# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1600 data_2-major _audit_creation_method SHELXL-93 _audit_creation_date 'Aug 11 16:37:37 1998' _audit_update_record 'Jul 28 19:39:37 1999' _computing_data_collection 'MSC/AFC Diffractometer Control' _computing_cell_refinement 'MSC/AFC Diffractometer Control' _computing_data_reduction 'teXsan: PROCESS (MSC)' _computing_structure_solution 'SHELXS-86 Sheldrick (1986)' _computing_publication_material 'SHELXL-93 and modified' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' # Johnson C. K. (1976). ORTEP-II, A FORTRAN Thermal-Ellipsoid Plot Program, # Report ORNL-5138, Oak Ridge National Labratory, Oak Ridge, Tennessee. _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H49 B F4 O P Rh' _chemical_formula_weight 814.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Rh' 'Rh' -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'P1' _symmetry_space_group_name_H-M 'triclinic' _symmetry_Int_Tables_number 1 _symmetry_space_group_name_Hall 'P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 10.0645(14) _cell_length_b 10.9349(13) _cell_length_c 9.9598(13) _cell_angle_alpha 108.124(9) _cell_angle_beta 106.426(10) _cell_angle_gamma 84.967(11) _cell_volume 999.2(2) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 14.92 _cell_measurement_theta_max 14.99 _exptl_crystal_description 'prismatic' _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 422 _exptl_absorpt_coefficient_mu 0.519 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_process_details '( North, Phillips, & Mathews, (1968). Acta Cryst. A24, 351-359.)' _exptl_absorpt_correction_T_min 0.7342 _exptl_absorpt_correction_T_max 0.8773 _exptl_special_details ; \w scan width (1.70 + 0.30tan\q) deg, \w scan rate 16.0 deg/min. The ratio of peak counting time to background counting time was 2:1. The diameter of the incident beam collimeter was 1.0 mm, the crystal to detector distance was 235 mm, and the detector aperture was 3.0 x 3.0 mm (horizontal x vertical). ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_method \w-2\t _diffrn_measurement_device_type 'AFC7R' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 2 0 2 1 0 1 0 1 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 18387 _diffrn_reflns_av_R_equivalents 0.0099 _diffrn_reflns_av_sigmaI/netI 0.0245 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 34.99 _reflns_number_total 17568 _reflns_number_gt 15803 _reflns_threshold_expression >2sigma(I) _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 w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.021(14) _refine_ls_number_reflns 17568 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0416 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0875 _refine_ls_wR_factor_gt 0.0826 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.5000 0.5000 0.5000 0.03501(3) Uani 1 d . . . P P 0.55825(6) 0.70592(4) 0.63749(6) 0.04085(9) Uani 1 d . . . F1 F 1.2159(5) 1.0112(7) 