9) C63 0.0246(12) 0.0248(11) 0.0176(10) 0.0057(9) 0.0035(9) 0.0092(10) C64 0.0183(10) 0.0222(11) 0.0190(10) 0.0043(8) 0.0006(8) 0.0073(9) C4 0.0200(11) 0.0215(11) 0.0263(12) 0.0098(9) 0.0067(9) 0.0062(9) C39 0.0226(11) 0.0214(11) 0.0192(10) 0.0030(8) 0.0080(9) 0.0090(9) C60 0.0268(12) 0.0286(12) 0.0162(10) 0.0049(9) 0.0079(9) 0.0091(10) C59 0.0213(11) 0.0230(11) 0.0167(10) 0.0050(8) 0.0061(8) 0.0082(9) C53 0.0156(10) 0.0257(11) 0.0192(10) 0.0055(9) 0.0074(8) 0.0058(9) C61 0.0270(12) 0.0277(12) 0.0183(10) 0.0075(9) 0.0060(9) 0.0095(10) C43 0.0301(13) 0.0224(11) 0.0213(11) 0.0079(9) 0.0133(10) 0.0129(10) C30 0.0248(11) 0.0166(10) 0.0203(10) 0.0047(8) 0.0091(9) 0.0079(9) F2 0.0409(12) 0.0490(13) 0.0608(15) -0.0241(11) 0.0099(11) -0.0042(10) C9 0.0241(11) 0.0201(10) 0.0199(10) 0.0028(8) 0.0062(9) 0.0109(9) C3 0.0190(11) 0.0239(12) 0.0328(13) 0.0089(10) 0.0046(10) 0.0050(10) C68 0.0293(14) 0.0255(12) 0.0289(13) 0.0035(10) 0.0006(11) 0.0104(11) F1 0.0243(8) 0.0410(10) 0.0423(10) 0.0077(8) 0.0091(7) 0.0135(8) C65 0.0266(13) 0.0227(11) 0.0250(12) 0.0032(9) 0.0019(10) 0.0086(10) C10 0.0234(12) 0.0286(13) 0.0278(13) -0.0036(10) 0.0087(10) 0.0069(10) C17 0.0336(15) 0.0351(15) 0.0235(12) -0.0007(11) 0.0127(11) 0.0065(12) C7 0.0315(14) 0.0306(13) 0.0223(12) 0.0085(10) 0.0016(10) 0.0092(12) C2 0.0235(12) 0.0191(11) 0.0327(14) 0.0092(10) -0.0017(10) 0.0035(10) C18 0.0260(13) 0.0300(13) 0.0263(12) 0.0028(10) 0.0142(10) 0.0042(11) C6 0.0272(12) 0.0277(12) 0.0198(11) 0.0070(9) 0.0049(9) 0.0136(10) C29 0.0341(15) 0.0209(12) 0.0290(13) 0.0061(10) 0.0010(11) 0.0046(11) C66 0.0419(16) 0.0283(13) 0.0213(12) 0.0075(10) 0.0048(11) 0.0170(12) C21 0.0221(12) 0.0325(13) 0.0196(11) 0.0018(10) 0.0078(9) 0.0024(10) C1 0.0291(14) 0.0279(14) 0.0381(16) 0.0127(12) -0.0081(12) 0.0039(12) C46 0.0430(16) 0.0299(13) 0.0266(13) 0.0124(11) 0.0186(12) 0.0220(13) C11 0.0315(14) 0.0334(14) 0.0300(14) -0.0047(12) 0.0106(11) 0.0136(12) C45 0.0431(16) 0.0307(13) 0.0227(12) 0.0133(10) 0.0189(11) 0.0207(13) B1 0.0202(12) 0.0231(13) 0.0255(13) 0.0021(10) 0.0070(10) 0.0081(10) C14 0.0256(13) 0.0394(16) 0.0308(14) -0.0079(12) -0.0009(11) 0.0160(12) C70 0.0459(18) 0.0300(14) 0.0293(14) 0.0051(12) 0.0018(13) 0.0185(14) C22 0.0283(13) 0.0353(15) 0.0228(12) -0.0033(11) 0.0080(10) 0.0009(12) C47 0.0385(15) 0.0277(13) 0.0247(12) 0.0127(10) 0.0144(11) 0.0184(12) C48 0.0401(15) 0.0305(13) 0.0231(12) 