# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Freixa, Zoraida' _publ_contact_author_email zfreixa@iciq.es _publ_section_title ; An Approach to Bimetallic Catalysts by Ligand Design ; loop_ _publ_author_name J.M.Lopez-Valbuena E.Escudero J.Benet-Buchholz Z.Freixa ; P.W.N.Van Leeuwen ; # Attachment '- 17 -19-20-22-24.cif' data_jm045p21c_17 _database_code_depnum_ccdc_archive 'CCDC 762010' #TrackingRef '- 17 -19-20-22-24.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H76 Cl14 O6 P4 Rh2' _chemical_formula_weight 2079.51 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 16.6357(4) _cell_length_b 18.7449(5) _cell_length_c 14.8117(4) _cell_angle_alpha 90.00 _cell_angle_beta 100.5780(10) _cell_angle_gamma 90.00 _cell_volume 4540.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9892 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 39.51 _exptl_crystal_description Block _exptl_crystal_colour colourless _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 1.521 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2104 _exptl_absorpt_coefficient_mu 0.898 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9601 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2008/1 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 70 _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_reflns_number 90973 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0227 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 39.65 _reflns_number_total 26435 _reflns_number_gt 22591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. 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^)+(0.0519P)^2^+3.4554P] 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 26435 _refine_ls_number_parameters 527 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0435 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.1021 _refine_ls_wR_factor_gt 0.0955 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 1.196000(4) 0.550045(4) 0.105490(5) 0.01116(2) Uani 1 1 d . . . P1 P 1.314337(16) 0.512664(15) 0.058169(18) 0.01143(4) Uani 1 1 d . . . Cl1 Cl 1.265657(17) 0.535082(18) 0.259601(18) 0.01888(5) Uani 1 1 d . . . C1 C 1.14411(6) 0.55566(6) -0.01302(7) 0.01390(15) Uani 1 1 d . . . O1 O 1.11075(6) 0.55729(5) -0.08836(6) 0.01865(15) Uani 1 1 d . . . P2 P 1.088002(16) 0.611833(15) 0.150435(19) 0.01194(4) Uani 1 1 d . . . C2 C 1.39514(6) 0.57424(6) 0.10731(7) 0.01427(15) Uani 1 1 d . . . O2 O 1.21469(5) 0.42198(4) -0.09465(5) 0.01363(12) Uani 1 1 d . . . C3 C 1.37802(7) 0.64743(6) 0.09641(9) 0.01926(18) Uani 1 1 d . . . H3 H 1.3264 0.6627 0.0634 0.023 Uiso 1 1 calc R . . O3 O 1.10113(5) 0.36210(4) -0.17403(6) 0.01412(12) Uani 1 1 d . . . C4 C 1.43620(9) 0.69773(7) 0.13371(11) 0.0249(2) Uani 1 1 d . . . H4 H 1.4246 0.7472 0.1258 0.030 Uiso 1 1 calc R . . C5 C 1.51177(9) 0.67522(9) 0.18278(10) 0.0274(3) Uani 1 1 d . . . H5 H 1.5516 0.7095 0.2083 0.033 Uiso 1 1 calc R . . C6 C 1.52885(8) 0.60267(9) 0.19448(10) 0.0259(2) Uani 1 1 d . . . H6 H 1.5802 0.5875 0.2282 0.031 Uiso 1 1 calc R . . C7 C 1.47061(7) 0.55222(7) 0.15661(9) 0.01925(19) Uani 1 1 d . . . H7 H 1.4824 0.5028 0.1644 0.023 Uiso 1 1 calc R . . C8 C 1.35143(6) 0.42191(6) 0.08357(7) 0.01356(15) Uani 1 1 d . . . C9 C 1.32069(8) 0.38124(6) 0.14835(9) 0.01879(18) Uani 1 1 d . . . H9 H 1.2850 0.4023 0.1840 0.023 Uiso 1 1 calc R . . C10 C 1.34237(9) 0.30952(7) 0.16074(11) 0.0246(2) Uani 1 1 d . . . H10 H 1.3214 0.2820 0.2050 0.030 Uiso 1 1 calc R . . C11 C 1.39436(9) 0.27806(7) 0.10898(10) 0.0241(2) Uani 1 1 d . . . H11 H 1.4079 0.2289 0.1168 0.029 Uiso 1 1 calc R . . C12 C 1.42650(9) 0.31875(7) 0.04554(9) 0.0233(2) Uani 1 1 d . . . H12 H 1.4629 0.2976 0.0108 0.028 Uiso 1 1 calc R . . C13 C 1.40540(8) 0.39054(7) 0.03286(8) 0.01888(18) Uani 1 1 d . . . H13 H 1.4277 0.4183 -0.0103 0.023 Uiso 1 1 calc R . . C14 C 1.31426(6) 0.51830(5) -0.06470(7) 0.01262(14) Uani 1 1 d . . . C15 C 1.36162(6) 0.56614(6) -0.10645(7) 0.01429(15) Uani 1 1 d . . . H15 H 1.3983 0.5973 -0.0686 0.017 Uiso 1 1 calc R . . C16 C 1.35646(7) 0.56933(6) -0.20180(8) 0.01549(16) Uani 1 1 d . . . C17 C 1.30096(7) 0.52472(6) -0.25846(7) 0.01606(16) Uani 1 1 d . . . H17 H 1.2955 0.5272 -0.3234 0.019 Uiso 1 1 calc R . . C18 C 1.25425(6) 0.47705(6) -0.21862(7) 0.01362(15) Uani 1 1 d . . . C19 C 1.18988(6) 0.42367(6) -0.25947(7) 0.01443(15) Uani 1 1 d . . . C20 