# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'J. Gladysz' _publ_contact_author_address ; Institut f\"ur Organische Chemie I Friedrich Alexander University Erlangen-Nurnberg Henkestrasse 42 Erlangen D-91054 GERMANY ; _publ_contact_author_email JOHN.GLADYSZ@ORGANIK.UNI-ERLANGEN.DE _publ_section_title ; Gyroscope-Like Molecules Consisting of Three-Spoke Stators that Enclose Switchable Neutral Dipolar Rhodium Rotators; Reversible Cycling between Faster and Slower Spinning Rh(CO)I and Rh(CO)2I Species ; loop_ _publ_author_name J.Gladysz 'Frank Hampel' 'Takanori Shima' 'Leyong Wang.' # Attachment 'LW08.CIF' data_lw08 _database_code_depnum_ccdc_archive 'CCDC 602258' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H84 I O P2 Rh' _chemical_formula_weight 908.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.4154(4) _cell_length_b 12.3194(3) _cell_length_c 34.0731(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.0660(10) _cell_angle_gamma 90.00 _cell_volume 9289.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10410 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3824 _exptl_absorpt_coefficient_mu 1.130 _exptl_absorpt_correction_type 'empirical (Scalepack)' _exptl_absorpt_correction_T_min 0.8056 _exptl_absorpt_correction_T_max 0.8954 _exptl_absorpt_process_details Scalepack _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18326 _diffrn_reflns_av_R_equivalents 0.0562 _diffrn_reflns_av_sigmaI/netI 0.1116 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 27.49 _reflns_number_total 10641 _reflns_number_gt 5767 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL NT' _computing_publication_material 'SHEXLTL NT' _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^)+(0.0670P)^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 'riding model' _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10641 _refine_ls_number_parameters 447 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1181 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1433 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 0.947 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.007 _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 0.470834(16) 0.86902(3) 0.116501(12) 0.03477(14) Uani 1 1 d D . . I1 I 0.444462(16) 0.79780(3) 0.182905(12) 0.04680(17) Uani 0.8872(15) 1 d PD . . I1' I 0.4741(2) 0.9703(5) 0.04914(19) 0.04680(17) Uani 0.11(15) 1 d PD . . P1 P 0.40883(6) 0.73878(12) 0.07402(4) 0.0419(4) Uani 1 1 d . . . P2 P 0.53358(5) 0.99552(11) 0.16044(4) 0.0366(3) Uani 1 1 d . . . O10 O 0.4920(2) 0.9667(5) 0.04341(16) 