0.0143(10) 0.0161(11) 0.0191(12) C24 0.0397(16) 0.0236(12) 0.0288(13) 0.0080(10) 0.0060(12) 0.0164(12) C50 0.0496(18) 0.0296(14) 0.0330(15) 0.0164(12) 0.0202(13) 0.0245(14) C12 0.0386(16) 0.0377(16) 0.0282(14) -0.0092(12) 0.0010(12) 0.0191(14) C49 0.0520(19) 0.0393(16) 0.0333(15) 0.0225(13) 0.0264(14) 0.0285(15) C13 0.0329(16) 0.051(2) 0.0342(16) -0.0163(15) -0.0076(13) 0.0196(15) C28 0.053(2) 0.0256(14) 0.0337(16) -0.0007(12) -0.0021(15) -0.0021(14) C16 0.0379(17) 0.056(2) 0.0303(16) -0.0119(15) 0.0133(13) 0.0037(16) C15 0.052(2) 0.060(2) 0.0385(19) -0.0233(18) -0.0047(16) 0.0264(19) C26 0.068(2) 0.0194(12) 0.0287(14) 0.0033(11) 0.0101(15) 0.0019(14) C25 0.069(2) 0.0235(13) 0.0323(15) 0.0114(12) 0.0093(16) 0.0212(15) C71 0.050(2) 0.0311(15) 0.0391(17) 0.0062(13) 0.0018(15) 0.0225(15) C51 0.0463(18) 0.0302(14) 0.0313(14) 0.0154(12) 0.0150(13) 0.0199(13) C52 0.0473(18) 0.0342(15) 0.0289(14) 0.0184(12) 0.0181(13) 0.0188(14) C76 0.046(2) 0.053(2) 0.045(2) 0.0103(18) 0.0100(17) 0.0093(18) C67 0.076(3) 0.0384(17) 0.0322(16) 0.0191(14) 0.0238(17) 0.0325(18) C69 0.079(3) 0.0446(19) 0.0317(16) 0.0191(14) 0.0202(17) 0.040(2) C75 0.065(3) 0.053(3) 0.087(4) 0.020(3) -0.010(3) 0.005(2) C27 0.116(4) 0.0212(15) 0.052(2) 0.0001(15) 0.010(3) -0.003(2) C73 0.102(4) 0.058(3) 0.048(2) 0.022(2) 0.025(2) 0.056(3) C72 0.175(6) 0.080(3) 0.066(3) 0.053(3) 0.077(4) 0.092(4) C74 0.205(8) 0.098(4) 0.078(4) 0.066(3) 0.082(5) 0.120(5) N15 0.063(2) 0.053(2) 0.073(3) 0.0180(18) 0.026(2) 0.0360(18) N14 0.0374(17) 0.089(3) 0.0413(18) -0.0027(18) 0.0023(14) 0.0078(18) C77 0.067(3) 0.082(3) 0.058(3) 0.015(3) 0.003(2) 0.035(3) N13 0.086(3) 0.0450(19) 0.049(2) 0.0064(16) 0.015(2) 0.015(2) C78 0.075(3) 0.044(2) 0.040(2) 0.0031(17) 0.000(2) 0.026(2) C84 0.0436(19) 0.0299(15) 0.0472(19) 0.0052(14) 0.0065(15) 0.0150(14) C83 0.065(3) 0.064(3) 0.066(3) -0.018(2) 0.006(2) 0.035(2) _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 N7 2.030(2) . ? Rh1 N8 2.045(2) . ? Rh1 N1 2.068(2) . ? Rh1 N3 2.081(2) . ? Rh1 Cl1 2.4577(12) . ? Rh1 Rh2 2.5816(11) . ? Rh2 N4 2.027(2) . ? Rh2 N6 2.031(2) . ? Rh2 N2 2.043(2) . ? Rh2 N5 2.054(2) . ? N7 C31 1.340(3) . ? N7 C35 1.354(3) . ? N6 C53 1.339(3) . ? N6 C57 1.357(3) . ? N3 C23 1.328(3) . ? N3 C20 1.420(3) . ? N5 C59 1.339(3) . ? N5 C58 1.357(3) . ? N8 C40 1.346(3) . ? N8 C36 1.373(3) . ? N2 C8 1.325(3) . ? N2 C9 1.421(3) . ? N4 C23 1.310(3) . ? N4 