C 1.10426(6) 0.45543(6) -0.27430(7) 0.01469(16) Uani 1 1 d . . . C21 C 1.05774(6) 0.41757(6) -0.22159(7) 0.01327(15) Uani 1 1 d . . . C22 C 1.18478(6) 0.37585(6) -0.17364(7) 0.01388(15) Uani 1 1 d . . . C23 C 1.26238(6) 0.47350(6) -0.12374(7) 0.01251(14) Uani 1 1 d . . . C24 C 1.41151(8) 0.61872(7) -0.24329(9) 0.0221(2) Uani 1 1 d . . . H24A H 1.4600 0.5925 -0.2535 0.033 Uiso 1 1 calc R . . H24B H 1.4283 0.6586 -0.2013 0.033 Uiso 1 1 calc R . . H24C H 1.3819 0.6371 -0.3020 0.033 Uiso 1 1 calc R . . C25 C 1.20812(8) 0.38418(7) -0.34358(8) 0.0209(2) Uani 1 1 d . . . H25A H 1.2062 0.4178 -0.3945 0.031 Uiso 1 1 calc R . . H25B H 1.1672 0.3467 -0.3613 0.031 Uiso 1 1 calc R . . H25C H 1.2626 0.3626 -0.3289 0.031 Uiso 1 1 calc R . . C26 C 1.23154(7) 0.30680(6) -0.15943(9) 0.01942(19) Uani 1 1 d . . . H26A H 1.2254 0.2858 -0.1005 0.029 Uiso 1 1 calc R . . H26B H 1.2896 0.3159 -0.1593 0.029 Uiso 1 1 calc R . . H26C H 1.2102 0.2736 -0.2092 0.029 Uiso 1 1 calc R . . C27 C 1.07091(7) 0.51292(7) -0.32675(8) 0.01896(19) Uani 1 1 d . . . H27 H 1.1027 0.5388 -0.3627 0.023 Uiso 1 1 calc R . . C28 C 1.01613(6) 0.64885(6) 0.05363(7) 0.01379(15) Uani 1 1 d . . . C29 C 0.96133(7) 0.60262(6) -0.00009(8) 0.01671(17) Uani 1 1 d . . . H29 H 0.9607 0.5536 0.0160 0.020 Uiso 1 1 calc R . . C30 C 0.90777(8) 0.62745(7) -0.07676(9) 0.0217(2) Uani 1 1 d . . . H30 H 0.8704 0.5957 -0.1126 0.026 Uiso 1 1 calc R . . C31 C 0.90916(9) 0.69915(8) -0.10086(11) 0.0278(3) Uani 1 1 d . . . H31 H 0.8726 0.7164 -0.1532 0.033 Uiso 1 1 calc R . . C32 C 0.96421(10) 0.74553(8) -0.04830(11) 0.0280(3) Uani 1 1 d . . . H32 H 0.9653 0.7944 -0.0651 0.034 Uiso 1 1 calc R . . C33 C 1.01759(8) 0.72057(6) 0.02874(9) 0.02015(19) Uani 1 1 d . . . H33 H 1.0550 0.7524 0.0644 0.024 Uiso 1 1 calc R . . C34 C 1.12468(7) 0.69043(6) 0.21746(8) 0.01584(16) Uani 1 1 d . . . C35 C 1.07203(8) 0.73321(8) 0.25771(11) 0.0256(3) Uani 1 1 d . . . H35 H 1.0169 0.7189 0.2553 0.031 Uiso 1 1 calc R . . C36 C 1.10003(10) 0.79665(9) 0.30125(14) 0.0347(4) Uani 1 1 d . . . H36 H 1.0636 0.8262 0.3270 0.042 Uiso 1 1 calc R . . C37 C 1.18114(11) 0.81684(10) 0.30711(16) 0.0406(5) Uani 1 1 d . . . H37 H 1.2001 0.8605 0.3361 0.049 Uiso 1 1 calc R . . C38 C 1.23465(10) 0.77314(10) 0.27058(16) 0.0413(5) Uani 1 1 d . . . H38 H 1.2906 0.7860 0.2770 0.050 Uiso 1 1 calc R . . C39 C 1.20644(8) 0.71053(8) 0.22463(11) 0.0262(3) Uani 1 1 d . . . H39 H 1.2428 0.6815 0.1982 0.031 Uiso 1 1 calc R . . C40 C 1.02321(6) 0.56495(6) 0.21816(7) 0.01347(15) Uani 1 1 d . . . C41 C 1.05554(7) 0.50599(7) 0.27196(8) 0.01767(17) Uani 1 1 d . . . H41 H 1.1103 0.4919 0.2713 0.021 Uiso 1 1 calc R . . C42 C 1.01039(7) 0.46751(7) 0.32619(9) 0.0213(2) Uani 1 1 d . . . C43 C 1.04830(9) 0.40515(10) 0.38293(14) 0.0351(4) Uani 1 1 d . . . H43A H 1.1038 0.3971 0.3715 0.053 Uiso 1 1 calc R . . H43B H 1.0152 0.3623 0.3659 0.053 Uiso 1 1 calc R . . H43C H 1.0506 0.4155 0.4482 0.053 Uiso 1 1 calc R . . C1S C 1.37004(9) 0.42271(9) 0.44146(11) 0.0282(3) Uani 1 1 d . . . H1S H 1.3527 0.4698 0.4127 0.034 Uiso 1 1 calc R . . Cl1S Cl 1.41239(4) 0.43677(3) 0.55825(3) 0.04081(10) Uani 1 1 d . . . Cl2S Cl 1.28388(3) 0.36727(3) 0.43088(4) 0.04464(11) Uani 1 1 d . . . Cl3S Cl 1.44332(4) 0.38608(6) 0.38538(4) 0.0769(3) Uani 1 1 d . . . C2S C 1.24856(11) 0.63200(10) 0.45529(12) 0.0333(3) Uani 1 1 d . . . H2S H 1.2291 0.6432 0.3889 0.040 Uiso 1 1 calc R . . Cl4S Cl 1.21985(5) 0.70146(5) 0.52163(8) 0.0829(3) Uani 1 1 d . . . Cl5S Cl 1.20477(4) 0.55040(3) 0.48125(3) 0.04476(11) Uani 1 1 d . . . Cl6S Cl 1.35561(3) 0.62529(3) 0.47641(4) 0.04503(11) 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 0.00996(3) 0.01321(3) 0.01047(3) 0.00012(2) 0.00229(2) 0.00088(2) P1 0.01005(9) 0.01302(10) 0.01134(9) 0.00044(8) 0.00231(7) 0.00065(7) Cl1 0.01605(10) 0.02810(13) 0.01196(9) 0.00008(8) 0.00120(7) 0.00339(9) C1 0.0131(3) 0.0155(4) 0.0134(4) 0.0005(3) 0.0033(3) 0.0016(3) O1 0.0196(4) 0.0226(4) 0.0131(3) 0.0017(3) 0.0014(3) 0.0040(3) P2 0.01081(9) 0.01306(10) 0.01218(10) -0.00082(8) 0.00268(7) 0.00012(7) C2 0.0121(3) 0.0161(4) 0.0148(4) -0.0019(3) 0.0032(3) -0.0006(3) O2 0.0142(3) 0.0146(3) 0.0126(3) -0.0003(2) 0.0040(2) -0.0025(2) C3 0.0184(4) 0.0156(4) 0.0244(5) -0.0026(4) 0.0054(4) -0.0004(3) O3 0.0112(3) 0.0144(3) 0.0170(3) 0.0011(2) 0.0031(2) 0.0005(2) C4 0.0282(6) 0.0185(5) 0.0297(6) -0.0077(4) 