Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_00srv144 _database_code_CSD 171634 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name _publ_author_address 'Rourke, Jonathan P.' ; Department of Chemistry, University of Warwick, Coventry CV4 7AL UK ; 'Batsanov, AS.' ; Chemistry Department, University of Durham, South Rd., Durham DH1 3LE UK ; 'Howard, Judith A.K.' ; Chemistry Department, University of Durham, South Rd., Durham DH1 3LE UK ; 'Marder, Todd B.' ; Chemistry Department, University of Durham, South Rd., Durham DH1 3LE UK ; _audit_creation_method SHELXL-97 _publ_contact_author_name 'Dr. Jonathan Rourke' _publ_contact_author_address ; Department of Chemistry, University of Warwick, Coventry, CV4 7AL UK ; _publ_contact_author_email 'j.rourke@warwick.ac.uk' _publ_contact_letter ; The CIF file contains data for the structure (5) from the paper "Regiospecific High Yield Reductive Coupling of Diynes to Give Luminescent Rhodium Complexes by J P Rourke, A S Batsanov, J A K Howard and T B Marder The paper will be submitted to Chem Comm. ; _publ_section_title ; Regiospecific High Yield Reductive Coupling of Diynes to Give a Luminescent Rhodium Complex ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H64 P3 Rh Si' _chemical_formula_weight 888.92 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' '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 Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 10.500(2) _cell_length_b 19.180(1) _cell_length_c 47.927(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9652(2) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 732 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3744 _exptl_absorpt_coefficient_mu 0.509 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8912 _exptl_absorpt_correction_T_max 0.9672 _exptl_absorpt_process_details ? loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0.00 -1.00 0.00 0.0350 0.00 1.00 0.00 0.0350 1.00 2.00 0.00 0.0450 -1.00 -2.00 0.00 0.0450 1.00 -2.00 0.00 0.0400 -1.00 2.00 0.00 0.0400 0.00 0.00 1.00 0.2300 0.00 0.00 -1.00 0.2300 _exptl_special_details ; The data collection nominally covered over a hemisphere of reciprocal space, by a combination of 4 sets of \w scans; each set at different \f and/or 2\q angles and each scan (20 sec exposure) covering 0.3\% in \w. Crystal decay was monitored by repeating 50 initial frames at the end of data collection and comparing 269 duplicate reflections. Crystal to detector distance 6.0 cm. ; _diffrn_ambient_temperature 