0.4793(7) 0.193(3) Uani 1 d . . . F2 F 1.1991(6) 1.1181(7) 0.3242(10) 0.241(4) Uani 1 d . . . F3 F 1.4044(5) 1.0840(6) 0.4733(10) 0.217(3) Uani 1 d . . . F4 F 1.2946(10) 0.9346(9) 0.3069(7) 0.269(5) Uani 1 d . . . O O 0.5370(2) 0.41110(18) 0.66293(19) 0.0524(4) Uani 1 d . . . C1 C 0.5846(2) 0.55813(19) 0.3510(2) 0.0445(4) Uani 1 d . . . C2 C 0.6796(2) 0.4649(2) 0.4004(3) 0.0416(4) Uani 1 d . . . H2 H 0.7722 0.4799 0.4520 0.050 Uiso 1 calc R . . C3 C 0.60862(19) 0.34594(17) 0.3573(2) 0.0381(3) Uani 1 d . . . C4 C 0.4709(2) 0.36136(18) 0.2677(2) 0.0407(3) Uani 1 d . . . C5 C 0.4568(2) 0.4921(2) 0.2616(2) 0.0442(4) Uani 1 d . . . C6 C 0.3335(3) 0.5315(3) 0.1739(3) 0.0578(6) Uani 1 d . . . H6 H 0.3223 0.6156 0.1695 0.069 Uiso 1 calc R . . C7 C 0.2323(3) 0.4419(4) 0.0967(3) 0.0676(8) Uani 1 d . . . H7 H 0.1524 0.4653 0.0358 0.081 Uiso 1 calc R . . C8 C 0.2441(3) 0.3136(3) 0.1055(3) 0.0631(7) Uani 1 d . . . H8 H 0.1715 0.2562 0.0518 0.076 Uiso 1 calc R . . C9 C 0.3596(2) 0.2735(2) 0.1910(3) 0.0516(5) Uani 1 d . . . H9 H 0.3653 0.1906 0.1990 0.062 Uiso 1 calc R . . C10 C 0.6167(3) 0.6992(2) 0.3854(3) 0.0547(5) Uani 1 d . . . H10A H 0.5871 0.7233 0.2956 0.066 Uiso 1 calc R . . H10B H 0.7160 0.7122 0.4237 0.066 Uiso 1 calc R . . C11 C 0.5450(3) 0.7863(2) 0.4971(3) 0.0517(5) Uani 1 d . . . H11A H 0.4486 0.7986 0.4496 0.062 Uiso 1 calc R . . H11B H 0.5899 0.8697 0.5414 0.062 Uiso 1 calc R . . C12 C 0.4700(2) 0.8025(2) 0.7698(2) 0.0463(4) Uani 1 d . . . C13 C 0.3998(3) 0.9145(2) 0.7550(3) 0.0610(6) Uani 1 d . . . H13 H 0.4004 0.9448 0.6776 0.073 Uiso 1 calc R . . C14 C 0.3285(4) 0.9814(3) 0.8570(4) 0.0753(9) Uani 1 d . . . H14 H 0.2810 1.0563 0.8467 0.090 Uiso 1 calc R . . C15 C 0.3270(3) 0.9388(3) 0.9724(4) 0.0701(8) Uani 1 d . . . H15 H 0.2782 0.9840 1.0392 0.084 Uiso 1 calc R . . C16 C 0.3981(4) 0.8290(4) 0.9886(4) 0.0706(8) Uani 1 d . . . H16 H 0.3993 0.8009 1.0679 0.085 Uiso 1 calc R . . C17 C 0.4684(3) 0.7598(3) 0.8873(3) 0.0635(6) Uani 1 d . . . H17 H 0.5146 0.6846 0.8980 0.076 Uiso 1 calc R . . C18 C 0.7397(2) 0.7149(2) 0.7395(3) 0.0504(4) Uani 1 d . . . C19 C 0.7911(3) 0.6283(3) 0.8169(4) 0.0689(7) Uani 1 d . . . H19 H 0.7336 0.5646 0.8132 0.083 Uiso 1 calc R . . C20 C 0.9270(4) 0.6354(5) 0.8996(6) 0.0959(13) Uani 1 d . . . H20 H 0.9596 0.5801 0.9563 0.115 Uiso 1 calc R . . C21 C 1.0154(4) 0.7255(5) 0.8982(6) 0.1022(15) Uani 1 d . . . H21 H 1.1080 0.7290 0.9514 0.123 Uiso 1 calc R . . C22 C 0.9663(4) 0.8079(5) 0.8192(6) 0.0970(13) Uani 1 d . . . H22 H 1.0261 0.8668 0.8168 0.116 Uiso 1 calc R . . C23 C 0.8291(3) 0.8062(3) 0.7419(5) 0.0738(8) Uani 1 d . . . H23 H 0.7961 0.8661 0.6914 0.089 Uiso 1 calc R . . C24 C 0.6615(2) 0.22675(18) 0.3995(2) 0.0426(3) Uani 1 d . . . H24 H 0.5880 0.1998 0.4311 0.051 Uiso 1 calc R . . C25 C 0.6860(3) 0.1101(2) 0.2711(3) 0.0501(4) Uani 1 d . . . H25 H 0.5967 0.0899 0.1970 0.060 Uiso 1 calc R . . C26 C 0.7234(4) -0.0039(2) 0.3348(4) 0.0687(8) Uani 1 d . . . H26A H 0.6434 -0.0248 0.3596 