Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Piet W. N. M. van Leeuwen' _publ_contact_author_address ; Insititute of Chemical Research of Catalonia Paisos Catalans 16 Tarragona 43007 SPAIN ; _publ_contact_author_email PVANLEEUWEN@ICIQ.ES _publ_section_title ; SPANphos: trans-spanning diphosphines as cia chelating ligands ; loop_ _publ_author_name 'P.W.N.M.van Leeuwen' 'Jordi Benet-Buchholz' 'Carles Bo' 'Eduardo Escudero-Adan' ; Z.Freixa ; 'Cristina Jimenez-Rodriguez' 'Francesc X. Roca' # Attachment 'B513870C-SPANphos cis.cif' data_cj24_0m _database_code_depnum_ccdc_archive 'CCDC 286677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H78 B F4 O5 P2 Rh' _chemical_formula_weight 1202.94 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' O O 0.0106 0.0060 '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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3904(5) _cell_length_b 19.1948(8) _cell_length_c 24.8906(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.6620(10) _cell_angle_gamma 90.00 _cell_volume 5907.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8394 _cell_measurement_theta_min 2.68 _cell_measurement_theta_max 39.37 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.353 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2520 _exptl_absorpt_coefficient_mu 0.406 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7228 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 120149 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 39.54 _reflns_number_total 31008 _reflns_number_gt 25525 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. the THF molecules localized are highly disordered. ; _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^)+(0.0521P)^2^+3.1715P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 31008 _refine_ls_number_parameters 847 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1076 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.006 _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 0.209371(7) 0.721859(4) 0.298422(3) 0.01271(2) Uani 1 1 d . . . P1 P 0.04187(2) 0.683284(14) 0.320272(10) 0.01278(5) Uani 1 1 d . . . O1 O 0.10202(7) 0.78009(4) 0.41480(3) 0.01491(14) Uani 1 1 d . . . C1 C 0.15023(10) 0.84829(5) 0.42242(4) 0.01478(17) Uani 1 1 d . . . P2 P 0.15395(2) 0.826785(14) 0.256903(10) 0.01228(5) Uani 1 1 d . . . C2 C 0.07862(10) 0.89701(6) 0.45450(4) 0.01668(19) Uani 1 1 d . . . H2A H 0.1228 0.9159 0.4857 0.020 Uiso 1 1 calc R . . H2B H 0.0552 0.9368 0.4312 0.020 Uiso 1 1 calc R . . O2 O 0.15312(7) 0.87478(5) 0.36835(3) 0.01648(14) Uani 1 1 d . . . C3 C -0.02231(10) 0.86157(6) 0.47508(4) 0.01581(18) Uani 1 1 d . . . C4 C -0.07529(10) 0.82519(5) 0.42632(4) 0.01495(17) Uani 1 1 d . . . C5 C -0.18229(10) 0.83333(6) 0.40716(5) 0.01775(19) Uani 1 1 d . . . H5 H -0.2285 0.8630 0.4259 0.021 Uiso 1 1 calc R . . C6 C -0.22323(10) 0.79867(6) 0.36081(5) 0.01765(19) Uani 1 1 d . . . C7 C -0.15496(10) 0.75376(6) 0.33482(4) 0.01621(18) Uani 1 1 d . . . H7 H -0.1829 0.7287 0.3041 0.019 Uiso 1 1 calc R . . C8 C -0.04651(9) 0.74448(5) 0.35267(4) 0.01401(17) Uani 1 1 d . . . C9 C -0.00685(9) 0.78334(5) 0.39730(4) 0.01367(16) Uani 1 1 d . . . C10 C 0.00860(12) 0.80850(6) 0.52027(5) 0.0207(2) Uani 1 1 d . . . H10A H -0.0573 0.7884 0.5337 0.031 Uiso 1 1 calc R . . H10B H 0.0499 0.8322 0.5498 0.031 Uiso 1 1 calc R . . H10C H 0.0527 0.7713 0.5060 0.031 Uiso 1 1 calc R . . C11 C -0.09410(11) 0.91739(6) 0.49831(5) 0.0218(2) Uani 1 1 d . . . H11A H -0.1175 0.9504 0.4699 0.033 Uiso 1 1 calc R . . H11B H -0.0531 0.9422 0.5274 0.033 Uiso 1 1 calc R . . H11C H -0.1576 0.8953 0.5126 0.033 Uiso 1 1 calc R . . C12 C -0.33887(12) 0.80914(8) 0.34015(6) 0.0256(2) Uani 1 1 d . . . H12A H -0.3481 0.7932 0.3027 0.038 Uiso 1 1 calc R . . H12B H -0.3573 0.8587 0.3419 0.038 Uiso 1 1 calc R . . H12C H -0.3866 0.7823 0.3623 0.038 Uiso 1 1 calc R . . C13 C 0.26330(10) 0.83817(6) 0.44823(4) 0.01698(18) Uani 1 1 d . . . H13A H 0.2942 0.7951 0.4337 0.020 Uiso 1 1 calc R . . H13B H 0.2584 0.8316 0.4874 0.020 Uiso 1 1 calc R . . C14 C 0.34183(10) 0.89972(6) 0.43903(4) 0.01749(19) Uani 1 1 d . . . C15 C 0.34100(9) 0.91077(5) 0.37863(4) 0.01498(17) Uani 1 1 d . . . C16 C 0.42890(10) 0.93702(6) 0.35243(5) 0.01682(18) Uani 1 1 d . . . H16 H 0.4909 0.9529 0.3733 0.020 Uiso 1 1 calc R . . C17 C 0.42776(10) 0.94054(6) 0.29649(5) 0.01705(18) Uani 1 1 d . . . C18 C 0.33925(9) 0.91284(5) 0.26605(4) 0.01528(17) Uani 1 1 d . . . H18 H 0.3407 0.9110 0.2280 0.018 Uiso 1 1 calc R . . C19 C 0.24852(9) 0.88781(5) 0.29062(4) 0.01295(16) Uani 1 1 d . . . C20 C 0.24889(9) 0.89159(5) 0.34700(4) 0.01329(16) Uani 1 1 d . . . C21 C 0.31183(12) 0.96929(7) 0.46555(5) 0.0245(2) Uani 1 1 d . . . H21A H 0.3687 1.0037 0.4605 0.037 Uiso 1 1 calc R . . H21B H 0.3047 0.9619 0.5041 0.037 Uiso 1 1 calc R . . H21C H 0.2431 0.9863 0.4489 0.037 Uiso 1 1 calc R . . C22 C 0.45368(12) 0.87688(9) 0.46273(6) 0.0278(3) Uani 1 1 d . . . H22A H 0.4771 0.8354 0.4437 0.042 Uiso 1 1 calc R . . H22B H 0.4496 0.8660 0.5010 0.042 Uiso 1 1 calc R . . H22C H 0.5058 0.9146 0.4587 0.042 Uiso 1 1 calc R . . C23 C 0.52119(12) 0.97128(9) 0.26887(6) 0.0293(3) Uani 1 1 d . . . H23A H 0.4995 1.0161 0.2527 0.044 Uiso 1 1 calc R . . H23B H 0.5425 0.9394 0.2407 0.044 Uiso 1 1 calc R . . H23C H 0.5824 0.9783 0.2952 0.044 Uiso 1 1 calc R . . C24 C 0.05244(10) 0.60970(5) 0.36742(4) 0.01529(17) Uani 1 1 d . . . C25 C 0.06182(11) 0.61941(6) 0.42338(4) 0.0192(2) Uani 1 1 d . . . H25 H 0.0575 0.6650 0.4379 0.023 Uiso 1 1 calc R . . C26 C 0.07747(13) 0.56253(7) 0.45759(5) 0.0241(2) Uani 1 1 d . . . H26 H 0.0835 0.5696 0.4954 0.029 Uiso 1 1 calc R . . C27 C 0.08433(13) 0.49564(7) 0.43703(5) 0.0263(3) Uani 1 1 d . . . H27 H 0.0947 0.4571 0.4607 0.032 Uiso 1 1 calc R . . C28 C 0.07602(13) 0.48525(6) 0.38163(5) 0.0248(2) Uani 1 1 d . . . H28 H 0.0808 0.4395 0.3674 0.030 Uiso 1 1 calc R . . C29 C 0.06063(11) 0.54200(6) 0.34709(5) 0.0199(2) Uani 1 1 d . . . H29 H 0.0556 0.5347 0.3093 0.024 Uiso 1 1 calc R . . C30 C -0.03847(10) 0.64368(6) 0.26441(4) 0.01595(18) Uani 1 1 d . . . C31 C -0.13645(11) 0.60948(6) 0.27152(5) 0.0211(2) Uani 1 1 d . . . H31 H -0.1653 0.6092 0.3060 0.025 Uiso 1 1 calc R . . C32 C -0.19160(13) 0.57606(7) 0.22859(6) 0.0275(3) Uani 1 1 d . . . H32 H -0.2588 0.5539 0.2335 0.033 Uiso 1 1 calc R . . C33 C -0.14828(15) 0.57508(8) 0.17826(6) 0.0322(3) Uani 1 1 d . . . H33 H -0.1863 0.5525 0.1488 0.039 Uiso 1 1 calc R . . C34 C -0.04990(15) 0.60691(8) 0.17101(5) 0.0294(3) Uani 1 1 d . . . H34 H -0.0197 0.6052 0.1369 0.035 Uiso 1 1 calc R . . C35 C 0.00466(12) 0.64146(6) 0.21387(4) 0.0203(2) Uani 1 1 d . . . H35 H 0.0717 0.6637 0.2087 0.024 Uiso 1 1 calc R . . C36 C 0.01737(10) 0.86268(6) 0.25423(4) 0.01576(18) Uani 1 1 d . . . C37 C -0.06047(11) 0.82964(7) 0.21968(5) 0.0219(2) Uani 1 1 d . . . H37 H -0.0412 0.7899 0.1997 0.026 Uiso 1 1 calc R . . C38 C -0.16577(12) 0.85501(9) 0.21466(6) 0.0292(3) Uani 1 1 d . . . H38 H -0.2184 0.8328 0.1911 0.035 Uiso 1 1 calc R . . C39 C -0.19388(13) 0.91320(9) 0.24434(7) 0.0322(3) Uani 1 1 d . . . H39 H -0.2658 0.9306 0.2408 0.039 Uiso 1 1 calc R . . C40 C -0.11785(13) 0.94573(8) 0.27879(6) 0.0287(3) Uani 1 1 d . . . H40 H -0.1377 0.9849 0.2993 0.034 Uiso 1 1 calc R . . C41 C -0.01184(11) 0.92095(7) 0.28343(5) 0.0208(2) Uani 1 1 d . . . H41 H 0.0407 0.9439 0.3066 0.025 Uiso 1 1 calc R . . C42 C 0.18153(10) 0.83306(6) 0.18573(4) 0.01579(18) Uani 1 1 d . . . C43 C 0.20971(11) 0.77451(6) 0.15638(5) 0.0194(2) Uani 1 1 d . . . H43 H 0.2163 0.7304 0.1737 0.023 Uiso 1 1 calc R . . C44 C 0.22828(14) 0.78032(8) 0.10188(5) 0.0269(3) Uani 1 1 d . . . H44 H 0.2471 0.7403 0.0821 0.032 Uiso 1 1 calc R . . C45 C 0.21920(15) 0.84465(9) 0.07675(5) 0.0330(3) Uani 1 1 d . . . H45 H 0.2331 0.8488 0.0398 0.040 Uiso 1 1 calc R . . C46 C 0.18983(14) 0.90326(8) 0.10540(5) 0.0298(3) Uani 1 1 d . . . H46 H 0.1833 0.9472 0.0879 0.036 Uiso 1 1 calc R . . C47 C 0.17003(12) 0.89764(7) 0.15954(5) 0.0209(2) Uani 1 1 d . . . H47 H 0.1487 0.9375 0.1788 0.025 Uiso 1 1 calc R . . C48 C 0.28420(11) 0.61979(6) 0.29519(5) 0.0197(2) Uani 1 1 d . . . H48 H 0.2423 0.5764 0.2860 0.024 Uiso 1 1 calc R . . C49 C 0.30042(11) 0.64484(6) 0.34759(5) 0.0190(2) Uani 1 1 d . . . H49 H 0.2707 0.6213 0.3793 0.023 Uiso 1 1 calc R . . C50 C 0.41032(11) 0.68251(6) 0.35053(5) 0.0188(2) Uani 1 1 d . . . H50 H 0.4457 0.6911 0.3872 0.023 Uiso 1 1 calc R . . C51 C 0.47287(12) 0.63699(7) 0.31151(5) 0.0227(2) Uani 1 1 d . . . H51A H 0.5421 0.6582 0.3022 0.027 Uiso 1 1 calc R . . H51B H 0.4848 0.5887 0.3246 0.027 Uiso 1 1 calc R . . C52 C 0.38318(11) 0.64229(7) 0.26534(5) 0.0213(2) Uani 1 1 d . . . H52 H 0.3961 0.6176 0.2310 0.026 Uiso 1 1 calc R . . C53 C 0.36937(10) 0.72212(6) 0.26264(5) 0.01823(19) Uani 1 1 d . . . H53 H 0.3852 0.7505 0.2304 0.022 Uiso 1 1 calc R . . C54 C 0.38555(10) 0.74633(6) 0.31480(5) 0.01767(19) Uani 1 1 d . . . H54 H 0.4132 0.7941 0.3239 0.021 Uiso 1 1 calc R . . B1 B 0.24720(17) 0.56656(9) 0.11426(6) 0.0291(3) Uani 1 1 d . . . F1 F 0.23859(10) 0.59109(7) 0.16635(4) 0.0426(3) Uani 1 1 d . . . F3 F 0.31047(10) 0.50721(6) 0.11412(5) 0.0447(3) Uani 1 1 d . . . F2 F 0.14426(11) 0.55063(8) 0.09198(5) 0.0517(3) Uani 1 1 d . . . F4 F 0.28912(15) 0.61807(7) 0.08261(5) 0.0622(4) Uani 1 1 d . . . O1X O 0.6787(3) 0.6192(2) 0.41288(11) 0.0403(10) Uani 0.459(6) 1 d PD A 1 C1X C 0.6080(6) 0.6486(5) 0.4435(4) 0.0499(19) Uani 0.459(6) 1 d PD A 1 H1XA H 0.5677 0.6131 0.4630 0.060 Uiso 0.459(6) 1 calc PR A 1 H1XB H 0.5560 0.6780 0.4219 0.060 Uiso 0.459(6) 1 calc PR A 1 C2X C 0.6730(11) 0.6882(6) 0.4785(5) 0.125(5) Uani 0.459(6) 1 d PD A 1 H2XA H 0.6480 0.6842 0.5154 0.150 Uiso 0.459(6) 1 calc PR A 1 H2XB H 0.6687 0.7378 0.4676 0.150 Uiso 0.459(6) 1 calc PR A 1 C3X C 0.7922(5) 0.6621(3) 0.4777(3) 0.0454(17) Uani 0.459(6) 1 d PD A 1 H3XA H 0.8372 0.6935 0.4569 0.054 Uiso 0.459(6) 1 calc PR A 1 H3XB H 0.8263 0.6557 0.5144 0.054 Uiso 0.459(6) 1 calc PR A 1 C4X C 0.7710(4) 0.59621(18) 0.4505(2) 0.0296(10) Uani 0.459(6) 1 d PD A 1 H4XA H 0.7494 0.5594 0.4755 0.035 Uiso 0.459(6) 1 calc PR A 1 H4XB H 0.8337 0.5802 0.4310 0.035 Uiso 0.459(6) 1 calc PR A 1 O1X' O 0.6434(14) 0.6237(13) 0.4227(9) 0.57(3) Uani 0.541(6) 1 d PD A 2 C1X' C 0.6124(5) 0.6766(4) 0.4418(3) 0.0437(14) Uani 0.541(6) 1 d PD A 2 H1XC H 0.5369 0.6696 0.4514 0.052 Uiso 0.541(6) 1 calc PR A 2 H1XD H 0.6116 0.7132 0.4138 0.052 Uiso 0.541(6) 1 calc PR A 2 C2X' C 0.6717(5) 0.7005(4) 0.4865(2) 0.0487(14) Uani 0.541(6) 1 d PD A 2 H2XC H 0.6328 0.6911 0.5193 0.058 Uiso 0.541(6) 1 calc PR A 2 H2XD H 0.6831 0.7514 0.4838 0.058 Uiso 0.541(6) 1 calc PR A 2 C3X' C 0.7758(8) 0.6641(4) 0.4895(5) 0.102(4) Uani 0.541(6) 1 d PD A 2 H3XC H 0.7910 0.6446 0.5260 0.123 Uiso 0.541(6) 1 calc PR A 2 H3XD H 0.8345 0.6970 0.4820 0.123 Uiso 0.541(6) 1 calc PR A 2 C4X' C 0.7704(9) 0.6073(7) 0.4489(4) 0.117(4) Uani 0.541(6) 1 d PD A 2 H4XC H 0.7770 0.5605 0.4656 0.141 Uiso 0.541(6) 1 calc PR A 2 H4XD H 0.8252 0.6127 0.4219 0.141 Uiso 0.541(6) 1 calc PR A 2 C2Y C 0.5254(6) 0.4297(4) 0.4354(3) 0.171(3) Uani 1 1 d DU B 2 H2YA H 0.5185 0.3944 0.4623 0.205 Uiso 1 1 d R B 2 H2YB H 0.5910 0.4553 0.4436 0.205 Uiso 1 1 d R B 2 O1Y O 0.3606(14) 0.4523(11) 0.3827(8) 0.369(13) Uani 0.563(5) 1 d PD C 1 C1Y C 0.4272(4) 0.4775(3) 0.4324(2) 0.0515(11) Uani 0.563(5) 1 d PD C 1 H1YA H 0.3898 0.4749 0.4649 0.062 Uiso 0.563(5) 1 d PR C 1 H1YB H 0.4494 0.5248 0.4272 0.062 Uiso 0.563(5) 1 d PR C 1 C3Y C 0.5224(5) 0.3968(5) 0.3792(3) 0.108(3) Uani 0.563(5) 1 d PD C 1 H3YA H 0.5482 0.3496 0.3811 0.130 Uiso 0.563(5) 1 d PR C 1 H3YB H 0.5679 0.4231 0.3568 0.130 Uiso 0.563(5) 1 d PR C 1 C4Y C 0.4138(3) 0.4002(3) 0.35711(19) 0.0573(13) Uani 0.563(5) 1 d PD C 1 H4YA H 0.4128 0.4100 0.3180 0.069 Uiso 0.563(5) 1 calc PR C 1 H4YB H 0.3772 0.3550 0.3622 0.069 Uiso 0.563(5) 1 calc PR C 1 O1Y' O 0.3761(5) 0.4551(2) 0.38538(14) 0.0707(18) Uani 0.437(5) 1 d PD B 2 C4Y' C 0.4089(4) 0.5069(2) 0.43281(17) 0.0318(8) Uani 0.437(5) 1 d PDU B 2 H4YC H 0.3456 0.5201 0.4507 0.038 Uiso 0.437(5) 1 d PR C 2 H4YD H 0.4378 0.5484 0.4177 0.038 Uiso 0.437(5) 1 d PR C 2 C3Y' C 0.4927(3) 0.47764(18) 0.47503(13) 0.0284(8) Uani 0.437(5) 1 d PD . 2 H3YC H 0.4636 0.4542 0.5050 0.034 Uiso 0.437(5) 1 d PR C 2 H3YD H 0.5507 0.5087 0.4859 0.034 Uiso 0.437(5) 1 d PR C 2 C1Y' C 0.4818(19) 0.443(2) 0.3713(7) 0.52(4) Uani 0.437(5) 1 d PD B 2 H1YC H 0.5156 0.4724 0.3444 0.629 Uiso 0.437(5) 1 d PR C 2 H1YD H 0.4642 0.3956 0.3575 0.629 Uiso 0.437(5) 1 d PR C 2 O1Z O 0.3661(5) 0.2177(2) 0.31503(19) 0.0629(14) Uani 0.410(4) 1 d PD D 1 C1Z C 0.4233(4) 0.1510(3) 0.3141(2) 0.0411(11) Uani 0.410(4) 1 d PD D 1 H1ZA H 0.5014 0.1540 0.3080 0.049 Uiso 0.410(4) 1 calc PR D 1 H1ZB H 0.3862 0.1139 0.2924 0.049 Uiso 0.410(4) 1 calc PR D 1 C2Z C 0.3914(7) 0.1554(4) 0.3802(4) 0.077(3) Uani 0.410(4) 1 d PD D 1 H2ZA H 0.3622 0.1106 0.3926 0.093 Uiso 0.410(4) 1 calc PR D 1 H2ZB H 0.4548 0.1689 0.4042 0.093 Uiso 0.410(4) 1 calc PR D 1 C3Z C 0.3023(7) 0.2141(3) 0.3772(3) 0.057(2) Uani 0.410(4) 1 d PD D 1 H3ZA H 0.2506 0.2066 0.3458 0.068 Uiso 0.410(4) 1 d PR D 1 H3ZB H 0.2620 0.2114 0.4102 0.068 Uiso 0.410(4) 1 d PR D 1 C4Z C 0.3489(5) 0.2771(2) 0.3735(3) 0.0402(12) Uani 0.410(4) 1 d PD D 1 H4ZA H 0.4137 0.2866 0.3977 0.048 Uiso 0.410(4) 1 calc PR D 1 H4ZB H 0.3003 0.3177 0.3673 0.048 Uiso 0.410(4) 1 calc PR D 1 O1Z' O 0.5454(7) 0.7644(4) 0.1399(6) 0.264(7) Uani 0.590(4) 1 d PD D 2 C1Z' C 0.5344(9) 0.6911(4) 0.1585(5) 0.193(7) Uani 0.590(4) 1 d PD D 2 H1ZC H 0.4797 0.7005 0.1831 0.231 Uiso 0.590(4) 1 d PR D 2 H1ZD H 0.5959 0.6723 0.1791 0.231 Uiso 0.590(4) 1 d PR D 2 C2Z' C 0.5392(8) 0.6395(5) 0.1322(3) 0.136(4) Uani 0.590(4) 1 d PD D 2 H2ZC H 0.4686 0.6256 0.1145 0.163 Uiso 0.590(4) 1 calc PR D 2 H2ZD H 0.5728 0.5998 0.1524 0.163 Uiso 0.590(4) 1 calc PR D 2 C3Z' C 0.6137(8) 0.6728(4) 0.0939(3) 0.130(4) Uani 0.590(4) 1 d PD D 2 H3ZC H 0.5976 0.6837 0.0566 0.156 Uiso 0.590(4) 1 d PR D 2 H3ZD H 0.6559 0.6308 0.0949 0.156 Uiso 0.590(4) 1 d PR D 2 C4Z' C 0.6619(7) 0.7368(7) 0.1247(4) 0.147(5) Uani 0.590(4) 1 d PD D 2 H4ZC H 0.6993 0.7695 0.1013 0.176 Uiso 0.590(4) 1 calc PR D 2 H4ZD H 0.7096 0.7241 0.1566 0.176 Uiso 0.590(4) 1 calc PR D 2 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 0.01201(4) 0.01101(3) 0.01488(3) -0.00001(2) -0.00103(2) 0.00023(2) P1 0.01427(13) 0.01206(10) 0.01187(9) -0.00136(7) -0.00027(8) -0.00167(8) O1 0.0136(4) 0.0137(3) 0.0171(3) -0.0043(2) -0.0008(3) -0.0003(2) C1 0.0157(5) 0.0152(4) 0.0134(3) -0.0021(3) 0.0005(3) -0.0017(3) P2 0.01173(13) 0.01234(10) 0.01260(9) 0.00011(7) -0.00049(8) 0.00010(8) C2 0.0185(5) 0.0147(4) 0.0172(4) -0.0044(3) 0.0039(4) -0.0015(3) O2 0.0118(4) 0.0247(4) 0.0129(3) -0.0001(3) 0.0005(3) -0.0015(3) C3 0.0175(5) 0.0147(4) 0.0156(4) -0.0028(3) 0.0037(3) 0.0001(3) C4 0.0157(5) 0.0138(4) 0.0156(4) -0.0013(3) 0.0023(3) 0.0000(3) C5 0.0163(5) 0.0170(4) 0.0202(4) -0.0007(3) 0.0030(4) 0.0016(3) C6 0.0138(5) 0.0182(4) 0.0209(4) 0.0011(3) 0.0009(4) 0.0006(3) C7 0.0156(5) 0.0162(4) 0.0167(4) 0.0001(3) -0.0002(3) -0.0016(3) C8 0.0144(5) 0.0129(4) 0.0147(4) -0.0011(3) 0.0009(3) -0.0013(3) C9 0.0132(5) 0.0133(4) 0.0145(3) -0.0011(3) 0.0008(3) -0.0008(3) C10 0.0266(6) 0.0198(5) 0.0159(4) -0.0002(3) 0.0027(4) -0.0003(4) C11 0.0229(6) 0.0194(5) 0.0238(5) -0.0060(4) 0.0066(4) 0.0019(4) C12 0.0157(6) 0.0297(6) 0.0309(6) 0.0006(5) -0.0016(5) 0.0028(4) C13 0.0169(5) 0.0184(4) 0.0153(4) -0.0019(3) -0.0022(3) -0.0010(3) C14 0.0152(5) 0.0210(4) 0.0158(4) -0.0038(3) -0.0021(3) -0.0025(4) C15 0.0132(5) 0.0147(4) 0.0168(4) -0.0031(3) -0.0007(3) -0.0003(3) C16 0.0129(5) 0.0157(4) 0.0216(4) -0.0019(3) -0.0008(4) -0.0019(3) C17 0.0133(5) 0.0155(4) 0.0224(4) 0.0017(3) 0.0012(4) -0.0020(3) C18 0.0140(5) 0.0144(4) 0.0176(4) 0.0017(3) 0.0017(3) -0.0003(3) C19 0.0119(5) 0.0123(3) 0.0145(3) -0.0001(3) 0.0005(3) 0.0003(3) C20 0.0120(5) 0.0131(4) 0.0147(3) -0.0016(3) 0.0005(3) -0.0001(3) C21 0.0284(7) 0.0236(5) 0.0219(5) -0.0098(4) 0.0042(5) -0.0090(5) C22 0.0192(7) 0.0386(7) 0.0245(5) 0.0024(5) -0.0074(5) -0.0041(5) C23 0.0188(7) 0.0376(7) 0.0315(6) 0.0096(5) 0.0014(5) -0.0116(5) C24 0.0183(5) 0.0138(4) 0.0137(4) -0.0004(3) 0.0004(3) -0.0012(3) C25 0.0257(6) 0.0172(4) 0.0145(4) -0.0003(3) 0.0000(4) -0.0021(4) C26 0.0334(7) 0.0229(5) 0.0157(4) 0.0034(4) -0.0014(4) -0.0020(5) C27 0.0360(8) 0.0195(5) 0.0227(5) 0.0062(4) -0.0024(5) -0.0014(5) C28 0.0357(8) 0.0144(4) 0.0242(5) 0.0017(4) 0.0006(5) 0.0005(4) C29 0.0283(6) 0.0142(4) 0.0170(4) -0.0008(3) 0.0007(4) -0.0005(4) C30 0.0189(5) 0.0141(4) 0.0145(4) -0.0017(3) -0.0021(3) -0.0029(3) C31 0.0214(6) 0.0169(4) 0.0246(5) -0.0017(4) -0.0010(4) -0.0052(4) C32 0.0240(7) 0.0203(5) 0.0367(7) -0.0041(5) -0.0100(5) -0.0060(4) C33 0.0416(9) 0.0250(6) 0.0276(6) -0.0066(5) -0.0157(6) -0.0049(6) C34 0.0445(9) 0.0273(6) 0.0155(4) -0.0051(4) -0.0061(5) -0.0028(6) C35 0.0272(6) 0.0191(4) 0.0143(4) -0.0020(3) -0.0006(4) -0.0032(4) C36 0.0130(5) 0.0165(4) 0.0176(4) 0.0032(3) -0.0005(3) 0.0009(3) C37 0.0178(6) 0.0225(5) 0.0247(5) 0.0047(4) -0.0045(4) -0.0022(4) C38 0.0153(7) 0.0373(7) 0.0341(7) 0.0125(5) -0.0065(5) -0.0031(5) C39 0.0170(7) 0.0449(8) 0.0350(7) 0.0165(6) 0.0048(5) 0.0100(5) C40 0.0251(7) 0.0348(7) 0.0269(6) 0.0073(5) 0.0071(5) 0.0156(5) C41 0.0206(6) 0.0222(5) 0.0198(4) 0.0015(4) 0.0013(4) 0.0068(4) C42 0.0162(5) 0.0182(4) 0.0128(3) 0.0000(3) -0.0004(3) -0.0001(3) C43 0.0217(6) 0.0205(5) 0.0159(4) -0.0023(3) 0.0000(4) 0.0000(4) C44 0.0335(8) 0.0318(6) 0.0153(4) -0.0048(4) 0.0013(5) 0.0026(5) C45 0.0440(10) 0.0405(8) 0.0145(4) 0.0032(5) 0.0029(5) 0.0063(7) C46 0.0408(9) 0.0316(6) 0.0170(5) 0.0077(4) 0.0009(5) 0.0046(6) C47 0.0248(6) 0.0213(5) 0.0163(4) 0.0033(3) -0.0012(4) 0.0025(4) C48 0.0199(6) 0.0133(4) 0.0252(5) -0.0019(3) -0.0049(4) 0.0018(3) C49 0.0190(6) 0.0163(4) 0.0211(4) 0.0031(3) -0.0031(4) 0.0020(4) C50 0.0170(6) 0.0186(4) 0.0202(4) -0.0015(3) -0.0041(4) 0.0032(4) C51 0.0195(6) 0.0212(5) 0.0269(5) -0.0023(4) -0.0024(4) 0.0075(4) C52 0.0198(6) 0.0209(5) 0.0228(5) -0.0057(4) -0.0020(4) 0.0059(4) C53 0.0140(5) 0.0203(4) 0.0204(4) 0.0009(3) 0.0010(4) 0.0026(3) C54 0.0125(5) 0.0162(4) 0.0240(5) -0.0019(3) -0.0011(4) 0.0014(3) B1 0.0404(10) 0.0275(7) 0.0195(5) 0.0012(5) 0.0019(6) 0.0028(6) F1 0.0502(7) 0.0578(7) 0.0198(4) -0.0104(4) 0.0024(4) -0.0157(5) F3 0.0436(7) 0.0426(6) 0.0473(6) 0.0091(5) -0.0025(5) 0.0155(5) F2 0.0465(7) 0.0657(8) 0.0402(6) -0.0208(5) -0.0180(5) 0.0183(6) F4 0.1098(12) 0.0363(6) 0.0444(6) 0.0077(5) 0.0355(7) -0.0013(7) O1X 0.0194(14) 0.073(2) 0.0274(12) 0.0242(12) -0.0083(9) -0.0117(12) C1X 0.015(2) 0.083(5) 0.050(3) -0.002(4) -0.0098(19) 0.014(3) C2X 0.158(9) 0.065(5) 0.169(10) 0.052(5) 0.134(8) 0.055(6) C3X 0.030(2) 0.035(3) 0.070(4) 0.033(3) -0.003(2) 0.0006(17) C4X 0.023(2) 0.0165(11) 0.047(2) 0.0128(12) -0.0203(16) -0.0118(10) O1X' 0.201(17) 0.94(6) 0.54(3) 0.54(4) -0.176(18) -0.14(2) C1X' 0.021(2) 0.071(4) 0.0372(19) 0.012(2) -0.0119(14) 0.006(2) C2X' 0.047(3) 0.053(3) 0.044(2) 0.020(2) -0.013(2) -0.005(2) C3X' 0.120(8) 0.040(3) 0.133(7) -0.020(4) -0.095(6) 0.004(4) C4X' 0.085(7) 0.206(12) 0.061(5) 0.017(6) 0.006(4) 0.014(7) C2Y 0.141(5) 0.224(7) 0.148(5) 0.033(5) 0.008(4) 0.041(5) O1Y 0.28(2) 0.41(3) 0.40(2) -0.19(2) -0.069(17) -0.024(18) C1Y 0.040(2) 0.056(3) 0.059(2) -0.008(2) 0.0083(18) -0.003(2) C3Y 0.051(3) 0.201(9) 0.069(3) -0.061(4) -0.024(3) 0.054(4) C4Y 0.033(2) 0.087(3) 0.050(2) -0.029(2) -0.0161(16) 0.0183(19) O1Y' 0.122(4) 0.054(2) 0.0312(15) -0.0133(14) -0.034(2) 0.056(3) C4Y' 0.035(2) 0.0292(17) 0.0311(16) 0.0060(14) -0.0023(14) -0.0010(15) C3Y' 0.0332(19) 0.0262(14) 0.0254(13) 0.0047(10) -0.0013(12) -0.0030(12) C1Y' 0.90(10) 0.53(7) 0.16(2) -0.02(3) 0.14(4) 0.46(7) O1Z 0.074(3) 0.058(3) 0.056(3) 0.0052(19) 0.000(2) 0.010(2) C1Z 0.031(2) 0.043(2) 0.049(2) -0.0121(19) -0.0035(18) 0.0096(18) C2Z 0.052(5) 0.061(4) 0.113(8) -0.012(5) -0.035(5) -0.006(3) C3Z 0.061(5) 0.033(2) 0.072(4) -0.023(3) -0.028(3) 0.013(2) C4Z 0.035(3) 0.0246(17) 0.059(3) 0.0016(17) -0.013(2) -0.0011(15) O1Z' 0.143(7) 0.197(10) 0.47(2) 0.011(11) 0.156(10) -0.024(7) C1Z' 0.168(9) 0.097(6) 0.332(16) -0.102(8) 0.164(10) -0.088(6) C2Z' 0.179(9) 0.154(8) 0.070(4) 0.020(4) -0.035(5) -0.114(7) C3Z' 0.232(11) 0.091(5) 0.062(4) -0.002(3) -0.029(5) -0.079(6) C4Z' 0.097(7) 0.255(14) 0.091(6) -0.095(8) 0.031(5) -0.096(8) _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 C48 2.1712(11) . ? Rh1 C49 2.1862(12) . ? Rh1 C53 2.2246(12) . ? Rh1 C54 2.2446(12) . ? Rh1 P1 2.3012(3) . ? Rh1 P2 2.3463(3) . ? P1 C30 1.8235(11) . ? P1 C8 1.8281(11) . ? P1 C24 1.8357(11) . ? O1 C9 1.3922(15) . ? O1 C1 1.4464(13) . ? C1 O2 1.4411(13) . ? C1 C13 1.5160(17) . ? C1 C2 1.5459(15) . ? P2 C19 1.8231(11) . ? P2 C36 1.8245(12) . ? P2 C42 1.8296(10) . ? C2 C3 1.5397(16) . ? O2 C20 1.3694(13) . ? C3 C4 1.5130(16) . ? C3 C11 1.5296(16) . ? C3 C10 1.5474(16) . ? C4 C5 1.3888(17) . ? C4 C9 1.4017(15) . ? C5 C6 1.3986(17) . ? C6 C7 1.3953(16) . ? C6 C12 1.5046(19) . ? C7 C8 1.3994(17) . ? C8 C9 1.4008(15) . ? C13 C14 1.5567(17) . ? C14 C15 1.5175(15) . ? C14 C22 1.535(2) . ? C14 C21 1.5456(17) . ? C15 C20 1.3939(16) . ? C15 C16 1.3987(16) . ? C16 C17 1.3932(16) . ? C17 C18 1.3976(17) . ? C17 C23 1.5042(17) . ? C18 C19 1.3987(15) . ? C19 C20 1.4049(14) . ? C24 C29 1.4006(15) . ? C24 C25 1.4026(15) . ? C25 C26 1.3906(17) . ? C26 C27 1.3869(19) . ? C27 C28 1.3907(19) . ? C28 C29 1.3934(17) . ? C30 C35 1.3985(16) . ? C30 C31 1.4012(17) . ? C31 C32 1.3880(19) . ? C32 C33 1.394(2) . ? C33 C34 1.386(3) . ? C34 C35 1.3939(18) . ? C36 C41 1.3944(16) . ? C36 C37 1.4021(18) . ? C37 C38 1.391(2) . ? C38 C39 1.396(3) . ? C39 C40 1.382(3) . ? C40 C41 1.3948(19) . ? C42 C43 1.3968(16) . ? C42 C47 1.4035(16) . ? C43 C44 1.3949(17) . ? C44 C45 1.386(2) . ? C45 C46 1.393(2) . ? C46 C47 1.3892(17) . ? C48 C49 1.3925(17) . ? C48 C52 1.5359(19) . ? C49 C50 1.5395(19) . ? C50 C54 1.5335(17) . ? C50 C51 1.5504(17) . ? C51 C52 1.550(2) . ? C52 C53 1.5429(17) . ? C53 C54 1.3813(17) . ? B1 F3 1.383(2) . ? B1 F4 1.386(2) . ? B1 F1 1.3898(18) . ? B1 F2 1.392(2) . ? O1X C1X 1.323(9) . ? O1X C4X 1.497(5) . ? C1X C2X 1.377(17) . ? C2X C3X 1.560(13) . ? C3X C4X 1.451(9) . ? O1X' C1X' 1.19(3) . ? O1X' C4X' 1.693(17) . ? C1X' C2X' 1.374(9) . ? C2X' C3X' 1.465(12) . ? C3X' C4X' 1.487(14) . ? C2Y C3Y' 1.426(7) . ? C2Y C1Y' 1.671(17) . ? O1Y C4Y 1.376(14) . ? O1Y C1Y 1.521(13) . ? C3Y C4Y 1.422(7) . ? O1Y' C1Y' 1.397(19) . ? O1Y' C4Y' 1.576(6) . ? C4Y' C3Y' 1.535(6) . ? C3Y' C3Y' 1.512(7) 3_666 ? O1Z C1Z 1.465(6) . ? O1Z C3Z 1.783(11) . ? O1Z C4Z 1.871(7) . ? C1Z C2Z 1.719(11) . ? C2Z C3Z 1.576(10) . ? C3Z C4Z 1.346(8) . ? O1Z' C1Z' 1.489(11) . ? O1Z' C4Z' 1.605(11) . ? C1Z' C2Z' 1.192(10) . ? C1Z' C3Z' 1.968(11) . ? C1Z' C4Z' 2.036(12) . ? C2Z' C3Z' 1.510(10) . ? C3Z' C4Z' 1.547(10) . ? 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 C48 Rh1 C49 37.27(5) . . ? C48 Rh1 C53 66.02(5) . . ? C49 Rh1 C53 77.55(5) . . ? C48 Rh1 C54 77.47(5) . . ? C49 Rh1 C54 65.09(5) . . ? C53 Rh1 C54 36.00(4) . . ? C48 Rh1 P1 96.44(4) . . ? C49 Rh1 P1 95.22(4) . . ? C53 Rh1 P1 159.32(3) . . ? C54 Rh1 P1 154.92(3) . . ? C48 Rh1 P2 150.68(3) . . ? C49 Rh1 P2 162.38(3) . . ? C53 Rh1 P2 93.72(3) . . ? C54 Rh1 P2 98.87(3) . . ? P1 Rh1 P2 97.892(11) . . ? C30 P1 C8 106.92(5) . . ? C30 P1 C24 100.36(5) . . ? C8 P1 C24 103.45(5) . . ? C30 P1 Rh1 114.24(4) . . ? C8 P1 Rh1 118.18(4) . . ? C24 P1 Rh1 111.72(4) . . ? C9 O1 C1 112.60(8) . . ? O2 C1 O1 103.39(8) . . ? O2 C1 C13 111.31(9) . . ? O1 C1 C13 107.60(9) . . ? O2 C1 C2 108.56(9) . . ? O1 C1 C2 111.68(9) . . ? C13 C1 C2 113.83(9) . . ? C19 P2 C36 109.97(5) . . ? C19 P2 C42 104.43(5) . . ? C36 P2 C42 99.79(5) . . ? C19 P2 Rh1 100.80(3) . . ? C36 P2 Rh1 125.79(4) . . ? C42 P2 Rh1 114.55(4) . . ? C3 C2 C1 114.19(9) . . ? C20 O2 C1 121.29(9) . . ? C4 C3 C11 113.17(10) . . ? C4 C3 C2 104.90(8) . . ? C11 C3 C2 108.70(9) . . ? C4 C3 C10 110.72(9) . . ? C11 C3 C10 108.01(9) . . ? C2 C3 C10 111.35(10) . . ? C5 C4 C9 118.89(10) . . ? C5 C4 C3 125.41(10) . . ? C9 C4 C3 115.60(10) . . ? C4 C5 C6 121.19(10) . . ? C7 C6 C5 118.53(11) . . ? C7 C6 C12 121.09(11) . . ? C5 C6 C12 120.38(11) . . ? C6 C7 C8 121.99(10) . . ? C7 C8 C9 117.72(10) . . ? C7 C8 P1 122.13(8) . . ? C9 C8 P1 120.15(9) . . ? O1 C9 C8 120.53(9) . . ? O1 C9 C4 118.07(9) . . ? C8 C9 C4 121.38(11) . . ? C1 C13 C14 114.20(10) . . ? C15 C14 C22 111.69(10) . . ? C15 C14 C21 108.41(10) . . ? C22 C14 C21 108.57(11) . . ? C15 C14 C13 106.68(9) . . ? C22 C14 C13 106.51(10) . . ? C21 C14 C13 115.04(10) . . ? C20 C15 C16 117.74(10) . . ? C20 C15 C14 118.44(10) . . ? C16 C15 C14 123.78(11) . . ? C17 C16 C15 121.67(11) . . ? C16 C17 C18 118.74(10) . . ? C16 C17 C23 121.12(12) . . ? C18 C17 C23 120.11(11) . . ? C17 C18 C19 121.23(10) . . ? C18 C19 C20 117.88(10) . . ? C18 C19 P2 122.02(8) . . ? C20 C19 P2 117.00(8) . . ? O2 C20 C15 122.78(9) . . ? O2 C20 C19 115.34(10) . . ? C15 C20 C19 121.88(10) . . ? C29 C24 C25 118.61(10) . . ? C29 C24 P1 119.12(8) . . ? C25 C24 P1 122.05(8) . . ? C26 C25 C24 120.22(11) . . ? C27 C26 C25 120.69(11) . . ? C26 C27 C28 119.75(11) . . ? C27 C28 C29 119.89(11) . . ? C28 C29 C24 120.84(11) . . ? C35 C30 C31 118.89(11) . . ? C35 C30 P1 118.50(9) . . ? C31 C30 P1 122.29(9) . . ? C32 C31 C30 120.48(12) . . ? C31 C32 C33 119.93(14) . . ? C34 C33 C32 120.23(12) . . ? C33 C34 C35 119.85(13) . . ? C34 C35 C30 120.56(13) . . ? C41 C36 C37 119.43(12) . . ? C41 C36 P2 123.71(10) . . ? C37 C36 P2 116.85(9) . . ? C38 C37 C36 120.09(13) . . ? C37 C38 C39 119.80(15) . . ? C40 C39 C38 120.46(14) . . ? C39 C40 C41 119.89(14) . . ? C36 C41 C40 120.32(14) . . ? C43 C42 C47 119.28(10) . . ? C43 C42 P2 121.45(9) . . ? C47 C42 P2 119.22(8) . . ? C44 C43 C42 120.43(12) . . ? C45 C44 C43 119.77(12) . . ? C44 C45 C46 120.34(12) . . ? C47 C46 C45 120.13(13) . . ? C46 C47 C42 120.02(12) . . ? C49 C48 C52 106.50(11) . . ? C49 C48 Rh1 71.95(7) . . ? C52 C48 Rh1 96.91(7) . . ? C48 C49 C50 106.33(11) . . ? C48 C49 Rh1 70.78(7) . . ? C50 C49 Rh1 97.60(7) . . ? C54 C50 C49 101.77(10) . . ? C54 C50 C51 100.16(10) . . ? C49 C50 C51 100.46(10) . . ? C52 C51 C50 93.68(10) . . ? C48 C52 C53 102.15(9) . . ? C48 C52 C51 100.36(10) . . ? C53 C52 C51 99.77(10) . . ? C54 C53 C52 106.51(10) . . ? C54 C53 Rh1 72.79(7) . . ? C52 C53 Rh1 94.56(8) . . ? C53 C54 C50 106.74(10) . . ? C53 C54 Rh1 71.21(7) . . ? C50 C54 Rh1 95.42(8) . . ? F3 B1 F4 110.68(15) . . ? F3 B1 F1 111.03(14) . . ? F4 B1 F1 110.03(14) . . ? F3 B1 F2 108.86(14) . . ? F4 B1 F2 107.30(15) . . ? F1 B1 F2 108.85(15) . . ? C1X O1X C4X 105.8(5) . . ? O1X C1X C2X 102.6(7) . . ? C1X C2X C3X 109.3(8) . . ? C4X C3X C2X 98.2(7) . . ? C3X C4X O1X 98.2(4) . . ? C1X' O1X' C4X' 108.7(16) . . ? O1X' C1X' C2X' 115.9(10) . . ? C1X' C2X' C3X' 107.7(6) . . ? C2X' C3X' C4X' 108.4(7) . . ? C3X' C4X' O1X' 97.2(12) . . ? C3Y' C2Y C1Y' 118.2(11) . . ? C4Y O1Y C1Y 110.9(11) . . ? O1Y C4Y C3Y 108.9(7) . . ? C1Y' O1Y' C4Y' 95.3(14) . . ? C3Y' C4Y' O1Y' 114.4(3) . . ? C2Y C3Y' C3Y' 155.5(5) . 3_666 ? C2Y C3Y' C4Y' 88.4(4) . . ? C3Y' C3Y' C4Y' 113.3(4) 3_666 . ? O1Y' C1Y' C2Y 92.1(10) . . ? C1Z O1Z C3Z 102.8(4) . . ? C1Z O1Z C4Z 128.7(4) . . ? C3Z O1Z C4Z 43.2(3) . . ? O1Z C1Z C2Z 78.5(4) . . ? C3Z C2Z C1Z 101.1(6) . . ? C4Z C3Z C2Z 110.2(7) . . ? C4Z C3Z O1Z 71.9(5) . . ? C2Z C3Z O1Z 73.8(5) . . ? C3Z C4Z O1Z 64.9(4) . . ? C1Z' O1Z' C4Z' 82.2(7) . . ? C2Z' C1Z' O1Z' 127.3(11) . . ? C2Z' C1Z' C3Z' 50.0(5) . . ? O1Z' C1Z' C3Z' 81.6(6) . . ? C2Z' C1Z' C4Z' 93.7(7) . . ? O1Z' C1Z' C4Z' 51.4(5) . . ? C3Z' C1Z' C4Z' 45.4(3) . . ? C1Z' C2Z' C3Z' 92.7(6) . . ? C2Z' C3Z' C4Z' 104.9(6) . . ? C2Z' C3Z' C1Z' 37.2(4) . . ? C4Z' C3Z' C1Z' 69.6(5) . . ? C3Z' C4Z' O1Z' 93.1(7) . . ? C3Z' C4Z' C1Z' 65.0(5) . . ? O1Z' C4Z' C1Z' 46.5(5) . . ? 