data_gc3cbm _publ_author_name ; Giuseppe Canepa, Carsten D. Brandt, and Helmut Werner* ; _publ_author_address ; Prof. Dr. Helmut Werner Institut f\"ur Anorganische Chemie Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Deutschland ; _publ_contact_author ; Prof. Dr. Helmut Werner Institut f\"ur Anorganische Chemie Universit\"at W\"urzburg Am Hubland D-97074 W\"urzburg Deutschland ; _publ_contact_author_phone '049 931 888 5261' _publ_contact_author_fax '049 931 888 4623' _publ_contact_author_email helmut.werner@mail.uni-wuerzburg.de _publ_requested_journal 'Organometallics' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in "Organometallics" ; _publ_section_title ; Mono- and Dinuclear Rhodium(I) and Rhodium(III) Complexes with the Bulky Phosphine 2,6-Me2C6H3CH2CH2PtBu2 Including the First Structurally Characterized cis-Configurated Dicarbonyl Compound cis-[RhCl(CO)2(PR3)] ; _publ_section_abstract ; Abstract: The bulky functionalized phosphine 2,6-Me2C6H3CH2CH2PtBu2 (3) was prepared in a stepwise fashion from the Grignard reagent 2,6-Me2C6H3CH2CH2MgCl, tBuPCl2 and tBuLi. Phosphine 3 reacts with the olefin compounds [RhCl(C2H4)2]2 and [RhCl(C8H14)2]2 to give the substitution products [RhCl(olefin)(3)]2 (8, 9), of which 8 (olefin = C2H4) has been characterized crystallographically. While 8 is rather inert toward 3, it reacts with 3 under a hydrogen atmosphere to give the dihydrido complex [RhH2Cl(3)2] (11) via the dimer [RhH2Cl(3)]2 (10) as an intermediate. In the presence of ethene, 11 is reconverted to 8. The reaction of 9 (olefin = C8H14) with the phosphonium salt 3·HCl affords a mixture of [RhHCl2(3)]2 (12) and 3, which upon warming at 60 °C produce [RhHCl2(3)2] (13). The attempted separation of 12 by column chromatography on Al2O3 led unexpectedly to the formation of the novel halfsandwich-type compound [((6-2,6-Me2C6H3CH2CH2PtBu2-(-P)RhCl] (14). Treatment of either 9 or 14 with CO gives cis-[RhCl(CO)2(3)] (15), which represence the first structurally characterized dicarbonyl complex with the CO ligands in cis-disposition. In the absence of carbon monoxide, 15 is rather labile and readily converted to [RhCl(CO)(3)]2 (16). The reaction of 8 with HCl affords the dinuclear ethylrhodium(III) compound 18, being built up by two 14-electron [RhCl2(C2H5)(3)] units. These units are linked by two bridging chlorides which are unsymmetrically situated between the two metal centers. Compound 18 reacts with CO to give 15 and with 3 to give 13, in both cases via [RhHCl2(C2H4)(3)] as an intermediate. The halfsandwich-type complexes [((6-2,6-Me2C6H3CH2CH2PtBu2-(-P)Rh(olefin)]PF6 (20, 21), obtained from [Rh(acetone)2(C8H14)2]PF6 as the precursor, react in acetone in the presence of H2 to give [RhH2(acetone)3(3)]PF6 (22), which upon addition of diethyl ether generates the dihydride [((6-2,6-Me2C6H3CH2CH2PtBu2-(-P)RhH2]PF6 (23). Compound 23 is a suitable starting material for the preparation of compounds with the general composition [((6-2,6-Me2C6H3CH2CH2PtBu2-(-P)Rh(L)]PF6, where L is acetone, CH2=CHR (R = tBu, Ph), PhC(CH and CO, respectively. ; _publ_section_exptl_prep ; Crystals were grown from a mixture of the starting materials in benzene at room temperature. ; _publ_section_exptl_refinement ; The hydogen atoms of the co-ordinated ethene molecules were found in a differential Fourier synthesis. ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H70 Cl2 P2 Rh2' _chemical_formula_weight 889.62 _chemical_melting_point '_C (dec.)' _chemical_compound_source ? 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' 'P' 'P' 0.1023 0.0942 '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' '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 -1 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5713(17) _cell_length_b 8.5866(17) _cell_length_c 30.745(6) _cell_angle_alpha 94.76(3) _cell_angle_beta 94.61(3) _cell_angle_gamma 112.88(3) _cell_volume 2061.