120(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 'SMART 1K CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8 _diffrn_standards_number 'not measured' _diffrn_standards_interval_count 'not measured' _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 41968 _diffrn_reflns_av_R_equivalents 0.0945 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 56 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 25.30 _reflns_number_total 7981 _reflns_number_gt 5801 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0254P)^2^+3.9000P] 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 7981 _refine_ls_number_parameters 522 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.1007 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.1123 _refine_ls_wR_factor_gt 0.1058 _refine_ls_goodness_of_fit_ref 1.467 _refine_ls_restrained_S_all 1.514 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.25756(4) 0.489554(18) 0.130046(8) 0.01840(12) Uani 1 1 d . A . Si Si 0.54876(16) 0.40480(9) 0.20687(4) 0.0437(5) Uani 1 1 d D . . P1 P 0.12417(14) 0.54918(7) 0.16043(3) 0.0276(4) Uani 1 1 d D . . P2 P 0.37978(13) 0.41025(7) 0.10497(3) 0.0213(3) Uani 1 1 d . . . P3 P 0.40372(12) 0.58201(7) 0.12261(3) 0.0211(3) Uani 1 1 d . . . C1 C 0.3602(5) 0.4558(2) 0.16430(12) 0.0225(13) Uani 1 1 d . . . C2 C 0.4249(5) 0.4352(3) 0.18230(12) 0.0333(14) Uani 1 1 d D A . C3A C 0.7030(7) 0.4501(5) 0.1991(2) 0.049(4) Uiso 0.50 1 d PD A 1 H31A H 0.7685 0.4338 0.2121 0.073 Uiso 0.50 1 d PR A 1 H32A H 0.6910 0.5004 0.2014 0.073 Uiso 0.50 1 d PR A 1 H33A H 0.7299 0.4401 0.1799 0.073 Uiso 0.50 1 d PR A 1 C4A C 0.5065(10) 0.4144(6) 0.24357(12) 0.048(4) Uiso 0.50 1 d PD A 1 H41A H 0.5760 0.3974 0.2554 0.072 Uiso 0.50 1 d PR A 1 H42A H 0.4294 0.3872 0.2473 0.072 Uiso 0.50 1 d PR A 1 H43A H 0.4903 0.4637 0.2477 0.072 Uiso 0.50 1 d PR A 1 C5A C 0.5791(10) 0.3085(4) 0.1992(2) 0.040(4) Uiso 0.50 1 d PD A 1 H51A H 0.6447 0.2909 0.2119 0.060 Uiso 0.50 1 d PR A 1 H52A H 0.6081 0.3032 0.1799 0.060 Uiso 0.50 1 d PR A 1 H53A H 0.5002 0.2819 0.2019 0.060 Uiso 0.50 1 d PR A 1 C3B C 0.6758(9) 0.4741(5) 0.2097(2) 0.074(5) Uiso 0.50 1 d PD A 2 H31B H 0.7422 0.4585 0.2226 0.111 Uiso 0.50 1 d PR A 2 H32B H 0.6378 0.5175 0.2166 0.111 Uiso 0.50 1 d PR A 2 H33B H 0.7134 0.4824 0.1912 0.111 Uiso 0.50 1 d PR A 2 C4B C 0.4801(10) 0.3944(6) 0.24287(14) 0.054(5) Uiso 0.50 1 d PD A 2 H41B H 0.5465 0.3782 0.2557 0.081 Uiso 0.50 1 d PR A 2 H42B H 0.4111 0.3600 0.2422 0.081 Uiso 0.50 1 d PR A 2 H43B H 0.4464 0.4391 0.2494 0.081 Uiso 0.50 1 d PR A 2 C5B C 