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 C48 Rh1 P1 C30 -74.84(5) . . . . ? C49 Rh1 P1 C30 -112.29(5) . . . . ? C53 Rh1 P1 C30 -44.06(10) . . . . ? C54 Rh1 P1 C30 -148.93(8) . . . . ? P2 Rh1 P1 C30 79.51(4) . . . . ? C48 Rh1 P1 C8 158.05(5) . . . . ? C49 Rh1 P1 C8 120.60(5) . . . . ? C53 Rh1 P1 C8 -171.17(10) . . . . ? C54 Rh1 P1 C8 83.97(8) . . . . ? P2 Rh1 P1 C8 -47.60(4) . . . . ? C48 Rh1 P1 C24 38.22(5) . . . . ? C49 Rh1 P1 C24 0.77(5) . . . . ? C53 Rh1 P1 C24 69.00(10) . . . . ? C54 Rh1 P1 C24 -35.87(8) . . . . ? P2 Rh1 P1 C24 -167.43(4) . . . . ? C9 O1 C1 O2 -69.44(10) . . . . ? C9 O1 C1 C13 172.69(8) . . . . ? C9 O1 C1 C2 47.09(11) . . . . ? C48 Rh1 P2 C19 -110.71(8) . . . . ? C49 Rh1 P2 C19 -6.98(12) . . . . ? C53 Rh1 P2 C19 -66.41(5) . . . . ? C54 Rh1 P2 C19 -30.54(4) . . . . ? P1 Rh1 P2 C19 130.74(3) . . . . ? C48 Rh1 P2 C36 124.81(9) . . . . ? C49 Rh1 P2 C36 -131.46(12) . . . . ? C53 Rh1 P2 C36 169.11(6) . . . . ? C54 Rh1 P2 C36 -155.02(6) . . . . ? P1 Rh1 P2 C36 6.26(5) . . . . ? C48 Rh1 P2 C42 0.76(9) . . . . ? C49 Rh1 P2 C42 104.49(12) . . . . ? C53 Rh1 P2 C42 45.06(5) . . . . ? C54 Rh1 P2 C42 80.93(5) . . . . ? P1 Rh1 P2 C42 -117.79(4) . . . . ? O2 C1 C2 C3 117.94(10) . . . . ? O1 C1 C2 C3 4.60(14) . . . . ? C13 C1 C2 C3 -117.49(11) . . . . ? O1 C1 O2 C20 -118.99(10) . . . . ? C13 C1 O2 C20 -3.75(13) . . . . ? C2 C1 O2 C20 122.30(10) . . . . ? C1 C2 C3 C4 -50.16(12) . . . . ? C1 C2 C3 C11 -171.48(10) . . . . ? C1 C2 C3 C10 69.65(12) . . . . ? C11 C3 C4 C5 -7.84(15) . . . . ? C2 C3 C4 C5 -126.17(11) . . . . ? C10 C3 C4 C5 113.60(12) . . . . ? C11 C3 C4 C9 168.33(10) . . . . ? C2 C3 C4 C9 50.00(12) . . . . ? C10 C3 C4 C9 -70.23(12) . . . . ? C9 C4 C5 C6 2.29(16) . . . . ? C3 C4 C5 C6 178.35(10) . . . . ? C4 C5 C6 C7 1.89(17) . . . . ? C4 C5 C6 C12 -178.93(11) . . . . ? C5 C6 C7 C8 -2.28(17) . . . . ? C12 C6 C7 C8 178.54(11) . . . . ? C6 C7 C8 C9 -1.52(16) . . . . ? C6 C7 C8 P1 177.67(9) . . . . ? C30 P1 C8 C7 1.01(10) . . . . ? C24 P1 C8 C7 -104.42(9) . . . . ? Rh1 P1 C8 C7 131.54(8) . . . . ? C30 P1 C8 C9 -179.82(8) . . . . ? C24 P1 C8 C9 74.75(9) . . . . ? Rh1 P1 C8 C9 -49.29(9) . . . . ? C1 O1 C9 C8 130.06(10) . . . . ? C1 O1 C9 C4 -51.35(12) . . . . ? C7 C8 C9 O1 -175.60(9) . . . . ? P1 C8 C9 O1 5.20(13) . . . . ? C7 C8 C9 C4 5.86(15) . . . . ? P1 C8 C9 C4 -173.34(8) . . . . ? C5 C4 C9 O1 175.13(9) . . . . ? C3 C4 C9 O1 -1.30(14) . . . . ? C5 C4 C9 C8 -6.29(15) . . . . ? C3 C4 C9 C8 177.27(9) . . . . ? O2 C1 C13 C14 44.40(12) . . . . ? O1 C1 C13 C14 157.01(8) . . . . ? C2 C1 C13 C14 -78.67(11) . . . . ? C1 C13 C14 C15 -54.86(12) . . . . ? C1 C13 C14 C22 -174.28(10) . . . . ? C1 C13 C14 C21 65.39(13) . . . . ? C22 C14 C15 C20 142.96(11) . . . . ? C21 C14 C15 C20 -97.47(12) . . . . ? C13 C14 C15 C20 26.95(14) . . . . ? C22 C14 C15 C16 -34.81(16) . . . . ? C21 C14 C15 C16 84.76(14) . . . . ? C13 C14 C15 C16 -150.81(11) . . . . ? C20 C15 C16 C17 -3.51(16) . . . . ? C14 C15 C16 C17 174.27(11) . . . . ? C15 C16 C17 C18 -4.25(17) . . . . ? C15 C16 C17 C23 177.77(12) . . . . ? C16 C17 C18 C19 5.92(17) . . . . ? C23 C17 C18 C19 -176.07(12) . . . . ? C17 C18 C19 C20 0.21(16) . . . . ? C17 C18 C19 P2 -159.27(9) . . . . ? C36 P2 C19 C18 -123.76(9) . . . . ? C42 P2 C19 C18 -17.48(10) . . . . ? Rh1 P2 C19 C18 101.59(9) . . . . ? C36 P2 C19 C20 76.58(9) . . . . ? C42 P2 C19 C20 -177.14(8) . . . . ? Rh1 P2 C19 C20 -58.07(8) . . . . ? C1 O2 C20 C15 -25.73(15) . . . . ? C1 O2 C20 C19 153.90(9) . . . . ? C16 C15 C20 O2 -170.41(10) . . . . ? C14 C15 C20 O2 11.68(16) . . . . ? C16 C15 C20 C19 9.99(16) . . . . ? C14 C15 C20 C19 -167.92(10) . . . . ? C18 C19 C20 O2 171.98(9) . . . . ? P2 C19 C20 O2 -27.49(12) . . . . ? C18 C19 C20 C15 -8.39(15) . . . . ? P2 C19 C20 C15 152.13(9) . . . . ? C30 P1 C24 C29 35.31(11) . . . . ? C8 P1 C24 C29 145.67(10) . . . . ? Rh1 P1 C24 C29 -86.17(10) . . . . ? C30 P1 C24 C25 -150.22(11) . . . . ? C8 P1 C24 C25 -39.85(12) . . . . ? Rh1 P1 C24 C25 88.31(11) . . . . ? C29 C24 C25 C26 -0.8(2) . . . . ? P1 C24 C25 C26 -175.35(11) . . . . ? C24 C25 C26 C27 0.2(2) . . . . ? C25 C26 C27 C28 0.3(2) . . . . ? C26 C27 C28 C29 -0.1(2) . . . . ? C27 C28 C29 C24 -0.5(2) . . . . ? C25 C24 C29 C28 1.0(2) . . . . ? P1 C24 C29 C28 175.69(11) . . . . ? C8 P1 C30 C35 130.99(10) . . . . ? C24 P1 C30 C35 -121.38(10) . . . . ? Rh1 P1 C30 C35 -1.72(11) . . . . ? C8 P1 C30 C31 -55.47(11) . . . . ? C24 P1 C30 C31 52.15(11) . . . . ? Rh1 P1 C30 C31 171.82(9) . . . . ? C35 C30 C31 C32 -2.24(19) . . . . ? P1 C30 C31 C32 -175.75(11) . . . . ? C30 C31 C32 C33 1.4(2) . . . . ? C31 C32 C33 C34 0.5(2) . . . . ? C32 C33 C34 C35 -1.5(2) . . . . ? C33 C34 C35 C30 0.7(2) . . . . ? C31 C30 C35 C34 1.17(19) . . . . ? P1 C30 C35 C34 174.93(11) . . . . ? C19 P2 C36 C41 -12.13(11) . . . . ? C42 P2 C36 C41 -121.50(10) . . . . ? Rh1 P2 C36 C41 108.39(9) . . . . ? C19 P2 C36 C37 166.50(8) . . . . ? C42 P2 C36 C37 57.12(10) . . . . ? Rh1 P2 C36 C37 -72.99(10) . . . . ? C41 C36 C37 C38 0.08(18) . . . . ? P2 C36 C37 C38 -178.61(10) . . . . ? C36 C37 C38 C39 -0.4(2) . . . . ? C37 C38 C39 C40 -0.1(2) . . . . ? C38 C39 C40 C41 0.9(2) . . . . ? C37 C36 C41 C40 0.71(18) . . . . ? P2 C36 C41 C40 179.30(10) . . . . ? C39 C40 C41 C36 -1.2(2) . . . . ? C19 P2 C42 C43 123.24(11) . . . . ? C36 P2 C42 C43 -123.04(11) . . . . ? Rh1 P2 C42 C43 13.96(12) . . . . ? C19 P2 C42 C47 -59.26(11) . . . . ? C36 P2 C42 C47 54.47(11) . . . . ? Rh1 P2 C42 C47 -168.54(9) . . . . ? C47 C42 C43 C44 1.2(2) . . . . ? P2 C42 C43 C44 178.72(11) . . . . ? C42 C43 C44 C45 0.3(2) . . . . ? C43 C44 C45 C46 -1.1(3) . . . . ? C44 C45 C46 C47 0.4(3) . . . . ? C45 C46 C47 C42 1.2(2) . . . . ? C43 C42 C47 C46 -2.0(2) . . . . ? P2 C42 C47 C46 -179.51(12) . . . . ? C53 Rh1 C48 C49 101.23(8) . . . . ? C54 Rh1 C48 C49 65.15(8) . . . . ? P1 Rh1 C48 C49 -90.17(7) . . . . ? P2 Rh1 C48 C49 150.94(7) . . . . ? C49 Rh1 C48 C52 -105.15(11) . . . . ? C53 Rh1 C48 C52 -3.92(7) . . . . ? C54 Rh1 C48 C52 -40.01(7) . . . . ? P1 Rh1 C48 C52 164.67(7) . . . . ? P2 Rh1 C48 C52 45.79(12) . . . . ? C52 C48 C49 C50 -0.48(12) . . . . ? Rh1 C48 C49 C50 -92.51(8) . . . . ? C52 C48 C49 Rh1 92.03(8) . . . . ? C53 Rh1 C49 C48 -66.60(8) . . . . ? C54 Rh1 C49 C48 -102.42(8) . . . . ? P1 Rh1 C49 C48 93.77(7) . . . . ? P2 Rh1 C49 C48 -128.23(10) . . . . ? C48 Rh1 C49 C50 104.70(11) . . . . ? C53 Rh1 C49 C50 38.10(7) . . . . ? C54 Rh1 C49 C50 2.28(7) . . . . ? P1 Rh1 C49 C50 -161.52(6) . . . . ? P2 Rh1 C49 C50 -23.53(16) . . . . ? C48 C49 C50 C54 69.02(11) . . . . ? Rh1 C49 C50 C54 -3.10(9) . . . . ? C48 C49 C50 C51 -33.78(12) . . . . ? Rh1 C49 C50 C51 -105.90(8) . . . . ? C54 C50 C51 C52 -52.26(11) . . . . ? C49 C50 C51 C52 51.85(11) . . . . ? C49 C48 C52 C53 -67.88(12) . . . . ? Rh1 C48 C52 C53 5.28(10) . . . . ? C49 C48 C52 C51 34.58(12) . . . . ? Rh1 C48 C52 C51 107.75(8) . . . . ? C50 C51 C52 C48 -52.13(11) . . . . ? C50 C51 C52 C53 52.27(11) . . . . ? C48 C52 C53 C54 68.25(12) . . . . ? C51 C52 C53 C54 -34.68(13) . . . . ? C48 C52 C53 Rh1 -5.14(9) . . . . ? C51 C52 C53 Rh1 -108.06(9) . . . . ? C48 Rh1 C53 C54 -102.00(8) . . . . ? C49 Rh1 C53 C54 -64.54(7) . . . . ? P1 Rh1 C53 C54 -135.82(8) . . . . ? P2 Rh1 C53 C54 99.98(7) . . . . ? C48 Rh1 C53 C52 3.89(7) . . . . ? C49 Rh1 C53 C52 41.35(7) . . . . ? C54 Rh1 C53 C52 105.89(10) . . . . ? P1 Rh1 C53 C52 -29.93(14) . . . . ? P2 Rh1 C53 C52 -154.13(7) . . . . ? C52 C53 C54 C50 0.39(13) . . . . ? Rh1 C53 C54 C50 90.11(9) . . . . ? C52 C53 C54 Rh1 -89.71(9) . . . . ? C49 C50 C54 C53 -68.97(12) . . . . ? C51 C50 C54 C53 34.07(13) . . . . ? C49 C50 C54 Rh1 3.01(9) . . . . ? C51 C50 C54 Rh1 106.05(9) . . . . ? C48 Rh1 C54 C53 66.29(7) . . . . ? C49 Rh1 C54 C53 103.58(8) . . . . ? P1 Rh1 C54 C53 144.51(7) . . . . ? P2 Rh1 C54 C53 -84.09(7) . . . . ? C48 Rh1 C54 C50 -39.58(7) . . . . ? C49 Rh1 C54 C50 -2.28(6) . . . . ? C53 Rh1 C54 C50 -105.86(9) . . . . ? P1 Rh1 C54 C50 38.65(11) . . . . ? P2 Rh1 C54 C50 170.05(6) . . . . ? C4X O1X C1X C2X 43.2(8) . . . . ? O1X C1X C2X C3X -17.7(10) . . . . ? C1X C2X C3X C4X -14.3(9) . . . . ? C2X C3X C4X O1X 36.0(6) . . . . ? C1X O1X C4X C3X -53.0(6) . . . . ? C4X' O1X' C1X' C2X' -14.5(19) . . . . ? O1X' C1X' C2X' C3X' 16.0(15) . . . . ? C1X' C2X' C3X' C4X' -9.5(11) . . . . ? C2X' C3X' C4X' O1X' 2.0(13) . . . . ? C1X' O1X' C4X' C3X' 7.1(17) . . . . ? C1Y O1Y C4Y C3Y -12(2) . . . . ? C1Y' O1Y' C4Y' C3Y' -54.1(15) . . . . ? C1Y' C2Y C3Y' C3Y' -140.7(17) . . . 3_666 ? C1Y' C2Y C3Y' C4Y' 12.7(16) . . . . ? O1Y' C4Y' C3Y' C2Y 22.4(5) . . . . ? O1Y' C4Y' C3Y' C3Y' -169.3(5) . . . 3_666 ? C4Y' O1Y' C1Y' C2Y 47.3(17) . . . . ? C3Y' C2Y C1Y' O1Y' -46(3) . . . . ? C3Z O1Z C1Z C2Z -14.2(4) . . . . ? C4Z O1Z C1Z C2Z 24.9(6) . . . . ? O1Z C1Z C2Z C3Z 16.0(5) . . . . ? C1Z C2Z C3Z C4Z -76.5(7) . . . . ? C1Z C2Z C3Z O1Z -13.3(4) . . . . ? C1Z O1Z C3Z C4Z 134.0(5) . . . . ? C1Z O1Z C3Z C2Z 15.8(5) . . . . ? C4Z O1Z C3Z C2Z -118.2(6) . . . . ? C2Z C3Z C4Z O1Z 64.4(6) . . . . ? C1Z O1Z C4Z C3Z -64.0(6) . . . . ? C4Z' O1Z' C1Z' C2Z' -59.7(14) . . . . ? C4Z' O1Z' C1Z' C3Z' -37.8(6) . . . . ? O1Z' C1Z' C2Z' C3Z' 28.8(15) . . . . ? C4Z' C1Z' C2Z' C3Z' -13.7(9) . . . . ? C1Z' C2Z' C3Z' C4Z' 18.8(12) . . . . ? O1Z' C1Z' C3Z' C2Z' -157.2(14) . . . . ? C4Z' C1Z' C3Z' C2Z' 160.6(13) . . . . ? C2Z' C1Z' C3Z' C4Z' -160.6(13) . . . . ? O1Z' C1Z' C3Z' C4Z' 42.2(8) . . . . ? C2Z' C3Z' C4Z' O1Z' -50.1(10) . . . . ? C1Z' C3Z' C4Z' O1Z' -38.1(7) . . . . ? C2Z' C3Z' C4Z' C1Z' -12.0(8) . . . . ? C1Z' O1Z' C4Z' C3Z' 50.5(9) . . . . ? C2Z' C1Z' C4Z' C3Z' 14.8(10) . . . . ? O1Z' C1Z' C4Z' C3Z' -121.7(11) . . . . ? C2Z' C1Z' C4Z' O1Z' 136.5(14) . . . . ? C3Z' C1Z' C4Z' O1Z' 121.7(11) . . . . ? _diffrn_measured_fraction_theta_max 0.872 _diffrn_reflns_theta_full 39.54 _diffrn_measured_fraction_theta_full 0.872 _refine_diff_density_max 1.441 _refine_diff_density_min -0.765 _refine_diff_density_rms 0.085 #===END data_cj-i38_0m _database_code_depnum_ccdc_archive 'CCDC 286678' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H64 B Cl6 F4 O2 P2 Rh' _chemical_formula_weight 1089.31 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' 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' Cl Cl 0.1484 0.1585 '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' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0532(8) _cell_length_b 19.6411(12) _cell_length_c 19.8764(13) _cell_angle_alpha 90.00 _cell_angle_beta 94.746(2) _cell_angle_gamma 90.00 _cell_volume 5078.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9611 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 39.30 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2248 _exptl_absorpt_coefficient_mu 0.764 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7497 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 100953 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_sigmaI/netI 0.0334 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 39.54 _reflns_number_total 28230 _reflns_number_gt 22813 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The two chloroform molecules are each disordered in two positions. ; _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^)+(0.0379P)^2^+2.3070P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 28230 _refine_ls_number_parameters 581 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.005 _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 0.058420(5) 0.713949(4) 0.748783(4) 0.01309(2) Uani 1 1 d . . . C1 C 0.43273(7) 0.85642(6) 0.75980(6) 0.01755(17) Uani 1 1 d . . . O1 O 0.33391(5) 0.88197(4) 0.73347(4) 0.01637(13) Uani 1 1 d . . . P1 P 0.102517(18) 0.822721(14) 0.706261(13) 0.01299(4) Uani 1 1 d . . . P2 P 0.224741(18) 0.689103(14) 0.800087(12) 0.01320(4) Uani 1 1 d . . . C2 C 0.47468(8) 0.89308(6) 0.82430(6) 0.02107(19) Uani 1 1 d . . . H2A H 0.5482 0.9038 0.8208 0.025 Uiso 1 1 calc R . . H2B H 0.4705 0.8619 0.8631 0.025 Uiso 1 1 calc R . . O2 O 0.41759(6) 0.78742(4) 0.78156(4) 0.01746(13) Uani 1 1 d . . . C3 C 0.41735(8) 0.95939(6) 0.83851(6) 0.01849(17) Uani 1 1 d . . . C4 C 0.30409(7) 0.94020(5) 0.83563(5) 0.01614(16) Uani 1 1 d . . . C5 C 0.23757(8) 0.95691(6) 0.88449(5) 0.01822(17) Uani 1 1 d . . . H5 H 0.2623 0.9836 0.9222 0.022 Uiso 1 1 calc R . . C6 C 0.13503(8) 0.93518(6) 0.87908(5) 0.01715(16) Uani 1 1 d . . . C7 C 0.09995(7) 0.89641(5) 0.82329(5) 0.01569(15) Uani 1 1 d . . . H7 H 0.0302 0.8821 0.8191 0.019 Uiso 1 1 calc R . . C8 C 0.16427(7) 0.87751(5) 0.77278(5) 0.01336(14) Uani 1 1 d . . . C9 C 0.26660(7) 0.89948(5) 0.78084(5) 0.01387(14) Uani 1 1 d . . . C10 C 0.43707(9) 1.01428(6) 0.78567(7) 0.0237(2) Uani 1 1 d . . . H10A H 0.4086 0.9991 0.7410 0.036 Uiso 1 1 calc R . . H10B H 0.5112 1.0217 0.7850 0.036 Uiso 1 1 calc R . . H10C H 0.4039 1.0569 0.7974 0.036 Uiso 1 1 calc R . . C11 C 0.45893(9) 0.98515(8) 0.90832(7) 0.0279(2) Uani 1 1 d . . . H11A H 0.4240 1.0276 0.9186 0.042 Uiso 1 1 calc R . . H11B H 0.5330 0.9934 0.9085 0.042 Uiso 1 1 calc R . . H11C H 0.4463 0.9509 0.9425 0.042 Uiso 1 1 calc R . . C12 C 0.06402(9) 0.95181(7) 0.93325(6) 0.0253(2) Uani 1 1 d . . . H12A H -0.0022 0.9677 0.9121 0.038 Uiso 1 1 calc R . . H12B H 0.0950 0.9876 0.9627 0.038 Uiso 1 1 calc R . . H12C H 0.0533 0.9109 0.9600 0.038 Uiso 1 1 calc R . . C13 C 0.49927(8) 0.86063(7) 0.69923(7) 0.0237(2) Uani 1 1 d . . . H13A H 0.4565 0.8782 0.6596 0.028 Uiso 1 1 calc R . . H13B H 0.5556 0.8936 0.7100 0.028 Uiso 1 1 calc R . . C14 C 0.54615(9) 0.79184(7) 0.68048(7) 0.0247(2) Uani 1 1 d . . . C15 C 0.45884(8) 0.74039(6) 0.67620(6) 0.02040(19) Uani 1 1 d . . . C16 C 0.43507(9) 0.69494(7) 0.62332(6) 0.0238(2) Uani 1 1 d . . . H16 H 0.4755 0.6950 0.5857 0.029 Uiso 1 1 calc R . . C17 C 0.35301(9) 0.64922(6) 0.62448(6) 0.02101(19) Uani 1 1 d . . . C18 C 0.29602(8) 0.64848(6) 0.68087(5) 0.01790(17) Uani 1 1 d . . . H18 H 0.2424 0.6161 0.6830 0.021 Uiso 1 1 calc R . . C19 C 0.31582(7) 0.69454(6) 0.73487(5) 0.01515(15) Uani 1 1 d . . . C20 C 0.39648(7) 0.74054(6) 0.73055(5) 0.01627(16) Uani 1 1 d . . . C21 C 0.63029(9) 0.76933(8) 0.73507(9) 0.0311(3) Uani 1 1 d . . . H21A H 0.6000 0.7636 0.7782 0.047 Uiso 1 1 calc R . . H21B H 0.6843 0.8041 0.7399 0.047 Uiso 1 1 calc R . . H21C H 0.6600 0.7260 0.7218 0.047 Uiso 1 1 calc R . . C22 C 0.59524(12) 0.80040(9) 0.61357(9) 0.0376(3) Uani 1 1 d . . . H22A H 0.6288 0.7578 0.6022 0.056 Uiso 1 1 calc R . . H22B H 0.6464 0.8370 0.6180 0.056 Uiso 1 1 calc R . . H22C H 0.5419 0.8119 0.5777 0.056 Uiso 1 1 calc R . . C23 C 0.32212(11) 0.60378(7) 0.56501(6) 0.0277(2) Uani 1 1 d . . . H23A H 0.3011 0.5592 0.5813 0.042 Uiso 1 1 calc R . . H23B H 0.3806 0.5981 0.5376 0.042 Uiso 1 1 calc R . . H23C H 0.2646 0.6245 0.5375 0.042 Uiso 1 1 calc R . . C24 C 0.18502(8) 0.81443(6) 0.63531(5) 0.01820(17) Uani 1 1 d . . . H24 H 0.2530 0.7979 0.6558 0.022 Uiso 1 1 calc R . . C25 C 0.14347(10) 0.75750(7) 0.58746(6) 0.0251(2) Uani 1 1 d . . . H25A H 0.0801 0.7729 0.5621 0.038 Uiso 1 1 calc R . . H25B H 0.1289 0.7170 0.6138 0.038 Uiso 1 1 calc R . . H25C H 0.1949 0.7463 0.5559 0.038 Uiso 1 1 calc R . . C26 C 0.20803(10) 0.87914(8) 0.59616(6) 0.0270(2) Uani 1 1 d . . . H26A H 0.2643 0.8702 0.5676 0.041 Uiso 1 1 calc R . . H26B H 0.2281 0.9158 0.6281 0.041 Uiso 1 1 calc R . . H26C H 0.1465 0.8928 0.5678 0.041 Uiso 1 1 calc R . . C27 C -0.00998(8) 0.87789(6) 0.67810(6) 0.01791(17) Uani 1 1 d . . . H27 H -0.0583 0.8746 0.7145 0.021 Uiso 1 1 calc R . . C28 C -0.07144(9) 0.85424(7) 0.61304(6) 0.0241(2) Uani 1 1 d . . . H28A H -0.1360 0.8798 0.6069 0.036 Uiso 1 1 calc R . . H28B H -0.0865 0.8055 0.6163 0.036 Uiso 1 1 calc R . . H28C H -0.0310 0.8623 0.5744 0.036 Uiso 1 1 calc R . . C29 C 0.01488(10) 0.95387(6) 0.67186(7) 0.0253(2) Uani 1 1 d . . . H29A H 0.0540 0.9611 0.6325 0.038 Uiso 1 1 calc R . . H29B H 0.0557 0.9691 0.7127 0.038 Uiso 1 1 calc R . . H29C H -0.0492 0.9800 0.6664 0.038 Uiso 1 1 calc R . . C30 C 0.25821(8) 0.74686(6) 0.87223(5) 0.01713(16) Uani 1 1 d . . . H30 H 0.2699 0.7926 0.8522 0.021 Uiso 1 1 calc R . . C31 C 0.16251(10) 0.75445(6) 0.91225(6) 0.0224(2) Uani 1 1 d . . . H31A H 0.1506 0.7118 0.9360 0.034 Uiso 1 1 calc R . . H31B H 0.1025 0.7649 0.8811 0.034 Uiso 1 1 calc R . . H31C H 0.1736 0.7915 0.9451 0.034 Uiso 1 1 calc R . . C32 C 0.35467(10) 0.73141(7) 0.91906(6) 0.0249(2) Uani 1 1 d . . . H32A H 0.3688 0.7696 0.9501 0.037 Uiso 1 1 calc R . . H32B H 0.4133 0.7247 0.8920 0.037 Uiso 1 1 calc R . . H32C H 0.3435 0.6900 0.9450 0.037 Uiso 1 1 calc R . . C33 C 0.24958(8) 0.59930(6) 0.82885(5) 0.01778(17) Uani 1 1 d . . . H33 H 0.2194 0.5696 0.7914 0.021 Uiso 1 1 calc R . . C34 C 0.36397(9) 0.57964(7) 0.83952(6) 0.0236(2) Uani 1 1 d . . . H34A H 0.3944 0.6004 0.8814 0.035 Uiso 1 1 calc R . . H34B H 0.4000 0.5960 0.8013 0.035 Uiso 1 1 calc R . . H34C H 0.3703 0.5300 0.8427 0.035 Uiso 1 1 calc R . . C35 C 0.19496(9) 0.57953(6) 0.89151(6) 0.02217(19) Uani 1 1 d . . . H35A H 0.2027 0.5305 0.8996 0.033 Uiso 1 1 calc R . . H35B H 0.1218 0.5908 0.8841 0.033 Uiso 1 1 calc R . . H35C H 0.2255 0.6046 0.9308 0.033 Uiso 1 1 calc R . . C36 C -0.07017(8) 0.68722(6) 0.67546(6) 0.02122(19) Uani 1 1 d . . . H36 H -0.0743 0.7021 0.6272 0.025 Uiso 1 1 calc R . . C37 C -0.10870(8) 0.72578(6) 0.72639(6) 0.02001(19) Uani 1 1 d . . . H37 H -0.1428 0.7709 0.7182 0.024 Uiso 1 1 calc R . . C38 C -0.14061(8) 0.67481(6) 0.77958(7) 0.0234(2) Uani 1 1 d . . . H38 H -0.1884 0.6915 0.8128 0.028 Uiso 1 1 calc R . . C39 C -0.03506(8) 0.64803(6) 0.80790(6) 0.02102(19) Uani 1 1 d . . . H39 H -0.0178 0.6387 0.8570 0.025 Uiso 1 1 calc R . . C40 C 0.00387(8) 0.60948(6) 0.75714(6) 0.02066(19) Uani 1 1 d . . . H40 H 0.0510 0.5698 0.7664 0.025 Uiso 1 1 calc R . . C41 C -0.07771(9) 0.61234(6) 0.69671(7) 0.0241(2) Uani 1 1 d . . . H41 H -0.0734 0.5771 0.6607 0.029 Uiso 1 1 calc R . . C42 C -0.17740(9) 0.61429(7) 0.73379(8) 0.0280(2) Uani 1 1 d . . . H42A H -0.1885 0.5721 0.7595 0.034 Uiso 1 1 calc R . . H42B H -0.2392 0.6252 0.7034 0.034 Uiso 1 1 calc R . . C1SA C 0.30276(13) 0.40193(9) 0.04827(8) 0.0347(3) Uani 1 1 d . . . H1S H 0.2978 0.3580 0.0227 0.042 Uiso 1 1 calc R A 1 Cl1A Cl 0.17701(6) 0.43218(4) 0.05408(7) 0.04727(16) Uani 0.913(4) 1 d P B 1 Cl2A Cl 0.36619(5) 0.38517(7) 0.12834(3) 0.0459(2) Uani 0.913(4) 1 d P B 1 Cl3A Cl 0.37144(11) 0.45934(5) 0.00190(5) 0.0644(2) Uani 0.913(4) 1 d P B 1 C1SB C 0.23281(12) 0.32686(8) 0.54593(7) 0.0323(3) Uani 1 1 d . . . H2S H 0.2234 0.3552 0.5867 0.039 Uiso 1 1 calc R C 1 Cl1B Cl 0.22382(13) 0.37886(8) 0.47472(7) 0.0760(4) Uani 0.891(4) 1 d P D 1 Cl2B Cl 0.13791(9) 0.26313(6) 0.53895(4) 0.0547(2) Uani 0.891(4) 1 d P D 1 Cl3B Cl 0.35630(8) 0.28791(5) 0.55500(6) 0.0534(3) Uani 0.891(4) 1 d P D 1 B1S B 0.20809(10) 0.44068(8) 0.69981(9) 0.0278(3) Uani 1 1 d . . . F1S F 0.25162(10) 0.43779(6) 0.76594(7) 0.0574(3) Uani 1 1 d . . . F2S F 0.28299(8) 0.45121(6) 0.65510(7) 0.0491(3) Uani 1 1 d . . . F3S F 0.16045(7) 0.37819(5) 0.68379(5) 0.03254(18) Uani 1 1 d . . . F4S F 0.13610(7) 0.49276(5) 0.69382(6) 0.0384(2) Uani 1 1 d . . . Cl1' Cl 0.2326(5) 0.3720(5) 0.4659(4) 0.0312(11) Uiso 0.109(4) 1 d P D 2 Cl2' Cl 0.1087(4) 0.2846(4) 0.5341(3) 0.0408(12) Uiso 0.109(4) 1 d P D 2 Cl3' Cl 0.3264(5) 0.2791(3) 0.5706(3) 0.0396(12) Uiso 0.109(4) 1 d P D 2 Cl2" Cl 0.3472(7) 0.4108(5) 0.1311(4) 0.0456(17) Uiso 0.087(4) 1 d P B 2 Cl3" Cl 0.4019(8) 0.4479(6) 0.0084(4) 0.051(2) Uiso 0.087(4) 1 d P B 2 Cl1" Cl 0.1834(5) 0.4349(4) 0.0702(3) 0.0244(11) Uiso 0.087(4) 1 d P B 2 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 0.01154(3) 0.01034(3) 0.01723(3) -0.00087(2) 0.00022(2) 0.00042(2) C1 0.0113(3) 0.0165(5) 0.0250(4) 0.0023(3) 0.0023(3) 0.0005(3) O1 0.0121(2) 0.0188(4) 0.0185(3) -0.0001(2) 0.0025(2) 0.0018(2) P1 0.01276(9) 0.01153(11) 0.01441(9) -0.00076(7) -0.00056(7) 0.00149(7) P2 0.01369(9) 0.01232(11) 0.01346(9) 0.00032(7) 0.00039(7) 0.00029(7) C2 0.0146(3) 0.0187(5) 0.0290(5) 0.0019(4) -0.0034(3) -0.0020(3) O2 0.0159(3) 0.0152(4) 0.0214(3) 0.0009(3) 0.0026(2) -0.0007(2) C3 0.0148(3) 0.0171(5) 0.0233(4) -0.0003(3) 0.0000(3) -0.0051(3) C4 0.0151(3) 0.0144(4) 0.0188(4) -0.0010(3) 0.0005(3) -0.0028(3) C5 0.0181(4) 0.0174(5) 0.0192(4) -0.0039(3) 0.0021(3) -0.0037(3) C6 0.0171(4) 0.0161(5) 0.0185(4) -0.0036(3) 0.0035(3) -0.0012(3) C7 0.0135(3) 0.0149(4) 0.0188(4) -0.0022(3) 0.0026(3) -0.0010(3) C8 0.0124(3) 0.0122(4) 0.0154(3) -0.0006(3) 0.0007(2) 0.0001(3) C9 0.0119(3) 0.0138(4) 0.0159(3) -0.0001(3) 0.0014(3) -0.0001(3) C10 0.0205(4) 0.0173(5) 0.0336(6) 0.0045(4) 0.0037(4) -0.0042(4) C11 0.0228(5) 0.0321(7) 0.0280(5) -0.0045(5) -0.0027(4) -0.0112(4) C12 0.0235(5) 0.0296(6) 0.0237(5) -0.0084(4) 0.0083(4) -0.0024(4) C13 0.0164(4) 0.0224(6) 0.0336(6) 0.0058(4) 0.0105(4) 0.0017(4) C14 0.0168(4) 0.0253(6) 0.0333(6) 0.0027(4) 0.0103(4) 0.0029(4) C15 0.0158(4) 0.0223(5) 0.0240(5) 0.0023(4) 0.0066(3) 0.0047(3) C16 0.0236(4) 0.0265(6) 0.0224(5) 0.0000(4) 0.0081(4) 0.0082(4) C17 0.0240(4) 0.0206(5) 0.0186(4) -0.0015(3) 0.0026(3) 0.0082(4) C18 0.0195(4) 0.0169(5) 0.0172(4) -0.0009(3) 0.0004(3) 0.0038(3) C19 0.0143(3) 0.0155(4) 0.0156(4) 0.0005(3) 0.0011(3) 0.0031(3) C20 0.0138(3) 0.0163(5) 0.0189(4) 0.0009(3) 0.0023(3) 0.0027(3) C21 0.0147(4) 0.0283(7) 0.0506(8) 0.0016(6) 0.0037(4) 0.0045(4) C22 0.0311(6) 0.0400(9) 0.0450(8) 0.0011(6) 0.0238(6) -0.0005(6) C23 0.0365(6) 0.0263(6) 0.0202(5) -0.0044(4) 0.0019(4) 0.0106(5) C24 0.0200(4) 0.0203(5) 0.0143(4) 0.0009(3) 0.0013(3) 0.0045(3) C25 0.0287(5) 0.0294(6) 0.0165(4) -0.0056(4) -0.0019(4) 0.0090(4) C26 0.0283(5) 0.0314(7) 0.0217(5) 0.0097(4) 0.0041(4) 0.0024(4) C27 0.0163(3) 0.0136(4) 0.0230(4) -0.0014(3) -0.0036(3) 0.0029(3) C28 0.0233(4) 0.0206(5) 0.0266(5) -0.0007(4) -0.0087(4) 0.0044(4) C29 0.0264(5) 0.0136(5) 0.0345(6) 0.0016(4) -0.0058(4) 0.0036(4) C30 0.0214(4) 0.0154(5) 0.0144(4) -0.0002(3) 0.0001(3) -0.0024(3) C31 0.0315(5) 0.0195(5) 0.0170(4) -0.0021(3) 0.0074(4) -0.0025(4) C32 0.0291(5) 0.0231(6) 0.0210(5) 0.0021(4) -0.0078(4) -0.0047(4) C33 0.0194(4) 0.0134(4) 0.0200(4) 0.0014(3) -0.0019(3) 0.0013(3) C34 0.0210(4) 0.0207(5) 0.0283(5) 0.0044(4) -0.0020(4) 0.0048(4) C35 0.0246(4) 0.0180(5) 0.0235(5) 0.0049(4) -0.0004(4) -0.0028(4) C36 0.0184(4) 0.0162(5) 0.0279(5) -0.0033(4) -0.0049(3) -0.0003(3) C37 0.0134(3) 0.0146(5) 0.0314(5) -0.0013(4) -0.0019(3) 0.0008(3) C38 0.0141(4) 0.0188(5) 0.0375(6) 0.0003(4) 0.0040(4) -0.0009(3) C39 0.0166(4) 0.0181(5) 0.0287(5) 0.0030(4) 0.0043(3) -0.0009(3) C40 0.0163(4) 0.0122(5) 0.0334(5) 0.0010(4) 0.0011(3) -0.0010(3) C41 0.0200(4) 0.0143(5) 0.0372(6) -0.0053(4) -0.0024(4) -0.0015(3) C42 0.0162(4) 0.0170(5) 0.0502(8) -0.0009(5) -0.0011(4) -0.0032(4) C1SA 0.0407(7) 0.0291(7) 0.0341(7) -0.0036(5) 0.0026(5) 0.0011(6) Cl1A 0.0421(3) 0.0434(3) 0.0549(5) -0.0153(3) -0.0043(3) 0.0061(2) Cl2A 0.0332(2) 0.0660(6) 0.0373(2) 0.0026(2) -0.00379(16) -0.0085(3) Cl3A 0.0712(6) 0.0551(4) 0.0715(4) 0.0267(4) 0.0323(4) 0.0093(4) C1SB 0.0434(7) 0.0232(7) 0.0292(6) -0.0024(5) -0.0030(5) -0.0029(5) Cl1B 0.1121(8) 0.0511(6) 0.0595(7) 0.0298(5) -0.0244(5) -0.0199(5) Cl2B 0.0586(5) 0.0458(5) 0.0582(3) 0.0028(3) -0.0044(3) -0.0222(4) Cl3B 0.0466(4) 0.0505(4) 0.0596(5) -0.0190(3) -0.0162(4) 0.0104(3) B1S 0.0180(5) 0.0224(7) 0.0428(8) -0.0070(5) 0.0007(5) 0.0017(4) F1S 0.0670(8) 0.0416(6) 0.0581(7) -0.0158(5) -0.0283(6) 0.0120(5) F2S 0.0297(4) 0.0318(5) 0.0893(9) 0.0028(5) 0.0266(5) -0.0007(4) F3S 0.0286(4) 0.0259(4) 0.0443(5) -0.0098(3) 0.0099(3) -0.0054(3) F4S 0.0269(4) 0.0310(5) 0.0566(6) -0.0138(4) -0.0013(4) 0.0121(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 C40 2.1828(11) . ? Rh1 C39 2.1870(11) . ? Rh1 C36 2.1937(11) . ? Rh1 C37 2.2024(10) . ? Rh1 P2 2.3717(3) . ? Rh1 P1 2.3854(3) . ? C1 O2 1.4412(14) . ? C1 O1 1.4415(12) . ? C1 C2 1.5316(16) . ? C1 C13 1.5439(15) . ? O1 C9 1.3833(12) . ? P1 C8 1.8384(10) . ? P1 C24 1.8510(11) . ? P1 C27 1.8729(10) . ? P2 C19 1.8331(10) . ? P2 C30 1.8520(11) . ? P2 C33 1.8741(11) . ? C2 C3 1.5398(17) . ? O2 C20 1.3803(14) . ? C3 C4 1.5222(14) . ? C3 C11 1.5335(16) . ? C3 C10 1.5414(16) . ? C4 C5 1.3944(15) . ? C4 C9 1.4060(14) . ? C5 C6 1.4006(14) . ? C6 C7 1.3911(14) . ? C6 C12 1.5133(15) . ? C7 C8 1.4108(13) . ? C8 C9 1.4001(13) . ? C13 C14 1.5416(18) . ? C14 C15 1.5203(17) . ? C14 C22 1.5324(19) . ? C14 C21 1.5434(19) . ? C15 C16 1.3944(18) . ? C15 C20 1.4054(14) . ? C16 C17 1.3995(19) . ? C17 C18 1.3957(15) . ? C17 C23 1.5091(17) . ? C18 C19 1.4111(15) . ? C19 C20 1.3955(15) . ? C24 C26 1.5330(17) . ? C24 C25 1.5374(17) . ? C27 C29 1.5344(17) . ? C27 C28 1.5361(15) . ? C30 C32 1.5329(15) . ? C30 C31 1.5427(16) . ? C33 C35 1.5353(16) . ? C33 C34 1.5400(15) . ? C36 C37 1.3913(17) . ? C36 C41 1.5355(18) . ? C37 C38 1.5382(18) . ? C38 C39 1.5374(16) . ? C38 C42 1.5490(19) . ? C39 C40 1.3908(17) . ? C40 C41 1.5390(17) . ? C41 C42 1.5481(18) . ? C1SA Cl2" 1.709(7) . ? C1SA Cl3A 1.7496(18) . ? C1SA Cl1A 1.7585(18) . ? C1SA Cl2A 1.7632(17) . ? C1SA Cl1" 1.774(7) . ? C1SA Cl3" 1.813(9) . ? C1SB Cl3' 1.586(6) . ? C1SB Cl1B 1.741(2) . ? C1SB Cl2B 1.7584(16) . ? C1SB Cl3B 1.7799(18) . ? C1SB Cl2' 1.818(6) . ? C1SB Cl1' 1.822(9) . ? B1S F4S 1.3875(17) . ? B1S F1S 1.389(2) . ? B1S F2S 1.3901(19) . ? B1S F3S 1.4007(18) . ? Cl2" Cl1" 2.415(13) . ? 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 C40 Rh1 C39 37.12(5) . . ? C40 Rh1 C36 65.74(4) . . ? C39 Rh1 C36 77.59(5) . . ? C40 Rh1 C37 77.92(4) . . ? C39 Rh1 C37 65.40(4) . . ? C36 Rh1 C37 36.90(4) . . ? C40 Rh1 P2 93.82(3) . . ? C39 Rh1 P2 100.30(3) . . ? C36 Rh1 P2 149.24(3) . . ? C37 Rh1 P2 164.75(3) . . ? C40 Rh1 P1 163.47(3) . . ? C39 Rh1 P1 151.91(3) . . ? C36 Rh1 P1 99.95(3) . . ? C37 Rh1 P1 95.62(3) . . ? P2 Rh1 P1 95.594(9) . . ? O2 C1 O1 107.18(8) . . ? O2 C1 C2 103.84(9) . . ? O1 C1 C2 112.79(9) . . ? O2 C1 C13 112.61(9) . . ? O1 C1 C13 104.04(8) . . ? C2 C1 C13 116.25(9) . . ? C9 O1 C1 116.05(8) . . ? C8 P1 C24 110.57(5) . . ? C8 P1 C27 99.36(5) . . ? C24 P1 C27 108.32(5) . . ? C8 P1 Rh1 111.95(3) . . ? C24 P1 Rh1 111.33(4) . . ? C27 P1 Rh1 114.70(4) . . ? C19 P2 C30 112.74(5) . . ? C19 P2 C33 99.47(5) . . ? C30 P2 C33 108.45(5) . . ? C19 P2 Rh1 107.95(3) . . ? C30 P2 Rh1 110.84(4) . . ? C33 P2 Rh1 116.99(3) . . ? C1 C2 C3 113.94(9) . . ? C20 O2 C1 115.51(8) . . ? C4 C3 C11 112.68(9) . . ? C4 C3 C2 105.59(9) . . ? C11 C3 C2 107.70(10) . . ? C4 C3 C10 111.34(9) . . ? C11 C3 C10 108.62(10) . . ? C2 C3 C10 110.83(10) . . ? C5 C4 C9 118.45(9) . . ? C5 C4 C3 125.05(9) . . ? C9 C4 C3 116.41(9) . . ? C4 C5 C6 121.41(9) . . ? C7 C6 C5 118.52(9) . . ? C7 C6 C12 120.31(9) . . ? C5 C6 C12 121.16(10) . . ? C6 C7 C8 122.36(9) . . ? C9 C8 C7 117.12(9) . . ? C9 C8 P1 128.32(7) . . ? C7 C8 P1 114.48(7) . . ? O1 C9 C8 119.94(8) . . ? O1 C9 C4 117.94(8) . . ? C8 C9 C4 122.11(9) . . ? C14 C13 C1 113.68(10) . . ? C15 C14 C22 112.94(12) . . ? C15 C14 C13 106.58(9) . . ? C22 C14 C13 108.45(11) . . ? C15 C14 C21 109.60(11) . . ? C22 C14 C21 108.50(11) . . ? C13 C14 C21 110.78(12) . . ? C16 C15 C20 118.29(11) . . ? C16 C15 C14 125.92(10) . . ? C20 C15 C14 115.77(11) . . ? C15 C16 C17 121.41(10) . . ? C18 C17 C16 118.65(11) . . ? C18 C17 C23 119.83(11) . . ? C16 C17 C23 121.45(11) . . ? C17 C18 C19 121.87(11) . . ? C20 C19 C18 117.39(9) . . ? C20 C19 P2 128.17(8) . . ? C18 C19 P2 114.32(8) . . ? O2 C20 C19 119.50(9) . . ? O2 C20 C15 118.22(10) . . ? C19 C20 C15 122.26(10) . . ? C26 C24 C25 111.27(10) . . ? C26 C24 P1 117.68(8) . . ? C25 C24 P1 109.73(8) . . ? C29 C27 C28 108.98(9) . . ? C29 C27 P1 114.90(7) . . ? C28 C27 P1 114.75(8) . . ? C32 C30 C31 111.43(9) . . ? C32 C30 P2 118.57(8) . . ? C31 C30 P2 108.01(7) . . ? C35 C33 C34 109.57(9) . . ? C35 C33 P2 113.91(8) . . ? C34 C33 P2 114.79(8) . . ? C37 C36 C41 106.62(11) . . ? C37 C36 Rh1 71.89(6) . . ? C41 C36 Rh1 96.28(7) . . ? C36 C37 C38 106.29(10) . . ? C36 C37 Rh1 71.21(6) . . ? C38 C37 Rh1 96.45(7) . . ? C39 C38 C37 100.89(8) . . ? C39 C38 C42 100.22(10) . . ? C37 C38 C42 100.61(11) . . ? C40 C39 C38 106.91(10) . . ? C40 C39 Rh1 71.28(7) . . ? C38 C39 Rh1 97.10(7) . . ? C39 C40 C41 105.99(10) . . ? C39 C40 Rh1 71.61(7) . . ? C41 C40 Rh1 96.62(7) . . ? C36 C41 C40 101.17(9) . . ? C36 C41 C42 100.53(10) . . ? C40 C41 C42 100.60(11) . . ? C41 C42 C38 93.83(9) . . ? Cl2" C1SA Cl3A 107.1(3) . . ? Cl2" C1SA Cl1A 98.4(4) . . ? Cl3A C1SA Cl1A 109.79(11) . . ? Cl2" C1SA Cl2A 18.6(4) . . ? Cl3A C1SA Cl2A 111.91(11) . . ? Cl1A C1SA Cl2A 112.02(11) . . ? Cl2" C1SA Cl1" 87.8(5) . . ? Cl3A C1SA Cl1" 113.1(2) . . ? Cl1A C1SA Cl1" 10.7(2) . . ? Cl2A C1SA Cl1" 101.7(2) . . ? Cl2" C1SA Cl3" 100.0(4) . . ? Cl3A C1SA Cl3" 14.9(3) . . ? Cl1A C1SA Cl3" 124.4(4) . . ? Cl2A C1SA Cl3" 100.9(3) . . ? Cl1" C1SA Cl3" 126.8(4) . . ? Cl3' C1SB Cl1B 126.6(2) . . ? Cl3' C1SB Cl2B 97.1(2) . . ? Cl1B C1SB Cl2B 110.71(10) . . ? Cl3' C1SB Cl3B 17.5(2) . . ? Cl1B C1SB Cl3B 109.51(11) . . ? Cl2B C1SB Cl3B 109.16(9) . . ? Cl3' C1SB Cl2' 115.2(3) . . ? Cl1B C1SB Cl2' 99.4(2) . . ? Cl2B C1SB Cl2' 18.3(2) . . ? Cl3B C1SB Cl2' 127.3(2) . . ? Cl3' C1SB Cl1' 120.3(3) . . ? Cl1B C1SB Cl1' 7.8(3) . . ? Cl2B C1SB Cl1' 109.1(3) . . ? Cl3B C1SB Cl1' 103.5(2) . . ? Cl2' C1SB Cl1' 99.9(3) . . ? F4S B1S F1S 109.41(13) . . ? F4S B1S F2S 110.04(14) . . ? F1S B1S F2S 110.91(13) . . ? F4S B1S F3S 109.98(11) . . ? F1S B1S F3S 108.57(14) . . ? F2S B1S F3S 107.91(12) . . ? C1SA Cl2" Cl1" 47.2(3) . . ? C1SA Cl1" Cl2" 45.0(3) . . ? 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 O2 C1 O1 C9 75.77(11) . . . . ? C2 C1 O1 C9 -37.90(12) . . . . ? C13 C1 O1 C9 -164.74(9) . . . . ? C40 Rh1 P1 C8 -177.34(11) . . . . ? C39 Rh1 P1 C8 71.48(8) . . . . ? C36 Rh1 P1 C8 153.73(5) . . . . ? C37 Rh1 P1 C8 116.72(5) . . . . ? P2 Rh1 P1 C8 -52.92(3) . . . . ? C40 Rh1 P1 C24 -53.01(11) . . . . ? C39 Rh1 P1 C24 -164.19(7) . . . . ? C36 Rh1 P1 C24 -81.94(5) . . . . ? C37 Rh1 P1 C24 -118.95(5) . . . . ? P2 Rh1 P1 C24 71.41(4) . . . . ? C40 Rh1 P1 C27 70.43(11) . . . . ? C39 Rh1 P1 C27 -40.75(8) . . . . ? C36 Rh1 P1 C27 41.50(5) . . . . ? C37 Rh1 P1 C27 4.49(5) . . . . ? P2 Rh1 P1 C27 -165.15(4) . . . . ? C40 Rh1 P2 C19 109.88(5) . . . . ? C39 Rh1 P2 C19 146.74(5) . . . . ? C36 Rh1 P2 C19 63.74(8) . . . . ? C37 Rh1 P2 C19 166.34(12) . . . . ? P1 Rh1 P2 C19 -56.51(4) . . . . ? C40 Rh1 P2 C30 -126.20(5) . . . . ? C39 Rh1 P2 C30 -89.34(5) . . . . ? C36 Rh1 P2 C30 -172.33(7) . . . . ? C37 Rh1 P2 C30 -69.74(12) . . . . ? P1 Rh1 P2 C30 67.41(4) . . . . ? C40 Rh1 P2 C33 -1.17(5) . . . . ? C39 Rh1 P2 C33 35.69(5) . . . . ? C36 Rh1 P2 C33 -47.30(8) . . . . ? C37 Rh1 P2 C33 55.29(13) . . . . ? P1 Rh1 P2 C33 -167.56(4) . . . . ? O2 C1 C2 C3 -129.33(9) . . . . ? O1 C1 C2 C3 -13.64(13) . . . . ? C13 C1 C2 C3 106.40(11) . . . . ? O1 C1 O2 C20 71.05(10) . . . . ? C2 C1 O2 C20 -169.36(8) . . . . ? C13 C1 O2 C20 -42.76(11) . . . . ? C1 C2 C3 C4 52.51(12) . . . . ? C1 C2 C3 C11 173.14(9) . . . . ? C1 C2 C3 C10 -68.18(11) . . . . ? C11 C3 C4 C5 13.23(16) . . . . ? C2 C3 C4 C5 130.54(12) . . . . ? C10 C3 C4 C5 -109.11(13) . . . . ? C11 C3 C4 C9 -163.29(11) . . . . ? C2 C3 C4 C9 -45.98(12) . . . . ? C10 C3 C4 C9 74.37(13) . . . . ? C9 C4 C5 C6 -1.30(17) . . . . ? C3 C4 C5 C6 -177.76(11) . . . . ? C4 C5 C6 C7 -0.30(17) . . . . ? C4 C5 C6 C12 178.27(11) . . . . ? C5 C6 C7 C8 0.96(17) . . . . ? C12 C6 C7 C8 -177.63(11) . . . . ? C6 C7 C8 C9 0.03(16) . . . . ? C6 C7 C8 P1 177.07(9) . . . . ? C24 P1 C8 C9 -13.86(11) . . . . ? C27 P1 C8 C9 -127.57(10) . . . . ? Rh1 P1 C8 C9 110.89(9) . . . . ? C24 P1 C8 C7 169.49(8) . . . . ? C27 P1 C8 C7 55.78(9) . . . . ? Rh1 P1 C8 C7 -65.75(8) . . . . ? C1 O1 C9 C8 -133.07(10) . . . . ? C1 O1 C9 C4 47.85(13) . . . . ? C7 C8 C9 O1 179.24(9) . . . . ? P1 C8 C9 O1 2.67(14) . . . . ? C7 C8 C9 C4 -1.71(15) . . . . ? P1 C8 C9 C4 -178.28(8) . . . . ? C5 C4 C9 O1 -178.59(10) . . . . ? C3 C4 C9 O1 -1.83(14) . . . . ? C5 C4 C9 C8 2.35(16) . . . . ? C3 C4 C9 C8 179.11(9) . . . . ? O2 C1 C13 C14 -7.06(13) . . . . ? O1 C1 C13 C14 -122.79(10) . . . . ? C2 C1 C13 C14 112.57(12) . . . . ? C1 C13 C14 C15 49.14(13) . . . . ? C1 C13 C14 C22 171.02(11) . . . . ? C1 C13 C14 C21 -70.02(13) . . . . ? C22 C14 C15 C16 11.89(18) . . . . ? C13 C14 C15 C16 130.88(12) . . . . ? C21 C14 C15 C16 -109.20(14) . . . . ? C22 C14 C15 C20 -166.90(11) . . . . ? C13 C14 C15 C20 -47.91(14) . . . . ? C21 C14 C15 C20 72.01(13) . . . . ? C20 C15 C16 C17 -1.56(17) . . . . ? C14 C15 C16 C17 179.67(11) . . . . ? C15 C16 C17 C18 -1.63(17) . . . . ? C15 C16 C17 C23 175.24(11) . . . . ? C16 C17 C18 C19 3.06(16) . . . . ? C23 C17 C18 C19 -173.87(10) . . . . ? C17 C18 C19 C20 -1.19(15) . . . . ? C17 C18 C19 P2 175.08(8) . . . . ? C30 P2 C19 C20 -7.58(11) . . . . ? C33 P2 C19 C20 -122.28(9) . . . . ? Rh1 P2 C19 C20 115.19(9) . . . . ? C30 P2 C19 C18 176.64(7) . . . . ? C33 P2 C19 C18 61.94(8) . . . . ? Rh1 P2 C19 C18 -60.60(8) . . . . ? C1 O2 C20 C19 -133.25(9) . . . . ? C1 O2 C20 C15 47.71(12) . . . . ? C18 C19 C20 O2 178.82(9) . . . . ? P2 C19 C20 O2 3.14(14) . . . . ? C18 C19 C20 C15 -2.18(15) . . . . ? P2 C19 C20 C15 -177.86(8) . . . . ? C16 C15 C20 O2 -177.45(10) . . . . ? C14 C15 C20 O2 1.44(14) . . . . ? C16 C15 C20 C19 3.54(16) . . . . ? C14 C15 C20 C19 -177.57(10) . . . . ? C8 P1 C24 C26 -63.02(9) . . . . ? C27 P1 C24 C26 44.87(10) . . . . ? Rh1 P1 C24 C26 171.87(8) . . . . ? C8 P1 C24 C25 168.41(7) . . . . ? C27 P1 C24 C25 -83.70(8) . . . . ? Rh1 P1 C24 C25 43.30(8) . . . . ? C8 P1 C27 C29 42.22(9) . . . . ? C24 P1 C27 C29 -73.22(10) . . . . ? Rh1 P1 C27 C29 161.74(8) . . . . ? C8 P1 C27 C28 169.72(9) . . . . ? C24 P1 C27 C28 54.28(10) . . . . ? Rh1 P1 C27 C28 -70.76(9) . . . . ? C19 P2 C30 C32 -68.86(10) . . . . ? C33 P2 C30 C32 40.28(10) . . . . ? Rh1 P2 C30 C32 170.00(8) . . . . ? C19 P2 C30 C31 163.22(7) . . . . ? C33 P2 C30 C31 -87.64(8) . . . . ? Rh1 P2 C30 C31 42.08(8) . . . . ? C19 P2 C33 C35 172.28(8) . . . . ? C30 P2 C33 C35 54.32(9) . . . . ? Rh1 P2 C33 C35 -71.90(8) . . . . ? C19 P2 C33 C34 44.81(9) . . . . ? C30 P2 C33 C34 -73.14(9) . . . . ? Rh1 P2 C33 C34 160.64(7) . . . . ? C40 Rh1 C36 C37 102.58(8) . . . . ? C39 Rh1 C36 C37 65.37(7) . . . . ? P2 Rh1 C36 C37 154.68(6) . . . . ? P1 Rh1 C36 C37 -86.10(7) . . . . ? C40 Rh1 C36 C41 -2.88(7) . . . . ? C39 Rh1 C36 C41 -40.10(7) . . . . ? C37 Rh1 C36 C41 -105.47(11) . . . . ? P2 Rh1 C36 C41 49.22(11) . . . . ? P1 Rh1 C36 C41 168.43(7) . . . . ? C41 C36 C37 C38 -0.10(11) . . . . ? Rh1 C36 C37 C38 -91.39(7) . . . . ? C41 C36 C37 Rh1 91.29(7) . . . . ? C40 Rh1 C37 C36 -65.50(8) . . . . ? C39 Rh1 C37 C36 -102.48(8) . . . . ? P2 Rh1 C37 C36 -123.76(12) . . . . ? P1 Rh1 C37 C36 99.10(7) . . . . ? C40 Rh1 C37 C38 39.55(7) . . . . ? C39 Rh1 C37 C38 2.58(7) . . . . ? C36 Rh1 C37 C38 105.05(10) . . . . ? P2 Rh1 C37 C38 -18.71(17) . . . . ? P1 Rh1 C37 C38 -155.85(7) . . . . ? C36 C37 C38 C39 68.87(11) . . . . ? Rh1 C37 C38 C39 -3.39(9) . . . . ? C36 C37 C38 C42 -33.83(10) . . . . ? Rh1 C37 C38 C42 -106.10(7) . . . . ? C37 C38 C39 C40 -69.11(11) . . . . ? C42 C38 C39 C40 33.91(12) . . . . ? C37 C38 C39 Rh1 3.42(9) . . . . ? C42 C38 C39 Rh1 106.44(9) . . . . ? C36 Rh1 C39 C40 66.03(7) . . . . ? C37 Rh1 C39 C40 102.92(8) . . . . ? P2 Rh1 C39 C40 -82.65(6) . . . . ? P1 Rh1 C39 C40 153.92(6) . . . . ? C40 Rh1 C39 C38 -105.50(10) . . . . ? C36 Rh1 C39 C38 -39.47(8) . . . . ? C37 Rh1 C39 C38 -2.58(7) . . . . ? P2 Rh1 C39 C38 171.85(7) . . . . ? P1 Rh1 C39 C38 48.42(12) . . . . ? C38 C39 C40 C41 0.14(12) . . . . ? Rh1 C39 C40 C41 -91.78(8) . . . . ? C38 C39 C40 Rh1 91.92(8) . . . . ? C36 Rh1 C40 C39 -101.82(7) . . . . ? C37 Rh1 C40 C39 -65.00(7) . . . . ? P2 Rh1 C40 C39 102.04(6) . . . . ? P1 Rh1 C40 C39 -133.32(10) . . . . ? C39 Rh1 C40 C41 104.70(9) . . . . ? C36 Rh1 C40 C41 2.88(7) . . . . ? C37 Rh1 C40 C41 39.70(7) . . . . ? P2 Rh1 C40 C41 -153.26(7) . . . . ? P1 Rh1 C40 C41 -28.63(15) . . . . ? C37 C36 C41 C40 -69.13(11) . . . . ? Rh1 C36 C41 C40 3.80(9) . . . . ? C37 C36 C41 C42 34.02(11) . . . . ? Rh1 C36 C41 C42 106.95(8) . . . . ? C39 C40 C41 C36 68.89(11) . . . . ? Rh1 C40 C41 C36 -3.82(9) . . . . ? C39 C40 C41 C42 -34.21(12) . . . . ? Rh1 C40 C41 C42 -106.92(8) . . . . ? C36 C41 C42 C38 -51.60(11) . . . . ? C40 C41 C42 C38 52.01(11) . . . . ? C39 C38 C42 C41 -51.66(11) . . . . ? C37 C38 C42 C41 51.58(10) . . . . ? Cl3A C1SA Cl2" Cl1" 113.5(3) . . . . ? Cl1A C1SA Cl2" Cl1" -0.3(2) . . . . ? Cl2A C1SA Cl2" Cl1" -138.5(8) . . . . ? Cl3" C1SA Cl2" Cl1" 127.0(4) . . . . ? Cl3A C1SA Cl1" Cl2" -107.7(4) . . . . ? Cl1A C1SA Cl1" Cl2" 178.5(13) . . . . ? Cl2A C1SA Cl1" Cl2" 12.5(3) . . . . ? Cl3" C1SA Cl1" Cl2" -100.8(6) . . . . ? _diffrn_measured_fraction_theta_max 0.923 _diffrn_reflns_theta_full 39.54 _diffrn_measured_fraction_theta_full 0.923 _refine_diff_density_max 1.106 _refine_diff_density_min -0.809 _refine_diff_density_rms 0.080 #===END data_cji40_0m _database_code_depnum_ccdc_archive 'CCDC 286679' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H80 B Cl6 F4 O2 P2 Rh' _chemical_formula_weight 1249.56 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' 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4171(6) _cell_length_b 27.9184(14) _cell_length_c 17.4627(9) _cell_angle_alpha 90.00 _cell_angle_beta 104.4700(10) _cell_angle_gamma 90.00 _cell_volume 5861.