# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 loop_ _publ_author_name _publ_author_address M.Kubicki ; Department of Chemistry Adam Mickiewicz University Grunwaldzka 6 60-780 Pozna\'n Poland ; I.Kownacki ; Department of Chemistry Adam Mickiewicz University Grunwaldzka 6 60-780 Pozna\'n Poland ; B.Marciniec ; Department of Chemistry Adam Mickiewicz University Grunwaldzka 6 60-780 Pozna\'n Poland ; #TrackingRef '1.cif' _publ_contact_author ; Maciej Kubicki Faculty of Chemistry Adam Mickiewicz University Grunwaldzka 6 60-780 Pozna\'n Poland ; _publ_contact_author_email mkubicki@chem.amu.edu.pl _publ_contact_author_name 'Maciej Kubicki' # Attachment '2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 776149' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C72 H150 O26 Rh2 Si16' _chemical_formula_sum 'C72 H150 O26 Rh2 Si16' _chemical_formula_weight 2087.18 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.084(2) _cell_length_b 19.082(2) _cell_length_c 28.570(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.940(10) _cell_angle_gamma 90.00 _cell_volume 10816.2(19) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 13335 _cell_measurement_theta_min 2.0472 _cell_measurement_theta_max 28.0312 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4416 _exptl_absorpt_coefficient_mu 0.544 _exptl_absorpt_correction_T_min 0.74362 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Xcalibur, Sapphire2, large Be window' _diffrn_detector_area_resol_mean 8.1929 _diffrn_measurement_method '/w scan' _diffrn_reflns_number 50571 _diffrn_reflns_av_R_equivalents 0.0508 _diffrn_reflns_av_sigmaI/netI 0.0788 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.49 _diffrn_reflns_theta_max 27.96 _reflns_number_total 12106 _reflns_number_gt 7342 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_cell_refinement 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_data_reduction 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Stereochemical Workstation (Siemens, 1989)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.0966P)^2^+2.0792P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12106 _refine_ls_number_parameters 501 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.2041 _refine_ls_wR_factor_gt 0.1946 _refine_ls_goodness_of_fit_ref 1.181 _refine_ls_restrained_S_all 1.197 _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 0.95326(2) 0.74398(2) 0.205031(15) 0.03346(14) Uani 1 1 d . . . C1 C 0.8484(3) 0.7466(3) 0.1825(2) 0.0495(15) Uani 1 1 d . . . H1A H 0.8428 0.7108 0.2036 0.059 Uiso 1 1 calc R . . C2 C 0.8709(3) 0.8112(4) 0.2015(3) 0.0559(18) Uani 1 1 d . . . H2A H 0.8829 0.8151 0.2342 0.067 Uiso 1 1 calc R . . C3 C 0.8765(4) 0.8754(4) 0.1711(3) 0.082(3) Uani 1 1 d . . . H3A H 0.8416 0.8734 0.1435 0.098 Uiso 1 1 calc R . . H3B H 0.8686 0.9170 0.1890 0.098 Uiso 1 1 calc R . . C4 C 0.9432(4) 0.8818(4) 0.1550(3) 0.067(2) Uani 1 1 d . . . H4A H 0.9708 0.9145 0.1756 0.080 Uiso 1 1 calc R . . H4B H 0.9366 0.9014 0.1232 0.080 Uiso 1 1 calc R . . C5 C 0.9806(3) 0.8143(3) 0.1545(2) 0.0459(15) Uani 1 1 d . . . H5A H 1.0245 0.8130 0.1707 0.055 Uiso 1 1 calc R . . C6 C 0.9549(3) 0.7527(4) 0.1317(2) 0.0511(16) Uani 1 1 d . . . H6A H 0.9824 0.7132 0.1344 0.061 Uiso 1 1 calc R . . C7 C 0.8839(4) 0.7463(4) 0.1024(2) 0.065(2) Uani 1 1 d . . . H7A H 0.8726 0.7901 0.0858 0.079 Uiso 1 1 calc R . . H7B H 0.8845 0.7099 0.0788 0.079 Uiso 1 1 calc R . . C8 C 0.8323(4) 0.7302(5) 0.1303(3) 0.074(2) Uani 1 1 d . . . H8A H 0.8220 0.6806 0.1268 0.089 Uiso 1 1 calc R . . H8B H 0.7919 0.7558 0.1172 0.089 Uiso 1 1 calc R . . O1 O 1.05276(17) 0.70819(19) 0.22657(12) 0.0340(8) Uani 1 1 d . . . Si1 Si 1.10028(8) 0.66959(8) 0.19510(5) 0.0349(4) Uani 1 1 d . . . O12 O 1.05996(19) 0.6069(2) 0.16521(14) 0.0419(10) Uani 1 1 d . . . Si2 Si 1.04256(8) 0.54327(9) 0.12905(6) 0.0405(4) Uani 1 1 d . . . C21 C 0.9536(3) 0.5171(4) 0.1221(2) 0.0568(18) Uani 1 1 d . . . H21A H 0.9267 0.5585 0.1126 0.068 Uiso 1 1 calc R . . H21B H 0.9457 0.4843 0.0959 0.068 Uiso 1 1 calc R . . C22 C 0.9268(3) 0.4851(4) 0.1625(3) 0.066(2) Uani 1 1 d . . . H22A H 0.9579 0.4481 0.1760 0.079 Uiso 1 1 calc R . . C23 C 0.9210(4) 0.5383(4) 0.2007(3) 0.073(2) Uani 1 1 d . . . H23A H 0.9645 0.5582 0.2117 0.109 Uiso 1 1 calc R . . H23B H 0.9044 0.5158 0.2267 0.109 Uiso 1 1 calc R . . H23C H 0.8903 0.5747 0.1881 0.109 Uiso 1 1 calc R . . C24 C 0.8573(4) 0.4514(6) 0.1449(4) 0.117(4) Uani 1 1 d . . . H24A H 0.8405 0.4298 0.1710 0.175 Uiso 1 1 calc R . . H24B H 0.8620 0.4166 0.1213 0.175 Uiso 1 1 calc R . . H24C H 0.8263 0.4869 0.1313 0.175 Uiso 1 1 calc R . . O23 O 1.09150(19) 0.4783(2) 0.14722(15) 0.0440(10) Uani 1 1 d . . . Si3 Si 1.17081(8) 0.45885(8) 0.16223(6) 0.0388(4) Uani 1 1 d . . . C31 C 1.1814(3) 0.3673(3) 0.1822(2) 0.0511(16) Uani 1 1 d D B . H31A H 1.1546 0.3382 0.1586 0.061 Uiso 1 1 calc R . . H31B H 1.2282 0.3547 0.1822 0.061 Uiso 1 1 calc R . . C32 C 1.1640(3) 0.3476(3) 0.2295(3) 0.067(2) Uani 1 1 d D . . H32A H 1.1847 0.3859 0.2495 0.080 Uiso 1 1 calc R A 1 C33 C 1.0895(3) 0.3575(4) 0.2328(3) 0.083(3) Uani 1 1 d D B . H33A H 1.0780 0.4062 0.2290 0.125 Uiso 1 1 calc R . . H33B H 1.0809 0.3416 0.2632 0.125 Uiso 1 1 calc R . . H33C H 1.0627 0.3309 0.2083 0.125 Uiso 1 1 calc R . . C34A C 1.1960(6) 0.2849(7) 0.2548(5) 0.074(4) Uiso 0.55 1 d PD B 1 H34A H 1.2247 0.2995 0.2831 0.111 Uiso 0.55 1 calc PR B 1 H34B H 1.2222 0.2605 0.2346 0.111 Uiso 0.55 1 calc PR B 1 H34C H 1.1616 0.2543 0.2630 0.111 Uiso 0.55 1 calc PR B 1 C34B C 1.1788(7) 0.2662(5) 0.2367(5) 0.058(4) Uiso 0.45 1 d PD B 2 H34D H 1.2255 0.2573 0.2353 0.087 Uiso 0.45 1 calc PR B 2 H34E H 1.1513 0.2403 0.2121 0.087 Uiso 0.45 1 calc PR B 2 H34F H 1.1686 0.2519 0.2670 0.087 Uiso 0.45 1 calc PR B 2 O34 O 1.20290(19) 0.51001(19) 0.20491(14) 0.0435(10) Uani 1 1 d . . . Si4 Si 1.23010(8) 0.58401(8) 0.22763(6) 0.0344(4) Uani 1 1 d . . . C41 C 1.2705(3) 0.5746(3) 0.2902(2) 0.0457(15) Uani 1 1 d . . . H41A H 1.2759 0.6213 0.3037 0.055 Uiso 1 1 calc R . . H41B H 1.2392 0.5499 0.3069 0.055 Uiso 1 1 calc R . . C42 C 1.3388(4) 0.5375(5) 0.3015(3) 0.073(2) Uani 1 1 d . . . H42A H 1.3710 0.5626 0.2851 0.088 Uiso 1 1 calc R . . C43 C 1.3626(4) 0.5435(6) 0.3548(3) 0.107(4) Uani 1 1 d . . . H43A H 1.3644 0.5919 0.3639 0.161 Uiso 1 1 calc R . . H43B H 1.4067 0.5231 0.3625 0.161 Uiso 1 1 calc R . . H43C H 1.3318 0.5190 0.3715 0.161 Uiso 1 1 calc R . . C44 C 1.3373(5) 0.4621(6) 0.2859(4) 0.115(4) Uiso 1 1 d . . . H44A H 1.3220 0.4594 0.2524 0.173 Uiso 1 1 calc R . . H44B H 1.3071 0.4361 0.3024 0.173 Uiso 1 1 calc R . . H44C H 1.3818 0.4425 0.2930 0.173 Uiso 1 1 calc R . . O45 O 1.2833(2) 0.6160(2) 0.19583(15) 0.0498(11) Uani 1 1 d . . . Si5 Si 1.29486(9) 0.64435(10) 0.14428(7) 0.0500(5) Uani 1 1 d . . . C51 C 1.3800(3) 0.6801(3) 0.1474(2) 0.0502(16) Uani 1 1 d . . . H51A H 1.3915 0.6795 0.1157 0.060 Uiso 1 1 calc R . . H51B H 1.3788 0.7288 0.1571 0.060 Uiso 1 1 calc R . . C52 C 1.4336(4) 0.6457(4) 0.1786(4) 0.096(3) Uani 1 1 d D . . H52A H 1.4216 0.6497 0.2105 