# Electronic Supplementary Material (ESI) for Catalysis Science & Technology # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_compnd_2a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_melting_point ? _chemical_formula_moiety 'C35 H58 Cl N2 O3 Rh Si, 0.5(C6 H14)' _chemical_formula_sum 'C38 H65 Cl N2 O3 Rh Si' _chemical_formula_weight 764.37 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2529(12) _cell_length_b 12.6020(15) _cell_length_c 16.390(2) _cell_angle_alpha 73.082(2) _cell_angle_beta 87.303(2) _cell_angle_gamma 89.419(2) _cell_volume 2023.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 231 _cell_measurement_theta_min 2.334 _cell_measurement_theta_max 26.445 _exptl_crystal_description NEEDLE _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.211 _exptl_crystal_size_mid 0.211 _exptl_crystal_size_min 0.141 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.254 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 814 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.6753 _exptl_absorpt_correction_T_max 0.9255 _exptl_absorpt_process_details ; Multi-scan correction included in APEX2 package (Bruker AXS, 2008) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX DUO system' _diffrn_measurement_method '\w rotations with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_reflns_number 19266 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0752 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 30.49 _reflns_number_total 10794 _reflns_number_gt 8226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_cell_refinement 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_data_reduction 'SAINT+ in APEX2 v. 2008.4 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'XP program, SHELXTL v6.12, Bruker2000' _computing_publication_material ENCIFER _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. The structure was solved by Patterson and an anisotropic refinement was applied to all non-disordered atoms of the metal complex. A typical disorder of the oxygen atoms of the alcoxy groups was observed; two positions were considered for each oxygen with complementary occupancy factors (0.839 and 0.161(6)). Hydrogen atoms were included in all cases in calculated positions and refined with a riding model. Hydrogens for the tertiary carbons were only included in the calculated positions for the high occupancy oxygen atoms. At this point of refinement, several residual peaks were observed far away from the metal complex. They were interpreted as a highly disordered solvent molecule. Six residual peaks, with no reasonable geometry, were included in the refinement to compensate the presence of half an hexane molecule. All residual peaks above 1.0 are in close proximity of the metal atom and have no chemical sense. ; _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^)+(0.0827P)^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 10794 _refine_ls_number_parameters 442 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_gt 0.0545 _refine_ls_wR_factor_ref 0.1460 _refine_ls_wR_factor_gt 0.1325 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _iucr_refine_instructions_details ; TITL fjl13dm in P -1 CELL 0.71073 10.2529 12.6020 16.3901 73.082 87.303 89.419 ZERR 2.00 0.0012 0.0015 0.0020 0.002 0.002 0.002 LATT 1 SFAC C H CL N O RH SI UNIT 76 130 2 4 6 2 2 MERG 2 SUMP 3.0 0.01 1.0 2 1.0 3 1.0 4 1.0 5 1.0 6 1.0 7 OMIT 1 0 0 FREE O1a O1b FREE O1b C27 FREE O1b H27 FREE O1b C28 FREE O2A O2B FREE C30 O2b FREE O2B H30 FREE O3A O3B FREE C33 O3b DFIX 91.0 0.01 Si O1a Si O1b Si O2a Si O2b Si O3a Si O3b FMAP 2 PLAN 10 ACTA 