0.0631(15) Uani 1 1 d . . . C10 C 0.4821(3) 0.9283(6) 0.0721(2) 0.0635(18) Uani 1 1 d . . . C11 C 0.3295(2) 0.7822(5) 0.05203(17) 0.0492(14) Uani 1 1 d . . . H11A H 0.3262 0.8378 0.0304 0.059 Uiso 1 1 calc R . . H11B H 0.3045 0.7192 0.0385 0.059 Uiso 1 1 calc R . . C12 C 0.3047(2) 0.8286(5) 0.08431(17) 0.0496(14) Uani 1 1 d . . . H12A H 0.3319 0.8873 0.0995 0.060 Uiso 1 1 calc R . . H12B H 0.3050 0.7710 0.1046 0.060 Uiso 1 1 calc R . . C13 C 0.2407(2) 0.8739(4) 0.06649(16) 0.0461(14) Uani 1 1 d . . . H13A H 0.2400 0.9308 0.0458 0.055 Uiso 1 1 calc R . . H13B H 0.2131 0.8150 0.0520 0.055 Uiso 1 1 calc R . . C14 C 0.2184(2) 0.9212(5) 0.09934(17) 0.0492(14) Uani 1 1 d . . . H14A H 0.2471 0.9777 0.1146 0.059 Uiso 1 1 calc R . . H14B H 0.2177 0.8634 0.1194 0.059 Uiso 1 1 calc R . . C15 C 0.1561(2) 0.9706(5) 0.08232(18) 0.0550(16) Uani 1 1 d . . . H15A H 0.1272 0.9131 0.0681 0.066 Uiso 1 1 calc R . . H15B H 0.1564 1.0257 0.0613 0.066 Uiso 1 1 calc R . . C16 C 0.1334(2) 1.0237(6) 0.11487(19) 0.0632(18) Uani 1 1 d . . . H16A H 0.0930 1.0550 0.1007 0.076 Uiso 1 1 calc R . . H16B H 0.1286 0.9667 0.1340 0.076 Uiso 1 1 calc R . . C17 C 0.1738(2) 1.1120(5) 0.14026(17) 0.0528(16) Uani 1 1 d . . . H17A H 0.2118 1.0783 0.1581 0.063 Uiso 1 1 calc R . . H17B H 0.1535 1.1448 0.1587 0.063 Uiso 1 1 calc R . . C18 C 0.1894(2) 1.2016(5) 0.11520(17) 0.0505(15) Uani 1 1 d . . . H18A H 0.1515 1.2348 0.0971 0.061 Uiso 1 1 calc R . . H18B H 0.2103 1.1691 0.0970 0.061 Uiso 1 1 calc R . . C19 C 0.2296(2) 1.2910(5) 0.14124(19) 0.0576(16) Uani 1 1 d . . . H19A H 0.2362 1.3466 0.1222 0.069 Uiso 1 1 calc R . . H19B H 0.2076 1.3262 0.1582 0.069 Uiso 1 1 calc R . . C20 C 0.2907(2) 1.2531(5) 0.16996(17) 0.0513(15) Uani 1 1 d . . . H20A H 0.2842 1.1939 0.1877 0.062 Uiso 1 1 calc R . . H20B H 0.3102 1.3141 0.1884 0.062 Uiso 1 1 calc R . . C21 C 0.3330(2) 1.2133(5) 0.14820(16) 0.0480(14) Uani 1 1 d . . . H21A H 0.3393 1.2721 0.1302 0.058 Uiso 1 1 calc R . . H21B H 0.3139 1.1515 0.1301 0.058 Uiso 1 1 calc R . . C22 C 0.3945(2) 1.1772(5) 0.17777(17) 0.0498(14) Uani 1 1 d . . . H22A H 0.4148 1.2404 0.1945 0.060 Uiso 1 1 calc R . . H22B H 0.3880 1.1223 0.1971 0.060 Uiso 1 1 calc R . . C23 C 0.4360(2) 1.1296(5) 0.15619(16) 0.0461(14) Uani 1 1 d . . . H23A H 0.4469 1.1871 0.1396 0.055 Uiso 1 1 calc R . . H23B H 0.4140 1.0721 0.1368 0.055 Uiso 1 1 calc R . . C24 C 0.4937(2) 1.0815(4) 0.18655(16) 0.0445(13) Uani 1 1 d . . . H24A H 0.4833 1.0381 0.2077 0.053 Uiso 1 1 calc R . . H24B H 0.5207 1.1412 0.2010 0.053 Uiso 1 1 calc R . . C31 C 0.4042(2) 0.6076(4) 0.09723(17) 0.0467(14) Uani 1 1 d . . . H31A H 0.3803 0.6161 0.1162 0.056 Uiso 1 1 calc R . . H31B H 0.3819 0.5570 0.0749 0.056 Uiso 1 1 calc R . . C32 C 0.4651(2) 0.5557(5) 0.12155(17) 0.0465(14) Uani 1 1 d . . . H32A H 0.4932 0.6129 0.1370 0.056 Uiso 1 1 calc R . . H32B H 0.4828 0.5220 0.1018 0.056 Uiso 1 1 calc R . . C33 C 0.4585(2) 0.4703(5) 0.15184(18) 0.0539(15) Uani 1 1 d . . . H33A H 0.4336 0.4099 0.1359 0.065 Uiso 1 1 calc R . . H33B H 0.4367 0.5025 0.1695 0.065 Uiso 1 1 calc R . . C34 C 0.5178(2) 0.4249(5) 0.17951(18) 0.0559(16) Uani 1 1 d . . . H34A H 0.5411 0.3976 0.1619 0.067 Uiso 1 1 calc R . . H34B H 0.5096 0.3625 0.1952 0.067 Uiso 1 1 calc R . . C35 C 0.5568(2) 0.5087(5) 0.2106(2) 0.0620(17) Uani 1 1 d . . . H35A H 0.5709 0.5644 0.1950 0.074 Uiso 1 1 calc R . . H35B H 0.5311 0.5455 0.2246 0.074 Uiso 1 1 calc R . . C36 C 0.6106(3) 0.4607(5) 0.2430(2) 0.0690(19) Uani 1 1 d . . . H36A H 0.6379 0.4299 0.2291 0.083 Uiso 1 1 calc R . . H36B H 0.5966 0.4000 0.2566 0.083 Uiso 1 1 calc R . . C37 C 0.6469(2) 0.5397(5) 0.27674(17) 0.0545(15) Uani 1 1 d . . . H37A H 0.6191 0.5746 0.2895 0.065 Uiso 1 1 calc R . . H37B H 0.6771 0.4979 0.2987 0.065 Uiso 1 1 calc R . . C38 C 0.6794(2) 0.6277(5) 0.26086(16) 0.0493(14) Uani 1 1 d . . . H38A H 0.6492 0.6773 0.2424 0.059 Uiso 1 1 calc R . . H38B H 0.7025 0.5938 0.2444 0.059 Uiso 1 1 calc R . . C39 C 0.7226(2) 0.6931(5) 0.29674(17) 0.0510(15) Uani 1 1 d . . . H39A H 0.7498 0.6419 0.3166 0.061 Uiso 1 1 calc R . . H39B H 0.6986 0.7318 0.3115 0.061 Uiso 1 1 calc R . . C40 C 0.7609(2) 0.7752(5) 0.28330(17) 0.0498(15) Uani 1 1 d . . . H40A H 0.7859 0.8154 0.3081 0.060 Uiso 1 1 calc R . . H40B H 0.7887 0.7356 0.2719 0.060 Uiso 1 1 calc R . . C41 C 0.7255(2) 0.8561(4) 0.25136(16) 0.0436(13) Uani 1 1 d . . . H41A H 0.7000 0.8159 0.2267 0.052 Uiso 1 1 calc R . . H41B H 0.7542 0.9010 0.2426 0.052 Uiso 1 1 calc R . . C42 C 0.6851(2) 0.9311(4) 0.26625(16) 0.0444(13) Uani 1 1 d . . . H42A H 0.7108 0.9805 0.2877 0.053 Uiso 1 1 calc R . . H42B H 0.6609 0.8869 0.2793 0.053 Uiso 1 1 calc R . . C43 C 0.6418(2) 0.9996(5) 0.23098(16) 0.0463(14) Uani 1 1 d . . . H43A H 0.6220 1.0553 0.2431 0.056 Uiso 1 1 calc R . . H43B H 0.6652 1.0373 0.2156 0.056 Uiso 1 1 calc R . . C44 C 0.59413(19) 0.9289(4) 0.20135(15) 0.0374(12) Uani 1 1 d . . . H44A H 0.5753 0.8845 0.2180 0.045 Uiso 1 1 calc R . . H44B H 0.6148 0.8782 0.1879 0.045 Uiso 1 1 calc R . . C51 C 0.4249(2) 0.7068(5) 0.02588(17) 0.0546(16) Uani 1 1 d . . . H51A H 0.3960 0.6506 0.0105 0.065 Uiso 1 1 calc R . . H51B H 0.4175 0.7727 0.0083 0.065 Uiso 1 1 calc R . . C52 C 0.4881(2) 0.6672(5) 0.03186(18) 