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.433 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.034 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'IPDS (STOE)' _diffrn_measurement_method 'IPDS (STOE)' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 6781 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6781 _reflns_number_gt 5948 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (STOE)' _computing_cell_refinement 'IPDS (STOE)' _computing_data_reduction 'IPDS (STOE)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-97' _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^)+(0.0769P)^2^+6.5760P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson _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_number_reflns 6781 _refine_ls_number_parameters 455 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1420 _refine_ls_wR_factor_gt 0.1394 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.162 _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 0.91243(5) 0.07526(5) 0.304014(11) 0.02093(14) Uani 1 1 d . . . Rh2 Rh 0.92517(5) 0.08795(5) 0.195978(11) 0.02150(14) Uani 1 1 d . . . P1 P 0.68948(17) -0.04101(17) 0.34258(4) 0.0198(3) Uani 1 1 d . . . P2 P 1.04112(16) 0.31096(17) 0.15734(4) 0.0209(3) Uani 1 1 d . . . Cl1 Cl 0.80928(18) -0.14007(17) 0.24115(4) 0.0292(3) Uani 1 1 d . . . Cl2 Cl 1.14063(16) 0.19132(19) 0.25882(4) 0.0294(3) Uani 1 1 d . . . C1 C 1.0033(8) 0.3175(8) 0.34113(18) 0.0317(12) Uani 1 1 d D . . H1A H 0.923(7) 0.347(9) 0.3574(19) 0.038 Uiso 1 1 d D . . H1B H 1.057(8) 0.402(6) 0.3216(18) 0.038 Uiso 1 1 d D . . C2 C 1.0885(7) 0.2210(8) 0.35859(18) 0.0325(13) Uani 1 1 d D . . H2A H 1.200(4) 0.243(9) 0.348(2) 0.039 Uiso 1 1 d D . . H2B H 1.068(8) 0.172(8) 0.3864(12) 0.039 Uiso 1 1 d D . . C3 C 0.7794(8) -0.0874(8) 0.14131(17) 0.0320(12) Uani 1 1 d D . . H3A H 0.825(8) -0.062(9) 0.1133(12) 0.038 Uiso 1 1 d D . . H3B H 0.777(9) -0.198(4) 0.147(2) 0.038 Uiso 1 1 d D . . C4 C 0.6832(7) -0.0028(8) 0.15882(18) 0.0304(12) Uani 1 1 d D . . H4A H 0.657(9) 0.078(7) 0.1424(18) 0.036 Uiso 1 1 d D . . H4B H 0.602(6) -0.071(7) 0.1776(18) 0.036 Uiso 1 1 d D . . C5 C 0.6293(7) -0.2768(7) 0.34547(16) 0.0263(11) Uani 1 1 d . . . C6 C 0.5228(8) -0.3855(7) 0.30314(18) 0.0310(12) Uani 1 1 d . . . H6A H 0.5799 -0.3410 0.2778 0.046 Uiso 1 1 calc R . . H6B H 0.4098 -0.3815 0.3008 0.046 Uiso 1 1 calc R . . H6C H 0.5106 -0.5035 0.3038 0.046 Uiso 1 1 calc R . . C7 C 0.7986(8) -0.3016(8) 0.3512(2) 0.0353(13) Uani 1 1 d . . . H7A H 0.7746 -0.4206 0.3550 0.053 Uiso 1 1 calc R . . H7B H 0.8716 -0.2271 0.3771 0.053 Uiso 1 1 calc R . . H7C H 0.8571 -0.2729 0.3250 0.053 Uiso 1 1 calc R . . C8 C 0.5311(9) -0.3444(8) 0.38420(19) 0.0373(14) Uani 1 1 d . . . H8A H 0.4232 -0.3295 0.3814 0.056 Uiso 1 1 calc R . . H8B H 0.5998 -0.2813 0.4119 0.056 Uiso 1 1 calc R . . H8C H 0.5075 -0.4657 0.3840 0.056 Uiso 1 1 calc R . . C9 C 0.4976(7) -0.0023(7) 0.31962(16) 0.0244(11) Uani 1 1 d . . . C10 C 0.3295(7) -0.1034(8) 0.33748(18) 0.0320(12) Uani 1 1 d . . . H10A H 0.2447 -0.0575 0.3290 0.048 Uiso 1 1 calc R . . H10B H 0.3494 -0.0936 0.3696 0.048 Uiso 1 1 calc R . . H10C H 0.2872 -0.2235 0.3252 0.048 Uiso 1 1 calc R . . C11 C 0.5431(8) 0.1909(7) 0.33106(18) 0.0300(12) Uani 1 1 d . . . H11A H 0.4515 0.2193 0.3176 0.045 Uiso 1 1 calc R . . H11B H 0.6501 0.2562 0.3198 0.045 Uiso 1 1 calc R . . H11C H 0.5565 0.2192 0.3631 0.045 Uiso 1 1 calc R . . C12 C 0.4710(8) -0.0383(8) 0.26913(16) 0.0297(12) Uani 1 1 d . . . H12A H 0.4593 -0.1550 0.2602 0.044 Uiso 1 1 calc R . . H12B H 0.5694 0.0421 0.2572 0.044 Uiso 1 1 calc R . . H12C H 0.3674 -0.0250 0.2577 0.044 Uiso 1 1 calc R . . C13 C 0.7439(7) 0.0523(7) 0.40185(15) 0.0234(10) Uani 1 1 d . . . H13A H 0.8188 0.0013 0.4153 0.028 Uiso 1 1 calc R . . H13B H 0.8159 0.1747 0.4021 0.028 Uiso 1 1 calc R . . C14 C 0.6124(7) 0.0435(7) 0.43444(16) 0.0259(11) Uani 1 1 d . . . H14A H 0.5341 0.0939 0.4227 0.031 Uiso 1 1 calc R . . H14B H 0.5435 -0.0770 0.4377 0.031 Uiso 1 1 calc R . . C15 C 0.7034(7) 0.1398(7) 0.47920(17) 0.0285(12) Uani 1 1 d . . . C16 C 0.7335(8) 0.3115(8) 0.48962(18) 0.0323(12) Uani 1 1 d . . . C17 C 0.8142(9) 0.3964(8) 0.5313(2) 0.0390(14) Uani 1 1 d . . . H17 H 0.8327 0.5124 0.5386 0.047 Uiso 1 1 calc R . . C18 C 0.8672(8) 0.3121(8) 0.56187(18) 0.0367(14) Uani 1 1 d . . . H18 H 0.9209 0.3698 0.5902 0.044 Uiso 1 1 calc R . . C19 C 0.8424(8) 0.1460(8) 0.55129(18) 