0.0096(5) -0.0059(4) C5 0.0254(6) 0.0304(6) 0.0266(6) -0.0107(5) 0.0054(5) -0.0113(5) C6 0.0162(4) 0.0347(7) 0.0251(6) -0.0051(5) -0.0007(4) -0.0048(4) C7 0.0136(4) 0.0240(5) 0.0191(4) -0.0014(4) -0.0001(3) -0.0004(3) C8 0.0131(3) 0.0141(4) 0.0133(3) 0.0007(3) 0.0018(3) 0.0012(3) C9 0.0198(4) 0.0174(4) 0.0204(4) 0.0050(4) 0.0068(4) 0.0026(3) C10 0.0278(6) 0.0176(5) 0.0296(6) 0.0082(4) 0.0080(5) 0.0024(4) C11 0.0292(6) 0.0153(4) 0.0262(6) 0.0013(4) 0.0010(5) 0.0041(4) C12 0.0282(6) 0.0202(5) 0.0215(5) -0.0002(4) 0.0049(4) 0.0093(4) C13 0.0208(4) 0.0190(4) 0.0178(4) 0.0021(4) 0.0060(4) 0.0057(4) C14 0.0113(3) 0.0141(4) 0.0128(3) 0.0009(3) 0.0030(3) 0.0003(3) C15 0.0123(3) 0.0160(4) 0.0151(4) 0.0019(3) 0.0040(3) -0.0006(3) C16 0.0141(4) 0.0176(4) 0.0159(4) 0.0033(3) 0.0056(3) -0.0002(3) C17 0.0154(4) 0.0204(4) 0.0135(4) 0.0027(3) 0.0056(3) 0.0007(3) C18 0.0128(3) 0.0167(4) 0.0119(3) 0.0004(3) 0.0038(3) 0.0000(3) C19 0.0130(3) 0.0188(4) 0.0122(3) -0.0018(3) 0.0041(3) -0.0007(3) C20 0.0125(3) 0.0197(4) 0.0120(4) 0.0005(3) 0.0027(3) -0.0010(3) C21 0.0121(3) 0.0156(4) 0.0122(3) 0.0000(3) 0.0025(3) -0.0001(3) C22 0.0121(3) 0.0149(4) 0.0151(4) -0.0018(3) 0.0039(3) 0.0002(3) C23 0.0119(3) 0.0140(4) 0.0122(3) 0.0007(3) 0.0037(3) 0.0002(3) C24 0.0198(5) 0.0252(5) 0.0234(5) 0.0078(4) 0.0093(4) -0.0020(4) C25 0.0212(5) 0.0270(5) 0.0163(4) -0.0064(4) 0.0077(4) -0.0029(4) C26 0.0170(4) 0.0169(4) 0.0244(5) -0.0016(4) 0.0041(4) 0.0033(3) C27 0.0152(4) 0.0244(5) 0.0170(4) 0.0069(4) 0.0021(3) -0.0017(4) C28 0.0132(3) 0.0143(4) 0.0140(4) 0.0008(3) 0.0028(3) 0.0013(3) C29 0.0158(4) 0.0168(4) 0.0168(4) 0.0003(3) 0.0013(3) -0.0003(3) C30 0.0182(4) 0.0237(5) 0.0208(5) 0.0003(4) -0.0025(4) 0.0009(4) C31 0.0263(6) 0.0267(6) 0.0261(6) 0.0066(5) -0.0060(5) 0.0046(5) C32 0.0307(6) 0.0195(5) 0.0304(6) 0.0079(5) -0.0038(5) 0.0031(5) C33 0.0205(5) 0.0153(4) 0.0233(5) 0.0028(4) 0.0004(4) 0.0005(3) C34 0.0148(4) 0.0164(4) 0.0168(4) -0.0034(3) 0.0043(3) -0.0021(3) C35 0.0178(5) 0.0266(6) 0.0342(6) -0.0167(5) 0.0093(4) -0.0051(4) C36 0.0258(6) 0.0323(7) 0.0498(9) -0.0256(7) 0.0172(6) -0.0092(5) C37 0.0313(7) 0.0330(8) 0.0630(12) -0.0298(8) 0.0235(8) -0.0162(6) C38 0.0271(7) 0.0344(8) 0.0685(13) -0.0282(8) 0.0246(8) -0.0170(6) C39 0.0204(5) 0.0228(5) 0.0389(7) -0.0122(5) 0.0144(5) -0.0079(4) C40 0.0112(3) 0.0158(4) 0.0134(4) 0.0006(3) 0.0023(3) -0.0001(3) C41 0.0130(4) 0.0197(4) 0.0198(4) 0.0050(4) 0.0017(3) 0.0004(3) C42 0.0152(4) 0.0243(5) 0.0235(5) 0.0104(4) 0.0011(4) 0.0000(4) C43 0.0210(5) 0.0364(8) 0.0463(9) 0.0265(7) 0.0019(6) 0.0018(5) C1S 0.0253(6) 0.0353(7) 0.0243(6) 0.0011(5) 0.0057(5) 0.0015(5) Cl1S 0.0526(3) 0.0428(2) 0.02568(17) -0.00387(15) 0.00374(16) -0.00239(19) Cl2S 0.0391(2) 0.0416(2) 0.0532(3) -0.0044(2) 0.0084(2) -0.01184(18) Cl3S 0.0334(2) 0.1554(8) 0.0435(3) -0.0329(4) 0.0112(2) 0.0203(3) C2S 0.0320(7) 0.0403(8) 0.0262(6) -0.0010(6) 0.0017(5) 0.0013(6) Cl4S 0.0554(4) 0.0642(4) 0.1340(8) -0.0463(5) 0.0302(4) 0.0071(3) Cl5S 0.0547(3) 0.0545(3) 0.02676(18) -0.00171(17) 0.01205(18) -0.0148(2) Cl6S 0.03242(19) 0.0562(3) 0.0445(2) -0.0160(2) 0.00179(17) 0.00052(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 C1 1.8114(11) . ? Rh1 P1 2.3161(3) . ? Rh1 P2 2.3349(3) . ? Rh1 Cl1 2.3792(3) . ? P1 C2 1.8192(11) . ? P1 C14 1.8227(10) . ? P1 C8 1.8251(11) . ? C1 O1 1.1519(14) . ? P2 C34 1.8183(11) . ? P2 C28 1.8269(11) . ? P2 C40 1.8268(11) . ? C2 C7 1.3939(16) . ? C2 C3 1.4046(16) . ? O2 C23 1.3687(13) . ? O2 C22 1.4665(13) . ? C3 C4 1.3909(18) . ? O3 C21 1.3825(13) . ? O3 C22 1.4142(13) . ? C4 C5 1.397(2) . ? C5 C6 1.394(2) . ? C6 C7 1.3958(18) . ? C8 C9 1.3942(16) . ? C8 C13 1.4013(15) . ? C9 C10 1.3953(18) . ? C10 C11 1.388(2) . ? C11 C12 1.391(2) . ? C12 C13 1.3947(18) . ? C14 C23 1.3920(15) . ? C14 C15 1.4093(14) . ? C15 C16 1.4003(15) . ? C16 C17 1.4041(17) . ? C16 C24 1.5099(16) . ? C17 C18 1.3853(15) . ? C18 C23 1.3886(14) . ? C18 C19 1.5086(15) . ? C19 C20 1.5221(15) . ? C19 C25 1.5267(15) . ? C19 C22 1.5704(15) . ? C20 C27 1.3835(16) . ? C20 C21 1.3908(15) . ? C21 C40 1.3958(14) 3_765 ? C22 C26 1.5051(16) . ? C27 C42 1.4030(17) 3_765 ? C28 C33 1.3954(16) . ? C28 C29 1.3960(16) . ? C29 C30 1.3888(17) . ? C30 C31 1.392(2) . ? C31 C32 1.392(2) . ? C32 C33 1.3920(19) . ? C34 C39 1.3966(17) . ? C34 C35 1.3991(17) . ? C35 C36 1.3916(19) . ? C36 C37 1.389(2) . ? C37 C38 1.390(2) . ? C38 