0.115 Uiso 1 1 calc R . . C53 C 1.4445(5) 0.5693(4) 0.1711(5) 0.144(6) Uani 1 1 d D . . H53A H 1.4027 0.5447 0.1706 0.216 Uiso 1 1 calc R . . H53B H 1.4772 0.5516 0.1964 0.216 Uiso 1 1 calc R . . H53C H 1.4605 0.5626 0.1415 0.216 Uiso 1 1 calc R . . C54 C 1.5014(4) 0.6842(5) 0.1808(4) 0.106(4) Uani 1 1 d . . . H54A H 1.5355 0.6598 0.2019 0.159 Uiso 1 1 calc R . . H54B H 1.4971 0.7311 0.1921 0.159 Uiso 1 1 calc R . . H54C H 1.5138 0.6857 0.1497 0.159 Uiso 1 1 calc R . . O56 O 1.2843(2) 0.5799(3) 0.10661(18) 0.0680(14) Uani 1 1 d . . . Si6 Si 1.23639(9) 0.52083(10) 0.07891(6) 0.0466(4) Uani 1 1 d . . . C61 C 1.2842(3) 0.4689(4) 0.0412(2) 0.0598(19) Uani 1 1 d D C . H61A H 1.3034 0.5015 0.0209 0.072 Uiso 1 1 calc R . . H61B H 1.3217 0.4476 0.0619 0.072 Uiso 1 1 calc R . . C62 C 1.2504(5) 0.4126(4) 0.0105(3) 0.092(3) Uani 1 1 d D . . C63 C 1.3063(5) 0.3743(7) -0.0144(5) 0.155(5) Uiso 1 1 d D C . H63A H 1.2856 0.3375 -0.0346 0.233 Uiso 1 1 calc R . . H63B H 1.3402 0.3547 0.0093 0.233 Uiso 1 1 calc R . . H63C H 1.3266 0.4076 -0.0331 0.233 Uiso 1 1 calc R . . C64A C 1.1959(6) 0.4375(9) -0.0284(5) 0.133(7) Uiso 0.64 1 d PD C 1 H62A H 1.2305 0.3788 0.0302 0.160 Uiso 0.64 1 d PR C 1 H64A H 1.1611 0.4606 -0.0147 0.200 Uiso 0.64 1 d PR C 1 H64B H 1.1771 0.3981 -0.0468 0.200 Uiso 0.64 1 d PR C 1 H64C H 1.2149 0.4697 -0.0485 0.200 Uiso 0.64 1 d PR C 1 C64B C 1.2152(10) 0.3570(8) 0.0356(7) 0.111(10) Uiso 0.36 1 d PD C 2 H62B H 1.2176 0.4340 -0.0148 0.133 Uiso 0.36 1 d PR C 2 H64D H 1.1823 0.3791 0.0518 0.166 Uiso 0.36 1 d PR C 2 H64E H 1.2478 0.3331 0.0582 0.166 Uiso 0.36 1 d PR C 2 H64F H 1.1932 0.3239 0.0130 0.166 Uiso 0.36 1 d PR C 2 O67 O 1.1741(2) 0.5584(3) 0.04731(16) 0.0627(13) Uani 1 1 d . . . Si7 Si 1.10668(10) 0.60678(11) 0.04649(6) 0.0554(5) Uani 1 1 d . . . C71 C 1.0657(4) 0.6197(4) -0.0141(2) 0.076(2) Uani 1 1 d D E . H71A H 1.1001 0.6355 -0.0320 0.091 Uiso 1 1 calc R . . H71B H 1.0510 0.5740 -0.0265 0.091 Uiso 1 1 calc R . . C72 C 1.0085(5) 0.6671(4) -0.0254(3) 0.115(4) Uani 1 1 d D . . H72A H 1.0246 0.7130 -0.0131 0.138 Uiso 1 1 calc R D 1 C73 C 0.9891(6) 0.6768(7) -0.0793(4) 0.144(5) Uiso 1 1 d . E . H73A H 1.0291 0.6840 -0.0932 0.215 Uiso 1 1 calc R . . H73B H 0.9600 0.7168 -0.0855 0.215 Uiso 1 1 calc R . . H73C H 0.9660 0.6357 -0.0928 0.215 Uiso 1 1 calc R . . C74A C 0.9477(6) 0.6511(11) -0.0026(8) 0.171(9) Uiso 0.67 1 d PD E 1 H74A H 0.9614 0.6439 0.0308 0.257 Uiso 0.67 1 calc PR E 1 H74B H 0.9260 0.6095 -0.0165 0.257 Uiso 0.67 1 calc PR E 1 H74C H 0.9167 0.6897 -0.0074 0.257 Uiso 0.67 1 calc PR E 1 C74B C 0.9939(12) 0.7262(10) 0.0048(9) 0.096(9) Uiso 0.33 1 d PD E 2 H74D H 1.0074 0.7141 0.0375 0.145 Uiso 0.33 1 calc PR E 2 H74E H 0.9464 0.7359 -0.0008 0.145 Uiso 0.33 1 calc PR E 2 H74F H 1.0182 0.7669 -0.0027 0.145 Uiso 0.33 1 calc PR E 2 O78 O 1.1271(2) 0.6816(2) 0.07024(15) 0.0557(12) Uani 1 1 d . F . Si8 Si 1.16367(10) 0.73129(9) 0.11238(6) 0.0482(5) Uani 1 1 d . . . C81A C 1.1704(5) 0.8249(6) 0.0982(3) 0.057(3) Uiso 0.67 1 d PD F 1 H81A H 1.1255 0.8445 0.0962 0.068 Uiso 0.67 1 calc PR F 1 H81B H 1.1977 0.8465 0.1254 0.068 Uiso 0.67 1 calc PR F 1 C82A C 1.1989(6) 0.8507(7) 0.0537(4) 0.101(5) Uiso 0.67 1 d PD F 1 H82A H 1.2033 0.9019 0.0550 0.121 Uiso 0.67 1 calc PR F 1 C83A C 1.2684(6) 0.8180(11) 0.0529(6) 0.158(8) Uiso 0.67 1 d PD F 1 H83A H 1.2851 0.8326 0.0248 0.237 Uiso 0.67 1 calc PR F 1 H83B H 1.2646 0.7678 0.0531 0.237 Uiso 0.67 1 calc PR F 1 H83C H 1.2989 0.8330 0.0803 0.237 Uiso 0.67 1 calc PR F 1 C84A C 1.1511(8) 0.8298(12) 0.0085(4) 0.178(9) Uiso 0.67 1 d PD F 1 H84A H 1.1699 0.8446 -0.0187 0.266 Uiso 0.67 1 calc PR F 1 H84B H 1.1081 0.8519 0.0084 0.266 Uiso 0.67 1 calc PR F 1 H84C H 1.1455 0.7798 0.0078 0.266 Uiso 0.67 1 calc PR F 1 C81B C 1.1359(9) 0.8159(10) 0.0860(6) 0.047(5) Uiso 0.33 1 d PD F 2 H81C H 1.0872 0.8180 0.0828 0.056 Uiso 0.33 1 calc PR F 2 H81D H 1.1538 0.8526 0.1078 0.056 Uiso 0.33 1 calc PR F 2 C82B C 1.1560(9) 0.8322(11) 0.0375(7) 0.097(9) Uiso 0.33 1 d PD F 2 H82B H 1.1445 0.7913 0.0171 0.116 Uiso 0.33 1 calc PR F 2 C83B C 1.2320(8) 0.8439(14) 0.0417(8) 0.079(7) Uiso 0.33 1 d PD F 2 H83D H 1.2439 0.8502 0.0108 0.118 Uiso 0.33 1 calc PR F 2 H83E H 1.2554 0.8038 0.0566 0.118 Uiso 0.33 1 calc PR F 2 H83F H 1.2444 0.8848 0.0606 0.118 Uiso 0.33 1 calc PR F 2 C84B C 1.1166(12) 0.8948(15) 0.0142(9) 0.125(12) Uiso 0.33 1 d PD F 2 H84D H 1.1277 0.9018 -0.0170 0.188 Uiso 0.33 1 calc PR F 2 H84E H 1.1281 0.9360 0.0330 0.188 Uiso 0.33 1 calc PR F 2 H84F H 1.0692 0.8859 0.0119 0.188 Uiso 0.33 1 calc PR F 2 O14 O 1.16706(18) 0.6366(2) 0.22668(14) 0.0402(9) Uani 1 1 d . . . O15 O 1.1254(2) 0.7239(2) 0.15799(14) 0.0459(10) Uani 1 1 d . F . O58 O 1.2405(2) 0.7049(2) 0.12698(16) 0.0576(12) Uani 1 1 d . F . O36 O 1.2081(2) 0.4714(2) 0.11676(15) 0.0498(11) Uani 1 1 d . . . O27 O 1.0567(2) 0.5671(3) 0.07733(15) 0.0593(12) 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 0.0391(2) 0.0286(2) 0.0355(2) 0.0020(2) 0.01450(18) 0.0046(2) C1 0.045(3) 0.054(4) 0.051(4) 0.011(3) 0.012(3) 0.005(3) C2 0.045(4) 0.056(4) 0.070(5) 0.016(4) 0.022(3) 0.013(3) C3 0.085(6) 0.049(4) 0.125(7) 0.038(5) 0.058(5) 0.037(4) C4 0.069(5) 0.048(4) 0.088(6) 0.027(4) 0.026(4) 0.017(4) C5 0.054(4) 0.043(4) 0.045(3) 0.015(3) 0.021(3) 0.011(3) C6 0.060(4) 0.062(4) 0.034(3) 0.018(3) 0.016(3) 0.016(3) C7 0.073(5) 0.078(5) 0.044(4) 0.006(4) 0.003(3) 0.025(4) C8 0.056(4) 0.104(7) 0.057(5) 0.001(4) -0.005(4) -0.003(4) O1 0.034(2) 0.038(2) 0.032(2) 0.0003(17) 0.0111(16) 0.0059(16) Si1 0.0373(8) 0.0350(8) 0.0351(8) 0.0021(7) 0.0140(7) 0.0046(7) O12 0.043(2) 0.036(2) 0.047(2) -0.0084(18) 0.0076(19) 0.0033(18) Si2 0.0328(8) 0.0488(10) 0.0413(9) -0.0102(8) 0.0100(7) -0.0015(7) C21 0.042(4) 0.069(5) 0.062(4) -0.025(4) 0.014(3) -0.006(3) C22 0.050(4) 0.065(5) 0.084(6) -0.016(4) 0.022(4) -0.007(4) C23 0.083(5) 0.054(4) 0.089(6) -0.025(4) 0.036(5) -0.017(4) C24 0.069(6) 0.132(9) 0.160(10) -0.052(8) 0.047(6) -0.047(6) O23 0.038(2) 0.035(2) 0.060(3) -0.013(2) 0.013(2) -0.0037(18) Si3 0.0406(9) 0.0332(8) 0.0451(9) -0.0069(7) 0.0149(7) -0.0028(7) C31 0.041(3) 0.039(3) 0.075(5) -0.011(3) 0.014(3) 0.001(3) C32 0.052(4) 0.046(4) 0.111(6) 0.021(4) 0.042(4) 0.009(3) C33 0.059(5) 0.079(6) 0.123(8) 0.017(5) 0.048(5) 0.009(4) O34 0.052(2) 0.035(2) 0.045(2) -0.0026(19) 0.011(2) -0.0063(19) Si4 0.0316(8) 0.0324(8) 0.0408(9) -0.0028(7) 0.0105(7) -0.0020(6) C41 0.037(3) 0.053(4) 0.047(4) -0.005(3) 0.007(3) 0.005(3) C42 0.052(4) 0.092(6) 0.068(5) -0.005(5) -0.012(4) 0.015(4) C43 0.072(6) 0.167(10) 0.075(6) 0.008(7) -0.012(5) 0.043(6) O45 0.045(2) 0.050(3) 0.059(3) -0.010(2) 0.024(2) -0.014(2) Si5 0.0469(10) 0.0503(11) 0.0596(11) -0.0146(9) 0.0299(9) -0.0174(8) C51 0.045(4) 0.040(3) 0.070(4) -0.009(3) 0.026(3) -0.011(3) C52 0.066(5) 0.059(5) 0.162(10) 0.022(6) 0.019(6) -0.013(4) C53 0.057(6) 0.065(6) 0.311(18) -0.012(9) 0.035(8) -0.001(5) C54 0.066(6) 0.074(6) 0.169(11) 0.021(7) -0.010(6) -0.015(5) O56 0.068(3) 0.070(3) 0.075(3) -0.035(3) 0.041(3) -0.026(3) Si6 0.0457(10) 0.0522(11) 