0.0355(13) Uani 1 1 d . . . H19 H 0.8810 0.0899 0.5724 0.043 Uiso 1 1 calc R . . C20 C 0.7620(7) 0.0571(8) 0.51045(17) 0.0297(12) Uani 1 1 d . . . C21 C 0.7388(9) -0.1269(8) 0.50158(19) 0.0360(13) Uani 1 1 d . . . H21A H 0.8026 -0.1396 0.4774 0.054 Uiso 1 1 calc R . . H21B H 0.6174 -0.1991 0.4935 0.054 Uiso 1 1 calc R . . H21C H 0.7813 -0.1613 0.5281 0.054 Uiso 1 1 calc R . . C22 C 0.6800(10) 0.4086(9) 0.4568(2) 0.0451(16) Uani 1 1 d . . . H22A H 0.7319 0.4026 0.4298 0.068 Uiso 1 1 calc R . . H22B H 0.7178 0.5280 0.4694 0.068 Uiso 1 1 calc R . . H22C H 0.5554 0.3583 0.4500 0.068 Uiso 1 1 calc R . . C23 C 1.2767(7) 0.3704(8) 0.15463(17) 0.0291(12) Uani 1 1 d . . . C24 C 1.3867(7) 0.4768(8) 0.19676(18) 0.0312(12) Uani 1 1 d . . . H24A H 1.3438 0.4191 0.2222 0.047 Uiso 1 1 calc R . . H24B H 1.3815 0.5892 0.1995 0.047 Uiso 1 1 calc R . . H24C H 1.5051 0.4902 0.1956 0.047 Uiso 1 1 calc R . . C25 C 1.3027(7) 0.2024(8) 0.14870(19) 0.0356(14) Uani 1 1 d . . . H25A H 1.4234 0.2276 0.1466 0.053 Uiso 1 1 calc R . . H25B H 1.2338 0.1325 0.1217 0.053 Uiso 1 1 calc R . . H25C H 1.2674 0.1403 0.1740 0.053 Uiso 1 1 calc R . . C26 C 1.3449(7) 0.4702(9) 0.11578(18) 0.0356(13) Uani 1 1 d . . . H26A H 1.4666 0.4947 0.1160 0.053 Uiso 1 1 calc R . . H26B H 1.3289 0.5774 0.1187 0.053 Uiso 1 1 calc R . . H26C H 1.2823 0.4016 0.0880 0.053 Uiso 1 1 calc R . . C27 C 1.0013(7) 0.5019(7) 0.18013(16) 0.0252(11) Uani 1 1 d . . . C28 C 1.1045(8) 0.6705(7) 0.16238(19) 0.0342(13) Uani 1 1 d . . . H28A H 1.0863 0.6535 0.1302 0.051 Uiso 1 1 calc R . . H28B H 1.2262 0.7061 0.1724 0.051 Uiso 1 1 calc R . . H28C H 1.0666 0.7588 0.1733 0.051 Uiso 1 1 calc R . . C29 C 0.8103(7) 0.4594(8) 0.16920(18) 0.0309(12) Uani 1 1 d . . . H29A H 0.7821 0.5479 0.1845 0.046 Uiso 1 1 calc R . . H29B H 0.7440 0.3490 0.1787 0.046 Uiso 1 1 calc R . . H29C H 0.7830 0.4541 0.1374 0.046 Uiso 1 1 calc R . . C30 C 1.0383(8) 0.5291(8) 0.23070(17) 0.0309(12) Uani 1 1 d . . . H30A H 1.0213 0.6304 0.2422 0.046 Uiso 1 1 calc R . . H30B H 1.1565 0.5448 0.2394 0.046 Uiso 1 1 calc R . . H30C H 0.9607 0.4293 0.2427 0.046 Uiso 1 1 calc R . . C31 C 0.9478(7) 0.2561(7) 0.09809(16) 0.0248(11) Uani 1 1 d . . . H31A H 0.9990 0.1815 0.0846 0.030 Uiso 1 1 calc R . . H31B H 0.8251 0.1840 0.0979 0.030 Uiso 1 1 calc R . . C32 C 0.9563(7) 0.3873(7) 0.06555(16) 0.0289(12) Uani 1 1 d . . . H32A H 0.9053 0.4650 0.0773 0.035 Uiso 1 1 calc R . . H32B H 1.0770 0.4564 0.0623 0.035 Uiso 1 1 calc R . . C33 C 0.8604(7) 0.2960(7) 0.02083(16) 0.0277(11) Uani 1 1 d . . . C34 C 0.9435(8) 0.2381(8) -0.01061(17) 0.0312(12) Uani 1 1 d . . . C35 C 0.8542(8) 0.1575(8) -0.05154(18) 0.0350(13) Uani 1 1 d . . . H35 H 0.9098 0.1183 -0.0727 0.042 Uiso 1 1 calc R . . C36 C 0.6877(9) 0.1339(9) -0.06182(19) 0.0400(15) Uani 1 1 d . . . H36 H 0.6300 0.0819 -0.0903 0.048 Uiso 1 1 calc R . . C37 C 0.6037(8) 0.1848(9) -0.0313(2) 0.0406(15) Uani 1 1 d . . . H37 H 0.4870 0.1647 -0.0384 0.049 Uiso 1 1 calc R . . C38 C 0.6895(8) 0.2673(9) 0.01088(19) 0.0357(13) Uani 1 1 d . . . C39 C 0.5904(9) 0.3190(11) 0.0429(2) 0.0486(17) Uani 1 1 d . . . H39A H 0.5915 0.2635 0.0695 0.073 Uiso 1 1 calc R . . H39B H 0.4724 0.2844 0.0295 0.073 Uiso 1 1 calc R . . H39C H 0.6425 0.4429 0.0508 0.073 Uiso 1 1 calc R . . C40 C 1.1267(8) 0.2610(9) -0.00176(19) 0.0395(14) Uani 1 1 d . . . H40A H 1.1622 0.2212 -0.0285 0.059 Uiso 1 1 calc R . . H40B H 1.1385 0.1949 0.0218 0.059 Uiso 1 1 calc R . . H40C H 1.1987 0.3818 0.0072 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.0233(2) 0.0203(3) 0.0159(2) -0.00032(14) -0.00009(15) 0.00613(19) Rh2 0.0241(2) 0.0212(2) 0.0159(2) 0.00011(14) -0.00059(15) 0.00642(19) P1 0.0235(6) 0.0173(7) 0.0159(6) 0.0005(4) -0.0013(5) 0.0062(6) P2 0.0216(6) 0.0216(7) 0.0161(6) -0.0004(5) 0.0004(5) 0.0061(6) Cl1 0.0424(7) 0.0210(7) 0.0189(6) -0.0006(4) 0.0039(5) 0.0075(6) Cl2 0.0228(6) 0.0400(8) 0.0209(6) 0.0047(5) -0.0001(5) 0.0081(6) C1 0.031(3) 0.022(3) 0.029(3) -0.004(2) 0.004(2) -0.003(3) C2 0.024(3) 0.040(4) 0.024(3) -0.005(2) -0.005(2) 0.006(3) C3 0.039(3) 0.028(3) 0.020(2) -0.004(2) -0.006(2) 0.006(3) C4 0.024(3) 0.035(3) 0.025(3) 0.002(2) -0.007(2) 0.007(3) C5 0.033(3) 0.016(3) 