C39 1.394(2) . ? C40 C21 1.3958(14) 3_765 ? C40 C41 1.4101(16) . ? C41 C42 1.3968(17) . ? C42 C27 1.4030(17) 3_765 ? C42 C43 1.5086(19) . ? C1S Cl3S 1.7375(16) . ? C1S Cl2S 1.7540(17) . ? C1S Cl1S 1.7637(16) . ? C2S Cl4S 1.750(2) . ? C2S Cl6S 1.7551(19) . ? C2S Cl5S 1.767(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 C1 Rh1 P1 90.27(3) . . ? C1 Rh1 P2 89.58(3) . . ? P1 Rh1 P2 167.857(10) . . ? C1 Rh1 Cl1 176.46(3) . . ? P1 Rh1 Cl1 87.899(10) . . ? P2 Rh1 Cl1 92.847(10) . . ? C2 P1 C14 103.16(5) . . ? C2 P1 C8 108.17(5) . . ? C14 P1 C8 101.43(5) . . ? C2 P1 Rh1 107.07(3) . . ? C14 P1 Rh1 116.09(3) . . ? C8 P1 Rh1 119.58(3) . . ? O1 C1 Rh1 178.16(10) . . ? C34 P2 C28 103.09(5) . . ? C34 P2 C40 105.23(5) . . ? C28 P2 C40 104.27(5) . . ? C34 P2 Rh1 111.03(4) . . ? C28 P2 Rh1 113.06(3) . . ? C40 P2 Rh1 118.71(4) . . ? C7 C2 C3 119.58(10) . . ? C7 C2 P1 123.37(9) . . ? C3 C2 P1 117.03(8) . . ? C23 O2 C22 107.23(8) . . ? C4 C3 C2 120.32(12) . . ? C21 O3 C22 106.64(8) . . ? C3 C4 C5 119.74(13) . . ? C6 C5 C4 120.20(12) . . ? C5 C6 C7 120.03(13) . . ? C2 C7 C6 120.13(12) . . ? C9 C8 C13 119.44(10) . . ? C9 C8 P1 119.91(8) . . ? C13 C8 P1 120.42(8) . . ? C8 C9 C10 119.91(11) . . ? C11 C10 C9 120.60(12) . . ? C10 C11 C12 119.72(12) . . ? C11 C12 C13 120.11(12) . . ? C12 C13 C8 120.19(11) . . ? C23 C14 C15 116.12(9) . . ? C23 C14 P1 118.61(7) . . ? C15 C14 P1 125.24(8) . . ? C16 C15 C14 122.27(10) . . ? C15 C16 C17 119.29(10) . . ? C15 C16 C24 120.47(11) . . ? C17 C16 C24 120.21(10) . . ? C18 C17 C16 119.23(10) . . ? C17 C18 C23 120.26(10) . . ? C17 C18 C19 132.02(10) . . ? C23 C18 C19 107.72(9) . . ? C18 C19 C20 112.02(9) . . ? C18 C19 C25 114.58(9) . . ? C20 C19 C25 113.13(9) . . ? C18 C19 C22 101.17(8) . . ? C20 C19 C22 98.74(8) . . ? C25 C19 C22 115.61(10) . . ? C27 C20 C21 120.37(10) . . ? C27 C20 C19 130.84(10) . . ? C21 C20 C19 108.77(9) . . ? O3 C21 C20 112.18(9) . . ? O3 C21 C40 125.10(9) . 3_765 ? C20 C21 C40 122.72(10) . 3_765 ? O3 C22 O2 107.47(8) . . ? O3 C22 C26 109.08(9) . . ? O2 C22 C26 107.73(9) . . ? O3 C22 C19 107.46(8) . . ? O2 C22 C19 104.39(8) . . ? C26 C22 C19 120.04(9) . . ? O2 C23 C18 113.45(9) . . ? O2 C23 C14 123.80(9) . . ? C18 C23 C14 122.75(9) . . ? C20 C27 C42 119.21(10) . 3_765 ? C33 C28 C29 119.26(10) . . ? C33 C28 P2 122.19(9) . . ? C29 C28 P2 118.44(8) . . ? C30 C29 C28 120.78(11) . . ? C29 C30 C31 119.67(12) . . ? C30 C31 C32 119.98(12) . . ? C33 C32 C31 120.24(13) . . ? C32 C33 C28 120.07(12) . . ? C39 C34 C35 119.34(11) . . ? C39 C34 P2 118.99(9) . . ? C35 C34 P2 121.57(9) . . ? C36 C35 C34 120.32(12) . . ? C37 C36 C35 120.03(13) . . ? C36 C37 C38 119.95(14) . . ? C37 C38 C39 120.26(14) . . ? C38 C39 C34 120.01(12) . . ? C21 C40 C41 115.71(9) 3_765 . ? C21 C40 P2 125.27(8) 3_765 . ? C41 C40 P2 119.02(8) . . ? C42 C41 C40 122.70(10) . . ? C41 C42 C27 119.28(11) . 3_765 ? C41 C42 C43 120.44(12) . . ? C27 C42 C43 120.28(11) 3_765 . ? Cl3S C1S Cl2S 110.90(10) . . ? Cl3S C1S Cl1S 109.82(9) . . ? Cl2S C1S Cl1S 110.42(9) . . ? Cl4S C2S Cl6S 109.02(10) . . ? Cl4S C2S Cl5S 110.86(11) . . ? Cl6S C2S Cl5S 110.16(11) . . ? 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 C1 Rh1 P1 C2 124.04(5) . . . . ? P2 Rh1 P1 C2 34.79(6) . . . . ? Cl1 Rh1 P1 C2 -58.98(4) . . . . ? C1 Rh1 P1 C14 9.48(5) . . . . ? P2 Rh1 P1 C14 -79.77(6) . . . . ? Cl1 Rh1 P1 C14 -173.54(4) . . . . ? C1 Rh1 P1 C8 -112.63(5) . . . . ? P2 Rh1 P1 C8 158.12(6) . . . . ? Cl1 Rh1 P1 C8 64.35(4) . . . . ? P1 Rh1 C1 O1 82(3) . . . . ? P2 Rh1 C1 O1 -111(3) . . . . ? Cl1 Rh1 C1 O1 23(3) . . . . ? C1 Rh1 P2 C34 -125.13(5) . . . . ? P1 Rh1 P2 C34 -35.81(7) . . . . ? Cl1 Rh1 P2 C34 57.44(4) . . . . ? C1 Rh1 P2 C28 -9.83(5) . . . . ? P1 Rh1 P2 C28 79.50(6) . . . . ? Cl1 Rh1 P2 C28 172.74(4) . . . . ? C1 Rh1 P2 C40 112.77(5) . . . . ? P1 Rh1 P2 C40 -157.91(5) . . . . ? Cl1 Rh1 P2 C40 -64.66(4) . . . . ? C14 P1 C2 C7 -107.93(10) . . . . ? C8 P1 C2 C7 -1.02(11) . . . . ? Rh1 P1 C2 C7 129.09(9) . . . . ? C14 P1 C2 C3 74.08(10) . . . . ? C8 P1 C2 C3 -179.01(9) . . . . ? Rh1 P1 C2 C3 -48.89(9) . . . . ? C7 C2 C3 C4 0.65(18) . . . . ? P1 C2 C3 C4 178.71(10) . . . . ? C2 C3 C4 C5 -0.5(2) . . . . ? C3 C4 C5 C6 -0.1(2) . . . . ? C4 C5 C6 C7 0.4(2) . . . . ? C3 C2 C7 C6 -0.30(18) . . . . ? P1 C2 C7 C6 -178.23(10) . . . . ? C5 C6 C7 C2 -0.2(2) . . . . ? C2 P1 C8 C9 107.93(10) . . . . ? C14 