0.0469(10) -0.0122(8) 0.0228(8) -0.0038(8) C61 0.057(4) 0.072(5) 0.055(4) -0.016(4) 0.024(3) 0.003(4) C62 0.115(8) 0.080(6) 0.091(7) -0.044(5) 0.051(6) 0.001(5) O67 0.065(3) 0.079(3) 0.048(3) -0.004(2) 0.023(2) 0.010(3) Si7 0.0580(12) 0.0756(14) 0.0349(9) -0.0039(9) 0.0150(9) 0.0110(10) C71 0.101(6) 0.088(6) 0.039(4) -0.001(4) 0.010(4) 0.015(5) C72 0.193(12) 0.061(6) 0.066(6) -0.008(5) -0.056(7) 0.033(7) O78 0.061(3) 0.063(3) 0.043(2) -0.003(2) 0.009(2) 0.013(2) Si8 0.0589(11) 0.0457(10) 0.0463(10) 0.0088(8) 0.0280(9) 0.0049(8) O14 0.038(2) 0.040(2) 0.044(2) 0.0004(18) 0.0129(18) 0.0058(17) O15 0.054(3) 0.043(2) 0.047(2) 0.0073(19) 0.025(2) 0.0046(19) O58 0.047(3) 0.067(3) 0.065(3) -0.001(2) 0.028(2) -0.007(2) O36 0.047(2) 0.055(3) 0.051(3) -0.007(2) 0.020(2) -0.003(2) O27 0.050(3) 0.088(4) 0.042(3) -0.001(2) 0.012(2) 0.001(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 O1 2.091(3) 2_755 ? Rh1 O1 2.111(3) . ? Rh1 Rh1 2.9373(10) 2_755 ? C1 C2 1.394(9) . ? C1 C8 1.509(10) . ? C1 H1A 0.9300 . ? C2 C3 1.518(9) . ? C2 H2A 0.9300 . ? C3 C4 1.488(9) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.491(8) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.404(9) . ? C5 H5A 0.9300 . ? C6 C7 1.542(9) . ? C6 H6A 0.9300 . ? C7 C8 1.433(10) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? O1 Si1 1.590(4) . ? O1 Rh1 2.091(3) 2_755 ? Si1 O12 1.612(4) . ? Si1 O15 1.618(4) . ? Si1 O14 1.622(4) . ? O12 Si2 1.598(4) . ? Si2 O27 1.613(5) . ? Si2 O23 1.617(4) . ? Si2 C21 1.836(6) . ? C21 C22 1.481(10) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C23 1.507(9) . ? C22 C24 1.548(10) . ? C22 H22A 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? O23 Si3 1.627(4) . ? Si3 O36 1.615(4) . ? Si3 O34 1.616(4) . ? Si3 C31 1.840(6) . ? C31 C32 1.495(9) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 C34A 1.491(7) . ? C32 C33 1.525(8) . ? C32 C34B 1.589(8) . ? C32 H32A 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34A H34A 0.9600 . ? C34A H34B 0.9600 . ? C34A H34C 0.9600 . ? C34B H34D 0.9600 . ? C34B H34E 0.9600 . ? C34B H34F 0.9600 . ? O34 Si4 1.614(4) . ? Si4 O14 1.613(4) . ? Si4 O45 1.625(4) . ? Si4 C41 1.854(6) . ? C41 C42 1.531(9) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C44 1.506(13) . ? C42 C43 1.529(11) . ? C42 H42A 0.9800 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? O45 Si5 1.619(4) . ? Si5 O58 1.613(5) . ? Si5 O56 1.626(5) . ? Si5 C51 1.830(6) . ? C51 C52 1.445(11) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.494(8) . ? C52 C54 1.539(10) . ? C52 H52A 0.9800 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? O56 Si6 1.608(5) . ? Si6 O67 1.594(5) . ? Si6 O36 1.604(4) . ? Si6 C61 1.840(6) . ? C61 C62 1.484(10) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C64A 1.511(8) . ? C62 C64B 1.515(9) . ? C62 C63 1.596(12) . ? C62 H62A 0.9809 . ? C62 H62B 0.9875 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64A H64A 0.9600 . ? C64A H64B 0.9600 . ? C64A H64C 0.9600 . ? C64A H62B 0.5418 . ? C64B H62A 0.5530 . ? C64B H64D 0.9600 . ? C64B H64E 0.9600 . ? C64B H64F 0.9600 . ? O67 Si7 1.636(5) . ? Si7 O78 1.606(5) . ? Si7 O27 1.623(5) . ? Si7 C71 1.814(7) . ? C71 C72 1.458(7) . ? C71 H71A 0.9700 . ? C71 H71B 0.9700 . ? C72 C74B 1.478(9) . ? C72 C74A 1.504(9) . ? C72 C73 1.539(13) . ? C72 H72A 0.9800 . ? C73 H73A 0.9600 . ? C73 H73B 0.9600 . ? C73 H73C 0.9600 . ? C74A H74A 0.9600 . ? C74A H74B 0.9600 . ? C74A H74C 0.9600 . ? C74B H74D 0.9600 . ? C74B H74E 0.9600 . ? C74B H74F 0.9600 . ? O78 Si8 1.616(5) . ? Si8 O58 1.616(5) . ? Si8 O15 1.618(4) . ? Si8 C81B 1.832(17) . ? Si8 C81A 1.841(10) . ? C81A C82A 1.551(9) . ? C81A H81A 0.9700 . ? C81A H81B 0.9700 . ? C82A C83A 1.533(9) . ? C82A C84A 1.537(9) . ? C82A H82A 0.9800 . ? C83A H83A 0.9600 . ? C83A H83B 0.9600 . ? C83A H83C 0.9600 . ? C84A H84A 0.9600 . ? C84A H84B 0.9600 . ? C84A H84C 0.9600 . ? C81B C82B 1.534(10) . ? C81B H81C 0.9700 . ? C81B H81D 0.9700 . ? C82B C84B 1.527(10) . ? C82B C83B 1.528(10) . ? C82B H82B 0.9800 . ? C83B H83D 0.9600 . ? C83B H83E 0.9600 . ? C83B H83F 0.9600 . ? C84B H84D 0.9600 . ? C84B H84E 0.9600 . ? C84B H84F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Rh1 O1 79.14(15) 2_755 . ? O1 Rh1 Rh1 45.93(10) 2_755 2_755 ? O1 Rh1 Rh1 45.38(9) . 2_755 ? C2 C1 C8 125.1(6) . . ? C2 C1 H1A 117.4 . . ? C8 C1 H1A 117.4 . . ? C1 C2 C3 122.6(7) . . ? C1 C2 H2A 118.7 . . ? C3 C2 H2A 118.7 . . ? C4 C3 C2 113.2(6) . . ? C4 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C4 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C3 C4 C5 114.2(6) . . ? C3 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? C3 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? C6 C5 C4 125.4(6) . . ? C6 C5 H5A 117.3 . . ? C4 C5 H5A 117.3 . . ? C5 C6 C7 124.1(6) . . ? C5 C6 H6A 118.0 . . ? C7 C6 H6A 118.0 . . ? C8 C7 C6 113.8(6) . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7B 108.8 . . ? C6 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C1 116.3(6) . . ? C7 C8 H8A 108.2 . . ? C1 C8 H8A 108.2 . . ? C7 C8 H8B 108.2 . . ? C1 C8 H8B 108.2 . . ? H8A C8 H8B 107.4 . . ? Si1 O1 Rh1 143.8(2) . 2_755 ? Si1 O1 Rh1 127.5(2) . . ? Rh1 O1 Rh1 88.69(13) 2_755 . ? O1 Si1 O12 110.3(2) . . ? O1 Si1 O15 110.5(2) . . ? O12 Si1 O15 108.0(2) . . ? O1 Si1 O14 112.5(2) . . ? O12 Si1 O14 108.1(2) . . ? O15 Si1 O14 107.3(2) . . ? Si2 O12 Si1 161.4(3) . . ? O12 Si2 O27 109.0(2) . . ? O12 Si2 O23 108.3(2) . . ? O27 Si2 O23 109.0(2) . . ? O12 Si2 C21 112.8(3) . . ? O27 Si2 C21 106.5(3) . . ? O23 Si2 C21 111.0(3) . . ? C22 C21 Si2 119.6(5) . . ? C22 C21 H21A 107.4 . . ? Si2 C21 H21A 107.4 . . ? C22 C21 H21B 107.4 . . ? Si2 C21 H21B 107.4 . . ? H21A C21 H21B 106.9 . . ? C21 C22 C23 111.4(6) . . ? C21 C22 C24 109.6(7) . . ? C23 C22 C24 110.4(6) . . ? C21 C22 H22A 108.4 . . ? C23 C22 H22A 108.4 . . ? C24 C22 H22A 108.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si2 O23 Si3 141.3(3) . . ? O36 Si3 O34 109.7(2) . . ? O36 Si3 O23 108.2(2) . . ? O34 Si3 O23 108.7(2) . . ? O36 Si3 C31 110.1(3) . . ? O34 Si3 C31 109.0(3) . . ? O23 Si3 C31 111.1(3) . . ? C32 C31 Si3 119.1(4) . . ? C32 C31 H31A 107.5 . . ? Si3 C31 H31A 107.5 . . ? C32 C31 H31B 107.5 . . ? Si3 C31 H31B 107.5 . . ? H31A C31 H31B 107.0 . . ? C34A C32 C31 119.7(6) . . ? C34A C32 C33 115.0(6) . . ? C31 C32 C33 113.3(6) . . ? C31 C32 C34B 107.2(6) . . ? C33 C32 C34B 106.2(6) . . ? C34A C32 H32A 101.7 . . ? C31 C32 H32A 101.7 . . ? C33 C32 H32A 101.7 . . ? C34B C32 H32A 126.