0.0563(16) Uani 1 1 d . . . H52A H 0.5167 0.7111 0.0540 0.068 Uiso 1 1 calc R . . H52B H 0.4913 0.5911 0.0417 0.068 Uiso 1 1 calc R . . C53 C 0.5074(3) 0.6720(9) -0.0062(2) 0.101(3) Uani 1 1 d D . . H53A H 0.4987 0.7437 -0.0176 0.121 Uiso 1 1 d R . . H53B H 0.4811 0.6231 -0.0258 0.121 Uiso 1 1 d R . . C54 C 0.5634(4) 0.6489(10) -0.0042(3) 0.077(4) Uani 0.641(12) 1 d PD . . H54A H 0.5685 0.5722 -0.0068 0.092 Uiso 0.641(12) 1 d PR . . H54B H 0.5919 0.6738 0.0215 0.092 Uiso 0.641(12) 1 d PR . . C54' C 0.5219(6) 0.7548(13) -0.0212(5) 0.047(5) Uani 0.359(12) 1 d PD . . H54C H 0.5389 0.8083 -0.0002 0.057 Uiso 0.359(12) 1 d PR . . H54D H 0.4860 0.7839 -0.0411 0.057 Uiso 0.359(12) 1 d PR . . C55 C 0.5692(7) 0.7096(14) -0.0463(4) 0.287(15) Uani 1 1 d D . . H55A H 0.5594 0.7852 -0.0459 0.345 Uiso 1 1 d R . . H55B H 0.5462 0.6778 -0.0724 0.345 Uiso 1 1 d R . . C56 C 0.6181(7) 0.7086(14) -0.0391(3) 0.201(7) Uani 1 1 d . . . H56A H 0.6259 0.7307 -0.0648 0.241 Uiso 1 1 calc R . . H56B H 0.6307 0.6316 -0.0342 0.241 Uiso 1 1 calc R . . C57 C 0.6637(5) 0.7757(10) -0.0025(3) 0.159(5) Uani 1 1 d . . . H57A H 0.6459 0.7820 0.0200 0.191 Uiso 1 1 calc R . . H57B H 0.7012 0.7325 0.0085 0.191 Uiso 1 1 calc R . . C58 C 0.6817(4) 0.8912(8) -0.0121(2) 0.115(3) Uani 1 1 d . . . H58A H 0.7095 0.8846 -0.0285 0.138 Uiso 1 1 calc R . . H58B H 0.6449 0.9291 -0.0296 0.138 Uiso 1 1 calc R . . C59 C 0.7114(3) 0.9597(7) 0.0252(2) 0.084(2) Uani 1 1 d . . . H59A H 0.7306 1.0230 0.0167 0.101 Uiso 1 1 calc R . . H59B H 0.7436 0.9168 0.0453 0.101 Uiso 1 1 calc R . . C60 C 0.6677(3) 0.9991(7) 0.0460(2) 0.074(2) Uani 1 1 d . . . H60A H 0.6331 1.0340 0.0248 0.089 Uiso 1 1 calc R . . H60B H 0.6518 0.9354 0.0568 0.089 Uiso 1 1 calc R . . C61 C 0.6929(2) 1.0777(5) 0.0809(2) 0.0670(19) Uani 1 1 d . . . H61A H 0.7127 1.1377 0.0709 0.080 Uiso 1 1 calc R . . H61B H 0.7244 1.0403 0.1035 0.080 Uiso 1 1 calc R . . C62 C 0.6467(2) 1.1259(5) 0.0986(2) 0.0625(17) Uani 1 1 d . . . H62A H 0.6132 1.1578 0.0757 0.075 Uiso 1 1 calc R . . H62B H 0.6660 1.1852 0.1180 0.075 Uiso 1 1 calc R . . C63 C 0.6208(2) 1.0427(5) 0.12145(17) 0.0486(14) Uani 1 1 d . . . H63A H 0.6540 1.0117 0.1448 0.058 Uiso 1 1 calc R . . H63B H 0.6018 0.9828 0.1023 0.058 Uiso 1 1 calc R . . C64 C 0.5738(2) 1.0938(4) 0.13822(17) 0.0462(14) Uani 1 1 d . . . H64A H 0.5438 1.1335 0.1154 0.055 Uiso 1 1 calc R . . H64B H 0.5943 1.1475 0.1599 0.055 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0350(2) 0.0359(3) 0.0330(2) -0.00206(19) 0.01043(16) -0.00203(17) I1 0.0492(3) 0.0528(3) 0.0419(3) -0.0003(2) 0.01967(19) -0.00870(19) I1' 