0.6226(10) 0.3223(4) 0.1960(2) 0.064(5) Uiso 0.50 1 d PD A 2 H51B H 0.6874 0.3084 0.2096 0.096 Uiso 0.50 1 d PR A 2 H52B H 0.6623 0.3285 0.1777 0.096 Uiso 0.50 1 d PR A 2 H53B H 0.5570 0.2860 0.1948 0.096 Uiso 0.50 1 d PR A 2 C6A C 0.0082(9) 0.4978(4) 0.1788(2) 0.073(3) Uani 0.75 1 d PD B 1 H61A H 0.0500 0.4568 0.1869 0.110 Uiso 0.75 1 d PR B 1 H62A H -0.0586 0.4826 0.1659 0.110 Uiso 0.75 1 d PR B 1 H63A H -0.0297 0.5259 0.1937 0.110 Uiso 0.75 1 d PR B 1 C7A C 0.0330(8) 0.6201(5) 0.14711(18) 0.068(3) Uani 0.75 1 d PD B 1 H71A H 0.0884 0.6517 0.1365 0.102 Uiso 0.75 1 d PR B 1 H72A H -0.0060 0.6456 0.1626 0.102 Uiso 0.75 1 d PR B 1 H73A H -0.0339 0.6020 0.1348 0.102 Uiso 0.75 1 d PR B 1 C8A C 0.2055(7) 0.5885(4) 0.19057(15) 0.043(2) Uani 0.75 1 d PD B 1 H81A H 0.2595 0.5533 0.1995 0.065 Uiso 0.75 1 d PR B 1 H82A H 0.1425 0.6056 0.2040 0.065 Uiso 0.75 1 d PR B 1 H83A H 0.2585 0.6274 0.1842 0.065 Uiso 0.75 1 d PR B 1 C6B C 0.127(2) 0.6417(7) 0.1670(5) 0.073(3) Uani 0.25 1 d PD B 2 H61B H 0.1291 0.6672 0.1493 0.110 Uiso 0.25 1 d PR B 2 H62B H 0.2039 0.6527 0.1779 0.110 Uiso 0.25 1 d PR B 2 H63B H 0.0515 0.6552 0.1777 0.110 Uiso 0.25 1 d PR B 2 C7B C 0.121(2) 0.5123(12) 0.1948(3) 0.068(3) Uani 0.25 1 d PD B 2 H71B H 0.1179 0.4614 0.1934 0.102 Uiso 0.25 1 d PR B 2 H72B H 0.0454 0.5290 0.2047 0.102 Uiso 0.25 1 d PR B 2 H73B H 0.1978 0.5263 0.2050 0.102 Uiso 0.25 1 d PR B 2 C8B C -0.0457(14) 0.5395(11) 0.1505(4) 0.043(2) Uani 0.25 1 d PD B 2 H81B H -0.0634 0.4906 0.1460 0.065 Uiso 0.25 1 d PR B 2 H82B H -0.0631 0.5687 0.1342 0.065 Uiso 0.25 1 d PR B 2 H83B H -0.1003 0.5542 0.1661 0.065 Uiso 0.25 1 d PR B 2 C9 C 0.3447(5) 0.3182(2) 0.11082(12) 0.0310(14) Uani 1 1 d . B . H91 H 0.2565 0.3083 0.1054 0.030(8) Uiso 1 1 d R . . H92 H 0.3561 0.3073 0.1306 0.030(8) Uiso 1 1 d R . . H93 H 0.4027 0.2895 0.0997 0.030(8) Uiso 1 1 d R . . C10 C 0.3691(5) 0.4153(3) 0.06736(11) 0.0320(14) Uani 1 1 d . B . H101 H 0.3937 0.4621 0.0612 0.041(9) Uiso 1 1 d R . . H102 H 0.2814 0.4057 0.0615 0.041(9) Uiso 1 1 d R . . H103 H 0.4265 0.3808 0.0590 0.041(9) Uiso 1 1 d R . . C11 C 0.5502(5) 0.4087(3) 0.11231(10) 0.0247(13) Uani 1 1 d . B . H111 H 0.5914 0.3746 0.1000 0.034(9) Uiso 1 1 d R . . H112 H 0.5643 0.3954 0.1318 0.034(9) Uiso 1 1 d R . . H113 H 0.5866 0.4550 0.1090 0.034(9) Uiso 1 1 d R . . C12 C 0.5422(5) 0.5854(3) 0.14616(12) 0.0331(14) Uani 1 1 d . B . H121 H 0.5958 0.6251 0.1409 0.069(12) Uiso 1 1 d R . . H122 H 0.5917 0.5422 0.1446 0.069(12) Uiso 1 1 d R . . H123 H 0.5131 0.5912 0.1655 0.069(12) Uiso 1 1 d