P1 C8 C9 -143.96(10) . . . . ? Rh1 P1 C8 C9 -14.86(11) . . . . ? C2 P1 C8 C13 -77.58(10) . . . . ? C14 P1 C8 C13 30.53(10) . . . . ? Rh1 P1 C8 C13 159.62(8) . . . . ? C13 C8 C9 C10 -1.39(19) . . . . ? P1 C8 C9 C10 173.15(11) . . . . ? C8 C9 C10 C11 -0.1(2) . . . . ? C9 C10 C11 C12 1.4(2) . . . . ? C10 C11 C12 C13 -1.1(2) . . . . ? C11 C12 C13 C8 -0.3(2) . . . . ? C9 C8 C13 C12 1.60(18) . . . . ? P1 C8 C13 C12 -172.92(10) . . . . ? C2 P1 C14 C23 175.72(8) . . . . ? C8 P1 C14 C23 63.76(9) . . . . ? Rh1 P1 C14 C23 -67.52(9) . . . . ? C2 P1 C14 C15 -5.90(10) . . . . ? C8 P1 C14 C15 -117.86(9) . . . . ? Rh1 P1 C14 C15 110.86(9) . . . . ? C23 C14 C15 C16 0.71(15) . . . . ? P1 C14 C15 C16 -177.71(8) . . . . ? C14 C15 C16 C17 1.55(16) . . . . ? C14 C15 C16 C24 -176.81(11) . . . . ? C15 C16 C17 C18 -1.88(16) . . . . ? C24 C16 C17 C18 176.49(11) . . . . ? C16 C17 C18 C23 -0.04(16) . . . . ? C16 C17 C18 C19 179.18(11) . . . . ? C17 C18 C19 C20 -91.54(14) . . . . ? C23 C18 C19 C20 87.76(11) . . . . ? C17 C18 C19 C25 39.08(17) . . . . ? C23 C18 C19 C25 -141.63(10) . . . . ? C17 C18 C19 C22 164.17(11) . . . . ? C23 C18 C19 C22 -16.53(11) . . . . ? C18 C19 C20 C27 59.63(15) . . . . ? C25 C19 C20 C27 -71.72(16) . . . . ? C22 C19 C20 C27 165.51(12) . . . . ? C18 C19 C20 C21 -118.58(10) . . . . ? C25 C19 C20 C21 110.07(11) . . . . ? C22 C19 C20 C21 -12.70(11) . . . . ? C22 O3 C21 C20 17.23(12) . . . . ? C22 O3 C21 C40 -162.48(10) . . . 3_765 ? C27 C20 C21 O3 179.97(10) . . . . ? C19 C20 C21 O3 -1.60(12) . . . . ? C27 C20 C21 C40 -0.31(17) . . . 3_765 ? C19 C20 C21 C40 178.12(10) . . . 3_765 ? C21 O3 C22 O2 86.62(10) . . . . ? C21 O3 C22 C26 -156.84(9) . . . . ? C21 O3 C22 C19 -25.23(10) . . . . ? C23 O2 C22 O3 -136.90(9) . . . . ? C23 O2 C22 C26 105.69(10) . . . . ? C23 O2 C22 C19 -22.97(10) . . . . ? C18 C19 C22 O3 137.48(8) . . . . ? C20 C19 C22 O3 22.84(10) . . . . ? C25 C19 C22 O3 -98.12(10) . . . . ? C18 C19 C22 O2 23.55(10) . . . . ? C20 C19 C22 O2 -91.09(9) . . . . ? C25 C19 C22 O2 147.95(9) . . . . ? C18 C19 C22 C26 -97.22(11) . . . . ? C20 C19 C22 C26 148.14(10) . . . . ? C25 C19 C22 C26 27.18(14) . . . . ? C22 O2 C23 C18 13.22(12) . . . . ? C22 O2 C23 C14 -166.75(9) . . . . ? C17 C18 C23 O2 -177.51(10) . . . . ? C19 C18 C23 O2 3.09(12) . . . . ? C17 C18 C23 C14 2.46(16) . . . . ? C19 C18 C23 C14 -176.93(9) . . . . ? C15 C14 C23 O2 177.24(9) . . . . ? P1 C14 C23 O2 -4.23(14) . . . . ? C15 C14 C23 C18 -2.73(15) . . . . ? P1 C14 C23 C18 175.80(8) . . . . ? C21 C20 C27 C42 -0.06(18) . . . 3_765 ? C19 C20 C27 C42 -178.10(12) . . . 3_765 ? C34 P2 C28 C33 19.44(11) . . . . ? C40 P2 C28 C33 129.15(10) . . . . ? Rh1 P2 C28 C33 -100.53(10) . . . . ? C34 P2 C28 C29 -164.42(9) . . . . ? C40 P2 C28 C29 -54.70(10) . . . . ? Rh1 P2 C28 C29 75.62(9) . . . . ? C33 C28 C29 C30 -0.99(17) . . . . ? P2 C28 C29 C30 -177.25(10) . . . . ? C28 C29 C30 C31 0.6(2) . . . . ? C29 C30 C31 C32 0.2(2) . . . . ? C30 C31 C32 C33 -0.4(3) . . . . ? C31 C32 C33 C28 0.0(2) . . . . ? C29 C28 C33 C32 0.70(19) . . . . ? P2 C28 C33 C32 176.82(11) . . . . ? C28 P2 C34 C39 -113.18(12) . . . . ? C40 P2 C34 C39 137.81(11) . . . . ? Rh1 P2 C34 C39 8.16(12) . . . . ? C28 P2 C34 C35 63.32(12) . . . . ? C40 P2 C34 C35 -45.68(13) . . . . ? Rh1 P2 C34 C35 -175.33(11) . . . . ? C39 C34 C35 C36 2.6(2) . . . . ? P2 C34 C35 C36 -173.92(14) . . . . ? C34 C35 C36 C37 -1.8(3) . . . . ? C35 C36 C37 C38 -0.9(4) . . . . ? C36 C37 C38 C39 2.7(4) . . . . ? C37 C38 C39 C34 -1.9(3) . . . . ? C35 C34 C39 C38 -0.8(3) . . . . ? P2 C34 C39 C38 175.81(16) . . . . ? C34 P2 C40 C21 80.33(10) . . . 3_765 ? C28 P2 C40 C21 -27.82(11) . . . 3_765 ? Rh1 P2 C40 C21 -154.70(8) . . . 3_765 ? C34 P2 C40 C41 -99.84(10) . . . . ? C28 P2 C40 C41 152.01(9) . . . . ? Rh1 P2 C40 C41 25.13(10) . . . . ? C21 C40 C41 C42 -0.60(18) 3_765 . . . ? P2 C40 C41 C42 179.56(10) . . . . ? C40 C41 C42 C27 1.0(2) . . . 3_765 ? C40 C41 C42 C43 -179.56(14) . . . . ? _diffrn_measured_fraction_theta_max 0.960 _diffrn_reflns_theta_full 39.65 _diffrn_measured_fraction_theta_full 0.960 _refine_diff_density_max 2.153 _refine_diff_density_min -1.885 _refine_diff_density_rms 0.096 #===END data_jm233-5_19 _database_code_depnum_ccdc_archive 'CCDC 762011' #TrackingRef '1764_web_deposit_cif_file_0_EduardoC.Escudero-Adan_1279182185.