0.082 Uiso 1 calc R . . H26B H 0.7434 -0.0783 0.2595 0.082 Uiso 1 calc R . . C27 C 0.8455(4) 0.0202(3) 0.4691(4) 0.0690(7) Uani 1 d . . . H27A H 0.9280 0.0325 0.4427 0.083 Uiso 1 calc R . . H27B H 0.8602 -0.0547 0.5040 0.083 Uiso 1 calc R . . C28 C 0.8237(3) 0.1383(3) 0.5921(3) 0.0606(6) Uani 1 d . . . H28 H 0.7436 0.1212 0.6211 0.073 Uiso 1 calc R . . C29 C 0.7885(2) 0.2538(2) 0.5332(3) 0.0495(4) Uani 1 d . . . H29A H 0.8671 0.2741 0.5058 0.059 Uiso 1 calc R . . H29B H 0.7701 0.3279 0.6097 0.059 Uiso 1 calc R . . C30 C 0.7896(3) 0.1364(3) 0.1944(3) 0.0643(6) Uani 1 d . . . H30 H 0.8605 0.1959 0.2683 0.077 Uiso 1 calc R . . C31 C 0.7180(5) 0.1991(4) 0.0783(4) 0.0826(10) Uani 1 d . . . H31A H 0.7841 0.2157 0.0331 0.099 Uiso 1 calc R . . H31B H 0.6771 0.2787 0.1224 0.099 Uiso 1 calc R . . H31C H 0.6470 0.1428 0.0055 0.099 Uiso 1 calc R . . C32 C 0.8623(7) 0.0162(6) 0.1221(7) 0.120(2) Uani 1 d . . . H32A H 0.9088 -0.0260 0.1938 0.145 Uiso 1 calc R . . H32B H 0.9287 0.0401 0.0819 0.145 Uiso 1 calc R . . H32C H 0.7952 -0.0411 0.0449 0.145 Uiso 1 calc R . . C33 C 0.9467(4) 0.1656(5) 0.7269(5) 0.0893(12) Uani 1 d . . . H33A H 0.9647 0.0918 0.7622 0.107 Uiso 1 calc R . . H33B H 0.9266 0.2385 0.8019 0.107 Uiso 1 calc R . . H33C H 1.0267 0.1837 0.7018 0.107 Uiso 1 calc R . . C34 C 0.4320(3) 0.3987(3) 0.7024(3) 0.0603(6) Uani 1 d . . . C35 C 0.3030(3) 0.4494(3) 0.6369(3) 0.0583(5) Uani 1 d . . . C36 C 0.3109(2) 0.5060(2) 0.5353(3) 0.0437(4) Uani 1 d . . . C37 C 0.4517(6) 0.3305(5) 0.8151(5) 0.1028(16) Uani 1 d . . . H37A H 0.5468 0.3051 0.8426 0.123 Uiso 1 calc R . . H37B H 0.3936 0.2555 0.7753 0.123 Uiso 1 calc R . . H37C H 0.4272 0.3869 0.8999 0.123 Uiso 1 calc R . . C38 C 0.1740(4) 0.4340(6) 0.6780(5) 0.0971(14) Uani 1 d . . . H38A H 0.1967 0.3920 0.7531 0.116 Uiso 1 calc R . . H38B H 0.1077 0.3831 0.5933 0.116 Uiso 1 calc R . . H38C H 0.1352 0.5172 0.7139 0.116 Uiso 1 calc R . . C39 C 0.1865(2) 0.5496(2) 0.4435(3) 0.0473(4) Uani 1 d . . . C40 C 0.1693(3) 0.6766(3) 0.4399(3) 0.0592(6) Uani 1 d . . . H40 H 0.2389 0.7365 0.4965 0.071 Uiso 1 calc R . . C41 C 0.0492(4) 0.7144(4) 0.3526(5) 0.0771(9) Uani 1 d . . . H41 H 0.0382 0.7997 0.3525 0.092 Uiso 1 calc R . . C42 C -0.0525(3) 0.6274(5) 0.2674(4) 0.0821(10) Uani 1 d . . . H42 H -0.1327 0.6537 0.2096 0.098 Uiso 1 calc R . . C43 C -0.0374(3) 0.5001(4) 0.2662(4) 0.0771(9) Uani 1 d . . . H43 H -0.1068 0.4410 0.2063 0.093 Uiso 1 calc R . . C44 C 0.0815(3) 0.4599(3) 0.3542(3) 0.0606(6) Uani 1 d . . . H44 H 0.0912 0.3745 0.3538 0.073 Uiso 1 calc R . . B B 1.2763(6) 1.0486(6) 0.4047(8) 0.0914(14) Uani 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 Rh 0.04132(5) 0.03028(4) 0.03696(5) 0.01361(3) 0.01366(4) 0.00516(3) P 0.0470(2) 0.03260(18) 0.0432(2) 0.01179(16) 0.01337(18) 0.00428(16) F1 0.129(3) 0.312(8) 0.203(5) 0.171(6) 0.033(3) -0.036(4) F2 0.172(5) 0.235(6) 0.400(10) 0.256(8) 0.044(5) 0.045(4) F3 0.103(3) 0.183(5) 0.387(10) 0.109(6) 0.065(4) -0.029(3) F4 0.326(11) 