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34A H34A 109.5 . . ? C32 C34A H34B 109.5 . . ? H34A C34A H34B 109.5 . . ? C32 C34A H34C 109.5 . . ? H34A C34A H34C 109.5 . . ? H34B C34A H34C 109.5 . . ? C32 C34B H34D 109.5 . . ? C32 C34B H34E 109.5 . . ? H34D C34B H34E 109.5 . . ? C32 C34B H34F 109.5 . . ? H34D C34B H34F 109.5 . . ? H34E C34B H34F 109.5 . . ? Si4 O34 Si3 154.5(3) . . ? O14 Si4 O34 108.8(2) . . ? O14 Si4 O45 109.8(2) . . ? O34 Si4 O45 108.4(2) . . ? O14 Si4 C41 107.6(2) . . ? O34 Si4 C41 111.9(3) . . ? O45 Si4 C41 110.4(3) . . ? C42 C41 Si4 119.4(5) . . ? C42 C41 H41A 107.5 . . ? Si4 C41 H41A 107.5 . . ? C42 C41 H41B 107.5 . . ? Si4 C41 H41B 107.5 . . ? H41A C41 H41B 107.0 . . ? C44 C42 C43 110.7(8) . . ? C44 C42 C41 113.8(7) . . ? C43 C42 C41 107.8(6) . . ? C44 C42 H42A 108.1 . . ? C43 C42 H42A 108.1 . . ? C41 C42 H42A 108.1 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si5 O45 Si4 146.5(3) . . ? O58 Si5 O45 109.4(2) . . ? O58 Si5 O56 109.0(3) . . ? O45 Si5 O56 109.1(3) . . ? O58 Si5 C51 109.3(3) . . ? O45 Si5 C51 110.2(3) . . ? O56 Si5 C51 109.8(3) . . ? C52 C51 Si5 117.6(5) . . ? C52 C51 H51A 107.9 . . ? Si5 C51 H51A 107.9 . . ? C52 C51 H51B 107.9 . . ? Si5 C51 H51B 107.9 . . ? H51A C51 H51B 107.2 . . ? C51 C52 C53 117.7(9) . . ? C51 C52 C54 112.3(7) . . ? C53 C52 C54 108.9(7) . . ? C51 C52 H52A 105.7 . . ? C53 C52 H52A 105.7 . . ? C54 C52 H52A 105.7 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? Si6 O56 Si5 149.6(3) . . ? O67 Si6 O36 108.5(2) . . ? O67 Si6 O56 108.7(3) . . ? O36 Si6 O56 109.1(3) . . ? O67 Si6 C61 110.2(3) . . ? O36 Si6 C61 110.4(3) . . ? O56 Si6 C61 109.8(3) . . ? C62 C61 Si6 120.2(5) . . ? C62 C61 H61A 107.3 . . ? Si6 C61 H61A 107.3 . . ? C62 C61 H61B 107.3 . . ? Si6 C61 H61B 107.3 . . ? H61A C61 H61B 106.9 . . ? C61 C62 C64A 114.8(8) . . ? C61 C62 C64B 115.5(8) . . ? C61 C62 C63 107.9(7) . . ? C64A C62 C63 107.2(7) . . ? C64B C62 C63 107.7(8) . . ? C61 C62 H62A 109.1 . . ? C64A C62 H62A 108.4 . . ? C63 C62 H62A 109.4 . . ? C61 C62 H62B 108.9 . . ? C64B C62 H62B 109.2 . . ? C63 C62 H62B 107.4 . . ? H62A C62 H62B 114.0 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64A H64A 109.5 . . ? C62 C64A H64B 109.5 . . ? H64A C64A H64B 109.5 . . ? C62 C64A H64C 109.4 . . ? H64A C64A H64C 109.5 . . ? H64B C64A H64C 109.5 . . ? H64A C64A H62B 108.5 . . ? H64B C64A H62B 120.1 . . ? H64C C64A H62B 99.2 . . ? C62 C64B H64D 109.1 . . ? C62 C64B H64E 109.3 . . ? H64D C64B H64E 109.5 . . ? C62 C64B H64F 110.0 . . ? H64D C64B H64F 109.5 . . ? H64E C64B H64F 109.5 . . ? Si6 O67 Si7 146.8(3) . . ? O78 Si7 O27 108.9(2) . . ? O78 Si7 O67 109.8(3) . . ? O27 Si7 O67 108.0(3) . . ? O78 Si7 C71 109.3(3) . . ? O27 Si7 C71 110.8(3) . . ? O67 Si7 C71 110.0(3) . . ? C72 C71 Si7 121.4(5) . . ? C72 C71 H71A 107.0 . . ? Si7 C71 H71A 107.0 . . ? C72 C71 H71B 107.0 . . ? Si7 C71 H71B 107.0 . . ? H71A C71 H71B 106.7 . . ? C71 C72 C74B 124.4(9) . . ? C71 C72 C74A 116.3(8) . . ? C71 C72 C73 111.4(8) . . ? C74B C72 C73 116.7(13) . . ? C74A C72 C73 111.2(12) . . ? C71 C72 H72A 105.6 . . ? C74A C72 H72A 105.6 . . ? C73 C72 H72A 105.6 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74A H74A 109.5 . . ? C72 C74A H74B 109.5 . . ? H74A C74A H74B 109.5 . . ? C72 C74A H74C 109.5 . . ? H74A C74A H74C 109.5 . . ? H74B C74A H74C 109.5 . . ? C72 C74B H74D 109.5 . . ? C72 C74B H74E 109.5 . . ? H74D C74B H74E 109.5 . . ? C72 C74B H74F 109.5 . . ? H74D C74B H74F 109.5 . . ? H74E C74B H74F 109.5 . . ? Si7 O78 Si8 153.2(3) . . ? O58 Si8 O78 108.3(2) . . ? O58 Si8 O15 108.6(2) . . ? O78 Si8 O15 109.3(2) . . ? O58 Si8 C81B 126.7(6) . . ? O78 Si8 C81B 97.8(7) . . ? O15 Si8 C81B 104.9(5) . . ? O58 Si8 C81A 105.0(4) . . ? O78 Si8 C81A 116.4(4) . . ? O15 Si8 C81A 108.9(3) . . ? C82A C81A Si8 122.6(7) . . ? C82A C81A H81A 106.7 . . ? Si8 C81A H81A 106.7 . . ? C82A C81A H81B 106.7 . . ? Si8 C81A H81B 106.7 . . ? H81A C81A H81B 106.6 . . ? C83A C82A C84A 109.4(8) . . ? C83A C82A C81A 109.6(8) . . ? C84A C82A C81A 110.1(8) . . ? C83A C82A H82A 109.2 . . ? C84A C82A H82A 109.2 . . ? C81A C82A H82A 109.2 . . ? C82A C83A H83A 109.5 . . ? C82A C83A H83B 109.5 . . ? H83A C83A H83B 109.5 . . ? C82A C83A H83C 109.5 . . ? H83A C83A H83C 109.5 . . ? H83B C83A H83C 109.5 . . ? C82A C84A H84A 109.5 . . ? C82A C84A H84B 109.5 . . ? H84A C84A H84B 109.5 . . ? C82A C84A H84C 109.5 . . ? H84A C84A H84C 109.5 . . ? H84B C84A H84C 109.5 . . ? C82B C81B Si8 116.4(12) . . ? C82B C81B H81C 108.2 . . ? Si8 C81B H81C 108.2 . . ? C82B C81B H81D 108.2 . . ? Si8 C81B H81D 108.2 . . ? H81C C81B H81D 107.3 . . ? C84B C82B C83B 111.4(10) . . ? C84B C82B C81B 111.1(10) . . ? C83B C82B C81B 110.9(10) . . ? C84B C82B H82B 107.7 . . ? C83B C82B H82B 107.7 . . ? C81B C82B H82B 107.7 . . ? C82B C83B H83D 109.5 . . ? C82B C83B H83E 109.5 . . ? H83D C83B H83E 109.5 . . ? C82B C83B H83F 109.5 . . ? H83D C83B H83F 109.5 . . ? H83E C83B H83F 109.5 . . ? C82B C84B H84D 109.5 . . ? C82B C84B H84E 109.5 . . ? H84D C84B H84E 109.5 . . ? C82B C84B H84F 109.5 . . ? H84D C84B H84F 109.5 . . ? H84E C84B H84F 109.5 . . ? Si4 O14 Si1 146.1(3) . . ? Si1 O15 Si8 145.0(3) . . ? Si5 O58 Si8 151.1(3) . . ? Si6 O36 Si3 152.4(3) . . ? Si2 O27 Si7 147.2(3) . . ? _diffrn_measured_fraction_theta_max 0.930 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.862 _refine_diff_density_min -1.082 _refine_diff_density_rms 0.107 data_1 _database_code_depnum_ccdc_archive 'CCDC 776150' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C54 H108 O13 P Rh Si8' _chemical_formula_sum 'C54 H108 O13 P Rh Si8' _chemical_formula_weight 1324.00 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9023(12) _cell_length_b 14.8954(18) _cell_length_c 21.769(3) _cell_angle_alpha 99.731(12) _cell_angle_beta 98.469(9) _cell_angle_gamma 104.467(10) _cell_volume 3306.6(7) _cell_formula_units_Z 2 _cell_measurement_temperature 100(1) _cell_measurement_reflns_used 9078 _cell_measurement_theta_min 2.8394 _cell_measurement_theta_max 28.1799 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.483 _exptl_absorpt_correction_T_min 0.95761 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET) (compiled Nov 6 2009,16:24:50) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_detector_area_resol_mean 16.1544 _diffrn_measurement_method '/w scan' _diffrn_reflns_number 24946 _diffrn_reflns_av_R_equivalents 0.0489 _diffrn_reflns_av_sigmaI/netI 0.1298 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12709 _reflns_number_gt 7712 _reflns_threshold_expression >2\s(I) _computing_data_collection 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_cell_refinement 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_data_reduction 'CrysAlis Pro (Oxford Diffraction (2009))' _computing_structure_solution 'SIR92 (Altomare et al., 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Stereochemical Workstation (Siemens, 1989)' _computing_publication_material 'SHELXL-97 (Sheldrick, 2008)' _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^ > 2\s(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^)+(0.0650P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 12709 _refine_ls_number_parameters 719 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0958 _refine_ls_R_factor_gt 0.0563 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1313 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.960 _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 0.62013(4) 0.54436(3) 0.24466(2) 0.01190(11) Uani 1 1 d . . . P1 P 0.56109(12) 0.51768(9) 0.33982(6) 0.0132(3) Uani 1 1 d . . . C111 C 