0.023(2) 0.0019(19) -0.005(2) 0.004(2) C6 0.037(3) 0.020(3) 0.028(3) 0.002(2) -0.004(2) 0.004(3) C7 0.040(3) 0.028(3) 0.037(3) 0.003(2) -0.008(2) 0.015(3) C8 0.052(4) 0.023(3) 0.029(3) 0.008(2) 0.000(3) 0.006(3) C9 0.025(3) 0.025(3) 0.021(2) 0.0038(19) -0.0006(19) 0.009(2) C10 0.023(3) 0.042(4) 0.030(3) 0.005(2) -0.001(2) 0.014(3) C11 0.036(3) 0.028(3) 0.028(3) 0.004(2) 0.001(2) 0.016(3) C12 0.036(3) 0.031(3) 0.021(3) 0.001(2) -0.005(2) 0.014(3) C13 0.023(2) 0.023(3) 0.019(2) 0.0005(19) -0.0021(19) 0.005(2) C14 0.027(3) 0.028(3) 0.020(2) 0.004(2) 0.002(2) 0.009(3) C15 0.029(3) 0.029(3) 0.022(3) 0.001(2) 0.006(2) 0.005(3) C16 0.033(3) 0.033(3) 0.027(3) 0.002(2) 0.003(2) 0.010(3) C17 0.046(4) 0.028(4) 0.036(3) -0.006(2) 0.003(3) 0.009(3) C18 0.040(3) 0.041(4) 0.022(3) -0.005(2) -0.003(2) 0.011(3) C19 0.039(3) 0.042(4) 0.025(3) 0.005(2) 0.001(2) 0.016(3) C20 0.028(3) 0.037(4) 0.021(3) 0.004(2) 0.003(2) 0.011(3) C21 0.046(4) 0.037(4) 0.028(3) 0.006(2) 0.000(2) 0.020(3) C22 0.066(5) 0.034(4) 0.033(3) 0.001(3) -0.001(3) 0.019(4) C23 0.022(3) 0.036(3) 0.024(3) -0.003(2) 0.003(2) 0.007(3) C24 0.021(3) 0.035(4) 0.029(3) -0.005(2) 0.000(2) 0.003(3) C25 0.025(3) 0.048(4) 0.034(3) -0.009(3) 0.002(2) 0.017(3) C26 0.028(3) 0.045(4) 0.025(3) 0.000(2) 0.006(2) 0.005(3) C27 0.028(3) 0.026(3) 0.020(2) -0.0021(19) 0.0024(19) 0.010(2) C28 0.044(3) 0.023(3) 0.032(3) 0.002(2) 0.006(2) 0.011(3) C29 0.031(3) 0.034(3) 0.033(3) 0.001(2) 0.004(2) 0.019(3) C30 0.038(3) 0.033(3) 0.021(3) -0.003(2) 0.002(2) 0.015(3) C31 0.029(3) 0.022(3) 0.017(2) 0.0001(19) 0.0006(19) 0.005(2) C32 0.032(3) 0.025(3) 0.021(2) 0.001(2) -0.001(2) 0.004(3) C33 0.030(3) 0.026(3) 0.019(2) 0.006(2) -0.002(2) 0.002(3) C34 0.040(3) 0.029(3) 0.021(3) 0.006(2) 0.004(2) 0.008(3) C35 0.046(4) 0.033(4) 0.024(3) 0.001(2) 0.001(2) 0.014(3) C36 0.047(4) 0.039(4) 0.023(3) -0.002(2) -0.007(2) 0.009(3) C37 0.031(3) 0.045(4) 0.035(3) 0.002(3) -0.008(2) 0.007(3) C38 0.038(3) 0.040(4) 0.027(3) 0.007(2) 0.004(2) 0.012(3) C39 0.034(3) 0.067(5) 0.041(4) 0.001(3) 0.002(3) 0.018(4) C40 0.042(3) 0.046(4) 0.031(3) 0.003(3) 0.007(2) 0.018(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 C2 2.106(5) . ? Rh1 C1 2.107(6) . ? Rh1 P1 2.2653(16) . ? Rh1 Cl1 2.4077(16) . ? Rh1 Cl2 2.4293(15) . ? Rh2 C4 2.104(5) . ? Rh2 C3 2.105(5) . ? Rh2 P2 2.2701(16) . ? Rh2 Cl2 2.4078(16) . ? Rh2 Cl1 2.4310(16) . ? P1 C13 1.874(5) . ? P1 C9 1.895(5) . ? P1 C5 1.897(5) . ? P2 C31 1.874(5) . ? P2 C27 1.891(5) . ? P2 C23 1.892(5) . ? C1 C2 1.410(9) . ? C3 C4 1.403(9) . ? C5 C6 1.531(7) . ? C5 C8 1.537(8) . ? C5 C7 1.545(8) . ? C9 C10 1.538(8) . ? C9 C12 1.538(7) . ? C9 C11 1.551(8) . ? C13 C14 1.552(7) . ? C14 C15 1.524(7) . ? C15 C16 1.399(8) . ? C15 C20 1.411(8) . ? C16 C17 1.400(8) . ? C16 C22 1.511(8) . ? C17 C18 1.384(9) . ? C18 C19 1.364(9) . ? C19 C20 1.388(8) . ? C20 C21 1.512(8) . ? C23 C24 1.529(7) . ? C23 C25 1.541(8) . ? C23 C26 1.548(8) . ? C27 C29 1.533(7) . ? C27 C30 1.541(7) . ? C27 C28 1.546(8) . ? C31 C32 1.552(7) . ? C32 C33 1.523(7) . ? C33 C38 1.391(8) . ? C33 C34 1.412(8) . ? C34 C35 1.392(8) . ? C34 C40 1.503(9) . ? C35 C36 1.367(9) . ? C36 C37 1.369(9) . ? C37 C38 1.420(8) . ? C38 C39 1.499(9) . ? 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 C2 Rh1 C1 39.1(2) . . ? C2 Rh1 P1 96.00(17) . . ? C1 Rh1 P1 94.50(17) . . ? C2 Rh1 Cl1 154.18(17) . . ? C1 Rh1 Cl1 159.59(17) . . ? P1 Rh1 Cl1 96.99(6) . . ? C2 Rh1 Cl2 87.30(17) . . ? C1 Rh1 Cl2 87.97(17) . . ? P1 Rh1 Cl2 176.70(4) . . ? Cl1 Rh1 Cl2 80.01(6) . . ? C4 Rh2 C3 38.9(2) . . ? C4 Rh2 P2 94.24(17) . . ? C3 Rh2 P2 95.80(17) . . ? C4 Rh2 Cl2 159.72(16) . . ? C3 Rh2 Cl2 154.35(17) . . ? P2 Rh2 Cl2 97.10(6) . . ? C4 Rh2 Cl1 88.16(17) . . ? C3 Rh2 Cl1 87.44(17) . . ? P2 Rh2 Cl1 176.75(5) . . ? Cl2 Rh2 Cl1 79.98(6) . . ? C13 P1 C9 107.6(2) . . ? C13 P1 C5 103.0(2) . . ? C9 P1 C5 110.4(3) . . ? C13 P1 Rh1 111.47(18) . . ? C9 P1 Rh1 111.02(17) . . ? C5 P1 Rh1 112.97(18) . . ? C31 P2 C27 107.4(2) . . ? C31 P2 C23 103.2(2) . . ? C27 P2 C23 110.7(3) . . ? C31 P2 Rh2 111.47(18) . . ? C27 P2 Rh2 111.16(17) . . ? C23 P2 Rh2 112.54(19) . . ? Rh1 Cl1 Rh2 87.35(5) . . ? Rh2 Cl2 Rh1 87.39(5) . . ? C2 C1 Rh1 