0.283(9) 0.152(5) 0.055(6) 0.045(6) 0.137(8) O 0.0634(9) 0.0536(8) 0.0503(8) 0.0278(7) 0.0211(7) 0.0116(7) C1 0.0590(11) 0.0365(7) 0.0475(9) 0.0191(7) 0.0242(8) 0.0072(7) C2 0.0432(9) 0.0383(8) 0.0479(10) 0.0149(8) 0.0181(8) 0.0032(7) C3 0.0400(8) 0.0333(7) 0.0408(7) 0.0112(6) 0.0121(6) 0.0049(6) C4 0.0425(8) 0.0399(8) 0.0382(7) 0.0110(6) 0.0114(6) 0.0067(6) C5 0.0512(10) 0.0467(9) 0.0410(8) 0.0199(7) 0.0186(7) 0.0129(7) C6 0.0650(13) 0.0707(14) 0.0479(10) 0.0333(10) 0.0219(10) 0.0273(11) C7 0.0565(13) 0.100(2) 0.0452(11) 0.0299(13) 0.0116(10) 0.0274(14) C8 0.0474(11) 0.0772(17) 0.0484(11) 0.0062(11) 0.0034(9) 0.0061(11) C9 0.0473(10) 0.0492(10) 0.0477(10) 0.0044(8) 0.0083(8) 0.0026(8) C10 0.0775(15) 0.0402(9) 0.0606(12) 0.0237(9) 0.0320(11) 0.0025(9) C11 0.0683(13) 0.0341(8) 0.0592(12) 0.0201(8) 0.0223(10) 0.0056(8) C12 0.0492(10) 0.0380(8) 0.0458(9) 0.0050(7) 0.0128(8) 0.0022(7) C13 0.0712(17) 0.0427(10) 0.0656(14) 0.0088(10) 0.0249(13) 0.0118(11) C14 0.0774(19) 0.0488(12) 0.089(2) 0.0003(13) 0.0323(17) 0.0150(12) C15 0.0658(15) 0.0594(14) 0.0709(16) -0.0143(12) 0.0309(13) -0.0099(12) C16 0.0753(18) 0.0769(19) 0.0584(14) 0.0072(13) 0.0290(13) -0.0063(15) C17 0.0738(17) 0.0634(14) 0.0576(13) 0.0173(11) 0.0283(12) 0.0096(12) C18 0.0471(10) 0.0462(10) 0.0532(11) 0.0100(8) 0.0129(8) 0.0033(8) C19 0.0526(13) 0.0708(17) 0.083(2) 0.0350(15) 0.0075(13) 0.0110(12) C20 0.0594(17) 0.112(3) 0.115(3) 0.055(3) 0.0043(19) 0.0218(19) C21 0.0479(15) 0.113(3) 0.128(4) 0.033(3) 0.0011(19) 0.0032(18) C22 0.0582(18) 0.098(3) 0.123(4) 0.024(3) 0.012(2) -0.0166(18) C23 0.0589(15) 0.0662(17) 0.092(2) 0.0248(16) 0.0100(15) -0.0113(13) C24 0.0422(8) 0.0339(7) 0.0544(10) 0.0174(7) 0.0148(7) 0.0075(6) C25 0.0521(11) 0.0339(8) 0.0618(12) 0.0094(8) 0.0181(9) 0.0043(7) C26 0.0747(17) 0.0332(9) 0.101(2) 0.0219(11) 0.0286(16) 0.0112(10) C27 0.0713(16) 0.0501(12) 0.097(2) 0.0397(14) 0.0283(15) 0.0236(11) C28 0.0581(13) 0.0621(14) 0.0724(15) 0.0393(12) 0.0172(11) 0.0141(11) C29 0.0488(10) 0.0434(10) 0.0556(11) 0.0210(8) 0.0085(8) 0.0086(8) C30 0.0662(15) 0.0633(14) 0.0620(14) 0.0080(11) 0.0286(12) 0.0059(12) C31 0.106(3) 0.081(2) 0.0707(19) 0.0243(16) 0.0414(19) 0.014(2) C32 0.147(5) 0.118(4) 0.123(4) 0.042(3) 0.090(4) 0.068(4) C33 0.079(2) 0.099(3) 0.094(3) 0.060(2) -0.0026(19) 0.0105(19) C34 0.0796(17) 0.0619(13) 0.0574(12) 0.0335(11) 0.0321(12) 0.0099(12) C35 0.0631(13) 0.0712(15) 0.0546(12) 0.0271(11) 0.0289(10) 0.0019(11) C36 0.0477(10) 0.0421(9) 0.0460(10) 0.0138(8) 0.0201(9) 0.0025(7) C37 0.120(3) 0.134(4) 0.103(3) 0.089(3) 0.056(3) 0.030(3) C38 0.074(2) 0.156(4) 0.097(3) 0.069(3) 0.046(2) 0.002(2) C39 0.0427(9) 0.0505(10) 0.0519(10) 0.0143(8) 0.0201(8) 0.0039(7) C40 0.0526(12) 0.0524(12) 0.0711(15) 0.0177(11) 0.0186(11) 0.0106(10) C41 0.0636(16) 0.080(2) 0.095(2) 0.0375(18) 0.0286(16) 0.0323(15) C42 0.0462(13) 0.118(3) 0.081(2) 0.036(2) 0.0157(13) 0.0222(16) C43 0.0444(12) 0.107(3) 0.0735(18) 0.0170(18) 0.0135(12) -0.0091(14) C44 