0.4271(5) 0.5700(4) 0.3519(2) 0.0155(11) Uani 1 1 d . . . H111 H 0.4645 0.6397 0.3557 0.019 Uiso 1 1 calc R . . C112 C 0.3754(5) 0.5616(4) 0.4132(2) 0.0190(12) Uani 1 1 d . . . H11A H 0.3295 0.4945 0.4111 0.023 Uiso 1 1 calc R . . H11B H 0.4485 0.5824 0.4501 0.023 Uiso 1 1 calc R . . C113 C 0.2830(5) 0.6228(4) 0.4220(2) 0.0219(13) Uani 1 1 d . . . H11C H 0.2482 0.6149 0.4609 0.026 Uiso 1 1 calc R . . H11D H 0.3308 0.6905 0.4275 0.026 Uiso 1 1 calc R . . C114 C 0.1723(5) 0.5950(4) 0.3651(3) 0.0245(13) Uani 1 1 d . . . H11E H 0.1187 0.5297 0.3626 0.029 Uiso 1 1 calc R . . H11F H 0.1172 0.6383 0.3706 0.029 Uiso 1 1 calc R . . C115 C 0.2218(5) 0.5997(4) 0.3039(3) 0.0232(13) Uani 1 1 d . . . H11G H 0.2667 0.6664 0.3045 0.028 Uiso 1 1 calc R . . H11H H 0.1476 0.5775 0.2676 0.028 Uiso 1 1 calc R . . C116 C 0.3144(5) 0.5394(4) 0.2946(2) 0.0183(12) Uani 1 1 d . . . H11I H 0.3480 0.5470 0.2554 0.022 Uiso 1 1 calc R . . H11J H 0.2679 0.4716 0.2898 0.022 Uiso 1 1 calc R . . C121 C 0.5189(5) 0.3934(3) 0.3490(2) 0.0156(11) Uani 1 1 d . . . H121 H 0.5840 0.3661 0.3307 0.019 Uiso 1 1 calc R . . C122 C 0.5295(5) 0.3743(4) 0.4170(2) 0.0188(12) Uani 1 1 d . . . H12A H 0.6147 0.4124 0.4432 0.023 Uiso 1 1 calc R . . H12B H 0.4617 0.3942 0.4369 0.023 Uiso 1 1 calc R . . C123 C 0.5138(5) 0.2688(4) 0.4155(3) 0.0224(13) Uani 1 1 d . . . H12C H 0.5878 0.2512 0.4005 0.027 Uiso 1 1 calc R . . H12D H 0.5152 0.2579 0.4592 0.027 Uiso 1 1 calc R . . C124 C 0.3886(5) 0.2054(4) 0.3724(3) 0.0239(13) Uani 1 1 d . . . H12E H 0.3875 0.1382 0.3693 0.029 Uiso 1 1 calc R . . H12F H 0.3146 0.2152 0.3914 0.029 Uiso 1 1 calc R . . C125 C 0.3737(5) 0.2260(4) 0.3068(3) 0.0212(13) Uani 1 1 d . . . H12G H 0.2878 0.1877 0.2815 0.025 Uiso 1 1 calc R . . H12H H 0.4404 0.2072 0.2854 0.025 Uiso 1 1 calc R . . C126 C 0.3869(5) 0.3307(4) 0.3093(2) 0.0176(12) Uani 1 1 d . . . H12I H 0.3169 0.3485 0.3282 0.021 Uiso 1 1 calc R . . H12J H 0.3778 0.3420 0.2655 0.021 Uiso 1 1 calc R . . C131 C 0.6898(4) 0.5806(3) 0.4105(2) 0.0126(11) Uani 1 1 d . . . H131 H 0.6566 0.5637 0.4487 0.015 Uiso 1 1 calc R . . C132 C 0.7272(5) 0.6887(3) 0.4205(3) 0.0167(12) Uani 1 1 d . . . H13A H 0.7590 0.7077 0.3829 0.020 Uiso 1 1 calc R . . H13B H 0.6500 0.7111 0.4246 0.020 Uiso 1 1 calc R . . C133 C 0.8319(5) 0.7351(4) 0.4800(2) 0.0187(12) Uani 1 1 d . . . H13C H 0.8575 0.8048 0.4838 0.022 Uiso 1 1 calc R . . H13D H 0.7965 0.7218 0.5179 0.022 Uiso 1 1 calc R . . C134 C 0.9506(5) 0.6994(4) 0.4785(3) 0.0217(13) Uani 1 1 d . . . H13E H 1.0129 0.7273 0.5194 0.026 Uiso 1 1 calc R . . H13F H 0.9931 0.7202 0.4441 0.026 Uiso 1 1 calc R . . C135 C 0.9145(5) 0.5916(4) 0.4675(3) 0.0209(13) Uani 1 1 d . . . H13G H 0.9923 0.5699 0.4635 0.025 Uiso 1 1 calc R . . H13H H 0.8821 0.5713 0.5046 0.025 Uiso 1 1 calc R . . C136 C 0.8115(5) 0.5462(4) 0.4078(2) 0.0188(12) Uani 1 1 d . . . H13I H 0.7876 0.4763 0.4026 0.023 Uiso 1 1 calc R . . H13J H 0.8469 0.5620 0.3703 0.023 Uiso 1 1 calc R . . C1C C 0.7197(5) 0.5884(4) 0.1686(3) 0.0194(12) Uani 1 1 d . . . H1C H 0.7490 0.6510 0.1940 0.023 Uiso 1 1 d R . . C2C C 0.5893(5) 0.5524(3) 0.1441(2) 0.0143(11) Uani 1 1 d U . . H2C H 0.5359 0.5923 0.1536 0.017 Uiso 1 1 calc R . . C3C C 0.5252(5) 0.4555(4) 0.1037(3) 0.0225(13) Uani 1 1 d . . . H3C1 H 0.5447 0.4539 0.0606 0.027 Uiso 1 1 calc R . . H3C2 H 0.4304 0.4424 0.0997 0.027 Uiso 1 1 calc R . . C4C C 0.5686(5) 0.3777(4) 0.1306(2) 0.0176(12) Uani 1 1 d . . . H4C1 H 0.4987 0.3173 0.1158 0.021 Uiso 1 1 calc R . . H4C2 H 0.6453 0.3686 0.1139 0.021 Uiso 1 1 calc R . . C5C C 0.6017(5) 0.4006(3) 0.2027(3) 0.0171(12) Uani 1 1 d . . . H5C H 0.5340 0.3839 0.2252 0.021 Uiso 1 1 calc R . . C6C C 0.7290(5) 0.4457(3) 0.2383(3) 0.0182(12) Uani 1 1 d . . . H6C H 0.7411 0.4526 0.2831 0.022 Uiso 1 1 calc R . . C7C C 0.8464(5) 0.4838(4) 0.2117(3) 0.0229(13) Uani 1 1 d . . . H7C1 H 0.8799 0.4304 0.1954 0.027 Uiso 1 1 calc R . . H7C2 H 0.9143 0.5281 0.2465 0.027 Uiso 1 1 calc R . . C8C C 0.8211(5) 0.5357(4) 0.1579(3) 0.0242(13) Uani 1 1 d . . . H8C1 H 0.9027 0.5816 0.1558 0.029 Uiso 1 1 calc R . . H8C2 H 0.7908 0.4892 0.1168 0.029 Uiso 1 1 calc R . . Si1 Si 0.56837(13) 0.76196(9) 0.24410(7) 0.0106(3) Uani 1 1 d . . . O1 O 0.5988(3) 0.6769(2) 0.27097(16) 0.0148(8) Uani 1 1 d . . . Si2 Si 0.53831(13) 0.94576(10) 0.33076(7) 0.0121(3) Uani 1 1 d . . . C21 C 0.5733(5) 0.9647(4) 0.4179(2) 0.0143(11) Uani 1 1 d . . . H21A H 0.5609 1.0269 0.4353 0.017 Uiso 1 1 calc R . . H21B H 0.5075 0.9156 0.4301 0.017 Uiso 1 1 calc R . . C22 C 0.7063(5) 0.9630(4) 0.4513(3) 0.0191(12) Uani 1 1 d . . . H22 H 0.7301 0.9096 0.4260 0.023 Uiso 1 1 calc R . . C23 C 0.7055(5) 0.9458(4) 0.5176(3) 0.0229(13) Uani 1 1 d . . . H23A H 0.7904 0.9410 0.5363 0.030 Uiso 1 1 calc R . . H23B H 0.6395 0.8866 0.5157 0.030 Uiso 1 1 calc R . . H23C H 0.6859 0.9987 0.5439 0.030 Uiso 1 1 calc R . . C24 C 0.8087(5) 1.0544(4) 0.4535(3) 0.0326(15) Uani 1 1 d . . . H24A H 0.7849 1.1084 0.4758 0.042 Uiso 1 1 calc R . . H24B H 0.8151 1.0616 0.4101 0.042 Uiso 1 1 calc R . . H24C H 0.8923 1.0522 0.4761 0.042 Uiso 1 1 calc R . . Si3 Si 0.66849(13) 1.07107(10) 0.24547(7) 0.0121(3) Uani 1 1 d . . . C31 C 0.7825(5) 1.1920(3) 0.2689(3) 0.0186(12) Uani 1 1 d . B . H31A H 0.8106 1.2085 0.2300 0.022 Uiso 1 1 calc R . . H31B H 0.7333 1.2363 0.2833 0.022 Uiso 1 1 calc R . . C32 C 0.9039(5) 1.2125(4) 0.3198(3) 0.0239(13) Uani 1 1 d D . . H32 H 0.8700 1.1990 0.3585 0.029 Uiso 1 1 calc R A 1 C33A C 0.9908(11) 1.1498(9) 0.3110(9) 0.026(4) Uani 0.52(4) 1 d PDU B 1 H33A H 1.0234 1.1550 0.2718 0.039 Uiso 0.52(4) 1 calc PR B 1 H33B H 0.9422 1.0838 0.3082 0.039 Uiso 0.52(4) 1 calc PR B 1 H33C H 1.0636 1.1695 0.3473 0.039 Uiso 0.52(4) 1 calc PR B 1 C33B C 0.9963(14) 1.1669(14) 0.2854(11) 0.042(5) Uani 0.48(4) 1 d PDU B 2 H33D H 1.0839 1.1903 0.3113 0.063 Uiso 0.48(4) 1 calc PR B 2 H33E H 0.9968 1.1840 0.2439 0.063 Uiso 0.48(4) 1 calc PR B 2 H33F H 0.9662 1.0977 0.2795 0.063 Uiso 0.48(4) 1 calc PR B 2 C34 C 0.9752(6) 1.3178(4) 0.3380(3) 0.0337(15) Uani 1 1 d . B . H34A H 1.0519 1.3286 0.3711 0.044 Uiso 1 1 calc R . . H34B H 0.9181 1.3534 0.3542 0.044 Uiso 1 1 calc R . . H34C H 1.0017 1.3391 0.3006 0.044 Uiso 1 1 calc R . . Si4 Si 0.39488(13) 1.04196(10) 0.15953(7) 0.0126(3) Uani 1 1 d . . . C41 C 0.3412(5) 1.1434(3) 0.1396(2) 0.0156(11) Uani 1 1 d . . . H41A H 0.3877 1.2005 0.1733 0.019 Uiso 1 1 calc R . . H41B H 0.3673 1.1551 0.0994 0.019 Uiso 1 1 calc R . . C42 C 0.1948(5) 1.1325(4) 0.1322(2) 0.0163(12) Uani 1 1 d . . . H42 H 0.1655 1.1115 0.1702 0.020 Uiso 1 1 calc R . . C43 C 0.1202(5) 1.0587(4) 0.0735(3) 0.0241(13) Uani 1 1 d . . . H43A H 0.0280 1.0546 0.0689 0.031 Uiso 1 1 calc R . . H43B H 0.1329 0.9969 0.0775 0.031 Uiso 1 1 calc R . . H43C H 0.1511 1.0766 0.0361 0.031 Uiso 1 1 calc R . . C44 C 0.1692(6) 1.2280(4) 0.1296(3) 0.0301(15) Uani 1 1 d . . . H44A H 0.1965 1.2492 0.0922 0.039 Uiso 1 1 calc R . . H44B H 0.2180 1.2748 0.1682 0.039 Uiso 1 1 calc R . . H44C H 0.0767 1.2213 0.1266 0.039 Uiso 1 1 calc R . . Si5 Si 0.42175(13) 0.86699(10) 0.07475(7) 