70.4(3) . . ? C1 C2 Rh1 70.5(3) . . ? C4 C3 Rh2 70.5(3) . . ? C3 C4 Rh2 70.6(3) . . ? C6 C5 C8 107.9(5) . . ? C6 C5 C7 108.4(5) . . ? C8 C5 C7 107.9(4) . . ? C6 C5 P1 111.8(4) . . ? C8 C5 P1 114.2(4) . . ? C7 C5 P1 106.4(4) . . ? C10 C9 C12 109.1(4) . . ? C10 C9 C11 109.0(4) . . ? C12 C9 C11 106.5(4) . . ? C10 C9 P1 115.4(4) . . ? C12 C9 P1 110.2(4) . . ? C11 C9 P1 106.4(4) . . ? C14 C13 P1 125.2(4) . . ? C15 C14 C13 110.4(4) . . ? C16 C15 C20 119.0(5) . . ? C16 C15 C14 120.8(5) . . ? C20 C15 C14 120.1(5) . . ? C15 C16 C17 119.8(5) . . ? C15 C16 C22 121.4(5) . . ? C17 C16 C22 118.8(6) . . ? C18 C17 C16 120.3(6) . . ? C19 C18 C17 119.9(5) . . ? C18 C19 C20 121.5(6) . . ? C19 C20 C15 119.4(6) . . ? C19 C20 C21 118.0(5) . . ? C15 C20 C21 122.6(5) . . ? C24 C23 C25 108.2(5) . . ? C24 C23 C26 107.4(5) . . ? C25 C23 C26 107.9(5) . . ? C24 C23 P2 112.5(4) . . ? C25 C23 P2 106.9(4) . . ? C26 C23 P2 113.8(4) . . ? C29 C27 C30 106.4(4) . . ? C29 C27 C28 109.0(5) . . ? C30 C27 C28 108.6(5) . . ? C29 C27 P2 107.5(4) . . ? C30 C27 P2 109.9(4) . . ? C28 C27 P2 115.1(4) . . ? C32 C31 P2 125.2(4) . . ? C33 C32 C31 110.3(5) . . ? C38 C33 C34 119.5(5) . . ? C38 C33 C32 120.1(5) . . ? C34 C33 C32 120.4(5) . . ? C35 C34 C33 119.4(5) . . ? C35 C34 C40 118.2(5) . . ? C33 C34 C40 122.5(5) . . ? C36 C35 C34 121.1(6) . . ? C35 C36 C37 120.3(5) . . ? C36 C37 C38 120.5(6) . . ? C33 C38 C37 119.1(5) . . ? C33 C38 C39 122.9(5) . . ? C37 C38 C39 118.0(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C2 Rh1 P1 C13 5.8(3) . . . . ? C1 Rh1 P1 C13 -33.5(2) . . . . ? Cl1 Rh1 P1 C13 163.42(18) . . . . ? Cl2 Rh1 P1 C13 -171.9(8) . . . . ? C2 Rh1 P1 C9 125.7(3) . . . . ? C1 Rh1 P1 C9 86.4(2) . . . . ? Cl1 Rh1 P1 C9 -76.69(19) . . . . ? Cl2 Rh1 P1 C9 -52.0(9) . . . . ? C2 Rh1 P1 C5 -109.6(2) . . . . ? C1 Rh1 P1 C5 -148.9(2) . . . . ? Cl1 Rh1 P1 C5 48.00(18) . . . . ? Cl2 Rh1 P1 C5 72.6(9) . . . . ? C4 Rh2 P2 C31 -33.5(2) . . . . ? C3 Rh2 P2 C31 5.6(3) . . . . ? Cl2 Rh2 P2 C31 163.38(19) . . . . ? Cl1 Rh2 P2 C31 -171.0(8) . . . . ? C4 Rh2 P2 C27 86.3(2) . . . . ? C3 Rh2 P2 C27 125.3(2) . . . . ? Cl2 Rh2 P2 C27 -76.89(18) . . . . ? Cl1 Rh2 P2 C27 -51.3(9) . . . . ? C4 Rh2 P2 C23 -148.9(2) . . . . ? C3 Rh2 P2 C23 -109.8(2) . . . . ? Cl2 Rh2 P2 C23 47.94(19) . . . . ? Cl1 Rh2 P2 C23 73.5(9) . . . . ? C2 Rh1 Cl1 Rh2 -98.3(4) . . . . ? C1 Rh1 Cl1 Rh2 18.3(5) . . . . ? P1 Rh1 Cl1 Rh2 142.06(5) . . . . ? Cl2 Rh1 Cl1 Rh2 -36.54(5) . . . . ? C4 Rh2 Cl1 Rh1 -126.55(17) . . . . ? C3 Rh2 Cl1 Rh1 -165.52(17) . . . . ? P2 Rh2 Cl1 Rh1 11.1(9) . . . . ? Cl2 Rh2 Cl1 Rh1 36.93(5) . . . . ? C4 Rh2 Cl2 Rh1 18.5(5) . . . . ? C3 Rh2 Cl2 Rh1 -98.3(4) . . . . ? P2 Rh2 Cl2 Rh1 142.03(5) . . . . ? Cl1 Rh2 Cl2 Rh1 -36.54(5) . . . . ? C2 Rh1 Cl2 Rh2 -165.63(18) . . . . ? C1 Rh1 Cl2 Rh2 -126.48(17) . . . . ? P1 Rh1 Cl2 Rh2 12.1(8) . . . . ? Cl1 Rh1 Cl2 Rh2 36.95(5) . . . . ? P1 Rh1 C1 C2 94.0(3) . . . . ? Cl1 Rh1 C1 C2 -141.9(4) . . . . ? Cl2 Rh1 C1 C2 -88.2(3) . . . . ? P1 Rh1 C2 C1 -89.8(3) . . . . ? Cl1 Rh1 C2 C1 150.4(3) . . . . ? Cl2 Rh1 C2 C1 90.1(3) . . . . ? P2 Rh2 C3 C4 -89.6(3) . . . . ? Cl2 Rh2 C3 C4 150.5(3) . . . . ? Cl1 Rh2 C3 C4 90.2(3) . . . . ? P2 Rh2 C4 C3 94.0(3) . . . . ? Cl2 Rh2 C4 C3 -142.1(4) . . . . ? Cl1 Rh2 C4 C3 -88.2(3) . . . . ? C13 P1 C5 C6 160.2(4) . . . . ? C9 P1 C5 C6 45.6(5) . . . . ? Rh1 P1 C5 C6 -79.4(4) . . . . ? C13 P1 C5 C8 37.4(5) . . . . ? C9 P1 C5 C8 -77.2(4) . . . . ? Rh1 P1 C5 C8 157.7(4) . . . . ? C13 P1 C5 C7 -81.6(4) . . . . ? C9 P1 C5 C7 163.8(3) . . . . ? Rh1 P1 C5 C7 38.8(4) . . . . ? C13 P1 C9 C10 -68.8(4) . . . . ? C5 P1 C9 C10 42.9(5) . . . . ? Rh1 P1 C9 C10 169.0(3) . . . . ? C13 P1 C9 C12 167.2(4) . . . . ? C5 P1 C9 C12 -81.2(4) . . . . ? Rh1 P1 C9 C12 45.0(4) . . . . ? C13 P1 C9 C11 52.1(4) . . . . ? C5 P1 C9 C11 163.8(3) . . . . ? Rh1 P1 C9 C11 -70.1(3) . . . . ? C9 P1 C13 C14 39.5(5) . . . . ? C5 P1 C13 C14 -77.2(5) . . . . ? Rh1 P1 C13 C14 161.4(4) . . . . ? P1 C13 C14 C15 -177.6(4) . . . . ? C13 C14 C15 C16 92.4(6) . . . . ? C13 C14 C15 C20 -86.2(6) . . . . ? C20 C15 C16 C17 -2.7(9) . . . . ? C14 C15 C16 C17 178.7(5) . . . . ? C20 C15 C16 C22 177.6(6) . . . . ? C14 C15 C16 C22 -1.1(9) . . . . ? C15 C16 C17 C18 1.2(9) . . . . ? C22 C16 C17 C18 -179.0(6) . . . . ? C16 C17 C18 C19 0.7(10) . . . . ? C17 C18 C19 C20 -1.1(10) . . . . ? C18 C19 C20 C15 -0.4(9) . . . . ? C18 C19 C20 C21 -179.6(6) . . . . ? C16 C15 C20 C19 2.3(8) . . . . ? C14 C15 C20 C19 -179.0(5) . . . . ? C16 C15 C20 C21 -178.5(5) . . . . ? C14 C15 C20 C21 0.1(8) . . . . ? C31 P2 C23 C24 160.3(4) . . . . ? C27 P2 C23 C24 45.7(5) . . . . ? Rh2 P2 C23 C24 -79.4(4) . . . . ? C31 P2 C23 C25 -81.2(4) . . . . ? C27 P2 C23 C25 164.2(3) . . . . ? Rh2 P2 C23 C25 39.1(4) . . . . ? C31 P2 C23 C26 37.9(5) . . . . ? C27 P2 C23 C26 -76.7(4) . . . . ? Rh2 P2 C23 C26 158.2(4) . . . . ? C31 P2 C27 C29 52.1(4) . . . . ? C23 P2 C27 C29 164.1(4) . . . . ? Rh2 P2 C27 C29 -70.1(4) . . . . ? C31 P2 C27 C30 167.4(4) . . . . ? C23 P2 C27 C30 -80.6(4) . . . . ? Rh2 P2 C27 C30 45.3(4) . . . . ? C31 P2 C27 C28 -69.5(4) . . . . ? C23 P2 C27 C28 42.5(5) . . . . ? Rh2 P2 C27 C28 168.3(3) . . . . ? C27 P2 C31 C32 39.6(5) . . . . ? C23 P2 C31 C32 -77.5(5) . . . . ? Rh2 P2 C31 C32 161.5(4) . . . . ? P2 C31 C32 C33 -177.7(4) . . . . ? C31 C32 C33 C38 92.8(6) . . . . ? C31 C32 C33 C34 -86.4(6) . . . . ? C38 C33 C34 C35 1.8(9) . . . . ? C32 C33 C34 C35 -178.9(5) . . . . ? C38 C33 C34 C40 -178.6(6) . . . . ? C32 C33 C34 C40 0.7(9) . . . . ? C33 C34 C35 C36 0.2(9) . . . . ? C40 C34 C35 C36 -179.5(6) . . . . ? C34 C35 C36 C37 -2.0(10) . . . . ? C35 C36 C37 C38 1.9(10) . . . . ? C34 C33 C38 C37 -1.9(9) . . . . ? C32 C33 C38 C37 178.8(6) . . . . ? C34 C33 C38 C39 177.8(6) . . . . ? C32 C33 C38 C39 -1.5(10) . . . . ? C36 C37 C38 C33 0.1(10) . . . . ? C36 C37 C38 C39 -179.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 2.000 _refine_diff_density_min -1.529 _refine_diff_density_rms 0.142 #===END data_gc7cb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H31 Cl O2 P Rh' _chemical_formula_weight 472.78 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' 'Cl' 'Cl' 0.1484 0.1585 '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' 'P' 'P' 0.1023 0.0942 '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 7.9221(4) _cell_length_b 8.6663(4) _cell_length_c 16.9724(9) _cell_angle_alpha 90.0310(10) _cell_angle_beta 90.6400(10) _cell_angle_gamma 111.7650(10) _cell_volume 1082.10(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6959 _cell_measurement_theta_min 4.800 _cell_measurement_theta_max 56.270 _exptl_crystal_description block _exptl_crystal_colour light yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.451 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.997 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'SADABS2.0 (Sheldrick 2000)' _exptl_special_details ; Crystals were grown from a saturated solution in pentane at 4 degrees under CO atmosphere. ; _diffrn_ambient_temperature 173(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 Smart Apex with D8-Goniometer' _diffrn_measurement_method 'omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17545 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 26.37 _reflns_number_total 4416 _reflns_number_gt 4309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART-NT V5.6' _computing_cell_refinement 'SAINT-NT V6.0' _computing_data_reduction 'SAINT-NT V6.0' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSHELL in SHELXTL-97' _computing_publication_material 'XSHELL in SHELXTL-97' _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^)+(0.0295P)^2^+0.4618P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary Patterson methods _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_number_reflns 4416 _refine_ls_number_parameters 234 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0210 _refine_ls_wR_factor_ref 0.0546 _refine_ls_wR_factor_gt 0.0542 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 C1 C 0.0992(3) 0.3478(3) 0.45805(12) 0.0474(5) Uani 1 1 d . . . C2 C -0.1828(3) 0.0728(2) 0.44422(11) 0.0389(4) Uani 1 1 d . . . C3 C 0.4492(2) 0.3092(2) 0.30432(10) 0.0299(3) Uani 1 1 d . . . C4 C 0.4974(3) 0.3214(3) 0.39254(12) 0.0425(4) Uani 1 1 d . . . H4A H 0.6050 0.2931 0.4010 0.064 Uiso 1 1 calc R . . H4B H 0.3950 0.2440 0.4218 0.064 Uiso 1 1 calc R . . H4C