0.0500(12) 0.0670(15) 0.0653(14) 0.0148(12) 0.0195(10) -0.0079(11) B 0.087(3) 0.092(3) 0.127(4) 0.065(3) 0.047(3) 0.013(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. Least-squares planes (x,y,z in crystal coordinates) and deviations from them (* indicates atom used to define plane) 6.0635 (0.0043) x + 0.1661 (0.0085) y - 8.8551 (0.0034) z = 0.5749 (0.0042) * -0.0456 (0.0017) C1 * 0.0775 (0.0017) C2 * 0.0091 (0.0016) C3 * -0.0303 (0.0018) C4 * -0.0393 (0.0018) C5 * -0.0046 (0.0019) C6 * 0.0510 (0.0021) C7 * 0.0229 (0.0023) C8 * -0.0408 (0.0019) C9 Rms deviation of fitted atoms = 0.0414 - 6.6777 (0.0098) x - 0.7848 (0.0153) y + 8.7258 (0.0064) z = 2.1860 (0.0083) Angle to previous plane (with approximate esd) = 5.37 ( 0.12 ) * 0.0076 (0.0018) C39 * -0.0086 (0.0022) C40 * 0.0020 (0.0026) C41 * 0.0055 (0.0026) C42 * -0.0063 (0.0025) C43 * -0.0003 (0.0021) C44 Rms deviation of fitted atoms = 0.0059 6.3005 (0.0080) x + 0.0809 (0.0109) y - 8.7208 (0.0049) z = 0.6412 (0.0059) Angle to previous plane (with approximate esd) = 4.47 ( 0.14 ) * 0.0202 (0.0015) C4 * -0.0041 (0.0015) C5 * -0.0137 (0.0017) C6 * 0.0152 (0.0019) C7 * 0.0020 (0.0020) C8 * -0.0195 (0.0018) C9 Rms deviation of fitted atoms = 0.0143 ; 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 C36 2.023(2) . yes Rh O 2.0719(15) . yes Rh C1 2.1743(19) . yes Rh C2 2.248(2) . yes Rh C3 2.2626(18) . yes Rh C5 2.2652(19) . yes Rh P 2.2690(6) . yes Rh C4 2.2909(19) . yes P C12 1.809(2) . yes P C18 1.816(2) . yes P C11 1.840(2) . yes F1 B 1.255(6) . yes F2 B 1.322(6) . yes F3 B 1.305(8) . yes F4 B 1.357(10) . yes O C34 1.258(3) . yes C1 C2 1.438(3) . yes C1 C5 1.443(3) . yes C1 C10 1.516(3) . yes C2 C3 1.425(3) . yes C2 H2 0.9300 . ? C3 C4 1.448(3) . yes C3 C24 1.501(3) . yes C4 C9 1.418(3) . yes C4 C5 1.443(3) . yes C4 C39 3.880(3) . ? C4 C44 4.226(3) . ? C4 C40 4.634(3) . ? C4 C43 5.204(4) . ? C4 C41 5.546(4) . ? C4 C42 5.790(4) . ? C5 C6 1.419(3) . yes C5 C39 3.587(3) . ? C5 C40 3.906(3) . ? C5 C44 4.201(3) . ? C5 C41 4.749(4) . ? C5 C43 4.980(4) . ? C5 C42 5.220(4) . ? C6 C7 1.361(5) . yes C6 C39 3.362(3) . ? C6 C40 3.416(4) . ? C6 C44 3.751(4) . ? C6 C41 3.876(4) . ? C6 C43 4.154(4) . ? C6 C42 4.217(4) . ? C6 H6 0.9300 . ? C7 C8 1.426(5) . yes C7 C44 3.280(4) . ? C7 C39 3.436(4) . ? C7 C43 3.499(4) . ? C7 C40 3.763(4) . ? C7 C42 3.849(4) . ? C7 C41 3.968(5) . ? C7 H7 0.9300 . ? C8 C9 1.360(4) . yes C8 C44 3.278(4) . ? C8 C39 3.710(4) . ? C8 C43 3.777(5) . ? C8 C40 4.482(4) . ? C8 C42 4.557(5) . ? C8 C41 4.861(5) . ? C8 H8 0.9300 . ? C9 C44 3.760(4) . ? C9 C39 3.912(3) . ? C9 C43 4.633(4) . ? C9 C40 4.863(4) . ? C9 C42 5.467(4) . ? C9 C41 5.565(4) . ? C9 H9 0.9300 . ? C10 C11 1.529(3) . yes C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.387(3) . yes C12 C17 1.393(4) . yes C13 C14 1.393(4) . yes C13 H13 0.9300 . ? C14 C15 1.372(6) . yes C14 H14 0.9300 . ? C15 C16 1.373(5) . yes C15 H15 0.9300 . ? C16 C17 1.387(4) . yes