C30 1.417(3) . ? F4 B1 1.398(3) . ? N1 C8 1.324(3) . ? N1 C5 1.428(3) . ? C35 C34 1.385(3) . ? C35 C36 1.444(3) . ? N9 C42 1.311(3) . ? N9 C44 1.364(3) . ? C20 C21 1.396(4) . ? C20 C19 1.402(3) . ? C42 C41 1.446(3) . ? C42 C34 1.463(3) . ? C58 C62 1.395(4) . ? C58 C57 1.449(3) . ? C36 C37 1.388(3) . ? C31 C32 1.395(3) . ? N10 C41 1.305(3) . ? N10 C43 1.369(3) . ? C54 C55 1.365(4) . ? C54 C53 1.387(4) . ? N12 C64 1.310(3) . ? N12 C65 1.366(4) . ? C32 C33 1.369(4) . ? C55 C56 1.409(3) . ? C37 C38 1.397(3) . ? C37 C41 1.472(3) . ? C5 C6 1.389(3) . ? C5 C4 1.400(4) . ? C40 C39 1.382(4) . ? C62 C61 1.398(3) . ? C62 C63 1.455(4) . ? F3 B1 1.397(4) . ? C33 C34 1.401(3) . ? C57 C56 1.388(4) . ? C19 C18 1.389(4) . ? C56 C64 1.455(4) . ? N11 C63 1.313(4) . ? N11 C66 1.364(4) . ? C44 C45 1.391(4) . ? C44 C43 1.435(3) . ? C38 C39 1.391(3) . ? C63 C64 1.450(3) . ? C4 C3 1.394(4) . ? C60 C61 1.377(4) . ? C60 C59 1.390(4) . ? C43 C46 1.394(4) . ? C30 C29 1.393(4) . ? C30 C24 1.401(4) . ? F2 B1 1.377(4) . ? C9 C10 1.391(4) . ? C9 C14 1.398(4) . ? C3 C2 1.390(4) . ? C68 C70 1.392(4) . ? C68 C65 1.392(4) . ? F1 B1 1.386(4) . ? C65 C66 1.436(4) . ? C10 C11 1.396(4) . ? C17 C18 1.376(4) . ? C17 C22 1.400(4) . ? C17 C16 1.498(4) . ? C7 C2 1.394(4) . ? C7 C6 1.397(4) . ? C2 C1 1.509(4) . ? C29 C28 1.387(4) . ? C66 C67 1.389(4) . ? C21 C22 1.389(4) . ? C46 C47 1.390(4) . ? C11 C12 1.382(5) . ? C45 C48 1.387(4) . ? C14 C13 1.382(4) . ? C70 C71 1.430(5) . ? C70 C69 1.431(5) . ? C47 C50 1.421(4) . ? C47 C48 1.446(4) . ? C48 C49 1.421(4) . ? C24 C25 1.388(4) . ? C50 C51 1.365(4) . ? C12 C13 1.386(4) . ? C12 C15 1.516(4) . ? C49 C52 1.355(4) . ? C28 C26 1.386(5) . ? C26 C25 1.394(6) . ? C26 C27 1.507(5) . ? C71 C73 1.350(5) . ? C51 C52 1.422(4) . ? C76 N14 1.152(6) . ? C76 C75 1.387(7) . ? C67 C69 1.384(5) . ? C69 C72 1.420(5) . ? C73 C74 1.416(6) . ? C72 C74 1.353(7) . ? N15 C84 1.127(5) . ? C77 C78 1.476(7) . ? N13 C78 1.143(6) . ? C84 C83 1.455(5) . ? 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 N7 Rh1 N8 80.73(8) . . ? N7 Rh1 N1 92.97(8) . . ? N8 Rh1 N1 173.59(7) . . ? N7 Rh1 N3 173.90(8) . . ? N8 Rh1 N3 96.90(8) . . ? N1 Rh1 N3 89.25(8) . . ? N7 Rh1 Cl1 83.31(6) . . ? N8 Rh1 Cl1 86.43(6) . . ? N1 Rh1 Cl1 94.05(7) . . ? N3 Rh1 Cl1 102.22(6) . . ? N7 Rh1 Rh2 90.25(6) . . ? N8 Rh1 Rh2 94.45(6) . . ? N1 Rh1 Rh2 84.33(6) . . ? N3 Rh1 Rh2 84.31(6) . . ? Cl1 Rh1 