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H76 Cl2 O12 P4 Rh2' _chemical_formula_weight 1654.03 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 18.1626(9) _cell_length_b 17.4391(9) _cell_length_c 13.3646(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.713(2) _cell_angle_gamma 90.00 _cell_volume 4009.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4749 _cell_measurement_theta_min 2.84 _cell_measurement_theta_max 36.32 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1696 _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.81 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ; TWINABS Version 2008/4 Bruker AXS 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 The best data completeness obtained reached 90.2 % since overlapping reflections of the two different crystals were omitted. ; _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 70 _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_reflns_number 49393 _diffrn_reflns_av_R_equivalents 0.0674 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 36.54 _reflns_number_total 17840 _reflns_number_gt 13571 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. 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 sample was a twin made up of two crystal domains with ratio 64:36. One phenyl ring is disordered in two positions with occupation ratio 60:40. The asymmetric unit contains seven positions of water molecules which correspond to a total of three water molecules, two of them disordered, in two and four positions, with occupation ratio 50:50 and 25:25:25:25 respectively. High residual electron density remains due to residual absorption artifacts. ; _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^)+(0.1109P)^2^+10.5465P] 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 17840 _refine_ls_number_parameters 546 _refine_ls_number_restraints 124 _refine_ls_R_factor_all 0.0999 _refine_ls_R_factor_gt 0.0728 _refine_ls_wR_factor_ref 0.2213 _refine_ls_wR_factor_gt 0.1971 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.257550(11) 0.500084(12) 0.856564(17) 0.01614(3) Uani 1 1 d . A . P1 P 0.22924(4) 0.55604(5) 0.99621(6) 0.01925(14) Uani 1 1 d . . . Cl1 Cl 0.16666(4) 0.40133(5) 0.85333(7) 0.02838(16) Uani 1 1 d . . . C1 C 0.32338(16) 0.5791(2) 0.8582(3) 0.0251(6) Uani 1 1 d . . . C2 C 0.27273(16) 0.64815(18) 1.0498(2) 0.0225(6) Uani 1 1 d . A . O1 O 0.36295(14) 0.63022(14) 0.8618(2) 0.0280(5) Uani 1 1 d . A . P2 P 0.31122(4) 0.42273(5) 0.75648(6) 0.01889(14) Uani 1 1 d . . . C7 C 0.2566(2) 0.7113(2) 0.9826(3) 0.0313(7) Uani 1 1 d . . . H7A H 0.2296 0.7045 0.9095 0.038 Uiso 1 1 calc R A . O2 O 0.46807(12) 0.50638(12) 0.86020(16) 0.0173(4) Uani 1 1 d . A . C6 C 0.2795(2) 0.7843(2) 1.0217(3) 0.0359(8) Uani 1 1 d . A . H6A H 0.2682 0.8272 0.9754 0.043 Uiso 1 1 calc R . . O3 O 0.60350(11) 0.50442(12) 0.92072(17) 0.0182(4) Uani 1 1 d . A . C5 C 0.3189(2) 0.7945(2) 1.1286(3) 0.0327(8) Uani 1 1 d . . . H5A H 0.3338 0.8445 1.1558 0.039 Uiso 1 1 calc R A . C4 C 0.3363(2) 0.7325(2) 1.1947(3) 0.0315(8) Uani 1 1 d . A . H4A H 0.3642 0.7395 1.2675 0.038 Uiso 1 1 calc R . . C3 C 0.3132(2) 0.6586(2) 1.1559(3) 0.0274(7) Uani 1 1 d . . . H3A H 0.3254 0.6158 1.2023 0.033 Uiso 1 1 calc R A . C8 C 0.12836(12) 0.57169(17) 0.9937(2) 0.0197(9) Uani 0.645(6) 1 d PGU A 1 C9 C 0.11123(17) 0.6061(2) 1.0774(2) 0.0351(13) Uani 0.645(6) 1 d PGU A 1 H9A H 0.1518 0.6176 1.1409 0.042 Uiso 0.645(6) 1 calc PR A 1 C10 C 0.0347(2) 0.6237(3) 1.0682(3) 0.0354(12) Uani 0.645(6) 1 d PGU A 1 H10A H 0.0230 0.6472 1.1254 0.042 Uiso 0.645(6) 1 calc PR A 1 C11 C -0.02471(14) 0.6069(3) 0.9753(4) 0.0324(12) Uani 0.645(6) 1 d PGU A 1 H11A H -0.0770 0.6189 0.9691 0.039 Uiso 0.645(6) 1 calc PR A 1 C12 C -0.00758(13) 0.5724(3) 0.8916(3) 0.0356(13) Uani 0.645(6) 1 d PGU A 1 H12A H -0.0482 0.5609 0.8281 0.043 Uiso 0.645(6) 1 calc PR A 1 C13 C 0.06896(15) 0.5549(2) 0.9008(2) 0.0303(12) Uani 0.645(6) 1 d PGU A 1 H13A H 0.0807 0.5313 0.8436 0.036 Uiso 0.645(6) 1 calc PR A 1 C8' C 0.1299(6) 0.5794(7) 0.9767(9) 0.0250(17) Uani 0.355(6) 1 d PU A 2 C9' C 0.1089(7) 0.6146(8) 1.0551(10) 0.037(2) Uani 0.355(6) 1 d PU A 2 H9A' H 0.1462 0.6240 1.1223 0.044 Uiso 0.355(6) 1 calc PR A 2 C10' C 0.0284(9) 0.6371(10) 1.0333(13) 0.052(3) Uani 0.355(6) 1 d PU A 2 H10' H 0.0148 0.6649 1.0860 0.062 Uiso 0.355(6) 1 calc PR A 2 C11' C -0.0292(7) 0.6206(8) 0.9406(11) 