C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.379(4) . yes C18 C23 1.392(4) . yes C19 C20 1.377(5) . yes C19 H19 0.9300 . ? C20 C21 1.390(7) . yes C20 H20 0.9300 . ? C21 C22 1.348(7) . yes C21 H21 0.9300 . ? C22 C23 1.376(5) . yes C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C29 1.533(3) . yes C24 C25 1.559(3) . yes C24 H24 0.9800 . ? C25 C26 1.541(4) . yes C25 C30 1.547(4) . yes C25 H25 0.9800 . ? C26 C27 1.509(5) . yes C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.528(5) . yes C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C33 1.516(5) . yes C28 C29 1.527(3) . yes C28 H28 0.9800 . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.503(5) . yes C30 C32 1.524(5) . yes C30 H30 0.9800 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 C35 1.428(4) . yes C34 C37 1.491(4) . yes C35 C36 1.362(3) . yes C35 C38 1.505(4) . yes C36 C39 1.466(3) . yes C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.395(4) . yes C39 C44 1.405(4) . yes C40 C41 1.389(4) . yes C40 H40 0.9300 . ? C41 C42 1.360(6) . yes C41 H41 0.9300 . ? C42 C43 1.383(6) . yes C42 H42 0.9300 . ? C43 C44 1.396(5) . yes C43 H43 0.9300 . ? C44 H44 0.9300 . ? 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 C36 Rh O 77.98(8) . . yes C36 Rh C1 135.27(9) . . yes O Rh C1 146.69(8) . . yes C36 Rh C2 164.90(8) . . yes O Rh C2 109.60(8) . . yes C1 Rh C2 37.91(8) . . yes C36 Rh C3 132.01(9) . . yes O Rh C3 94.17(7) . . yes C1 Rh C3 63.32(7) . . yes C2 Rh C3 36.82(7) . . yes C36 Rh C5 104.92(9) . . yes O Rh C5 151.44(8) . . yes C1 Rh C5 37.87(9) . . yes C2 Rh C5 62.04(8) . . yes C3 Rh C5 62.35(7) . . yes C36 Rh P 95.70(7) . . yes O Rh P 100.55(6) . . yes C1 Rh P 80.85(6) . . yes C2 Rh P 95.65(6) . . yes C3 Rh P 132.13(5) . . yes C5 Rh P 107.30(6) . . yes C36 Rh C4 103.82(9) . . yes O Rh C4 114.52(7) . . yes C1 Rh C4 62.73(8) . . yes C2 Rh C4 61.29(8) . . yes C3 Rh C4 37.09(7) . . yes C5 Rh C4 36.93(7) . . yes P Rh C4 142.53(5) . . yes C12 P C18 104.40(11) . . yes C12 P C11 108.94(11) . . yes C18 P C11 105.86(12) . . yes C12 P Rh 123.97(8) . . yes C18 P Rh 110.15(8) . . yes C11 P Rh 102.35(8) . . yes C34 O Rh 114.79(17) . . yes C2 C1 C5 107.65(17) . . yes C2 C1 C10 125.3(2) . . yes C5 C1 C10 127.0(2) . . yes C2 C1 Rh 73.82(12) . . yes C5 C1 Rh 74.48(11) . . yes C10 C1 Rh 118.60(14) . . yes C3 C2 C1 108.96(19) . . yes C3 C2 Rh 72.15(11) . . yes C1 C2 Rh 68.27(11) . . yes C3 C2 H2 125.5 . . ? C1 C2 H2 125.5 . . ? Rh C2 H2 125.6 . . ? C2 C3 C4 107.30(16) . . yes C2 C3 C24 127.52(18) . . yes C4 C3 C24 125.15(17) . . yes C2 C3 Rh 71.03(11) . . yes C4 C3 Rh 72.52(10) . . yes C24 C3 Rh 120.13(13) . . yes C9 C4 C5 120.05(19) . . yes C9 C4 C3 131.63(19) . . yes C5 C4 C3 108.31(18) . . yes C9 C4 Rh 125.30(15) . . yes C5 C4 Rh 70.57(11) . . yes C3 C4 Rh 70.39(10) . . yes C6 C5 C4 120.0(2) . . yes C6 C5 C1 132.6(2) . . yes C4 C5 C1 107.40(17) . . yes C6 C5 Rh 126.70(15) . . yes C4 C5 Rh 72.50(11) . . yes C1 C5 Rh 67.65(11) . . yes C7 C6 C5 