0.0492(3) 0.0528(3) 0.0419(3) -0.0003(2) 0.01967(19) -0.00870(19) P1 0.0362(7) 0.0422(9) 0.0444(9) -0.0075(7) 0.0091(6) -0.0009(6) P2 0.0353(7) 0.0360(8) 0.0365(8) -0.0011(6) 0.0090(6) -0.0001(6) O10 0.072(4) 0.078(3) 0.049(3) 0.004(2) 0.032(2) -0.009(3) C10 0.079(4) 0.065(5) 0.048(4) 0.001(4) 0.023(4) -0.016(4) C11 0.043(3) 0.053(4) 0.048(4) -0.005(3) 0.009(3) -0.001(3) C12 0.043(3) 0.050(4) 0.048(3) -0.006(3) 0.003(3) 0.000(3) C13 0.043(3) 0.042(4) 0.049(3) 0.001(3) 0.008(2) 0.006(3) C14 0.042(3) 0.049(4) 0.052(4) 0.003(3) 0.009(3) 0.001(3) C15 0.040(3) 0.063(4) 0.053(4) -0.002(3) 0.003(3) 0.004(3) C16 0.045(3) 0.083(5) 0.061(4) 0.000(4) 0.016(3) -0.001(3) C17 0.051(3) 0.068(5) 0.044(3) 0.008(3) 0.021(3) 0.015(3) C18 0.043(3) 0.060(4) 0.046(3) 0.008(3) 0.013(3) 0.016(3) C19 0.059(4) 0.059(4) 0.064(4) 0.010(3) 0.031(3) 0.019(3) C20 0.059(3) 0.049(4) 0.051(4) -0.009(3) 0.023(3) 0.006(3) C21 0.057(3) 0.047(4) 0.045(3) 0.003(3) 0.023(3) 0.005(3) C22 0.056(3) 0.051(4) 0.048(4) 0.002(3) 0.025(3) 0.008(3) C23 0.050(3) 0.046(4) 0.044(3) 0.002(3) 0.019(3) 0.008(3) C24 0.052(3) 0.039(3) 0.041(3) -0.007(3) 0.012(2) 0.003(3) C31 0.040(3) 0.040(4) 0.062(4) -0.009(3) 0.019(3) -0.001(2) C32 0.041(3) 0.044(4) 0.056(4) -0.001(3) 0.016(3) 0.000(2) C33 0.049(3) 0.051(4) 0.064(4) 0.002(3) 0.022(3) -0.008(3) C34 0.057(3) 0.043(4) 0.066(4) 0.011(3) 0.019(3) -0.009(3) C35 0.055(4) 0.052(4) 0.082(5) 0.013(4) 0.027(3) 0.004(3) C36 0.069(4) 0.050(4) 0.079(5) 0.020(4) 0.013(3) 0.001(3) C37 0.066(4) 0.050(4) 0.047(4) 0.010(3) 0.017(3) 0.001(3) C38 0.055(3) 0.050(4) 0.042(3) 0.003(3) 0.015(3) 0.005(3) C39 0.055(3) 0.051(4) 0.045(3) 0.007(3) 0.013(3) 0.008(3) C40 0.040(3) 0.057(4) 0.047(3) 0.000(3) 0.007(2) 0.003(3) C41 0.036(3) 0.052(4) 0.044(3) -0.003(3) 0.015(2) -0.006(3) C42 0.047(3) 0.043(4) 0.039(3) -0.007(3) 0.008(2) -0.008(3) C43 0.045(3) 0.050(4) 0.040(3) -0.009(3) 0.008(2) -0.003(3) C44 0.037(3) 0.036(3) 0.035(3) 0.000(2) 0.007(2) 0.001(2) C51 0.057(3) 0.062(4) 0.037(3) -0.012(3) 0.004(3) -0.005(3) C52 0.056(3) 0.059(4) 0.059(4) -0.021(3) 0.025(3) -0.009(3) C53 0.078(6) 0.173(9) 0.062(5) -0.063(6) 0.037(4) -0.058(6) C54 0.048(6) 0.116(11) 0.063(7) -0.030(7) 0.012(5) -0.009(6) C54' 0.037(9) 0.067(13) 0.038(9) -0.001(9) 0.012(7) 0.015(8) C55 0.35(2) 0.43(3) 0.170(14) -0.179(17) 0.219(18) -0.28(2) C56 0.276(18) 0.31(2) 0.063(7) -0.047(9) 0.114(11) -0.064(16) C57 0.236(12) 0.202(13) 0.067(7) -0.009(7) 0.088(7) -0.077(10) C58 0.124(7) 0.185(11) 0.053(5) 0.034(6) 0.052(5) 0.010(7) C59 0.083(5) 0.123(7) 0.059(5) 0.038(5) 0.040(4) 0.018(5) C60 0.058(4) 