0.0113(3) Uani 1 1 d . . . C51 C 0.4210(5) 0.8366(4) -0.0112(2) 0.0164(12) Uani 1 1 d . . . H51A H 0.4902 0.8873 -0.0199 0.020 Uiso 1 1 calc R . . H51B H 0.4482 0.7777 -0.0187 0.020 Uiso 1 1 calc R . . C52 C 0.3008(5) 0.8216(3) -0.0624(2) 0.0150(11) Uani 1 1 d . . . H52 H 0.3240 0.8025 -0.1045 0.018 Uiso 1 1 calc R . . C53 C 0.1877(5) 0.7408(4) -0.0566(3) 0.0218(13) Uani 1 1 d . . . H53A H 0.1554 0.7601 -0.0182 0.028 Uiso 1 1 calc R . . H53B H 0.2168 0.6843 -0.0538 0.028 Uiso 1 1 calc R . . H53C H 0.1182 0.7264 -0.0940 0.028 Uiso 1 1 calc R . . C54 C 0.2613(5) 0.9119(4) -0.0631(3) 0.0247(13) Uani 1 1 d . . . H54A H 0.2341 0.9314 -0.0232 0.032 Uiso 1 1 calc R . . H54B H 0.1894 0.9006 -0.0989 0.032 Uiso 1 1 calc R . . H54C H 0.3348 0.9621 -0.0676 0.032 Uiso 1 1 calc R . . Si6 Si 0.29474(13) 0.73988(10) 0.15914(7) 0.0118(3) Uani 1 1 d . . . C61 C 0.1718(4) 0.6241(3) 0.1315(2) 0.0149(11) Uani 1 1 d . . . H61A H 0.1333 0.6080 0.1681 0.018 Uiso 1 1 calc R . . H61B H 0.1021 0.6312 0.0996 0.018 Uiso 1 1 calc R . . C62 C 0.2168(5) 0.5397(3) 0.1021(3) 0.0171(12) Uani 1 1 d . . . H62 H 0.2905 0.5347 0.1334 0.021 Uiso 1 1 calc R . . C63 C 0.2643(5) 0.5537(4) 0.0411(3) 0.0243(13) Uani 1 1 d . . . H63A H 0.1931 0.5578 0.0094 0.032 Uiso 1 1 calc R . . H63B H 0.2952 0.4998 0.0245 0.032 Uiso 1 1 calc R . . H63C H 0.3351 0.6124 0.0500 0.032 Uiso 1 1 calc R . . C64 C 0.1084(5) 0.4475(4) 0.0899(3) 0.0311(15) Uani 1 1 d . . . H64A H 0.0340 0.4514 0.0602 0.040 Uiso 1 1 calc R . . H64B H 0.0828 0.4376 0.1301 0.040 Uiso 1 1 calc R . . H64C H 0.1387 0.3943 0.0714 0.040 Uiso 1 1 calc R . . Si7 Si 0.26640(13) 0.91627(10) 0.24820(7) 0.0120(3) Uani 1 1 d . . . C71 C 0.1243(5) 0.9339(4) 0.2801(3) 0.0195(12) Uani 1 1 d . . . H71A H 0.1481 0.9999 0.3051 0.023 Uiso 1 1 calc R . . H71B H 0.0550 0.9283 0.2436 0.023 Uiso 1 1 calc R . . C72 C 0.0666(5) 0.8675(4) 0.3224(3) 0.0209(12) Uani 1 1 d . . . H72 H 0.1388 0.8653 0.3557 0.025 Uiso 1 1 calc R . . C73 C 0.0001(5) 0.7668(4) 0.2848(3) 0.0308(15) Uani 1 1 d . . . H73A H -0.0697 0.7676 0.2511 0.040 Uiso 1 1 calc R . . H73B H -0.0358 0.7275 0.3133 0.040 Uiso 1 1 calc R . . H73C H 0.0630 0.7405 0.2657 0.040 Uiso 1 1 calc R . . C74 C -0.0294(5) 0.9068(4) 0.3559(3) 0.0341(15) Uani 1 1 d . . . H74A H -0.1044 0.9049 0.3242 0.044 Uiso 1 1 calc R . . H74B H 0.0127 0.9725 0.3788 0.044 Uiso 1 1 calc R . . H74C H -0.0579 0.8680 0.3861 0.044 Uiso 1 1 calc R . . Si8 Si 0.69694(13) 0.89026(10) 0.16228(7) 0.0111(3) Uani 1 1 d . . . C81 C 0.8321(5) 0.8844(3) 0.1205(2) 0.0145(11) Uani 1 1 d . . . H81A H 0.8246 0.9179 0.0851 0.017 Uiso 1 1 calc R . . H81B H 0.9142 0.9197 0.1505 0.017 Uiso 1 1 calc R . . C82 C 0.8412(5) 0.7845(3) 0.0932(3) 0.0164(12) Uani 1 1 d . . . H82 H 0.8484 0.7507 0.1290 0.020 Uiso 1 1 calc R . . C83 C 0.7213(5) 0.7277(4) 0.0444(3) 0.0267(14) Uani 1 1 d . . . H83A H 0.6454 0.7215 0.0643 0.035 Uiso 1 1 calc R . . H83B H 0.7296 0.6645 0.0280 0.035 Uiso 1 1 calc R . . H83C H 0.7111 0.7604 0.0093 0.035 Uiso 1 1 calc R . . C84 C 0.9621(5) 0.7905(4) 0.0644(3) 0.0224(13) Uani 1 1 d . . . H84A H 0.9690 0.7263 0.0497 0.029 Uiso 1 1 calc R . . H84B H 1.0388 0.8273 0.0966 0.029 Uiso 1 1 calc R . . H84C H 0.9558 0.8217 0.0283 0.029 Uiso 1 1 calc R . . O2 O 0.5657(3) 0.8479(2) 0.30068(16) 0.0149(8) Uani 1 1 d . . . O3 O 0.4276(3) 0.7286(2) 0.19561(17) 0.0153(8) Uani 1 1 d . . . O4 O 0.3206(3) 0.7857(2) 0.09759(16) 0.0138(8) Uani 1 1 d . . . O5 O 0.3886(3) 0.9671(2) 0.09468(16) 0.0156(8) Uani 1 1 d . . . O6 O 0.5430(3) 1.0786(2) 0.19839(17) 0.0158(8) Uani 1 1 d . . . O7 O 0.6247(3) 1.0344(2) 0.30719(16) 0.0163(8) Uani 1 1 d . . . O8 O 0.6733(3) 0.8089(2) 0.20336(16) 0.0131(8) Uani 1 1 d . . . O9 O 0.7319(3) 0.9954(2) 0.20839(16) 0.0137(8) Uani 1 1 d . . . O10 O 0.3870(3) 0.9379(2) 0.30752(16) 0.0174(8) Uani 1 1 d . . . O11 O 0.5657(3) 0.8760(2) 0.11145(16) 0.0145(8) Uani 1 1 d . . . O12 O 0.2396(3) 0.8098(2) 0.20682(17) 0.0159(8) Uani 1 1 d . . . O13 O 0.3027(3) 0.9909(2) 0.20298(16) 0.0143(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 0.0129(2) 0.0112(2) 0.0131(2) 0.00412(17) 0.00374(17) 0.00437(16) P1 0.0144(7) 0.0121(7) 0.0138(7) 0.0042(6) 0.0029(6) 0.0041(6) C111 0.017(3) 0.016(3) 0.015(3) 0.005(2) 0.004(2) 0.005(2) C112 0.019(3) 0.030(3) 0.008(3) 0.006(3) 0.002(2) 0.008(3) C113 0.025(3) 0.030(3) 0.014(3) 0.004(3) 0.007(2) 0.013(3) C114 0.024(3) 0.033(3) 0.023(3) 0.009(3) 0.008(3) 0.014(3) C115 0.017(3) 0.035(4) 0.018(3) 0.009(3) 0.000(2) 0.009(3) C116 0.016(3) 0.023(3) 0.017(3) 0.007(3) 0.003(2) 0.006(2) C121 0.020(3) 0.014(3) 0.013(3) 0.000(2) 0.006(2) 0.004(2) C122 0.017(3) 0.020(3) 0.011(3) 0.001(2) -0.003(2) -0.003(2) C123 0.029(3) 0.021(3) 0.013(3) 0.005(3) 0.001(2) 0.000(3) C124 0.026(3) 0.018(3) 0.025(3) 0.006(3) 0.007(3) 0.000(3) C125 0.024(3) 0.020(3) 0.019(3) 0.004(3) 0.004(2) 0.007(2) C126 0.019(3) 0.020(3) 0.014(3) 0.005(2) 0.002(2) 0.007(2) C131 0.012(3) 0.013(3) 0.013(3) 0.006(2) 0.003(2) 0.002(2) C132 0.015(3) 0.013(3) 0.021(3) 0.003(2) 0.002(2) 0.004(2) C133 0.024(3) 0.013(3) 0.017(3) 0.000(2) 0.000(2) 0.005(2) C134 0.014(3) 0.026(3) 0.021(3) 0.004(3) -0.001(2) 0.002(2) C135 0.017(3) 0.028(3) 0.019(3) 0.004(3) 0.002(2) 0.012(3) C136 0.017(3) 0.022(3) 0.018(3) 0.006(3) 0.003(2) 0.005(2) C1C 0.028(3) 0.017(3) 0.019(3) 0.009(3) 0.015(3) 0.008(2) C2C 0.0137(14) 0.0158(14) 0.0145(14) 0.0022(9) 0.0033(9) 0.0063(9) C3C 0.019(3) 0.025(3) 0.023(3) 0.000(3) 0.002(2) 0.010(3) C4C 0.019(3) 0.011(3) 0.022(3) -0.001(2) 0.006(2) 0.003(2) C5C 0.012(3) 0.012(3) 0.029(3) 0.002(3) 0.008(2) 0.005(2) C6C 0.023(3) 0.014(3) 0.018(3) 0.000(2) 0.005(2) 0.008(2) C7C 0.018(3) 0.023(3) 0.028(3) 0.002(3) 0.006(3) 0.008(2) C8C 0.013(3) 0.035(4) 0.025(3) 0.006(3) 0.010(2) 0.005(3) Si1 0.0117(7) 0.0085(7) 0.0114(8) 0.0024(6) 0.0017(6) 0.0027(6) O1 0.0220(19) 0.0085(18) 0.015(2) 0.0050(16) 0.0026(16) 0.0057(15) Si2 0.0130(7) 0.0101(7) 0.0129(8) 0.0022(6) 0.0014(6) 0.0036(6) C21 0.016(3) 0.012(3) 0.015(3) 0.002(2) 0.001(2) 0.006(2) C22 0.019(3) 0.022(3) 0.016(3) 0.001(3) 0.002(2) 0.009(2) C23 0.023(3) 0.029(3) 0.018(3) 0.007(3) 0.001(2) 0.010(3) C24 0.026(3) 0.038(4) 0.026(4) 0.013(3) -0.005(3) -0.005(3) Si3 0.0114(7) 0.0109(7) 0.0138(8) 0.0027(6) 0.0010(6) 0.0034(6) C31 0.020(3) 0.013(3) 0.025(3) 0.007(3) 0.005(2) 0.007(2) C32 0.022(3) 0.016(3) 0.025(3) 0.005(3) -0.003(3) -0.006(2) C33A 0.026(4) 0.026(4) 0.026(5) 0.0061(13) 0.0044(13) 0.0072(16) C33B 0.042(5) 0.042(5) 0.042(5) 0.0092(15) 0.0077(14) 0.0121(18) C34 0.032(4) 0.018(3) 0.039(4) 0.003(3) -0.005(3) -0.005(3) Si4 0.0121(7) 0.0121(7) 0.0143(8) 0.0038(6) 0.0021(6) 0.0043(6) C41 0.018(3) 0.015(3) 0.014(3) 0.005(2) 0.003(2) 0.004(2) C42 0.018(3) 0.020(3) 0.016(3) 0.007(2) 0.005(2) 0.012(2) C43 0.016(3) 0.028(3) 0.028(3) 0.005(3) 0.001(2) 0.010(3) C44 0.033(3) 0.028(3) 0.030(4) 0.000(3) 0.001(3) 0.016(3) Si5 0.0117(7) 0.0105(7) 0.0114(8) 0.0028(6) 0.0014(6) 0.0029(6) C51 0.018(3) 0.016(3) 0.015(3) 0.004(2) 0.003(2) 0.003(2) C52 0.019(3) 0.015(3) 0.012(3) 0.005(2) 0.001(2) 0.005(2) C53 0.023(3) 