Rh2 173.276(16) . . ? N4 Rh2 N6 94.48(9) . . ? N4 Rh2 N2 86.83(9) . . ? N6 Rh2 N2 178.63(8) . . ? N4 Rh2 N5 174.24(8) . . ? N6 Rh2 N5 80.29(8) . . ? N2 Rh2 N5 98.42(9) . . ? N4 Rh2 Rh1 83.10(7) . . ? N6 Rh2 Rh1 95.34(6) . . ? N2 Rh2 Rh1 84.43(6) . . ? N5 Rh2 Rh1 99.69(6) . . ? C31 N7 C35 118.7(2) . . ? C31 N7 Rh1 127.42(17) . . ? C35 N7 Rh1 113.86(15) . . ? C53 N6 C57 117.4(2) . . ? C53 N6 Rh2 128.16(18) . . ? C57 N6 Rh2 114.43(15) . . ? C23 N3 C20 114.5(2) . . ? C23 N3 Rh1 114.85(15) . . ? C20 N3 Rh1 130.63(16) . . ? C59 N5 C58 117.8(2) . . ? C59 N5 Rh2 128.87(18) . . ? C58 N5 Rh2 113.28(15) . . ? C40 N8 C36 117.4(2) . . ? C40 N8 Rh1 129.27(17) . . ? C36 N8 Rh1 113.35(15) . . ? C8 N2 C9 116.8(2) . . ? C8 N2 Rh2 118.45(16) . . ? C9 N2 Rh2 124.16(17) . . ? C23 N4 C30 118.9(2) . . ? C23 N4 Rh2 121.00(17) . . ? C30 N4 Rh2 120.14(16) . . ? C8 N1 C5 116.1(2) . . ? C8 N1 Rh1 118.34(17) . . ? C5 N1 Rh1 125.09(16) . . ? N7 C35 C34 122.4(2) . . ? N7 C35 C36 116.6(2) . . ? C34 C35 C36 120.9(2) . . ? C42 N9 C44 116.9(2) . . ? C21 C20 C19 118.0(2) . . ? C21 C20 N3 122.2(2) . . ? C19 C20 N3 119.7(2) . . ? N4 C23 N3 123.2(2) . . ? N9 C42 C41 122.1(2) . . ? N9 C42 C34 118.0(2) . . ? C41 C42 C34 119.9(2) . . ? N5 C58 C62 123.2(2) . . ? N5 C58 C57 116.3(2) . . ? C62 C58 C57 120.5(2) . . ? N8 C36 C37 123.0(2) . . ? N8 C36 C35 115.3(2) . . ? C37 C36 C35 121.7(2) . . ? N7 C31 C32 121.7(2) . . ? C41 N10 C43 117.1(2) . . ? C55 C54 C53 119.4(2) . . ? C64 N12 C65 117.5(2) . . ? C33 C32 C31 119.6(2) . . ? C54 C55 C56 119.3(2) . . ? C36 C37 C38 118.4(2) . . ? C36 C37 C41 119.1(2) . . ? C38 C37 C41 122.5(2) . . ? N1 C8 N2 123.6(2) . . ? C6 C5 C4 118.7(2) . . ? C6 C5 N1 120.4(2) . . ? C4 C5 N1 120.8(2) . . ? N10 C41 C42 122.1(2) . . ? N10 C41 C37 119.0(2) . . ? C42 C41 C37 118.9(2) . . ? N8 C40 C39 122.7(2) . . ? C58 C62 C61 117.6(2) . . ? C58 C62 C63 119.5(2) . . ? C61 C62 C63 122.9(2) . . ? C32 C33 C34 119.2(2) . . ? C35 C34 C33 118.3(2) . . ? C35 C34 C42 119.3(2) . . ? C33 C34 C42 122.3(2) . . ? N6 C57 C56 123.1(2) . . ? N6 C57 C58 115.5(2) . . ? C56 C57 C58 121.4(2) . . ? C18 C19 C20 120.5(2) . . ? C57 C56 C55 117.7(2) . . ? C57 C56 C64 119.4(2) . . ? C55 C56 C64 122.9(2) . . ? C63 N11 C66 117.3(2) . . ? N9 C44 C45 119.2(2) . . ? N9 C44 C43 121.0(2) . . ? C45 C44 C43 119.9(3) . . ? C39 C38 C37 118.7(2) . . ? N11 C63 C64 121.8(2) . . ? N11 C63 C62 118.7(2) . . ? C64 