52.00 BOND $H L.S. 6 TEMP -173.00 WGHT 0.082700 FVAR 0.58410 0.63966 0.78248 0.29170 0.58663 0.42743 0.30990 FVAR 0.83878 1.62245 RH1 6 0.806834 0.820788 0.621257 11.00000 0.01598 0.02162 = 0.02475 -0.00424 -0.00066 -0.00295 SI 7 0.769828 0.959403 0.204193 11.00000 0.02551 0.03933 = 0.03694 -0.01516 0.00739 -0.00665 CL1 3 0.705307 0.983909 0.640734 11.00000 0.02745 0.02641 = 0.02997 -0.00834 -0.00220 0.00062 PART 1 O1A 5 0.842130 0.841966 0.216296 81.00000 0.03754 0.04843 = 0.04002 -0.01890 -0.00496 0.00484 C27 1 0.937117 0.800951 0.276521 11.00000 0.03332 0.08008 = 0.06242 -0.01247 -0.00527 -0.00168 AFIX 13 H27 2 0.917731 0.833110 0.324797 81.00000 -1.20000 AFIX 0 PART 2 O2A 5 0.650451 0.957410 0.139262 81.00000 0.03447 0.03362 = 0.03694 -0.00814 -0.00501 -0.00900 C30 1 0.565009 0.869236 0.145849 11.00000 0.03587 0.05873 = 0.03792 -0.01783 -0.00609 0.00097 AFIX 13 H30 2 0.590807 0.805899 0.195127 81.00000 -1.20000 AFIX 0 PART 3 O3A 5 0.859585 1.064507 0.153447 81.00000 0.02763 0.05129 = 0.02504 -0.01363 0.00495 -0.00672 C33 1 0.909375 1.086643 0.067125 11.00000 0.04145 0.06313 = 0.03296 -0.02336 0.01500 -0.02080 AFIX 13 H33 2 0.911813 1.015830 0.051177 81.00000 -1.20000 AFIX 0 PART 0 O1B 5 0.894041 0.885795 0.254102 -81.00000 0.03974 O2B 5 0.688549 0.871665 0.178044 -81.00000 0.02358 O3B 5 0.825135 1.078675 0.146472 -81.00000 0.02405 N1 4 0.560091 0.830687 0.524161 11.00000 0.01735 0.02173 = 0.02657 -0.00377 -0.00054 -0.00491 N2 4 0.544552 0.696016 0.639487 11.00000 0.01787 0.02200 = 0.02791 -0.00161 -0.00177 -0.00389 C1 1 0.893344 0.662942 0.641966 11.00000 0.01746 0.02905 = 0.04003 -0.00465 0.00214 -0.00035 AFIX 43 H1 2 0.809966 0.633417 0.664513 11.00000 -1.20000 AFIX 0 C2 1 0.906466 0.721736 0.555215 11.00000 0.02428 0.03160 = 0.03761 -0.01371 -0.00328 0.00509 AFIX 43 H2 2 0.832062 0.725745 0.522035 11.00000 -1.20000 AFIX 0 C3 1 1.028846 0.779019 0.510377 11.00000 0.03356 0.04071 = 0.03960 -0.00910 0.01065 0.00400 AFIX 23 H3A 2 1.006585 0.829150 0.454086 11.00000 -1.20000 H3B 2 1.090090 0.722535 0.500100 11.00000 -1.20000 AFIX 0 C4 1 1.098059 0.846644 0.559898 11.00000 0.02304 0.04056 = 0.04474 0.00025 0.00321 -0.00348 AFIX 23 H4A 2 1.159981 0.798211 0.598438 11.00000 -1.20000 H4B 2 1.148808 0.907360 0.519157 11.00000 -1.20000 AFIX 0 C5 1 1.002705 0.894939 0.611460 11.00000 0.01649 0.03201 = 0.03975 -0.00457 -0.00534 -0.00576 AFIX 43 H5 2 0.963420 0.963878 0.583923 11.00000 -1.20000 AFIX 0 C6 1 0.968516 0.845412 0.696436 11.00000 0.02216 0.03640 = 0.03635 -0.00923 -0.00985 -0.00025 AFIX 43 H6 2 0.912022 0.885236 0.724509 11.00000 -1.20000 AFIX 0 C7 1 1.014276 0.732514 0.748162 11.00000 0.03627 0.04614 = 0.04081 -0.00346 -0.01615 0.00455 AFIX 23 H7A 2 0.960773 0.708788 0.802274 11.00000 -1.20000 H7B 2 1.105958 0.738660 0.762741 11.00000 -1.20000 AFIX 0 C8 1 1.005883 0.643784 0.702207 11.00000 0.02812 0.03228 = 0.04284 0.00414 -0.00587 0.00506 AFIX 23 H8A 2 0.994713 0.570342 0.745119 11.00000 -1.20000 H8B 2 1.088948 0.642689 0.669129 11.00000 -1.20000 AFIX 0 C9 1 0.628349 0.774910 0.592135 11.00000 0.01970 0.01780 = 0.02484 -0.00361 0.00003 -0.00306 C10 1 0.424327 0.704713 0.602212 11.00000 0.01435 0.03203 = 0.03436 -0.00439 -0.00028 -0.00495 AFIX 43 H10 2 0.349366 0.659943 0.624051 11.00000 -1.20000 AFIX 0 C11 1 0.434369 0.788722 0.529222 11.00000 0.01653 0.02850 = 0.02907 -0.00543 -0.00186 -0.00340 AFIX 43 H11 2 0.368560 0.814135 0.489232 11.00000 -1.20000 AFIX 0 C12 1 0.575954 0.608001 0.714657 11.00000 0.01906 0.02329 = 0.03230 0.00221 -0.00211 -0.00713 C13 1 0.582471 0.630877 0.792496 11.00000 0.02719 0.02682 = 0.03297 -0.00149 -0.00207 -0.00705 C14 1 0.549383 0.741238 0.805004 11.00000 0.04086 0.03414 = 0.03037 -0.00501 0.00486 -0.00051 AFIX 13 H14 2 0.543179 0.796026 0.747299 11.00000 -1.20000 AFIX 0 C15 1 0.653900 0.782893 0.852098 11.00000 0.07830 0.03702 = 0.04380 -0.01711 -0.00775 -0.00130 AFIX 137 H15A 2 0.655444 0.734942 0.911048 11.00000 -1.50000 H15B 2 0.633675 0.859031 0.852188 11.00000 -1.50000 H15C 2 0.739473 0.781366 0.823196 11.00000 -1.50000 AFIX 0 C16 1 0.416413 0.737613 0.853000 11.00000 0.05351 0.06632 = 0.07720 0.00089 0.03073 0.01132 AFIX 137 H16A 2 0.347436 0.723474 0.818038 11.00000 -1.50000 H16B 2 0.400526 0.808849 0.864488 11.00000 -1.50000 H16C 2 0.416434 0.678203 0.907099 11.00000 -1.50000 AFIX 0 C17 1 0.617929 0.543949 0.862198 11.00000 0.04683 0.03455 = 0.03507 -0.00011 -0.01018 -0.00952 AFIX 43 H17 2 0.622555 0.556352 0.916455 11.00000 -1.20000 AFIX 0 C18 1 0.646546 0.439914 0.854014 11.00000 0.05866 0.03182 = 0.04297 0.00460 -0.02169 -0.00621 AFIX 43 H18 2 0.672498 0.382259 0.902106 11.00000 -1.20000 AFIX 0 C19 1 0.637491 0.419831 0.776413 11.00000 0.06006 0.02122 = 0.04662 -0.00112 -0.01679 -0.00487 AFIX 43 H19 2 0.656233 0.347751 0.771828 11.00000 -1.20000 AFIX 0 C20 1 0.601391 0.502954 0.704254 11.00000 0.03549 0.02623 = 0.03626 -0.00166 -0.00692 -0.00739 C21 1 0.589176 0.477311 0.620270 11.00000 0.04740 0.02428 = 0.04065 -0.00900 -0.00561 -0.00419 AFIX 13 H21 2 0.579572 0.549426 0.574920 11.00000 -1.20000 AFIX 0 C22 1 0.708810 0.418097 0.594485 11.00000 0.06845 0.04870 = 0.07068 -0.02949 -0.01083 0.01215 AFIX 137 H22A 2 0.787826 0.460697 0.595542 11.00000 -1.50000 H22B 2 0.699497 0.412047 0.536769 11.00000 -1.50000 H22C 2 0.715486 0.343741 0.634680 11.00000 -1.50000 AFIX 0 C23 1 0.465853 0.409595 0.623705 11.00000 0.06905 0.04981 = 0.04973 -0.01316 -0.01564 -0.01994 AFIX 137 H23A 2 0.471291 0.339143 0.668913 11.00000 -1.50000 H23B 2 0.457187 0.394875 0.568696 11.00000 -1.50000 H23C 2 0.389689 0.451174 0.635718 11.00000 -1.50000 AFIX 0 C24 1 0.612073 0.922350 0.453172 11.00000 0.02479 0.02105 = 0.02535 -0.00301 -0.00061 -0.00450 AFIX 23 H24A 2 0.690177 0.953201 0.471535 11.00000 -1.20000 H24B 2 0.545820 0.981804 0.438922 11.00000 -1.20000 AFIX 0 C25 1 0.648715 0.888360 0.374298 11.00000 0.02577 0.02715 = 0.03103 -0.00755 0.00739 -0.00265 AFIX 23 H25A 2 0.569784 0.863149 0.352618 11.00000 -1.20000 H25B 2 0.710974 0.825812 0.388633 11.00000 -1.20000 AFIX 0 C26 1 0.711332 0.986471 0.304927 11.00000 0.02903 0.03372 = 0.02495 -0.00857 0.00300 -0.00758 AFIX 23 H26A 2 0.786224 1.013507 0.329383 11.00000 -1.20000 H26B 2 0.646697 1.047236 0.290817 11.00000 -1.20000 AFIX 0 C28 1 1.074944 0.834326 0.243909 11.00000 0.05509 0.12292 = 0.07323 0.00160 -0.00466 -0.01455 AFIX 137 H28A 2 1.106843 0.787903 0.208562 11.00000 -1.50000 H28B 2 1.131071 0.824450 0.292325 11.00000 -1.50000 H28C 2 1.076575 0.912335 0.209625 11.00000 -1.50000 AFIX 0 C29 1 0.920043 0.679121 0.311430 11.00000 0.06849 0.05881 = 0.18517 -0.00794 -0.03589 0.00211 AFIX 137 H29A 2 0.826958 0.661453 0.323470 11.00000 -1.50000 H29B 2 0.966882 0.652392 0.364277 11.00000 -1.50000 H29C 2 0.955008 0.643022 0.269608 11.00000 -1.50000 AFIX 0 C31 1 0.431080 0.901057 0.164412 11.00000 0.04615 0.03723 = 0.06279 -0.00405 0.02189 -0.00426 AFIX 137 H31A 2 0.428948 0.926274 0.215658 11.00000 -1.50000 H31B 2 0.372889 0.836950 0.173999 11.00000 -1.50000 H31C 2 0.402086 0.961169 0.115960 11.00000 -1.50000 AFIX 0 C32 1 0.581068 0.832942 0.066492 11.00000 0.04429 0.05922 = 0.04234 -0.02198 0.00466 -0.01274 AFIX 137 H32A 2 0.553751 0.892892 0.017367 11.00000 -1.50000 H32B 2 0.527039 0.767083 0.072796 11.00000 -1.50000 H32C 2 0.672901 0.815153 0.057497 11.00000 -1.50000 AFIX 0 C34 1 0.826716 1.168890 0.006436 11.00000 0.06753 0.10390 = 0.03121 -0.00531 0.00165 -0.02549 AFIX 137 H34A 2 0.740097 1.136831 0.006210 11.00000 -1.50000 H34B 2 0.867999 1.187343 -0.051138 11.00000 -1.50000 H3C 2 0.817968 1.236309 0.024528 11.00000 -1.50000 AFIX 0 C35 1 1.047773 1.128778 0.065560 11.00000 0.04071 0.09556 = 0.06826 -0.03713 0.01577 -0.02129 AFIX 137 H35A 2 1.045922 1.199083 0.079863 11.00000 -1.50000 H35B 2 1.088888 1.140387 0.008425 11.00000 -1.50000 H35C 2 1.097941 1.074092 0.107380 11.00000 -1.50000 AFIX 0 C51 1 0.244208 0.446623 0.856325 21.00000 0.08842 C52 1 0.044719 0.500030 0.978893 31.00000 0.13357 C53 1 0.064150 0.456711 0.939495 41.00000 0.05857 C54 1 0.204798 0.456420 0.906585 51.00000 0.09301 C55 1 0.150131 0.483797 0.961812 61.00000 0.10150 C56 1 0.120072 0.422582 0.912620 71.00000 0.08435 HKLF 4 1.0 1.00 0.00 0.00 0.00 1.00 0.00 0.00 0.00 1.00 REM fjl13dm in P -1 REM R1 = 0.0545 for 8226 Fo > 4sig(Fo) and 0.0772 for all 10794 data REM 442 parameters refined using 7 restraints END WGHT 0.0827 0.0000 REM Highest difference peak 1.706, deepest hole -1.230, 1-sigma level 0.115 Q1 1 0.8319 0.8165 0.6691 11.00000 0.05 1.71 Q2 1 0.7794 0.8221 0.5728 11.00000 0.05 1.67 Q3 1 0.7792 0.8905 0.6086 11.00000 0.05 1.39 Q4 1 0.8353 0.7527 0.6430 11.00000 0.05 1.36 Q5 1 0.5860 0.9323 0.1176 11.00000 0.05 0.83 Q6 1 0.7448 0.9111 0.6528 11.00000 0.05 0.79 Q7 1 0.9502 0.7776 0.2309 11.00000 0.05 0.78 Q8 1 0.7965 0.9477 0.2459 11.00000 0.05 0.77 Q9 1 0.7003 0.9661 0.5929 11.00000 0.05 0.69 Q10 1 0.1959 0.4627 0.9415 11.00000 0.05 0.68 ; 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 0.80683(2) 0.82079(2) 0.621257(16) 0.02130(8) Uani 1 1 d . . . Si Si 0.76983(10) 0.95940(9) 0.20419(7) 0.0333(2) Uani 1 1 d D . . Cl1 Cl 0.70531(8) 0.98391(6) 0.64073(5) 0.02789(17) Uani 1 1 d . . . O1A O 0.8421(3) 0.8420(3) 0.2163(2) 0.0406(9) Uani 0.839(5) 1 d PD A 1 C27 C 0.9371(5) 0.8010(5) 0.2765(3) 0.0602(13) Uani 1 1 d . A 1 H27 H 0.9177 0.8331 0.3248 0.072 Uiso 0.839(5) 1 calc PR A 1 O2A O 0.6505(3) 0.9574(2) 0.13926(19) 0.0353(8) Uani 0.839(5) 1 d PD A 2 C30 C 0.5650(4) 0.8692(4) 0.1458(3) 0.0432(9) Uani 1 1 d . A 2 H30 H 0.5908 0.8059 0.1951 0.052 Uiso 0.839(5) 1 calc PR A 2 O3A O 0.8596(5) 1.0645(3) 0.1534(3) 0.0343(10) Uani 0.839(5) 1 d PD A 3 C33 C 0.9094(4) 1.0866(4) 0.0671(3) 0.0443(10) Uani 1 1 d . A 3 H33 H 0.9118 1.0158 0.0512 0.053 Uiso 0.839(5) 1 calc PR A 3 O1B O 0.8940(13) 0.8858(13) 0.2541(10) 0.040(5) Uiso 0.161(5) 1 d PD A . O2B O 0.6885(12) 0.8717(10) 0.1780(8) 0.024(3) Uiso 0.161(5) 1 d PD A . O3B O 0.825(2) 1.0787(13) 0.1465(15) 0.024(6) Uiso 0.161(5) 1 d PD A . N1 N 0.5601(2) 0.8307(2) 0.52416(17) 0.0226(5) Uani 1 1 d . . . N2 N 0.5446(3) 0.6960(2) 0.63949(17) 0.0237(5) Uani 1 1 d . . . C1 C 0.8933(3) 0.6629(3) 0.6420(2) 0.0301(7) Uani 1 1 d . . . H1 H 0.8100 0.6334 0.6645 0.036 Uiso 1 1 calc R . . C2 C 0.9065(3) 0.7217(3) 0.5552(2) 0.0304(7) Uani 1 1 d . . . H2 H 0.8321 0.7257 0.5220 0.036 Uiso 1 1 calc R . . C3 C 1.0288(4) 0.7790(3) 0.5104(3) 0.0389(9) Uani 1 1 d . . . H3A H 1.0066 0.8292 0.4541 0.047 Uiso 1 1 calc R . . H3B H 1.0901 0.7225 0.5001 0.047 Uiso 1 1 calc R . . C4 C 1.0981(4) 0.8466(3) 0.5599(3) 0.0389(9) Uani 1 1 d . . . H4A H 1.1600 0.7982 0.5984 0.047 Uiso 1 1 calc R . . H4B H 1.1488 0.9074 0.5192 0.047 Uiso 1 1 calc R . . C5 C 1.0027(3) 0.8949(3) 0.6115(2) 0.0305(7) Uani 1 1 d . . . H5 H 0.9634 0.9639 0.5839 0.037 Uiso 1 1 calc R . . C6 C 0.9685(3) 0.8454(3) 0.6964(2) 0.0316(8) Uani 1 1 d . . . H6 H 0.9120 0.8852 0.7245 0.038 Uiso 