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8292 _cell_measurement_theta_min 2.73 _cell_measurement_theta_max 39.18 _exptl_crystal_description Block _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.416 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2600 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6924 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 119031 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -48 _diffrn_reflns_limit_k_max 49 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 39.64 _reflns_number_total 30269 _reflns_number_gt 24476 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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^)+(0.0638P)^2^+6.1836P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 30269 _refine_ls_number_parameters 668 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.004 _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 0.732705(8) 0.167411(3) 0.252793(7) 0.01119(3) Uani 1 1 d . . . P1 P 0.62642(3) 0.109877(12) 0.16456(2) 0.01113(6) Uani 1 1 d . . . C1 C 0.75012(10) -0.03357(4) 0.24725(9) 0.0132(2) Uani 1 1 d . . . O1 O 0.67003(8) -0.00354(3) 0.19536(7) 0.01351(17) Uani 1 1 d . . . P2 P 0.84963(3) 0.111339(12) 0.33698(2) 0.01140(6) Uani 1 1 d . . . C2 C 0.69812(11) -0.06482(5) 0.30081(10) 0.0158(2) Uani 1 1 d . . . H2A H 0.7218 -0.0525 0.3556 0.019 Uiso 1 1 calc R . . H2B H 0.7270 -0.0979 0.3008 0.019 Uiso 1 1 calc R . . O2 O 0.82577(8) -0.00229(3) 0.30059(7) 0.01341(17) Uani 1 1 d . . . C3 C 0.56981(12) -0.06629(5) 0.27543(10) 0.0167(2) Uani 1 1 d . . . C4 C 0.53337(11) -0.01425(5) 0.26848(10) 0.0152(2) Uani 1 1 d . . . C5 C 0.45159(12) 0.00501(5) 0.30080(11) 0.0188(3) Uani 1 1 d . . . H5 H 0.4111 -0.0156 0.3268 0.023 Uiso 1 1 calc R . . C6 C 0.42723(12) 0.05409(5) 0.29607(10) 0.0175(3) Uani 1 1 d . . . C7 C 0.48571(11) 0.08339(5) 0.25631(10) 0.0153(2) Uani 1 1 d . . . H7 H 0.4708 0.1168 0.2537 0.018 Uiso 1 1 calc R . . C8 C 0.56656(10) 0.06531(4) 0.21958(9) 0.0125(2) Uani 1 1 d . . . C9 C 0.59042(10) 0.01649(4) 0.22857(9) 0.0126(2) Uani 1 1 d . . . C10 C 0.52804(14) -0.09215(6) 0.19562(12) 0.0236(3) Uani 1 1 d . . . H10A H 0.4466 -0.0935 0.1819 0.035 Uiso 1 1 calc R . . H10B H 0.5582 -0.1248 0.1997 0.035 Uiso 1 1 calc R . . H10C H 0.5527 -0.0746 0.1545 0.035 Uiso 1 1 calc R . . C11 C 0.52901(14) -0.09366(6) 0.33893(13) 0.0252(3) Uani 1 1 d . . . H11A H 0.5528 -0.0768 0.3896 0.038 Uiso 1 1 calc R . . H11B H 0.5605 -0.1260 0.3444 0.038 Uiso 1 1 calc R . . H11C H 0.4476 -0.0957 0.3235 0.038 Uiso 1 1 calc R . . C12 C 0.34197(14) 0.07427(7) 0.33576(12) 0.0241(3) Uani 1 1 d . . . H12A H 0.3277 0.1079 0.3206 0.036 Uiso 1 1 calc R . . H12B H 0.3702 0.0720 0.3933 0.036 Uiso 1 1 calc R . . H12C H 0.2727 0.0560 0.3191 0.036 Uiso 1 1 calc R . . C13 C 0.80724(12) -0.06130(5) 0.19246(10) 0.0162(2) Uani 1 1 d . . . H13A H 0.7804 -0.0487 0.1380 0.019 Uiso 1 1 calc R . . H13B H 0.7853 -0.0954 0.1918 0.019 Uiso 1 1 calc R . . C14 C 0.93531(12) -0.05795(5) 0.21720(11) 0.0178(3) Uani 1 1 d . . . C15 C 0.96100(11) -0.00479(5) 0.22469(10) 0.0152(2) Uani 1 1 d . . . C16 C 1.03649(12) 0.01881(5) 0.19102(11) 0.0185(3) Uani 1 1 d . . . H16 H 1.0789 0.0009 0.1627 0.022 Uiso 1 1 calc R . . C17 C 1.05090(12) 0.06851(5) 0.19828(10) 0.0176(3) Uani 1 1 d . . . C18 C 0.98986(11) 0.09386(5) 0.24144(10) 0.0153(2) Uani 1 1 d . . . H18 H 0.9991 0.1276 0.2462 0.018 Uiso 1 1 calc R . . C19 C 0.91443(10) 0.07120(4) 0.27845(9) 0.0123(2) Uani 1 1 d . . . C20 C 0.89992(10) 0.02203(4) 0.26726(9) 0.0126(2) Uani 1 1 d . . . C21 C 0.98050(15) -0.08245(6) 0.15311(14) 0.0271(4) Uani 1 1 d . . . H21A H 0.9543 -0.0653 0.1030 0.041 Uiso 1 1 calc R . . H21B H 0.9541 -0.1156 0.1467 0.041 Uiso 1 1 calc R . . H21C H 1.0620 -0.0821 0.1687 0.041 Uiso 1 1 calc R . . C22 C 0.98346(14) -0.08328(6) 0.29680(13) 0.0247(3) Uani 1 1 d . . . H22A H 1.0647 -0.0803 0.3111 0.037 Uiso 1 1 calc R . . H22B H 0.9628 -0.1172 0.2921 0.037 Uiso 1 1 calc R . . H22C H 0.9535 -0.0684 0.3379 0.037 Uiso 1 1 calc R . . C23 C 1.12881(14) 0.09416(7) 0.15798(12) 0.0251(3) Uani 1 1 d . . . H23A H 1.0922 0.0984 0.1018 0.038 Uiso 1 1 calc R . . H23B H 1.1966 0.0751 0.1633 0.038 Uiso 1 1 calc R . . H23C H 1.1481 0.1256 0.1827 0.038 Uiso 1 1 calc R . . C24 C 0.49373(11) 0.13422(4) 0.09995(9) 0.0133(2) Uani 1 1 d . . . H24 H 0.4622 0.1551 0.1355 0.016 Uiso 1 1 calc R . . C25 C 0.50989(11) 0.16766(5) 0.03358(9) 0.0141(2) Uani 1 1 d . . . H25A H 0.5702 0.1908 0.0553 0.017 Uiso 1 1 calc R . . H25B H 0.5317 0.1486 -0.0079 0.017 Uiso 1 1 calc R . . C26 C 0.40193(12) 0.19475(5) -0.00248(10) 0.0167(2) Uani 1 1 d . . . H26A H 0.3826 0.2152 0.0384 0.020 Uiso 1 1 calc R . . H26B H 0.4129 0.2158 -0.0456 0.020 Uiso 1 1 calc R . . C27 C 0.30669(12) 0.15993(6) -0.03522(11) 0.0189(3) Uani 1 1 d . . . H27A H 0.3222 0.1420 -0.0803 0.023 Uiso 1 1 calc R . . H27B H 0.2368 0.1781 -0.0549 0.023 Uiso 1 1 calc R . . C28 C 0.29222(12) 0.12455(6) 0.02836(10) 0.0180(3) Uani 1 1 d . . . H28A H 0.2335 0.1011 0.0046 0.022 Uiso 1 1 calc R . . H28B H 0.2679 0.1421 0.0703 0.022 Uiso 1 1 calc R . . C29 C 0.40068(11) 0.09781(5) 0.06507(10) 0.0159(2) Uani 1 1 d . . . H29A H 0.4224 0.0781 0.0242 0.019 Uiso 1 1 calc R . . H29B H 0.3896 0.0761 0.1073 0.019 Uiso 1 1 calc R . . C30 C 0.70419(11) 0.08054(5) 0.09949(9) 0.0135(2) Uani 1 1 d . . . H30 H 0.7591 0.0585 0.1339 0.016 Uiso 1 1 calc R . . C31 C 0.63476(12) 0.04976(5) 0.03182(10) 0.0160(2) Uani 1 1 d . . . H31A H 0.5948 0.0248 0.0540 0.019 Uiso 1 1 calc R . . H31B H 0.5787 0.0702 -0.0039 0.019 Uiso 1 1 calc R . . C32 C 0.70888(15) 0.02595(6) -0.01544(11) 0.0218(3) Uani 1 1 d . . . H32A H 0.7599 0.0031 0.0190 0.026 Uiso 1 1 calc R . . H32B H 0.6619 0.0077 -0.0601 0.026 Uiso 1 1 calc R . . C33 C 0.77680(15) 0.06323(6) -0.04736(11) 0.0229(3) Uani 1 1 d . . . H33A H 0.8267 0.0468 -0.0751 0.028 Uiso 1 1 calc R . . H33B H 0.7260 0.0841 -0.0859 0.028 Uiso 1 1 calc R . . C34 C 0.84576(13) 0.09368(6) 0.01956(11) 0.0200(3) Uani 1 1 d . . . H34A H 0.8863 0.1184 -0.0028 0.024 Uiso 1 1 calc R . . H34B H 0.9014 0.0732 0.0553 0.024 Uiso 1 1 calc R . . C35 C 0.77263(12) 0.11810(5) 0.06693(10) 0.0161(2) Uani 1 1 d . . . H35A H 0.7216 0.1410 0.0325 0.019 Uiso 1 1 calc R . . H35B H 0.8201 0.1363 0.1114 0.019 Uiso 1 1 calc R . . C36 C 0.97968(11) 0.13703(5) 0.40346(9) 0.0142(2) Uani 1 1 d . . . H36 H 1.0082 0.1605 0.3699 0.017 Uiso 1 1 calc R . . C37 C 1.07620(12) 0.10150(5) 0.43395(10) 0.0169(2) Uani 1 1 d . . . H37A H 1.0559 0.0787 0.4715 0.020 Uiso 1 1 calc R . . H37B H 1.0901 0.0830 0.3891 0.020 Uiso 1 1 calc R . . C38 C 1.18172(12) 0.12889(6) 0.47536(11) 0.0199(3) Uani 1 1 d . . . H38A H 1.2428 0.1059 0.4956 0.024 Uiso 1 1 calc R . . H38B H 1.2044 0.1501 0.4368 0.024 Uiso 1 1 calc R . . C39 C 1.16203(13) 0.15881(6) 0.54388(11) 0.0204(3) Uani 1 1 d . . . H39A H 1.2302 0.1771 0.5683 0.025 Uiso 1 1 calc R . . H39B H 1.1457 0.1373 0.5846 0.025 Uiso 1 1 calc R . . C40 C 1.06507(13) 0.19352(5) 0.51533(10) 0.0188(3) Uani 1 1 d . . . H40A H 1.0845 0.2171 0.4787 0.023 Uiso 1 1 calc R . . H40B H 1.0513 0.2112 0.5611 0.023 Uiso 1 1 calc R . . C41 C 0.95924(12) 0.16654(5) 0.47296(10) 0.0154(2) Uani 1 1 d . . . H41A H 0.8985 0.1898 0.4530 0.018 Uiso 1 1 calc R . . H41B H 0.9360 0.1449 0.5109 0.018 Uiso 1 1 calc R . . C42 C 0.77585(11) 0.07713(5) 0.39943(9) 0.0140(2) Uani 1 1 d . . . H42 H 0.7242 0.0548 0.3629 0.017 Uiso 1 1 calc R . . C43 C 0.84722(12) 0.04571(5) 0.46503(10) 0.0170(2) Uani 1 1 d . . . H43A H 0.8910 0.0229 0.4416 0.020 Uiso 1 1 calc R . . H43B H 0.9000 0.0662 0.5031 0.020 Uiso 1 1 calc R . . C44 C 0.77404(16) 0.01795(6) 0.50846(12) 0.0236(3) Uani 1 1 d . . . H44A H 0.7263 -0.0047 0.4713 0.028 Uiso 1 1 calc R . . H44B H 0.8219 -0.0009 0.5519 0.028 Uiso 1 1 calc R . . C45 C 0.70088(17) 0.05172(7) 0.54238(12) 0.0272(4) Uani 1 1 d . . . H45A H 0.7484 0.0722 0.5835 0.033 Uiso 1 1 calc R . . H45B H 0.6517 0.0327 0.5675 0.033 Uiso 1 1 calc R . . C46 C 0.63011(14) 0.08328(6) 0.47742(12) 0.0224(3) Uani 1 1 d . . . H46A H 0.5769 0.0629 0.4395 0.027 Uiso 1 1 calc R . . H46B H 0.5867 0.1060 0.5013 0.027 Uiso 1 1 calc R . . C47 C 0.70142(12) 0.11130(5) 0.43313(10) 0.0168(2) Uani 1 1 d . . . H47A H 0.7486 0.1344 0.4696 0.020 Uiso 1 1 calc R . . H47B H 0.6526 0.1296 0.3894 0.020 Uiso 1 1 calc R . . C48 C 0.71703(11) 0.22897(5) 0.17335(9) 0.0143(2) Uani 1 1 d . . . H48 H 0.7124 0.2258 0.1156 0.017 Uiso 1 1 calc R . . C49 C 0.62395(11) 0.22772(5) 0.20417(10) 0.0149(2) Uani 1 1 d . . . H49 H 0.5465 0.2235 0.1706 0.018 Uiso 1 1 calc R . . C50 C 0.65211(13) 0.25879(5) 0.27898(10) 0.0172(2) Uani 1 1 d . . . H50 H 0.5887 0.2701 0.3001 0.021 Uiso 1 1 calc R . . C51 C 0.74186(13) 0.22795(5) 0.33414(10) 0.0165(2) Uani 1 1 d . . . H51 H 0.7469 0.2239 0.3918 0.020 Uiso 1 1 calc R . . C52 C 0.83493(12) 0.22941(5) 0.30312(10) 0.0158(2) Uani 1 1 d . . . H52 H 0.9128 0.2265 0.3365 0.019 Uiso 1 1 calc R . . C53 C 0.80335(12) 0.26077(5) 0.22877(10) 0.0158(2) Uani 1 1 d . . . H53 H 0.8655 0.2736 0.2078 0.019 Uiso 1 1 calc R . . C54 C 0.72616(14) 0.29763(5) 0.25425(10) 0.0192(3) Uani 1 1 d . . . H54A H 0.6850 0.3178 0.2099 0.023 Uiso 1 1 calc R . . H54B H 0.7655 0.3179 0.2990 0.023 Uiso 1 1 calc R . . Cl1B Cl 0.98466(6) 0.20338(2) -0.07517(5) 0.04507(15) Uani 1 1 d . . . C1LB C 0.90160(18) 0.25153(8) -0.06044(18) 0.0371(5) Uani 1 1 d . . . H1LA H 0.8288 0.2496 -0.1009 0.045 Uiso 1 1 calc R . . Cl2B Cl 0.96561(7) 0.30593(2) -0.07317(6) 0.0594(2) Uani 1 1 d . . . Cl3B Cl 0.87634(9) 0.24819(4) 0.03227(7) 0.0718(3) Uani 1 1 d . . . C1LA C 0.23749(19) -0.23020(10) 0.32425(17) 0.0412(6) Uani 1 1 d . . . H1LB H 0.2852 -0.2151 0.2925 0.049 Uiso 1 1 calc R A 1 Cl1A Cl 0.16877(10) -0.28216(3) 0.27343(8) 0.0460(2) Uani 0.864(3) 1 d P B 1 Cl1' Cl 0.2061(5) -0.28322(17) 0.3024(4) 0.0341(10) Uiso 0.136(3) 1 d P B 2 Cl2A Cl 0.13599(9) -0.19025(4) 0.33518(9) 0.0715(4) Uani 0.864(3) 1 d P B 1 Cl2' Cl 0.1353(13) -0.1884(5) 0.2696(10) 0.126(5) Uiso 0.136(3) 1 d P B 2 Cl3A Cl 0.32053(10) -0.24942(8) 0.41587(10) 0.1076(9) Uani 0.864(3) 1 d P B 1 Cl3' Cl 0.2932(8) -0.2185(4) 0.4266(6) 0.074(2) Uiso 0.136(3) 1 d P B 2 B1 B 0.3870(2) -0.21547(11) 0.1728(2) 0.0440(7) Uani 1 1 d . . . F1 F 0.46500(14) -0.20232(5) 0.13522(11) 0.0451(4) Uani 1 1 d . . . F2 F 0.36053(16) -0.26311(6) 0.16226(12) 0.0519(4) Uani 1 1 d . . . F3 F 0.29259(15) -0.18996(8) 0.15894(16) 0.0746(7) Uani 1 1 d . . . F4 F 0.43816(16) -0.20910(10) 0.25540(13) 0.0737(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.01337(4) 0.00922(4) 0.00981(6) 0.00024(3) 0.00071(3) -0.00006(3) P1 0.01261(12) 0.01042(11) 0.00974(18) 0.00087(10) 0.00165(11) -0.00085(9) C1 0.0132(4) 0.0111(4) 0.0147(7) 0.0001(4) 0.0025(4) -0.0008(3) O1 0.0140(4) 0.0134(4) 0.0138(5) 0.0023(3) 0.0048(3) 0.0016(3) P2 0.01316(12) 0.01030(11) 0.00981(18) -0.00021(10) 0.00110(11) 0.00034(9) C2 0.0156(5) 0.0129(4) 0.0183(8) 0.0035(4) 0.0035(5) -0.0012(4) O2 0.0147(4) 0.0120(3) 0.0139(5) -0.0014(3) 0.0043(3) -0.0027(3) C3 0.0159(5) 0.0133(5) 0.0208(8) 0.0039(4) 0.0043(5) -0.0021(4) C4 0.0147(5) 0.0145(5) 0.0173(8) 0.0040(4) 0.0053(4) -0.0010(4) C5 0.0168(5) 0.0203(6) 0.0214(8) 0.0062(5) 0.0088(5) 0.0003(4) C6 0.0153(5) 0.0219(6) 0.0169(8) 0.0042(5) 0.0070(5) 0.0030(4) C7 0.0155(5) 0.0162(5) 0.0145(8) 0.0027(4) 0.0046(4) 0.0024(4) C8 0.0131(4) 0.0128(4) 0.0115(7) 0.0019(4) 0.0029(4) -0.0002(3) C9 0.0130(4) 0.0120(4) 0.0130(7) 0.0019(4) 0.0035(4) -0.0001(3) C10 0.0220(6) 0.0180(6) 0.0280(10) -0.0010(5) 0.0010(6) -0.0050(5) C11 0.0245(6) 0.0197(6) 0.0336(11) 0.0111(6) 0.0115(7) -0.0020(5) C12 0.0207(6) 0.0314(8) 0.0239(10) 0.0057(6) 0.0122(6) 0.0069(5) C13 0.0171(5) 0.0132(5) 0.0182(8) -0.0041(4) 0.0040(5) -0.0005(4) C14 0.0165(5) 0.0140(5) 0.0235(8) -0.0044(5) 0.0062(5) 0.0011(4) C15 0.0143(5) 0.0147(5) 0.0171(8) -0.0031(4) 0.0050(4) 0.0000(4) C16 0.0161(5) 0.0210(6) 0.0208(8) -0.0044(5) 0.0088(5) -0.0023(4) C17 0.0158(5) 0.0210(6) 0.0170(8) -0.0022(5) 0.0060(5) -0.0046(4) C18 0.0162(5) 0.0154(5) 0.0146(7) -0.0011(4) 0.0043(4) -0.0044(4) C19 0.0133(4) 0.0121(4) 0.0111(7) -0.0010(4) 0.0023(4) -0.0015(3) C20 0.0127(4) 0.0119(4) 0.0133(7) -0.0010(4) 0.0036(4) -0.0013(3) C21 0.0257(7) 0.0211(6) 0.0381(12) -0.0118(6) 0.0150(7) 0.0004(5) C22 0.0218(6) 0.0175(6) 0.0318(11) 0.0021(5) 0.0013(6) 0.0037(5) C23 0.0221(6) 0.0312(8) 0.0254(10) -0.0011(6) 0.0119(6) -0.0087(6) C24 0.0142(4) 0.0124(4) 0.0119(7) 0.0018(4) 0.0006(4) -0.0014(3) C25 0.0147(5) 0.0136(4) 0.0128(7) 0.0025(4) 0.0012(4) -0.0015(4) C26 0.0172(5) 0.0160(5) 0.0155(8) 0.0036(4) 0.0013(5) 0.0013(4) C27 0.0145(5) 0.0245(6) 0.0155(8) 0.0047(5) -0.0004(5) 0.0001(4) C28 0.0141(5) 0.0223(6) 0.0164(8) 0.0021(5) 0.0012(5) -0.0028(4) C29 0.0154(5) 0.0156(5) 0.0146(8) 0.0017(4) 0.0000(4) -0.0031(4) C30 0.0155(5) 0.0130(4) 0.0122(7) -0.0002(4) 0.0042(4) -0.0018(3) C31 0.0187(5) 0.0156(5) 0.0141(8) -0.0023(4) 0.0045(5) -0.0035(4) C32 0.0276(7) 0.0194(6) 0.0205(9) -0.0056(5) 0.0101(6) -0.0021(5) C33 0.0260(7) 0.0285(7) 0.0168(9) -0.0029(6) 0.0102(6) -0.0021(5) C34 0.0183(5) 0.0244(6) 0.0193(9) -0.0002(5) 0.0084(5) -0.0026(5) C35 0.0170(5) 0.0159(5) 0.0160(8) 0.0003(4) 0.0055(5) -0.0031(4) C36 0.0146(5) 0.0129(4) 0.0127(7) -0.0013(4) -0.0009(4) 0.0009(3) C37 0.0165(5) 0.0154(5) 0.0161(8) -0.0014(4) -0.0011(5) 0.0029(4) C38 0.0159(5) 0.0217(6) 0.0190(9) -0.0026(5) -0.0011(5) 0.0011(4) C39 0.0193(6) 0.0223(6) 0.0156(9) -0.0029(5) -0.0034(5) -0.0002(4) C40 0.0218(6) 0.0159(5) 0.0155(8) -0.0037(4) -0.0011(5) -0.0010(4) C41 0.0178(5) 0.0136(5) 0.0129(7) -0.0019(4) 0.0003(4) 0.0012(4) C42 0.0166(5) 0.0137(4) 0.0117(7) 0.0014(4) 0.0035(4) 0.0013(4) C43 0.0209(5) 0.0160(5) 0.0143(8) 0.0033(4) 0.0045(5) 0.0038(4) C44 0.0314(7) 0.0209(6) 0.0208(9) 0.0088(5) 0.0111(6) 0.0039(5) C45 0.0337(8) 0.0327(8) 0.0191(10) 0.0085(6) 0.0141(7) 0.0077(7) C46 0.0217(6) 0.0275(7) 0.0206(9) 0.0044(6) 0.0098(6) 0.0043(5) C47 0.0189(5) 0.0175(5) 0.0147(8) 0.0014(4) 0.0055(5) 0.0038(4) C48 0.0171(5) 0.0125(4) 0.0121(7) 0.0003(4) 0.0014(4) -0.0012(4) C49 0.0158(5) 0.0125(4) 0.0151(7) 0.0016(4) 0.0014(4) 0.0017(4) C50 0.0220(6) 0.0141(5) 0.0146(8) -0.0007(4) 0.0028(5) 0.0038(4) C51 0.0225(6) 0.0131(5) 0.0123(7) -0.0003(4) 0.0014(5) 0.0013(4) C52 0.0175(5) 0.0118(4) 0.0153(8) -0.0012(4) -0.0010(4) -0.0009(4) C53 0.0193(5) 0.0127(5) 0.0135(7) 0.0001(4) 0.0004(5) -0.0032(4) C54 0.0289(7) 0.0100(4) 0.0160(8) -0.0006(4) 0.0005(5) 0.0002(4) Cl1B 0.0557(3) 0.0321(2) 0.0595(4) -0.0059(2) 0.0370(3) -0.0008(2) C1LB 0.0279(8) 0.0298(9) 0.0541(16) -0.0005(9) 0.0109(9) -0.0030(7) Cl2B 0.0539(4) 0.0315(3) 0.0782(6) 0.0161(3) -0.0108(4) -0.0134(2) Cl3B 0.0791(6) 0.0768(6) 0.0809(7) -0.0145(5) 0.0603(6) 0.0009(4) C1LA 0.0269(8) 0.0533(14) 0.0463(16) 0.0146(11) 0.0148(9) 0.0043(8) Cl1A 0.0446(5) 0.0449(4) 0.0566(7) 0.0085(4) 0.0281(5) 0.0030(3) Cl2A 0.0573(5) 0.0633(6) 0.1012(11) -0.0287(6) 0.0338(6) 0.0078(4) Cl3A 0.0493(6) 0.1568(18) 0.0905(11) 0.0680(11) -0.0314(6) -0.0444(8) B1 0.0291(10) 0.0470(14) 0.062(2) -0.0229(13) 0.0227(12) -0.0093(9) F1 0.0515(8) 0.0351(7) 0.0593(11) 0.0028(6) 0.0339(8) -0.0014(6) F2 0.0567(10) 0.0455(9) 0.0572(12) 0.0013(7) 0.0214(9) -0.0187(7) F3 0.0358(8) 0.0725(14) 0.112(2) -0.0182(13) 0.0123(10) 0.0138(8) F4 0.0439(9) 0.131(2) 0.0498(13) -0.0266(12) 0.0176(9) -0.0239(11) _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 C48 2.1865(14) . ? Rh1 C49 2.1925(13) . ? Rh1 C51 2.1925(15) . ? Rh1 C52 2.1961(13) . ? Rh1 P2 2.3776(4) . ? Rh1 P1 2.3832(4) . ? P1 C8 1.8386(13) . ? P1 C30 1.8555(14) . ? P1 C24 1.8763(14) . ? C1 O1 1.4362(17) . ? C1 O2 1.4407(17) . ? C1 C2 1.534(2) . ? C1 C13 1.535(2) . ? O1 C9 1.3830(16) . ? P2 C19 1.8327(14) . ? P2 C42 1.8546(14) . ? P2 C36 1.8796(14) . ? C2 C3 1.5439(19) . ? O2 C20 1.3839(16) . ? C3 C4 1.5175(19) . ? C3 C11 1.533(2) . ? C3 C10 1.540(3) . ? C4 C5 1.387(2) . ? C4 C9 1.4039(18) . ? C5 C6 1.401(2) . ? C6 C7 1.389(2) . ? C6 C12 1.512(2) . ? C7 C8 1.4127(19) . ? C8 C9 1.3953(18) . ? C13 C14 1.543(2) . ? C14 C15 1.5170(19) . ? C14 C21 1.533(2) . ? C14 C22 1.541(3) . ? C15 C16 1.391(2) . ? C15 C20 1.4037(19) . ? C16 C17 1.401(2) . ? C17 C18 1.389(2) . ? C17 C23 1.511(2) . ? C18 C19 1.4134(19) . ? C19 C20 1.3920(17) . ? C24 C25 1.540(2) . ? C24 C29 1.5453(18) . ? C25 C26 1.5310(19) . ? C26 C27 1.527(2) . ? C27 C28 1.530(2) . ? C28 C29 1.533(2) . ? C30 C31 1.539(2) . ? C30 C35 1.5449(19) . ? C31 C32 1.533(2) . ? C32 C33 1.530(2) . ? C33 C34 1.524(3) . ? C34 C35 1.533(2) . ? C36 C41 1.540(2) . ? C36 C37 1.5442(19) . ? C37 C38 1.533(2) . ? C38 C39 1.528(2) . ? C39 C40 1.529(2) . ? C40 C41 1.535(2) . ? C42 C43 1.536(2) . ? C42 C47 1.5434(19) . ? C43 C44 1.532(2) . ? C44 C45 1.528(3) . ? C45 C46 1.529(3) . ? C46 C47 1.529(2) . ? C48 C49 1.392(2) . ? C48 C53 1.535(2) . ? C49 C50 1.534(2) . ? C50 C51 1.541(2) . ? C50 C54 1.551(2) . ? C51 C52 1.394(2) . ? C52 C53 1.533(2) . ? C53 C54 1.545(2) . ? Cl1B C1LB 1.752(2) . ? C1LB Cl3B 1.727(3) . ? C1LB Cl2B 1.754(2) . ? C1LA Cl1' 1.554(6) . ? C1LA Cl2A 1.729(3) . ? C1LA Cl3A 1.757(3) . ? C1LA Cl3' 1.779(10) . ? C1LA Cl1A 1.800(3) . ? C1LA Cl2' 1.811(15) . ? B1 F3 1.341(3) . ? B1 F1 1.349(3) . ? B1 F2 1.371(3) . ? B1 F4 1.435(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 C48 Rh1 C49 37.07(5) . . ? C48 Rh1 C51 77.71(6) . . ? C49 Rh1 C51 65.54(6) . . ? C48 Rh1 C52 65.50(6) . . ? C49 Rh1 C52 77.77(5) . . ? C51 Rh1 C52 37.04(6) . . ? C48 Rh1 P2 148.60(4) . . ? C49 Rh1 P2 165.23(4) . . ? C51 Rh1 P2 100.50(4) . . ? C52 Rh1 P2 93.95(4) . . ? C48 Rh1 P1 99.93(4) . . ? C49 Rh1 P1 94.54(4) . . ? C51 Rh1 P1 150.36(4) . . ? C52 Rh1 P1 164.02(4) . . ? P2 Rh1 P1 96.312(13) . . ? C8 P1 C30 111.19(6) . . ? C8 P1 C24 98.65(6) . . ? C30 P1 C24 107.75(7) . . ? C8 P1 Rh1 110.43(5) . . ? C30 P1 Rh1 113.86(4) . . ? C24 P1 Rh1 113.94(4) . . ? O1 C1 O2 106.91(10) . . ? O1 C1 C2 112.71(10) . . ? O2 C1 C2 104.85(12) . . ? O1 C1 C13 104.83(12) . . ? O2 C1 C13 112.36(10) . . ? C2 C1 C13 115.05(11) . . ? C9 O1 C1 115.23(11) . . ? C19 P2 C42 111.30(6) . . ? C19 P2 C36 98.54(6) . . ? C42 P2 C36 107.92(7) . . ? C19 P2 Rh1 110.06(5) . . ? C42 P2 Rh1 112.81(4) . . ? C36 P2 Rh1 115.36(4) . . ? C1 C2 C3 113.66(12) . . ? C20 O2 C1 114.85(11) . . ? C4 C3 C11 112.89(13) . . ? C4 C3 C10 110.51(13) . . ? C11 C3 C10 108.87(13) . . ? C4 C3 C2 105.26(11) . . ? C11 C3 C2 108.02(13) . . ? C10 C3 C2 111.24(13) . . ? C5 C4 C9 118.45(12) . . ? C5 C4 C3 124.92(12) . . ? C9 C4 C3 116.59(12) . . ? C4 C5 C6 121.61(13) . . ? C7 C6 C5 118.24(13) . . ? C7 C6 C12 121.53(14) . . ? C5 C6 C12 120.20(14) . . ? C6 C7 C8 122.41(13) . . ? C9 C8 C7 116.93(12) . . ? C9 C8 P1 128.14(10) . . ? C7 C8 P1 114.92(9) . . ? O1 C9 C8 120.12(11) . . ? O1 C9 C4 117.59(11) . . ? C8 C9 C4 122.25(12) . . ? C1 C13 C14 113.53(12) . . ? C15 C14 C21 113.09(13) . . ? C15 C14 C22 110.21(14) . . ? C21 C14 C22 108.88(14) . . ? C15 C14 C13 105.26(11) . . ? C21 C14 C13 107.95(14) . . ? C22 C14 C13 111.43(13) . . ? C16 C15 C20 118.81(12) . . ? C16 C15 C14 125.21(13) . . ? C20 C15 C14 115.96(12) . . ? C15 C16 C17 121.02(13) . . ? C18 C17 C16 118.63(13) . . ? C18 C17 C23 120.73(14) . . ? C16 C17 C23 120.62(14) . . ? C17 C18 C19 122.28(13) . . ? C20 C19 C18 117.03(12) . . ? C20 C19 P2 128.44(10) . . ? C18 C19 P2 114.52(9) . . ? O2 C20 C19 120.08(12) . . ? O2 C20 C15 117.74(11) . . ? C19 C20 C15 122.15(12) . . ? C25 C24 C29 109.10(12) . . ? C25 C24 P1 114.34(9) . . ? C29 C24 P1 117.16(9) . . ? C26 C25 C24 110.10(11) . . ? C27 C26 C25 110.85(11) . . ? C26 C27 C28 111.08(13) . . ? C27 C28 C29 111.57(12) . . ? C28 C29 C24 109.67(11) . . ? C31 C30 C35 110.51(12) . . ? C31 C30 P1 116.06(9) . . ? C35 C30 P1 110.13(9) . . ? C32 C31 C30 111.04(12) . . ? C33 C32 C31 111.16(13) . . ? C34 C33 C32 110.83(15) . . ? C33 C34 C35 111.53(12) . . ? C34 C35 C30 110.57(12) . . ? C41 C36 C37 109.79(12) . . ? C41 C36 P2 113.94(9) . . ? C37 C36 P2 116.16(9) . . ? C38 C37 C36 109.92(11) . . ? C39 C38 C37 110.90(13) . . ? C38 C39 C40 111.00(14) . . ? C39 C40 C41 110.84(12) . . ? C40 C41 C36 110.66(12) . . ? C43 C42 C47 110.94(13) . . ? C43 C42 P2 117.06(10) . . ? C47 C42 P2 109.68(9) . . ? C44 C43 C42 110.81(13) . . ? C45 C44 C43 111.33(13) . . ? C44 C45 C46 110.81(15) . . ? C47 C46 C45 111.85(14) . . ? C46 C47 C42 110.76(12) . . ? C49 C48 C53 106.69(13) . . ? C49 C48 Rh1 71.70(8) . . ? C53 C48 Rh1 96.73(9) . . ? C48 C49 C50 106.29(12) . . ? C48 C49 Rh1 71.23(8) . . ? C50 C49 Rh1 96.73(9) . . ? C49 C50 C51 101.06(11) . . ? C49 C50 C54 100.54(13) . . ? C51 C50 C54 100.26(12) . . ? C52 C51 C50 106.32(13) . . ? C52 C51 Rh1 71.62(8) . . ? C50 C51 Rh1 96.51(10) . . ? C51 C52 C53 106.51(12) . . ? C51 C52 Rh1 71.34(8) . . ? C53 C52 Rh1 96.38(9) . . ? C52 C53 C48 101.20(11) . . ? C52 C53 C54 100.49(13) . . ? C48 C53 C54 100.43(11) . . ? C53 C54 C50 93.91(10) . . ? Cl3B C1LB Cl1B 110.34(15) . . ? Cl3B C1LB Cl2B 111.09(15) . . ? Cl1B C1LB Cl2B 110.11(12) . . ? Cl1' C1LA Cl2A 119.8(2) . . ? Cl1' C1LA Cl3A 89.2(3) . . ? Cl2A C1LA Cl3A 112.00(19) . . ? Cl1' C1LA Cl3' 115.6(4) . . ? Cl2A C1LA Cl3' 83.2(3) . . ? Cl3A C1LA Cl3' 31.6(3) . . ? Cl1' C1LA Cl1A 18.6(2) . . ? Cl2A C1LA Cl1A 107.79(13) . . ? Cl3A C1LA Cl1A 107.50(16) . . ? Cl3' C1LA Cl1A 131.4(4) . . ? Cl1' C1LA Cl2' 112.6(6) . . ? Cl2A C1LA Cl2' 37.7(5) . . ? Cl3A C1LA Cl2' 148.4(6) . . ? Cl3' C1LA Cl2' 117.2(6) . . ? Cl1A C1LA Cl2' 94.4(5) . . ? F3 B1 F1 118.0(3) . . ? F3 B1 F2 108.7(2) . . ? F1 B1 F2 112.1(2) . . ? F3 B1 F4 105.2(2) . . ? F1 B1 F4 105.3(2) . . ? F2 B1 F4 106.6(3) . . ? 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 C48 Rh1 P1 C8 -152.63(6) . . . . ? C49 Rh1 P1 C8 -115.63(6) . . . . ? C51 Rh1 P1 C8 -70.06(10) . . . . ? C52 Rh1 P1 C8 -175.99(14) . . . . ? P2 Rh1 P1 C8 54.34(4) . . . . ? C48 Rh1 P1 C30 81.45(6) . . . . ? C49 Rh1 P1 C30 118.45(6) . . . . ? C51 Rh1 P1 C30 164.02(10) . . . . ? C52 Rh1 P1 C30 58.09(15) . . . . ? P2 Rh1 P1 C30 -71.57(5) . . . . ? C48 Rh1 P1 C24 -42.68(6) . . . . ? C49 Rh1 P1 C24 -5.69(6) . . . . ? C51 Rh1 P1 C24 39.89(10) . . . . ? C52 Rh1 P1 C24 -66.05(15) . . . . ? P2 Rh1 P1 C24 164.29(5) . . . . ? O2 C1 O1 C9 -75.18(13) . . . . ? C2 C1 O1 C9 39.51(15) . . . . ? C13 C1 O1 C9 165.36(10) . . . . ? C48 Rh1 P2 C19 -67.88(9) . . . . ? C49 Rh1 P2 C19 -169.84(15) . . . . ? C51 Rh1 P2 C19 -151.45(6) . . . . ? C52 Rh1 P2 C19 -114.67(6) . . . . ? P1 Rh1 P2 C19 53.07(4) . . . . ? C48 Rh1 P2 C42 167.15(9) . . . . ? C49 Rh1 P2 C42 65.20(15) . . . . ? C51 Rh1 P2 C42 83.58(7) . . . . ? C52 Rh1 P2 C42 120.36(7) . . . . ? P1 Rh1 P2 C42 -71.90(5) . . . . ? C48 Rh1 P2 C36 42.50(10) . . . . ? C49 Rh1 P2 C36 -59.46(16) . . . . ? C51 Rh1 P2 C36 -41.07(7) . . . . ? C52 Rh1 P2 C36 -4.29(7) . . . . ? P1 Rh1 P2 C36 163.45(5) . . . . ? O1 C1 C2 C3 13.16(17) . . . . ? O2 C1 C2 C3 129.08(12) . . . . ? C13 C1 C2 C3 -106.97(14) . . . . ? O1 C1 O2 C20 -73.58(13) . . . . ? C2 C1 O2 C20 166.55(10) . . . . ? C13 C1 O2 C20 40.90(15) . . . . ? C1 C2 C3 C4 -52.64(17) . . . . ? C1 C2 C3 C11 -173.49(13) . . . . ? C1 C2 C3 C10 67.08(15) . . . . ? C11 C3 C4 C5 -14.5(2) . . . . ? C10 C3 C4 C5 107.74(18) . . . . ? C2 C3 C4 C5 -132.06(17) . . . . ? C11 C3 C4 C9 163.16(15) . . . . ? C10 C3 C4 C9 -74.64(17) . . . . ? C2 C3 C4 C9 45.56(19) . . . . ? C9 C4 C5 C6 -1.6(3) . . . . ? C3 C4 C5 C6 175.98(16) . . . . ? C4 C5 C6 C7 1.4(3) . . . . ? C4 C5 C6 C12 -176.68(16) . . . . ? C5 C6 C7 C8 1.2(2) . . . . ? C12 C6 C7 C8 179.29(16) . . . . ? C6 C7 C8 C9 -3.5(2) . . . . ? C6 C7 C8 P1 175.92(13) . . . . ? C30 P1 C8 C9 13.19(16) . . . . ? C24 P1 C8 C9 126.13(14) . . . . ? Rh1 P1 C8 C9 -114.22(13) . . . . ? C30 P1 C8 C7 -166.17(11) . . . . ? C24 P1 C8 C7 -53.23(12) . . . . ? Rh1 P1 C8 C7 66.43(12) . . . . ? C1 O1 C9 C8 131.78(13) . . . . ? C1 O1 C9 C4 -50.33(17) . . . . ? C7 C8 C9 O1 -178.92(13) . . . . ? P1 C8 C9 O1 1.7(2) . . . . ? C7 C8 C9 C4 3.3(2) . . . . ? P1 C8 C9 C4 -176.04(12) . . . . ? C5 C4 C9 O1 -178.69(14) . . . . ? C3 C4 C9 O1 3.5(2) . . . . ? C5 C4 C9 C8 -0.9(2) . . . . ? C3 C4 C9 C8 -178.63(14) . . . . ? O1 C1 C13 C14 127.69(12) . . . . ? O2 C1 C13 C14 11.94(17) . . . . ? C2 C1 C13 C14 -107.94(14) . . . . ? C1 C13 C14 C15 -53.01(17) . . . . ? C1 C13 C14 C21 -174.05(13) . . . . ? C1 C13 C14 C22 66.44(16) . . . . ? C21 C14 C15 C16 -13.2(2) . . . . ? C22 C14 C15 C16 108.95(18) . . . . ? C13 C14 C15 C16 -130.79(17) . . . . ? C21 C14 C15 C20 164.76(15) . . . . ? C22 C14 C15 C20 -73.12(17) . . . . ? C13 C14 C15 C20 47.14(19) . . . . ? C20 C15 C16 C17 -0.8(2) . . . . ? C14 C15 C16 C17 177.08(16) . . . . ? C15 C16 C17 C18 1.4(3) . . . . ? C15 C16 C17 C23 -176.85(16) . . . . ? C16 C17 C18 C19 0.3(2) . . . . ? C23 C17 C18 C19 178.58(15) . . . . ? C17 C18 C19 C20 -2.6(2) . . . . ? C17 C18 C19 P2 176.51(13) . . . . ? C42 P2 C19 C20 10.76(16) . . . . ? C36 P2 C19 C20 123.87(14) . . . . ? Rh1 P2 C19 C20 -115.06(13) . . . . ? C42 P2 C19 C18 -168.18(11) . . . . ? C36 P2 C19 C18 -55.07(12) . . . . ? Rh1 P2 C19 C18 65.99(11) . . . . ? C1 O2 C20 C19 131.34(13) . . . . ? C1 O2 C20 C15 -50.57(17) . . . . ? C18 C19 C20 O2 -178.80(13) . . . . ? P2 C19 C20 O2 2.3(2) . . . . ? C18 C19 C20 C15 3.2(2) . . . . ? P2 C19 C20 C15 -175.73(12) . . . . ? C16 C15 C20 O2 -179.64(14) . . . . ? C14 C15 C20 O2 2.3(2) . . . . ? C16 C15 C20 C19 -1.6(2) . . . . ? C14 C15 C20 C19 -179.66(14) . . . . ? C8 P1 C24 C25 -170.07(10) . . . . ? C30 P1 C24 C25 -54.44(11) . . . . ? Rh1 P1 C24 C25 72.93(11) . . . . ? C8 P1 C24 C29 -40.59(12) . . . . ? C30 P1 C24 C29 75.04(12) . . . . ? Rh1 P1 C24 C29 -157.59(10) . . . . ? C29 C24 C25 C26 60.19(15) . . . . ? P1 C24 C25 C26 -166.43(10) . . . . ? C24 C25 C26 C27 -58.33(17) . . . . ? C25 C26 C27 C28 55.34(18) . . . . ? C26 C27 C28 C29 -55.16(18) . . . . ? C27 C28 C29 C24 57.22(18) . . . . ? C25 C24 C29 C28 -59.33(16) . . . . ? P1 C24 C29 C28 168.76(11) . . . . ? C8 P1 C30 C31 64.74(12) . . . . ? C24 P1 C30 C31 -42.33(12) . . . . ? Rh1 P1 C30 C31 -169.74(9) . . . . ? C8 P1 C30 C35 -168.77(10) . . . . ? C24 P1 C30 C35 84.16(11) . . . . ? Rh1 P1 C30 C35 -43.25(11) . . . . ? C35 C30 C31 C32 55.97(16) . . . . ? P1 C30 C31 C32 -177.74(11) . . . . ? C30 C31 C32 C33 -56.23(19) . . . . ? C31 C32 C33 C34 56.2(2) . . . . ? C32 C33 C34 C35 -56.54(19) . . . . ? C33 C34 C35 C30 56.49(18) . . . . ? C31 C30 C35 C34 -55.86(16) . . . . ? P1 C30 C35 C34 174.60(11) . . . . ? C19 P2 C36 C41 -169.40(10) . . . . ? C42 P2 C36 C41 -53.64(11) . . . . ? Rh1 P2 C36 C41 73.52(11) . . . . ? C19 P2 C36 C37 -40.29(13) . . . . ? C42 P2 C36 C37 75.47(13) . . . . ? Rh1 P2 C36 C37 -157.37(10) . . . . ? C41 C36 C37 C38 -58.35(17) . . . . ? P2 C36 C37 C38 170.56(12) . . . . ? C36 C37 C38 C39 58.04(18) . . . . ? C37 C38 C39 C40 -56.91(18) . . . . ? C38 C39 C40 C41 55.99(19) . . . . ? C39 C40 C41 C36 -56.77(18) . . . . ? C37 C36 C41 C40 57.91(15) . . . . ? P2 C36 C41 C40 -169.83(10) . . . . ? C19 P2 C42 C43 65.02(12) . . . . ? C36 P2 C42 C43 -42.06(12) . . . . ? Rh1 P2 C42 C43 -170.69(9) . . . . ? C19 P2 C42 C47 -167.47(10) . . . . ? C36 P2 C42 C47 85.45(11) . . . . ? Rh1 P2 C42 C47 -43.18(11) . . . . ? C47 C42 C43 C44 55.94(17) . . . . ? P2 C42 C43 C44 -177.16(11) . . . . ? C42 C43 C44 C45 -56.5(2) . . . . ? C43 C44 C45 C46 56.1(2) . . . . ? C44 C45 C46 C47 -55.7(2) . . . . ? C45 C46 C47 C42 55.4(2) . . . . ? C43 C42 C47 C46 -55.30(17) . . . . ? P2 C42 C47 C46 173.84(12) . . . . ? C51 Rh1 C48 C49 -65.51(9) . . . . ? C52 Rh1 C48 C49 -102.53(10) . . . . ? P2 Rh1 C48 C49 -155.57(7) . . . . ? P1 Rh1 C48 C49 84.36(8) . . . . ? C49 Rh1 C48 C53 105.40(13) . . . . ? C51 Rh1 C48 C53 39.88(9) . . . . ? C52 Rh1 C48 C53 2.87(8) . . . . ? P2 Rh1 C48 C53 -50.17(13) . . . . ? P1 Rh1 C48 C53 -170.24(8) . . . . ? C53 C48 C49 C50 0.00(15) . . . . ? Rh1 C48 C49 C50 91.70(10) . . . . ? C53 C48 C49 Rh1 -91.70(10) . . . . ? C51 Rh1 C49 C48 102.36(10) . . . . ? C52 Rh1 C49 C48 65.36(9) . . . . ? P2 Rh1 C49 C48 122.28(14) . . . . ? P1 Rh1 C49 C48 -100.47(8) . . . . ? C48 Rh1 C49 C50 -104.97(12) . . . . ? C51 Rh1 C49 C50 -2.61(9) . . . . ? C52 Rh1 C49 C50 -39.61(9) . . . . ? P2 Rh1 C49 C50 17.3(2) . . . . ? P1 Rh1 C49 C50 154.56(8) . . . . ? C48 C49 C50 C51 -68.92(14) . . . . ? Rh1 C49 C50 C51 3.44(11) . . . . ? C48 C49 C50 C54 33.85(14) . . . . ? Rh1 C49 C50 C54 106.21(9) . . . . ? C49 C50 C51 C52 69.26(14) . . . . ? C54 C50 C51 C52 -33.73(15) . . . . ? C49 C50 C51 Rh1 -3.44(11) . . . . ? C54 C50 C51 Rh1 -106.44(10) . . . . ? C48 Rh1 C51 C52 -65.43(9) . . . . ? C49 Rh1 C51 C52 -102.48(10) . . . . ? P2 Rh1 C51 C52 82.58(9) . . . . ? P1 Rh1 C51 C52 -153.93(8) . . . . ? C48 Rh1 C51 C50 39.65(9) . . . . ? C49 Rh1 C51 C50 2.59(9) . . . . ? C52 Rh1 C51 C50 105.08(13) . . . . ? P2 Rh1 C51 C50 -172.34(8) . . . . ? P1 Rh1 C51 C50 -48.85(14) . . . . ? C50 C51 C52 C53 -0.28(15) . . . . ? Rh1 C51 C52 C53 91.28(10) . . . . ? C50 C51 C52 Rh1 -91.56(10) . . . . ? C48 Rh1 C52 C51 102.45(10) . . . . ? C49 Rh1 C52 C51 65.42(9) . . . . ? P2 Rh1 C52 C51 -102.22(8) . . . . ? P1 Rh1 C52 C51 127.87(13) . . . . ? C48 Rh1 C52 C53 -2.87(8) . . . . ? C49 Rh1 C52 C53 -39.89(9) . . . . ? C51 Rh1 C52 C53 -105.31(12) . . . . ? P2 Rh1 C52 C53 152.47(8) . . . . ? P1 Rh1 C52 C53 22.6(2) . . . . ? C51 C52 C53 C48 -68.60(14) . . . . ? Rh1 C52 C53 C48 3.79(11) . . . . ? C51 C52 C53 C54 34.37(14) . . . . ? Rh1 C52 C53 C54 106.76(9) . . . . ? C49 C48 C53 C52 69.05(14) . . . . ? Rh1 C48 C53 C52 -3.81(11) . . . . ? C49 C48 C53 C54 -33.97(14) . . . . ? Rh1 C48 C53 C54 -106.83(10) . . . . ? C52 C53 C54 C50 -52.05(12) . . . . ? C48 C53 C54 C50 51.54(13) . . . . ? C49 C50 C54 C53 -51.67(12) . . . . ? C51 C50 C54 C53 51.74(13) . . . . ? _diffrn_measured_fraction_theta_max 0.852 _diffrn_reflns_theta_full 39.64 _diffrn_measured_fraction_theta_full 0.852 _refine_diff_density_max 2.123 _refine_diff_density_min -2.059 _refine_diff_density_rms 0.111 #===END data_cj27pbcn _database_code_depnum_ccdc_archive 'CCDC 286680' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H78 B F4 O2 P2 Rh' _chemical_formula_weight 1082.88 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' O O 0.0106 0.0060 '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' 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 Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 31.357(10) _cell_length_b 19.516(5) _cell_length_c 20.294(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 12419(6) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5020 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 25.44 _exptl_crystal_description Plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.158 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4560 _exptl_absorpt_coefficient_mu 0.375 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5453 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 108796 _diffrn_reflns_av_R_equivalents 0.1735 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 26.48 _reflns_number_total 11767 _reflns_number_gt 7595 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The crystal contains disordered n-hexane molecules. ; _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^)+(0.0390P)^2^+141.3019P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11767 _refine_ls_number_parameters 745 _refine_ls_number_restraints 78 _refine_ls_R_factor_all 0.1367 _refine_ls_R_factor_gt 0.0777 _refine_ls_wR_factor_ref 0.2172 _refine_ls_wR_factor_gt 0.1813 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.115 _refine_ls_shift/su_max 0.000 _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 0.237285(16) 0.39302(2) 0.27094(3) 0.01514(15) Uani 1 1 d . . . P1 P 0.16580(6) 0.37161(8) 0.23229(10) 0.0176(4) Uani 1 1 d . . . C1 C 0.0750(2) 0.4183(3) 0.3938(4) 0.0199(15) Uani 1 1 d . . . O1 O 0.08313(14) 0.3928(2) 0.3284(2) 0.0177(10) Uani 1 1 d . . . P2 P 0.21702(6) 0.42116(8) 0.38136(9) 0.0157(4) Uani 1 1 d . . . C2 C 0.0556(2) 0.3633(3) 0.4398(4) 0.0204(16) Uani 1 1 d . . . H2A H 0.0312 0.3835 0.4639 0.025 Uiso 1 1 calc R . . H2B H 0.0772 0.3494 0.4727 0.025 Uiso 1 1 calc R . . O2 O 0.11614(15) 0.4349(2) 0.4225(2) 0.0173(10) Uani 1 1 d . . . C3 C 0.0400(2) 0.2985(3) 0.4018(4) 0.0237(17) Uani 1 1 d . . . C4 C 0.0779(2) 0.2750(3) 0.3612(4) 0.0207(16) Uani 1 1 d . . . C5 C 0.0933(2) 0.2083(3) 0.3580(4) 0.0241(17) Uani 1 1 d . . . H5 H 0.0787 0.1731 0.3812 0.029 Uiso 1 1 calc R . . C6 C 0.1297(2) 0.1915(3) 0.3215(4) 0.0250(17) Uani 1 1 d . . . C7 C 0.1505(2) 0.2428(3) 0.2859(4) 0.0196(16) Uani 1 1 d . . . H7 H 0.1752 0.2317 0.2610 0.024 Uiso 1 1 calc R . . C8 C 0.1351(2) 0.3120(3) 0.2863(4) 0.0193(16) Uani 1 1 d . . . C9 C 0.0998(2) 0.3258(3) 0.3250(3) 0.0167(14) Uani 1 1 d . . . C10 C 0.0009(2) 0.3158(4) 0.3576(5) 0.034(2) Uani 1 1 d . . . H10A H 0.0092 0.3496 0.3243 0.050 Uiso 1 1 calc R . . H10B H -0.0220 0.3348 0.3850 0.050 Uiso 1 1 calc R . . H10C H -0.0092 0.2741 0.3359 0.050 Uiso 1 1 calc R . . C11 C 0.0261(3) 0.2455(4) 0.4539(5) 0.036(2) Uani 1 1 d . . . H11A H 0.0167 0.2035 0.4318 0.054 Uiso 1 1 calc R . . H11B H 0.0026 0.2642 0.4800 0.054 Uiso 1 1 calc R . . H11C H 0.0502 0.2350 0.4829 0.054 Uiso 1 1 calc R . . C12 C 0.1477(3) 0.1188(3) 0.3210(4) 0.033(2) Uani 1 1 d . . . H12A H 0.1478 0.1012 0.2758 0.049 Uiso 1 1 calc R . . H12B H 0.1300 0.0892 0.3488 0.049 Uiso 1 1 calc R . . H12C H 0.1769 0.1193 0.3382 0.049 Uiso 1 1 calc R . . C13 C 0.0469(2) 0.4826(3) 0.3835(4) 0.0213(16) Uani 1 1 d . . . H13A H 0.0177 0.4727 0.3997 0.026 Uiso 1 1 calc R . . H13B H 0.0449 0.4924 0.3357 0.026 Uiso 1 1 calc R . . C14 C 0.0641(2) 0.5472(3) 0.4193(4) 0.0220(16) Uani 1 1 d . . . C15 C 0.1106(2) 0.5546(3) 0.3975(4) 0.0194(15) Uani 1 1 d . . . C16 C 0.1297(2) 0.6144(3) 0.3759(4) 0.0203(15) Uani 1 1 d . . . H16 H 0.1133 0.6554 0.3750 0.024 Uiso 1 1 calc R . . C17 C 0.1723(2) 0.6166(3) 0.3552(4) 0.0189(15) Uani 1 1 d . . . C18 C 0.1961(2) 0.5563(3) 0.3573(4) 0.0170(15) Uani 1 1 d . . . H18 H 0.2248 0.5572 0.3426 0.020 Uiso 1 1 calc R . . C19 C 0.1787(2) 0.4934(3) 0.3807(4) 0.0172(15) Uani 1 1 d . . . C20 C 0.1359(2) 0.4940(3) 0.3994(4) 0.0171(14) Uani 1 1 d . . . C21 C 0.0614(2) 0.5396(4) 0.4950(4) 0.0274(18) Uani 1 1 d . . . H21A H 0.0789 0.5006 0.5091 0.041 Uiso 1 1 calc R . . H21B H 0.0317 0.5319 0.5080 0.041 Uiso 1 1 calc R . . H21C H 0.0720 0.5815 0.5160 0.041 Uiso 1 1 calc R . . C22 C 0.0359(2) 0.6085(3) 0.3984(4) 0.0260(17) Uani 1 1 d . . . H22A H 0.0458 0.6500 0.4209 0.039 Uiso 1 1 calc R . . H22B H 0.0062 0.5993 0.4106 0.039 Uiso 1 1 calc R . . H22C H 0.0379 0.6149 0.3507 0.039 Uiso 1 1 calc R . . C23 C 0.1924(2) 0.6837(3) 0.3318(4) 0.0235(17) Uani 1 1 d . . . H23A H 0.2008 0.7111 0.3700 0.035 Uiso 1 1 calc R . . H23B H 0.1716 0.7093 0.3054 0.035 Uiso 1 1 calc R . . H23C H 0.2175 0.6736 0.3048 0.035 Uiso 1 1 calc R . . C24 C 0.1364(2) 0.4543(3) 0.2218(4) 0.0182(15) Uani 1 1 d . . . H24 H 0.1302 0.4712 0.2673 0.022 Uiso 1 1 calc R . . C25 C 0.1665(2) 0.5084(3) 0.1902(4) 0.0207(15) Uani 1 1 d . . . H25A H 0.1933 0.5112 0.2159 0.025 Uiso 1 1 calc R . . H25B H 0.1739 0.4941 0.1448 0.025 Uiso 1 1 calc R . . C26 C 0.1450(2) 0.5795(3) 0.1885(4) 0.0251(17) Uani 1 1 d . . . H26A H 0.1400 0.5956 0.2342 0.030 Uiso 1 1 calc R . . H26B H 0.1641 0.6127 0.1665 0.030 Uiso 1 1 calc R . . C27 C 0.1023(3) 0.5765(3) 0.1516(4) 0.0292(19) Uani 1 1 d . . . H27A H 0.1074 0.5636 0.1050 0.035 Uiso 1 1 calc R . . H27B H 0.0887 0.6222 0.1522 0.035 Uiso 1 1 calc R . . C28 C 0.0724(2) 0.5238(3) 0.1838(4) 0.0282(18) Uani 1 1 d . . . H28A H 0.0453 0.5219 0.1587 0.034 Uiso 1 1 calc R . . H28B H 0.0657 0.5387 0.2293 0.034 Uiso 1 1 calc R . . C29 C 0.0927(2) 0.4516(3) 0.1857(4) 0.0213(16) Uani 1 1 d . . . H29A H 0.0969 0.4347 0.1402 0.026 Uiso 1 1 calc R . . H29B H 0.0734 0.4195 0.2088 0.026 Uiso 1 1 calc R . . C30 C 0.1622(2) 0.3215(3) 0.1525(4) 0.0172(14) Uani 1 1 d . . . H30 H 0.1828 0.2827 0.1571 0.021 Uiso 1 1 calc R . . C31 C 0.1767(2) 0.3621(3) 0.0901(4) 0.0211(16) Uani 1 1 d . . . H31A H 0.1554 0.3978 0.0793 0.025 Uiso 1 1 calc R . . H31B H 0.2044 0.3849 0.0987 0.025 Uiso 1 1 calc R . . C32 C 0.1813(2) 0.3116(4) 0.0316(4) 0.0255(17) Uani 1 1 d . . . H32A H 0.1905 0.3369 -0.0082 0.031 Uiso 1 1 calc R . . H32B H 0.2035 0.2771 0.0421 0.031 Uiso 1 1 calc R . . C33 C 0.1388(3) 0.2751(4) 0.0177(4) 0.0272(17) Uani 1 1 d . . . H33A H 0.1174 0.3093 0.0031 0.033 Uiso 1 1 calc R . . H33B H 0.1428 0.2416 -0.0184 0.033 Uiso 1 1 calc R . . C34 C 0.1221(3) 0.2379(3) 0.0790(4) 0.0257(17) Uani 1 1 d . . . H34A H 0.1419 0.2003 0.0908 0.031 Uiso 1 1 calc R . . H34B H 0.0939 0.2175 0.0692 0.031 Uiso 1 1 calc R . . C35 C 0.1179(2) 0.2877(3) 0.1378(4) 0.0250(17) Uani 1 1 d . . . H35A H 0.1079 0.2624 0.1772 0.030 Uiso 1 1 calc R . . H35B H 0.0967 0.3236 0.1274 0.030 Uiso 1 1 calc R . . C36 C 0.1948(2) 0.3481(3) 0.4293(4) 0.0167(15) Uani 1 1 d . . . H36 H 0.1666 0.3369 0.4091 0.020 Uiso 1 1 calc R . . C37 C 0.2234(2) 0.2844(3) 0.4194(4) 0.0193(15) Uani 1 1 d . . . H37A H 0.2264 0.2749 0.3717 0.023 Uiso 1 1 calc R . . H37B H 0.2522 0.2937 0.4374 0.023 Uiso 1 1 calc R . . C38 C 0.2043(2) 0.2213(3) 0.4541(4) 0.0225(16) Uani 1 1 d . . . H38A H 0.1776 0.2078 0.4313 0.027 Uiso 1 1 calc R . . H38B H 0.2246 0.1826 0.4507 0.027 Uiso 1 1 calc R . . C39 C 0.1945(3) 0.2350(3) 0.5273(4) 0.0281(18) Uani 1 1 d . . . H39A H 0.1800 0.1946 0.5466 0.034 Uiso 1 1 calc R . . H39B H 0.2214 0.2425 0.5515 0.034 Uiso 1 1 calc R . . C40 C 0.1659(2) 0.2981(3) 0.5346(4) 0.0236(16) Uani 1 1 d . . . H40A H 0.1606 0.3069 0.5819 0.028 Uiso 1 1 calc R . . H40B H 0.1380 0.2891 0.5132 0.028 Uiso 1 1 calc R . . C41 C 0.1865(2) 0.3618(3) 0.5032(4) 0.0211(16) Uani 1 1 d . . . H41A H 0.2137 0.3723 0.5258 0.025 Uiso 1 1 calc R . . H41B H 0.1673 0.4017 0.5082 0.025 Uiso 1 1 calc R . . C42 C 0.2618(2) 0.4613(3) 0.4307(3) 0.0169(14) Uani 1 1 d . . . H42 H 0.2766 0.4923 0.3989 0.020 Uiso 1 1 calc R . . C43 C 0.2967(2) 0.4098(3) 0.4528(4) 0.0202(15) Uani 1 1 d . . . H43A H 0.2854 0.3807 0.4887 0.024 Uiso 1 1 calc R . . H43B H 0.3042 0.3796 0.4153 0.024 Uiso 1 1 calc R . . C44 C 0.3372(2) 0.4469(3) 0.4770(4) 0.0239(16) Uani 1 1 d . . . H44A H 0.3581 0.4128 0.4932 0.029 Uiso 1 1 calc R . . H44B H 0.3504 0.4719 0.4397 0.029 Uiso 1 1 calc R . . C45 C 0.3267(2) 0.4974(4) 0.5322(4) 0.0259(17) Uani 1 1 d . . . H45A H 0.3525 0.5241 0.5435 0.031 Uiso 1 1 calc R . . H45B H 0.3177 0.4717 0.5719 0.031 Uiso 1 1 calc R . . C46 C 0.2907(2) 0.5468(3) 0.5113(4) 0.0234(16) Uani 1 1 d . . . H46A H 0.3009 0.5757 0.4744 0.028 Uiso 1 1 calc R . . H46B H 0.2837 0.5774 0.5487 0.028 Uiso 1 1 calc R . . C47 C 0.2501(2) 0.5081(3) 0.4896(4) 0.0206(16) Uani 1 1 d . . . H47A H 0.2277 0.5412 0.4764 0.025 Uiso 1 1 calc R . . H47B H 0.2390 0.4802 0.5266 0.025 Uiso 1 1 calc R . . C48 C 0.3038(2) 0.3584(3) 0.2845(4) 0.0218(17) Uani 1 1 d . . . H48 H 0.3137 0.3330 0.3245 0.026 Uiso 1 1 calc R . . C49 C 0.3037(2) 0.4307(3) 0.2803(4) 0.0194(16) Uani 1 1 d . . . H49 H 0.3134 0.4610 0.3171 0.023 Uiso 1 1 calc R . . C50 C 0.3104(2) 0.4482(3) 0.2069(4) 0.0190(15) Uani 1 1 d . . . H50 H 0.3194 0.4961 0.1959 0.023 Uiso 1 1 calc R . . C51 C 0.2678(2) 0.4224(3) 0.1779(3) 0.0168(15) Uani 1 1 d U . . H51 H 0.2523 0.4476 0.1423 0.020 Uiso 1 1 calc R . . C52 C 0.2681(2) 0.3522(3) 0.1819(4) 0.0186(15) Uani 1 1 d . . . H52 H 0.2528 0.3225 0.1496 0.022 Uiso 1 1 calc R . . C53 C 0.3108(2) 0.3312(3) 0.2134(4) 0.0226(16) Uani 1 1 d . . . H53 H 0.3203 0.2826 0.2081 0.027 Uiso 1 1 calc R . . C54 C 0.3409(2) 0.3890(3) 0.1860(4) 0.0231(16) Uani 1 1 d . . . H54A H 0.3688 0.3906 0.2087 0.028 Uiso 1 1 calc R . . H54B H 0.3450 0.3862 0.1377 0.028 Uiso 1 1 calc R . . B1 B 0.2300(3) 0.1277(4) 0.1776(5) 0.027(2) Uani 1 1 d . . . F1 F 0.18637(15) 0.1285(2) 0.1664(3) 0.0379(12) Uani 1 1 d . . . F2 F 0.25066(16) 0.0886(2) 0.1286(3) 0.0394(12) Uani 1 1 d . . . F3 F 0.23810(14) 0.0962(2) 0.2388(2) 0.0358(11) Uani 1 1 d . . . F4 F 0.24639(19) 0.1940(2) 0.1788(3) 0.0572(16) Uani 1 1 d . . . C1Y C 0.0808(12) 0.069(2) 0.148(2) 0.090(13) Uani 0.50 1 d P . . C2Y C 0.0572(17) 0.101(2) 0.185(3) 0.122(17) Uani 0.50 1 d P . . C3Y C 0.0348(10) 0.1196(15) 0.142(2) 0.103(12) Uani 0.50 1 d P . . C4Y C 0.044(2) 0.055(2) 0.220(2) 0.15(2) Uani 0.50 1 d P . . C5Y C 0.022(3) 0.114(3) 0.218(3) 0.21(5) Uani 0.50 1 d P . . C6Y C 0.0725(19) 0.030(3) 0.162(3) 0.17(3) Uani 0.50 1 d P . . C1X C 0.4284(11) 0.401(2) 0.342(2) 0.047(9) Uani 0.25 1 d PU . . C2X C 0.4353(12) 0.2732(16) 0.152(2) 0.046(9) Uani 0.25 1 d PU . . C3X C 0.4107(14) 0.333(2) 0.358(3) 0.061(12) Uani 0.25 1 d PU . . C4X C 0.4500(18) 0.402(3) 0.395(3) 0.075(15) Uani 0.25 1 d PU . . C5X C 0.4535(15) 0.497(3) 0.430(3) 0.074(13) Uani 0.25 1 d PU . . C6X C 0.4353(15) 0.297(2) 0.379(3) 0.068(13) Uani 0.25 1 d PU . . C7X C 0.4283(17) 0.289(3) 0.306(3) 0.083(15) Uani 0.25 1 d PU . . C8X C 0.4505(17) 0.349(3) 0.421(3) 0.084(16) Uani 0.25 1 d PU . . C9X C 0.4329(18) 0.253(3) 0.239(3) 0.087(16) Uani 0.25 1 d PU . . C10X C 0.492(2) 0.473(3) 0.475(4) 0.11(2) Uani 0.25 1 d PU . . C11X C 0.4462(19) 0.444(4) 0.394(4) 0.093(19) Uani 0.25 1 d PU . . C12X C 0.475(2) 0.256(4) 0.222(4) 0.13(3) Uani 0.25 1 d PU . . 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 0.0300(3) 0.0120(2) 0.0034(3) 0.00051(19) 0.0001(2) -0.0003(2) P1 0.0322(9) 0.0165(7) 0.0041(11) 0.0006(6) 0.0001(8) -0.0002(6) C1 0.032(4) 0.017(3) 0.010(5) -0.002(3) 0.005(3) 0.002(3) O1 0.031(3) 0.017(2) 0.005(3) -0.0010(18) 0.0013(19) 0.0031(19) P2 0.0322(9) 0.0099(7) 0.0050(11) 0.0014(6) 0.0006(7) 0.0002(6) C2 0.028(4) 0.023(3) 0.011(5) 0.001(3) 0.004(3) -0.001(3) O2 0.032(3) 0.014(2) 0.006(3) 0.0043(17) -0.001(2) -0.0014(18) C3 0.031(4) 0.020(3) 0.021(5) 0.001(3) 0.003(3) -0.007(3) C4 0.032(4) 0.019(3) 0.011(5) -0.001(3) 0.002(3) -0.003(3) C5 0.040(4) 0.017(3) 0.016(5) 0.000(3) 0.007(3) -0.008(3) C6 0.045(5) 0.015(3) 0.015(5) -0.002(3) -0.003(3) 0.000(3) C7 0.037(4) 0.015(3) 0.007(5) -0.006(2) -0.002(3) 0.002(3) C8 0.031(4) 0.014(3) 0.013(5) -0.002(2) -0.003(3) -0.002(3) C9 0.032(4) 0.015(3) 0.003(4) -0.001(2) -0.004(3) 0.003(3) C10 0.034(4) 0.038(4) 0.028(6) -0.007(4) 0.005(4) -0.006(3) C11 0.051(5) 0.026(4) 0.031(6) -0.001(3) 0.016(4) -0.008(3) C12 0.060(5) 0.017(3) 0.022(6) 0.002(3) 0.009(4) 0.004(3) C13 0.032(4) 0.017(3) 0.015(5) 0.001(3) -0.003(3) 0.003(3) C14 0.034(4) 0.022(3) 0.010(5) -0.001(3) 0.000(3) 0.005(3) C15 0.036(4) 0.017(3) 0.005(4) -0.003(3) -0.003(3) 0.002(3) C16 0.038(4) 0.010(3) 0.013(5) -0.002(3) -0.006(3) 0.006(3) C17 0.044(4) 0.010(3) 0.002(4) 0.001(2) -0.006(3) -0.001(3) C18 0.034(4) 0.013(3) 0.004(4) -0.004(2) -0.001(3) -0.002(3) C19 0.038(4) 0.011(3) 0.002(4) 0.002(2) -0.008(3) 0.000(3) C20 0.035(4) 0.014(3) 0.002(4) 0.000(2) -0.001(3) -0.002(3) C21 0.039(4) 0.025(4) 0.018(5) -0.003(3) 0.002(3) -0.001(3) C22 0.033(4) 0.022(3) 0.022(5) -0.002(3) -0.002(3) 0.004(3) C23 0.038(4) 0.013(3) 0.020(5) 0.005(3) 0.000(3) -0.001(3) C24 0.035(4) 0.019(3) 0.001(4) 0.001(3) -0.001(3) 0.001(3) C25 0.037(4) 0.014(3) 0.011(5) 0.000(3) -0.002(3) -0.003(3) C26 0.048(5) 0.011(3) 0.016(5) 0.005(3) -0.002(3) 0.000(3) C27 0.050(5) 0.015(3) 0.023(5) 0.004(3) -0.008(4) 0.000(3) C28 0.038(4) 0.025(4) 0.022(6) -0.001(3) -0.006(4) 0.005(3) C29 0.039(4) 0.015(3) 0.010(5) -0.003(3) -0.006(3) 0.001(3) C30 0.034(4) 0.015(3) 0.002(4) 0.001(2) 0.000(3) -0.006(3) C31 0.043(4) 0.016(3) 0.005(5) 0.006(3) 0.001(3) -0.006(3) C32 0.048(5) 0.026(4) 0.003(5) -0.004(3) -0.001(3) -0.002(3) C33 0.053(5) 0.024(3) 0.005(5) -0.004(3) -0.003(3) 0.003(3) C34 0.050(5) 0.019(3) 0.008(5) -0.003(3) -0.007(3) -0.005(3) C35 0.040(4) 0.018(3) 0.016(5) -0.003(3) 0.000(3) -0.003(3) C36 0.036(4) 0.009(3) 0.006(4) 0.001(2) 0.002(3) 0.003(3) C37 0.038(4) 0.015(3) 0.005(4) 0.001(2) 0.004(3) 0.000(3) C38 0.039(4) 0.015(3) 0.014(5) -0.001(3) 0.001(3) 0.000(3) C39 0.052(5) 0.016(3) 0.016(5) 0.004(3) 0.006(4) 0.002(3) C40 0.044(4) 0.021(3) 0.007(5) -0.001(3) 0.004(3) 0.000(3) C41 0.040(4) 0.011(3) 0.012(5) -0.001(3) -0.001(3) 0.002(3) C42 0.037(4) 0.008(3) 0.005(4) 0.000(2) 0.000(3) 0.002(3) C43 0.032(4) 0.020(3) 0.009(5) -0.001(3) -0.003(3) 0.001(3) C44 0.037(4) 0.020(3) 0.015(5) -0.001(3) -0.002(3) 0.000(3) C45 0.039(4) 0.024(3) 0.014(5) 0.002(3) -0.007(3) -0.002(3) C46 0.048(5) 0.016(3) 0.006(5) -0.004(3) 0.001(3) -0.006(3) C47 0.043(4) 0.008(3) 0.011(5) -0.006(2) 0.001(3) 0.001(3) C48 0.031(4) 0.016(3) 0.019(5) 0.006(3) 0.000(3) 0.003(3) C49 0.029(4) 0.014(3) 0.016(5) -0.001(3) 0.001(3) -0.003(2) C50 0.031(4) 0.015(3) 0.011(5) -0.003(3) 0.002(3) -0.003(3) C51 0.039(4) 0.007(3) 0.005(4) 0.005(2) 0.003(3) 0.000(2) C52 0.034(4) 0.014(3) 0.008(4) 0.002(2) 0.004(3) -0.002(3) C53 0.040(4) 0.021(3) 0.008(5) -0.004(3) 0.001(3) 0.003(3) C54 0.030(4) 0.027(3) 0.013(5) 0.004(3) 0.006(3) -0.003(3) B1 0.048(5) 0.014(3) 0.020(6) -0.001(3) 0.003(4) 0.004(3) F1 0.053(3) 0.038(3) 0.022(3) 0.002(2) -0.003(2) 0.013(2) F2 0.058(3) 0.037(2) 0.023(3) -0.007(2) 0.008(2) 0.005(2) F3 0.045(3) 0.046(3) 0.016(3) 0.006(2) -0.003(2) 0.003(2) F4 0.093(4) 0.017(2) 0.062(5) 0.002(2) -0.013(3) -0.007(2) C1Y 0.057(18) 0.10(3) 0.11(4) 0.00(2) 0.024(19) -0.04(2) C2Y 0.14(4) 0.10(3) 0.13(5) 0.05(3) -0.02(3) -0.01(3) C3Y 0.10(2) 0.072(18) 0.13(4) 0.05(2) -0.03(2) 0.020(15) C4Y 0.28(6) 0.10(2) 0.08(3) 0.07(2) -0.10(3) -0.10(3) C5Y 0.34(14) 0.15(4) 0.15(10) -0.01(4) -0.15(8) 0.04(6) C6Y 0.15(5) 0.18(6) 0.18(6) 0.04(5) 0.06(4) 0.10(4) C1X 0.036(14) 0.071(17) 0.034(18) -0.004(14) 0.000(13) -0.014(13) C2X 0.053(16) 0.023(12) 0.062(19) -0.024(13) 0.006(14) 0.000(12) C3X 0.062(18) 0.068(18) 0.05(2) 0.013(15) 0.006(15) -0.001(15) C4X 0.07(2) 0.07(2) 0.08(2) -0.004(17) 0.031(17) 0.013(17) C5X 0.062(18) 0.08(2) 0.08(2) 0.019(17) 0.027(16) -0.005(16) C6X 0.064(18) 0.060(18) 0.08(2) 0.018(16) 0.009(16) -0.002(15) C7X 0.09(2) 0.07(2) 0.09(2) 0.033(17) -0.007(17) 0.003(16) C8X 0.08(2) 0.09(2) 0.08(2) 0.006(18) 0.018(17) 0.021(17) C9X 0.08(2) 0.08(2) 0.10(2) 0.006(17) -0.017(18) -0.008(17) C10X 0.12(3) 0.11(3) 0.10(3) 0.014(18) 0.021(19) -0.015(19) C11X 0.08(2) 0.11(2) 0.10(3) 0.010(19) 0.028(18) -0.002(18) C12X 0.14(3) 0.12(3) 0.13(3) 0.011(19) 0.009(19) 0.028(19) _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 C51 2.194(7) . ? Rh1 C52 2.199(7) . ? Rh1 C48 2.211(7) . ? Rh1 C49 2.215(7) . ? Rh1 P2 2.393(2) . ? Rh1 P1 2.411(2) . ? P1 C8 1.865(7) . ? P1 C24 1.871(6) . ? P1 C30 1.895(7) . ? C1 O1 1.439(9) . ? C1 O2 1.451(8) . ? C1 C2 1.548(9) . ? C1 C13 1.549(9) . ? O1 C9 1.410(7) . ? P2 C19 1.853(6) . ? P2 C36 1.861(6) . ? P2 C42 1.895(7) . ? C2 C3 1.560(9) . ? O2 C20 1.390(7) . ? C3 C4 1.517(10) . ? C3 C11 1.541(10) . ? C3 C10 1.558(11) . ? C4 C5 1.391(9) . ? C4 C9 1.411(9) . ? C5 C6 1.400(11) . ? C6 C7 1.395(10) . ? C6 C12 1.528(9) . ? C7 C8 1.434(8) . ? C8 C9 1.385(10) . ? C13 C14 1.551(9) . ? C14 C15 1.532(10) . ? C14 C22 1.546(9) . ? C14 C21 1.546(11) . ? C15 C16 1.382(9) . ? C15 C20 1.426(9) . ? C16 C17 1.402(10) . ? C17 C18 1.392(9) . ? C17 C23 1.529(8) . ? C18 C19 1.425(9) . ? C19 C20 1.394(10) . ? C24 C29 1.553(10) . ? C24 C25 1.556(9) . ? C25 C26 1.545(9) . ? C26 C27 1.535(11) . ? C27 C28 1.536(10) . ? C28 C29 1.547(9) . ? C30 C31 1.560(9) . ? C30 C35 1.568(9) . ? C31 C32 1.550(10) . ? C32 C33 1.539(10) . ? C33 C34 1.532(11) . ? C34 C35 1.544(10) . ? C36 C41 1.546(10) . ? C36 C37 1.547(8) . ? C37 C38 1.541(9) . ? C38 C39 1.540(11) . ? C39 C40 1.530(9) . ? C40 C41 1.538(9) . ? C42 C47 1.549(9) . ? C42 C43 1.553(9) . ? C43 C44 1.542(9) . ? C44 C45 1.527(10) . ? C45 C46 1.542(10) . ? C46 C47 1.544(9) . ? C48 C49 1.413(8) . ? C48 C53 1.552(10) . ? C49 C50 1.543(10) . ? C50 C51 1.545(9) . ? C50 C54 1.559(9) . ? C51 C52 1.372(8) . ? C52 C53 1.539(10) . ? C53 C54 1.570(9) . ? B1 F1 1.387(10) . ? B1 F4 1.392(9) . ? B1 F3 1.409(10) . ? B1 F2 1.411(10) . ? C1Y C6Y 0.85(6) . ? C1Y C2Y 1.24(7) . ? C1Y C3Y 1.75(6) . ? C1Y C4Y 1.90(7) . ? C2Y C3Y 1.18(6) . ? C2Y C4Y 1.23(5) . ? C2Y C5Y 1.33(8) . ? C2Y C6Y 1.54(7) . ? C3Y C5Y 1.61(8) . ? C4Y C5Y 1.36(8) . ? C4Y C6Y 1.56(7) . ? C5Y C5Y 1.86(18) 3 ? C1X C4X 1.27(7) . ? C1X C11X 1.45(9) . ? C1X C3X 1.47(6) . ? C1X C8X 2.02(8) . ? C2X C9X 1.81(8) . ? C2X C12X 1.93(9) . ? C3X C6X 1.12(6) . ? C3X C7X 1.48(8) . ? C3X C8X 1.81(8) . ? C3X C4X 1.97(8) . ? C4X C11X 0.82(7) . ? C4X C8X 1.16(7) . ? C4X C5X 1.98(8) . ? C5X C11X 1.29(8) . ? C5X C10X 1.60(9) . ? C6X C8X 1.40(8) . ? C6X C7X 1.52(8) . ? C7X C9X 1.53(9) . ? C8X C11X 1.94(9) . ? C9X C12X 1.36(8) . ? C10X C10X 1.55(14) 5_666 ? C12X C12X 1.94(16) 3_655 ? 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 C51 Rh1 C52 36.4(2) . . ? C51 Rh1 C48 77.0(3) . . ? C52 Rh1 C48 64.9(3) . . ? C51 Rh1 C49 65.0(3) . . ? C52 Rh1 C49 77.1(3) . . ? C48 Rh1 C49 37.2(2) . . ? C51 Rh1 P2 149.54(16) . . ? C52 Rh1 P2 165.79(19) . . ? C48 Rh1 P2 101.8(2) . . ? C49 Rh1 P2 95.3(2) . . ? C51 Rh1 P1 99.87(19) . . ? C52 Rh1 P1 94.5(2) . . ? C48 Rh1 P1 149.87(18) . . ? C49 Rh1 P1 163.49(19) . . ? P2 Rh1 P1 95.60(7) . . ? C8 P1 C24 110.5(3) . . ? C8 P1 C30 98.6(3) . . ? C24 P1 C30 108.6(3) . . ? C8 P1 Rh1 113.3(2) . . ? C24 P1 Rh1 110.2(2) . . ? C30 P1 Rh1 115.0(2) . . ? O1 C1 O2 106.9(5) . . ? O1 C1 C2 112.7(5) . . ? O2 C1 C2 105.2(6) . . ? O1 C1 C13 104.9(6) . . ? O2 C1 C13 112.3(5) . . ? C2 C1 C13 114.7(6) . . ? C9 O1 C1 115.6(5) . . ? C19 P2 C36 110.1(3) . . ? C19 P2 C42 99.8(3) . . ? C36 P2 C42 108.5(3) . . ? C19 P2 Rh1 109.9(2) . . ? C36 P2 Rh1 114.4(2) . . ? C42 P2 Rh1 113.2(2) . . ? C1 C2 C3 112.8(6) . . ? C20 O2 C1 116.5(5) . . ? C4 C3 C11 113.1(6) . . ? C4 C3 C10 111.7(7) . . ? C11 C3 C10 108.5(6) . . ? C4 C3 C2 105.6(5) . . ? C11 C3 C2 107.1(7) . . ? C10 C3 C2 110.8(6) . . ? C5 C4 C9 117.7(6) . . ? C5 C4 C3 125.4(6) . . ? C9 C4 C3 116.9(6) . . ? C4 C5 C6 121.8(6) . . ? C7 C6 C5 119.1(6) . . ? C7 C6 C12 119.4(7) . . ? C5 C6 C12 121.4(7) . . ? C6 C7 C8 121.1(7) . . ? C9 C8 C7 117.1(6) . . ? C9 C8 P1 128.7(5) . . ? C7 C8 P1 114.3(5) . . ? C8 C9 O1 120.3(6) . . ? C8 C9 C4 123.2(6) . . ? O1 C9 C4 116.5(6) . . ? C1 C13 C14 113.4(6) . . ? C15 C14 C22 113.0(6) . . ? C15 C14 C21 110.3(6) . . ? C22 C14 C21 108.4(6) . . ? C15 C14 C13 105.9(6) . . ? C22 C14 C13 107.6(6) . . ? C21 C14 C13 111.7(6) . . ? C16 C15 C20 117.9(6) . . ? C16 C15 C14 125.7(6) . . ? C20 C15 C14 116.3(6) . . ? C15 C16 C17 122.2(6) . . ? C18 C17 C16 118.4(6) . . ? C18 C17 C23 120.9(6) . . ? C16 C17 C23 120.7(6) . . ? C17 C18 C19 122.2(6) . . ? C20 C19 C18 116.9(6) . . ? C20 C19 P2 128.9(5) . . ? C18 C19 P2 114.2(5) . . ? O2 C20 C19 121.0(5) . . ? O2 C20 C15 116.7(6) . . ? C19 C20 C15 122.3(6) . . ? C29 C24 C25 111.3(6) . . ? C29 C24 P1 117.4(4) . . ? C25 C24 P1 109.4(5) . . ? C26 C25 C24 110.6(6) . . ? C27 C26 C25 111.0(6) . . ? C26 C27 C28 110.5(6) . . ? C27 C28 C29 111.6(6) . . ? C28 C29 C24 110.2(5) . . ? C31 C30 C35 108.6(6) . . ? C31 C30 P1 114.5(4) . . ? C35 C30 P1 115.6(5) . . ? C32 C31 C30 109.0(5) . . ? C33 C32 C31 110.7(6) . . ? C34 C33 C32 111.5(6) . . ? C33 C34 C35 111.0(6) . . ? C34 C35 C30 109.6(6) . . ? C41 C36 C37 111.3(5) . . ? C41 C36 P2 116.0(4) . . ? C37 C36 P2 109.3(5) . . ? C38 C37 C36 110.9(6) . . ? C39 C38 C37 112.3(6) . . ? C40 C39 C38 110.5(6) . . ? C39 C40 C41 111.3(6) . . ? C40 C41 C36 109.5(5) . . ? C47 C42 C43 109.1(6) . . ? C47 C42 P2 118.4(5) . . ? C43 C42 P2 114.1(4) . . ? C44 C43 C42 111.6(5) . . ? C45 C44 C43 111.0(6) . . ? C44 C45 C46 111.1(6) . . ? C45 C46 C47 112.1(5) . . ? C46 C47 C42 108.2(6) . . ? C49 C48 C53 106.6(6) . . ? C49 C48 Rh1 71.6(4) . . ? C53 C48 Rh1 97.0(4) . . ? C48 C49 C50 106.2(6) . . ? C48 C49 Rh1 71.2(4) . . ? C50 C49 Rh1 96.9(4) . . ? C49 C50 C51 100.2(5) . . ? C49 C50 C54 100.5(5) . . ? C51 C50 C54 100.5(5) . . ? C52 C51 C50 107.3(6) . . ? C52 C51 Rh1 72.0(4) . . ? C50 C51 Rh1 97.7(4) . . ? C51 C52 C53 107.2(6) . . ? C51 C52 Rh1 71.6(4) . . ? C53 C52 Rh1 97.9(5) . . ? C52 C53 C48 99.9(5) . . ? C52 C53 C54 100.6(5) . . ? C48 C53 C54 99.7(5) . . ? C50 C54 C53 93.9(5) . . ? F1 B1 F4 110.9(6) . . ? F1 B1 F3 109.1(7) . . ? F4 B1 F3 108.9(7) . . ? F1 B1 F2 110.1(7) . . ? F4 B1 F2 110.2(7) . . ? F3 B1 F2 107.6(6) . . ? C6Y C1Y C2Y 94(6) . . ? C6Y C1Y C3Y 106(6) . . ? C2Y C1Y C3Y 42(3) . . ? C6Y C1Y C4Y 55(5) . . ? C2Y C1Y C4Y 39(3) . . ? C3Y C1Y C4Y 68(3) . . ? C3Y C2Y C4Y 117(5) . . ? C3Y C2Y C1Y 93(6) . . ? C4Y C2Y C1Y 101(6) . . ? C3Y C2Y C5Y 79(5) . . ? C4Y C2Y C5Y 64(5) . . ? C1Y C2Y C5Y 156(6) . . ? C3Y C2Y C6Y 103(6) . . ? C4Y C2Y C6Y 68(4) . . ? C1Y C2Y C6Y 33(3) . . ? C5Y C2Y C6Y 126(5) . . ? C2Y C3Y C5Y 54(4) . . ? C2Y C3Y C1Y 45(4) . . ? C5Y C3Y C1Y 97(3) . . ? C2Y C4Y C5Y 62(4) . . ? C2Y C4Y C6Y 66(4) . . ? C5Y C4Y C6Y 122(4) . . ? C2Y C4Y C1Y 40(4) . . ? C5Y C4Y C1Y 100(4) . . ? C6Y C4Y C1Y 26(2) . . ? C2Y C5Y C4Y 54(4) . . ? C2Y C5Y C3Y 46(4) . . ? C4Y C5Y C3Y 87(5) . . ? C2Y C5Y C5Y 163(6) . 3 ? C4Y C5Y C5Y 111(5) . 3 ? C3Y C5Y C5Y 148(6) . 3 ? C1Y C6Y C2Y 53(5) . . ? C1Y C6Y C4Y 99(7) . . ? C2Y C6Y C4Y 46(3) . . ? C4X C1X C11X 34(3) . . ? C4X C1X C3X 92(4) . . ? C11X C1X C3X 120(5) . . ? C4X C1X C8X 32(3) . . ? C11X C1X C8X 65(4) . . ? C3X C1X C8X 60(3) . . ? C9X C2X C12X 42(3) . . ? C6X C3X C1X 113(4) . . ? C6X C3X C7X 70(4) . . ? C1X C3X C7X 102(4) . . ? C6X C3X C8X 51(4) . . ? C1X C3X C8X 75(3) . . ? C7X C3X C8X 111(4) . . ? C6X C3X C4X 82(4) . . ? C1X C3X C4X 40(3) . . ? C7X C3X C4X 116(4) . . ? C8X C3X C4X 35(2) . . ? C11X C4X C8X 154(10) . . ? C11X C4X C1X 85(9) . . ? C8X C4X C1X 112(7) . . ? C11X C4X C3X 125(9) . . ? C8X C4X C3X 64(5) . . ? C1X C4X C3X 48(3) . . ? C11X C4X C5X 25(7) . . ? C8X C4X C5X 132(6) . . ? C1X C4X C5X 110(5) . . ? C3X C4X C5X 144(4) . . ? C11X C5X C10X 103(5) . . ? C11X C5X C4X 16(4) . . ? C10X C5X C4X 88(4) . . ? C3X C6X C8X 91(5) . . ? C3X C6X C7X 66(4) . . ? C8X C6X C7X 136(5) . . ? C3X C7X C6X 44(3) . . ? C3X C7X C9X 160(5) . . ? C6X C7X C9X 155(5) . . ? C4X C8X C6X 111(7) . . ? C4X C8X C3X 80(5) . . ? C6X C8X C3X 38(3) . . ? C4X C8X C11X 11(4) . . ? C6X C8X C11X 119(5) . . ? C3X C8X C11X 85(4) . . ? C4X C8X C1X 36(4) . . ? C6X C8X C1X 76(4) . . ? C3X C8X C1X 45(2) . . ? C11X C8X C1X 43(3) . . ? C12X C9X C7X 107(6) . . ? C12X C9X C2X 73(5) . . ? C7X C9X C2X 140(4) . . ? C10X C10X C5X 114(7) 5_666 . ? C4X C11X C5X 139(10) . . ? C4X C11X C1X 61(8) . . ? C5X C11X C1X 160(7) . . ? C4X C11X C8X 15(6) . . ? C5X C11X C8X 127(6) . . ? C1X C11X C8X 71(4) . . ? C9X C12X C2X 64(4) . . ? C9X C12X C12X 130(9) . 3_655 ? C2X C12X C12X 163(6) . 3_655 ? 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 C51 Rh1 P1 C8 156.0(3) . . . . ? C52 Rh1 P1 C8 119.6(3) . . . . ? C48 Rh1 P1 C8 75.0(5) . . . . ? C49 Rh1 P1 C8 178.4(6) . . . . ? P2 Rh1 P1 C8 -50.4(2) . . . . ? C51 Rh1 P1 C24 -79.6(3) . . . . ? C52 Rh1 P1 C24 -115.9(3) . . . . ? C48 Rh1 P1 C24 -160.6(5) . . . . ? C49 Rh1 P1 C24 -57.1(7) . . . . ? P2 Rh1 P1 C24 74.1(3) . . . . ? C51 Rh1 P1 C30 43.5(3) . . . . ? C52 Rh1 P1 C30 7.2(3) . . . . ? C48 Rh1 P1 C30 -37.5(5) . . . . ? C49 Rh1 P1 C30 66.0(7) . . . . ? P2 Rh1 P1 C30 -162.8(2) . . . . ? O2 C1 O1 C9 74.7(6) . . . . ? C2 C1 O1 C9 -40.4(8) . . . . ? C13 C1 O1 C9 -165.8(5) . . . . ? C51 Rh1 P2 C19 63.2(4) . . . . ? C52 Rh1 P2 C19 167.5(7) . . . . ? C48 Rh1 P2 C19 147.5(3) . . . . ? C49 Rh1 P2 C19 110.4(3) . . . . ? P1 Rh1 P2 C19 -57.2(2) . . . . ? C51 Rh1 P2 C36 -172.4(4) . . . . ? C52 Rh1 P2 C36 -68.1(8) . . . . ? C48 Rh1 P2 C36 -88.1(3) . . . . ? C49 Rh1 P2 C36 -125.2(3) . . . . ? P1 Rh1 P2 C36 67.2(3) . . . . ? C51 Rh1 P2 C42 -47.4(4) . . . . ? C52 Rh1 P2 C42 56.9(7) . . . . ? C48 Rh1 P2 C42 36.9(3) . . . . ? C49 Rh1 P2 C42 -0.2(3) . . . . ? P1 Rh1 P2 C42 -167.8(2) . . . . ? O1 C1 C2 C3 -12.5(8) . . . . ? O2 C1 C2 C3 -128.7(6) . . . . ? C13 C1 C2 C3 107.4(7) . . . . ? O1 C1 O2 C20 74.3(6) . . . . ? C2 C1 O2 C20 -165.7(5) . . . . ? C13 C1 O2 C20 -40.2(8) . . . . ? C1 C2 C3 C4 53.2(8) . . . . ? C1 C2 C3 C11 174.0(6) . . . . ? C1 C2 C3 C10 -67.8(8) . . . . ? C11 C3 C4 C5 14.5(11) . . . . ? C10 C3 C4 C5 -108.2(8) . . . . ? C2 C3 C4 C5 131.3(8) . . . . ? C11 C3 C4 C9 -163.8(7) . . . . ? C10 C3 C4 C9 73.4(8) . . . . ? C2 C3 C4 C9 -47.1(9) . . . . ? C9 C4 C5 C6 1.3(12) . . . . ? C3 C4 C5 C6 -177.0(8) . . . . ? C4 C5 C6 C7 -1.8(12) . . . . ? C4 C5 C6 C12 177.0(7) . . . . ? C5 C6 C7 C8 0.1(11) . . . . ? C12 C6 C7 C8 -178.6(7) . . . . ? C6 C7 C8 C9 1.9(10) . . . . ? C6 C7 C8 P1 -177.1(6) . . . . ? C24 P1 C8 C9 -11.4(8) . . . . ? C30 P1 C8 C9 -125.1(7) . . . . ? Rh1 P1 C8 C9 112.9(6) . . . . ? C24 P1 C8 C7 167.4(5) . . . . ? C30 P1 C8 C7 53.8(6) . . . . ? Rh1 P1 C8 C7 -68.3(5) . . . . ? C7 C8 C9 O1 179.3(6) . . . . ? P1 C8 C9 O1 -1.9(10) . . . . ? C7 C8 C9 C4 -2.4(11) . . . . ? P1 C8 C9 C4 176.5(6) . . . . ? C1 O1 C9 C8 -131.2(7) . . . . ? C1 O1 C9 C4 50.4(8) . . . . ? C5 C4 C9 C8 0.8(11) . . . . ? C3 C4 C9 C8 179.3(7) . . . . ? C5 C4 C9 O1 179.2(6) . . . . ? C3 C4 C9 O1 -2.3(10) . . . . ? O1 C1 C13 C14 -128.3(6) . . . . ? O2 C1 C13 C14 -12.5(9) . . . . ? C2 C1 C13 C14 107.6(7) . . . . ? C1 C13 C14 C15 52.6(8) . . . . ? C1 C13 C14 C22 173.8(6) . . . . ? C1 C13 C14 C21 -67.5(8) . . . . ? C22 C14 C15 C16 15.0(10) . . . . ? C21 C14 C15 C16 -106.5(8) . . . . ? C13 C14 C15 C16 132.5(7) . . . . ? C22 C14 C15 C20 -164.4(6) . . . . ? C21 C14 C15 C20 74.1(8) . . . . ? C13 C14 C15 C20 -46.9(8) . . . . ? C20 C15 C16 C17 1.0(11) . . . . ? C14 C15 C16 C17 -178.4(7) . . . . ? C15 C16 C17 C18 -0.6(11) . . . . ? C15 C16 C17 C23 -179.9(7) . . . . ? C16 C17 C18 C19 -1.2(10) . . . . ? C23 C17 C18 C19 178.2(7) . . . . ? C17 C18 C19 C20 2.3(10) . . . . ? C17 C18 C19 P2 -178.0(5) . . . . ? C36 P2 C19 C20 -12.8(8) . . . . ? C42 P2 C19 C20 -126.7(7) . . . . ? Rh1 P2 C19 C20 114.1(6) . . . . ? C36 P2 C19 C18 167.6(5) . . . . ? C42 P2 C19 C18 53.6(6) . . . . ? Rh1 P2 C19 C18 -65.5(5) . . . . ? C1 O2 C20 C19 -132.0(7) . . . . ? C1 O2 C20 C15 49.4(8) . . . . ? C18 C19 C20 O2 179.6(6) . . . . ? P2 C19 C20 O2 0.0(10) . . . . ? C18 C19 C20 C15 -1.9(10) . . . . ? P2 C19 C20 C15 178.5(6) . . . . ? C16 C15 C20 O2 178.8(6) . . . . ? C14 C15 C20 O2 -1.7(9) . . . . ? C16 C15 C20 C19 0.3(11) . . . . ? C14 C15 C20 C19 179.7(7) . . . . ? C8 P1 C24 C29 -64.5(6) . . . . ? C30 P1 C24 C29 42.7(6) . . . . ? Rh1 P1 C24 C29 169.5(5) . . . . ? C8 P1 C24 C25 167.5(5) . . . . ? C30 P1 C24 C25 -85.3(5) . . . . ? Rh1 P1 C24 C25 41.4(5) . . . . ? C29 C24 C25 C26 55.4(8) . . . . ? P1 C24 C25 C26 -173.2(5) . . . . ? C24 C25 C26 C27 -56.6(8) . . . . ? C25 C26 C27 C28 57.7(9) . . . . ? C26 C27 C28 C29 -57.8(9) . . . . ? C27 C28 C29 C24 56.2(9) . . . . ? C25 C24 C29 C28 -54.9(8) . . . . ? P1 C24 C29 C28 178.0(5) . . . . ? C8 P1 C30 C31 168.3(5) . . . . ? C24 P1 C30 C31 53.1(6) . . . . ? Rh1 P1 C30 C31 -70.9(5) . . . . ? C8 P1 C30 C35 41.0(5) . . . . ? C24 P1 C30 C35 -74.2(5) . . . . ? Rh1 P1 C30 C35 161.8(4) . . . . ? C35 C30 C31 C32 -61.0(7) . . . . ? P1 C30 C31 C32 168.2(5) . . . . ? C30 C31 C32 C33 59.1(8) . . . . ? C31 C32 C33 C34 -56.4(8) . . . . ? C32 C33 C34 C35 55.7(8) . . . . ? C33 C34 C35 C30 -57.7(8) . . . . ? C31 C30 C35 C34 60.5(7) . . . . ? P1 C30 C35 C34 -169.3(5) . . . . ? C19 P2 C36 C41 -62.9(6) . . . . ? C42 P2 C36 C41 45.4(6) . . . . ? Rh1 P2 C36 C41 172.8(4) . . . . ? C19 P2 C36 C37 170.3(5) . . . . ? C42 P2 C36 C37 -81.4(5) . . . . ? Rh1 P2 C36 C37 46.0(5) . . . . ? C41 C36 C37 C38 54.8(8) . . . . ? P2 C36 C37 C38 -175.7(5) . . . . ? C36 C37 C38 C39 -53.3(8) . . . . ? C37 C38 C39 C40 54.5(8) . . . . ? C38 C39 C40 C41 -57.5(8) . . . . ? C39 C40 C41 C36 59.0(8) . . . . ? C37 C36 C41 C40 -57.5(8) . . . . ? P2 C36 C41 C40 176.8(5) . . . . ? C19 P2 C42 C47 38.5(5) . . . . ? C36 P2 C42 C47 -76.7(5) . . . . ? Rh1 P2 C42 C47 155.2(4) . . . . ? C19 P2 C42 C43 169.0(5) . . . . ? C36 P2 C42 C43 53.8(6) . . . . ? Rh1 P2 C42 C43 -74.3(5) . . . . ? C47 C42 C43 C44 -59.3(8) . . . . ? P2 C42 C43 C44 165.7(5) . . . . ? C42 C43 C44 C45 55.6(8) . . . . ? C43 C44 C45 C46 -53.0(8) . . . . ? C44 C45 C46 C47 56.3(8) . . . . ? C45 C46 C47 C42 -59.4(8) . . . . ? C43 C42 C47 C46 59.9(7) . . . . ? P2 C42 C47 C46 -167.4(5) . . . . ? C51 Rh1 C48 C49 65.6(5) . . . . ? C52 Rh1 C48 C49 102.1(5) . . . . ? P2 Rh1 C48 C49 -83.2(4) . . . . ? P1 Rh1 C48 C49 152.8(4) . . . . ? C51 Rh1 C48 C53 -39.6(4) . . . . ? C52 Rh1 C48 C53 -3.1(4) . . . . ? C49 Rh1 C48 C53 -105.2(6) . . . . ? P2 Rh1 C48 C53 171.6(3) . . . . ? P1 Rh1 C48 C53 47.6(6) . . . . ? C53 C48 C49 C50 0.1(7) . . . . ? Rh1 C48 C49 C50 -91.9(5) . . . . ? C53 C48 C49 Rh1 92.0(5) . . . . ? C51 Rh1 C49 C48 -101.7(5) . . . . ? C52 Rh1 C49 C48 -65.3(5) . . . . ? P2 Rh1 C49 C48 102.5(4) . . . . ? P1 Rh1 C49 C48 -126.2(6) . . . . ? C51 Rh1 C49 C50 3.1(3) . . . . ? C52 Rh1 C49 C50 39.5(4) . . . . ? C48 Rh1 C49 C50 104.8(6) . . . . ? P2 Rh1 C49 C50 -152.7(3) . . . . ? P1 Rh1 C49 C50 -21.4(9) . . . . ? C48 C49 C50 C51 68.3(6) . . . . ? Rh1 C49 C50 C51 -4.0(4) . . . . ? C48 C49 C50 C54 -34.5(7) . . . . ? Rh1 C49 C50 C54 -106.9(4) . . . . ? C49 C50 C51 C52 -69.4(6) . . . . ? C54 C50 C51 C52 33.4(7) . . . . ? C49 C50 C51 Rh1 4.1(4) . . . . ? C54 C50 C51 Rh1 106.9(5) . . . . ? C48 Rh1 C51 C52 65.2(4) . . . . ? C49 Rh1 C51 C52 102.7(5) . . . . ? P2 Rh1 C51 C52 156.4(3) . . . . ? P1 Rh1 C51 C52 -84.2(4) . . . . ? C52 Rh1 C51 C50 -105.8(6) . . . . ? C48 Rh1 C51 C50 -40.6(4) . . . . ? C49 Rh1 C51 C50 -3.1(3) . . . . ? P2 Rh1 C51 C50 50.6(6) . . . . ? P1 Rh1 C51 C50 170.0(3) . . . . ? C50 C51 C52 C53 -0.1(8) . . . . ? Rh1 C51 C52 C53 -92.8(5) . . . . ? C50 C51 C52 Rh1 92.7(5) . . . . ? C48 Rh1 C52 C51 -102.4(5) . . . . ? C49 Rh1 C52 C51 -65.1(4) . . . . ? P2 Rh1 C52 C51 -124.1(6) . . . . ? P1 Rh1 C52 C51 100.5(4) . . . . ? C51 Rh1 C52 C53 105.6(6) . . . . ? C48 Rh1 C52 C53 3.2(4) . . . . ? C49 Rh1 C52 C53 40.5(4) . . . . ? P2 Rh1 C52 C53 -18.5(9) . . . . ? P1 Rh1 C52 C53 -153.9(4) . . . . ? C51 C52 C53 C48 69.0(7) . . . . ? Rh1 C52 C53 C48 -4.1(5) . . . . ? C51 C52 C53 C54 -33.0(7) . . . . ? Rh1 C52 C53 C54 -106.1(5) . . . . ? C49 C48 C53 C52 -68.7(7) . . . . ? Rh1 C48 C53 C52 4.1(5) . . . . ? C49 C48 C53 C54 34.0(7) . . . . ? Rh1 C48 C53 C54 106.8(4) . . . . ? C49 C50 C54 C53 52.5(6) . . . . ? C51 C50 C54 C53 -50.0(6) . . . . ? C52 C53 C54 C50 50.1(6) . . . . ? C48 C53 C54 C50 -52.0(6) . . . . ? C6Y C1Y C2Y C3Y -110(7) . . . . ? C4Y C1Y C2Y C3Y -118(5) . . . . ? C6Y C1Y C2Y C4Y 9(8) . . . . ? C3Y C1Y C2Y C4Y 118(5) . . . . ? C6Y C1Y C2Y C5Y -39(18) . . . . ? C3Y C1Y C2Y C5Y 70(15) . . . . ? C4Y C1Y C2Y C5Y -48(13) . . . . ? C3Y C1Y C2Y C6Y 110(7) . . . . ? C4Y C1Y C2Y C6Y -9(8) . . . . ? C4Y C2Y C3Y C5Y 54(6) . . . . ? C1Y C2Y C3Y C5Y 157(6) . . . . ? C6Y C2Y C3Y C5Y 125(6) . . . . ? C4Y C2Y C3Y C1Y -104(8) . . . . ? C5Y C2Y C3Y C1Y -157(6) . . . . ? C6Y C2Y C3Y C1Y -32(3) . . . . ? C6Y C1Y C3Y C2Y 78(8) . . . . ? C4Y C1Y C3Y C2Y 37(3) . . . . ? C6Y C1Y C3Y C5Y 59(9) . . . . ? C2Y C1Y C3Y C5Y -19(5) . . . . ? C4Y C1Y C3Y C5Y 19(3) . . . . ? C3Y C2Y C4Y C5Y -62(7) . . . . ? C1Y C2Y C4Y C5Y -161(6) . . . . ? C6Y C2Y C4Y C5Y -155(5) . . . . ? C3Y C2Y C4Y C6Y 94(8) . . . . ? C1Y C2Y C4Y C6Y -5(5) . . . . ? C5Y C2Y C4Y C6Y 155(5) . . . . ? C3Y C2Y C4Y C1Y 99(9) . . . . ? C5Y C2Y C4Y C1Y 161(6) . . . . ? C6Y C2Y C4Y C1Y 5(5) . . . . ? C6Y C1Y C4Y C2Y -170(10) . . . . ? C3Y C1Y C4Y C2Y -40(5) . . . . ? C6Y C1Y C4Y C5Y -152(8) . . . . ? C2Y C1Y C4Y C5Y 17(6) . . . . ? C3Y C1Y C4Y C5Y -22(4) . . . . ? C2Y C1Y C4Y C6Y 170(10) . . . . ? C3Y C1Y C4Y C6Y 130(8) . . . . ? C3Y C2Y C5Y C4Y 127(4) . . . . ? C1Y C2Y C5Y C4Y 54(14) . . . . ? C6Y C2Y C5Y C4Y 28(6) . . . . ? C4Y C2Y C5Y C3Y -127(4) . . . . ? C1Y C2Y C5Y C3Y -73(16) . . . . ? C6Y C2Y C5Y C3Y -99(7) . . . . ? C3Y C2Y C5Y C5Y 155(19) . . . 