0.040(2) Uani 0.355(6) 1 d PU A 2 H11' H -0.0823 0.6314 0.9307 0.048 Uiso 0.355(6) 1 calc PR A 2 C12' C -0.0041(10) 0.5856(11) 0.8585(14) 0.058(3) Uani 0.355(6) 1 d PU A 2 H12' H -0.0410 0.5769 0.7908 0.070 Uiso 0.355(6) 1 calc PR A 2 C13' C 0.0704(7) 0.5653(8) 0.8770(11) 0.038(2) Uani 0.355(6) 1 d PU A 2 H13' H 0.0844 0.5407 0.8224 0.045 Uiso 0.355(6) 1 calc PR A 2 C14 C 0.24455(16) 0.36697(19) 0.6524(2) 0.0237(6) Uani 1 1 d . A . C15 C 0.1744(2) 0.4006(3) 0.5904(4) 0.0387(10) Uani 1 1 d . . . H15A H 0.1622 0.4517 0.6041 0.046 Uiso 1 1 calc R A . C16 C 0.1229(2) 0.3590(3) 0.5092(4) 0.0452(11) Uani 1 1 d . A . H16A H 0.0759 0.3821 0.4665 0.054 Uiso 1 1 calc R . . C17 C 0.1397(2) 0.2844(3) 0.4901(3) 0.0430(9) Uani 1 1 d . . . H17A H 0.1041 0.2562 0.4345 0.052 Uiso 1 1 calc R A . C18 C 0.2072(2) 0.2506(2) 0.5506(3) 0.0357(8) Uani 1 1 d . A . H18A H 0.2179 0.1989 0.5380 0.043 Uiso 1 1 calc R . . C19 C 0.2601(2) 0.2921(2) 0.6308(3) 0.0286(7) Uani 1 1 d . . . H19A H 0.3076 0.2688 0.6713 0.034 Uiso 1 1 calc R A . C20 C 0.37528(15) 0.35164(18) 0.8428(2) 0.0213(6) Uani 1 1 d . A . C21 C 0.44971(16) 0.33568(19) 0.8399(3) 0.0261(6) Uani 1 1 d . . . H21A H 0.4672 0.3587 0.7871 0.031 Uiso 1 1 calc R A . C22 C 0.49869(18) 0.2865(2) 0.9132(3) 0.0296(7) Uani 1 1 d . A . H22A H 0.5498 0.2771 0.9114 0.036 Uiso 1 1 calc R . . C23 C 0.47304(18) 0.2510(2) 0.9896(3) 0.0274(7) Uani 1 1 d . . . H23A H 0.5068 0.2183 1.0410 0.033 Uiso 1 1 calc R A . C24 C 0.39733(18) 0.26384(19) 0.9896(3) 0.0265(6) Uani 1 1 d . A . H24A H 0.3786 0.2378 1.0391 0.032 Uiso 1 1 calc R . . C25 C 0.34907(16) 0.31460(18) 0.9176(2) 0.0235(6) Uani 1 1 d . . . H25A H 0.2980 0.3241 0.9194 0.028 Uiso 1 1 calc R A . C26 C 0.37243(14) 0.47167(17) 0.6919(2) 0.0187(5) Uani 1 1 d . A . C27 C 0.35008(16) 0.48311(19) 0.5816(2) 0.0212(6) Uani 1 1 d . . . H27A H 0.3055 0.4571 0.5374 0.025 Uiso 1 1 calc R A . C28 C 0.39160(16) 0.53166(19) 0.5350(2) 0.0213(6) Uani 1 1 d . A . C29 C 0.45564(17) 0.57202(18) 0.6008(2) 0.0215(6) Uani 1 1 d . . . H29A H 0.4838 0.6059 0.5708 0.026 Uiso 1 1 calc R A . C30 C 0.47779(14) 0.56274(16) 0.7083(2) 0.0174(5) Uani 1 1 d . A . C31 C 0.43845(15) 0.51042(17) 0.7515(2) 0.0173(5) Uani 1 1 d . . . C32 C 0.3664(2) 0.5437(2) 0.4178(3) 0.0304(7) Uani 1 1 d . . . H32A H 0.3977 0.5114 0.3870 0.046 Uiso 1 1 calc R A . H32B H 0.3736 0.5977 0.4027 0.046 Uiso 1 1 calc R . . H32C H 0.3114 0.5300 0.3869 0.046 Uiso 1 1 calc R . . C33 C 0.53841(15) 0.60207(17) 0.7972(2) 0.0187(5) Uani 1 1 d . . . H33A H 0.5257 0.6572 0.8040 0.022 Uiso 1 1 calc R A . C34 C 0.53527(14) 0.55375(17) 0.8929(2) 0.0176(5) Uani 1 1 d . A . H34A H 0.5351 0.5872 0.9535 0.021 Uiso 1 1 calc R . . C35 C 0.65378(15) 0.53410(17) 0.8733(2) 0.0187(5) Uani 1 1 d . . . C36 C 0.62110(14) 0.59105(17) 0.8000(2) 0.0180(5) Uani 1 1 d . A . C37 C 0.66381(15) 0.62537(18) 0.7434(2) 0.0207(5) Uani 1 1 d . . . H37A H 0.6413 0.6640 0.6926 0.025 Uiso 1 1 calc R A . C38 C 0.74098(16) 0.60222(18) 0.7621(2) 0.0221(5) Uani 1 1 d . A . C39 C 0.77301(16) 0.54589(18) 0.8372(2) 0.0223(6) Uani 1 1 d . . . H39A H 0.8255 0.5311 0.8493 0.027 Uiso 1 1 calc R A . C40 C 0.26914(14) 0.49029(17) 1.1039(2) 0.0195(5) Uani 1 1 d . . . C41 C 0.78895(19) 0.6393(2) 0.7019(3) 0.0328(8) Uani 1 1 d . . . H41A H 0.8167 0.6836 0.7417 0.049 Uiso 1 1 calc R A . H41B H 0.7547 0.6563 0.6327 0.049 Uiso 1 1 calc R . . H41C H 0.8266 0.6022 0.6923 0.049 Uiso 1 1 calc R . . O1W O 0.1325(4) 0.9296(4) 0.8450(5) 0.1050(16) Uani 1 1 d DU B 1 H11 H 0.1402 0.9144 0.7889 0.157 Uiso 1 1 d RD B 1 H12 H 0.1772 0.9313 0.8914 0.157 Uiso 1 1 d RD B 1 O4W O 0.0384(7) 0.6949(7) 0.7457(9) 0.0397(18) Uani 0.25 1 d PDU C 1 H41 H 0.0553 0.7348 0.7825 0.060 Uiso 0.25 1 d PRD C 1 H42 H 0.0714 0.6857 0.7143 0.060 Uiso 0.25 1 d PRD C 1 O5W O 0.1074(8) 0.6176(8) 0.5503(11) 0.0441(18) Uani 0.25 1 d PDU D 1 H51 H 0.1559 0.6260 0.5759 0.066 Uiso 0.25 1 d PRD D 1 H52 H 0.0917 0.6133 0.6036 0.066 Uiso 0.25 1 d PRD D 1 O6W O 0.0049(7) 0.8799(8) 0.8434(10) 0.0441(18) Uani 0.25 1 d PDU E 1 H61 H 0.0425 0.9084 0.8422 0.066 Uiso 0.25 1 d PRD E 1 H62 H 0.0237 0.8348 0.8534 0.066 Uiso 0.25 1 d PRD E 1 O7W O 0.1005(9) 0.8097(9) 0.7929(12) 0.056(2) Uani 0.25 1 d PDU F 3 H71 H 0.0607 0.8098 0.8134 0.084 Uiso 0.25 1 d PRD F 3 H72 H 0.0970 0.7685 0.7576 0.084 Uiso 0.25 1 d PRD F 3 O2W O 0.0054(3) 0.9684(4) 0.8962(7) 0.057(2) Uani 0.50 