1 1 calc R . . C7 C 1.0143(4) 0.7325(3) 0.7482(3) 0.0426(9) Uani 1 1 d . . . H7A H 0.9608 0.7088 0.8023 0.051 Uiso 1 1 calc R . . H7B H 1.1060 0.7387 0.7627 0.051 Uiso 1 1 calc R . . C8 C 1.0059(4) 0.6438(3) 0.7022(2) 0.0375(9) Uani 1 1 d . . . H8A H 0.9947 0.5703 0.7451 0.045 Uiso 1 1 calc R . . H8B H 1.0889 0.6427 0.6691 0.045 Uiso 1 1 calc R . . C9 C 0.6283(3) 0.7749(2) 0.5921(2) 0.0213(6) Uani 1 1 d . . . C10 C 0.4243(3) 0.7047(3) 0.6022(2) 0.0280(7) Uani 1 1 d . . . H10 H 0.3494 0.6599 0.6241 0.034 Uiso 1 1 calc R . . C11 C 0.4344(3) 0.7887(3) 0.5292(2) 0.0253(6) Uani 1 1 d . . . H11 H 0.3686 0.8141 0.4892 0.030 Uiso 1 1 calc R . . C12 C 0.5760(3) 0.6080(3) 0.7147(2) 0.0270(7) Uani 1 1 d . . . C13 C 0.5825(3) 0.6309(3) 0.7925(2) 0.0304(7) Uani 1 1 d . . . C14 C 0.5494(4) 0.7412(3) 0.8050(2) 0.0363(8) Uani 1 1 d . . . H14 H 0.5432 0.7960 0.7473 0.044 Uiso 1 1 calc R . . C15 C 0.6539(5) 0.7829(4) 0.8521(3) 0.0517(12) Uani 1 1 d . . . H15A H 0.6554 0.7349 0.9110 0.078 Uiso 1 1 calc R . . H15B H 0.6337 0.8590 0.8522 0.078 Uiso 1 1 calc R . . H15C H 0.7395 0.7814 0.8232 0.078 Uiso 1 1 calc R . . C16 C 0.4164(5) 0.7376(5) 0.8530(4) 0.0715(16) Uani 1 1 d . . . H16A H 0.3474 0.7235 0.8180 0.107 Uiso 1 1 calc R . . H16B H 0.4005 0.8088 0.8645 0.107 Uiso 1 1 calc R . . H16C H 0.4164 0.6782 0.9071 0.107 Uiso 1 1 calc R . . C17 C 0.6179(4) 0.5439(3) 0.8622(3) 0.0406(9) Uani 1 1 d . . . H17 H 0.6226 0.5564 0.9165 0.049 Uiso 1 1 calc R . . C18 C 0.6465(5) 0.4399(3) 0.8540(3) 0.0471(11) Uani 1 1 d . . . H18 H 0.6725 0.3823 0.9021 0.057 Uiso 1 1 calc R . . C19 C 0.6375(4) 0.4198(3) 0.7764(3) 0.0440(10) Uani 1 1 d . . . H19 H 0.6562 0.3478 0.7718 0.053 Uiso 1 1 calc R . . C20 C 0.6014(4) 0.5030(3) 0.7043(2) 0.0340(8) Uani 1 1 d . . . C21 C 0.5892(4) 0.4773(3) 0.6203(2) 0.0374(9) Uani 1 1 d . . . H21 H 0.5796 0.5494 0.5749 0.045 Uiso 1 1 calc R . . C22 C 0.7088(5) 0.4181(4) 0.5945(3) 0.0599(13) Uani 1 1 d . . . H22A H 0.7878 0.4607 0.5955 0.090 Uiso 1 1 calc R . . H22B H 0.6995 0.4120 0.5368 0.090 Uiso 1 1 calc R . . H22C H 0.7155 0.3437 0.6347 0.090 Uiso 1 1 calc R . . C23 C 0.4659(5) 0.4096(4) 0.6237(3) 0.0559(13) Uani 1 1 d . . . H23A H 0.4713 0.3391 0.6689 0.084 Uiso 1 1 calc R . . H23B H 0.4572 0.3949 0.5687 0.084 Uiso 1 1 calc R . . H23C H 0.3897 0.4512 0.6357 0.084 Uiso 1 1 calc R . . C24 C 0.6121(3) 0.9224(3) 0.4532(2) 0.0245(6) Uani 1 1 d . A . H24A H 0.6902 0.9532 0.4715 0.029 Uiso 1 1 calc R . . H24B H 0.5458 0.9818 0.4389 0.029 Uiso 1 1 calc R . . C25 C 0.6487(3) 0.8884(3) 0.3743(2) 0.0284(7) Uani 1 1 d . . . H25A H 0.5698 0.8631 0.3526 0.034 Uiso 1 1 calc R A . H25B H 0.7110 0.8258 0.3886 0.034 Uiso 1 1 calc R . . C26 C 0.7113(3) 0.9865(3) 0.3049(2) 0.0293(7) Uani 1 1 d . A . H26A H 0.7862 1.0135 0.3294 0.035 Uiso 1 1 calc R . . H26B H 0.6467 1.0472 0.2908 0.035 Uiso 1 1 calc R . . C28 C 1.0749(6) 0.8343(6) 0.2439(4) 0.090(2) Uani 1 1 d . . . H28A H 1.1068 0.7879 0.2086 0.135 Uiso 1 1 calc R A 1 H28B H 1.1311 0.8245 0.2923 0.135 Uiso 1 1 calc R A 1 H28C H 1.0766 0.9123 0.2096 0.135 Uiso 1 1 calc R A 1 C29 C 0.9200(7) 0.6791(5) 0.3114(6) 0.109(3) Uani 1 1 d . . . H29A H 0.8270 0.6615 0.3235 0.164 Uiso 1 1 calc R A 1 H29B H 0.9669 0.6524 0.3643 0.164 Uiso 1 1 calc R A 1 H29C H 0.9550 0.6430 0.2696 0.164 Uiso 1 1 calc R A 1 C31 C 0.4311(4) 0.9011(4) 0.1644(3) 0.0517(11) Uani 1 1 d . . . H31A H 0.4289 0.9263 0.2157 0.078 Uiso 1 1 calc R A 2 H31B H 0.3729 0.8369 0.1740 0.078 Uiso 1 1 calc R A 2 H31C H 0.4021 0.9612 0.1160 0.078 Uiso 1 1 calc R A 2 C32 C 0.5811(4) 0.8329(4) 0.0665(3) 0.0472(10) Uani 1 1 d . . . H32A H 0.5538 0.8929 0.0174 0.071 Uiso 