3 ? C4Y C2Y C5Y C5Y 28(20) . . . 3 ? C1Y C2Y C5Y C5Y 82(28) . . . 3 ? C6Y C2Y C5Y C5Y 57(23) . . . 3 ? C6Y C4Y C5Y C2Y -27(6) . . . . ? C1Y C4Y C5Y C2Y -13(4) . . . . ? C2Y C4Y C5Y C3Y 35(4) . . . . ? C6Y C4Y C5Y C3Y 9(6) . . . . ? C1Y C4Y C5Y C3Y 23(4) . . . . ? C2Y C4Y C5Y C5Y -172(7) . . . 3 ? C6Y C4Y C5Y C5Y 162(5) . . . 3 ? C1Y C4Y C5Y C5Y 176(4) . . . 3 ? C1Y C3Y C5Y C2Y 16(4) . . . . ? C2Y C3Y C5Y C4Y -40(4) . . . . ? C1Y C3Y C5Y C4Y -25(4) . . . . ? C2Y C3Y C5Y C5Y -167(7) . . . 3 ? C1Y C3Y C5Y C5Y -151(4) . . . 3 ? C3Y C1Y C6Y C2Y -41(4) . . . . ? C4Y C1Y C6Y C2Y 7(6) . . . . ? C2Y C1Y C6Y C4Y -7(6) . . . . ? C3Y C1Y C6Y C4Y -48(7) . . . . ? C3Y C2Y C6Y C1Y 75(8) . . . . ? C4Y C2Y C6Y C1Y -171(9) . . . . ? C5Y C2Y C6Y C1Y 162(9) . . . . ? C3Y C2Y C6Y C4Y -114(5) . . . . ? C1Y C2Y C6Y C4Y 171(9) . . . . ? C5Y C2Y C6Y C4Y -28(6) . . . . ? C2Y C4Y C6Y C1Y 7(7) . . . . ? C5Y C4Y C6Y C1Y 33(10) . . . . ? C5Y C4Y C6Y C2Y 26(6) . . . . ? C1Y C4Y C6Y C2Y -7(7) . . . . ? C4X C1X C3X C6X -42(6) . . . . ? C11X C1X C3X C6X -63(7) . . . . ? C8X C1X C3X C6X -35(5) . . . . ? C4X C1X C3X C7X -116(4) . . . . ? C11X C1X C3X C7X -136(5) . . . . ? C8X C1X C3X C7X -108(4) . . . . ? C4X C1X C3X C8X -7(4) . . . . ? C11X C1X C3X C8X -27(5) . . . . ? C11X C1X C3X C4X -20(4) . . . . ? C8X C1X C3X C4X 7(4) . . . . ? C3X C1X C4X C11X -148(7) . . . . ? C8X C1X C4X C11X -160(10) . . . . ? C11X C1X C4X C8X 160(10) . . . . ? C3X C1X C4X C8X 12(6) . . . . ? C11X C1X C4X C3X 148(7) . . . . ? C8X C1X C4X C3X -12(6) . . . . ? C11X C1X C4X C5X 3(5) . . . . ? C3X C1X C4X C5X -145(4) . . . . ? C8X C1X C4X C5X -157(7) . . . . ? C6X C3X C4X C11X -179(10) . . . . ? C1X C3X C4X C11X 40(9) . . . . ? C7X C3X C4X C11X 118(9) . . . . ? C8X C3X C4X C11X -152(11) . . . . ? C6X C3X C4X C8X -27(5) . . . . ? C1X C3X C4X C8X -168(6) . . . . ? C7X C3X C4X C8X -90(5) . . . . ? C6X C3X C4X C1X 141(5) . . . . ? C7X C3X C4X C1X 78(5) . . . . ? C8X C3X C4X C1X 168(6) . . . . ? C6X C3X C4X C5X -154(7) . . . . ? C1X C3X C4X C5X 64(7) . . . . ? C7X C3X C4X C5X 143(6) . . . . ? C8X C3X C4X C5X -128(9) . . . . ? C8X C4X C5X C11X -157(17) . . . . ? C1X C4X C5X C11X -6(11) . . . . ? C3X C4X C5X C11X -52(13) . . . . ? C11X C4X C5X C10X -157(14) . . . . ? C8X C4X C5X C10X 46(7) . . . . ? C1X C4X C5X C10X -163(5) . . . . ? C3X C4X C5X C10X 151(7) . . . . ? C1X C3X C6X C8X 46(6) . . . . ? C7X C3X C6X C8X 141(5) . . . . ? C4X C3X C6X C8X 20(4) . . . . ? C1X C3X C6X C7X -95(5) . . . . ? C8X C3X C6X C7X -141(5) . . . . ? C4X C3X C6X C7X -121(3) . . . . ? C1X C3X C7X C6X 110(5) . . . . ? C8X C3X C7X C6X 31(4) . . . . ? C4X C3X C7X C6X 70(4) . . . . ? C6X C3X C7X C9X 165(14) . . . . ? C1X C3X C7X C9X -85(14) . . . . ? C8X C3X C7X C9X -164(13) . . . . ? C4X C3X C7X C9X -125(13) . . . . ? C8X C6X C7X C3X -64(7) . . . . ? C3X C6X C7X C9X -168(12) . . . . ? C8X C6X C7X C9X 128(11) . . . . ? C11X C4X C8X C6X 141(22) . . . . ? C1X C4X C8X C6X 13(7) . . . . ? C3X C4X C8X C6X 23(4) . . . . ? C5X C4X C8X C6X 163(5) . . . . ? C11X C4X C8X C3X 118(23) . . . . ? C1X C4X C8X C3X -10(5) . . . . ? C5X C4X C8X C3X 141(6) . . . . ? C1X C4X C8X C11X -128(25) . . . . ? C3X C4X C8X C11X -118(23) . . . . ? C5X C4X C8X C11X 23(19) . . . . ? C11X C4X C8X C1X 128(25) . . . . ? C3X C4X C8X C1X 10(5) . . . . ? C5X C4X C8X C1X 150(9) . . . . ? C3X C6X C8X C4X -38(6) . . . . ? C7X C6X C8X C4X 18(9) . . . . ? C7X C6X C8X C3X 55(6) . . . . ? C3X C6X C8X C11X -30(6) . . . . ? C7X C6X C8X C11X 25(9) . . . . ? C3X C6X C8X C1X -30(4) . . . . ? C7X C6X C8X C1X 25(6) . . . . ? C6X C3X C8X C4X 145(6) . . . . ? C1X C3X C8X C4X 8(4) . . . . ? C7X C3X C8X C4X 106(5) . . . . ? C1X C3X C8X C6X -137(5) . . . . ? C7X C3X C8X C6X -39(5) . . . . ? C4X C3X C8X C6X -145(6) . . . . ? C6X C3X C8X C11X 154(6) . . . . ? C1X C3X C8X C11X 17(3) . . . . ? C7X C3X C8X C11X 115(4) . . . . ? C4X C3X C8X C11X 9(4) . . . . ? C6X C3X C8X C1X 137(5) . . . . ? C7X C3X C8X C1X 98(4) . . . . ? C4X C3X C8X C1X -8(4) . . . . ? C11X C1X C8X C4X -12(6) . . . . ? C3X C1X C8X C4X -166(7) . . . . ? C4X C1X C8X C6X -168(7) . . . . ? C11X C1X C8X C6X 180(5) . . . . ? C3X C1X C8X C6X 26(3) . . . . ? C4X C1X C8X C3X 166(7) . . . . ? C11X C1X C8X C3X 154(4) . . . . ? C4X C1X C8X C11X 12(6) . . . . ? C3X C1X C8X C11X -154(4) . . . . ? C3X C7X C9X C12X 139(13) . . . . ? C6X C7X C9X C12X -66(13) . . . . ? C3X C7X C9X C2X 55(17) . . . . ? C6X C7X C9X C2X -150(9) . . . . ? C12X C2X C9X C7X 97(8) . . . . ? C11X C5X C10X C10X -179(7) . . . 5_666 ? C4X C5X C10X C10X -172(7) . . . 5_666 ? C8X C4X C11X C5X 42(30) . . . . ? C1X C4X C11X C5X 174(11) . . . . ? C3X C4X C11X C5X 145(9) . . . . ? C8X C4X C11X C1X -133(24) . . . . ? C3X C4X C11X C1X -29(6) . . . . ? C5X C4X C11X C1X -174(11) . . . . ? C1X C4X C11X C8X 133(24) . . . . ? C3X C4X C11X C8X 104(23) . . . . ? C5X C4X C11X C8X -42(30) . . . . ? C10X C5X C11X C4X 23(14) . . . . ? C10X C5X C11X C1X -171(16) . . . . ? C4X C5X C11X C1X 165(28) . . . . ? C10X C5X C11X C8X 36(7) . . . . ? C4X C5X C11X C8X 13(9) . . . . ? C3X C1X C11X C4X 38(8) . . . . ? C8X C1X C11X C4X 12(6) . . . . ? C4X C1X C11X C5X -169(21) . . . . ? C3X C1X C11X C5X -131(16) . . . . ? C8X C1X C11X C5X -157(18) . . . . ? C4X C1X C11X C8X -12(6) . . . . ? C3X C1X C11X C8X 26(4) . . . . ? C6X C8X C11X C4X -43(24) . . . . ? C3X C8X C11X C4X -61(23) . . . . ? C1X C8X C11X C4X -43(23) . . . . ? C4X C8X C11X C5X -147(26) . . . . ? C6X C8X C11X C5X 170(6) . . . . ? C3X C8X C11X C5X 152(6) . . . . ? C1X C8X C11X C5X 170(7) . . . . ? C4X C8X C11X C1X 43(23) . . . . ? C6X C8X C11X C1X 0(5) . . . . ? C3X C8X C11X C1X -18(3) . . . . ? C7X C9X C12X C2X -138(4) . . . . ? C7X C9X C12X C12X 31(6) . . . 3_655 ? C2X C9X C12X C12X 169(4) . . . 3_655 ? C9X C2X C12X C12X -151(19) . . . 3_655 ? _diffrn_measured_fraction_theta_max 0.915 _diffrn_reflns_theta_full 26.48 _diffrn_measured_fraction_theta_full 0.915 _refine_diff_density_max 1.761 _refine_diff_density_min -1.605 _refine_diff_density_rms 0.136 #===END data_cji19a_0m _database_code_depnum_ccdc_archive 'CCDC 286681' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H78 Cl2 O2 P2 Rh2' _chemical_formula_weight 1061.79 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' 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.3860(15) _cell_length_b 18.114(2) _cell_length_c 21.617(3) _cell_angle_alpha 90.00 _cell_angle_beta 97.392(4) _cell_angle_gamma 90.00 _cell_volume 4809.9(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5830 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 33.37 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 0.903 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6919 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 70795 _diffrn_reflns_av_R_equivalents 0.0645 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 36.03 _reflns_number_total 20080 _reflns_number_gt 13264 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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^)+(0.0791P)^2^+17.7269P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20080 _refine_ls_number_parameters 546 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1104 _refine_ls_R_factor_gt 0.0683 _refine_ls_wR_factor_ref 0.1957 _refine_ls_wR_factor_gt 0.1741 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _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 1.19014(2) 0.296777(16) 0.696974(15) 0.01893(7) Uani 1 1 d . . . P1 P 1.10968(8) 0.19033(5) 0.64734(5) 0.01709(17) Uani 1 1 d . . . Cl1 Cl 1.16261(10) 0.24967(6) 0.79546(5) 0.0300(2) Uani 1 1 d . . . C1 C 0.8687(3) 0.3427(2) 0.55067(18) 0.0174(6) Uani 1 1 d . . . O1 O 0.9584(2) 0.29952(14) 0.57787(12) 0.0161(4) Uani 1 1 d . . . Rh2 Rh 0.54385(3) 0.272965(19) 0.409417(18) 0.02686(8) Uani 1 1 d . . . P2 P 0.63959(8) 0.17501(5) 0.46438(5) 0.01972(18) Uani 1 1 d . . . Cl2 Cl 0.57010(10) 0.22134(7) 0.31226(6) 0.0363(3) Uani 1 1 d . . . O2 O 0.7819(2) 0.29444(15) 0.52655(13) 0.0188(5) Uani 1 1 d . . . C2 C 0.9003(3) 0.38835(18) 0.49719(18) 0.0179(6) Uani 1 1 d . . . H2A H 0.9580 0.4236 0.5138 0.022 Uiso 1 1 calc R . . H2B H 0.8363 0.4175 0.4791 0.022 Uiso 1 1 calc R . . C3 C 0.9415(3) 0.34281(19) 0.44485(18) 0.0168(6) Uani 1 1 d . . . C4 C 0.9964(3) 0.27227(18) 0.47236(17) 0.0152(6) Uani 1 1 d . . . C5 C 1.0417(3) 0.22306(19) 0.43284(18) 0.0174(6) Uani 1 1 d . . . H5 H 1.0313 0.2317 0.3891 0.021 Uiso 1 1 calc R . . C6 C 1.1013(3) 0.16211(19) 0.45605(18) 0.0188(6) Uani 1 1 d . . . C7 C 1.1210(3) 0.15276(18) 0.52002(18) 0.0196(7) Uani 1 1 d . . . H7 H 1.1659 0.1129 0.5361 0.023 Uiso 1 1 calc R . . C8 C 1.0772(3) 0.19993(18) 0.56234(16) 0.0153(6) Uani 1 1 d . . . C9 C 1.0086(3) 0.25728(17) 0.53608(17) 0.0154(6) Uani 1 1 d . . . C10 C 0.8467(3) 0.3266(2) 0.39281(19) 0.0213(7) Uani 1 1 d . . . H10A H 0.8730 0.2957 0.3607 0.032 Uiso 1 1 calc R . . H10B H 0.8185 0.3732 0.3742 0.032 Uiso 1 1 calc R . . H10C H 0.7885 0.3006 0.4106 0.032 Uiso 1 1 calc R . . C11 C 1.0283(3) 0.3888(2) 0.41632(19) 0.0209(7) Uani 1 1 d . . . H11A H 1.0908 0.3976 0.4481 0.031 Uiso 1 1 calc R . . H11B H 0.9967 0.4361 0.4014 0.031 Uiso 1 1 calc R . . H11C H 1.0523 0.3617 0.3813 0.031 Uiso 1 1 calc R . . C12 C 1.1448(4) 0.1079(2) 0.4120(2) 0.0250(8) Uani 1 1 d . . . H12A H 1.1970 0.1330 0.3888 0.038 Uiso 1 1 calc R . . H12B H 1.0844 0.0887 0.3827 0.038 Uiso 1 1 calc R . . H12C H 1.1811 0.0670 0.4360 0.038 Uiso 1 1 calc R . . C13 C 0.8321(3) 0.3917(2) 0.60123(19) 0.0223(7) Uani 1 1 d . . . H13A H 0.7720 0.4236 0.5821 0.027 Uiso 1 1 calc R . . H13B H 0.8933 0.4242 0.6177 0.027 Uiso 1 1 calc R . . C14 C 0.7933(3) 0.3494(2) 0.6561(2) 0.0254(8) Uani 1 1 d . . . C15 C 0.7461(3) 0.2752(2) 0.63358(19) 0.0227(7) Uani 1 1 d . . . C16 C 0.7058(3) 0.2269(3) 0.6762(2) 0.0284(9) Uani 1 1 d . . . H16 H 0.7131 0.2401 0.7190 0.034 Uiso 1 1 calc R . . C17 C 0.6556(4) 0.1607(3) 0.6575(2) 0.0302(9) Uani 1 1 d . . . C18 C 0.6376(3) 0.1448(2) 0.5939(2) 0.0267(8) Uani 1 1 d . . . H18 H 0.5990 0.1011 0.5805 0.032 Uiso 1 1 calc R . . C19 C 0.6746(3) 0.1911(2) 0.54889(19) 0.0212(7) Uani 1 1 d . . . C20 C 0.7354(3) 0.2541(2) 0.57089(19) 0.0203(7) Uani 1 1 d . . . C21 C 0.7021(4) 0.3952(3) 0.6800(2) 0.0344(11) Uani 1 1 d . . . H21A H 0.6392 0.3977 0.6476 0.052 Uiso 1 1 calc R . . H21B H 0.7288 0.4452 0.6903 0.052 Uiso 1 1 calc R . . H21C H 0.6804 0.3718 0.7174 0.052 Uiso 1 1 calc R . . C22 C 0.8873(3) 0.3422(3) 0.7092(2) 0.0290(9) Uani 1 1 d . . . H22A H 0.8625 0.3151 0.7439 0.044 Uiso 1 1 calc R . . H22B H 0.9121 0.3915 0.7233 0.044 Uiso 1 1 calc R . . H22C H 0.9476 0.3154 0.6942 0.044 Uiso 1 1 calc R . . C23 C 0.6216(5) 0.1076(3) 0.7051(3) 0.0417(12) Uani 1 1 d . . . H23A H 0.5464 0.1181 0.7119 0.063 Uiso 1 1 calc R . . H23B H 0.6698 0.1132 0.7444 0.063 Uiso 1 1 calc R . . H23C H 0.6264 0.0569 0.6898 0.063 Uiso 1 1 calc R . . C24 C 0.9780(4) 0.1508(2) 0.6654(2) 0.0268(8) Uani 1 1 d . . . H24 H 0.9203 0.1840 0.6441 0.032 Uiso 1 1 calc R . . C25 C 0.9578(4) 0.1483(3) 0.7335(2) 0.0318(9) Uani 1 1 d . . . H25A H 0.8835 0.1311 0.7359 0.048 Uiso 1 1 calc R . . H25B H 0.9672 0.1978 0.7516 0.048 Uiso 1 1 calc R . . H25C H 1.0098 0.1144 0.7567 0.048 Uiso 1 1 calc R . . C26 C 0.9554(5) 0.0746(3) 0.6352(3) 0.0371(11) Uani 1 1 d . . . H26A H 1.0003 0.0373 0.6592 0.056 Uiso 1 1 calc R . . H26B H 0.9731 0.0756 0.5923 0.056 Uiso 1 1 calc R . . H26C H 0.8782 0.0622 0.6348 0.056 Uiso 1 1 calc R . . C28 C 1.2084(4) 0.1118(2) 0.6574(2) 0.0263(8) Uani 1 1 d . . . H28 H 1.1804 0.0720 0.6276 0.032 Uiso 1 1 calc R . . C29 C 1.3202(4) 0.1345(3) 0.6424(3) 0.0369(11) Uani 1 1 d . . . H29A H 1.3526 0.1700 0.6736 0.055 Uiso 1 1 calc R . . H29B H 1.3132 0.1573 0.6009 0.055 Uiso 1 1 calc R . . H29C H 1.3670 0.0908 0.6429 0.055 Uiso 1 1 calc R . . C30 C 1.2186(5) 0.0795(3) 0.7237(2) 0.0362(11) Uani 1 1 d . . . H30A H 1.2780 0.0434 0.7290 0.054 Uiso 1 1 calc R . . H30B H 1.1502 0.0552 0.7301 0.054 Uiso 1 1 calc R . . H30C H 1.2341 0.1193 0.7543 0.054 Uiso 1 1 calc R . . C32 C 1.2066(4) 0.4068(2) 0.7404(2) 0.0273(8) Uani 1 1 d . . . H32 H 1.1765 0.4099 0.7810 0.033 Uiso 1 1 calc R . . C33 C 1.1626(4) 0.4645(2) 0.6941(2) 0.0282(9) Uani 1 1 d . . . H33A H 1.1945 0.5131 0.7070 0.034 Uiso 1 1 calc R . . H33B H 1.0827 0.4679 0.6932 0.034 Uiso 1 1 calc R . . C34 C 1.1907(3) 0.4447(2) 0.6260(2) 0.0268(8) Uani 1 1 d . . . H34A H 1.1358 0.4676 0.5945 0.032 Uiso 1 1 calc R . . H34B H 1.2627 0.4657 0.6206 0.032 Uiso 1 1 calc R . . C35 C 1.1926(3) 0.3628(2) 0.61500(19) 0.0212(7) Uani 1 1 d . . . H35 H 1.1389 0.3463 0.5792 0.025 Uiso 1 1 calc R . . C36 C 1.2862(3) 0.3180(2) 0.62464(19) 0.0225(7) Uani 1 1 d . . . H36 H 1.2863 0.2768 0.5939 0.027 Uiso 1 1 calc R . . C37 C 1.3989(3) 0.3440(3) 0.6511(2) 0.0319(9) Uani 1 1 d . . . H37A H 1.4327 0.3696 0.6179 0.038 Uiso 1 1 calc R . . H37B H 1.4445 0.3006 0.6646 0.038 Uiso 1 1 calc R . . C38 C 1.3967(4) 0.3964(3) 0.7066(2) 0.0313(9) Uani 1 1 d . . . H38A H 1.4685 0.3957 0.7327 0.038 Uiso 1 1 calc R . . H38B H 1.3829 0.4474 0.6911 0.038 Uiso 1 1 calc R . . C39 C 1.3114(3) 0.3750(2) 0.7452(2) 0.0268(8) Uani 1 1 d . . . H39 H 1.3407 0.3596 0.7885 0.032 Uiso 1 1 calc R . . C40 C 0.7729(3) 0.1380(2) 0.4462(2) 0.0230(7) Uani 1 1 d . . . H40 H 0.8289 0.1741 0.4650 0.028 Uiso 1 1 calc R . . C41 C 0.8017(5) 0.0647(3) 0.4803(3) 0.0362(10) Uani 1 1 d . . . H41A H 0.7527 0.0258 0.4619 0.054 Uiso 1 1 calc R . . H41B H 0.7936 0.0702 0.5245 0.054 Uiso 1 1 calc R . . H41C H 0.8771 0.0514 0.4761 0.054 Uiso 1 1 calc R . . C42 C 0.7901(4) 0.1320(2) 0.3775(2) 0.0262(8) Uani 1 1 d . . . H42A H 0.8672 0.1225 0.3745 0.039 Uiso 1 1 calc R . . H42B H 0.7681 0.1783 0.3560 0.039 Uiso 1 1 calc R . . H42C H 0.7461 0.0913 0.3579 0.039 Uiso 1 1 calc R . . C44 C 0.5464(4) 0.0944(3) 0.4601(2) 0.0331(10) Uani 1 1 d . . . H44 H 0.5791 0.0569 0.4909 0.040 Uiso 1 1 calc R . . C45 C 0.4350(4) 0.1150(5) 0.4775(3) 0.0586(19) Uani 1 1 d . . . H45A H 0.4032 0.1544 0.4498 0.088 Uiso 1 1 calc R . . H45B H 0.4426 0.1321 0.5208 0.088 Uiso 1 1 calc R . . H45C H 0.3873 0.0716 0.4729 0.088 Uiso 1 1 calc R . . C46 C 0.5340(5) 0.0587(3) 0.3952(3) 0.0466(14) Uani 1 1 d . . . H46A H 0.4762 0.0215 0.3924 0.070 Uiso 1 1 calc R . . H46B H 0.6027 0.0352 0.3884 0.070 Uiso 1 1 calc R . . H46C H 0.5150 0.0967 0.3634 0.070 Uiso 1 1 calc R . . C48 C 0.5092(7) 0.3782(4) 0.3623(5) 0.089(4) Uani 1 1 d . . . H48 H 0.5358 0.3813 0.3206 0.106 Uiso 1 1 calc R . . C49 C 0.4109(5) 0.3403(4) 0.3613(3) 0.0486(15) Uani 1 1 d . . . H49 H 0.3797 0.3214 0.3194 0.058 Uiso 1 1 calc R . . C50 C 0.3276(4) 0.3631(4) 0.4027(3) 0.0423(13) Uani 1 1 d . . . H50A H 0.3377 0.4159 0.4138 0.051 Uiso 1 1 calc R . . H50B H 0.2536 0.3569 0.3799 0.051 Uiso 1 1 calc R . . C51 C 0.3383(5) 0.3181(5) 0.4603(3) 0.0549(17) Uani 1 1 d . . . H51A H 0.2962 0.2720 0.4519 0.066 Uiso 1 1 calc R . . H51B H 0.3060 0.3456 0.4930 0.066 Uiso 1 1 calc R . . C52 C 0.4560(6) 0.2985(5) 0.4849(3) 0.063(2) Uani 1 1 d . . . H52 H 0.4627 0.2600 0.5184 0.075 Uiso 1 1 calc R . . C53 C 0.5411(6) 0.3433(5) 0.4878(5) 0.093(4) Uani 1 1 d . . . H53 H 0.5992 0.3318 0.5230 0.112 Uiso 1 1 calc R . . C54 C 0.5351(7) 0.4231(6) 0.4706(9) 0.161(8) Uani 1 1 d . . . H54A H 0.4625 0.4420 0.4773 0.193 Uiso 1 1 calc R . . H54B H 0.5900 0.4502 0.4993 0.193 Uiso 1 1 calc R . . C55 C 0.5526(7) 0.4396(4) 0.4073(7) 0.104(5) Uani 1 1 d . . . H55A H 0.6315 0.4461 0.4055 0.125 Uiso 1 1 calc R . . H55B H 0.5157 0.4866 0.3941 0.125 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 0.02329(13) 0.02072(12) 0.01354(14) 0.00004(9) 0.00527(10) -0.00165(10) P1 0.0229(4) 0.0172(4) 0.0112(4) 0.0000(3) 0.0023(3) -0.0009(3) Cl1 0.0448(6) 0.0309(4) 0.0158(5) 0.0000(3) 0.0093(4) -0.0084(4) C1 0.0162(13) 0.0219(14) 0.0148(17) -0.0054(11) 0.0046(12) -0.0005(11) O1 0.0163(10) 0.0207(10) 0.0120(12) -0.0024(9) 0.0048(9) 0.0018(8) Rh2 0.02133(14) 0.03154(16) 0.0289(2) -0.00231(12) 0.00759(13) -0.00181(11) P2 0.0223(4) 0.0250(4) 0.0121(5) -0.0019(3) 0.0031(4) -0.0052(3) Cl2 0.0360(5) 0.0533(7) 0.0212(6) 0.0026(4) 0.0095(5) 0.0052(5) O2 0.0178(11) 0.0256(12) 0.0139(13) -0.0036(9) 0.0062(10) -0.0032(9) C2 0.0192(14) 0.0169(13) 0.0183(18) -0.0005(11) 0.0046(13) 0.0011(11) C3 0.0177(14) 0.0197(14) 0.0136(17) 0.0017(11) 0.0045(12) 0.0009(11) C4 0.0163(13) 0.0188(13) 0.0115(16) 0.0009(11) 0.0058(12) 0.0000(10) C5 0.0223(15) 0.0183(13) 0.0123(17) -0.0012(11) 0.0050(13) 0.0011(11) C6 0.0241(15) 0.0182(13) 0.0145(17) -0.0026(11) 0.0043(13) 0.0010(11) C7 0.0292(17) 0.0148(13) 0.0149(18) -0.0010(11) 0.0039(14) 0.0029(12) C8 0.0201(14) 0.0174(13) 0.0083(15) -0.0005(10) 0.0012(12) -0.0003(11) C9 0.0190(14) 0.0153(12) 0.0126(16) -0.0025(10) 0.0053(12) -0.0022(10) C10 0.0213(15) 0.0242(16) 0.018(2) 0.0044(13) 0.0026(14) 0.0029(12) C11 0.0223(16) 0.0216(15) 0.020(2) 0.0064(13) 0.0082(14) 0.0020(12) C12 0.035(2) 0.0244(16) 0.016(2) -0.0040(13) 0.0037(16) 0.0073(14) C13 0.0211(16) 0.0282(17) 0.018(2) -0.0091(13) 0.0058(14) 0.0010(13) C14 0.0221(16) 0.036(2) 0.019(2) -0.0119(15) 0.0092(15) -0.0032(14) C15 0.0186(15) 0.0383(19) 0.0123(18) -0.0074(14) 0.0060(14) -0.0065(14) C16 0.0230(17) 0.048(2) 0.015(2) -0.0059(16) 0.0082(15) -0.0076(16) C17 0.0275(19) 0.050(3) 0.014(2) 0.0003(17) 0.0059(16) -0.0114(17) C18 0.0280(18) 0.036(2) 0.017(2) 0.0001(15) 0.0054(16) -0.0116(15) C19 0.0224(16) 0.0296(18) 0.0118(18) -0.0009(12) 0.0029(14) -0.0046(13) C20 0.0191(15) 0.0295(17) 0.0135(18) -0.0043(13) 0.0070(13) -0.0032(12) C21 0.0264(19) 0.048(3) 0.032(3) -0.019(2) 0.0149(19) -0.0028(17) C22 0.0259(18) 0.041(2) 0.021(2) -0.0115(17) 0.0064(16) -0.0081(16) C23 0.045(3) 0.060(3) 0.019(3) 0.004(2) 0.003(2) -0.023(2) C24 0.0318(19) 0.0321(19) 0.017(2) 0.0007(14) 0.0052(16) -0.0144(15) C25 0.039(2) 0.039(2) 0.019(2) 0.0035(16) 0.0073(18) -0.0144(18) C26 0.049(3) 0.033(2) 0.028(3) -0.0035(18) 0.001(2) -0.021(2) C28 0.039(2) 0.0206(15) 0.019(2) 0.0029(13) 0.0023(17) 0.0073(14) C29 0.034(2) 0.039(2) 0.038(3) 0.000(2) 0.004(2) 0.0144(18) C30 0.058(3) 0.0272(19) 0.022(3) 0.0058(16) -0.001(2) 0.0085(19) C32 0.038(2) 0.0260(17) 0.018(2) -0.0039(14) 0.0070(17) -0.0066(15) C33 0.032(2) 0.0170(15) 0.033(3) 0.0025(14) -0.0034(18) -0.0041(13) C34 0.0270(18) 0.0262(17) 0.026(2) 0.0082(15) -0.0010(16) -0.0031(14) C35 0.0233(16) 0.0248(16) 0.0157(19) 0.0021(13) 0.0041(14) -0.0018(12) C36 0.0235(16) 0.0300(17) 0.0149(19) -0.0001(13) 0.0063(14) -0.0011(13) C37 0.0226(18) 0.042(2) 0.033(3) 0.0056(19) 0.0078(18) -0.0008(16) C38 0.0276(19) 0.040(2) 0.025(3) 0.0058(18) 0.0001(17) -0.0049(16) C39 0.0289(19) 0.0282(18) 0.020(2) -0.0007(15) -0.0075(16) -0.0075(14) C40 0.0271(17) 0.0250(16) 0.017(2) -0.0014(13) 0.0036(15) -0.0014(13) C41 0.049(3) 0.034(2) 0.025(3) 0.0022(17) 0.003(2) 0.0122(19) C42 0.033(2) 0.0292(18) 0.017(2) -0.0030(14) 0.0062(16) 0.0025(15) C44 0.029(2) 0.046(3) 0.024(2) 0.0041(18) 0.0006(18) -0.0171(18) C45 0.027(2) 0.110(6) 0.039(4) 0.018(3) 0.003(2) -0.019(3) C46 0.062(3) 0.042(3) 0.033(3) -0.008(2) -0.001(3) -0.032(3) C48 0.091(6) 0.059(4) 0.135(9) 0.052(5) 0.084(6) 0.034(4) C49 0.053(3) 0.069(4) 0.023(3) 0.006(2) 0.003(2) 0.033(3) C50 0.028(2) 0.069(4) 0.030(3) -0.007(2) 0.006(2) 0.007(2) C51 0.039(3) 0.097(5) 0.032(3) 0.009(3) 0.018(2) 0.023(3) C52 0.054(4) 0.109(6) 0.025(3) -0.007(3) 0.006(3) 0.043(4) C53 0.049(4) 0.108(6) 0.109(8) -0.082(6) -0.039(4) 0.046(4) C54 0.036(4) 0.095(7) 0.34(2) -0.137(12) -0.005(7) 0.005(4) C55 0.063(5) 0.025(3) 0.239(15) -0.006(5) 0.081(7) -0.005(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 C36 2.118(4) . ? Rh1 C35 2.141(4) . ? Rh1 C32 2.200(4) . ? Rh1 C39 2.225(4) . ? Rh1 Cl1 2.3589(11) . ? Rh1 P1 2.3637(10) . ? P1 C8 1.838(4) . ? P1 C24 1.868(4) . ? P1 C28 1.869(4) . ? C1 O1 1.421(4) . ? C1 O2 1.431(4) . ? C1 C2 1.514(5) . ? C1 C13 1.522(5) . ? O1 C9 1.390(4) . ? Rh2 C53 2.123(7) . ? Rh2 C52 2.126(6) . ? Rh2 C48 2.179(7) . ? Rh2 C49 2.199(5) . ? Rh2 Cl2 2.3594(13) . ? Rh2 P2 2.3673(11) . ? P2 C19 1.846(4) . ? P2 C44 1.856(4) . ? P2 C40 1.870(4) . ? O2 C20 1.388(4) . ? C2 C3 1.540(5) . ? C3 C4 1.531(5) . ? C3 C10 1.546(6) . ? C3 C11 1.549(5) . ? C4 C9 1.393(5) . ? C4 C5 1.401(5) . ? C5 C6 1.386(5) . ? C6 C7 1.383(6) . ? C6 C12 1.515(5) . ? C7 C8 1.410(5) . ? C8 C9 1.414(5) . ? C13 C14 1.539(6) . ? C14 C15 1.522(6) . ? C14 C22 1.532(7) . ? C14 C21 1.543(5) . ? C15 C20 1.398(6) . ? C15 C16 1.407(6) . ? C16 C17 1.386(7) . ? C17 C18 1.395(6) . ? C17 C23 1.507(6) . ? C18 C19 1.405(5) . ? C19 C20 1.415(5) . ? C24 C25 1.526(6) . ? C24 C26 1.538(6) . ? C28 C29 1.520(7) . ? C28 C30 1.538(7) . ? C32 C39 1.411(6) . ? C32 C33 1.500(6) . ? C33 C34 1.595(7) . ? C34 C35 1.503(6) . ? C35 C36 1.408(6) . ? C36 C37 1.514(6) . ? C37 C38 1.534(7) . ? C38 C39 1.479(6) . ? C40 C42 1.533(6) . ? C40 C41 1.538(6) . ? C44 C45 1.522(8) . ? C44 C46 1.534(8) . ? C48 C49 1.396(11) . ? C48 C55 1.528(16) . ? C49 C50 1.508(7) . ? C50 C51 1.479(9) . ? C51 C52 1.529(9) . ? C52 C53 1.325(13) . ? C53 C54 1.493(17) . ? C54 C55 1.44(2) . ? 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 Rh1 C35 38.61(15) . . ? C36 Rh1 C32 96.90(16) . . ? C35 Rh1 C32 80.59(16) . . ? C36 Rh1 C39 79.68(17) . . ? C35 Rh1 C39 87.20(16) . . ? C32 Rh1 C39 37.18(17) . . ? C36 Rh1 Cl1 153.14(12) . . ? C35 Rh1 Cl1 165.48(11) . . ? C32 Rh1 Cl1 87.65(12) . . ? C39 Rh1 Cl1 88.56(13) . . ? C36 Rh1 P1 93.27(12) . . ? C35 Rh1 P1 97.48(11) . . ? C32 Rh1 P1 160.51(13) . . ? C39 Rh1 P1 162.23(12) . . ? Cl1 Rh1 P1 90.75(4) . . ? C8 P1 C24 99.21(18) . . ? C8 P1 C28 104.15(18) . . ? C24 P1 C28 105.0(2) . . ? C8 P1 Rh1 113.70(11) . . ? C24 P1 Rh1 123.12(14) . . ? C28 P1 Rh1 109.65(15) . . ? O1 C1 O2 109.0(3) . . ? O1 C1 C2 110.6(3) . . ? O2 C1 C2 108.2(3) . . ? O1 C1 C13 108.2(3) . . ? O2 C1 C13 109.7(3) . . ? C2 C1 C13 111.1(3) . . ? C9 O1 C1 115.1(3) . . ? C53 Rh2 C52 36.4(4) . . ? C53 Rh2 C48 80.0(4) . . ? C52 Rh2 C48 94.5(3) . . ? C53 Rh2 C49 87.5(3) . . ? C52 Rh2 C49 79.4(2) . . ? C48 Rh2 C49 37.2(3) . . ? C53 Rh2 Cl2 165.1(3) . . ? C52 Rh2 Cl2 155.8(2) . . ? C48 Rh2 Cl2 88.4(3) . . ? C49 Rh2 Cl2 88.83(16) . . ? C53 Rh2 P2 96.2(3) . . ? C52 Rh2 P2 92.9(2) . . ? C48 Rh2 P2 161.2(3) . . ? C49 Rh2 P2 161.6(2) . . ? Cl2 Rh2 P2 91.85(4) . . ? C19 P2 C44 103.8(2) . . ? C19 P2 C40 99.34(19) . . ? C44 P2 C40 105.6(2) . . ? C19 P2 Rh2 114.69(13) . . ? C44 P2 Rh2 107.24(17) . . ? C40 P2 Rh2 124.20(13) . . ? C20 O2 C1 115.4(3) . . ? C1 C2 C3 114.3(3) . . ? C4 C3 C2 109.5(3) . . ? C4 C3 C10 112.4(3) . . ? C2 C3 C10 110.1(3) . . ? C4 C3 C11 107.9(3) . . ? C2 C3 C11 108.5(3) . . ? C10 C3 C11 108.3(3) . . ? C9 C4 C5 118.5(3) . . ? C9 C4 C3 122.2(3) . . ? C5 C4 C3 119.1(3) . . ? C6 C5 C4 121.5(4) . . ? C7 C6 C5 118.5(3) . . ? C7 C6 C12 121.2(3) . . ? C5 C6 C12 120.3(4) . . ? C6 C7 C8 122.8(3) . . ? C7 C8 C9 116.5(3) . . ? C7 C8 P1 122.6(3) . . ? C9 C8 P1 120.9(2) . . ? O1 C9 C4 122.3(3) . . ? O1 C9 C8 116.1(3) . . ? C4 C9 C8 121.6(3) . . ? C1 C13 C14 114.5(3) . . ? C15 C14 C22 112.8(4) . . ? C15 C14 C13 109.8(3) . . ? C22 C14 C13 109.7(3) . . ? C15 C14 C21 108.4(3) . . ? C22 C14 C21 108.3(4) . . ? C13 C14 C21 107.8(4) . . ? C20 C15 C16 117.8(4) . . ? C20 C15 C14 122.4(4) . . ? C16 C15 C14 119.6(4) . . ? C17 C16 C15 122.1(4) . . ? C16 C17 C18 118.3(4) . . ? C16 C17 C23 120.5(4) . . ? C18 C17 C23 121.2(4) . . ? C17 C18 C19 122.3(4) . . ? C18 C19 C20 117.1(4) . . ? C18 C19 P2 122.4(3) . . ? C20 C19 P2 120.4(3) . . ? O2 C20 C15 121.9(3) . . ? O2 C20 C19 116.3(3) . . ? C15 C20 C19 121.8(3) . . ? C25 C24 C26 109.8(4) . . ? C25 C24 P1 117.9(3) . . ? C26 C24 P1 111.8(3) . . ? C29 C28 C30 109.5(4) . . ? C29 C28 P1 111.7(3) . . ? C30 C28 P1 111.9(3) . . ? C39 C32 C33 125.8(4) . . ? C39 C32 Rh1 72.4(2) . . ? C33 C32 Rh1 109.9(3) . . ? C32 C33 C34 110.8(3) . . ? C35 C34 C33 112.2(3) . . ? C36 C35 C34 125.1(4) . . ? C36 C35 Rh1 69.8(2) . . ? C34 C35 Rh1 114.7(3) . . ? C35 C36 C37 125.3(4) . . ? C35 C36 Rh1 71.6(2) . . ? C37 C36 Rh1 110.9(3) . . ? C36 C37 C38 112.3(4) . . ? C39 C38 C37 111.4(4) . . ? C32 C39 C38 124.6(4) . . ? C32 C39 Rh1 70.5(2) . . ? C38 C39 Rh1 113.0(3) . . ? C42 C40 C41 110.5(3) . . ? C42 C40 P2 117.8(3) . . ? C41 C40 P2 111.4(3) . . ? C45 C44 C46 109.9(5) . . ? C45 C44 P2 112.0(4) . . ? C46 C44 P2 111.4(3) . . ? C49 C48 C55 127.1(7) . . ? C49 C48 Rh2 72.2(3) . . ? C55 C48 Rh2 107.9(7) . . ? C48 C49 C50 121.2(7) . . ? C48 C49 Rh2 70.6(4) . . ? C50 C49 Rh2 113.5(4) . . ? C51 C50 C49 110.8(5) . . ? C50 C51 C52 113.5(5) . . ? C53 C52 C51 126.2(8) . . ? C53 C52 Rh2 71.7(4) . . ? C51 C52 Rh2 110.0(4) . . ? C52 C53 C54 124.6(6) . . ? C52 C53 Rh2 72.0(4) . . ? C54 C53 Rh2 112.8(9) . . ? C55 C54 C53 115.3(8) . . ? C54 C55 C48 111.6(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 C36 Rh1 P1 C8 -39.38(17) . . . . ? C35 Rh1 P1 C8 -0.82(16) . . . . ? C32 Rh1 P1 C8 82.1(4) . . . . ? C39 Rh1 P1 C8 -105.2(4) . . . . ? Cl1 Rh1 P1 C8 167.19(12) . . . . ? C36 Rh1 P1 C24 -159.1(2) . . . . ? C35 Rh1 P1 C24 -120.5(2) . . . . ? C32 Rh1 P1 C24 -37.6(4) . . . . ? C39 Rh1 P1 C24 135.1(4) . . . . ? Cl1 Rh1 P1 C24 47.51(19) . . . . ? C36 Rh1 P1 C28 76.74(18) . . . . ? C35 Rh1 P1 C28 115.30(18) . . . . ? C32 Rh1 P1 C28 -161.8(4) . . . . ? C39 Rh1 P1 C28 10.9(4) . . . . ? Cl1 Rh1 P1 C28 -76.69(15) . . . . ? O2 C1 O1 C9 67.1(3) . . . . ? C2 C1 O1 C9 -51.7(4) . . . . ? C13 C1 O1 C9 -173.5(3) . . . . ? C53 Rh2 P2 C19 0.6(3) . . . . ? C52 Rh2 P2 C19 -35.7(3) . . . . ? C48 Rh2 P2 C19 77.5(9) . . . . ? C49 Rh2 P2 C19 -100.2(5) . . . . ? Cl2 Rh2 P2 C19 167.98(13) . . . . ? C53 Rh2 P2 C44 115.3(3) . . . . ? C52 Rh2 P2 C44 79.0(3) . . . . ? C48 Rh2 P2 C44 -167.8(9) . . . . ? C49 Rh2 P2 C44 14.5(5) . . . . ? Cl2 Rh2 P2 C44 -77.34(17) . . . . ? C53 Rh2 P2 C40 -121.3(3) . . . . ? C52 Rh2 P2 C40 -157.6(3) . . . . ? C48 Rh2 P2 C40 -44.4(9) . . . . ? C49 Rh2 P2 C40 137.9(5) . . . . ? Cl2 Rh2 P2 C40 46.09(17) . . . . ? O1 C1 O2 C20 66.2(3) . . . . ? C2 C1 O2 C20 -173.5(3) . . . . ? C13 C1 O2 C20 -52.2(4) . . . . ? O1 C1 C2 C3 58.2(4) . . . . ? O2 C1 C2 C3 -61.2(4) . . . . ? C13 C1 C2 C3 178.4(3) . . . . ? C1 C2 C3 C4 -29.8(4) . . . . ? C1 C2 C3 C10 94.3(4) . . . . ? C1 C2 C3 C11 -147.4(3) . . . . ? C2 C3 C4 C9 -2.8(4) . . . . ? C10 C3 C4 C9 -125.5(4) . . . . ? C11 C3 C4 C9 115.1(4) . . . . ? C2 C3 C4 C5 -178.9(3) . . . . ? C10 C3 C4 C5 58.3(4) . . . . ? C11 C3 C4 C5 -61.0(4) . . . . ? C9 C4 C5 C6 -2.6(5) . . . . ? C3 C4 C5 C6 173.7(3) . . . . ? C4 C5 C6 C7 -3.7(5) . . . . ? C4 C5 C6 C12 177.1(3) . . . . ? C5 C6 C7 C8 4.1(6) . . . . ? C12 C6 C7 C8 -176.7(4) . . . . ? C6 C7 C8 C9 1.6(5) . . . . ? C6 C7 C8 P1 -176.5(3) . . . . ? C24 P1 C8 C7 -106.5(3) . . . . ? C28 P1 C8 C7 1.7(3) . . . . ? Rh1 P1 C8 C7 121.0(3) . . . . ? C24 P1 C8 C9 75.4(3) . . . . ? C28 P1 C8 C9 -176.4(3) . . . . ? Rh1 P1 C8 C9 -57.1(3) . . . . ? C1 O1 C9 C4 19.2(4) . . . . ? C1 O1 C9 C8 -163.6(3) . . . . ? C5 C4 C9 O1 -174.3(3) . . . . ? C3 C4 C9 O1 9.6(5) . . . . ? C5 C4 C9 C8 8.7(5) . . . . ? C3 C4 C9 C8 -167.5(3) . . . . ? C7 C8 C9 O1 174.7(3) . . . . ? P1 C8 C9 O1 -7.2(4) . . . . ? C7 C8 C9 C4 -8.1(5) . . . . ? P1 C8 C9 C4 170.1(3) . . . . ? O1 C1 C13 C14 -61.1(4) . . . . ? O2 C1 C13 C14 57.7(4) . . . . ? C2 C1 C13 C14 177.3(3) . . . . ? C1 C13 C14 C15 -29.1(5) . . . . ? C1 C13 C14 C22 95.3(4) . . . . ? C1 C13 C14 C21 -147.0(4) . . . . ? C22 C14 C15 C20 -126.5(4) . . . . ? C13 C14 C15 C20 -3.9(5) . . . . ? C21 C14 C15 C20 113.6(4) . . . . ? C22 C14 C15 C16 57.2(5) . . . . ? C13 C14 C15 C16 179.8(4) . . . . ? C21 C14 C15 C16 -62.7(5) . . . . ? C20 C15 C16 C17 -0.7(7) . . . . ? C14 C15 C16 C17 175.7(4) . . . . ? C15 C16 C17 C18 -5.0(7) . . . . ? C15 C16 C17 C23 175.0(5) . . . . ? C16 C17 C18 C19 4.1(7) . . . . ? C23 C17 C18 C19 -175.8(5) . . . . ? C17 C18 C19 C20 2.3(6) . . . . ? C17 C18 C19 P2 -173.9(4) . . . . ? C44 P2 C19 C18 3.3(4) . . . . ? C40 P2 C19 C18 -105.4(4) . . . . ? Rh2 P2 C19 C18 120.0(3) . . . . ? C44 P2 C19 C20 -172.7(3) . . . . ? C40 P2 C19 C20 78.5(3) . . . . ? Rh2 P2 C19 C20 -56.1(3) . . . . ? C1 O2 C20 C15 20.0(5) . . . . ? C1 O2 C20 C19 -161.3(3) . . . . ? C16 C15 C20 O2 -173.7(4) . . . . ? C14 C15 C20 O2 9.9(6) . . . . ? C16 C15 C20 C19 7.6(6) . . . . ? C14 C15 C20 C19 -168.8(4) . . . . ? C18 C19 C20 O2 172.9(4) . . . . ? P2 C19 C20 O2 -10.8(5) . . . . ? C18 C19 C20 C15 -8.3(6) . . . . ? P2 C19 C20 C15 168.0(3) . . . . ? C8 P1 C24 C25 -167.3(4) . . . . ? C28 P1 C24 C25 85.2(4) . . . . ? Rh1 P1 C24 C25 -41.0(4) . . . . ? C8 P1 C24 C26 63.9(4) . . . . ? C28 P1 C24 C26 -43.6(4) . . . . ? Rh1 P1 C24 C26 -169.8(3) . . . . ? C8 P1 C28 C29 74.4(4) . . . . ? C24 P1 C28 C29 178.2(3) . . . . ? Rh1 P1 C28 C29 -47.6(4) . . . . ? C8 P1 C28 C30 -162.4(3) . . . . ? C24 P1 C28 C30 -58.6(4) . . . . ? Rh1 P1 C28 C30 75.6(4) . . . . ? C36 Rh1 C32 C39 -62.7(3) . . . . ? C35 Rh1 C32 C39 -97.8(3) . . . . ? Cl1 Rh1 C32 C39 90.7(3) . . . . ? P1 Rh1 C32 C39 176.3(3) . . . . ? C36 Rh1 C32 C33 59.8(3) . . . . ? C35 Rh1 C32 C33 24.7(3) . . . . ? C39 Rh1 C32 C33 122.5(4) . . . . ? Cl1 Rh1 C32 C33 -146.8(3) . . . . ? P1 Rh1 C32 C33 -61.1(5) . . . . ? C39 C32 C33 C34 44.7(6) . . . . ? Rh1 C32 C33 C34 -37.4(4) . . . . ? C32 C33 C34 C35 32.8(5) . . . . ? C33 C34 C35 C36 -93.7(5) . . . . ? C33 C34 C35 Rh1 -11.8(4) . . . . ? C32 Rh1 C35 C36 113.8(3) . . . . ? C39 Rh1 C35 C36 76.9(3) . . . . ? Cl1 Rh1 C35 C36 150.1(4) . . . . ? P1 Rh1 C35 C36 -85.9(2) . . . . ? C36 Rh1 C35 C34 -120.3(4) . . . . ? C32 Rh1 C35 C34 -6.6(3) . . . . ? C39 Rh1 C35 C34 -43.4(3) . . . . ? Cl1 Rh1 C35 C34 29.8(7) . . . . ? P1 Rh1 C35 C34 153.8(3) . . . . ? C34 C35 C36 C37 3.7(7) . . . . ? Rh1 C35 C36 C37 -102.9(4) . . . . ? C34 C35 C36 Rh1 106.6(4) . . . . ? C32 Rh1 C36 C35 -65.4(3) . . . . ? C39 Rh1 C36 C35 -98.5(3) . . . . ? Cl1 Rh1 C36 C35 -163.9(2) . . . . ? P1 Rh1 C36 C35 97.9(2) . . . . ? C35 Rh1 C36 C37 121.7(4) . . . . ? C32 Rh1 C36 C37 56.2(3) . . . . ? C39 Rh1 C36 C37 23.1(3) . . . . ? Cl1 Rh1 C36 C37 -42.3(5) . . . . ? P1 Rh1 C36 C37 -140.4(3) . . . . ? C35 C36 C37 C38 42.4(6) . . . . ? Rh1 C36 C37 C38 -39.3(5) . . . . ? C36 C37 C38 C39 35.9(5) . . . . ? C33 C32 C39 C38 2.8(7) . . . . ? Rh1 C32 C39 C38 105.0(4) . . . . ? C33 