0.112(6) 0.053(4) 0.021(4) 0.018(3) 0.006(4) C61 0.055(4) 0.076(5) 0.082(5) 0.029(4) 0.038(3) -0.002(3) C62 0.056(4) 0.058(4) 0.073(4) 0.021(3) 0.020(3) -0.003(3) C63 0.043(3) 0.050(4) 0.055(4) 0.009(3) 0.019(3) -0.001(3) C64 0.044(3) 0.039(3) 0.054(4) 0.004(3) 0.014(3) -0.006(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 C10 1.775(7) . ? Rh1 P1 2.3247(14) . ? Rh1 P2 2.3220(14) . ? Rh1 I1' 2.635(6) . ? Rh1 I1 2.6801(5) . ? I1' O10 0.519(5) . ? I1' C10 0.905(7) . ? P1 C31 1.818(5) . ? P1 C11 1.842(5) . ? P1 C51 1.841(5) . ? P2 C24 1.825(5) . ? P2 C44 1.826(5) . ? P2 C64 1.842(5) . ? O10 C10 1.176(8) . ? C11 C12 1.513(7) . ? C12 C13 1.527(6) . ? C13 C14 1.499(7) . ? C14 C15 1.511(7) . ? C15 C16 1.524(8) . ? C16 C17 1.514(8) . ? C17 C18 1.512(7) . ? C18 C19 1.529(8) . ? C19 C20 1.519(7) . ? C20 C21 1.501(7) . ? C21 C22 1.529(7) . ? C22 C23 1.514(7) . ? C23 C24 1.528(6) . ? C31 C32 1.536(7) . ? C32 C33 1.517(7) . ? C33 C34 1.508(7) . ? C34 C35 1.545(8) . ? C35 C36 1.499(8) . ? C36 C37 1.533(8) . ? C37 C38 1.522(7) . ? C38 C39 1.536(7) . ? C39 C40 1.518(7) . ? C40 C41 1.508(7) . ? C41 C42 1.523(7) . ? C42 C43 1.545(7) . ? C43 C44 1.512(6) . ? C51 C52 1.506(7) . ? C52 C53 1.507(8) . ? C53 C54' 1.238(13) . ? C53 C54 1.321(9) . ? C54 C54' 1.617(19) . ? C54 C55 1.663(14) . ? C54' C55 1.697(15) . ? C55 C56 1.090(18) . ? C56 C57 1.583(15) . ? C57 C58 1.549(13) . ? C58 C59 1.494(10) . ? C59 C60 1.504(8) . ? C60 C61 1.496(9) . ? C61 C62 1.520(8) . ? C62 C63 1.527(7) . ? C63 C64 1.532(7) . ? 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 C10 Rh1 P1 89.5(2) . . ? C10 Rh1 P2 91.9(2) . . ? P1 Rh1 P2 178.38(5) . . ? C10 Rh1 I1' 7.5(3) . . ? P1 Rh1 I1' 88.54(13) . . ? P2 Rh1 I1' 92.95(13) . . ? C10 Rh1 I1 173.4(2) . . ? P1 Rh1 I1 91.75(4) . . ? P2 Rh1 I1 86.97(4) . . ? I1' Rh1 I1 166.04(11) . . ? O10 I1' C10 108.2(14) . . ? O10 I1' Rh1 122.9(13) . . ? C10 I1' Rh1 14.8(5) . . ? C31 P1 C11 103.9(2) . . ? C31 P1 C51 104.8(3) . . ? C11 P1 C51 99.9(2) . . ? C31 P1 Rh1 117.17(18) . . ? C11 P1 Rh1 113.25(19) . . ? C51 P1 Rh1 115.76(19) . . ? C24 P2 C44 106.4(2) . . ? C24 P2 C64 103.3(3) . . ? C44 P2 C64 103.6(2) . . ? C24 P2 Rh1 112.78(17) . . ? C44 P2 Rh1 111.13(17) . . ? C64 P2 Rh1 118.50(19) . . ? I1' O10 C10 47.0(10) . . ? I1' C10 O10 24.8(5) . . ? I1' C10 Rh1 157.7(7) . . ? O10 C10 Rh1 177.3(7) . . ? C12 C11 P1 112.9(4) . . ? C11 C12 C13 114.1(4) . . ? C14 C13 C12 112.4(4) . . ? C13 C14 C15 113.5(4) . . ? C14 C15 C16 114.5(5) . . ? C17 C16 C15 115.1(4) . . ? C16 C17 C18 115.0(5) . . ? C17 C18 C19 114.5(5) . . ? C20 C19 C18 115.1(5) . . ? C19 C20 