1 1 calc R A 2 H32B H 0.5270 0.7671 0.0728 0.071 Uiso 1 1 calc R A 2 H32C H 0.6729 0.8152 0.0575 0.071 Uiso 1 1 calc R A 2 C34 C 0.8267(6) 1.1689(5) 0.0064(3) 0.0705(16) Uani 1 1 d . . . H34A H 0.7401 1.1368 0.0062 0.106 Uiso 1 1 calc R A 3 H34B H 0.8680 1.1873 -0.0511 0.106 Uiso 1 1 calc R A 3 H3C H 0.8180 1.2363 0.0245 0.106 Uiso 1 1 calc R A 3 C35 C 1.0478(5) 1.1288(5) 0.0656(4) 0.0658(15) Uani 1 1 d . . . H35A H 1.0459 1.1991 0.0799 0.099 Uiso 1 1 calc R A 3 H35B H 1.0889 1.1404 0.0084 0.099 Uiso 1 1 calc R A 3 H35C H 1.0979 1.0741 0.1074 0.099 Uiso 1 1 calc R A 3 C51 C 0.2442(13) 0.4466(10) 0.8563(10) 0.088(5) Uiso 0.64(3) 1 d P . . C52 C 0.0447(17) 0.5000(14) 0.9789(10) 0.134(7) Uiso 0.78(3) 1 d P . . C53 C 0.064(2) 0.4567(18) 0.9395(14) 0.059(9) Uiso 0.29(3) 1 d P . . C54 C 0.2048(19) 0.4564(12) 0.9066(12) 0.093(7) Uiso 0.59(4) 1 d P . . C55 C 0.150(3) 0.4838(17) 0.9618(14) 0.102(10) Uiso 0.43(3) 1 d P . . C56 C 0.120(3) 0.423(2) 0.9126(16) 0.084(11) Uiso 0.31(3) 1 d P . . 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 0.01598(12) 0.02162(13) 0.02475(13) -0.00424(9) -0.00066(8) -0.00295(8) Si 0.0255(5) 0.0393(6) 0.0369(5) -0.0152(4) 0.0074(4) -0.0066(4) Cl1 0.0275(4) 0.0264(4) 0.0300(4) -0.0083(3) -0.0022(3) 0.0006(3) O1A 0.0375(19) 0.048(2) 0.0400(19) -0.0189(15) -0.0050(15) 0.0048(15) C27 0.033(2) 0.080(4) 0.062(3) -0.012(3) -0.005(2) -0.002(2) O2A 0.0345(17) 0.0336(17) 0.0369(17) -0.0081(13) -0.0050(13) -0.0090(13) C30 0.036(2) 0.059(3) 0.038(2) -0.0178(19) -0.0061(17) 0.0010(19) O3A 0.028(2) 0.051(2) 0.0250(18) -0.0136(14) 0.0049(17) -0.0067(19) C33 0.041(2) 0.063(3) 0.033(2) -0.0234(19) 0.0150(17) -0.021(2) N1 0.0173(13) 0.0217(13) 0.0266(13) -0.0038(10) -0.0005(10) -0.0049(10) N2 0.0179(13) 0.0220(13) 0.0279(14) -0.0016(10) -0.0018(10) -0.0039(10) C1 0.0175(15) 0.0290(17) 0.040(2) -0.0047(14) 0.0021(13) -0.0003(13) C2 0.0243(17) 0.0316(18) 0.0376(19) -0.0137(14) -0.0033(14) 0.0051(14) C3 0.034(2) 0.041(2) 0.040(2) -0.0091(16) 0.0106(16) 0.0040(16) C4 0.0230(18) 0.041(2) 0.045(2) 0.0003(16) 0.0032(15) -0.0035(15) C5 0.0165(15) 0.0320(18) 0.0398(19) -0.0046(14) -0.0053(13) -0.0058(13) C6 0.0222(17) 0.0364(19) 0.0363(19) -0.0092(15) -0.0099(14) -0.0002(14) C7 0.036(2) 0.046(2) 0.041(2) -0.0035(17) -0.0162(18) 0.0046(17) C8 0.0281(19) 0.0323(19) 0.043(2) 0.0041(15) -0.0059(16) 0.0051(15) C9 0.0197(15) 0.0178(14) 0.0248(15) -0.0036(11) 0.0000(12) -0.0031(11) C10 0.0144(15) 0.0320(17) 0.0344(18) -0.0044(13) -0.0003(13) -0.0050(13) C11 0.0165(15) 0.0285(16) 0.0291(16) -0.0054(12) -0.0019(12) -0.0034(12) C12 0.0191(15) 0.0233(15) 0.0323(17) 0.0022(12) -0.0021(13) -0.0071(12) C13 0.0272(17) 0.0268(17) 0.0330(18) -0.0015(13) -0.0021(14) -0.0071(13) C14 0.041(2) 0.0341(19) 0.0304(18) -0.0050(14) 0.0049(16) -0.0005(16) C15 0.078(3) 0.037(2) 0.044(2) -0.0171(18) -0.008(2) -0.001(2) C16 0.054(3) 0.066(3) 0.077(4) 0.001(3) 0.031(3) 0.011(3) C17 0.047(2) 0.035(2) 0.035(2) -0.0001(15) -0.0102(17) -0.0095(17) C18 0.059(3) 0.032(2) 0.043(2) 0.0046(16) -0.022(2) -0.0062(18) C19 0.060(3) 0.0212(17) 0.047(2) -0.0011(15) -0.017(2) -0.0049(17) C20 0.035(2) 0.0262(17) 0.0363(19) -0.0017(14) -0.0069(15) -0.0074(14) C21 0.047(2) 0.0243(17) 0.041(2) -0.0090(15) -0.0056(17) -0.0042(16) C22 0.068(3) 0.049(3) 0.071(3) -0.029(2) -0.011(3) 0.012(2) C23 0.069(3) 0.050(3) 0.050(3) -0.013(2) -0.016(2) -0.020(2) C24 0.0248(16) 0.0210(15) 0.0254(16) -0.0030(12) -0.0006(12) -0.0045(12) C25 0.0258(17) 0.0272(16) 0.0310(17) -0.0075(13) 0.0074(13) -0.0026(13) C26 0.0290(18) 0.0337(18) 0.0249(16) -0.0086(13) 0.0030(13) -0.0076(14) C28 0.055(4) 0.123(6) 0.073(4) 