C32 C39 Rh1 -102.2(4) . . . . ? C37 C38 C39 C32 -97.2(5) . . . . ? C37 C38 C39 Rh1 -15.7(5) . . . . ? C36 Rh1 C39 C32 116.2(3) . . . . ? C35 Rh1 C39 C32 78.1(3) . . . . ? Cl1 Rh1 C39 C32 -88.0(2) . . . . ? P1 Rh1 C39 C32 -176.0(3) . . . . ? C36 Rh1 C39 C38 -4.0(3) . . . . ? C35 Rh1 C39 C38 -42.2(3) . . . . ? C32 Rh1 C39 C38 -120.3(4) . . . . ? Cl1 Rh1 C39 C38 151.7(3) . . . . ? P1 Rh1 C39 C38 63.7(6) . . . . ? C19 P2 C40 C42 -167.2(3) . . . . ? C44 P2 C40 C42 85.6(3) . . . . ? Rh2 P2 C40 C42 -38.6(4) . . . . ? C19 P2 C40 C41 63.7(4) . . . . ? C44 P2 C40 C41 -43.6(4) . . . . ? Rh2 P2 C40 C41 -167.8(3) . . . . ? C19 P2 C44 C45 72.8(4) . . . . ? C40 P2 C44 C45 176.8(4) . . . . ? Rh2 P2 C44 C45 -48.9(4) . . . . ? C19 P2 C44 C46 -163.6(4) . . . . ? C40 P2 C44 C46 -59.6(5) . . . . ? Rh2 P2 C44 C46 74.6(4) . . . . ? C53 Rh2 C48 C49 -99.2(5) . . . . ? C52 Rh2 C48 C49 -65.8(5) . . . . ? Cl2 Rh2 C48 C49 90.2(4) . . . . ? P2 Rh2 C48 C49 -178.8(5) . . . . ? C53 Rh2 C48 C55 24.9(5) . . . . ? C52 Rh2 C48 C55 58.4(5) . . . . ? C49 Rh2 C48 C55 124.2(6) . . . . ? Cl2 Rh2 C48 C55 -145.7(4) . . . . ? P2 Rh2 C48 C55 -54.6(10) . . . . ? C55 C48 C49 C50 7.0(12) . . . . ? Rh2 C48 C49 C50 106.4(5) . . . . ? C55 C48 C49 Rh2 -99.3(9) . . . . ? C53 Rh2 C49 C48 76.6(6) . . . . ? C52 Rh2 C49 C48 112.3(6) . . . . ? Cl2 Rh2 C49 C48 -88.9(5) . . . . ? P2 Rh2 C49 C48 178.8(5) . . . . ? C53 Rh2 C49 C50 -39.9(6) . . . . ? C52 Rh2 C49 C50 -4.2(5) . . . . ? C48 Rh2 C49 C50 -116.5(8) . . . . ? Cl2 Rh2 C49 C50 154.6(5) . . . . ? P2 Rh2 C49 C50 62.3(8) . . . . ? C48 C49 C50 C51 -96.6(8) . . . . ? Rh2 C49 C50 C51 -15.8(7) . . . . ? C49 C50 C51 C52 36.0(9) . . . . ? C50 C51 C52 C53 42.0(10) . . . . ? C50 C51 C52 Rh2 -39.5(8) . . . . ? C48 Rh2 C52 C53 -66.2(6) . . . . ? C49 Rh2 C52 C53 -100.3(5) . . . . ? Cl2 Rh2 C52 C53 -162.5(5) . . . . ? P2 Rh2 C52 C53 96.5(5) . . . . ? C53 Rh2 C52 C51 122.8(9) . . . . ? C48 Rh2 C52 C51 56.6(7) . . . . ? C49 Rh2 C52 C51 22.5(6) . . . . ? Cl2 Rh2 C52 C51 -39.7(10) . . . . ? P2 Rh2 C52 C51 -140.7(6) . . . . ? C51 C52 C53 C54 3.9(15) . . . . ? Rh2 C52 C53 C54 105.8(12) . . . . ? C51 C52 C53 Rh2 -101.8(7) . . . . ? C48 Rh2 C53 C52 112.1(5) . . . . ? C49 Rh2 C53 C52 75.5(5) . . . . ? Cl2 Rh2 C53 C52 151.5(6) . . . . ? P2 Rh2 C53 C52 -86.5(5) . . . . ? C52 Rh2 C53 C54 -120.7(7) . . . . ? C48 Rh2 C53 C54 -8.6(6) . . . . ? C49 Rh2 C53 C54 -45.2(6) . . . . ? Cl2 Rh2 C53 C54 30.8(10) . . . . ? P2 Rh2 C53 C54 152.8(5) . . . . ? C52 C53 C54 C55 -94.3(12) . . . . ? Rh2 C53 C54 C55 -11.1(10) . . . . ? C53 C54 C55 C48 33.3(11) . . . . ? C49 C48 C55 C54 42.5(12) . . . . ? Rh2 C48 C55 C54 -38.4(8) . . . . ? _diffrn_measured_fraction_theta_max 0.880 _diffrn_reflns_theta_full 36.03 _diffrn_measured_fraction_theta_full 0.880 _refine_diff_density_max 2.282 _refine_diff_density_min -2.311 _refine_diff_density_rms 0.170 #===END data_cj-i16_0m _database_code_depnum_ccdc_archive 'CCDC 286682' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66.67 H69.67 Cl13 O2 P2 Rh2' _chemical_formula_weight 1631.48 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' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0174(19) _cell_length_b 14.210(2) _cell_length_c 19.617(3) _cell_angle_alpha 100.226(3) _cell_angle_beta 109.755(3) _cell_angle_gamma 101.837(3) _cell_volume 3467.6(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7976 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 38.07 _exptl_crystal_description Block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1653 _exptl_absorpt_coefficient_mu 1.066 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5817 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60660 _diffrn_reflns_av_R_equivalents 0.0418 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 38.25 _reflns_number_total 33678 _reflns_number_gt 20725 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The measured crystal contains disordered chloroform molecules. ; _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^)+(0.0819P)^2^+22.0001P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 33678 _refine_ls_number_parameters 874 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1396 _refine_ls_R_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.2369 _refine_ls_wR_factor_gt 0.1884 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.019 _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 0.93624(2) 0.21264(2) 0.298377(14) 0.01791(5) Uani 1 1 d . . . P1 P 0.76958(8) 0.11447(7) 0.21883(6) 0.02215(18) Uani 1 1 d . . . Cl1 Cl 0.98400(10) 0.20562(10) 0.19292(6) 0.0359(2) Uani 1 1 d . . . C1 C 0.7413(3) 0.4006(2) 0.19793(18) 0.0169(5) Uani 1 1 d . . . O1 O 0.7081(2) 0.29734(19) 0.19617(14) 0.0192(4) Uani 1 1 d . . . Rh2 Rh 0.46281(2) 0.46386(2) 0.232777(14) 0.01895(6) Uani 1 1 d . . . P2 P 0.61497(7) 0.54508(7) 0.33728(5) 0.01692(15) Uani 1 1 d . . . Cl2 Cl 0.49330(8) 0.60376(8) 0.18459(5) 0.0293(2) Uani 1 1 d . . . C2 C 0.6548(3) 0.4224(3) 0.13562(19) 0.0183(5) Uani 1 1 d . . . H2A H 0.6799 0.4927 0.1354 0.022 Uiso 1 1 calc R . . H2B H 0.5917 0.4160 0.1485 0.022 Uiso 1 1 calc R . . O2 O 0.7398(2) 0.44911(19) 0.26884(14) 0.0179(4) Uani 1 1 d . . . C3 C 0.6204(3) 0.3560(3) 0.05556(19) 0.0198(6) Uani 1 1 d . . . C4 C 0.6336(3) 0.2525(3) 0.05881(18) 0.0194(6) Uani 1 1 d . . . C5 C 0.6017(3) 0.1771(3) -0.00757(19) 0.0227(6) Uani 1 1 d . . . H5A H 0.5686 0.1907 -0.0542 0.027 Uiso 1 1 calc R . . C6 C 0.6163(3) 0.0824(3) -0.0083(2) 0.0249(7) Uani 1 1 d . . . C7 C 0.6669(3) 0.0650(3) 0.0616(2) 0.0251(7) Uani 1 1 d . . . H7A H 0.6788 0.0018 0.0629 0.030 Uiso 1 1 calc R . . C8 C 0.6999(3) 0.1379(3) 0.12898(19) 0.0199(6) Uani 1 1 d . . . C9 C 0.6809(3) 0.2309(2) 0.12737(18) 0.0178(5) Uani 1 1 d . . . C10 C 0.6851(4) 0.4007(3) 0.0131(2) 0.0287(8) Uani 1 1 d . . . H10A H 0.7590 0.4014 0.0374 0.043 Uiso 1 1 calc R . . H10B H 0.6816 0.4691 0.0140 0.043 Uiso 1 1 calc R . . H10C H 0.6559 0.3601 -0.0391 0.043 Uiso 1 1 calc R . . C11 C 0.5033(3) 0.3485(4) 0.0119(2) 0.0287(8) Uani 1 1 d . . . H11A H 0.4822 0.3145 -0.0412 0.043 Uiso 1 1 calc R . . H11B H 0.4945 0.4157 0.0163 0.043 Uiso 1 1 calc R . . H11C H 0.4589 0.3105 0.0328 0.043 Uiso 1 1 calc R . . C12 C 0.5834(4) 0.0032(4) -0.0801(2) 0.0352(10) Uani 1 1 d . . . H12A H 0.5378 -0.0580 -0.0785 0.053 Uiso 1 1 calc R . . H12B H 0.6463 -0.0103 -0.0861 0.053 Uiso 1 1 calc R . . H12C H 0.5445 0.0261 -0.1226 0.053 Uiso 1 1 calc R . . C13 C 0.8552(3) 0.4255(3) 0.2040(2) 0.0220(6) Uani 1 1 d . . . H13A H 0.8555 0.3952 0.1546 0.026 Uiso 1 1 calc R . . H13B H 0.8948 0.3936 0.2407 0.026 Uiso 1 1 calc R . . C14 C 0.9150(3) 0.5378(3) 0.2279(3) 0.0268(7) Uani 1 1 d . . . C15 C 0.8680(3) 0.5982(3) 0.2733(2) 0.0188(6) Uani 1 1 d . . . C16 C 0.9062(3) 0.7022(3) 0.2980(2) 0.0194(6) Uani 1 1 d . . . H16A H 0.9640 0.7343 0.2874 0.023 Uiso 1 1 calc R . . C17 C 0.8631(3) 0.7611(2) 0.33758(19) 0.0177(5) Uani 1 1 d . . . C18 C 0.7771(3) 0.7125(3) 0.35151(18) 0.0173(5) Uani 1 1 d . . . H18A H 0.7459 0.7509 0.3778 0.021 Uiso 1 1 calc R . . C19 C 0.7361(2) 0.6090(2) 0.32770(17) 0.0158(5) Uani 1 1 d . . . C20 C 0.7817(3) 0.5520(3) 0.28933(18) 0.0175(5) Uani 1 1 d . . . C21 C 0.9099(5) 0.5775(3) 0.1579(3) 0.0436(12) Uani 1 1 d . . . H21A H 0.9571 0.6456 0.1745 0.065 Uiso 1 1 calc R . . H21B H 0.8372 0.5776 0.1301 0.065 Uiso 1 1 calc R . . H21C H 0.9322 0.5342 0.1253 0.065 Uiso 1 1 calc R . . C22 C 1.0312(4) 0.5509(4) 0.2773(5) 0.059(2) Uani 1 1 d . . . H22A H 1.0362 0.5416 0.3265 0.089 Uiso 1 1 calc R . . H22B H 1.0741 0.6182 0.2837 0.089 Uiso 1 1 calc R . . H22C H 1.0572 0.5014 0.2530 0.089 Uiso 1 1 calc R . . C23 C 0.9049(3) 0.8735(3) 0.3600(2) 0.0227(6) Uani 1 1 d . . . H23A H 0.8628 0.9026 0.3840 0.034 Uiso 1 1 calc R . . H23B H 0.9002 0.8968 0.3152 0.034 Uiso 1 1 calc R . . H23C H 0.9789 0.8940 0.3954 0.034 Uiso 1 1 calc R . . C24 C 0.7675(4) -0.0155(3) 0.1937(3) 0.0367(11) Uani 1 1 d . . . C25 C 0.8265(5) -0.0559(4) 0.1584(3) 0.0470(15) Uani 1 1 d . . . H25A H 0.8770 -0.0151 0.1457 0.056 Uiso 1 1 calc R . . C26 C 0.8078(6) -0.1612(4) 0.1422(4) 0.069(2) Uani 1 1 d . . . H26A H 0.8455 -0.1920 0.1174 0.083 Uiso 1 1 calc R . . C27 C 0.7351(6) -0.2194(4) 0.1624(5) 0.083(3) Uani 1 1 d . . . H27A H 0.7246 -0.2895 0.1514 0.100 Uiso 1 1 calc R . . C28 C 0.6786(5) -0.1795(4) 0.1972(5) 0.076(3) Uani 1 1 d . . . H28A H 0.6290 -0.2214 0.2099 0.091 Uiso 1 1 calc R . . C29 C 0.6934(4) -0.0761(4) 0.2144(3) 0.0519(17) Uani 1 1 d . . . C30 C 0.6391(4) -0.0201(4) 0.2509(3) 0.0502(16) Uani 1 1 d . . . C31 C 0.5623(5) -0.0570(6) 0.2790(5) 0.082(3) Uani 1 1 d . . . H31A H 0.5438 -0.1256 0.2778 0.099 Uiso 1 1 calc R . . C32 C 0.5142(5) 0.0059(7) 0.3082(5) 0.080(3) Uani 1 1 d . . . H32A H 0.4627 -0.0201 0.3266 0.095 Uiso 1 1 calc R . . C33 C 0.5403(4) 0.1068(6) 0.3110(4) 0.0569(18) Uani 1 1 d . . . H33A H 0.5066 0.1496 0.3307 0.068 Uiso 1 1 calc R . . C34 C 0.6181(3) 0.1450(4) 0.2839(3) 0.0341(10) Uani 1 1 d . . . H34A H 0.6367 0.2138 0.2855 0.041 Uiso 1 1 calc R . . C35 C 0.6666(3) 0.0825(3) 0.2553(2) 0.0312(9) Uani 1 1 d . . . C36 C 0.6578(2) 0.4868(3) 0.41396(18) 0.0176(5) Uani 1 1 d . . . C37 C 0.6955(3) 0.4029(3) 0.4134(2) 0.0214(6) Uani 1 1 d . . . H37A H 0.7075 0.3723 0.3711 0.026 Uiso 1 1 calc R . . C38 C 0.7151(3) 0.3652(3) 0.4763(2) 0.0246(7) Uani 1 1 d . . . H38A H 0.7410 0.3085 0.4769 0.029 Uiso 1 1 calc R . . C39 C 0.6970(3) 0.4102(3) 0.5384(2) 0.0271(8) Uani 1 1 d . . . H39A H 0.7096 0.3830 0.5804 0.033 Uiso 1 1 calc R . . C40 C 0.6606(3) 0.4943(3) 0.5393(2) 0.0244(7) Uani 1 1 d . . . H40A H 0.6489 0.5247 0.5819 0.029 Uiso 1 1 calc R . . C41 C 0.6414(3) 0.5340(3) 0.47700(18) 0.0191(6) Uani 1 1 d . . . C42 C 0.6047(3) 0.6227(3) 0.46826(19) 0.0193(6) Uani 1 1 d . . . C43 C 0.5857(3) 0.6880(3) 0.5216(2) 0.0269(7) Uani 1 1 d . . . H43A H 0.5968 0.6774 0.5698 0.032 Uiso 1 1 calc R . . C44 C 0.5507(4) 0.7679(4) 0.5031(3) 0.0325(9) Uani 1 1 d . . . H44A H 0.5384 0.8125 0.5393 0.039 Uiso 1 1 calc R . . C45 C 0.5332(4) 0.7842(4) 0.4327(3) 0.0301(8) Uani 1 1 d . . . H45A H 0.5094 0.8397 0.4213 0.036 Uiso 1 1 calc R . . C46 C 0.5501(3) 0.7196(3) 0.3786(2) 0.0238(6) Uani 1 1 d . . . H46A H 0.5364 0.7296 0.3300 0.029 Uiso 1 1 calc R . . C47 C 0.5878(3) 0.6399(3) 0.39696(19) 0.0186(6) Uani 1 1 d . . . C48 C 0.9151(3) 0.1687(3) 0.3908(2) 0.0277(8) Uani 1 1 d . . . H48A H 0.8520 0.1103 0.3767 0.033 Uiso 1 1 calc R . . C49 C 0.8909(3) 0.2606(3) 0.3887(2) 0.0300(8) Uani 1 1 d . . . H49A H 0.8136 0.2542 0.3725 0.036 Uiso 1 1 calc R . . C50 C 0.9603(4) 0.3615(5) 0.4385(4) 0.0582(18) Uani 1 1 d . . . H50A H 0.9236 0.4118 0.4237 0.070 Uiso 1 1 calc R . . H50B H 0.9682 0.3630 0.4908 0.070 Uiso 1 1 calc R . . C51 C 1.0658(5) 0.3919(7) 0.4376(4) 0.076(3) Uani 1 1 d . . . H51A H 1.1175 0.3867 0.4848 0.091 Uiso 1 1 calc R . . H51B H 1.0822 0.4631 0.4377 0.091 Uiso 1 1 calc R . . C52 C 1.0828(3) 0.3333(4) 0.3721(2) 0.0355(11) Uani 1 1 d . . . H52A H 1.1160 0.3748 0.3454 0.043 Uiso 1 1 calc R . . C53 C 1.1043(3) 0.2429(5) 0.3713(3) 0.0350(10) Uani 1 1 d . . . H53A H 1.1502 0.2294 0.3435 0.042 Uiso 1 1 calc R . . C54 C 1.1089(5) 0.1879(8) 0.4307(4) 0.093(3) Uani 1 1 d . . . H54A H 1.1271 0.1259 0.4154 0.111 Uiso 1 1 calc R . . H54B H 1.1681 0.2295 0.4779 0.111 Uiso 1 1 calc R . . C55 C 1.0159(4) 0.1607(5) 0.4475(3) 0.0515(17) Uani 1 1 d . . . H55A H 1.0296 0.2039 0.4973 0.062 Uiso 1 1 calc R . . H55B H 1.0044 0.0910 0.4513 0.062 Uiso 1 1 calc R . . C56 C 0.4076(3) 0.3623(3) 0.2884(2) 0.0233(7) Uani 1 1 d . . . H56A H 0.4469 0.3828 0.3442 0.028 Uiso 1 1 calc R . . C57 C 0.4624(3) 0.3206(3) 0.2481(2) 0.0210(6) Uani 1 1 d . . . H57A H 0.5330 0.3168 0.2810 0.025 Uiso 1 1 calc R . . C58 C 0.4122(3) 0.2423(3) 0.1732(2) 0.0276(7) Uani 1 1 d . . . H58A H 0.3895 0.1762 0.1817 0.033 Uiso 1 1 calc R . . H58B H 0.4659 0.2401 0.1511 0.033 Uiso 1 1 calc R . . C59 C 0.3162(3) 0.2619(4) 0.1169(2) 0.0319(9) Uani 1 1 d . . . H59A H 0.3068 0.2295 0.0651 0.038 Uiso 1 1 calc R . . H59B H 0.2517 0.2316 0.1245 0.038 Uiso 1 1 calc R . . C60 C 0.3290(3) 0.3723(4) 0.1255(2) 0.0281(8) Uani 1 1 d . . . H60A H 0.3312 0.3942 0.0802 0.034 Uiso 1 1 calc R . . C61 C 0.2920(3) 0.4308(3) 0.1684(3) 0.0282(8) Uani 1 1 d . . . H61A H 0.2709 0.4864 0.1479 0.034 Uiso 1 1 calc R . . C62 C 0.2364(3) 0.3974(4) 0.2182(3) 0.0363(10) Uani 1 1 d . . . H62A H 0.1615 0.3609 0.1864 0.044 Uiso 1 1 calc R . . H62B H 0.2376 0.4571 0.2537 0.044 Uiso 1 1 calc R . . C63 C 0.2873(3) 0.3301(4) 0.2631(2) 0.0304(8) Uani 1 1 d . . . H63A H 0.2690 0.3329 0.3078 0.037 Uiso 1 1 calc R . . H63B H 0.2586 0.2602 0.2316 0.037 Uiso 1 1 calc R . . C1LA C 1.2616(5) -0.0931(5) 0.5062(4) 0.0267(12) Uani 0.660(8) 1 d P A 1 H1LA H 1.2824 -0.1142 0.5539 0.032 Uiso 0.660(8) 1 d PR A 1 Cl3A Cl 1.2217(2) 0.0152(2) 0.51693(19) 0.0386(6) Uani 0.660(8) 1 d P A 1 C1L' C 1.2489(10) -0.0614(11) 0.4597(8) 0.030(3) Uani 0.340(8) 1 d P A 2 H1LE H 1.2291 -0.0379 0.4131 0.036 Uiso 0.340(8) 1 d PR A 2 Cl3' Cl 1.2359(7) 0.0022(6) 0.5395(4) 0.0544(18) Uani 0.340(8) 1 d P A 2 Cl1A Cl 1.15659(12) -0.19124(11) 0.43559(9) 0.0488(3) Uani 1 1 d . . . Cl2A Cl 1.37334(11) -0.07171(15) 0.48002(10) 0.0558(4) Uani 1 1 d . . . C1LX C 0.9877(11) 0.2648(10) 0.0285(7) 0.046(3) Uani 0.50 1 d P B 1 H1LC H 1.0233 0.2507 0.0776 0.055 Uiso 0.50 1 calc PR B 1 Cl1X Cl 0.8564(2) 0.2135(3) 0.0003(2) 0.0548(8) Uani 0.50 1 d P B 1 Cl2X Cl 1.0223(3) 0.3973(3) 0.0437(2) 0.0579(8) Uani 0.50 1 d P B 1 Cl3X Cl 1.0417(4) 0.2170(4) -0.0340(4) 0.0884(14) Uani 0.50 1 d P B 1 C1LY C 0.9980(10) 0.1058(11) 0.0307(8) 0.052(3) Uani 0.50 1 d P . 2 H1LD H 1.0266 0.1223 0.0846 0.062 Uiso 0.50 1 d PR . 2 Cl1Y Cl 1.0090(4) 0.2161(4) 0.0056(2) 0.0731(11) Uani 0.50 1 d P C 2 Cl2Y Cl 1.0721(3) 0.0365(3) -0.0013(2) 0.0611(8) Uani 0.50 1 d P . 2 Cl3Y Cl 0.8644(3) 0.0317(5) -0.0029(3) 0.0848(16) Uani 0.50 1 d P . 2 C1D C 0.7334(10) 0.2970(9) -0.1754(9) 0.077(3) Uani 0.67 1 d P . . H1DA H 0.6796 0.3328 -0.1732 0.092 Uiso 0.67 1 calc PR . . Cl1D Cl 0.8497(2) 0.3730(2) -0.1228(3) 0.0815(10) Uani 0.67 1 d P . . Cl2D Cl 0.7036(3) 0.1868(2) -0.1468(3) 0.0960(12) Uani 0.67 1 d P . . Cl3D Cl 0.7163(3) 0.2568(4) -0.2762(3) 0.1026(14) Uani 0.67 1 d P . . C1LF C 0.1523(8) 0.0389(8) 0.2541(5) 0.53(3) Uani 1 1 d D D 1 H1LB H 0.1046 0.0830 0.2504 0.631 Uiso 1 1 calc R D 1 Cl1F Cl 0.2701(2) 0.0933(3) 0.33585(17) 0.0540(8) Uani 0.560(5) 1 d PD D 1 Cl2F Cl 0.1859(3) 0.0233(2) 0.17512(18) 0.0619(9) Uani 0.560(5) 1 d PD D 1 Cl3F Cl 0.0884(3) -0.0787(4) 0.2580(3) 0.0948(17) Uani 0.560(5) 1 d PD D 1 Cl1T Cl 0.1970(12) 0.0287(14) 0.3279(10) 0.213(7) Uani 0.440(5) 1 d P D 2 Cl2T Cl 0.2698(14) 0.0560(16) 0.2727(19) 0.306(15) Uani 0.440(5) 1 d P D 2 Cl3T Cl 0.112(2) -0.073(2) 0.2032(16) 0.404(18) Uani 0.440(5) 1 d P D 2 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 0.01675(10) 0.01382(10) 0.01634(9) 0.00222(8) 0.00190(8) -0.00044(9) P1 0.0214(4) 0.0120(4) 0.0213(4) 0.0051(3) -0.0024(3) -0.0016(3) Cl1 0.0402(5) 0.0356(6) 0.0212(4) 0.0015(4) 0.0120(4) -0.0064(5) C1 0.0183(12) 0.0110(12) 0.0164(11) 0.0032(10) 0.0035(10) -0.0001(10) O1 0.0255(11) 0.0116(10) 0.0149(9) 0.0039(8) 0.0035(8) 0.0009(9) Rh2 0.01447(10) 0.02034(12) 0.01521(9) 0.00444(9) 0.00270(7) -0.00367(9) P2 0.0152(3) 0.0167(4) 0.0148(3) 0.0043(3) 0.0042(3) -0.0012(3) Cl2 0.0248(4) 0.0322(5) 0.0225(3) 0.0142(4) 0.0029(3) -0.0046(4) C2 0.0200(13) 0.0165(13) 0.0179(12) 0.0053(10) 0.0066(10) 0.0048(11) O2 0.0196(10) 0.0108(9) 0.0172(9) 0.0010(8) 0.0047(8) -0.0018(8) C3 0.0231(14) 0.0180(14) 0.0177(12) 0.0060(11) 0.0060(11) 0.0066(12) C4 0.0217(13) 0.0174(14) 0.0149(11) 0.0038(10) 0.0028(10) 0.0044(12) C5 0.0219(14) 0.0231(16) 0.0154(12) 0.0020(11) 0.0007(11) 0.0047(13) C6 0.0246(15) 0.0208(16) 0.0174(13) -0.0022(12) -0.0009(11) 0.0036(14) C7 0.0244(15) 0.0157(15) 0.0228(14) 0.0002(12) -0.0019(12) 0.0030(13) C8 0.0215(13) 0.0105(12) 0.0180(12) 0.0014(10) -0.0004(11) 0.0006(11) C9 0.0195(12) 0.0116(12) 0.0145(11) 0.0029(10) 0.0013(10) -0.0022(11) C10 0.039(2) 0.0277(18) 0.0239(15) 0.0118(14) 0.0151(15) 0.0098(17) C11 0.0289(17) 0.033(2) 0.0213(14) 0.0080(14) 0.0032(13) 0.0134(16) C12 0.036(2) 0.026(2) 0.0217(15) -0.0082(14) -0.0067(15) 0.0052(18) C13 0.0197(13) 0.0159(14) 0.0275(15) 0.0018(12) 0.0080(12) 0.0041(12) C14 0.0205(14) 0.0140(14) 0.044(2) -0.0006(15) 0.0168(15) 0.0007(13) C15 0.0160(12) 0.0136(13) 0.0234(13) 0.0025(11) 0.0070(11) 0.0001(11) C16 0.0157(12) 0.0160(14) 0.0223(13) 0.0018(11) 0.0072(10) -0.0012(11) C17 0.0155(11) 0.0109(12) 0.0199(12) 0.0000(10) 0.0042(10) -0.0022(10) C18 0.0178(12) 0.0137(12) 0.0156(11) 0.0009(10) 0.0052(10) -0.0008(11) C19 0.0153(11) 0.0145(12) 0.0136(10) 0.0014(9) 0.0046(9) -0.0005(10) C20 0.0171(12) 0.0124(12) 0.0158(11) 0.0010(10) 0.0022(10) -0.0015(11) C21 0.066(3) 0.0184(17) 0.063(3) 0.0039(19) 0.053(3) 0.003(2) C22 0.0150(16) 0.026(2) 0.109(5) -0.020(3) 0.013(2) -0.0002(18) C23 0.0210(14) 0.0158(14) 0.0253(14) 0.0003(12) 0.0080(12) -0.0010(12) C24 0.036(2) 0.0116(14) 0.035(2) 0.0047(14) -0.0157(17) 0.0009(15) C25 0.055(3) 0.0210(19) 0.038(2) 0.0000(17) -0.015(2) 0.018(2) C26 0.075(4) 0.023(2) 0.060(4) -0.010(2) -0.031(3) 0.025(3) C27 0.070(4) 0.0129(19) 0.091(5) 0.010(3) -0.052(4) 0.000(2) C28 0.047(3) 0.017(2) 0.098(5) 0.028(3) -0.044(3) -0.013(2) C29 0.035(2) 0.0197(19) 0.059(3) 0.023(2) -0.027(2) -0.0131(17) C30 0.0262(18) 0.036(2) 0.060(3) 0.037(2) -0.0164(19) -0.0134(18) C31 0.031(2) 0.080(4) 0.111(5) 0.084(4) -0.010(3) -0.019(3) C32 0.028(2) 0.115(6) 0.097(5) 0.088(5) 0.010(3) -0.004(3) C33 0.027(2) 0.089(5) 0.052(3) 0.048(3) 0.009(2) -0.003(3) C34 0.0216(15) 0.044(3) 0.0287(17) 0.0211(19) 0.0026(13) -0.0049(17) C35 0.0210(15) 0.0282(19) 0.0288(17) 0.0190(16) -0.0059(13) -0.0085(14) C36 0.0134(11) 0.0171(13) 0.0149(11) 0.0026(10) 0.0020(9) -0.0038(11) C37 0.0171(12) 0.0208(15) 0.0200(13) 0.0045(12) 0.0034(11) -0.0003(12) C38 0.0221(14) 0.0244(17) 0.0229(14) 0.0111(13) 0.0039(12) 0.0023(13) C39 0.0239(15) 0.0293(19) 0.0231(15) 0.0115(15) 0.0050(12) 0.0004(15) C40 0.0231(14) 0.0296(19) 0.0169(12) 0.0074(13) 0.0075(11) -0.0007(14) C41 0.0170(12) 0.0195(14) 0.0155(11) 0.0053(11) 0.0047(10) -0.0035(11) C42 0.0184(12) 0.0218(15) 0.0172(11) 0.0048(11) 0.0091(10) 0.0010(12) C43 0.0288(16) 0.031(2) 0.0222(14) 0.0063(14) 0.0143(13) 0.0049(16) C44 0.038(2) 0.036(2) 0.0341(19) 0.0086(17) 0.0240(17) 0.0154(19) C45 0.0343(19) 0.0291(19) 0.0355(19) 0.0091(16) 0.0213(16) 0.0134(17) C46 0.0265(15) 0.0232(16) 0.0248(14) 0.0088(13) 0.0124(13) 0.0071(14) C47 0.0160(12) 0.0188(14) 0.0177(12) 0.0046(11) 0.0059(10) -0.0004(11) C48 0.0230(15) 0.0289(19) 0.0175(13) 0.0072(14) -0.0002(12) -0.0082(14) C49 0.0175(14) 0.0260(19) 0.0330(18) -0.0123(15) 0.0127(13) -0.0093(14) C50 0.031(2) 0.036(3) 0.080(4) -0.036(3) 0.034(3) -0.021(2) C51 0.046(3) 0.072(5) 0.072(4) -0.045(4) 0.040(3) -0.038(3) C52 0.0183(15) 0.045(3) 0.0255(16) -0.0054(18) 0.0084(13) -0.0145(17) C53 0.0178(14) 0.062(3) 0.0285(17) 0.016(2) 0.0089(13) 0.0140(18) C54 0.044(3) 0.216(8) 0.082(4) 0.111(5) 0.043(3) 0.077(4) C55 0.029(2) 0.055(3) 0.041(2) 0.031(3) -0.0138(18) -0.019(2) C56 0.0232(14) 0.0204(15) 0.0188(12) 0.0048(12) 0.0073(11) -0.0072(13) C57 0.0225(14) 0.0178(14) 0.0183(12) 0.0030(11) 0.0077(11) -0.0013(12) C58 0.0280(17) 0.0242(18) 0.0230(15) -0.0013(14) 0.0084(13) 0.0008(15) C59 0.0271(17) 0.032(2) 0.0192(14) -0.0023(15) 0.0018(13) -0.0080(17) C60 0.0221(15) 0.036(2) 0.0163(13) 0.0095(14) 0.0019(11) -0.0046(15) C61 0.0161(13) 0.0282(19) 0.0321(18) 0.0085(16) 0.0029(13) 0.0001(14) C62 0.0187(15) 0.044(3) 0.043(2) 0.010(2) 0.0120(16) 0.0020(18) C63 0.0229(15) 0.033(2) 0.0274(16) 0.0036(16) 0.0109(13) -0.0077(16) C1LA 0.028(3) 0.024(3) 0.026(2) 0.006(2) 0.007(2) 0.009(2) Cl3A 0.0378(9) 0.0263(9) 0.0542(15) 0.0046(9) 0.0216(10) 0.0133(7) C1L' 0.024(5) 0.030(6) 0.032(5) -0.001(5) 0.008(4) 0.013(5) Cl3' 0.068(3) 0.043(3) 0.057(3) -0.003(2) 0.047(3) 0.002(3) Cl1A 0.0414(6) 0.0311(6) 0.0524(7) -0.0002(6) -0.0005(6) 0.0081(5) Cl2A 0.0351(6) 0.0642(10) 0.0648(9) -0.0014(8) 0.0214(6) 0.0198(7) C1LX 0.069(7) 0.042(6) 0.035(4) 0.007(4) 0.026(5) 0.023(6) Cl1X 0.0365(12) 0.071(2) 0.0531(16) 0.0200(16) 0.0165(11) 0.0066(14) Cl2X 0.0584(18) 0.0399(16) 0.0608(18) 0.0022(14) 0.0121(15) 0.0125(15) Cl3X 0.094(3) 0.064(3) 0.133(4) 0.009(3) 0.086(3) 0.020(2) C1LY 0.042(5) 0.060(8) 0.050(6) 0.005(6) 0.013(5) 0.021(6) Cl1Y 0.097(3) 0.070(3) 0.0479(17) 0.0078(19) 0.024(2) 0.031(3) Cl2Y 0.0559(17) 0.061(2) 0.067(2) 0.0063(17) 0.0298(16) 0.0167(17) Cl3Y 0.0378(15) 0.124(5) 0.070(2) -0.004(3) 0.0218(16) 0.001(2) C1D 0.099(7) 0.076(6) 0.130(9) 0.062(6) 0.091(7) 0.069(6) Cl1D 0.0516(13) 0.0609(16) 0.154(3) 0.049(2) 0.0553(17) 0.0176(13) Cl2D 0.122(2) 0.0430(14) 0.171(3) 0.0323(19) 0.113(3) 0.0233(16) Cl3D 0.074(2) 0.131(4) 0.112(3) 0.047(3) 0.037(2) 0.036(3) C1LF 0.48(3) 0.74(7) 0.17(2) -0.12(3) -0.17(2) 0.51(4) Cl1F 0.0375(12) 0.0552(18) 0.0488(14) -0.0065(12) 0.0050(10) 0.0082(12) Cl2F 0.094(2) 0.0424(15) 0.0495(14) 0.0108(13) 0.0377(16) 0.0048(16) Cl3F 0.068(2) 0.100(3) 0.099(3) 0.040(3) 0.034(2) -0.029(2) Cl1T 0.159(11) 0.193(16) 0.198(14) 0.043(14) -0.020(10) 0.026(11) Cl2T 0.141(11) 0.181(18) 0.52(5) -0.01(2) 0.12(2) -0.011(12) Cl3T 0.34(2) 0.45(4) 0.39(3) -0.14(3) 0.21(2) 0.13(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 C48 2.111(4) . ? Rh1 C49 2.126(4) . ? Rh1 C53 2.207(4) . ? Rh1 C52 2.218(4) . ? Rh1 P1 2.2945(10) . ? Rh1 Cl1 2.3724(11) . ? P1 C24 1.817(4) . ? P1 C35 1.829(5) . ? P1 C8 1.830(3) . ? C1 O1 1.436(4) . ? C1 O2 1.447(4) . ? C1 C13 1.521(5) . ? C1 C2 1.532(4) . ? O1 C9 1.382(4) . ? Rh2 C57 2.110(4) . ? Rh2 C56 2.131(3) . ? Rh2 C61 2.198(4) . ? Rh2 C60 2.236(4) . ? Rh2 P2 2.2974(9) . ? Rh2 Cl2 2.3707(10) . ? P2 C47 1.812(4) . ? P2 C36 1.829(3) . ? P2 C19 1.840(3) . ? C2 C3 1.538(5) . ? O2 C20 1.387(4) . ? C3 C4 1.530(5) . ? C3 C11 1.544(5) . ? C3 C10 1.544(5) . ? C4 C5 1.400(5) . ? C4 C9 1.403(4) . ? C5 C6 1.399(6) . ? C6 C7 1.407(5) . ? C6 C12 1.500(6) . ? C7 C8 1.391(5) . ? C8 C9 1.405(5) . ? C13 C14 1.546(5) . ? C14 C15 1.524(5) . ? C14 C22 1.539(7) . ? C14 C21 1.560(7) . ? C15 C16 1.396(5) . ? C15 C20 1.412(5) . ? C16 C17 1.402(5) . ? C17 C18 1.398(5) . ? C17 C23 1.510(5) . ? C18 C19 1.393(5) . ? C19 C20 1.398(5) . ? C24 C25 1.391(9) . ? C24 C29 1.423(8) . ? C25 C26 1.422(7) . ? C26 C27 1.386(13) . ? C27 C28 1.351(14) . ? C28 C29 1.403(8) . ? C29 C30 1.464(11) . ? C30 C35 1.409(6) . ? C30 C31 1.418(9) . ? C31 C32 1.381(14) . ? C32 C33 1.392(11) . ? C33 C34 1.421(7) . ? C34 C35 1.376(8) . ? C36 C37 1.399(5) . ? C36 C41 1.411(5) . ? C37 C38 1.398(5) . ? C38 C39 1.398(6) . ? C39 C40 1.392(6) . ? C40 C41 1.404(5) . ? C41 C42 1.472(5) . ? C42 C43 1.403(6) . ? C42 C47 1.411(5) . ? C43 C44 1.384(7) . ? C44 C45 1.390(6) . ? C45 C46 1.392(6) . ? C46 C47 1.397(5) . ? C48 C49 1.418(7) . ? C48 C55 1.515(6) . ? C49 C50 1.499(7) . ? C50 C51 1.461(7) . ? C51 C52 1.519(8) . ? C52 C53 1.377(8) . ? C53 C54 1.506(8) . ? C54 C55 1.445(8) . ? C56 C57 1.414(6) . ? C56 C63 1.529(6) . ? C57 C58 1.513(6) . ? C58 C59 1.539(6) . ? C59 C60 1.513(7) . ? C60 C61 1.376(7) . ? C61 C62 1.521(7) . ? C62 C63 1.535(7) . ? C1LA Cl3A 1.745(7) . ? C1LA Cl1A 1.768(7) . ? C1LA Cl2A 1.793(7) . ? C1L' Cl2A 1.696(12) . ? C1L' Cl3' 1.748(15) . ? C1L' Cl1A 1.897(15) . ? C1LX Cl1X 1.686(15) . ? C1LX Cl3X 1.755(12) . ? C1LX Cl2X 1.788(13) . ? C1LY Cl1Y 1.719(16) . ? C1LY Cl2Y 1.757(13) . ? C1LY Cl3Y 1.777(14) . ? C1LY Cl2Y 1.942(16) 2_755 ? Cl2Y Cl3Y 1.439(7) 2_755 ? Cl2Y C1LY 1.942(16) 2_755 ? Cl2Y Cl2Y 2.096(8) 2_755 ? Cl3Y Cl2Y 1.439(7) 2_755 ? C1D Cl1D 1.624(15) . ? C1D Cl2D 1.773(11) . ? C1D Cl3D 1.877(15) . ? C1LF Cl3F 1.755(9) . ? C1LF Cl2F 1.756(9) . ? C1LF Cl1F 1.772(8) . ? Cl1T Cl2T 1.76(3) . ? Cl1T Cl3T 2.36(3) . ? Cl2T Cl3T 2.35(3) . ? 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 C48 Rh1 C49 39.11(19) . . ? C48 Rh1 C53 81.67(16) . . ? C49 Rh1 C53 94.34(17) . . ? C48 Rh1 C52 92.39(16) . . ? C49 Rh1 C52 81.14(16) . . ? C53 Rh1 C52 36.3(2) . . ? C48 Rh1 P1 91.17(11) . . ? C49 Rh1 P1 94.63(11) . . ? C53 Rh1 P1 155.58(16) . . ? C52 Rh1 P1 168.15(16) . . ? C48 Rh1 Cl1 157.41(14) . . ? C49 Rh1 Cl1 163.28(14) . . ? C53 Rh1 Cl1 89.24(12) . . ? C52 Rh1 Cl1 92.35(12) . . ? P1 Rh1 Cl1 88.67(4) . . ? C24 P1 C35 91.0(2) . . ? C24 P1 C8 104.17(18) . . ? C35 P1 C8 103.86(17) . . ? C24 P1 Rh1 110.83(14) . . ? C35 P1 Rh1 120.25(14) . . ? C8 P1 Rh1 121.55(12) . . ? O1 C1 O2 101.2(2) . . ? O1 C1 C13 108.2(3) . . ? O2 C1 C13 108.5(3) . . ? O1 C1 C2 108.7(3) . . ? O2 C1 C2 107.2(3) . . ? C13 C1 C2 121.2(3) . . ? C9 O1 C1 114.7(2) . . ? C57 Rh2 C56 38.94(15) . . ? C57 Rh2 C61 97.45(16) . . ? C56 Rh2 C61 81.53(15) . . ? C57 Rh2 C60 80.99(15) . . ? C56 Rh2 C60 88.48(14) . . ? C61 Rh2 C60 36.14(18) . . ? C57 Rh2 P2 94.58(10) . . ? C56 Rh2 P2 92.50(10) . . ? C61 Rh2 P2 152.16(13) . . ? C60 Rh2 P2 171.65(13) . . ? C57 Rh2 Cl2 158.29(10) . . ? C56 Rh2 Cl2 162.56(12) . . ? C61 Rh2 Cl2 89.58(12) . . ? C60 Rh2 Cl2 93.16(11) . . ? P2 Rh2 Cl2 88.39(3) . . ? C47 P2 C36 90.77(16) . . ? C47 P2 C19 105.35(16) . . ? C36 P2 C19 106.13(15) . . ? C47 P2 Rh2 108.66(11) . . ? C36 P2 Rh2 120.32(11) . . ? C19 P2 Rh2 120.59(10) . . ? C1 C2 C3 116.4(3) . . ? C20 O2 C1 113.3(3) . . ? C4 C3 C2 109.8(3) . . ? C4 C3 C11 110.5(3) . . ? C2 C3 C11 107.8(3) . . ? C4 C3 C10 108.8(3) . . ? C2 C3 C10 112.1(3) . . ? C11 C3 C10 107.8(3) . . ? C5 C4 C9 118.0(3) . . ? C5 C4 C3 120.3(3) . . ? C9 C4 C3 121.7(3) . . ? C6 C5 C4 122.9(3) . . ? C5 C6 C7 117.2(3) . . ? C5 C6 C12 122.1(3) . . ? C7 C6 C12 120.7(4) . . ? C8 C7 C6 121.8(3) . . ? C7 C8 C9 119.2(3) . . ? C7 C8 P1 120.8(3) . . ? C9 C8 P1 120.0(3) . . ? O1 C9 C4 122.7(3) . . ? O1 C9 C8 116.5(3) . . ? C4 C9 C8 120.8(3) . . ? C1 C13 C14 115.9(3) . . ? C15 C14 C22 109.0(4) . . ? C15 C14 C13 110.7(3) . . ? C22 C14 C13 107.9(4) . . ? C15 C14 C21 108.8(3) . . ? C22 C14 C21 109.4(5) . . ? C13 C14 C21 111.0(4) . . ? C16 C15 C20 117.6(3) . . ? C16 C15 C14 120.8(3) . . ? C20 C15 C14 121.6(3) . . ? C15 C16 C17 122.9(3) . . ? C18 C17 C16 117.7(3) . . ? C18 C17 C23 121.7(3) . . ? C16 C17 C23 120.4(3) . . ? C19 C18 C17 121.3(3) . . ? C18 C19 C20 119.6(3) . . ? C18 C19 P2 121.7(3) . . ? C20 C19 P2 118.4(3) . . ? O2 C20 C19 117.3(3) . . ? O2 C20 C15 121.9(3) . . ? C19 C20 C15 120.8(3) . . ? C25 C24 C29 121.8(5) . . ? C25 C24 P1 127.6(4) . . ? C29 C24 P1 110.6(4) . . ? C24 C25 C26 116.9(7) . . ? C27 C26 C25 120.7(8) . . ? C28 C27 C26 122.0(5) . . ? C27 C28 C29 119.9(7) . . ? C28 C29 C24 118.7(7) . . ? C28 C29 C30 127.6(6) . . ? C24 C29 C30 113.8(4) . . ? C35 C30 C31 118.3(7) . . ? C35 C30 C29 113.5(5) . . ? C31 C30 C29 128.2(6) . . ? C32 C31 C30 120.6(6) . . ? C31 C32 C33 120.8(6) . . ? C32 C33 C34 119.2(8) . . ? C35 C34 C33 120.0(5) . . ? C34 C35 C30 121.1(5) . . ? C34 C35 P1 128.0(3) . . ? C30 C35 P1 110.9(4) . . ? C37 C36 C41 121.2(3) . . ? C37 C36 P2 127.9(3) . . ? C41 C36 P2 110.8(3) . . ? C38 C37 C36 118.6(4) . . ? C37 C38 C39 120.6(4) . . ? C40 C39 C38 120.8(3) . . ? C39 C40 C41 119.5(4) . . ? C40 C41 C36 119.3(4) . . ? C40 C41 C42 127.3(3) . . ? C36 C41 C42 113.5(3) . . ? C43 C42 C47 119.4(3) . . ? C43 C42 C41 127.4(3) . . ? C47 C42 C41 113.2(3) . . ? C44 C43 C42 119.3(4) . . ? C43 C44 C45 121.2(4) . . ? C44 C45 C46 120.4(4) . . ? C45 C46 C47 119.0(4) . . ? C46 C47 C42 120.6(3) . . ? C46 C47 P2 127.8(3) . . ? C42 C47 P2 111.5(3) . . ? C49 C48 C55 123.1(4) . . ? C49 C48 Rh1 71.0(2) . . ? C55 C48 Rh1 113.0(3) . . ? C48 C49 C50 126.0(5) . . ? C48 C49 Rh1 69.9(2) . . ? C50 C49 Rh1 112.1(3) . . ? C51 C50 C49 116.2(5) . . ? C50 C51 C52 116.4(5) . . ? C53 C52 C51 122.1(6) . . ? C53 C52 Rh1 71.4(3) . . ? C51 C52 Rh1 109.9(3) . . ? C52 C53 C54 125.9(6) . . ? C52 C53 Rh1 72.3(2) . . ? C54 C53 Rh1 107.6(3) . . ? C55 C54 C53 118.2(4) . . ? C54 C55 C48 115.3(4) . . ? C57 C56 C63 123.8(4) . . ? C57 C56 Rh2 69.7(2) . . ? C63 C56 Rh2 113.7(3) . . ? C56 C57 C58 125.8(3) . . ? C56 C57 Rh2 71.3(2) . . ? C58 C57 Rh2 110.7(3) . . ? C57 C58 C59 113.2(4) . . ? C60 C59 C58 112.0(3) . . ? C61 C60 C59 125.5(4) . . ? C61 C60 Rh2 70.4(2) . . ? C59 C60 Rh2 111.2(3) . . ? C60 C61 C62 126.1(4) . . ? C60 C61 Rh2 73.4(2) . . ? C62 C61 Rh2 107.1(3) . . ? C61 C62 C63 113.0(4) . . ? C56 C63 C62 111.4(3) . . ? Cl3A C1LA Cl1A 109.6(3) . . ? Cl3A C1LA Cl2A 109.7(4) . . ? Cl1A C1LA Cl2A 109.4(4) . . ? Cl2A C1L' Cl3' 111.3(8) . . ? Cl2A C1L' Cl1A 107.8(7) . . ? Cl3' C1L' Cl1A 103.2(8) . . ? C1LA Cl1A C1L' 33.6(5) . . ? C1L' Cl2A C1LA 35.4(5) . . ? Cl1X C1LX Cl3X 114.1(8) . . ? Cl1X C1LX Cl2X 112.4(7) . . ? Cl3X C1LX Cl2X 107.2(7) . . ? Cl1Y C1LY Cl2Y 111.0(8) . . ? Cl1Y C1LY Cl3Y 112.4(7) . . ? Cl2Y C1LY Cl3Y 109.6(8) . . ? Cl1Y C1LY Cl2Y 147.2(8) . 2_755 ? Cl2Y C1LY Cl2Y 68.8(6) . 2_755 ? Cl3Y C1LY Cl2Y 45.2(4) . 2_755 ? Cl3Y Cl2Y C1LY 154.5(6) 2_755 . ? Cl3Y Cl2Y C1LY 61.3(4) 2_755 2_755 ? C1LY Cl2Y C1LY 111.2(6) . 2_755 ? Cl3Y Cl2Y Cl2Y 108.1(4) 2_755 2_755 ? C1LY Cl2Y Cl2Y 59.8(5) . 2_755 ? C1LY Cl2Y Cl2Y 51.4(4) 2_755 2_755 ? Cl2Y Cl3Y C1LY 73.5(5) 2_755 . ? Cl1D C1D Cl2D 113.8(8) . . ? Cl1D C1D Cl3D 112.1(6) . . ? Cl2D C1D Cl3D 106.9(7) . . ? Cl3F C1LF Cl2F 108.7(6) . . ? Cl3F C1LF Cl1F 109.3(6) . . ? Cl2F C1LF Cl1F 108.6(6) . . ? Cl2T Cl1T Cl3T 67.7(12) . . ? Cl1T Cl2T Cl3T 68.4(10) . . ? Cl2T Cl3T Cl1T 43.9(9) . . ? 