H 0.5230 0.4351 0.4111 0.064 Uiso 1 1 calc R . . C5 C 0.6160(2) 0.4183(3) 0.25807(13) 0.0430(5) Uani 1 1 d . . . H5A H 0.7141 0.3761 0.2649 0.065 Uiso 1 1 calc R . . H5B H 0.6566 0.5329 0.2777 0.065 Uiso 1 1 calc R . . H5C H 0.5838 0.4157 0.2020 0.065 Uiso 1 1 calc R . . C6 C 0.4016(3) 0.1273(2) 0.27905(13) 0.0406(4) Uani 1 1 d . . . H6A H 0.3863 0.1180 0.2217 0.061 Uiso 1 1 calc R . . H6B H 0.2884 0.0571 0.3041 0.061 Uiso 1 1 calc R . . H6C H 0.5000 0.0909 0.2953 0.061 Uiso 1 1 calc R . . C7 C 0.2983(2) 0.5941(2) 0.29337(10) 0.0290(3) Uani 1 1 d . . . C8 C 0.1164(2) 0.6196(2) 0.30025(11) 0.0342(4) Uani 1 1 d . . . H8A H 0.0554 0.5676 0.3487 0.051 Uiso 1 1 calc R . . H8B H 0.0385 0.5687 0.2547 0.051 Uiso 1 1 calc R . . H8C H 0.1395 0.7388 0.3018 0.051 Uiso 1 1 calc R . . C9 C 0.3971(2) 0.6852(2) 0.21966(11) 0.0352(4) Uani 1 1 d . . . H9A H 0.4236 0.8045 0.2253 0.053 Uiso 1 1 calc R . . H9B H 0.3197 0.6424 0.1730 0.053 Uiso 1 1 calc R . . H9C H 0.5111 0.6668 0.2137 0.053 Uiso 1 1 calc R . . C10 C 0.4168(3) 0.6738(2) 0.36579(12) 0.0390(4) Uani 1 1 d . . . H10A H 0.5388 0.6722 0.3590 0.059 Uiso 1 1 calc R . . H10B H 0.3621 0.6112 0.4131 0.059 Uiso 1 1 calc R . . H10C H 0.4250 0.7890 0.3714 0.059 Uiso 1 1 calc R . . C11 C 0.1845(2) 0.30194(19) 0.18337(9) 0.0247(3) Uani 1 1 d . . . H11A H 0.2965 0.3556 0.1526 0.030 Uiso 1 1 calc R . . H11B H 0.1534 0.1805 0.1794 0.030 Uiso 1 1 calc R . . C12 C 0.0309(2) 0.3410(2) 0.14191(9) 0.0264(3) Uani 1 1 d . . . H12A H -0.0826 0.2909 0.1721 0.032 Uiso 1 1 calc R . . H12B H 0.0630 0.4628 0.1412 0.032 Uiso 1 1 calc R . . C13 C -0.0012(2) 0.2745(2) 0.05780(9) 0.0274(3) Uani 1 1 d . . . C14 C -0.1526(2) 0.1302(2) 0.03838(10) 0.0321(4) Uani 1 1 d . . . C15 C -0.1765(3) 0.0726(2) -0.03943(11) 0.0384(4) Uani 1 1 d . . . H15 H -0.2778 -0.0251 -0.0526 0.046 Uiso 1 1 calc R . . C16 C -0.0567(3) 0.1541(3) -0.09728(11) 0.0427(5) Uani 1 1 d . . . H16 H -0.0747 0.1126 -0.1498 0.051 Uiso 1 1 calc R . . C17 C 0.0898(3) 0.2967(3) -0.07852(11) 0.0393(4) Uani 1 1 d . . . H17 H 0.1723 0.3531 -0.1186 0.047 Uiso 1 1 calc R . . C18 C 0.1192(2) 0.3597(2) -0.00183(10) 0.0312(4) Uani 1 1 d . . . C19 C 0.2767(3) 0.5218(2) 0.01373(11) 0.0364(4) Uani 1 1 d . . . H19A H 0.3348 0.5675 -0.0362 0.055 Uiso 1 1 calc R . . H19B H 0.3655 0.5019 0.0488 0.055 Uiso 1 1 calc R . . H19C H 0.2318 0.6010 0.0386 0.055 Uiso 1 1 calc R . . C20 C -0.2933(3) 0.0382(3) 0.09769(12) 0.0415(4) Uani 1 1 d . . . H20A H -0.2347 0.0024 0.1414 0.062 Uiso 1 1 calc R . . H20B H -0.3847 -0.0594 0.0725 0.062 Uiso 1 1 calc R . . H20C H -0.3521 0.1115 0.1179 0.062 Uiso 1 1 calc R . . Cl1 Cl -0.10565(7) -0.01857(6) 0.28630(3) 0.04394(12) Uani 1 1 d . . . O1 O 0.1470(3) 0.4255(3) 0.51363(11) 0.0825(7) Uani 1 1 d . . . O2 O -0.2991(2) 0.0026(2) 0.48277(11) 0.0675(5) Uani 1 1 d . . . P1 P 0.24113(5) 0.36203(5) 0.28777(2) 0.02227(9) Uani 1 1 d . . . Rh1 Rh 0.010156(16) 0.200423(15) 0.376901(7) 0.02730(5) 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 C1 0.0368(11) 0.0537(12) 0.0358(10) -0.0064(9) 0.0082(8) -0.0020(9) C2 0.0333(10) 0.0429(10) 0.0360(10) 0.0065(8) 0.0031(8) 0.0088(8) C3 0.0225(8) 0.0285(8) 0.0383(9) 0.0010(7) -0.0021(7) 0.0091(7) C4 0.0374(10) 0.0476(11) 0.0445(11) 0.0017(9) -0.0120(8) 0.0183(9) C5 0.0232(9) 0.0453(11) 0.0598(13) 0.0054(9) 0.0074(8) 0.0115(8) C6 0.0345(10) 0.0325(9) 0.0592(12) -0.0030(8) -0.0057(9) 0.0176(8) C7 0.0277(8) 0.0216(7) 0.0349(9) -0.0018(6) -0.0004(7) 0.0058(6) C8 0.0357(10) 0.0285(8) 0.0411(10) -0.0048(7) 0.0014(7) 0.0149(7) C9 0.0334(9) 0.0228(8) 0.0442(10) 0.0042(7) 0.0036(8) 0.0044(7) C10 0.0390(10) 0.0278(9) 0.0438(10) -0.0075(7) -0.0066(8) 0.0050(8) C11 0.0240(8) 0.0248(8) 0.0249(7) 0.0002(6) 0.0019(6) 0.0086(6) C12 0.0240(8) 0.0286(8) 0.0273(8) -0.0013(6) 0.0010(6) 0.0107(6) C13 0.0296(8) 0.0322(8) 0.0266(8) -0.0003(6) -0.0006(6) 0.0187(7) C14 0.0355(9) 0.0334(9) 0.0322(9) -0.0026(7) -0.0052(7) 0.0185(8) C15 0.0475(11) 0.0354(9) 0.0379(10) -0.0081(8) -0.0122(8) 0.0223(9) C16 0.0663(14) 0.0467(11) 0.0280(9) -0.0061(8) -0.0052(9) 0.0359(11) C17 0.0539(12) 0.0474(11) 0.0286(9) 0.0051(8) 0.0072(8) 0.0326(10) C18 0.0358(9) 0.0366(9) 0.0294(8) 0.0035(7) 0.0022(7) 