R . . C13 C 0.4797(5) 0.5865(3) 0.08848(11) 0.0293(13) Uani 1 1 d . B . H131 H 0.4140 0.5859 0.0739 0.049(10) Uiso 1 1 d R . . H132 H 0.5366 0.5464 0.0860 0.049(10) Uiso 1 1 d R . . H133 H 0.5290 0.6297 0.0871 0.049(10) Uiso 1 1 d R . . C14 C 0.3490(5) 0.6718(2) 0.12469(12) 0.0309(14) Uani 1 1 d . B . H141 H 0.4178 0.7035 0.1191 0.024(8) Uiso 1 1 d R . . H142 H 0.3234 0.6821 0.1439 0.024(8) Uiso 1 1 d R . . H143 H 0.2759 0.6783 0.1122 0.024(8) Uiso 1 1 d R . . C15 C 0.1226(4) 0.4098(2) 0.13222(10) 0.0187(11) Uani 1 1 d . . . C16 C 0.0364(4) 0.4072(2) 0.11027(10) 0.0165(11) Uani 1 1 d . A . C17 C 0.0469(4) 0.4648(2) 0.09032(10) 0.0182(12) Uani 1 1 d . . . C18 C 0.1418(4) 0.5131(2) 0.09531(10) 0.0193(11) Uani 1 1 d . A . C19 C 0.1236(4) 0.3594(3) 0.15372(11) 0.0221(12) Uani 1 1 d . A . C20 C 0.1250(5) 0.3191(3) 0.17316(12) 0.0256(13) Uani 1 1 d . . . C21 C 0.1303(5) 0.2729(3) 0.19643(11) 0.0279(13) Uani 1 1 d . A . C22 C 0.0344(6) 0.2228(3) 0.20074(12) 0.0381(15) Uani 1 1 d . . . H22 H -0.0351 0.2194 0.1881 0.046 Uiso 1 1 d R A . C23 C 0.0430(7) 0.1782(3) 0.22357(14) 0.0503(18) Uani 1 1 d . A . H23 H -0.0219 0.1444 0.2263 0.060 Uiso 1 1 d R . . C24 C 0.1424(7) 0.1816(3) 0.24228(13) 0.0510(18) Uani 1 1 d . . . C25 C 0.2377(7) 0.2314(3) 0.23776(12) 0.0465(16) Uani 1 1 d . A . H25 H 0.3076 0.2343 0.2503 0.056 Uiso 1 1 d R . . C26 C 0.2304(5) 0.2757(3) 0.21510(11) 0.0335(14) Uani 1 1 d . . . H26 H 0.2959 0.3092 0.2123 0.040 Uiso 1 1 d R A . C27 C 0.1534(9) 0.1313(4) 0.26684(16) 0.091(3) Uani 1 1 d . A . H271 H 0.0697 0.1107 0.2708 0.109(17) Uiso 1 1 d R . . H272 H 0.1830 0.1569 0.2833 0.109(17) Uiso 1 1 d R . . H273 H 0.2142 0.0940 0.2625 0.109(17) Uiso 1 1 d R . . C28 C -0.0541(5) 0.3485(2) 0.10634(11) 0.0198(12) Uani 1 1 d . . . C29 C -0.1346(5) 0.3246(2) 0.12746(11) 0.0239(12) Uani 1 1 d . A . H29 H -0.1329 0.3463 0.1453 0.029 Uiso 1 1 d R . . C30 C -0.2176(4) 0.2695(3) 0.12262(11) 0.0268(14) Uani 1 1 d . . . H30 H -0.2705 0.2540 0.1375 0.032 Uiso 1 1 d R A . C31 C -0.2258(4) 0.2367(3) 0.09710(12) 0.0256(13) Uani 1 1 d . A . C32 C -0.1462(5) 0.2597(3) 0.07599(11) 0.0278(13) Uani 1 1 d . . . H32 H -0.1494 0.2383 0.0581 0.033 Uiso 1 1 d R A . C33 C -0.0616(5) 0.3146(2) 0.08068(11) 0.0219(12) Uani 1 1 d . A . H33 H -0.0068 0.3291 0.0660 0.026 Uiso 1 1 d R . . C34 C -0.3195(6) 0.1769(3) 0.09211(14) 0.0462(18) Uani 1 1 d . . . H341 H -0.3071 0.1577 0.0734 0.097(15) Uiso 1 1 d R A . H342 H -0.4068 0.1944 0.0939 0.097(15) Uiso 1 1 d R . . H343 H -0.3048 0.1403 0.1060 0.097(15) Uiso 1 1 d R . . C35 C -0.0462(4) 0.4676(2) 0.06674(11) 0.0179(12) Uani 1 1 d . A . C36 C -0.1760(5) 0.4742(2) 0.07178(11) 0.0239(13) Uani 1 1 d . . . H36 H -0.2046 0.4842 0.0901 0.029 Uiso 1 1 d R A . C37 C -0.2653(5) 0.4666(2) 0.05040(10) 0.0255(12) Uani 1 1 d . A . H37 H -0.3533 0.4722 0.0545 0.031 Uiso 1 1 d R . . C38 C -0.2272(5) 0.4513(2) 0.02335(11) 0.0219(12) Uani 1 1 d . . . C39 C -0.0981(5) 0.4477(2) 0.01810(11) 0.0243(13) Uani 1 1 d . A . H39 H -0.0692 0.4394 -0.0004 0.029 Uiso 1 1 d R . . C40 C -0.0095(5) 0.4563(2) 0.03937(11) 0.0243(13) Uani 1 1 d . . . H40 H 0.0787 0.4548 0.0350 0.029 Uiso 1 1 d R A . C41 C -0.3247(5) 0.4384(3) 0.00065(12) 0.0315(14) Uani 1 1 d . A . H411 H -0.2931 0.4573 -0.0170 0.061(11) Uiso 1 1 d R . . H412 H -0.4048 0.4616 0.0056 0.061(11) Uiso 1 1 d R . . H413 H -0.3394 0.3882 -0.0013 0.061(11) Uiso 1 1 d R . . C42 C 0.1507(4) 0.5727(3) 0.07799(11) 0.0197(12) Uani 1 1 d . . . C43 C 0.1597(5) 0.6252(3) 0.06384(11) 0.0226(12) Uani 1 1 d . A . C44 C 0.1683(4) 0.6858(2) 0.04647(10) 0.0199(12) Uani 1 1 d . . . C45 C 0.0658(5) 0.7071(3) 0.02996(11) 0.0271(13) Uani 1 1 d . A . H45 H -0.0119 0.6818 0.0306 0.032 Uiso 1 1 d R . . C46 C 0.0760(5) 0.7646(3) 0.01229(11) 0.0293(13) Uani 1 1 d . . . H46 H 0.0045 0.7778 0.0013 0.035 Uiso 1 1 d R A . C47 C 0.1878(5) 0.8031(2) 0.01044(11) 0.0218(12) Uani 1 1 d . A . C48 C 0.2893(4) 0.7822(2) 0.02722(10) 0.0202(12) Uani 1 1 d . . . H48 H 0.3668 0.8078 0.0264 0.024 Uiso 1 1 d R A . C49 C 0.2808(4) 0.7252(2) 0.04486(10) 0.0214(12) Uani 1 1 d . A . H49 H 0.3520 0.7126 0.0560 0.026 Uiso 1 1 d R . . C50 C 0.1968(5) 0.8668(3) -0.00779(12) 0.0352(15) Uani 1 1 d . . . H501 H 0.1160 0.8742 -0.0176 0.090(14) Uiso 1 1 d R A . H502 H 0.2653 0.8603 -0.0214 0.090(14) Uiso 1 1 d R . . H503 H 0.2157 0.9076 0.0038 0.090(14) Uiso 1 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.0189(2) 0.01479(19) 0.0215(2) -0.00031(18) 0.0003(2) 0.00038(18) Si 0.0383(11) 0.0489(11) 0.0440(12) 0.0105(9) -0.0072(8) 0.0013(9) P1 0.0304(9) 0.0241(8) 0.0283(9) -0.0048(7) 0.0059(7) 0.0014(7) P2 0.0222(8) 0.0167(7) 0.0251(8) -0.0018(6) 0.0014(6) 0.0010(6) P3 0.0231(7) 0.0149(7) 0.0253(8) -0.0006(6) -0.0011(6) -0.0017(6) C1 0.016(3) 0.010(3) 0.041(4) -0.001(3) 0.005(3) -0.002(2) C2 0.032(4) 0.022(3) 0.045(4) -0.002(3) 0.005(3) -0.006(3) C6A 0.077(7) 0.048(6) 0.095(8) -0.041(6) 0.063(6) -0.020(5) C7A 0.068(7) 0.090(8) 0.047(6) -0.007(5) -0.004(5) 0.060(6) C8A 0.046(5) 0.045(5) 0.038(5) -0.016(4) 0.002(4) 0.006(4) C6B 0.077(7) 0.048(6) 0.095(8) -0.041(6) 0.063(6) -0.020(5) C7B 