0.018(3) 0.022(3) 0.003(3) -0.001(2) 0.006(2) C54 0.023(3) 0.022(3) 0.029(4) 0.007(3) 0.001(3) 0.009(3) Si6 0.0110(7) 0.0111(7) 0.0127(8) 0.0024(6) 0.0017(6) 0.0026(6) C61 0.012(3) 0.018(3) 0.016(3) 0.005(2) 0.001(2) 0.007(2) C62 0.020(3) 0.014(3) 0.017(3) 0.003(2) 0.000(2) 0.008(2) C63 0.040(4) 0.020(3) 0.016(3) 0.002(3) 0.005(3) 0.014(3) C64 0.033(4) 0.021(3) 0.034(4) 0.001(3) 0.003(3) 0.003(3) Si7 0.0117(7) 0.0122(7) 0.0127(8) 0.0033(6) 0.0030(6) 0.0038(6) C71 0.016(3) 0.021(3) 0.026(3) 0.007(3) 0.008(2) 0.012(2) C72 0.019(3) 0.023(3) 0.022(3) 0.005(3) 0.006(2) 0.006(2) C73 0.025(3) 0.020(3) 0.047(4) 0.009(3) 0.018(3) 0.000(3) C74 0.027(3) 0.042(4) 0.031(4) 0.004(3) 0.014(3) 0.003(3) Si8 0.0104(7) 0.0102(7) 0.0128(8) 0.0024(6) 0.0024(6) 0.0032(6) C81 0.015(3) 0.013(3) 0.017(3) 0.006(2) 0.005(2) 0.003(2) C82 0.022(3) 0.014(3) 0.019(3) 0.007(2) 0.009(2) 0.011(2) C83 0.030(3) 0.022(3) 0.025(3) -0.004(3) 0.010(3) 0.007(3) C84 0.022(3) 0.026(3) 0.025(3) 0.009(3) 0.009(3) 0.011(3) O2 0.024(2) 0.0087(18) 0.0142(19) 0.0024(16) 0.0025(16) 0.0102(16) O3 0.0101(18) 0.0136(19) 0.023(2) 0.0072(17) 0.0020(15) 0.0028(15) O4 0.0138(18) 0.0111(18) 0.016(2) 0.0040(16) 0.0025(15) 0.0010(15) O5 0.0183(19) 0.0152(19) 0.014(2) 0.0019(16) 0.0019(15) 0.0084(16) O6 0.0066(17) 0.0172(19) 0.024(2) 0.0042(17) 0.0010(15) 0.0049(15) O7 0.0202(19) 0.0119(19) 0.018(2) 0.0057(16) 0.0052(16) 0.0041(15) O8 0.0078(17) 0.0130(18) 0.022(2) 0.0100(16) 0.0073(15) 0.0028(14) O9 0.0102(17) 0.0088(18) 0.022(2) 0.0027(16) 0.0033(15) 0.0025(14) O10 0.0115(18) 0.024(2) 0.016(2) 0.0021(17) 0.0012(15) 0.0067(16) O11 0.0081(17) 0.0177(19) 0.017(2) 0.0045(16) 0.0003(15) 0.0027(15) O12 0.0148(18) 0.0090(18) 0.026(2) 0.0048(16) 0.0069(16) 0.0042(15) O13 0.0136(18) 0.0146(19) 0.019(2) 0.0082(16) 0.0074(15) 0.0065(15) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh1 O1 2.041(3) . ? Rh1 P1 2.3251(14) . ? P1 C121 1.845(5) . ? P1 C111 1.851(5) . ? P1 C131 1.853(5) . ? C111 C112 1.534(6) . ? C111 C116 1.534(7) . ? C111 H111 1.0000 . ? C112 C113 1.529(7) . ? C112 H11A 0.9900 . ? C112 H11B 0.9900 . ? C113 C114 1.516(7) . ? C113 H11C 0.9900 . ? C113 H11D 0.9900 . ? C114 C115 1.515(7) . ? C114 H11E 0.9900 . ? C114 H11F 0.9900 . ? C115 C116 1.522(7) . ? C115 H11G 0.9900 . ? C115 H11H 0.9900 . ? C116 H11I 0.9900 . ? C116 H11J 0.9900 . ? C121 C126 1.543(7) . ? C121 C122 1.548(7) . ? C121 H121 1.0000 . ? C122 C123 1.532(7) . ? C122 H12A 0.9900 . ? C122 H12B 0.9900 . ? C123 C124 1.521(7) . ? C123 H12C 0.9900 . ? C123 H12D 0.9900 . ? C124 C125 1.504(7) . ? C124 H12E 0.9900 . ? C124 H12F 0.9900 . ? C125 C126 1.522(7) . ? C125 H12G 0.9900 . ? C125 H12H 0.9900 . ? C126 H12I 0.9900 . ? C126 H12J 0.9900 . ? C131 C132 1.528(6) . ? C131 C136 1.543(6) . ? C131 H131 1.0000 . ? C132 C133 1.526(7) . ? C132 H13A 0.9900 . ? C132 H13B 0.9900 . ? C133 C134 1.519(7) . ? C133 H13C 0.9900 . ? C133 H13D 0.9900 . ? C134 C135 1.522(7) . ? C134 H13E 0.9900 . ? C134 H13F 0.9900 . ? C135 C136 1.518(7) . ? C135 H13G 0.9900 . ? C135 H13H 0.9900 . ? C136 H13I 0.9900 . ? C136 H13J 0.9900 . ? C1C C2C 1.376(7) . ? C1C C8C 1.529(7) . ? C1C H1C 0.9500 . ? C2C C3C 1.494(7) . ? C2C H2C 0.9500 . ? C3C C4C 1.527(7) . ? C3C H3C1 0.9900 . ? C3C H3C2 0.9900 . ? C4C C5C 1.517(7) . ? C4C H4C1 0.9900 . ? C4C H4C2 0.9900 . ? C5C C6C 1.420(7) . ? C5C H5C 0.9500 . ? C6C C7C 1.504(7) . ? C6C H6C 0.9500 . ? C7C C8C 1.537(7) . ? C7C H7C1 0.9900 . ? C7C H7C2 0.9900 . ? C8C H8C1 0.9900 . ? C8C H8C2 0.9900 . ? Si1 O1 1.569(3) . ? Si1 O2 1.629(3) . ? Si1 O3 1.637(3) . ? Si1 O8 1.641(3) . ? Si2 O2 1.611(3) . ? Si2 O10 1.622(3) . ? Si2 O7 1.626(4) . ? Si2 C21 1.837(5) . ? C21 C22 1.531(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.509(7) . ? C22 C24 1.518(7) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? Si3 O7 1.624(4) . ? Si3 O6 1.624(3) . ? Si3 O9 1.626(3) . ? Si3 C31 1.853(5) . ? C31 C32 1.525(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33A 1.497(8) . ? C32 C34 1.520(7) . ? C32 C33B 1.558(9) . ? C32 H32 1.0000 . ? C33A H33A 0.9800 . ? C33A H33B 0.9800 . ? C33A H33C 0.9800 . ? C33B H33D 0.9800 . ? C33B H33E 0.9800 . ? C33B H33F 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? Si4 O6 1.619(3) . ? Si4 O13 1.620(3) . ? Si4 O5 1.625(3) . ? Si4 C41 1.845(5) . ? C41 C42 1.544(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.508(7) . ? C42 C44 1.525(7) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? Si5 O11 1.615(3) . ? Si5 O4 1.621(3) . ? Si5 O5 1.625(3) . ? Si5 C51 1.847(5) . ? C51 C52 1.533(7) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C54 1.513(6) . ? C52 C53 1.530(7) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? Si6 O3 1.607(3) . ? Si6 O12 1.629(3) . ? Si6 O4 1.632(4) . ? Si6 C61 1.842(5) . ? C61 C62 1.536(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 C63 1.523(7) . ? C62 C64 1.525(7) . ? C62 H62 1.0000 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? Si7 O12 1.619(3) . ? Si7 O13 1.620(4) . ? Si7 O10 1.627(4) . ? Si7 C71 1.846(5) . ? C71 C72 1.545(7) . ? C71 H71A 0.9900 . ? C71 H71B 0.9900 . ? C72 C73 1.521(7) . ? C72 C74 1.535(7) . ? C72 H72 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? Si8 O8 1.617(3) . ? Si8 O11 1.618(3) . ? Si8 O9 1.632(3) . ? Si8 C81 1.854(5) . ? C81 C82 1.540(6) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C82 C83 1.513(7) . ? C82 C84 1.530(6) . ? C82 H82 1.0000 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Rh1 P1 86.16(10) . . ? C121 P1 C111 110.4(2) . . ? C121 P1 C131 103.6(2) . . ? C111 P1 C131 103.7(2) . . ? C121 P1 Rh1 116.62(16) . . ? C111 P1 Rh1 108.61(17) . . ? C131 P1 Rh1 113.17(16) . . ? C112 C111 C116 110.0(4) . . ? C112 C111 P1 116.8(3) . . ? C116 C111 P1 113.8(3) . . ? C112 C111 H111 105.0 . . ? C116 C111 H111 105.0 . . ? P1 C111 H111 105.0 . . ? C113 C112 C111 110.4(4) . . ? C113 C112 H11A 109.6 . . ? C111 C112 H11A 109.6 . . ? C113 C112 H11B 109.6 . . ? C111 C112 H11B 109.6 . . ? H11A C112 H11B 108.1 . . ? C114 C113 C112 110.9(4) . . ? C114 C113 H11C 109.5 . . ? C112 C113 H11C 109.5 . . ? C114 C113 H11D 109.5 . . ? C112 C113 H11D 109.5 . . ? H11C C113 H11D 108.1 . . ? C115 C114 C113 111.2(4) . . ? C115 C114 H11E 109.4 . . ? C113 C114 H11E 109.4 . . ? C115 C114 H11F 109.4 . . ? C113 C114 H11F 109.4 . . ? H11E C114 H11F 108.0 . . ? C114 C115 C116 112.2(4) . . ? C114 C115 H11G 109.2 . . ? C116 C115 H11G 109.2 . . ? C114 C115 H11H 109.2 . . ? C116 C115 H11H 109.2 . . ? H11G C115 H11H 107.9 . . ? C115 C116 C111 109.8(4) . . ? C115 C116 H11I 109.7 . . ? C111 C116 H11I 109.7 . . ? C115 C116 H11J 109.7 . . ? C111 C116 H11J 109.7 . . ? H11I C116 H11J 108.2 . . ? C126 C121 C122 107.9(4) . . ? C126 C121 P1 114.7(4) . . ? C122 C121 P1 118.4(3) . . ? C126 C121 H121 104.8 . . ? C122 C121 H121 104.8 . . ? P1 C121 H121 104.8 . . ? C123 C122 C121 110.8(4) . . ? C123 C122 H12A 109.5 . . ? C121 C122 H12A 109.5 . . ? C123 C122 H12B 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 108.1 . . ? C124 C123 C122 112.4(4) . . ? C124 C123 H12C 109.1 . . ? C122 