C21 114.7(5) . . ? C20 C21 C22 113.7(4) . . ? C23 C22 C21 114.1(4) . . ? C22 C23 C24 112.8(4) . . ? C23 C24 P2 112.1(3) . . ? C32 C31 P1 115.3(3) . . ? C31 C32 C33 111.9(4) . . ? C32 C33 C34 113.9(4) . . ? C33 C34 C35 113.4(5) . . ? C36 C35 C34 114.0(5) . . ? C35 C36 C37 115.4(5) . . ? C38 C37 C36 113.9(5) . . ? C37 C38 C39 111.5(5) . . ? C38 C39 C40 114.2(5) . . ? C41 C40 C39 114.7(4) . . ? C40 C41 C42 114.5(4) . . ? C41 C42 C43 113.1(4) . . ? C44 C43 C42 111.0(4) . . ? C43 C44 P2 118.1(4) . . ? C52 C51 P1 115.2(4) . . ? C53 C52 C51 115.4(6) . . ? C54' C53 C54 78.3(9) . . ? C54' C53 C52 126.1(10) . . ? C54 C53 C52 121.3(8) . . ? C53 C54 C54' 48.6(6) . . ? C53 C54 C55 102.6(8) . . ? C54' C54 C55 62.3(7) . . ? C53 C54' C54 53.2(6) . . ? C53 C54' C55 104.6(10) . . ? C54 C54' C55 60.2(6) . . ? C56 C55 C54 100.2(16) . . ? C56 C55 C54' 134.5(16) . . ? C54 C55 C54' 57.5(7) . . ? C55 C56 C57 124.1(16) . . ? C58 C57 C56 118.3(9) . . ? C59 C58 C57 114.9(7) . . ? C58 C59 C60 112.6(6) . . ? C61 C60 C59 115.6(5) . . ? C60 C61 C62 114.9(5) . . ? C61 C62 C63 113.1(5) . . ? C62 C63 C64 111.6(5) . . ? C63 C64 P2 114.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Rh1 I1' O10 -2.4(17) . . . . ? P1 Rh1 I1' O10 -99.4(14) . . . . ? P2 Rh1 I1' O10 80.0(14) . . . . ? I1 Rh1 I1' O10 169.3(10) . . . . ? P1 Rh1 I1' C10 -97(2) . . . . ? P2 Rh1 I1' C10 82(2) . . . . ? I1 Rh1 I1' C10 171.7(17) . . . . ? C10 Rh1 P1 C31 152.3(3) . . . . ? P2 Rh1 P1 C31 3.3(17) . . . . ? I1' Rh1 P1 C31 159.7(2) . . . . ? I1 Rh1 P1 C31 -34.24(18) . . . . ? C10 Rh1 P1 C11 -86.8(3) . . . . ? P2 Rh1 P1 C11 124.2(17) . . . . ? I1' Rh1 P1 C11 -79.4(2) . . . . ? I1 Rh1 P1 C11 86.6(2) . . . . ? C10 Rh1 P1 C51 27.8(3) . . . . ? P2 Rh1 P1 C51 -121.2(17) . . . . ? I1' Rh1 P1 C51 35.2(2) . . . . ? I1 Rh1 P1 C51 -158.8(2) . . . . ? C10 Rh1 P2 C24 116.1(3) . . . . ? P1 Rh1 P2 C24 -94.9(17) . . . . ? I1' Rh1 P2 C24 108.7(2) . . . . ? I1 Rh1 P2 C24 -57.3(2) . . . . ? C10 Rh1 P2 C44 -124.5(3) . . . . ? P1 Rh1 P2 C44 24.5(17) . . . . ? I1' Rh1 P2 C44 -131.9(2) . . . . ? I1 Rh1 P2 C44 62.03(17) . . . . ? C10 Rh1 P2 C64 -4.7(3) . . . . ? P1 Rh1 P2 C64 144.3(17) . . . . ? I1' Rh1 P2 C64 -12.1(2) . . . . ? I1 Rh1 P2 C64 -178.17(19) . . . . ? Rh1 I1' O10 C10 0.6(5) . . . . ? Rh1 I1' C10 O10 -177.9(15) . . . . ? O10 I1' C10 Rh1 177.9(15) . . . . ? I1' O10 C10 Rh1 -162(13) . . . . ? P1 Rh1 C10 I1' 83(2) . . . . ? P2 Rh1 C10 I1' -98(2) . . . . ? I1 Rh1 C10 I1' -18(3) . . . . ? P1 Rh1 C10 O10 -117(13) . . . . ? P2 Rh1 C10 O10 62(13) . . . . ? I1' Rh1 C10 O10 160(14) . . . . ? I1 Rh1 C10 O10 143(12) . . . . ? C31 