117.7(2) . . yes C7 C6 H6 121.1 . . ? C5 C6 H6 121.1 . . ? C6 C7 C8 122.5(2) . . yes C6 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C9 C8 C7 121.3(3) . . yes C9 C8 H8 119.4 . . ? C7 C8 H8 119.4 . . ? C8 C9 C4 118.3(3) . . yes C8 C9 H9 120.8 . . ? C4 C9 H9 120.8 . . ? C1 C10 C11 112.29(18) . . yes C1 C10 H10A 109.1 . . ? C11 C10 H10A 109.1 . . ? C1 C10 H10B 109.1 . . ? C11 C10 H10B 109.1 . . ? H10A C10 H10B 107.9 . . ? C10 C11 P 107.02(14) . . yes C10 C11 H11A 110.3 . . ? P C11 H11A 110.3 . . ? C10 C11 H11B 110.3 . . ? P C11 H11B 110.3 . . ? H11A C11 H11B 108.6 . . ? C13 C12 C17 119.1(2) . . yes C13 C12 P 122.2(2) . . yes C17 C12 P 118.61(18) . . yes C12 C13 C14 119.5(3) . . yes C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 121.2(3) . . yes C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 119.4(3) . . yes C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C16 C17 120.4(3) . . yes C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C16 C17 C12 120.4(3) . . yes C16 C17 H17 119.8 . . ? C12 C17 H17 119.8 . . ? C19 C18 C23 118.7(3) . . yes C19 C18 P 119.1(2) . . yes C23 C18 P 122.2(2) . . yes C20 C19 C18 120.5(4) . . yes C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 119.8(4) . . yes C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 119.6(3) . . yes C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 121.2(4) . . yes C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 119.9(4) . . yes C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? C3 C24 C29 112.24(17) . . yes C3 C24 C25 114.74(18) . . yes C29 C24 C25 111.78(18) . . yes C3 C24 H24 105.8 . . ? C29 C24 H24 105.8 . . ? C25 C24 H24 105.8 . . ? C26 C25 C30 115.2(2) . . yes C26 C25 C24 105.7(2) . . yes C30 C25 C24 114.5(2) . . yes C26 C25 H25 107.0 . . ? C30 C25 H25 107.0 . . ? C24 C25 H25 107.0 . . ? C27 C26 C25 114.4(2) . . yes C27 C26 H26A 108.7 . . ? C25 C26 H26A 108.7 . . ? C27 C26 H26B 108.7 . . ? C25 C26 H26B 108.7 . . ? H26A C26 H26B 107.6 . . ? C26 C27 C28 112.0(2) . . yes C26 C27 H27A 109.2 . . ? C28 C27 H27A 109.2 . . ? C26 C27 H27B 109.2 . . ? C28 C27 H27B 109.2 . . ? H27A C27 H27B 107.9 . . ? C33 C28 C29 111.7(3) . . yes C33 C28 C27 112.7(3) . . yes C29 C28 C27 109.2(2) . . yes C33 C28 H28 107.7 . . ? C29 C28 H28 107.7 . . ? C27 C28 H28 107.7 . . ? C28 C29 C24 111.3(2) . . yes C28 C29 H29A 109.4 . . ? C24 C29 H29A 109.4 . . ? C28 C29 H29B 109.4 . . ? C24 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? C31 C30 C32 107.7(3) . . yes C31 C30 C25 110.8(3) . . yes C32 C30 C25 113.9(3) . . yes C31 C30 H30 108.1 . . ? C32 C30 H30 108.1 . . ? C25 C30 H30 108.1 . . ? 