C123 H12C 109.1 . . ? C124 C123 H12D 109.1 . . ? C122 C123 H12D 109.1 . . ? H12C C123 H12D 107.9 . . ? C125 C124 C123 111.8(5) . . ? C125 C124 H12E 109.2 . . ? C123 C124 H12E 109.2 . . ? C125 C124 H12F 109.2 . . ? C123 C124 H12F 109.2 . . ? H12E C124 H12F 107.9 . . ? C124 C125 C126 111.4(4) . . ? C124 C125 H12G 109.3 . . ? C126 C125 H12G 109.3 . . ? C124 C125 H12H 109.3 . . ? C126 C125 H12H 109.3 . . ? H12G C125 H12H 108.0 . . ? C125 C126 C121 111.2(4) . . ? C125 C126 H12I 109.4 . . ? C121 C126 H12I 109.4 . . ? C125 C126 H12J 109.4 . . ? C121 C126 H12J 109.4 . . ? H12I C126 H12J 108.0 . . ? C132 C131 C136 109.4(4) . . ? C132 C131 P1 114.3(3) . . ? C136 C131 P1 110.8(3) . . ? C132 C131 H131 107.4 . . ? C136 C131 H131 107.4 . . ? P1 C131 H131 107.4 . . ? C133 C132 C131 111.1(4) . . ? C133 C132 H13A 109.4 . . ? C131 C132 H13A 109.4 . . ? C133 C132 H13B 109.4 . . ? C131 C132 H13B 109.4 . . ? H13A C132 H13B 108.0 . . ? C134 C133 C132 112.2(4) . . ? C134 C133 H13C 109.2 . . ? C132 C133 H13C 109.2 . . ? C134 C133 H13D 109.2 . . ? C132 C133 H13D 109.2 . . ? H13C C133 H13D 107.9 . . ? C133 C134 C135 111.1(4) . . ? C133 C134 H13E 109.4 . . ? C135 C134 H13E 109.4 . . ? C133 C134 H13F 109.4 . . ? C135 C134 H13F 109.4 . . ? H13E C134 H13F 108.0 . . ? C136 C135 C134 111.0(4) . . ? C136 C135 H13G 109.4 . . ? C134 C135 H13G 109.4 . . ? C136 C135 H13H 109.4 . . ? C134 C135 H13H 109.4 . . ? H13G C135 H13H 108.0 . . ? C135 C136 C131 111.6(4) . . ? C135 C136 H13I 109.3 . . ? C131 C136 H13I 109.3 . . ? C135 C136 H13J 109.3 . . ? C131 C136 H13J 109.3 . . ? H13I C136 H13J 108.0 . . ? C2C C1C C8C 125.1(5) . . ? C2C C1C H1C 117.3 . . ? C8C C1C H1C 117.6 . . ? C1C C2C C3C 125.1(4) . . ? C1C C2C H2C 117.5 . . ? C3C C2C H2C 117.5 . . ? C2C C3C C4C 112.9(4) . . ? C2C C3C H3C1 109.0 . . ? C4C C3C H3C1 109.0 . . ? C2C C3C H3C2 109.0 . . ? C4C C3C H3C2 109.0 . . ? H3C1 C3C H3C2 107.8 . . ? C5C C4C C3C 112.6(4) . . ? C5C C4C H4C1 109.1 . . ? C3C C4C H4C1 109.1 . . ? C5C C4C H4C2 109.1 . . ? C3C C4C H4C2 109.1 . . ? H4C1 C4C H4C2 107.8 . . ? C6C C5C C4C 123.2(5) . . ? C6C C5C H5C 118.4 . . ? C4C C5C H5C 118.4 . . ? C5C C6C C7C 126.2(5) . . ? C5C C6C H6C 116.9 . . ? C7C C6C H6C 116.9 . . ? C6C C7C C8C 114.0(4) . . ? C6C C7C H7C1 108.8 . . ? C8C C7C H7C1 108.8 . . ? C6C C7C H7C2 108.8 . . ? C8C C7C H7C2 108.8 . . ? H7C1 C7C H7C2 107.6 . . ? C1C C8C C7C 111.2(4) . . ? C1C C8C H8C1 109.4 . . ? C7C C8C H8C1 109.4 . . ? C1C C8C H8C2 109.4 . . ? C7C C8C H8C2 109.4 . . ? H8C1 C8C H8C2 108.0 . . ? O1 Si1 O2 111.75(19) . . ? O1 Si1 O3 111.38(18) . . ? O2 Si1 O3 107.41(17) . . ? O1 Si1 O8 113.68(17) . . ? O2 Si1 O8 106.46(18) . . ? O3 Si1 O8 105.74(18) . . ? Si1 O1 Rh1 143.1(2) . . ? O2 Si2 O10 109.18(18) . . ? O2 Si2 O7 110.81(18) . . ? O10 Si2 O7 108.29(18) . . ? O2 Si2 C21 109.1(2) . . ? O10 Si2 C21 108.5(2) . . ? O7 Si2 C21 110.9(2) . . ? C22 C21 Si2 118.8(3) . . ? C22 C21 H21A 107.6 . . ? Si2 C21 H21A 107.6 . . ? C22 C21 H21B 107.6 . . ? Si2 C21 H21B 107.6 . . ? H21A C21 H21B 107.1 . . ? C23 C22 C24 110.0(5) . . ? C23 C22 C21 112.0(4) . . ? C24 C22 C21 111.1(4) . . ? C23 C22 H22 107.9 . . ? C24 C22 H22 107.9 . . ? C21 C22 H22 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7 Si3 O6 109.47(18) . . ? O7 Si3 O9 108.83(18) . . ? O6 Si3 O9 109.63(18) . . ? O7 Si3 C31 111.0(2) . . ? O6 Si3 C31 106.4(2) . . ? O9 Si3 C31 111.5(2) . . ? C32 C31 Si3 119.8(4) . . ? C32 C31 H31A 107.4 . . ? Si3 C31 H31A 107.4 . . ? C32 C31 H31B 107.4 . . ? Si3 C31 H31B 107.4 . . ? H31A C31 H31B 106.9 . . ? C33A C32 C34 113.7(7) . . ? C33A C32 C31 117.7(7) . . ? C34 C32 C31 111.6(4) . . ? C34 C32 C33B 103.9(8) . . ? C31 C32 C33B 104.4(9) . . ? C33A C32 H32 104.1 . . ? C34 C32 H32 104.0 . . ? C31 C32 H32 104.0 . . ? C33B C32 H32 128.7 . . ? C32 C33A H33A 109.5 . . ? C32 C33A H33B 109.5 . . ? C32 C33A H33C 109.5 . . ? C32 C33B H33D 109.5 . . ? C32 C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C32 C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O6 Si4 O13 109.41(19) . . ? O6 Si4 O5 108.15(18) . . ? O13 Si4 O5 110.30(18) . . ? O6 Si4 C41 109.9(2) . . ? O13 Si4 C41 109.2(2) . . ? O5 Si4 C41 109.8(2) . . ? C42 C41 Si4 116.0(3) . . ? C42 C41 H41A 108.3 . . ? Si4 C41 H41A 108.3 . . ? C42 C41 H41B 108.3 . . ? Si4 C41 H41B 108.3 . . ? H41A C41 H41B 107.4 . . ? C43 C42 C44 110.7(4) . . ? C43 C42 C41 110.8(4) . . ? C44 C42 C41 109.7(4) . . ? C43 C42 H42 108.5 . . ? C44 C42 H42 108.5 . . ? C41 C42 H42 108.5 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? O11 Si5 O4 108.17(18) . . ? O11 Si5 O5 109.20(18) . . ? O4 Si5 O5 108.36(18) . . ? O11 Si5 C51 106.6(2) . . ? O4 Si5 C51 112.5(2) . . ? O5 Si5 C51 111.8(2) . . ? C52 C51 Si5 122.7(3) . . ? C52 C51 H51A 106.7 . . ? Si5 C51 H51A 106.7 . . ? C52 C51 H51B 106.7 . . ? Si5 C51 H51B 106.7 . . ? H51A C51 H51B 106.6 . . ? C54 C52 C53 111.0(4) . . ? C54 C52 C51 112.2(4) . . ? C53 C52 C51 112.1(4) . . ? C54 C52 H52 107.1 . . ? C53 C52 H52 107.1 . . ? C51 C52 H52 107.1 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O3 Si6 O12 109.72(19) . . ? O3 Si6 O4 109.62(18) . . ? O12 Si6 O4 109.02(18) . . ? O3 Si6 C61 111.0(2) . . ? O12 Si6 C61 108.76(19) . . ? O4 Si6 C61 108.6(2) . . ? C62 C61 Si6 117.1(3) . . ? C62 C61 H61A 108.0 . . ? Si6 C61 H61A 108.0 . . ? C62 C61 H61B 108.0 . . ? Si6 C61 H61B 108.0 . . ? H61A C61 H61B 107.3 . . ? C63 C62 C64 110.5(5) . . ? C63 C62 C61 111.7(4) . . ? C64 C62 C61 110.4(4) . . ? C63 C62 H62 108.0 . . ? C64 C62 H62 108.0 . . ? C61 C62 H62 108.0 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O12 Si7 O13 108.64(19) . . ? O12 Si7 O10 109.73(18) . . ? O13 Si7 O10 109.10(19) . . ? O12 Si7 C71 112.3(2) . . ? O13 Si7 C71 108.6(2) . . ? O10 Si7 C71 108.4(2) . . ? C72 C71 Si7 118.6(3) . . ? C72 C71 H71A 107.7 . . ? Si7 C71 H71A 107.7 . . ? C72 C71 H71B 107.7 . . ? Si7 C71 H71B 107.7 . . ? H71A C71 H71B 107.1 . . ? C73 C72 C74 109.6(4) . . ? C73 C72 C71 112.2(5) . . ? C74 C72 C71 110.4(4) . . ? C73 C72 H72 108.2 . . ? C74 C72 H72 108.2 . . ? C71 C72 H72 108.2 . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? O8 Si8 O11 109.14(18) . . ? O8 Si8 O9 110.57(19) . . ? O11 Si8 O9 107.79(17) . . ? O8 Si8 C81 110.5(2) . . ? O11 Si8 C81 110.2(2) . . ? O9 Si8 C81 108.6(2) . . ? C82 C81 Si8 116.4(3) . . ? C82 C81 H81A 108.2 . . ? Si8 C81 H81A 108.2 . . ? C82 C81 H81B 108.2 . . ? Si8 C81 H81B 108.2 . . ? H81A C81 H81B 107.3 . . ? C83 C82 C84 110.5(4) . . ? C83 C82 C81 111.2(4) . . ? C84 C82 C81 110.7(4) . . ? C83 C82 H82 108.1 . . ? C84 C82 H82 108.1 . . ? C81 C82 H82 108.1 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? Si2 O2 Si1 156.1(2) . . ? Si6 O3 Si1 156.9(2) . . ? Si5 O4 Si6 142.5(2) . . ? Si5 O5 Si4 137.9(2) . . ? Si4 O6 Si3 154.9(2) . . ? Si3 O7 Si2 144.3(2) . . ? Si8 O8 Si1 139.4(2) . . ? Si3 O9 Si8 143.2(2) . . ? Si2 O10 Si7 147.4(2) . . ? Si5 O11 Si8 167.2(2) . . ? Si7 O12 Si6 145.4(2) . . ? Si4 O13 Si7 152.4(2) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.314 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.114