0.002(4) -0.005(3) -0.015(4) C29 0.068(4) 0.059(4) 0.185(8) -0.008(4) -0.036(5) 0.002(3) C31 0.046(3) 0.037(2) 0.063(3) -0.0041(19) 0.022(2) -0.0043(19) C32 0.044(2) 0.059(3) 0.042(2) -0.022(2) 0.0047(19) -0.013(2) C34 0.068(4) 0.104(4) 0.031(2) -0.005(2) 0.002(2) -0.025(3) C35 0.041(3) 0.096(4) 0.068(3) -0.037(3) 0.016(2) -0.021(3) _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 C9 2.043(3) . ? Rh1 C2 2.105(3) . ? Rh1 C1 2.111(3) . ? Rh1 C6 2.188(3) . ? Rh1 C5 2.203(3) . ? Rh1 Cl1 2.3913(9) . ? Si O2B 1.558(9) . ? Si O1A 1.612(3) . ? Si O3A 1.614(3) . ? Si O3B 1.617(10) . ? Si O2A 1.664(3) . ? Si O1B 1.669(10) . ? Si C26 1.853(3) . ? O1A C27 1.405(6) . ? O1A O2B 1.720(13) . ? C27 C29 1.483(8) . ? C27 C28 1.507(7) . ? C27 H27 1.0000 . ? O2A C30 1.398(5) . ? C30 C31 1.470(6) . ? C30 C32 1.501(5) . ? C30 H30 1.0000 . ? O3A C33 1.430(6) . ? C33 C34 1.498(7) . ? C33 C35 1.517(6) . ? C33 H33 1.0000 . ? N1 C9 1.354(4) . ? N1 C11 1.388(4) . ? N1 C24 1.464(4) . ? N2 C9 1.354(4) . ? N2 C10 1.391(4) . ? N2 C12 1.444(4) . ? C1 C2 1.400(5) . ? C1 C8 1.526(5) . ? C1 H1 0.9500 . ? C2 C3 1.503(5) . ? C2 H2 0.9500 . ? C3 C4 1.535(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.500(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.380(5) . ? C5 H5 0.9500 . ? C6 C7 1.512(5) . ? C6 H6 0.9500 . ? C7 C8 1.524(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C10 C11 1.348(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.392(5) . ? C12 C20 1.403(5) . ? C13 C17 1.393(5) . ? C13 C14 1.497(5) . ? C14 C15 1.531(6) . ? C14 C16 1.536(6) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.383(6) . ? C17 H17 0.9500 . ? C18 C19 1.375(6) . ? C18 H18 0.9500 . ? C19 C20 1.395(5) . ? C19 H19 0.9500 . ? C20 C21 1.514(5) . ? C21 C23 1.522(6) . ? C21 C22 1.535(6) . ? C21 H21 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.506(4) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.537(5) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H3C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C51 C54 0.940(18) . ? C51 C56 1.52(4) . ? C52 C53 0.97(2) . ? C52 C55 1.14(2) . ? C53 C56 0.89(3) . ? C53 C55 1.07(3) . ? C53 C54 1.52(4) . ? C54 C56 0.96(3) . ? C54 C55 1.18(3) . ? C55 C56 1.32(4) . ? 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 C9 Rh1 C2 92.51(13) . . ? C9 Rh1 C1 95.77(12) . . ? C2 Rh1 C1 38.78(14) . . ? C9 Rh1 C6 160.34(13) . . ? C2 Rh1 C6 97.69(14) . . ? C1 Rh1 C6 82.09(13) . . ? C9 Rh1 C5 162.89(13) . . ? C2 Rh1 C5 81.35(14) . . ? C1 Rh1 C5 89.43(13) . . ? C6 Rh1 C5 36.64(13) . . ? C9 Rh1 Cl1 87.79(9) . . ? C2 Rh1 Cl1 157.08(10) . . ? C1 Rh1 Cl1 163.83(10) . . ? C6 Rh1 Cl1 89.26(10) . . ? C5 Rh1 Cl1 91.74(10) . . ? O2B Si O1A 65.7(5) . . ? O2B Si O3A 135.0(5) . . ? O1A Si O3A 113.4(2) . . ? O2B Si O3B 129.6(10) . . ? O1A Si O3B 125.7(9) . . ? O1A Si O2A 104.12(16) . . ? O3A Si O2A 105.0(2) . . ? O3B Si O2A 93.8(8) . . ? O2B Si O1B 103.3(8) . . ? O3A Si O1B 94.3(6) . . ? O3B Si O1B 108.4(10) . . ? O2A Si O1B 143.2(6) . . ? O2B Si C26 114.7(5) . . ? O1A Si C26 114.73(17) . . ? O3A Si C26 106.1(2) . . ? O3B Si C26 103.5(10) . . ? O2A Si C26 113.27(17) . . ? O1B Si C26 90.2(6) . . ? C27 O1A Si 123.6(3) . . ? C27 O1A O2B 157.6(6) . . ? Si O1A O2B 55.7(4) . . ? O1A C27 C29 108.6(4) . . ? O1A C27 C28 114.3(4) . . ? C29 C27 C28 112.9(5) . . ? O1A C27 H27 106.9 . . ? C29 C27 H27 106.9 . . ? C28 C27 H27 106.9 . . ? C30 O2A Si 126.4(3) . . ? O2A C30 C31 109.8(4) . . ? O2A C30 C32 109.1(4) . . ? C31 C30 C32 114.2(4) . . ? O2A C30 H30 107.8 . . ? C31 C30 H30 107.8 . . ? C32 C30 H30 107.8 . . ? C33 O3A Si 125.2(3) . . ? O3A C33 C34 111.7(4) . . ? O3A