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 . . ? C28 C33 H33A 109.5 . . ? C28 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C28 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O C34 C35 118.5(2) . . yes O C34 C37 117.0(3) . . yes C35 C34 C37 124.4(3) . . yes C36 C35 C34 113.5(2) . . yes C36 C35 C38 126.0(3) . . yes C34 C35 C38 120.4(3) . . yes C35 C36 C39 121.5(2) . . yes C35 C36 Rh 115.13(19) . . yes C39 C36 Rh 122.75(16) . . yes C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 118.7(2) . . yes C40 C39 C36 122.4(2) . . yes C44 C39 C36 118.9(2) . . yes C41 C40 C39 120.6(3) . . yes C41 C40 H40 119.7 . . ? C39 C40 H40 119.7 . . ? C42 C41 C40 120.3(3) . . yes C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 120.5(3) . . yes C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C42 C43 C44 120.3(3) . . yes C42 C43 H43 119.9 . . ? C44 C43 H43 119.9 . . ? C43 C44 C39 119.5(3) . . yes C43 C44 H44 120.2 . . ? C39 C44 H44 120.2 . . ? F1 B F3 113.7(6) . . yes F1 B F2 114.9(6) . . yes F3 B F2 118.3(5) . . yes F1 B F4 100.4(7) . . yes F3 B F4 101.2(6) . . yes F2 B F4 105.0(7) . . yes _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 34.99 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.396 _refine_diff_density_min -0.246 _refine_diff_density_rms 0.047 _publ_contact_author_name ' Prof. Kazuhide Tani ' _publ_contact_author_address ; Department of Chemistry Graduate School of Engineering Science Osaka University Machikaneyama, 1-3 Toyonaka Osaka, 560-8531 Japan ; _publ_contact_author_phone ' +81 6 6850 6245' _publ_contact_author_fax ' +81 6 6850 6245' _publ_contact_author_email tani@chem.es.osaka-u.ac.jp _publ_requested_journal ' ' _publ_requested_category FM _publ_requested_coeditor_name ' ' _publ_contact_letter ; ; _journal_date_recd_electronic ? _journal_date_to_coeditor ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_date_printers_first ? _journal_date_printers_final ? _journal_date_proofs_out ? _journal_date_proofs_in ? _journal_coeditor_name ? _journal_coeditor_code ? _journal_coeditor_notes ; ? ; _journal_techeditor_code ? _journal_techeditor_notes ; ? ; _journal_coden_ASTM ? _journal_name_full ' ' _journal_year ? _journal_volume ? _journal_issue ? _journal_page_first ? _journal_page_last ? _journal_suppl_publ_number ? _journal_suppl_publ_pages ? _publ_section_title ; ; loop_ _publ_author_name _publ_author_address 'Yasushi Kataoka*' ; Department of Chemistry Graduate School of Engineering Science Osaka University Machikaneyama, 1-3 Toyonaka Osaka, 560-8531 Japan ; 'Yoko Iwato ' ; Department of Chemistry Graduate School of Engineering Science Osaka University Machikaneyama, 1-3 Toyonaka Osaka, 560-8531 Japan ; 'Atsushi Shibahara' ; Department of Chemistry Graduate School of Engineering Science Osaka University Machikaneyama, 1-3 Toyonaka Osaka, 560-8531 Japan ; 'Tsunaki Yamaagata ' ; Department of Chemistry Graduate School of Engineering Science Osaka University Machikaneyama, 1-3 Toyonaka Osaka, 560-8531 Japan ; 'Tani, Kazuhide' ; Department of Chemistry Graduate School of Engineering Science Osaka University Machikaneyama, 1-3 Toyonaka Osaka, 560-8531 Japan ; _publ_section_abstract ; ; _publ_section_experimental ; ; _publ_section_comment ; ; _publ_section_references ; ; _publ_section_figure_captions ; ;