0.0228(8) C19 0.0341(9) 0.0427(10) 0.0357(9) 0.0109(8) 0.0081(7) 0.0179(8) C20 0.0323(10) 0.0420(10) 0.0427(10) -0.0030(8) -0.0040(8) 0.0053(8) Cl1 0.0432(3) 0.0331(2) 0.0390(2) -0.00474(18) 0.0037(2) -0.00509(19) O1 0.0681(12) 0.0929(14) 0.0498(10) -0.0333(10) 0.0127(9) -0.0132(11) O2 0.0507(10) 0.0778(12) 0.0601(10) 0.0256(9) 0.0212(8) 0.0069(9) P1 0.01906(19) 0.02038(19) 0.0252(2) -0.00040(15) 0.00043(15) 0.00477(15) Rh1 0.02324(8) 0.02826(8) 0.02574(8) 0.00104(5) 0.00241(5) 0.00408(6) _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 C1 O1 1.135(3) . ? C1 Rh1 1.826(2) . ? C2 O2 1.116(2) . ? C2 Rh1 1.9112(19) . ? C3 C5 1.534(2) . ? C3 C4 1.535(3) . ? C3 C6 1.538(2) . ? C3 P1 1.8856(17) . ? C7 C10 1.537(2) . ? C7 C9 1.538(2) . ? C7 C8 1.543(2) . ? C7 P1 1.8927(16) . ? C11 C12 1.542(2) . ? C11 P1 1.8493(16) . ? C12 C13 1.522(2) . ? C13 C18 1.407(2) . ? C13 C14 1.410(2) . ? C14 C15 1.397(2) . ? C14 C20 1.503(3) . ? C15 C16 1.374(3) . ? C16 C17 1.380(3) . ? C17 C18 1.395(3) . ? C18 C19 1.514(3) . ? Cl1 Rh1 2.3414(5) . ? P1 Rh1 2.4004(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 O1 C1 Rh1 172.8(2) . . ? O2 C2 Rh1 177.1(2) . . ? C5 C3 C4 109.23(15) . . ? C5 C3 C6 108.42(16) . . ? C4 C3 C6 107.40(15) . . ? C5 C3 P1 114.09(12) . . ? C4 C3 P1 109.64(12) . . ? C6 C3 P1 107.85(12) . . ? C10 C7 C9 108.00(14) . . ? C10 C7 C8 108.34(15) . . ? C9 C7 C8 108.76(14) . . ? C10 C7 P1 112.38(12) . . ? C9 C7 P1 112.49(12) . . ? C8 C7 P1 106.75(11) . . ? C12 C11 P1 119.63(11) . . ? C13 C12 C11 111.75(13) . . ? C18 C13 C14 119.39(16) . . ? C18 C13 C12 119.73(15) . . ? C14 C13 C12 120.87(15) . . ? C15 C14 C13 119.07(17) . . ? C15 C14 C20 118.35(17) . . ? C13 C14 C20 122.56(16) . . ? C16 C15 C14 121.45(19) . . ? C15 C16 C17 119.48(17) . . ? C16 C17 C18 121.29(18) . . ? C17 C18 C13 119.30(18) . . ? C17 C18 C19 118.51(17) . . ? C13 C18 C19 122.15(16) . . ? C11 P1 C3 101.96(7) . . ? C11 P1 C7 106.36(7) . . ? C3 P1 C7 111.42(8) . . ? C11 P1 Rh1 113.17(5) . . ? C3 P1 Rh1 108.37(6) . . ? C7 P1 Rh1 114.85(6) . . ? C1 Rh1 C2 88.19(9) . . ? C1 Rh1 Cl1 171.60(8) . . ? C2 Rh1 Cl1 86.43(6) . . ? C1 Rh1 P1 93.31(6) . . ? C2 Rh1 P1 177.08(6) . . ? Cl1 Rh1 P1 92.354(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag P1 C11 C12 C13 -177.18(11) . . . . ? C11 C12 C13 C18 -77.11(18) . . . . ? C11 C12 C13 C14 104.23(17) . . . . ? C18 C13 C14 C15 1.8(2) . . . . ? C12 C13 C14 C15 -179.55(15) . . . . ? C18 C13 C14 C20 -176.31(16) . . . . ? C12 C13 C14 C20 2.3(2) . . . . ? C13 C14 C15 C16 -0.5(3) . . . . ? C20 C14 C15 C16 177.67(17) . . . . ? C14 C15 C16 C17 -0.5(3) . . . . ? C15 C16 C17 C18 0.2(3) . . . . ? C16 C17 C18 C13 1.1(3) . . . . ? C16 C17 C18 C19 -176.66(16) . . . . ? C14 C13 C18 C17 -2.1(2) . . . . ? C12 C13 C18 C17 179.25(15) . . . . ? C14 C13 C18 C19 175.59(15) . . . . ? C12 C13 C18 C19 -3.1(2) . . . . ? C12 C11 P1 C3 -173.81(12) . . . . ? C12 C11 P1 C7 -56.99(14) . . . . ? C12 C11 P1 Rh1 70.02(13) . . . . ? C5 C3 P1 C11 67.23(15) . . . . ? C4 C3 P1 C11 -169.91(12) . . . . ? C6 C3 P1 C11 -53.27(14) . . . . ? C5 C3 P1 C7 -45.87(16) . . . . ? C4 C3 P1 C7 76.99(14) . . . . ? C6 C3 P1 C7 -166.37(12) . . . . ? C5 C3 P1 Rh1 -173.16(12) . . . . ? C4 C3 P1 Rh1 -50.30(13) . . . . ? C6 C3 P1 Rh1 66.34(13) . . . . ? C10 C7 P1 C11 -157.65(13) . . . . ? C9 C7 P1 C11 -35.50(14) . . . . ? C8 C7 P1 C11 83.72(12) . . . . ? C10 C7 P1 C3 -47.34(15) . . . . ? C9 C7 P1 C3 74.81(14) . . . . ? C8 C7 P1 C3 -165.97(11) . . . . ? C10 C7 P1 Rh1 76.35(13) . . . . ? C9 C7 P1 Rh1 -161.50(10) . . . . ? C8 C7 P1 Rh1 -42.28(13) . . . . ? O1 C1 Rh1 C2 30.9(18) . . . . ? O1 C1 Rh1 Cl1 -19(2) . . . . ? O1 C1 Rh1 P1 -151.6(18) . . . . ? O2 C2 Rh1 C1 82(4) . . . . ? O2 C2 Rh1 Cl1 -105(4) . . . . ? O2 C2 Rh1 P1 -39(5) . . . . ? C11 P1 Rh1 C1 -163.65(10) . . . . ? C3 P1 Rh1 C1 84.04(10) . . . . ? C7 P1 Rh1 C1 -41.26(10) . . . . ? C11 P1 Rh1 C2 -42.7(12) . . . . ? C3 P1 Rh1 C2 -155.0(12) . . . . ? C7 P1 Rh1 C2 79.7(12) . . . . ? C11 P1 Rh1 Cl1 22.55(6) . . . . ? C3 P1 Rh1 Cl1 -89.76(6) . . . . ? C7 P1 Rh1 Cl1 144.94(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.596 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.054