P1 C11 C12 79.3(5) . . . . ? C51 P1 C11 C12 -172.6(4) . . . . ? Rh1 P1 C11 C12 -48.8(5) . . . . ? P1 C11 C12 C13 175.2(4) . . . . ? C11 C12 C13 C14 -178.7(5) . . . . ? C12 C13 C14 C15 177.7(5) . . . . ? C13 C14 C15 C16 -177.4(5) . . . . ? C14 C15 C16 C17 56.9(7) . . . . ? C15 C16 C17 C18 53.9(7) . . . . ? C16 C17 C18 C19 179.3(4) . . . . ? C17 C18 C19 C20 60.0(6) . . . . ? C18 C19 C20 C21 67.2(7) . . . . ? C19 C20 C21 C22 179.2(5) . . . . ? C20 C21 C22 C23 175.9(5) . . . . ? C21 C22 C23 C24 -172.9(5) . . . . ? C22 C23 C24 P2 165.6(4) . . . . ? C44 P2 C24 C23 -171.5(4) . . . . ? C64 P2 C24 C23 79.7(4) . . . . ? Rh1 P2 C24 C23 -49.5(4) . . . . ? C11 P1 C31 C32 -174.9(4) . . . . ? C51 P1 C31 C32 80.6(4) . . . . ? Rh1 P1 C31 C32 -49.2(4) . . . . ? P1 C31 C32 C33 159.8(4) . . . . ? C31 C32 C33 C34 -174.2(5) . . . . ? C32 C33 C34 C35 67.1(7) . . . . ? C33 C34 C35 C36 170.0(5) . . . . ? C34 C35 C36 C37 -174.6(5) . . . . ? C35 C36 C37 C38 -67.3(7) . . . . ? C36 C37 C38 C39 -171.1(5) . . . . ? C37 C38 C39 C40 174.5(5) . . . . ? C38 C39 C40 C41 55.9(6) . . . . ? C39 C40 C41 C42 64.1(6) . . . . ? C40 C41 C42 C43 -170.5(4) . . . . ? C41 C42 C43 C44 68.9(5) . . . . ? C42 C43 C44 P2 173.7(3) . . . . ? C24 P2 C44 C43 -61.1(4) . . . . ? C64 P2 C44 C43 47.4(4) . . . . ? Rh1 P2 C44 C43 175.7(3) . . . . ? C31 P1 C51 C52 -72.7(5) . . . . ? C11 P1 C51 C52 180.0(5) . . . . ? Rh1 P1 C51 C52 58.0(5) . . . . ? P1 C51 C52 C53 -162.9(5) . . . . ? C51 C52 C53 C54' 75.3(12) . . . . ? C51 C52 C53 C54 173.9(9) . . . . ? C52 C53 C54 C54' -125.4(12) . . . . ? C54' C53 C54 C55 -33.6(10) . . . . ? C52 C53 C54 C55 -159.0(9) . . . . ? C52 C53 C54' C54 120.3(10) . . . . ? C54 C53 C54' C55 33.2(10) . . . . ? C52 C53 C54' C55 153.5(9) . . . . ? C55 C54 C54' C53 142.4(11) . . . . ? C53 C54 C54' C55 -142.4(11) . . . . ? C53 C54 C55 C56 164.8(16) . . . . ? C54' C54 C55 C56 136.9(19) . . . . ? C53 C54 C55 C54' 28.0(9) . . . . ? C53 C54' C55 C56 -101(3) . . . . ? C54 C54' C55 C56 -71(3) . . . . ? C53 C54' C55 C54 -30.3(9) . . . . ? C54 C55 C56 C57 -67(2) . . . . ? C54' C55 C56 C57 -13(4) . . . . ? C55 C56 C57 C58 -91(2) . . . . ? C56 C57 C58 C59 164.9(9) . . . . ? C57 C58 C59 C60 -73.4(10) . . . . ? C58 C59 C60 C61 -173.8(6) . . . . ? C59 C60 C61 C62 173.8(5) . . . . ? C60 C61 C62 C63 67.9(7) . . . . ? C61 C62 C63 C64 -179.1(5) . . . . ? C62 C63 C64 P2 172.7(4) . . . . ? C24 P2 C64 C63 168.8(4) . . . . ? C44 P2 C64 C63 58.0(4) . . . . ? Rh1 P2 C64 C63 -65.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.711 _refine_diff_density_min -0.647 _refine_diff_density_rms 0.154