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 C48 Rh1 P1 C24 -79.0(2) . . . . ? C49 Rh1 P1 C24 -118.0(2) . . . . ? C53 Rh1 P1 C24 -6.8(4) . . . . ? C52 Rh1 P1 C24 173.6(6) . . . . ? Cl1 Rh1 P1 C24 78.5(2) . . . . ? C48 Rh1 P1 C35 25.2(2) . . . . ? C49 Rh1 P1 C35 -13.8(2) . . . . ? C53 Rh1 P1 C35 97.4(3) . . . . ? C52 Rh1 P1 C35 -82.3(6) . . . . ? Cl1 Rh1 P1 C35 -177.41(17) . . . . ? C48 Rh1 P1 C8 158.3(2) . . . . ? C49 Rh1 P1 C8 119.3(2) . . . . ? C53 Rh1 P1 C8 -129.5(3) . . . . ? C52 Rh1 P1 C8 50.8(6) . . . . ? Cl1 Rh1 P1 C8 -44.29(16) . . . . ? O2 C1 O1 C9 167.4(3) . . . . ? C13 C1 O1 C9 -78.6(3) . . . . ? C2 C1 O1 C9 54.7(4) . . . . ? C57 Rh2 P2 C47 -124.74(15) . . . . ? C56 Rh2 P2 C47 -85.78(17) . . . . ? C61 Rh2 P2 C47 -9.3(3) . . . . ? C60 Rh2 P2 C47 177.6(7) . . . . ? Cl2 Rh2 P2 C47 76.80(12) . . . . ? C57 Rh2 P2 C36 -22.39(17) . . . . ? C56 Rh2 P2 C36 16.58(18) . . . . ? C61 Rh2 P2 C36 93.1(3) . . . . ? C60 Rh2 P2 C36 -80.0(7) . . . . ? Cl2 Rh2 P2 C36 179.15(14) . . . . ? C57 Rh2 P2 C19 113.65(16) . . . . ? C56 Rh2 P2 C19 152.61(18) . . . . ? C61 Rh2 P2 C19 -130.9(3) . . . . ? C60 Rh2 P2 C19 56.0(7) . . . . ? Cl2 Rh2 P2 C19 -44.82(14) . . . . ? O1 C1 C2 C3 -55.0(4) . . . . ? O2 C1 C2 C3 -163.6(3) . . . . ? C13 C1 C2 C3 71.2(4) . . . . ? O1 C1 O2 C20 172.6(3) . . . . ? C13 C1 O2 C20 58.9(3) . . . . ? C2 C1 O2 C20 -73.6(3) . . . . ? C1 C2 C3 C4 30.0(4) . . . . ? C1 C2 C3 C11 150.5(3) . . . . ? C1 C2 C3 C10 -91.1(4) . . . . ? C2 C3 C4 C5 176.4(3) . . . . ? C11 C3 C4 C5 57.6(5) . . . . ? C10 C3 C4 C5 -60.5(4) . . . . ? C2 C3 C4 C9 -5.8(5) . . . . ? C11 C3 C4 C9 -124.6(4) . . . . ? C10 C3 C4 C9 117.3(4) . . . . ? C9 C4 C5 C6 -1.0(6) . . . . ? C3 C4 C5 C6 176.9(4) . . . . ? C4 C5 C6 C7 -0.9(6) . . . . ? C4 C5 C6 C12 -178.8(4) . . . . ? C5 C6 C7 C8 0.9(6) . . . . ? C12 C6 C7 C8 178.8(4) . . . . ? C6 C7 C8 C9 1.0(6) . . . . ? C6 C7 C8 P1 -177.8(3) . . . . ? C24 P1 C8 C7 -4.9(4) . . . . ? C35 P1 C8 C7 -99.5(4) . . . . ? Rh1 P1 C8 C7 121.0(3) . . . . ? C24 P1 C8 C9 176.3(3) . . . . ? C35 P1 C8 C9 81.6(3) . . . . ? Rh1 P1 C8 C9 -57.9(3) . . . . ? C1 O1 C9 C4 -33.3(5) . . . . ? C1 O1 C9 C8 148.7(3) . . . . ? C5 C4 C9 O1 -175.0(3) . . . . ? C3 C4 C9 O1 7.1(5) . . . . ? C5 C4 C9 C8 2.9(5) . . . . ? C3 C4 C9 C8 -175.0(3) . . . . ? C7 C8 C9 O1 175.1(3) . . . . ? P1 C8 C9 O1 -6.0(5) . . . . ? C7 C8 C9 C4 -2.9(6) . . . . ? P1 C8 C9 C4 175.9(3) . . . . ? O1 C1 C13 C14 -164.2(3) . . . . ? O2 C1 C13 C14 -55.1(4) . . . . ? C2 C1 C13 C14 69.4(5) . . . . ? C1 C13 C14 C15 25.5(5) . . . . ? C1 C13 C14 C22 144.7(4) . . . . ? C1 C13 C14 C21 -95.5(4) . . . . ? C22 C14 C15 C16 64.6(5) . . . . ? C13 C14 C15 C16 -176.9(3) . . . . ? C21 C14 C15 C16 -54.7(5) . . . . ? C22 C14 C15 C20 -118.1(4) . . . . ? C13 C14 C15 C20 0.4(5) . . . . ? C21 C14 C15 C20 122.6(4) . . . . ? C20 C15 C16 C17 0.3(5) . . . . ? C14 C15 C16 C17 177.7(3) . . . . ? C15 C16 C17 C18 -1.0(5) . . . . ? C15 C16 C17 C23 -177.5(3) . . . . ? C16 C17 C18 C19 0.7(5) . . . . ? C23 C17 C18 C19 177.2(3) . . . . ? C17 C18 C19 C20 0.3(5) . . . . ? C17 C18 C19 P2 -173.8(2) . . . . ? C47 P2 C19 C18 -11.2(3) . . . . ? C36 P2 C19 C18 -106.6(3) . . . . ? Rh2 P2 C19 C18 112.0(2) . . . . ? C47 P2 C19 C20 174.7(2) . . . . ? C36 P2 C19 C20 79.3(3) . . . . ? Rh2 P2 C19 C20 -62.1(3) . . . . ? C1 O2 C20 C19 145.4(3) . . . . ? C1 O2 C20 C15 -35.5(4) . . . . ? C18 C19 C20 O2 178.2(3) . . . . ? P2 C19 C20 O2 -7.6(4) . . . . ? C18 C19 C20 C15 -1.0(5) . . . . ? P2 C19 C20 C15 173.3(2) . . . . ? C16 C15 C20 O2 -178.4(3) . . . . ? C14 C15 C20 O2 4.2(5) . . . . ? C16 C15 C20 C19 0.7(5) . . . . ? C14 C15 C20 C19 -176.7(3) . . . . ? C35 P1 C24 C25 178.1(4) . . . . ? C8 P1 C24 C25 73.5(4) . . . . ? Rh1 P1 C24 C25 -58.8(4) . . . . ? C35 P1 C24 C29 -1.2(3) . . . . ? C8 P1 C24 C29 -105.8(3) . . . . ? Rh1 P1 C24 C29 121.9(3) . . . . ? C29 C24 C25 C26 1.4(7) . . . . ? P1 C24 C25 C26 -177.8(4) . . . . ? C24 C25 C26 C27 -1.1(8) . . . . ? C25 C26 C27 C28 0.7(9) . . . . ? C26 C27 C28 C29 -0.5(9) . . . . ? C27 C28 C29 C24 0.8(8) . . . . ? C27 C28 C29 C30 179.3(5) . . . . ? C25 C24 C29 C28 -1.3(7) . . . . ? P1 C24 C29 C28 178.0(4) . . . . ? C25 C24 C29 C30 180.0(4) . . . . ? P1 C24 C29 C30 -0.7(5) . . . . ? C28 C29 C30 C35 -175.6(5) . . . . ? C24 C29 C30 C35 3.0(6) . . . . ? C28 C29 C30 C31 2.2(9) . . . . ? C24 C29 C30 C31 -179.2(5) . . . . ? C35 C30 C31 C32 1.5(9) . . . . ? C29 C30 C31 C32 -176.2(6) . . . . ? C30 C31 C32 C33 -0.3(10) . . . . ? C31 C32 C33 C34 -0.5(10) . . . . ? C32 C33 C34 C35 0.0(8) . . . . ? C33 C34 C35 C30 1.2(6) . . . . ? C33 C34 C35 P1 -178.9(4) . . . . ? C31 C30 C35 C34 -2.0(7) . . . . ? C29 C30 C35 C34 176.1(4) . . . . ? C31 C30 C35 P1 178.1(4) . . . . ? C29 C30 C35 P1 -3.8(5) . . . . ? C24 P1 C35 C34 -177.0(4) . . . . ? C8 P1 C35 C34 -72.1(4) . . . . ? Rh1 P1 C35 C34 68.0(4) . . . . ? C24 P1 C35 C30 2.9(3) . . . . ? C8 P1 C35 C30 107.7(3) . . . . ? Rh1 P1 C35 C30 -112.1(3) . . . . ? C47 P2 C36 C37 -179.1(3) . . . . ? C19 P2 C36 C37 -72.8(3) . . . . ? Rh2 P2 C36 C37 68.7(3) . . . . ? C47 P2 C36 C41 5.1(3) . . . . ? C19 P2 C36 C41 111.3(2) . . . . ? Rh2 P2 C36 C41 -107.2(2) . . . . ? C41 C36 C37 C38 1.1(5) . . . . ? P2 C36 C37 C38 -174.3(3) . . . . ? C36 C37 C38 C39 0.3(5) . . . . ? C37 C38 C39 C40 -1.0(6) . . . . ? C38 C39 C40 C41 0.4(6) . . . . ? C39 C40 C41 C36 1.0(5) . . . . ? C39 C40 C41 C42 -179.0(4) . . . . ? C37 C36 C41 C40 -1.8(5) . . . . ? P2 C36 C41 C40 174.4(3) . . . . ? C37 C36 C41 C42 178.2(3) . . . . ? P2 C36 C41 C42 -5.6(4) . . . . ? C40 C41 C42 C43 2.9(6) . . . . ? C36 C41 C42 C43 -177.1(4) . . . . ? C40 C41 C42 C47 -176.8(3) . . . . ? C36 C41 C42 C47 3.1(4) . . . . ? C47 C42 C43 C44 0.0(6) . . . . ? C41 C42 C43 C44 -179.8(4) . . . . ? C42 C43 C44 C45 0.6(7) . . . . ? C43 C44 C45 C46 0.3(7) . . . . ? C44 C45 C46 C47 -1.7(7) . . . . ? C45 C46 C47 C42 2.3(6) . . . . ? C45 C46 C47 P2 179.3(3) . . . . ? C43 C42 C47 C46 -1.5(5) . . . . ? C41 C42 C47 C46 178.3(3) . . . . ? C43 C42 C47 P2 -178.9(3) . . . . ? C41 C42 C47 P2 0.9(4) . . . . ? C36 P2 C47 C46 179.4(3) . . . . ? C19 P2 C47 C46 72.4(4) . . . . ? Rh2 P2 C47 C46 -58.1(3) . . . . ? C36 P2 C47 C42 -3.4(3) . . . . ? C19 P2 C47 C42 -110.3(3) . . . . ? Rh2 P2 C47 C42 119.1(2) . . . . ? C53 Rh1 C48 C49 107.5(3) . . . . ? C52 Rh1 C48 C49 72.8(3) . . . . ? P1 Rh1 C48 C49 -95.9(2) . . . . ? Cl1 Rh1 C48 C49 174.8(2) . . . . ? C49 Rh1 C48 C55 -118.8(5) . . . . ? C53 Rh1 C48 C55 -11.2(4) . . . . ? C52 Rh1 C48 C55 -46.0(4) . . . . ? P1 Rh1 C48 C55 145.3(4) . . . . ? Cl1 Rh1 C48 C55 56.0(5) . . . . ? C55 C48 C49 C50 2.3(7) . . . . ? Rh1 C48 C49 C50 -103.2(5) . . . . ? C55 C48 C49 Rh1 105.6(4) . . . . ? C53 Rh1 C49 C48 -71.1(3) . . . . ? C52 Rh1 C49 C48 -105.0(3) . . . . ? P1 Rh1 C49 C48 86.1(2) . . . . ? Cl1 Rh1 C49 C48 -173.0(3) . . . . ? C48 Rh1 C49 C50 121.8(5) . . . . ? C53 Rh1 C49 C50 50.7(5) . . . . ? C52 Rh1 C49 C50 16.8(5) . . . . ? P1 Rh1 C49 C50 -152.0(4) . . . . ? Cl1 Rh1 C49 C50 -51.2(7) . . . . ? C48 C49 C50 C51 57.1(10) . . . . ? Rh1 C49 C50 C51 -23.5(9) . . . . ? C49 C50 C51 C52 16.7(12) . . . . ? C50 C51 C52 C53 -81.9(9) . . . . ? C50 C51 C52 Rh1 -1.9(10) . . . . ? C48 Rh1 C52 C53 72.4(3) . . . . ? C49 Rh1 C52 C53 110.0(3) . . . . ? P1 Rh1 C52 C53 180(21) . . . . ? Cl1 Rh1 C52 C53 -85.5(3) . . . . ? C48 Rh1 C52 C51 -45.9(6) . . . . ? C49 Rh1 C52 C51 -8.3(5) . . . . ? C53 Rh1 C52 C51 -118.3(6) . . . . ? P1 Rh1 C52 C51 61.5(9) . . . . ? Cl1 Rh1 C52 C51 156.2(5) . . . . ? C51 C52 C53 C54 3.0(8) . . . . ? Rh1 C52 C53 C54 -99.3(5) . . . . ? C51 C52 C53 Rh1 102.3(4) . . . . ? C48 Rh1 C53 C52 -105.7(3) . . . . ? C49 Rh1 C53 C52 -68.6(3) . . . . ? P1 Rh1 C53 C52 -179.9(2) . . . . ? Cl1 Rh1 C53 C52 95.0(3) . . . . ? C48 Rh1 C53 C54 17.3(5) . . . . ? C49 Rh1 C53 C54 54.4(5) . . . . ? C52 Rh1 C53 C54 123.0(6) . . . . ? P1 Rh1 C53 C54 -56.9(6) . . . . ? Cl1 Rh1 C53 C54 -141.9(5) . . . . ? C52 C53 C54 C55 58.6(11) . . . . ? Rh1 C53 C54 C55 -22.0(10) . . . . ? C53 C54 C55 C48 13.9(12) . . . . ? C49 C48 C55 C54 -79.2(9) . . . . ? Rh1 C48 C55 C54 2.4(8) . . . . ? C61 Rh2 C56 C57 113.1(2) . . . . ? C60 Rh2 C56 C57 77.5(2) . . . . ? P2 Rh2 C56 C57 -94.2(2) . . . . ? Cl2 Rh2 C56 C57 173.2(3) . . . . ? C57 Rh2 C56 C63 -119.1(4) . . . . ? C61 Rh2 C56 C63 -6.0(3) . . . . ? C60 Rh2 C56 C63 -41.6(3) . . . . ? P2 Rh2 C56 C63 146.7(3) . . . . ? Cl2 Rh2 C56 C63 54.1(5) . . . . ? C63 C56 C57 C58 3.0(6) . . . . ? Rh2 C56 C57 C58 -102.5(4) . . . . ? C63 C56 C57 Rh2 105.5(4) . . . . ? C61 Rh2 C57 C56 -66.5(2) . . . . ? C60 Rh2 C57 C56 -98.8(2) . . . . ? P2 Rh2 C57 C56 88.3(2) . . . . ? Cl2 Rh2 C57 C56 -174.5(2) . . . . ? C56 Rh2 C57 C58 122.2(4) . . . . ? C61 Rh2 C57 C58 55.7(3) . . . . ? C60 Rh2 C57 C58 23.4(3) . . . . ? P2 Rh2 C57 C58 -149.5(3) . . . . ? Cl2 Rh2 C57 C58 -52.3(4) . . . . ? C56 C57 C58 C59 43.0(5) . . . . ? Rh2 C57 C58 C59 -38.4(4) . . . . ? C57 C58 C59 C60 33.9(5) . . . . ? C58 C59 C60 C61 -93.8(5) . . . . ? C58 C59 C60 Rh2 -13.3(4) . . . . ? C57 Rh2 C60 C61 116.1(3) . . . . ? C56 Rh2 C60 C61 77.7(3) . . . . ? P2 Rh2 C60 C61 174.5(6) . . . . ? Cl2 Rh2 C60 C61 -85.0(2) . . . . ? C57 Rh2 C60 C59 -5.5(3) . . . . ? C56 Rh2 C60 C59 -43.9(3) . . . . ? C61 Rh2 C60 C59 -121.6(4) . . . . ? P2 Rh2 C60 C59 53.0(8) . . . . ? Cl2 Rh2 C60 C59 153.5(3) . . . . ? C59 C60 C61 C62 3.3(6) . . . . ? Rh2 C60 C61 C62 -99.3(4) . . . . ? C59 C60 C61 Rh2 102.6(4) . . . . ? C57 Rh2 C61 C60 -63.5(3) . . . . ? C56 Rh2 C61 C60 -99.1(3) . . . . ? P2 Rh2 C61 C60 -178.30(19) . . . . ? Cl2 Rh2 C61 C60 95.9(2) . . . . ? C57 Rh2 C61 C62 60.0(4) . . . . ? C56 Rh2 C61 C62 24.4(3) . . . . ? C60 Rh2 C61 C62 123.5(5) . . . . ? P2 Rh2 C61 C62 -54.8(5) . . . . ? Cl2 Rh2 C61 C62 -140.6(3) . . . . ? C60 C61 C62 C63 41.9(6) . . . . ? Rh2 C61 C62 C63 -39.7(5) . . . . ? C57 C56 C63 C62 -94.6(5) . . . . ? Rh2 C56 C63 C62 -14.0(5) . . . . ? C61 C62 C63 C56 36.3(6) . . . . ? Cl3A C1LA Cl1A C1L' 58.8(7) . . . . ? Cl2A C1LA Cl1A C1L' -61.5(7) . . . . ? Cl2A C1L' Cl1A C1LA 66.9(7) . . . . ? Cl3' C1L' Cl1A C1LA -51.0(7) . . . . ? Cl3' C1L' Cl2A C1LA 52.6(8) . . . . ? Cl1A C1L' Cl2A C1LA -59.9(8) . . . . ? Cl3A C1LA Cl2A C1L' -50.7(8) . . . . ? Cl1A C1LA Cl2A C1L' 69.6(9) . . . . ? Cl1Y C1LY Cl2Y Cl3Y 147.8(10) . . . 2_755 ? Cl3Y C1LY Cl2Y Cl3Y -87.5(14) . . . 2_755 ? Cl2Y C1LY Cl2Y Cl3Y -67.4(13) 2_755 . . 2_755 ? Cl1Y C1LY Cl2Y C1LY -144.8(9) . . . 2_755 ? Cl3Y C1LY Cl2Y C1LY -20.0(5) . . . 2_755 ? Cl2Y C1LY Cl2Y C1LY 0.0 2_755 . . 2_755 ? Cl1Y C1LY Cl2Y Cl2Y -144.8(9) . . . 2_755 ? Cl3Y C1LY Cl2Y Cl2Y -20.0(5) . . . 2_755 ? Cl1Y C1LY Cl3Y Cl2Y 150.7(9) . . . 2_755 ? Cl2Y C1LY Cl3Y Cl2Y 26.7(7) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.877 _diffrn_reflns_theta_full 38.25 _diffrn_measured_fraction_theta_full 0.877 _refine_diff_density_max 3.049 _refine_diff_density_min -3.367 _refine_diff_density_rms 0.193 #===END data_xr001_0m _database_code_depnum_ccdc_archive 'CCDC 286683' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H54 O2 P2' _chemical_formula_weight 568.72 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' 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 10.8544(10) _cell_length_b 11.1005(11) _cell_length_c 15.1731(15) _cell_angle_alpha 85.280(2) _cell_angle_beta 89.538(2) _cell_angle_gamma 63.872(2) _cell_volume 1635.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6136 _cell_measurement_theta_min 3.46 _cell_measurement_theta_max 39.40 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 620 _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5978 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32900 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0498 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.24 _diffrn_reflns_theta_max 40.00 _reflns_number_total 18323 _reflns_number_gt 15056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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^)+(0.1041P)^2^+0.2670P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18323 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1721 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 P1 P 0.12081(2) 0.69550(2) 0.328110(14) 0.01221(5) Uani 1 1 d . . . C1 C 0.46418(8) 0.31768(7) 0.37955(5) 0.01022(11) Uani 1 1 d . . . O1 O 0.36516(6) 0.45503(6) 0.37615(4) 0.01155(10) Uani 1 1 d . . . P2 P 0.47953(2) 0.30156(2) 0.098975(14) 0.01334(5) Uani 1 1 d . . . C2 C 0.60416(8) 0.29884(8) 0.41178(5) 0.01200(12) Uani 1 1 d . . . H2A H 0.6710 0.2042 0.4063 0.014 Uiso 1 1 calc R . . H2B H 0.5992 0.3135 0.4755 0.014 Uiso 1 1 calc R . . O2 O 0.47640(6) 0.27434(6) 0.29230(4) 0.01161(10) Uani 1 1 d . . . C3 C 0.65969(8) 0.39099(8) 0.36360(5) 0.01100(11) Uani 1 1 d . . . C4 C 0.54237(8) 0.53163(8) 0.34666(5) 0.01047(11) Uani 1 1 d . . . C5 C 0.56927(8) 0.64206(8) 0.32337(5) 0.01306(12) Uani 1 1 d . . . H5A H 0.6620 0.6286 0.3223 0.016 Uiso 1 1 calc R . . C6 C 0.46528(9) 0.77106(8) 0.30169(6) 0.01433(13) Uani 1 1 d . . . C7 C 0.32931(9) 0.78946(8) 0.30284(6) 0.01408(13) Uani 1 1 d . . . H7A H 0.2574 0.8768 0.2876 0.017 Uiso 1 1 calc R . . C8 C 0.29611(8) 0.68265(8) 0.32588(5) 0.01187(12) Uani 1 1 d . . . C9 C 0.40523(8) 0.55436(7) 0.34907(5) 0.01045(11) Uani 1 1 d . . . C10 C 0.77391(9) 0.39015(9) 0.42295(6) 0.01632(14) Uani 1 1 d . . . H10A H 0.7346 0.4312 0.4775 0.024 Uiso 1 1 calc R . . H10B H 0.8172 0.4416 0.3917 0.024 Uiso 1 1 calc R . . H10C H 0.8429 0.2971 0.4375 0.024 Uiso 1 1 calc R . . C11 C 0.72041(9) 0.34031(9) 0.27409(6) 0.01533(13) Uani 1 1 d . . . H11A H 0.7623 0.3964 0.2477 0.023 Uiso 1 1 calc R . . H11B H 0.6472 0.3457 0.2343 0.023 Uiso 1 1 calc R . . H11C H 0.7904 0.2466 0.2835 0.023 Uiso 1 1 calc R . . C12 C 0.50072(11) 0.88541(10) 0.27410(8) 0.02280(18) Uani 1 1 d . . . H12A H 0.5721 0.8569 0.2299 0.034 Uiso 1 1 calc R . . H12B H 0.5344 0.9106 0.3259 0.034 Uiso 1 1 calc R . . H12C H 0.4187 0.9630 0.2486 0.034 Uiso 1 1 calc R . . C13 C 0.41376(8) 0.23518(8) 0.44160(5) 0.01271(12) Uani 1 1 d . . . H13A H 0.4021 0.2700 0.5006 0.015 Uiso 1 1 calc R . . H13B H 0.4859 0.1410 0.4480 0.015 Uiso 1 1 calc R . . C14 C 0.27891(8) 0.23461(8) 0.41323(5) 0.01243(12) Uani 1 1 d . . . C15 C 0.27212(8) 0.23639(8) 0.31270(5) 0.01175(12) Uani 1 1 d . . . C16 C 0.17024(9) 0.21366(9) 0.27163(6) 0.01500(13) Uani 1 1 d . . . H16A H 0.1037 0.2011 0.3072 0.018 Uiso 1 1 calc R . . C17 C 0.16273(9) 0.20872(10) 0.18064(6) 0.01666(14) Uani 1 1 d . . . C18 C 0.25928(9) 0.23057(9) 0.12915(6) 0.01524(13) Uani 1 1 d . . . H18A H 0.2557 0.2269 0.0669 0.018 Uiso 1 1 calc R . . C19 C 0.36078(8) 0.25755(8) 0.16593(5) 0.01227(12) Uani 1 1 d . . . C20 C 0.36737(8) 0.25743(8) 0.25890(5) 0.01080(11) Uani 1 1 d . . . C21 C 0.27891(11) 0.10399(9) 0.45678(6) 0.01868(15) Uani 1 1 d . . . H21A H 0.3502 0.0261 0.4310 0.028 Uiso 1 1 calc R . . H21B H 0.1891 0.1058 0.4465 0.028 Uiso 1 1 calc R . . H21C H 0.2975 0.0970 0.5206 0.028 Uiso 1 1 calc R . . C22 C 0.15368(9) 0.35519(9) 0.44557(6) 0.01682(14) Uani 1 1 d . . . H22A H 0.1522 0.4393 0.4190 0.025 Uiso 1 1 calc R . . H22B H 0.1598 0.3525 0.5102 0.025 Uiso 1 1 calc R . . H22C H 0.0693 0.3504 0.4281 0.025 Uiso 1 1 calc R . . C23 C 0.05405(12) 0.18150(14) 0.13807(8) 0.0275(2) Uani 1 1 d . . . H23A H 0.0027 0.1578 0.1841 0.041 Uiso 1 1 calc R . . H23B H 0.0974 0.1067 0.1007 0.041 Uiso 1 1 calc R . . H23C H -0.0088 0.2623 0.1016 0.041 Uiso 1 1 calc R . . C24 C 0.01140(9) 0.88032(8) 0.31180(6) 0.01423(13) Uani 1 1 d . . . H24A H 0.0437 0.9201 0.2605 0.017 Uiso 1 1 calc R . . C25 C 0.02105(10) 0.94281(10) 0.39643(7) 0.01957(16) Uani 1 1 d . . . H25A H -0.0329 1.0408 0.3880 0.029 Uiso 1 1 calc R . . H25B H 0.1172 0.9209 0.4096 0.029 Uiso 1 1 calc R . . H25C H -0.0151 0.9066 0.4458 0.029 Uiso 1 1 calc R . . C26 C -0.13764(9) 0.90716(10) 0.29476(7) 0.01989(16) Uani 1 1 d . . . H26A H -0.1983 1.0028 0.2992 0.030 Uiso 1 1 calc R . . H26B H -0.1624 0.8525 0.3388 0.030 Uiso 1 1 calc R . . H26C H -0.1477 0.8833 0.2354 0.030 Uiso 1 1 calc R . . C27 C 0.11738(10) 0.63258(10) 0.21744(7) 0.01970(16) Uani 1 1 d . . . H27A H 0.2055 0.5490 0.2151 0.024 Uiso 1 1 calc R . . C28 C 0.00313(13) 0.58851(12) 0.20940(9) 0.0300(2) Uani 1 1 d . . . H28A H 0.0144 0.5422 0.1555 0.045 Uiso 1 1 calc R . . H28B H -0.0862 0.6679 0.2065 0.045 Uiso 1 1 calc R . . H28C H 0.0080 0.5272 0.2610 0.045 Uiso 1 1 calc R . . C29 C 0.11615(13) 0.72744(13) 0.13785(7) 0.0268(2) Uani 1 1 d . . . H29A H 0.1338 0.6800 0.0840 0.040 Uiso 1 1 calc R . . H29B H 0.1876 0.7570 0.1468 0.040 Uiso 1 1 calc R . . H29C H 0.0263 0.8061 0.1318 0.040 Uiso 1 1 calc R . . C30 C 0.63454(9) 0.13442(9) 0.11182(6) 0.01646(14) Uani 1 1 d . . . H30A H 0.6479 0.1078 0.1769 0.020 Uiso 1 1 calc R . . C31 C 0.62170(11) 0.01928(10) 0.07069(7) 0.02195(17) Uani 1 1 d . . . H31A H 0.7028 -0.0655 0.0876 0.033 Uiso 1 1 calc R . . H31B H 0.6148 0.0367 0.0061 0.033 Uiso 1 1 calc R . . H31C H 0.5392 0.0127 0.0920 0.033 Uiso 1 1 calc R . . C32 C 0.76531(10) 0.14460(12) 0.08255(7) 0.02260(17) Uani 1 1 d . . . H32A H 0.8459 0.0623 0.1044 0.034 Uiso 1 1 calc R . . H32B H 0.7685 0.2224 0.1068 0.034 Uiso 1 1 calc R . . H32C H 0.7652 0.1556 0.0178 0.034 Uiso 1 1 calc R . . C33 C 0.41221(10) 0.31673(10) -0.01592(6) 0.01753(14) Uani 1 1 d . . . H33A H 0.3941 0.2376 -0.0248 0.021 Uiso 1 1 calc R . . C34 C 0.51788(12) 0.32196(13) -0.08193(7) 0.02490(19) Uani 1 1 d . . . H34A H 0.4771 0.3437 -0.1420 0.037 Uiso 1 1 calc R . . H34B H 0.5986 0.2342 -0.0785 0.037 Uiso 1 1 calc R . . H34C H 0.5454 0.3913 -0.0675 0.037 Uiso 1 1 calc R . . C35 C 0.27857(12) 0.44726(12) -0.03135(7) 0.02527(19) Uani 1 1 d . . . H35A H 0.2403 0.4529 -0.0907 0.038 Uiso 1 1 calc R . . H35B H 0.2978 0.5248 -0.0262 0.038 Uiso 1 1 calc R . . H35C H 0.2123 0.4474 0.0129 0.038 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 P1 0.00888(8) 0.01168(9) 0.01479(9) 0.00094(6) -0.00104(6) -0.00370(7) C1 0.0096(3) 0.0108(3) 0.0099(3) -0.0001(2) -0.0012(2) -0.0043(2) O1 0.0086(2) 0.0098(2) 0.0159(2) 0.00021(17) -0.00012(17) -0.00394(17) P2 0.01406(9) 0.01692(10) 0.01107(9) -0.00057(6) -0.00082(7) -0.00877(7) C2 0.0099(3) 0.0134(3) 0.0120(3) 0.0010(2) -0.0031(2) -0.0048(2) O2 0.0105(2) 0.0164(2) 0.0103(2) -0.00218(17) -0.00033(17) -0.00800(19) C3 0.0083(2) 0.0128(3) 0.0115(3) -0.0008(2) -0.0016(2) -0.0042(2) C4 0.0088(2) 0.0119(3) 0.0108(3) -0.0009(2) -0.0012(2) -0.0046(2) C5 0.0111(3) 0.0138(3) 0.0152(3) -0.0007(2) -0.0001(2) -0.0065(2) C6 0.0139(3) 0.0128(3) 0.0171(3) 0.0000(2) 0.0019(2) -0.0068(2) C7 0.0119(3) 0.0116(3) 0.0174(3) 0.0009(2) 0.0009(2) -0.0044(2) C8 0.0095(3) 0.0117(3) 0.0133(3) 0.0003(2) -0.0002(2) -0.0040(2) C9 0.0093(3) 0.0109(3) 0.0112(3) 0.0000(2) -0.0010(2) -0.0046(2) C10 0.0115(3) 0.0202(3) 0.0177(3) -0.0001(3) -0.0056(2) -0.0076(3) C11 0.0130(3) 0.0177(3) 0.0155(3) -0.0040(2) 0.0029(2) -0.0065(3) C12 0.0199(4) 0.0152(3) 0.0348(5) 0.0017(3) 0.0053(4) -0.0099(3) C13 0.0135(3) 0.0141(3) 0.0110(3) 0.0017(2) -0.0014(2) -0.0070(2) C14 0.0129(3) 0.0141(3) 0.0118(3) 0.0006(2) 0.0007(2) -0.0077(2) C15 0.0110(3) 0.0134(3) 0.0121(3) -0.0003(2) -0.0003(2) -0.0068(2) C16 0.0127(3) 0.0192(3) 0.0162(3) -0.0007(2) -0.0005(2) -0.0099(3) C17 0.0137(3) 0.0224(4) 0.0171(3) -0.0022(3) -0.0021(3) -0.0108(3) C18 0.0145(3) 0.0204(3) 0.0135(3) -0.0020(2) -0.0021(2) -0.0099(3) C19 0.0121(3) 0.0152(3) 0.0111(3) -0.0013(2) -0.0005(2) -0.0074(2) C20 0.0103(3) 0.0121(3) 0.0112(3) -0.0006(2) -0.0009(2) -0.0061(2) C21 0.0237(4) 0.0188(3) 0.0173(3) 0.0030(3) 0.0012(3) -0.0137(3) C22 0.0138(3) 0.0194(3) 0.0179(3) -0.0033(3) 0.0036(3) -0.0076(3) C23 0.0228(4) 0.0478(7) 0.0234(4) -0.0058(4) -0.0028(3) -0.0254(5) C24 0.0122(3) 0.0126(3) 0.0150(3) -0.0005(2) -0.0002(2) -0.0030(2) C25 0.0183(4) 0.0189(4) 0.0203(4) -0.0063(3) 0.0008(3) -0.0064(3) C26 0.0118(3) 0.0200(4) 0.0223(4) -0.0022(3) -0.0026(3) -0.0019(3) C27 0.0154(3) 0.0178(3) 0.0233(4) -0.0058(3) -0.0040(3) -0.0042(3) C28 0.0265(5) 0.0239(5) 0.0410(6) -0.0050(4) -0.0129(4) -0.0118(4) C29 0.0256(5) 0.0358(6) 0.0161(4) -0.0055(4) 0.0015(3) -0.0102(4) C30 0.0139(3) 0.0200(3) 0.0155(3) -0.0009(3) -0.0012(2) -0.0076(3) C31 0.0213(4) 0.0198(4) 0.0257(4) -0.0038(3) -0.0002(3) -0.0096(3) C32 0.0151(3) 0.0301(5) 0.0242(4) -0.0042(3) 0.0016(3) -0.0112(3) C33 0.0193(4) 0.0217(4) 0.0126(3) -0.0006(3) -0.0018(3) -0.0100(3) C34 0.0287(5) 0.0349(5) 0.0133(3) -0.0011(3) 0.0031(3) -0.0163(4) C35 0.0237(4) 0.0256(4) 0.0219(4) 0.0038(3) -0.0061(3) -0.0075(4) _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 P1 C8 1.8448(8) . ? P1 C24 1.8590(8) . ? P1 C27 1.8776(10) . ? C1 O1 1.4237(9) . ? C1 O2 1.4308(10) . ? C1 C2 1.5188(11) . ? C1 C13 1.5218(11) . ? O1 C9 1.3851(10) . ? P2 C19 1.8395(8) . ? P2 C33 1.8615(9) . ? P2 C30 1.8728(9) . ? C2 C3 1.5352(11) . ? O2 C20 1.3833(10) . ? C3 C4 1.5209(11) . ? C3 C10 1.5344(12) . ? C3 C11 1.5428(11) . ? C4 C9 1.3968(11) . ? C4 C5 1.3983(11) . ? C5 C6 1.3920(12) . ? C6 C7 1.3982(12) . ? C6 C12 1.5082(12) . ? C7 C8 1.4013(11) . ? C8 C9 1.4119(11) . ? C13 C14 1.5319(12) . ? C14 C15 1.5258(11) . ? C14 C22 1.5411(12) . ? C14 C21 1.5431(11) . ? C15 C16 1.3991(12) . ? C15 C20 1.3992(11) . ? C16 C17 1.3906(13) . ? C17 C18 1.3954(12) . ? C17 C23 1.5028(14) . ? C18 C19 1.3939(12) . ? C19 C20 1.4129(11) . ? C24 C26 1.5305(13) . ? C24 C25 1.5343(13) . ? C27 C28 1.5294(16) . ? C27 C29 1.5317(16) . ? C30 C31 1.5271(14) . ? C30 C32 1.5322(13) . ? C33 C34 1.5339(14) . ? C33 C35 1.5352(15) . ? 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 C8 P1 C24 102.74(4) . . ? C8 P1 C27 98.32(4) . . ? C24 P1 C27 104.85(4) . . ? O1 C1 O2 108.42(6) . . ? O1 C1 C2 111.73(6) . . ? O2 C1 C2 108.57(6) . . ? O1 C1 C13 108.19(6) . . ? O2 C1 C13 110.05(6) . . ? C2 C1 C13 109.87(6) . . ? C9 O1 C1 118.87(6) . . ? C19 P2 C33 102.71(4) . . ? C19 P2 C30 98.75(4) . . ? C33 P2 C30 105.23(4) . . ? C1 C2 C3 115.95(6) . . ? C20 O2 C1 116.94(6) . . ? C4 C3 C10 111.70(7) . . ? C4 C3 C2 108.70(6) . . ? C10 C3 C2 107.51(7) . . ? C4 C3 C11 108.64(6) . . ? C10 C3 C11 108.72(7) . . ? C2 C3 C11 111.59(7) . . ? C9 C4 C5 117.73(7) . . ? C9 C4 C3 121.73(7) . . ? C5 C4 C3 120.46(7) . . ? C6 C5 C4 122.46(8) . . ? C5 C6 C7 118.23(7) . . ? C5 C6 C12 120.07(8) . . ? C7 C6 C12 121.65(8) . . ? C6 C7 C8 121.85(7) . . ? C7 C8 C9 117.69(7) . . ? C7 C8 P1 125.32(6) . . ? C9 C8 P1 116.99(6) . . ? O1 C9 C4 123.18(7) . . ? O1 C9 C8 114.79(7) . . ? C4 C9 C8 122.01(7) . . ? C1 C13 C14 115.84(6) . . ? C15 C14 C13 109.24(6) . . ? C15 C14 C22 110.61(7) . . ? C13 C14 C22 111.42(7) . . ? C15 C14 C21 110.04(7) . . ? C13 C14 C21 107.29(7) . . ? C22 C14 C21 108.17(7) . . ? C16 C15 C20 117.87(7) . . ? C16 C15 C14 120.10(7) . . ? C20 C15 C14 122.02(7) . . ? C17 C16 C15 122.46(8) . . ? C16 C17 C18 117.99(8) . . ? C16 C17 C23 121.59(8) . . ? C18 C17 C23 120.42(8) . . ? C19 C18 C17 122.21(8) . . ? C18 C19 C20 117.91(7) . . ? C18 C19 P2 123.11(6) . . ? C20 C19 P2 118.90(6) . . ? O2 C20 C15 123.01(7) . . ? O2 C20 C19 115.46(6) . . ? C15 C20 C19 121.49(7) . . ? C26 C24 C25 109.28(7) . . ? C26 C24 P1 109.18(6) . . ? C25 C24 P1 108.46(6) . . ? C28 C27 C29 111.88(9) . . ? C28 C27 P1 111.96(8) . . ? C29 C27 P1 114.76(7) . . ? C31 C30 C32 110.96(8) . . ? C31 C30 P2 115.88(7) . . ? C32 C30 P2 112.15(7) . . ? C34 C33 C35 108.86(8) . . ? C34 C33 P2 109.47(7) . . ? C35 C33 P2 109.39(7) . . ? 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 O2 C1 O1 C9 -81.74(8) . . . . ? C2 C1 O1 C9 37.86(9) . . . . ? C13 C1 O1 C9 158.93(7) . . . . ? O1 C1 C2 C3 -51.60(9) . . . . ? O2 C1 C2 C3 67.92(8) . . . . ? C13 C1 C2 C3 -171.69(6) . . . . ? O1 C1 O2 C20 -71.44(8) . . . . ? C2 C1 O2 C20 166.99(6) . . . . ? C13 C1 O2 C20 46.71(9) . . . . ? C1 C2 C3 C4 40.76(9) . . . . ? C1 C2 C3 C10 161.84(7) . . . . ? C1 C2 C3 C11 -79.03(8) . . . . ? C10 C3 C4 C9 -137.37(8) . . . . ? C2 C3 C4 C9 -18.90(10) . . . . ? C11 C3 C4 C9 102.71(8) . . . . ? C10 C3 C4 C5 46.07(10) . . . . ? C2 C3 C4 C5 164.54(7) . . . . ? C11 C3 C4 C5 -73.86(9) . . . . ? C9 C4 C5 C6 -0.96(12) . . . . ? C3 C4 C5 C6 175.74(8) . . . . ? C4 C5 C6 C7 -0.48(13) . . . . ? C4 C5 C6 C12 -177.93(8) . . . . ? C5 C6 C7 C8 0.65(13) . . . . ? C12 C6 C7 C8 178.06(9) . . . . ? C6 C7 C8 C9 0.62(12) . . . . ? C6 C7 C8 P1 -179.16(7) . . . . ? C24 P1 C8 C7 -8.90(8) . . . . ? C27 P1 C8 C7 98.47(8) . . . . ? C24 P1 C8 C9 171.32(6) . . . . ? C27 P1 C8 C9 -81.31(7) . . . . ? C1 O1 C9 C4 -17.08(11) . . . . ? C1 O1 C9 C8 164.43(7) . . . . ? C5 C4 C9 O1 -176.07(7) . . . . ? C3 C4 C9 O1 7.27(11) . . . . ? C5 C4 C9 C8 2.30(11) . . . . ? C3 C4 C9 C8 -174.35(7) . . . . ? C7 C8 C9 O1 176.36(7) . . . . ? P1 C8 C9 O1 -3.84(9) . . . . ? C7 C8 C9 C4 -2.14(12) . . . . ? P1 C8 C9 C4 177.66(6) . . . . ? O1 C1 C13 C14 62.78(9) . . . . ? O2 C1 C13 C14 -55.52(9) . . . . ? C2 C1 C13 C14 -175.01(6) . . . . ? C1 C13 C14 C15 35.82(9) . . . . ? C1 C13 C14 C22 -86.69(8) . . . . ? C1 C13 C14 C21 155.08(7) . . . . ? C13 C14 C15 C16 169.33(7) . . . . ? C22 C14 C15 C16 -67.68(10) . . . . ? C21 C14 C15 C16 51.78(10) . . . . ? C13 C14 C15 C20 -9.26(10) . . . . ? C22 C14 C15 C20 113.74(8) . . . . ? C21 C14 C15 C20 -126.81(8) . . . . ? C20 C15 C16 C17 1.33(13) . . . . ? C14 C15 C16 C17 -177.31(8) . . . . ? C15 C16 C17 C18 -1.53(14) . . . . ? C15 C16 C17 C23 178.79(10) . . . . ? C16 C17 C18 C19 -0.38(14) . . . . ? C23 C17 C18 C19 179.30(10) . . . . ? C17 C18 C19 C20 2.35(13) . . . . ? C17 C18 C19 P2 -174.38(7) . . . . ? C33 P2 C19 C18 6.13(8) . . . . ? C30 P2 C19 C18 -101.76(8) . . . . ? C33 P2 C19 C20 -170.57(7) . . . . ? C30 P2 C19 C20 81.54(7) . . . . ? C1 O2 C20 C15 -21.86(10) . . . . ? C1 O2 C20 C19 160.48(7) . . . . ? C16 C15 C20 O2 -176.76(7) . . . . ? C14 C15 C20 O2 1.85(12) . . . . ? C16 C15 C20 C19 0.76(12) . . . . ? C14 C15 C20 C19 179.38(7) . . . . ? C18 C19 C20 O2 175.16(7) . . . . ? P2 C19 C20 O2 -7.96(10) . . . . ? C18 C19 C20 C15 -2.53(12) . . . . ? P2 C19 C20 C15 174.34(6) . . . . ? C8 P1 C24 C26 169.53(6) . . . . ? C27 P1 C24 C26 67.20(7) . . . . ? C8 P1 C24 C25 -71.48(7) . . . . ? C27 P1 C24 C25 -173.80(6) . . . . ? C8 P1 C27 C28 162.13(7) . . . . ? C24 P1 C27 C28 -92.25(8) . . . . ? C8 P1 C27 C29 -68.94(8) . . . . ? C24 P1 C27 C29 36.69(8) . . . . ? C19 P2 C30 C31 65.50(7) . . . . ? C33 P2 C30 C31 -40.32(8) . . . . ? C19 P2 C30 C32 -165.70(7) . . . . ? C33 P2 C30 C32 88.48(7) . . . . ? C19 P2 C33 C34 -167.36(7) . . . . ? C30 P2 C33 C34 -64.46(8) . . . . ? C19 P2 C33 C35 73.43(8) . . . . ? C30 P2 C33 C35 176.32(7) . . . . ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 40.00 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 1.486 _refine_diff_density_min -1.267 _refine_diff_density_rms 0.090 #===END data_cj079_0m _database_code_depnum_ccdc_archive 'CCDC 286684' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H42 O4 P2' _chemical_formula_weight 732.75 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7640(5) _cell_length_b 24.9675(11) _cell_length_c 12.5726(6) _cell_angle_alpha 90.00 _cell_angle_beta 96.9550(10) _cell_angle_gamma 90.00 _cell_volume 3665.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4167 _cell_measurement_theta_min 4.13 _cell_measurement_theta_max 39.14 _exptl_crystal_description block _exptl_crystal_colour translucent _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.328 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 0.166 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5381 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17439 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0391 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -4 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 39.50 _reflns_number_total 10811 _reflns_number_gt 8979 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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^)+(0.0627P)^2^+0.9500P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10811 _refine_ls_number_parameters 484 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0507 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1187 _refine_ls_wR_factor_gt 0.1116 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.002 _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 P1 P 0.48509(3) 0.152014(13) 0.61024(2) 0.01435(8) Uani 1 1 d . . . O1 O 0.24848(7) 0.12013(3) 0.53787(5) 0.01262(17) Uani 1 1 d . . . C1 C 0.14483(9) 0.09013(4) 0.51359(7) 0.0114(2) Uani 1 1 d . . . P2 P 0.09221(3) 0.015575(12) 0.813804(18) 0.01260(7) Uani 1 1 d . . . O2 O 0.12653(8) 0.05796(3) 0.60386(5) 0.01295(18) Uani 1 1 d . . . C2 C 0.04230(10) 0.12691(5) 0.48903(8) 0.0151(2) Uani 1 1 d . . . H2A H -0.0278 0.1046 0.4818 0.018 Uiso 1 1 calc R . . H2B H 0.0472 0.1440 0.4187 0.018 Uiso 1 1 calc R . . C3 C 0.02836(10) 0.17137(5) 0.57121(8) 0.0144(2) Uani 1 1 d . . . O3 O 0.62605(10) 0.18406(4) 0.83361(6) 0.0216(2) Uani 1 1 d . . . O4 O 0.19348(9) -0.00316(4) 1.06135(6) 0.0192(2) Uani 1 1 d . . . C4 C 0.14580(10) 0.19094(5) 0.62025(8) 0.0130(2) Uani 1 1 d . . . C5 C 0.15424(11) 0.23597(5) 0.68746(8) 0.0160(3) Uani 1 1 d . . . H5A H 0.0859 0.2525 0.7041 0.019 Uiso 1 1 calc R . . C6 C 0.25926(12) 0.25728(5) 0.73068(8) 0.0169(3) Uani 1 1 d . . . C7 C 0.35815(11) 0.23269(5) 0.70505(8) 0.0163(2) Uani 1 1 d . . . H7A H 0.4304 0.2475 0.7318 0.020 Uiso 1 1 calc R . . C8 C 0.35467(10) 0.18672(5) 0.64090(7) 0.0128(2) Uani 1 1 d . . . C9 C 0.24667(10) 0.16588(4) 0.60012(7) 0.0117(2) Uani 1 1 d . . . C10 C -0.04217(12) 0.15252(5) 0.65957(9) 0.0193(3) Uani 1 1 d . . . H10A H -0.0045 0.1216 0.6968 0.029 Uiso 1 1 calc R . . H10B H -0.1191 0.1423 0.6273 0.029 Uiso 1 1 calc R . . H10C H -0.0478 0.1817 0.7109 0.029 Uiso 1 1 calc R . . C11 C -0.03637(12) 0.21759(6) 0.50931(10) 0.0225(3) Uani 1 1 d . . . H11A H -0.0493 0.2465 0.5592 0.034 Uiso 1 1 calc R . . H11B H -0.1102 0.2045 0.4745 0.034 Uiso 1 1 calc R . . H11C H 0.0092 0.2312 0.4548 0.034 Uiso 1 1 calc R . . C12 C 0.26414(15) 0.30561(6) 0.80408(11) 0.0261(3) Uani 1 1 d . . . H12A H 0.3420 0.3203 0.8131 0.039 Uiso 1 1 calc R . . H12B H 0.2431 0.2949 0.8741 0.039 Uiso 1 1 calc R . . H12C H 0.2105 0.3330 0.7726 0.039 Uiso 1 1 calc R . . C13 C 0.15854(10) 0.05519(5) 0.41697(7) 0.0138(2) Uani 1 1 d . . . H13A H 0.1739 0.0787 0.3570 0.017 Uiso 1 1 calc R . . H13B H 0.0849 0.0367 0.3952 0.017 Uiso 1 1 calc R . . C14 C 0.25327(10) 0.01299(4) 0.43338(7) 0.0127(2) Uani 1 1 d . . . C15 C 0.25622(10) -0.01013(4) 0.54610(7) 0.0119(2) Uani 1 1 d . . . C16 C 0.32561(11) -0.05449(5) 0.57650(8) 0.0143(2) Uani 1 1 d . . . H16A H 0.3705 -0.0695 0.5261 0.017 Uiso 1 1 calc R . . C17 C 0.33106(11) -0.07741(5) 0.67830(8) 0.0152(2) Uani 1 1 d . . . C18 C 0.26078(10) -0.05633(5) 0.74949(7) 0.0145(2) Uani 1 1 d . . . H18A H 0.2604 -0.0727 0.8177 0.017 Uiso 1 1 calc R . . C19 C 0.19077(10) -0.01180(4) 0.72353(7) 0.0120(2) Uani 1 1 d . . . C20 C 0.19285(9) 0.01209(4) 0.62226(7) 0.0114(2) Uani 1 1 d . . . C21 C 0.22317(12) -0.03113(5) 0.34865(8) 0.0193(3) Uani 1 1 d . . . H21A H 0.1482 -0.0464 0.3576 0.029 Uiso 1 1 calc R . . H21B H 0.2814 -0.0594 0.3578 0.029 Uiso 1 1 calc R . . H21C H 0.2208 -0.0157 0.2768 0.029 Uiso 1 1 calc R . . C22 C 0.37048(11) 0.03626(5) 0.41614(7) 0.0158(2) Uani 1 1 d . . . H22A H 0.3905 0.0652 0.4677 0.024 Uiso 1 1 calc R . . H22B H 0.3671 0.0504 0.3431 0.024 Uiso 1 1 calc R . . H22C H 0.4286 0.0080 0.4266 0.024 Uiso 1 1 calc R . . C23 C 0.41456(14) -0.12247(6) 0.71033(10) 0.0235(3) Uani 1 1 d . . . H23A H 0.3878 -0.1431 0.7687 0.035 Uiso 1 1 calc R . . H23B H 0.4903 -0.1074 0.7343 0.035 Uiso 1 1 calc R . . H23C H 0.4196 -0.1460 0.6486 0.035 Uiso 1 1 calc R . . C24 C 0.59428(10) 0.20328(5) 0.64134(7) 0.0149(2) Uani 1 1 d . . . C25 C 0.62720(11) 0.23557(5) 0.55878(8) 0.0182(3) Uani 1 1 d . . . H25A H 0.5907 0.2307 0.4878 0.022 Uiso 1 1 calc R . . C26 C 0.71142(12) 0.27430(5) 0.57825(9) 0.0194(3) Uani 1 1 d . . . H26A H 0.7316 0.2959 0.5212 0.023 Uiso 1 1 calc R . . C27 C 0.76652(12) 0.28144(5) 0.68207(9) 0.0193(3) Uani 1 1 d . . . H27A H 0.8244 0.3079 0.6958 0.023 Uiso 1 1 calc R . . C28 C 0.73661(11) 0.24989(5) 0.76490(8) 0.0185(3) Uani 1 1 d . . . H28A H 0.7743 0.2545 0.8355 0.022 Uiso 1 1 calc R . . C29 C 0.65108(10) 0.21141(5) 0.74437(7) 0.0153(2) Uani 1 1 d . . . C30 C 0.57879(11) 0.13362(5) 0.82575(8) 0.0165(3) Uani 1 1 d . . . C31 C 0.59718(12) 0.10341(5) 0.91986(9) 0.0213(3) Uani 1 1 d . . . H31A H 0.6383 0.1184 0.9826 0.026 Uiso 1 1 calc R . . C32 C 0.55559(13) 0.05195(6) 0.92146(10) 0.0243(3) Uani 1 1 d . . . H32A H 0.5689 0.0313 0.9852 0.029 Uiso 1 1 calc R . . C33 C 0.49399(13) 0.02997(6) 0.82998(11) 0.0243(3) Uani 1 1 d . . . H33A H 0.4655 -0.0056 0.8310 0.029 Uiso 1 1 calc R . . C34 C 0.47467(11) 0.06069(5) 0.73725(10) 0.0196(3) Uani 1 1 d . . . H34A H 0.4322 0.0458 0.6752 0.024 Uiso 1 1 calc R . . C35 C 0.51618(10) 0.11279(5) 0.73327(8) 0.0156(2) Uani 1 1 d . . . C36 C 0.18856(10) 0.05670(5) 0.90478(7) 0.0140(2) Uani 1 1 d . . . C37 C 0.22499(13) 0.10568(5) 0.86808(8) 0.0195(3) Uani 1 1 d . . . H37A H 0.2023 0.1156 0.7957 0.023 Uiso 1 1 calc R . . C38 C 0.29366(14) 0.14052(6) 0.93416(9) 0.0230(3) Uani 1 1 d . . . H38A H 0.3178 0.1736 0.9072 0.028 Uiso 1 1 calc R . . C39 C 0.32649(13) 0.12598(5) 1.04091(9) 0.0222(3) Uani 1 1 d . . . H39A H 0.3729 0.1494 1.0872 0.027 Uiso 1 1 calc R . . C40 C 0.29163(12) 0.07770(5) 1.07917(8) 0.0194(3) Uani 1 1 d . . . H40A H 0.3146 0.0678 1.1516 0.023 Uiso 1 1 calc R . . C41 C 0.22241(11) 0.04314(5) 1.01166(7) 0.0145(2) Uani 1 1 d . . . C42 C 0.12967(10) -0.04323(5) 1.00914(7) 0.0136(2) Uani 1 1 d . . . C43 C 0.11567(12) -0.08809(5) 1.07329(7) 0.0170(3) Uani 1 1 d . . . H43A H 0.1509 -0.0890 1.1454 0.020 Uiso 1 1 calc R . . C44 C 0.05065(12) -0.13109(5) 1.03186(8) 0.0177(3) Uani 1 1 d . . . H44A H 0.0412 -0.1615 1.0754 0.021 Uiso 1 1 calc R . . C45 C -0.00117(12) -0.12972(5) 0.92579(9) 0.0193(3) Uani 1 1 d . . . H45A H -0.0466 -0.1590 0.8971 0.023 Uiso 1 1 calc R . . C46 C 0.01415(11) -0.08552(5) 0.86300(8) 0.0180(3) Uani 1 1 d . . . H46A H -0.0213 -0.0849 0.7910 0.022 Uiso 1 1 calc R . . C47 C 0.08068(10) -0.04128(5) 0.90238(7) 0.0134(2) 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 P1 0.01167(13) 0.01828(17) 0.01304(9) -0.00537(8) 0.00123(10) -0.00041(11) O1 0.0110(3) 0.0126(4) 0.0141(2) -0.0019(2) 