0.068(7) 0.090(8) 0.047(6) -0.007(5) -0.004(5) 0.060(6) C8B 0.046(5) 0.045(5) 0.038(5) -0.016(4) 0.002(4) 0.006(4) C9 0.036(3) 0.020(3) 0.037(4) -0.003(3) 0.008(3) 0.004(3) C10 0.028(3) 0.034(3) 0.034(4) -0.010(3) 0.002(3) 0.003(3) C11 0.023(3) 0.026(3) 0.026(3) -0.001(3) -0.002(2) 0.009(2) C12 0.032(3) 0.025(3) 0.042(4) 0.000(3) -0.011(3) -0.006(3) C13 0.028(3) 0.025(3) 0.035(4) 0.007(3) 0.001(3) -0.005(2) C14 0.037(3) 0.019(3) 0.037(4) -0.004(3) -0.003(3) 0.000(2) C15 0.024(3) 0.015(3) 0.017(3) 0.002(2) 0.001(2) 0.002(2) C16 0.013(3) 0.019(3) 0.018(3) -0.009(2) 0.003(2) 0.001(2) C17 0.016(3) 0.015(3) 0.023(3) 0.003(2) 0.006(2) 0.002(2) C18 0.024(3) 0.011(3) 0.023(3) -0.003(2) 0.009(2) 0.002(2) C19 0.016(3) 0.024(3) 0.026(3) -0.003(3) 0.003(2) -0.002(2) C20 0.025(3) 0.020(3) 0.032(4) 0.000(3) 0.003(3) -0.001(2) C21 0.039(4) 0.020(3) 0.024(3) 0.002(3) 0.006(3) 0.000(3) C22 0.044(4) 0.034(4) 0.036(4) 0.005(3) 0.004(3) -0.006(3) C23 0.068(5) 0.036(4) 0.047(5) 0.014(3) 0.013(4) -0.017(3) C24 0.084(5) 0.040(4) 0.029(4) 0.014(3) 0.013(4) -0.004(4) C25 0.069(5) 0.042(4) 0.029(3) 0.009(3) -0.002(4) 0.004(4) C26 0.042(4) 0.026(3) 0.032(3) 0.002(3) 0.000(3) -0.003(3) C27 0.132(8) 0.077(6) 0.064(6) 0.050(5) 0.002(5) -0.014(6) C28 0.021(3) 0.018(3) 0.021(3) 0.007(2) 0.002(2) 0.004(2) C29 0.024(3) 0.021(3) 0.026(3) 0.004(3) 0.003(3) -0.001(2) C30 0.021(3) 0.023(3) 0.037(4) 0.011(3) 0.004(2) 0.001(2) C31 0.016(3) 0.021(3) 0.040(3) 0.002(3) -0.010(2) 0.001(2) C32 0.035(3) 0.020(3) 0.028(3) -0.001(3) -0.004(3) 0.002(3) C33 0.027(3) 0.021(3) 0.019(3) 0.006(2) -0.001(2) 0.001(2) C34 0.044(4) 0.035(4) 0.061(5) 0.001(3) -0.006(3) -0.017(3) C35 0.017(3) 0.009(3) 0.028(3) 0.002(2) 0.000(2) -0.004(2) C36 0.027(3) 0.020(3) 0.025(3) -0.008(2) 0.005(2) 0.004(2) C37 0.021(3) 0.025(3) 0.030(3) 0.002(2) 0.001(3) -0.001(2) C38 0.021(3) 0.018(3) 0.027(3) 0.003(2) -0.006(2) -0.001(2) C39 0.031(3) 0.020(3) 0.021(3) 0.001(2) 0.000(3) -0.001(2) C40 0.019(3) 0.021(3) 0.033(4) 0.007(3) 0.000(3) -0.001(2) C41 0.029(3) 0.029(3) 0.036(4) -0.004(3) -0.005(3) 0.000(3) C42 0.010(3) 0.018(3) 0.031(3) -0.005(3) -0.003(2) -0.001(2) C43 0.025(3) 0.021(3) 0.022(3) -0.002(3) 0.004(2) -0.001(2) C44 0.021(3) 0.018(3) 0.021(3) 0.000(2) 0.001(2) 0.002(2) C45 0.023(3) 0.026(3) 0.033(4) 0.002(3) -0.004(3) -0.003(2) C46 0.033(3) 0.025(3) 0.030(3) 0.004(3) -0.008(3) 0.002(3) C47 0.031(3) 0.012(3) 0.023(3) -0.002(2) 0.000(2) 0.003(2) C48 0.017(3) 0.019(3) 0.024(3) 0.004(2) 0.006(2) -0.003(2) C49 0.018(3) 0.023(3) 0.024(3) -0.001(2) 