C33 C35 106.1(4) . . ? C34 C33 C35 111.8(4) . . ? O3A C33 H33 109.1 . . ? C34 C33 H33 109.1 . . ? C35 C33 H33 109.1 . . ? Si O2B O1A 58.7(4) . . ? C9 N1 C11 111.4(3) . . ? C9 N1 C24 124.7(2) . . ? C11 N1 C24 123.9(3) . . ? C9 N2 C10 110.8(3) . . ? C9 N2 C12 125.8(3) . . ? C10 N2 C12 123.2(3) . . ? C2 C1 C8 123.5(3) . . ? C2 C1 Rh1 70.3(2) . . ? C8 C1 Rh1 113.4(2) . . ? C2 C1 H1 118.3 . . ? C8 C1 H1 118.3 . . ? Rh1 C1 H1 86.4 . . ? C1 C2 C3 125.2(3) . . ? C1 C2 Rh1 70.9(2) . . ? C3 C2 Rh1 110.5(2) . . ? C1 C2 H2 117.4 . . ? C3 C2 H2 117.4 . . ? Rh1 C2 H2 88.6 . . ? C2 C3 C4 114.0(3) . . ? C2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? C2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C3 111.7(3) . . ? C5 C4 H4A 109.3 . . ? C3 C4 H4A 109.3 . . ? C5 C4 H4B 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 124.0(3) . . ? C6 C5 Rh1 71.10(19) . . ? C4 C5 Rh1 112.0(2) . . ? C6 C5 H5 118.0 . . ? C4 C5 H5 118.0 . . ? Rh1 C5 H5 86.9 . . ? C5 C6 C7 124.9(4) . . ? C5 C6 Rh1 72.26(18) . . ? C7 C6 Rh1 107.9(2) . . ? C5 C6 H6 117.6 . . ? C7 C6 H6 117.6 . . ? Rh1 C6 H6 89.8 . . ? C6 C7 C8 113.6(3) . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C1 112.7(3) . . ? C7 C8 H8A 109.0 . . ? C1 C8 H8A 109.0 . . ? C7 C8 H8B 109.0 . . ? C1 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N1 C9 N2 104.6(2) . . ? N1 C9 Rh1 125.3(2) . . ? N2 C9 Rh1 129.5(2) . . ? C11 C10 N2 107.0(3) . . ? C11 C10 H10 126.5 . . ? N2 C10 H10 126.5 . . ? C10 C11 N1 106.3(3) . . ? C10 C11 H11 126.9 . . ? N1 C11 H11 126.9 . . ? C13 C12 C20 123.3(3) . . ? C13 C12 N2 119.4(3) . . ? C20 C12 N2 117.2(3) . . ? C12 C13 C17 117.0(3) . . ? C12 C13 C14 123.6(3) . . ? C17 C13 C14 119.3(3) . . ? C13 C14 C15 112.6(3) . . ? C13 C14 C16 111.2(4) . . ? C15 C14 C16 109.5(4) . . ? C13 C14 H14 107.8 . . ? C15 C14 H14 107.8 . . ? C16 C14 H14 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C13 121.3(4) . . ? C18 C17 H17 119.3 . . ? C13 C17 H17 119.3 . . ? C19 C18 C17 120.1(4) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 121.4(4) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C12 116.8(3) . . ? C19 C20 C21 120.1(3) . . ? C12 C20 C21 123.1(3) . . ? C20 C21 C23 109.8(4) . . ? C20 C21 C22 113.5(3) . . ? C23 C21 C22 110.5(4) . . ? C20 C21 H21 107.6 . . ? C23 C21 H21 107.6 . . ? C22 C21 H21 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 C25 113.2(3) . . ? N1 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? N1 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.8 . . ? C24 C25 C26 110.2(3) . . ? C24 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? C24 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.1 . . ? C25 C26 Si 116.8(2) . . ? C25 C26 H26A 108.1 . . ? Si C26 H26A 108.1 . . ? C25 C26 H26B 108.1 . . ? Si C26 H26B 108.1 . . ? H26A C26 H26B 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C53 C52 C55 60.2(17) . . ? C55 C52 C56 46.7(16) . . ? C56 C53 C52 151(4) . . ? C56 C53 C55 84(3) . . ? C52 C53 C55 67.5(18) . . ? C52 C53 C54 117(2) . . ? C55 C53 C54 50.6(18) . . ? C51 C54 C56 106(3) . . ? C51 C54 C55 170(2) . . ? C56 C54 C55 75(3) . . ? C51 C54 C53 133(2) . . ? C53 C55 C52 52.3(18) . . ? C53 C55 C54 85(2) . . ? C52 C55 C54 136(2) . . ? C52 C55 C56 94(2) . . ? C53 C56 C54 110(4) . . ? C53 C56 C55 54(2) . . ? C54 C56 C55 60(2) . . ? C53 C56 C51 140(3) . . ? C55 C56 C51 96(2) . . ? C54 C56 C52 97(3) . . ? C51 C56 C52 130(2) . . ? _diffrn_measured_fraction_theta_max 0.875 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.706 _refine_diff_density_min -1.230 _refine_diff_density_rms 0.115 _database_code_depnum_ccdc_archive 'CCDC 945443'