0.0010(3) -0.0008(3) C1 0.0108(4) 0.0122(5) 0.0109(3) 0.0022(3) 0.0002(3) -0.0017(4) P2 0.01291(13) 0.01490(16) 0.01003(8) 0.00138(7) 0.00148(9) 0.00208(11) O2 0.0150(4) 0.0127(4) 0.0114(2) 0.0029(2) 0.0026(3) 0.0023(3) C2 0.0121(4) 0.0172(6) 0.0152(3) 0.0035(3) -0.0015(4) 0.0008(4) C3 0.0104(4) 0.0145(6) 0.0183(4) 0.0042(3) 0.0018(4) 0.0020(4) O3 0.0325(6) 0.0192(5) 0.0126(3) -0.0006(2) 0.0004(3) -0.0125(4) O4 0.0281(5) 0.0168(5) 0.0115(2) 0.0026(2) -0.0016(3) -0.0069(4) C4 0.0124(4) 0.0120(6) 0.0149(3) 0.0033(3) 0.0022(4) 0.0005(4) C5 0.0157(5) 0.0137(6) 0.0193(4) 0.0005(3) 0.0047(4) 0.0030(5) C6 0.0187(6) 0.0142(6) 0.0183(4) -0.0030(3) 0.0046(4) 0.0002(5) C7 0.0159(5) 0.0164(6) 0.0167(3) -0.0041(3) 0.0025(4) -0.0017(5) C8 0.0121(4) 0.0144(6) 0.0121(3) -0.0017(3) 0.0018(3) -0.0001(4) C9 0.0123(4) 0.0114(5) 0.0113(3) 0.0008(3) 0.0012(3) 0.0007(4) C10 0.0158(5) 0.0181(7) 0.0252(4) 0.0023(4) 0.0063(5) 0.0010(5) C11 0.0182(6) 0.0199(7) 0.0283(5) 0.0075(4) -0.0016(5) 0.0060(5) C12 0.0275(8) 0.0218(8) 0.0298(5) -0.0122(5) 0.0067(6) 0.0006(6) C13 0.0147(5) 0.0166(6) 0.0097(3) 0.0004(3) -0.0003(3) -0.0020(4) C14 0.0146(5) 0.0144(5) 0.0093(3) -0.0018(3) 0.0017(3) -0.0025(4) C15 0.0134(4) 0.0116(5) 0.0109(3) -0.0008(3) 0.0021(3) -0.0007(4) C16 0.0155(5) 0.0130(6) 0.0151(3) -0.0005(3) 0.0047(4) -0.0001(4) C17 0.0155(5) 0.0121(6) 0.0184(4) 0.0026(3) 0.0041(4) 0.0012(4) C18 0.0155(5) 0.0145(6) 0.0138(3) 0.0035(3) 0.0026(4) 0.0017(4) C19 0.0123(4) 0.0136(5) 0.0102(3) 0.0011(3) 0.0022(3) 0.0005(4) C20 0.0129(4) 0.0110(5) 0.0103(3) 0.0002(3) 0.0008(3) 0.0001(4) C21 0.0240(6) 0.0194(6) 0.0142(3) -0.0056(3) 0.0012(4) -0.0050(5) C22 0.0161(5) 0.0194(6) 0.0124(3) -0.0010(3) 0.0040(4) -0.0037(5) C23 0.0236(7) 0.0193(7) 0.0288(5) 0.0082(4) 0.0079(5) 0.0074(6) C24 0.0130(5) 0.0188(6) 0.0128(3) -0.0024(3) 0.0013(4) -0.0001(4) C25 0.0166(5) 0.0244(7) 0.0139(3) 0.0001(3) 0.0021(4) 0.0018(5) C26 0.0183(6) 0.0223(7) 0.0181(4) 0.0026(4) 0.0050(4) 0.0012(5) C27 0.0178(5) 0.0178(7) 0.0223(4) -0.0002(4) 0.0030(4) -0.0024(5) C28 0.0187(5) 0.0187(6) 0.0175(4) -0.0015(3) -0.0006(4) -0.0043(5) C29 0.0163(5) 0.0164(6) 0.0130(3) -0.0013(3) 0.0008(4) -0.0029(4) C30 0.0183(5) 0.0148(6) 0.0162(3) -0.0012(3) 0.0008(4) -0.0034(5) C31 0.0230(6) 0.0218(7) 0.0185(4) 0.0037(4) -0.0002(5) -0.0056(5) C32 0.0223(6) 0.0229(8) 0.0271(5) 0.0060(4) -0.0001(5) -0.0036(6) C33 0.0223(6) 0.0146(7) 0.0350(6) 0.0012(4) -0.0005(6) -0.0039(6) C34 0.0153(5) 0.0170(7) 0.0262(4) -0.0051(4) 0.0007(5) -0.0002(5) C35 0.0130(5) 0.0163(6) 0.0174(3) -0.0038(3) 0.0008(4) 0.0003(4) C36 0.0161(5) 0.0148(6) 0.0113(3) 0.0009(3) 0.0023(4) 0.0021(4) C37 0.0256(6) 0.0165(6) 0.0161(3) 0.0035(3) 0.0013(4) -0.0022(5) C38 0.0302(7) 0.0172(7) 0.0213(4) 0.0034(4) 0.0016(5) -0.0059(6) C39 0.0262(7) 0.0201(7) 0.0195(4) -0.0010(4) -0.0001(5) -0.0055(5) C40 0.0255(6) 0.0171(6) 0.0147(3) -0.0006(3) -0.0014(4) -0.0031(5) C41 0.0176(5) 0.0140(6) 0.0120(3) 0.0005(3) 0.0016(4) 0.0009(4) C42 0.0166(5) 0.0135(6) 0.0110(3) 0.0001(3) 0.0027(4) 0.0002(4) C43 0.0228(6) 0.0160(6) 0.0123(3) 0.0018(3) 0.0032(4) -0.0012(5) C44 0.0233(6) 0.0138(6) 0.0167(3) 0.0003(3) 0.0057(4) 0.0006(5) C45 0.0220(6) 0.0165(6) 0.0191(4) -0.0010(3) 0.0015(4) -0.0032(5) C46 0.0193(5) 0.0198(6) 0.0146(3) 0.0002(3) 0.0001(4) -0.0022(5) C47 0.0137(4) 0.0156(6) 0.0110(3) 0.0005(3) 0.0017(3) 0.0014(4) _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 P1 C24 1.8219(12) . ? P1 C35 1.8298(11) . ? P1 C8 1.8431(13) . ? O1 C9 1.3863(13) . ? O1 C1 1.4322(13) . ? C1 O2 1.4278(12) . ? C1 C2 1.5177(15) . ? C1 C13 1.5199(14) . ? P2 C47 1.8194(11) . ? P2 C36 1.8258(10) . ? P2 C19 1.8489(13) . ? O2 C20 1.3891(13) . ? C2 C3 1.5387(17) . ? C3 C4 1.5236(15) . ? C3 C10 1.539(2) . ? C3 C11 1.5406(15) . ? O3 C30 1.3753(15) . ? O3 C29 1.3755(14) . ? O4 C42 1.3697(13) . ? O4 C41 1.3762(15) . ? C4 C9 1.3915(18) . ? C4 C5 1.4028(16) . ? C5 C6 1.3935(17) . ? C6 C7 1.387(2) . ? C6 C12 1.5160(17) . ? C7 C8 1.4005(15) . ? C8 C9 1.4107(15) . ? C13 C14 1.5294(16) . ? C14 C15 1.5269(13) . ? C14 C22 1.5356(18) . ? C14 C21 1.5435(14) . ? C15 C20 1.3977(16) . ? C15 C16 1.4012(15) . ? C16 C17 1.3963(15) . ? C17 C18 1.3933(19) . ? C17 C23 1.5155(17) . ? C18 C19 1.3983(15) . ? C19 C20 1.4090(13) . ? C24 C29 1.3986(11) . ? C24 C25 1.4051(17) . ? C25 C26 1.3849(18) . ? C26 C27 1.3967(14) . ? C27 C28 1.3848(18) . ? C28 C29 1.3926(17) . ? C30 C31 1.3978(15) . ? C30 C35 1.3991(13) . ? C31 C32 1.376(2) . ? C32 C33 1.3955(17) . ? C33 C34 1.3911(19) . ? C34 C35 1.3925(19) . ? C36 C37 1.3928(18) . ? C36 C41 1.3961(12) . ? C37 C38 1.3917(17) . ? C38 C39 1.3988(15) . ? C39 C40 1.379(2) . ? C40 C41 1.4002(15) . ? C42 C47 1.3960(11) . ? C42 C43 1.4014(16) . ? C43 C44 1.3830(17) . ? C44 C45 1.3980(13) . ? C45 C46 1.3813(18) . ? C46 C47 1.4084(16) . ? 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 C24 P1 C35 97.53(5) . . ? C24 P1 C8 102.00(5) . . ? C35 P1 C8 99.27(5) . . ? C9 O1 C1 118.72(9) . . ? O2 C1 O1 109.35(6) . . ? O2 C1 C2 108.03(10) . . ? O1 C1 C2 111.23(9) . . ? O2 C1 C13 110.69(9) . . ? O1 C1 C13 107.49(10) . . ? C2 C1 C13 110.08(7) . . ? C47 P2 C36 98.16(4) . . ? C47 P2 C19 100.72(5) . . ? C36 P2 C19 101.81(5) . . ? C20 O2 C1 117.41(9) . . ? C1 C2 C3 116.53(7) . . ? C4 C3 C10 110.35(8) . . ? C4 C3 C2 109.75(10) . . ? C10 C3 C2 112.01(10) . . ? C4 C3 C11 109.44(10) . . ? C10 C3 C11 108.48(11) . . ? C2 C3 C11 106.71(8) . . ? C30 O3 C29 121.37(8) . . ? C42 O4 C41 123.18(7) . . ? C9 C4 C5 118.05(10) . . ? C9 C4 C3 122.26(10) . . ? C5 C4 C3 119.69(11) . . ? C6 C5 C4 122.39(12) . . ? C7 C6 C5 117.99(11) . . ? C7 C6 C12 121.50(11) . . ? C5 C6 C12 120.51(13) . . ? C6 C7 C8 121.97(10) . . ? C7 C8 C9 118.29(11) . . ? C7 C8 P1 122.60(8) . . ? C9 C8 P1 119.11(8) . . ? O1 C9 C4 123.01(9) . . ? O1 C9 C8 115.75(10) . . ? C4 C9 C8 121.22(10) . . ? C1 C13 C14 115.70(6) . . ? C15 C14 C13 108.67(9) . . ? C15 C14 C22 110.74(7) . . ? C13 C14 C22 111.86(10) . . ? C15 C14 C21 110.37(9) . . ? C13 C14 C21 107.22(8) . . ? C22 C14 C21 107.91(10) . . ? C20 C15 C16 117.93(9) . . ? C20 C15 C14 122.12(9) . . ? C16 C15 C14 119.94(10) . . ? C17 C16 C15 122.31(12) . . ? C18 C17 C16 117.97(10) . . ? C18 C17 C23 121.72(10) . . ? C16 C17 C23 120.27(12) . . ? C17 C18 C19 121.94(9) . . ? C18 C19 C20 118.26(11) . . ? C18 C19 P2 123.10(8) . . ? C20 C19 P2 118.61(8) . . ? O2 C20 C15 123.27(8) . . ? O2 C20 C19 115.39(10) . . ? C15 C20 C19 121.33(10) . . ? C29 C24 C25 117.22(10) . . ? C29 C24 P1 123.10(9) . . ? C25 C24 P1 119.65(7) . . ? C26 C25 C24 121.69(9) . . ? C25 C26 C27 119.70(12) . . ? C28 C27 C26 119.92(11) . . ? C27 C28 C29 119.78(9) . . ? O3 C29 C28 114.36(8) . . ? O3 C29 C24 123.92(10) . . ? C28 C29 C24 121.69(11) . . ? O3 C30 C31 114.42(8) . . ? O3 C30 C35 124.59(10) . . ? C31 C30 C35 120.98(12) . . ? C32 C31 C30 119.83(10) . . ? C31 C32 C33 120.36(12) . . ? C34 C33 C32 119.32(13) . . ? C33 C34 C35 121.52(10) . . ? C34 C35 C30 117.97(10) . . ? C34 C35 P1 119.69(7) . . ? C30 C35 P1 122.33(10) . . ? C37 C36 C41 117.93(10) . . ? C37 C36 P2 118.61(6) . . ? C41 C36 P2 123.35(9) . . ? C38 C37 C36 122.05(9) . . ? C37 C38 C39 118.91(13) . . ? C40 C39 C38 120.16(11) . . ? C39 C40 C41 120.20(9) . . ? O4 C41 C36 125.68(10) . . ? O4 C41 C40 113.58(8) . . ? C36 C41 C40 120.74(11) . . ? O4 C42 C47 125.02(10) . . ? O4 C42 C43 113.81(7) . . ? C47 C42 C43 121.17(10) . . ? C44 C43 C42 120.13(8) . . ? C43 C44 C45 119.84(11) . . ? C46 C45 C44 119.52(11) . . ? C45 C46 C47 122.08(8) . . ? C42 C47 C46 117.24(10) . . ? C42 C47 P2 124.27(9) . . ? C46 C47 P2 118.43(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 C9 O1 C1 O2 -78.96(11) . . . . ? C9 O1 C1 C2 40.26(11) . . . . ? C9 O1 C1 C13 160.83(8) . . . . ? O1 C1 O2 C20 -75.95(11) . . . . ? C2 C1 O2 C20 162.87(8) . . . . ? C13 C1 O2 C20 42.29(11) . . . . ? O2 C1 C2 C3 69.02(12) . . . . ? O1 C1 C2 C3 -50.99(13) . . . . ? C13 C1 C2 C3 -170.02(10) . . . . ? C1 C2 C3 C4 33.94(14) . . . . ? C1 C2 C3 C10 -88.99(12) . . . . ? C1 C2 C3 C11 152.43(11) . . . . ? C10 C3 C4 C9 116.56(12) . . . . ? C2 C3 C4 C9 -7.35(14) . . . . ? C11 C3 C4 C9 -124.14(12) . . . . ? C10 C3 C4 C5 -64.00(13) . . . . ? C2 C3 C4 C5 172.09(9) . . . . ? C11 C3 C4 C5 55.31(15) . . . . ? C9 C4 C5 C6 2.52(17) . . . . ? C3 C4 C5 C6 -176.95(11) . . . . ? C4 C5 C6 C7 0.30(18) . . . . ? C4 C5 C6 C12 -179.23(11) . . . . ? C5 C6 C7 C8 -2.21(18) . . . . ? C12 C6 C7 C8 177.33(12) . . . . ? C6 C7 C8 C9 1.21(17) . . . . ? C6 C7 C8 P1 -177.60(9) . . . . ? C24 P1 C8 C7 -18.38(10) . . . . ? C35 P1 C8 C7 81.44(10) . . . . ? C24 P1 C8 C9 162.82(8) . . . . ? C35 P1 C8 C9 -97.36(9) . . . . ? C1 O1 C9 C4 -14.90(13) . . . . ? C1 O1 C9 C8 166.39(9) . . . . ? C5 C4 C9 O1 177.83(9) . . . . ? C3 C4 C9 O1 -2.71(16) . . . . ? C5 C4 C9 C8 -3.53(15) . . . . ? C3 C4 C9 C8 175.92(10) . . . . ? C7 C8 C9 O1 -179.52(9) . . . . ? P1 C8 C9 O1 -0.67(13) . . . . ? C7 C8 C9 C4 1.75(16) . . . . ? P1 C8 C9 C4 -179.40(8) . . . . ? O2 C1 C13 C14 -56.08(12) . . . . ? O1 C1 C13 C14 63.28(12) . . . . ? C2 C1 C13 C14 -175.44(10) . . . . ? C1 C13 C14 C15 38.19(13) . . . . ? C1 C13 C14 C22 -84.38(11) . . . . ? C1 C13 C14 C21 157.49(10) . . . . ? C13 C14 C15 C20 -9.37(13) . . . . ? C22 C14 C15 C20 113.88(12) . . . . ? C21 C14 C15 C20 -126.68(11) . . . . ? C13 C14 C15 C16 171.76(9) . . . . ? C22 C14 C15 C16 -64.99(13) . . . . ? C21 C14 C15 C16 54.45(14) . . . . ? C20 C15 C16 C17 1.43(17) . . . . ? C14 C15 C16 C17 -179.65(10) . . . . ? C15 C16 C17 C18 2.80(17) . . . . ? C15 C16 C17 C23 -175.02(11) . . . . ? C16 C17 C18 C19 -3.36(17) . . . . ? C23 C17 C18 C19 174.42(11) . . . . ? C17 C18 C19 C20 -0.31(16) . . . . ? C17 C18 C19 P2 177.48(9) . . . . ? C47 P2 C19 C18 -18.80(10) . . . . ? C36 P2 C19 C18 81.99(10) . . . . ? C47 P2 C19 C20 158.98(8) . . . . ? C36 P2 C19 C20 -100.23(8) . . . . ? C1 O2 C20 C15 -14.67(13) . . . . ? C1 O2 C20 C19 166.52(8) . . . . ? C16 C15 C20 O2 175.98(10) . . . . ? C14 C15 C20 O2 -2.92(15) . . . . ? C16 C15 C20 C19 -5.28(15) . . . . ? C14 C15 C20 C19 175.83(10) . . . . ? C18 C19 C20 O2 -176.41(9) . . . . ? P2 C19 C20 O2 5.70(12) . . . . ? C18 C19 C20 C15 4.75(15) . . . . ? P2 C19 C20 C15 -173.14(8) . . . . ? C35 P1 C24 C29 -15.33(12) . . . . ? C8 P1 C24 C29 85.87(11) . . . . ? C35 P1 C24 C25 162.54(11) . . . . ? C8 P1 C24 C25 -96.26(11) . . . . ? C29 C24 C25 C26 -0.7(2) . . . . ? P1 C24 C25 C26 -178.68(11) . . . . ? C24 C25 C26 C27 0.7(2) . . . . ? C25 C26 C27 C28 -0.1(2) . . . . ? C26 C27 C28 C29 -0.4(2) . . . . ? C30 O3 C29 C28 -155.38(12) . . . . ? C30 O3 C29 C24 26.6(2) . . . . ? C27 C28 C29 O3 -177.64(13) . . . . ? C27 C28 C29 C24 0.4(2) . . . . ? C25 C24 C29 O3 178.02(12) . . . . ? P1 C24 C29 O3 -4.07(19) . . . . ? C25 C24 C29 C28 0.13(19) . . . . ? P1 C24 C29 C28 178.04(10) . . . . ? C29 O3 C30 C31 157.20(13) . . . . ? C29 O3 C30 C35 -23.3(2) . . . . ? O3 C30 C31 C32 -178.96(15) . . . . ? C35 C30 C31 C32 1.5(2) . . . . ? C30 C31 C32 C33 -0.7(3) . . . . ? C31 C32 C33 C34 -0.3(3) . . . . ? C32 C33 C34 C35 0.5(2) . . . . ? C33 C34 C35 C30 0.2(2) . . . . ? C33 C34 C35 P1 -178.42(12) . . . . ? O3 C30 C35 C34 179.29(14) . . . . ? C31 C30 C35 C34 -1.2(2) . . . . ? O3 C30 C35 P1 -2.1(2) . . . . ? C31 C30 C35 P1 177.38(11) . . . . ? C24 P1 C35 C34 -163.29(12) . . . . ? C8 P1 C35 C34 93.17(12) . . . . ? C24 P1 C35 C30 18.14(13) . . . . ? C8 P1 C35 C30 -85.39(12) . . . . ? C47 P2 C36 C37 178.15(11) . . . . ? C19 P2 C36 C37 75.33(12) . . . . ? C47 P2 C36 C41 -5.84(12) . . . . ? C19 P2 C36 C41 -108.66(11) . . . . ? C41 C36 C37 C38 0.4(2) . . . . ? P2 C36 C37 C38 176.66(13) . . . . ? C36 C37 C38 C39 -0.4(2) . . . . ? C37 C38 C39 C40 0.4(2) . . . . ? C38 C39 C40 C41 -0.5(2) . . . . ? C42 O4 C41 C36 2.5(2) . . . . ? C42 O4 C41 C40 -177.69(12) . . . . ? C37 C36 C41 O4 179.32(13) . . . . ? P2 C36 C41 O4 3.28(19) . . . . ? C37 C36 C41 C40 -0.5(2) . . . . ? P2 C36 C41 C40 -176.55(11) . . . . ? C39 C40 C41 O4 -179.28(14) . . . . ? C39 C40 C41 C36 0.6(2) . . . . ? C41 O4 C42 C47 -3.9(2) . . . . ? C41 O4 C42 C43 176.56(12) . . . . ? O4 C42 C43 C44 178.34(13) . . . . ? C47 C42 C43 C44 -1.2(2) . . . . ? C42 C43 C44 C45 0.0(2) . . . . ? C43 C44 C45 C46 0.7(2) . . . . ? C44 C45 C46 C47 -0.1(2) . . . . ? O4 C42 C47 C46 -177.75(13) . . . . ? C43 C42 C47 C46 1.75(19) . . . . ? O4 C42 C47 P2 -0.57(19) . . . . ? C43 C42 C47 P2 178.93(10) . . . . ? C45 C46 C47 C42 -1.1(2) . . . . ? C45 C46 C47 P2 -178.46(11) . . . . ? C36 P2 C47 C42 4.64(12) . . . . ? C19 P2 C47 C42 108.37(11) . . . . ? C36 P2 C47 C46 -178.22(11) . . . . ? C19 P2 C47 C46 -74.48(11) . . . . ? _diffrn_measured_fraction_theta_max 0.491 _diffrn_reflns_theta_full 39.50 _diffrn_measured_fraction_theta_full 0.491 _refine_diff_density_max 0.424 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.048 #===END data_xr-023_0m _database_code_depnum_ccdc_archive 'CCDC 286685' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H62 O2 P2' _chemical_formula_weight 624.83 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 39.0066(13) _cell_length_b 11.6480(5) _cell_length_c 16.9525(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.8800(10) _cell_angle_gamma 90.00 _cell_volume 7537.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6817 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 39.24 _exptl_crystal_description Block _exptl_crystal_colour translucent _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.101 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7870 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2.1 2003 Bruker-Nonius Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_special_details ; It should be noted that the esd's of the cell dimensions are probably too low; they should be multiplied by a factor of 2 to 10 ; _diffrn_ambient_temperature 100(2) _diffrn_measurement_specimen_suppport 'magnetic support whith 10 micron nylon fiber cryoloop' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_source 'rotating anode X-ray tube' _diffrn_source_type 'Bruker-Nonius FR 591' _diffrn_source_power 50 _diffrn_source_current 90 _diffrn_source_size '3 mm x 0.3 mm fine focus' _diffrn_radiation_monochromator 'Multilayer Montel 200 mirrors' _diffrn_detector_type '4K CCD area detector APEX II' _diffrn_measurement_device_type 'Kappa 4-axis goniometer bruker-nonius' _diffrn_measurement_method ; Fullsphere data collection, phi and omega scans ; _diffrn_detector_area_resol_mean 512 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 60102 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0574 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 69 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 39.49 _reflns_number_total 20428 _reflns_number_gt 16738 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker-Nonius Apex v1.0-22 2002' _computing_cell_refinement 'Bruker-Nonius Apex v1.0-22 2002' _computing_data_reduction 'SAINT+ Version 7.06A Bruker-Nonius, 2004' _computing_structure_solution 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_structure_refinement 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_molecular_graphics 'Shelxtl Version 6.12 (Sheldrick, 2001)' _computing_publication_material 'Shelxtl Version 6.12 (Sheldrick, 2001)' _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^)+(0.0578P)^2^+2.1080P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20428 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0417 _refine_ls_wR_factor_ref 0.1223 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 P1 P 0.171933(4) 0.438814(16) 0.378648(10) 0.01282(4) Uani 1 1 d . . . O1 O 0.144648(12) 0.63539(4) 0.27890(3) 0.01269(8) Uani 1 1 d . . . C1 C 0.135485(15) 0.74991(6) 0.25272(3) 0.01114(9) Uani 1 1 d . . . P2 P 0.077701(4) 0.847034(16) 0.428749(10) 0.01341(4) Uani 1 1 d . . . O2 O 0.120475(11) 0.80843(5) 0.31105(3) 0.01293(8) Uani 1 1 d . . . C2 C 0.107596(16) 0.74661(6) 0.17586(3) 0.01373(10) Uani 1 1 d . . . H2A H 0.1174 0.7087 0.1332 0.016 Uiso 1 1 calc R . . H2B H 0.1015 0.8263 0.1582 0.016 Uiso 1 1 calc R . . C3 C 0.073813(15) 0.68281(6) 0.18467(3) 0.01254(10) Uani 1 1 d . . . C4 C 0.082415(15) 0.59154(6) 0.25055(4) 0.01299(10) Uani 1 1 d . . . C5 C 0.055613(16) 0.52610(7) 0.27157(4) 0.01716(12) Uani 1 1 d . . . H5A H 0.0320 0.5432 0.2470 0.021 Uiso 1 1 calc R . . C6 C 0.062249(17) 0.43672(7) 0.32719(5) 0.01962(13) Uani 1 1 d . . . C7 C 0.097134(17) 0.40810(7) 0.35866(4) 0.01805(12) Uani 1 1 d . . . H7A H 0.1020 0.3431 0.3930 0.022 Uiso 1 1 calc R . . C8 C 0.125142(15) 0.47179(6) 0.34148(4) 0.01417(10) Uani 1 1 d . . . C9 C 0.116868(15) 0.56730(6) 0.28992(3) 0.01219(10) Uani 1 1 d . . . C10 C 0.046309(17) 0.76791(7) 0.20315(4) 0.01724(12) Uani 1 1 d . . . H10A H 0.0240 0.7279 0.2002 0.026 Uiso 1 1 calc R . . H10B H 0.0432 0.8304 0.1636 0.026 Uiso 1 1 calc R . . H10C H 0.0543 0.7996 0.2574 0.026 Uiso 1 1 calc R . . C11 C 0.058713(19) 0.62346(7) 0.10369(4) 0.01824(12) Uani 1 1 d . . . H11A H 0.0374 0.5815 0.1079 0.027 Uiso 1 1 calc R . . H11B H 0.0760 0.5697 0.0906 0.027 Uiso 1 1 calc R . . H11C H 0.0531 0.6815 0.0611 0.027 Uiso 1 1 calc R . . C12 C 0.03263(2) 0.37214(9) 0.35244(6) 0.0320(2) Uani 1 1 d . . . H12A H 0.0122 0.4227 0.3477 0.048 Uiso 1 1 calc R . . H12B H 0.0401 0.3468 0.4085 0.048 Uiso 1 1 calc R . . H12C H 0.0264 0.3051 0.3175 0.048 Uiso 1 1 calc R . . C13 C 0.168803(16) 0.81014(6) 0.24180(3) 0.01325(10) Uani 1 1 d . . . H13A H 0.1624 0.8865 0.2175 0.016 Uiso 1 1 calc R . . H13B H 0.1793 0.7653 0.2032 0.016 Uiso 1 1 calc R . . C14 C 0.196656(15) 0.82658(6) 0.31981(3) 0.01250(10) Uani 1 1 d . . . C15 C 0.178611(15) 0.85175(6) 0.38967(3) 0.01208(10) Uani 1 1 d . . . C16 C 0.198311(16) 0.88891(6) 0.46371(4) 0.01464(11) Uani 1 1 d . . . H16A H 0.2230 0.8957 0.4699 0.018 Uiso 1 1 calc R . . C17 C 0.183055(16) 0.91628(7) 0.52865(4) 0.01518(11) Uani 1 1 d . . . C18 C 0.146775(16) 0.90402(7) 0.51888(4) 0.01553(11) Uani 1 1 d . . . H18A H 0.1361 0.9225 0.5628 0.019 Uiso 1 1 calc R . . C19 C 0.125693(15) 0.86557(6) 0.44690(4) 0.01325(10) Uani 1 1 d . . . C20 C 0.142421(15) 0.83995(6) 0.38251(3) 0.01172(10) Uani 1 1 d . . . C21 C 0.220231(17) 0.72018(7) 0.33897(4) 0.01681(12) Uani 1 1 d . . . H21A H 0.2060 0.6540 0.3481 0.025 Uiso 1 1 calc R . . H21B H 0.2382 0.7346 0.3875 0.025 Uiso 1 1 calc R . . H21C H 0.2315 0.7041 0.2935 0.025 Uiso 1 1 calc R . . C22 C 0.219804(18) 0.92929(7) 0.30655(4) 0.01755(12) Uani 1 1 d . . . H22A H 0.2387 0.9390 0.3541 0.026 Uiso 1 1 calc R . . H22B H 0.2055 0.9992 0.2981 0.026 Uiso 1 1 calc R . . H22C H 0.2299 0.9150 0.2591 0.026 Uiso 1 1 calc R . . C23 C 0.204630(19) 0.96137(8) 0.60640(4) 0.02051(13) Uani 1 1 d . . . H23A H 0.2294 0.9638 0.6026 0.031 Uiso 1 1 calc R . . H23B H 0.2019 0.9108 0.6509 0.031 Uiso 1 1 calc R . . H23C H 0.1967 1.0389 0.6164 0.031 Uiso 1 1 calc R . . C24 C 0.175604(17) 0.37257(7) 0.48242(4) 0.01657(11) Uani 1 1 d . . . C25 C 0.15547(2) 0.45234(8) 0.52938(5) 0.02456(15) Uani 1 1 d . . . H25A H 0.1616 0.4336 0.5869 0.037 Uiso 1 1 calc R . . H25B H 0.1302 0.4419 0.5098 0.037 Uiso 1 1 calc R . . H25C H 0.1617 0.5323 0.5213 0.037 Uiso 1 1 calc R . . C26 C 0.21479(2) 0.38354(9) 0.52235(4) 0.02426(15) Uani 1 1 d . . . H26A H 0.2185 0.3576 0.5785 0.036 Uiso 1 1 calc R . . H26B H 0.2221 0.4639 0.5209 0.036 Uiso 1 1 calc R . . H26C H 0.2287 0.3361 0.4930 0.036 Uiso 1 1 calc R . . C27 C 0.16435(2) 0.24788(7) 0.49060(4) 0.02164(14) Uani 1 1 d . . . H27A H 0.1669 0.2287 0.5478 0.032 Uiso 1 1 calc R . . H27B H 0.1792 0.1967 0.4661 0.032 Uiso 1 1 calc R . . H27C H 0.1398 0.2384 0.4631 0.032 Uiso 1 1 calc R . . C28 C 0.178602(17) 0.32429(7) 0.30352(4) 0.01634(11) Uani 1 1 d . . . C29 C 0.215089(18) 0.27152(7) 0.33190(4) 0.02001(13) Uani 1 1 d . . . H29A H 0.2210 0.2248 0.2885 0.030 Uiso 1 1 calc R . . H29B H 0.2152 0.2231 0.3792 0.030 Uiso 1 1 calc R . . H29C H 0.2324 0.3330 0.3461 0.030 Uiso 1 1 calc R . . C30 C 0.15123(2) 0.22859(8) 0.28538(5) 0.02312(14) Uani 1 1 d . . . H30A H 0.1567 0.1783 0.2434 0.035 Uiso 1 1 calc R . . H30B H 0.1280 0.2624 0.2667 0.035 Uiso 1 1 calc R . . H30C H 0.1514 0.1838 0.3344 0.035 Uiso 1 1 calc R . . C31 C 0.17843(2) 0.39138(8) 0.22484(4) 0.02455(15) Uani 1 1 d . . . H31A H 0.1834 0.3387 0.1836 0.037 Uiso 1 1 calc R . . H31B H 0.1964 0.4515 0.2350 0.037 Uiso 1 1 calc R . . H31C H 0.1554 0.4266 0.2060 0.037 Uiso 1 1 calc R . . C32 C 0.068474(19) 0.78444(7) 0.52595(4) 0.01994(13) Uani 1 1 d . . . C33 C 0.09432(3) 0.68417(9) 0.54798(6) 0.02971(18) Uani 1 1 d . . . H33A H 0.0877 0.6384 0.5910 0.045 Uiso 1 1 calc R . . H33B H 0.1181 0.7145 0.5666 0.045 Uiso 1 1 calc R . . H33C H 0.0937 0.6358 0.5004 0.045 Uiso 1 1 calc R . . C34 C 0.06943(2) 0.86000(9) 0.60082(5) 0.02644(17) Uani 1 1 d . . . H34A H 0.0651 0.8124 0.6454 0.040 Uiso 1 1 calc R . . H34B H 0.0513 0.9194 0.5884 0.040 Uiso 1 1 calc R . . H34C H 0.0925 0.8963 0.6163 0.040 Uiso 1 1 calc R . . C35 C 0.03138(2) 0.73265(9) 0.50173(6) 0.03027(19) Uani 1 1 d . . . H35A H 0.0258 0.6906 0.5476 0.045 Uiso 1 1 calc R . . H35B H 0.0305 0.6800 0.4563 0.045 Uiso 1 1 calc R . . H35C H 0.0143 0.7944 0.4860 0.045 Uiso 1 1 calc R . . C36 C 0.062971(17) 1.00221(6) 0.41516(4) 0.01577(11) Uani 1 1 d . . . C37 C 0.02276(2) 1.00359(8) 0.39548(6) 0.02537(16) Uani 1 1 d . . . H37A H 0.0145 1.0818 0.3813 0.038 Uiso 1 1 calc R . . H37B H 0.0140 0.9777 0.4426 0.038 Uiso 1 1 calc R . . H37C H 0.0142 0.9521 0.3500 0.038 Uiso 1 1 calc R . . C38 C 0.07642(2) 1.08545(8) 0.48458(5) 0.02529(15) Uani 1 1 d . . . H38A H 0.0707 1.1644 0.4665 0.038 Uiso 1 1 calc R . . H38B H 0.1019 1.0774 0.5018 0.038 Uiso 1 1 calc R . . H38C H 0.0653 1.0679 0.5299 0.038 Uiso 1 1 calc R . . C39 C 0.07589(2) 1.04457(8) 0.34022(5) 0.02319(14) Uani 1 1 d . . . H39A H 0.0668 1.1219 0.3260 0.035 Uiso 1 1 calc R . . H39B H 0.0676 0.9923 0.2950 0.035 Uiso 1 1 calc R . . H39C H 0.1016 1.0465 0.3520 0.035 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 P1 0.00991(6) 0.01344(9) 0.01496(6) 0.00266(5) 0.00218(5) 0.00078(5) O1 0.01032(15) 0.0120(2) 0.01630(17) 0.00289(15) 0.00397(14) 0.00059(14) C1 0.01182(19) 0.0120(3) 0.01032(18) 0.00063(17) 0.00388(16) 0.00077(17) P2 0.01139(6) 0.01468(9) 0.01536(7) -0.00240(5) 0.00555(5) -0.00044(5) O2 0.01045(15) 0.0169(2) 0.01165(16) -0.00313(15) 0.00284(13) 0.00140(15) C2 0.0143(2) 0.0161(3) 0.01073(19) 0.00153(18) 0.00255(17) -0.00042(19) C3 0.0122(2) 0.0135(3) 0.01163(19) 0.00154(18) 0.00165(16) 0.00102(18) C4 0.01062(19) 0.0142(3) 0.0141(2) 0.00283(19) 0.00231(16) 0.00107(18) C5 0.0101(2) 0.0198(4) 0.0211(3) 0.0069(2) 0.00207(19) 0.0001(2) C6 0.0110(2) 0.0222(4) 0.0256(3) 0.0101(3) 0.0035(2) -0.0003(2) C7 0.0122(2) 0.0191(4) 0.0226(3) 0.0091(2) 0.0028(2) 0.0002(2) C8 0.01038(19) 0.0152(3) 0.0169(2) 0.0041(2) 0.00263(17) 0.00105(19) C9 0.01004(19) 0.0131(3) 0.0137(2) 0.00209(18) 0.00293(16) 0.00060(17) C10 0.0151(2) 0.0176(3) 0.0187(2) 0.0012(2) 0.0027(2) 0.0047(2) C11 0.0187(2) 0.0207(4) 0.0141(2) -0.0015(2) 0.0007(2) -0.0018(2) C12 0.0135(3) 0.0368(5) 0.0451(5) 0.0247(4) 0.0048(3) -0.0018(3) C13 0.0133(2) 0.0158(3) 0.01158(19) 0.00089(18) 0.00466(17) -0.00160(19) C14 0.01065(19) 0.0157(3) 0.01209(19) 0.00034(18) 0.00459(16) -0.00073(18) C15 0.01075(19) 0.0144(3) 0.01179(19) 0.00001(18) 0.00391(16) 0.00049(18) C16 0.0116(2) 0.0194(3) 0.0132(2) -0.0014(2) 0.00328(17) 0.0001(2) C17 0.0137(2) 0.0191(3) 0.0127(2) -0.0023(2) 0.00268(17) 0.0009(2) C18 0.0141(2) 0.0205(3) 0.0128(2) -0.0032(2) 0.00462(18) 0.0006(2) C19 0.0116(2) 0.0160(3) 0.0132(2) -0.00200(19) 0.00499(17) 0.00040(18) C20 0.01068(19) 0.0136(3) 0.01126(19) -0.00107(17) 0.00326(16) 0.00082(18) C21 0.0133(2) 0.0196(4) 0.0185(2) 0.0009(2) 0.00557(19) 0.0030(2) C22 0.0164(2) 0.0204(4) 0.0166(2) 0.0014(2) 0.0055(2) -0.0053(2) C23 0.0173(2) 0.0283(4) 0.0148(2) -0.0058(2) 0.0007(2) 0.0017(2) C24 0.0158(2) 0.0195(3) 0.0142(2) 0.0016(2) 0.00269(18) 0.0033(2) C25 0.0265(3) 0.0291(5) 0.0193(3) -0.0020(3) 0.0078(3) 0.0060(3) C26 0.0179(3) 0.0334(5) 0.0187(3) 0.0005(3) -0.0027(2) 0.0033(3) C27 0.0241(3) 0.0221(4) 0.0194(3) 0.0080(2) 0.0060(2) 0.0030(3) C28 0.0148(2) 0.0195(3) 0.0152(2) 0.0011(2) 0.00433(19) 0.0014(2) C29 0.0162(2) 0.0215(4) 0.0233(3) 0.0004(2) 0.0065(2) 0.0043(2) C30 0.0214(3) 0.0250(4) 0.0228(3) -0.0053(3) 0.0042(2) -0.0039(3) C31 0.0276(3) 0.0310(5) 0.0169(3) 0.0049(3) 0.0088(2) 0.0049(3) C32 0.0174(2) 0.0221(4) 0.0223(3) 0.0037(2) 0.0087(2) -0.0009(2) C33 0.0286(4) 0.0235(5) 0.0384(4) 0.0109(3) 0.0102(3) 0.0034(3) C34 0.0248(3) 0.0376(5) 0.0198(3) 0.0018(3) 0.0112(3) 0.0005(3) C35 0.0215(3) 0.0355(5) 0.0358(4) 0.0063(4) 0.0107(3) -0.0091(3) C36 0.0142(2) 0.0153(3) 0.0188(2) -0.0014(2) 0.00572(19) 0.0007(2) C37 0.0153(3) 0.0262(4) 0.0352(4) 0.0022(3) 0.0066(3) 0.0040(3) C38 0.0316(4) 0.0177(4) 0.0257(3) -0.0056(3) 0.0036(3) 0.0017(3) C39 0.0268(3) 0.0203(4) 0.0253(3) 0.0042(3) 0.0121(3) 0.0013(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 P1 C8 1.8445(6) . ? P1 C28 1.8989(7) . ? P1 C24 1.8992(7) . ? O1 C9 1.3861(7) . ? O1 C1 1.4279(8) . ? C1 O2 1.4226(7) . ? C1 C2 1.5162(9) . ? C1 C13 1.5213(8) . ? P2 C19 1.8462(6) . ? P2 C36 1.8962(8) . ? P2 C32 1.9028(7) . ? O2 C20 1.3814(7) . ? C2 C3 1.5467(9) . ? C3 C4 1.5282(9) . ? C3 C10 1.5395(9) . ? C3 C11 1.5416(9) . ? C4 C5 1.3980(9) . ? C4 C9 1.4007(8) . ? C5 C6 1.3927(10) . ? C6 C7 1.3959(9) . ? C6 C12 1.5123(10) . ? C7 C8 1.3999(9) . ? C8 C9 1.4106(9) . ? C13 C14 1.5408(9) . ? C14 C15 1.5255(7) . ? C14 C21 1.5376(10) . ? C14 C22 1.5430(9) . ? C15 C20 1.3986(8) . ? C15 C16 1.3986(9) . ? C16 C17 1.3920(8) . ? C17 C18 1.3978(9) . ? C17 C23 1.5048(9) . ? C18 C19 1.3974(9) . ? C19 C20 1.4139(8) . ? C24 C27 1.5318(11) . ? C24 C25 1.5398(10) . ? C24 C26 1.5443(10) . ? C28 C30 1.5304(11) . ? C28 C29 1.5339(10) . ? C28 C31 1.5448(10) . ? C32 C33 1.5379(12) . ? C32 C34 1.5386(12) . ? C32 C35 1.5432(11) . ? C36 C38 1.5318(11) . ? C36 C37 1.5349(10) . ? C36 C39 1.5412(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 C8 P1 C28 100.35(3) . . ? C8 P1 C24 106.36(3) . . ? C28 P1 C24 109.95(3) . . ? C9 O1 C1 115.08(5) . . ? O2 C1 O1 110.12(4) . . ? O2 C1 C2 106.52(5) . . ? O1 C1 C2 109.44(5) . . ? O2 C1 C13 110.35(5) . . ? O1 C1 C13 107.65(5) . . ? C2 C1 C13 112.77(5) . . ? C19 P2 C36 100.38(3) . . ? C19 P2 C32 105.46(3) . . ? C36 P2 C32 111.34(3) . . ? C20 O2 C1 117.88(4) . . ? C1 C2 C3 113.83(5) . . ? C4 C3 C10 110.89(5) . . ? C4 C3 C11 108.96(6) . . ? C10 C3 C11 108.39(5) . . ? C4 C3 C2 109.97(5) . . ? C10 C3 C2 110.70(6) . . ? C11 C3 C2 107.84(5) . . ? C5 C4 C9 117.59(6) . . ? C5 C4 C3 120.16(5) . . ? C9 C4 C3 122.22(5) . . ? C6 C5 C4 122.39(6) . . ? C5 C6 C7 117.90(6) . . ? C5 C6 C12 121.14(6) . . ? C7 C6 C12 120.96(7) . . ? C6 C7 C8 122.35(6) . . ? C7 C8 C9 117.26(6) . . ? C7 C8 P1 125.33(5) . . ? C9 C8 P1 117.39(4) . . ? O1 C9 C4 121.36(6) . . ? O1 C9 C8 116.70(5) . . ? C4 C9 C8 121.93(6) . . ? C1 C13 C14 114.96(5) . . ? C15 C14 C21 110.02(5) . . ? C15 C14 C13 109.49(5) . . ? C21 C14 C13 111.50(6) . . ? C15 C14 C22 109.96(5) . . ? C21 C14 C22 108.26(5) . . ? C13 C14 C22 107.56(5) . . ? C20 C15 C16 117.81(5) . . ? C20 C15 C14 122.18(5) . . ? C16 C15 C14 120.01(5) . . ? C17 C16 C15 122.37(5) . . ? C16 C17 C18 118.04(6) . . ? C16 C17 C23 121.30(6) . . ? C18 C17 C23 120.63(5) . . ? C19 C18 C17 122.39(5) . . ? C18 C19 C20 117.36(5) . . ? C18 C19 P2 125.26(4) . . ? C20 C19 P2 117.38(5) . . ? O2 C20 C15 122.30(5) . . ? O2 C20 C19 115.59(5) . . ? C15 C20 C19 122.03(5) . . ? C27 C24 C25 109.82(6) . . ? C27 C24 C26 108.37(6) . . ? C25 C24 C26 106.70(6) . . ? C27 C24 P1 120.05(5) . . ? C25 C24 P1 106.53(5) . . ? C26 C24 P1 104.57(5) . . ? C30 C28 C29 109.58(7) . . ? C30 C28 C31 108.44(6) . . ? C29 C28 C31 108.20(5) . . ? C30 C28 P1 117.40(4) . . ? C29 C28 P1 108.51(5) . . ? C31 C28 P1 104.29(5) . . ? C33 C32 C34 109.32(7) . . ? C33 C32 C35 107.44(8) . . ? C34 C32 C35 107.77(6) . . ? C33 C32 P2 105.65(5) . . ? C34 C32 P2 121.23(6) . . ? C35 C32 P2 104.68(5) . . ? C38 C36 C37 109.47(6) . . ? C38 C36 C39 108.20(7) . . ? C37 C36 C39 108.09(6) . . ? C38 C36 P2 117.56(5) . . ? C37 C36 P2 107.87(5) . . ? C39 C36 P2 105.25(5) . . ? 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 C9 O1 C1 O2 61.15(6) . . . . ? C9 O1 C1 C2 -55.62(6) . . . . ? C9 O1 C1 C13 -178.50(5) . . . . ? O1 C1 O2 C20 72.08(7) . . . . ? C2 C1 O2 C20 -169.34(5) . . . . ? C13 C1 O2 C20 -46.63(7) . . . . ? O2 C1 C2 C3 -60.44(7) . . . . ? O1 C1 C2 C3 58.58(6) . . . . ? C13 C1 C2 C3 178.37(5) . . . . ? C1 C2 C3 C4 -28.01(7) . . . . ? C1 C2 C3 C10 94.88(6) . . . . ? C1 C2 C3 C11 -146.71(6) . . . . ? C10 C3 C4 C5 54.51(8) . . . . ? C11 C3 C4 C5 -64.71(8) . . . . ? C2 C3 C4 C5 177.29(6) . . . . ? C10 C3 C4 C9 -127.68(7) . . . . ? C11 C3 C4 C9 113.10(7) . . . . ? C2 C3 C4 C9 -4.90(8) . . . . ? C9 C4 C5 C6 -2.38(11) . . . . ? C3 C4 C5 C6 175.52(7) . . . . ? C4 C5 C6 C7 -4.05(12) . . . . ? C4 C5 C6 C12 176.28(8) . . . . ? C5 C6 C7 C8 5.49(12) . . . . ? C12 C6 C7 C8 -174.85(9) . . . . ? C6 C7 C8 C9 -0.41(11) . . . . ? C6 C7 C8 P1 -178.74(6) . . . . ? C28 P1 C8 C7 81.68(7) . . . . ? C24 P1 C8 C7 -32.85(7) . . . . ? C28 P1 C8 C9 -96.66(6) . . . . ? C24 P1 C8 C9 148.82(5) . . . . ? C1 O1 C9 C4 23.13(8) . . . . ? C1 O1 C9 C8 -157.90(5) . . . . ? C5 C4 C9 O1 -173.31(6) . . . . ? C3 C4 C9 O1 8.83(9) . . . . ? C5 C4 C9 C8 7.78(10) . . . . ? C3 C4 C9 C8 -170.08(6) . . . . ? C7 C8 C9 O1 174.61(6) . . . . ? P1 C8 C9 O1 -6.92(8) . . . . ? C7 C8 C9 C4 -6.43(10) . . . . ? P1 C8 C9 C4 172.04(5) . . . . ? O2 C1 C13 C14 55.25(7) . . . . ? O1 C1 C13 C14 -64.95(7) . . . . ? C2 C1 C13 C14 174.23(6) . . . . ? C1 C13 C14 C15 -36.30(8) . . . . ? C1 C13 C14 C21 85.69(6) . . . . ? C1 C13 C14 C22 -155.76(6) . . . . ? C21 C14 C15 C20 -112.62(7) . . . . ? C13 C14 C15 C20 10.26(9) . . . . ? C22 C14 C15 C20 128.23(7) . . . . ? C21 C14 C15 C16 67.94(8) . . . . ? C13 C14 C15 C16 -169.19(6) . . . . ? C22 C14 C15 C16 -51.21(8) . . . . ? C20 C15 C16 C17 -1.38(11) . . . . ? C14 C15 C16 C17 178.09(7) . . . . ? C15 C16 C17 C18 0.99(11) . . . . ? C15 C16 C17 C23 -177.08(7) . . . . ? C16 C17 C18 C19 0.06(11) . . . . ? C23 C17 C18 C19 178.15(7) . . . . ? C17 C18 C19 C20 -0.65(11) . . . . ? C17 C18 C19 P2 -179.94(6) . . . . ? C36 P2 C19 C18 76.00(7) . . . . ? C32 P2 C19 C18 -39.75(7) . . . . ? C36 P2 C19 C20 -103.30(6) . . . . ? C32 P2 C19 C20 140.95(6) . . . . ? C1 O2 C20 C15 21.53(9) . . . . ? C1 O2 C20 C19 -161.75(6) . . . . ? C16 C15 C20 O2 177.26(6) . . . . ? C14 C15 C20 O2 -2.20(10) . . . . ? C16 C15 C20 C19 0.75(10) . . . . ? C14 C15 C20 C19 -178.71(6) . . . . ? C18 C19 C20 O2 -176.50(6) . . . . ? P2 C19 C20 O2 2.85(8) . . . . ? C18 C19 C20 C15 0.23(10) . . . . ? P2 C19 C20 C15 179.58(5) . . . . ? C8 P1 C24 C27 76.45(6) . . . . ? C28 P1 C24 C27 -31.36(6) . . . . ? C8 P1 C24 C25 -49.02(6) . . . . ? C28 P1 C24 C25 -156.83(5) . . . . ? C8 P1 C24 C26 -161.79(5) . . . . ? C28 P1 C24 C26 90.41(6) . . . . ? C8 P1 C28 C30 -46.60(6) . . . . ? C24 P1 C28 C30 65.17(6) . . . . ? C8 P1 C28 C29 -171.46(5) . . . . ? C24 P1 C28 C29 -59.69(5) . . . . ? C8 P1 C28 C31 73.38(5) . . . . ? C24 P1 C28 C31 -174.85(5) . . . . ? C19 P2 C32 C33 -48.48(7) . . . . ? C36 P2 C32 C33 -156.47(6) . . . . ? C19 P2 C32 C34 76.38(7) . . . . ? C36 P2 C32 C34 -31.60(7) . . . . ? C19 P2 C32 C35 -161.76(6) . . . . ? C36 P2 C32 C35 90.26(6) . . . . ? C19 P2 C36 C38 -58.11(6) . . . . ? C32 P2 C36 C38 53.14(6) . . . . ? C19 P2 C36 C37 177.60(5) . . . . ? C32 P2 C36 C37 -71.15(6) . . . . ? C19 P2 C36 C39 62.38(5) . . . . ? C32 P2 C36 C39 173.64(5) . . . . ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 39.49 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.691 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.068 #===END