0.002(2) 0.004(2) C50 0.046(4) 0.029(3) 0.031(4) 0.010(3) -0.007(3) -0.001(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 Rh C1 2.068(6) . ? Rh C15 2.087(5) . ? Rh C18 2.110(5) . ? Rh P1 2.3215(15) . ? Rh P2 2.3248(14) . ? Rh P3 2.3721(14) . ? Si C4A 1.823(6) . ? Si C5B 1.838(6) . ? Si C2 1.848(7) . ? Si C3A 1.875(6) . ? Si C4B 1.881(6) . ? Si C3B 1.888(7) . ? Si C5A 1.911(6) . ? P1 C7A 1.782(7) . ? P1 C7B 1.792(13) . ? P1 C6A 1.798(7) . ? P1 C6B 1.802(12) . ? P1 C8A 1.840(7) . ? P1 C8B 1.855(13) . ? P2 C10 1.808(5) . ? P2 C11 1.824(5) . ? P2 C9 1.826(5) . ? P3 C14 1.819(5) . ? P3 C13 1.822(5) . ? P3 C12 1.842(5) . ? C1 C2 1.167(7) . ? C15 C16 1.389(6) . ? C15 C19 1.413(7) . ? C16 C17 1.465(6) . ? C16 C28 1.485(7) . ? C17 C18 1.382(6) . ? C17 C35 1.495(7) . ? C18 C42 1.416(7) . ? C19 C20 1.211(7) . ? C20 C21 1.426(7) . ? C21 C26 1.382(7) . ? C21 C22 1.407(7) . ? C22 C23 1.391(8) . ? C23 C24 1.378(9) . ? C24 C25 1.401(8) . ? C24 C27 1.527(9) . ? C25 C26 1.381(7) . ? C28 C33 1.393(7) . ? C28 C29 1.397(7) . ? C29 C30 1.389(7) . ? C30 C31 1.378(7) . ? C31 C32 1.384(7) . ? C31 C34 1.530(7) . ? C32 C33 1.397(7) . ? C35 C40 1.384(7) . ? C35 C36 1.390(7) . ? C36 C37 1.397(7) . ? C37 C38 1.388(7) . ? C38 C39 1.381(7) . ? C38 C41 1.514(7) . ? C39 C40 1.390(7) . ? C42 C43 1.217(7) . ? C43 C44 1.432(7) . ? C44 C45 1.397(7) . ? C44 C49 1.404(6) . ? C45 C46 1.395(7) . ? C46 C47 1.390(7) . ? C47 C48 1.394(7) . ? C47 C50 1.506(7) . ? C48 C49 1.386(6) . ? 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 C1 Rh C15 94.85(19) . . ? C1 Rh C18 173.51(18) . . ? C15 Rh C18 78.78(18) . . ? C1 Rh P1 88.34(14) . . ? C15 Rh P1 85.43(13) . . ? C18 Rh P1 92.39(13) . . ? C1 Rh P2 85.28(14) . . ? C15 Rh P2 85.47(13) . . ? C18 Rh P2 92.89(13) . . ? P1 Rh P2 168.39(5) . . ? C1 Rh P3 90.93(14) . . ? C15 Rh P3 173.91(14) . . ? C18 Rh P3 95.40(13) . . ? P1 Rh P3 96.67(5) . . ? P2 Rh P3 93.11(5) . . ? C4A Si C5B 117.6(6) . . ? C4A Si C2 114.3(3) . . ? C5B Si C2 112.8(4) . . ? C4A Si C3A 110.8(4) . . ? C5B Si C3A 88.7(5) . . ? C2 Si C3A 109.6(3) . . ? C4A Si C4B 14.6(6) . . ? C5B Si C4B 109.3(4) . . ? C2 Si C4B 110.4(3) . . ? C3A Si C4B 124.3(5) . . ? C4A Si C3B 91.9(5) . . ? C5B Si C3B 109.2(4) . . ? C2 Si C3B 108.7(3) . . ? C3A Si C3B 22.8(5) . . ? C4B Si C3B 106.3(4) . . ? C4A Si C5A 108.9(4) . . ? C5B Si C5A 16.7(5) . . ? C2 Si C5A 107.4(3) . . ? C3A Si C5A 105.4(4) . . ? C4B Si C5A 97.9(5) . . ? C3B Si C5A 125.2(5) . . ? C7A P1 C7B 128.3(8) . . ? C7A P1 C6A 103.3(4) . . ? C7B P1 C6A 47.2(8) . . ? C7A P1 