C63 C62 119.4(2) . . ? N12 C64 C63 121.8(2) . . ? N12 C64 C56 118.8(2) . . ? C63 C64 C56 119.4(2) . . ? C3 C4 C5 120.2(2) . . ? C40 C39 C38 119.8(2) . . ? C61 C60 C59 119.6(2) . . ? N5 C59 C60 122.4(2) . . ? N6 C53 C54 123.1(2) . . ? C60 C61 C62 119.3(2) . . ? N10 C43 C46 120.2(2) . . ? N10 C43 C44 120.7(2) . . ? C46 C43 C44 119.0(2) . . ? C29 C30 C24 119.9(3) . . ? C29 C30 N4 118.8(2) . . ? C24 C30 N4 121.3(3) . . ? C10 C9 C14 118.7(2) . . ? C10 C9 N2 121.3(2) . . ? C14 C9 N2 120.0(2) . . ? C2 C3 C4 121.6(3) . . ? C70 C68 C65 120.8(3) . . ? N12 C65 C68 119.4(3) . . ? N12 C65 C66 120.6(2) . . ? C68 C65 C66 120.0(3) . . ? C9 C10 C11 120.0(3) . . ? C18 C17 C22 117.1(2) . . ? C18 C17 C16 121.0(3) . . ? C22 C17 C16 121.9(3) . . ? C2 C7 C6 121.5(3) . . ? C3 C2 C7 117.6(3) . . ? C3 C2 C1 121.6(3) . . ? C7 C2 C1 120.8(3) . . ? C17 C18 C19 122.1(2) . . ? C5 C6 C7 120.3(3) . . ? C28 C29 C30 119.5(3) . . ? N11 C66 C67 120.0(3) . . ? N11 C66 C65 120.9(3) . . ? C67 C66 C65 119.0(3) . . ? C22 C21 C20 120.1(2) . . ? C47 C46 C43 121.3(3) . . ? C12 C11 C10 121.6(3) . . ? C48 C45 C44 121.2(2) . . ? F2 B1 F1 110.0(2) . . ? F2 B1 F3 110.8(3) . . ? F1 B1 F3 108.1(2) . . ? F2 B1 F4 109.8(2) . . ? F1 B1 F4 109.2(2) . . ? F3 B1 F4 108.9(2) . . ? C13 C14 C9 119.9(3) . . ? C68 C70 C71 121.6(3) . . ? C68 C70 C69 118.7(3) . . ? C71 C70 C69 119.6(3) . . ? C21 C22 C17 122.1(3) . . ? C46 C47 C50 122.4(3) . . ? C46 C47 C48 119.4(3) . . ? C50 C47 C48 118.3(2) . . ? C45 C48 C49 122.2(3) . . ? C45 C48 C47 119.2(2) . . ? C49 C48 C47 118.6(3) . . ? C25 C24 C30 119.1(3) . . ? C51 C50 C47 121.0(3) . . ? C11 C12 C13 117.5(3) . . ? C11 C12 C15 121.5(3) . . ? C13 C12 C15 121.0(3) . . ? C52 C49 C48 121.2(3) . . ? C14 C13 C12 122.1(3) . . ? C26 C28 C29 121.9(3) . . ? C28 C26 C25 117.8(3) . . ? C28 C26 C27 121.3(4) . . ? C25 C26 C27 120.8(4) . . ? C24 C25 C26 121.8(3) . . ? C73 C71 C70 120.7(4) . . ? C50 C51 C52 120.4(3) . . ? C49 C52 C51 120.4(3) . . ? N14 C76 C75 177.0(5) . . ? C69 C67 C66 120.7(3) . . ? C67 C69 C72 122.5(3) . . ? C67 C69 C70 120.7(3) . . ? C72 C69 C70 116.8(3) . . ? C71 C73 C74 120.2(4) . . ? C74 C72 C69 122.3(4) . . ? C72 C74 C73 120.3(4) . . ? N13 C78 C77 179.5(5) . . ? N15 C84 C83 178.2(5) . . ? _refine_diff_density_max 1.211 _refine_diff_density_min -2.377 _refine_diff_density_rms 0.286 _shelxl_version_number 2013-3 _database_code_depnum_ccdc_archive 'CCDC 937906'