C6B 47.2(8) . . ? C7B P1 C6B 103.1(8) . . ? C6A P1 C6B 117.8(8) . . ? C7A P1 C8A 102.6(4) . . ? C7B P1 C8A 56.6(8) . . ? C6A P1 C8A 98.9(4) . . ? C6B P1 C8A 56.7(8) . . ? C7A P1 C8B 57.9(7) . . ? C7B P1 C8B 100.2(8) . . ? C6A P1 C8B 54.5(7) . . ? C6B P1 C8B 99.2(8) . . ? C8A P1 C8B 133.5(7) . . ? C7A P1 Rh 118.4(3) . . ? C7B P1 Rh 113.1(7) . . ? C6A P1 Rh 116.5(3) . . ? C6B P1 Rh 125.8(7) . . ? C8A P1 Rh 114.5(2) . . ? C8B P1 Rh 111.8(7) . . ? C10 P2 C11 104.7(2) . . ? C10 P2 C9 101.1(3) . . ? C11 P2 C9 98.8(2) . . ? C10 P2 Rh 116.49(18) . . ? C11 P2 Rh 116.91(17) . . ? C9 P2 Rh 116.23(18) . . ? C14 P3 C13 98.2(2) . . ? C14 P3 C12 100.5(2) . . ? C13 P3 C12 101.7(3) . . ? C14 P3 Rh 119.70(18) . . ? C13 P3 Rh 116.95(17) . . ? C12 P3 Rh 116.43(18) . . ? C2 C1 Rh 175.1(5) . . ? C1 C2 Si 170.8(5) . . ? C16 C15 C19 122.2(4) . . ? C16 C15 Rh 115.5(3) . . ? C19 C15 Rh 122.2(4) . . ? C15 C16 C17 114.7(4) . . ? C15 C16 C28 122.7(4) . . ? C17 C16 C28 122.5(4) . . ? C18 C17 C16 116.6(4) . . ? C18 C17 C35 125.3(4) . . ? C16 C17 C35 118.1(4) . . ? C17 C18 C42 119.2(4) . . ? C17 C18 Rh 114.1(3) . . ? C42 C18 Rh 126.7(3) . . ? C20 C19 C15 176.5(5) . . ? C19 C20 C21 178.1(6) . . ? C26 C21 C22 118.5(5) . . ? C26 C21 C20 120.7(5) . . ? C22 C21 C20 120.8(5) . . ? C23 C22 C21 119.3(6) . . ? C24 C23 C22 122.1(6) . . ? C23 C24 C25 118.2(6) . . ? C23 C24 C27 121.9(7) . . ? C25 C24 C27 119.8(7) . . ? C26 C25 C24 120.1(6) . . ? C25 C26 C21 121.8(6) . . ? C33 C28 C29 116.9(5) . . ? C33 C28 C16 120.1(4) . . ? C29 C28 C16 123.0(5) . . ? C30 C29 C28 120.5(5) . . ? C31 C30 C29 122.3(5) . . ? C30 C31 C32 117.7(5) . . ? C30 C31 C34 121.4(5) . . ? C32 C31 C34 120.9(5) . . ? C31 C32 C33 120.4(5) . . ? C28 C33 C32 122.0(5) . . ? C40 C35 C36 116.9(5) . . ? C40 C35 C17 121.9(4) . . ? C36 C35 C17 120.9(5) . . ? C35 C36 C37 121.5(5) . . ? C38 C37 C36 120.9(5) . . ? C39 C38 C37 117.6(5) . . ? C39 C38 C41 121.7(5) . . ? C37 C38 C41 120.7(5) . . ? C38 C39 C40 121.2(5) . . ? C35 C40 C39 121.8(5) . . ? C43 C42 C18 177.9(5) . . ? C42 C43 C44 178.1(6) . . ? C45 C44 C49 117.3(5) . . ? C45 C44 C43 121.2(5) . . ? C49 C44 C43 121.5(4) . . ? C46 C45 C44 121.1(5) . . ? C47 C46 C45 121.5(5) . . ? C46 C47 C48 117.2(5) . . ? C46 C47 C50 121.4(5) . . ? C48 C47 C50 121.3(5) . . ? C49 C48 C47 121.9(4) . . ? C48 C49 C44 120.9(4) . . ? _diffrn_measured_fraction_theta_max 0.908 _diffrn_reflns_theta_full 25.30 _diffrn_measured_fraction_theta_full 0.908 _refine_diff_density_max 0.646 _refine_diff_density_min -1.053 _refine_diff_density_rms 0.098