1 d PD G 2 H21 H -0.0123 1.0116 0.8694 0.085 Uiso 0.50 1 d PRD G 2 H22 H 0.0438 0.9595 0.8746 0.085 Uiso 0.50 1 d PRD G 2 O3W O 0.0290(4) 0.8024(5) 0.8500(7) 0.061(2) Uani 0.50 1 d PD H 2 H31 H 0.0517 0.8336 0.8992 0.092 Uiso 0.50 1 d PRD H 2 H32 H -0.0094 0.8272 0.8097 0.092 Uiso 0.50 1 d PRD H 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 0.01466(5) 0.01441(7) 0.01938(6) 0.00062(7) 0.00550(6) 0.00105(6) P1 0.0158(2) 0.0172(3) 0.0255(3) 0.0014(3) 0.0077(2) 0.0020(2) Cl1 0.0259(2) 0.0214(3) 0.0406(3) 0.0008(3) 0.0145(2) -0.0009(2) C1 0.0219(10) 0.0286(15) 0.0255(11) -0.0026(11) 0.0083(9) 0.0042(10) C2 0.0257(10) 0.0154(12) 0.0291(12) -0.0026(10) 0.0125(9) 0.0011(8) O1 0.0321(9) 0.0186(11) 0.0371(11) -0.0010(9) 0.0164(8) -0.0003(8) P2 0.0161(2) 0.0168(3) 0.0240(3) -0.0011(2) 0.0066(2) 0.0000(2) C7 0.0421(14) 0.0206(15) 0.0330(14) 0.0025(11) 0.0147(13) 0.0010(13) O2 0.0170(7) 0.0205(10) 0.0147(7) 0.0002(6) 0.0055(6) -0.0023(6) C6 0.0528(18) 0.0177(15) 0.0407(17) 0.0042(13) 0.0196(14) -0.0025(13) O3 0.0120(6) 0.0213(10) 0.0223(8) 0.0061(7) 0.0069(6) 0.0025(6) C5 0.0403(14) 0.0190(15) 0.0438(16) -0.0039(13) 0.0206(12) -0.0057(12) C4 0.0387(14) 0.0236(16) 0.0322(15) -0.0082(12) 0.0115(12) -0.0062(12) C3 0.0315(12) 0.0212(15) 0.0276(13) -0.0004(11) 0.0072(11) -0.0024(11) C8 0.0179(13) 0.0156(17) 0.0273(17) 0.0062(14) 0.0098(12) 0.0027(12) C9 0.0347(18) 0.041(3) 0.034(2) -0.0011(19) 0.0176(16) 0.0053(18) C10 0.0247(15) 0.043(3) 0.043(2) -0.004(2) 0.0168(15) 0.0088(16) C11 0.0199(14) 0.036(2) 0.046(2) 0.0030(19) 0.0163(15) 0.0056(16) C12 0.0182(15) 0.040(3) 0.049(2) -0.004(2) 0.0111(16) 0.0030(16) C13 0.0204(15) 0.031(2) 0.038(2) -0.0053(18) 0.0072(15) 0.0043(15) C8' 0.027(3) 0.023(3) 0.029(3) 0.002(2) 0.014(2) -0.002(2) C9' 0.034(3) 0.045(4) 0.034(3) -0.003(3) 0.015(2) 0.009(3) C10' 0.048(3) 0.061(4) 0.051(4) -0.004(3) 0.023(3) 0.010(3) C11' 0.036(3) 0.042(4) 0.042(3) 0.000(3) 0.013(3) 0.002(3) C12' 0.057(4) 0.060(4) 0.058(4) -0.001(3) 0.020(3) 0.001(3) C13' 0.037(3) 0.037(4) 0.039(3) -0.003(3) 0.011(3) 0.003(3) C14 0.0225(10) 0.0233(14) 0.0257(11) -0.0027(11) 0.0083(8) -0.0042(9) C15 0.0242(12) 0.036(2) 0.050(2) -0.0081(17) 0.0028(14) 0.0028(13) C16 0.0291(15) 0.057(3) 0.044(2) -0.008(2) 0.0033(15) -0.0074(16) C17 0.0400(14) 0.053(2) 0.0391(17) -0.0133(16) 0.0170(13) -0.0281(15) C18 0.0552(17) 0.0254(16) 0.0311(14) -0.0075(12) 0.0201(13) -0.0164(14) C19 0.0369(13) 0.0229(15) 0.0284(12) -0.0017(11) 0.0136(11) -0.0051(12) C20 0.0173(9) 0.0169(12) 0.0280(12) 0.0009(10) 0.0049(9) -0.0008(8) C21 0.0220(10) 0.0219(14) 0.0370(14) 0.0016(11) 0.0131(10) 0.0049(9) C22 0.0255(11) 0.0243(15) 0.0394(15) 0.0011(13) 0.0110(11) 0.0080(10) C23 0.0264(11) 0.0210(14) 0.0303(14) 0.0002(11) 0.0030(11) 0.0068(10) C24 0.0304(11) 0.0197(14) 0.0291(13) 0.0013(12) 0.0092(11) 0.0037(10) C25 0.0231(10) 0.0193(13) 0.0281(13) 0.0010(10) 0.0079(9) -0.0003(9) C26 0.0191(8) 0.0156(12) 0.0226(10) -0.0014(9) 0.0082(8) -0.0010(8) C27 0.0200(9) 0.0231(13) 0.0193(11) -0.0032(9) 0.0048(8) -0.0014(9) C28 0.0231(10) 0.0210(14) 0.0187(10) -0.0021(10) 0.0051(8) 0.0003(9) C29 0.0239(10) 0.0183(13) 0.0215(11) 0.0003(10) 0.0062(9) -0.0017(9) C30 0.0174(8) 0.0153(11) 0.0192(10) -0.0012(8) 0.0053(7) 0.0005(8) C31 0.0160(8) 0.0203(12) 0.0163(9) -0.0004(8) 0.0061(7) 0.0008(8) C32 0.0362(14) 0.0323(17) 0.0206(12) -0.0010(12) 0.0060(11) -0.0034(12) C33 0.0178(8) 0.0176(12) 0.0208(10) 0.0008(9) 0.0064(8) -0.0013(8) C34 0.0147(8) 0.0168(12) 0.0210(10) -0.0022(9) 0.0052(7) -0.0025(8) C35 0.0185(8) 0.0160(12) 0.0215(10) 0.0026(9) 0.0065(8) 0.0008(8) C36 0.0181(8) 0.0170(12) 0.0192(10) -0.0013(9) 0.0062(8) -0.0021(8) C37 0.0216(9) 0.0169(12) 0.0245(11) 0.0015(9) 0.0089(8) -0.0021(8) C38 0.0208(9) 0.0225(13) 0.0247(10) 0.0023(9) 0.0097(9) -0.0039(9) C39 0.0212(9) 0.0229(14) 0.0265(11) -0.0013(10) 0.0127(8) 0.0011(9) C40 0.0154(8) 0.0181(12) 0.0266(11) -0.0027(9) 0.0091(7) -0.0022(7) C41 0.0306(12) 0.0370(19) 0.0361(14) 0.0097(13) 0.0180(11) -0.0029(12) O1W 0.105(2) 0.096(2) 0.114(2) 0.0130(18) 0.0356(17) -0.0006(18) O4W 0.041(2) 0.038(3) 0.038(2) 0.001(2) 0.0105(18) 0.0062(19) O5W 0.046(2) 0.043(3) 0.045(3) 0.000(2) 0.0167(18) 0.001(2) O6W 0.044(2) 0.045(3) 0.043(3) -0.004(2) 0.0138(18) 0.003(2) O7W 0.056(3) 0.055(3) 0.055(3) 0.002(2) 0.0172(19) 0.000(2) O2W 0.031(2) 0.043(3) 0.097(5) -0.014(4) 0.021(3) -0.023(2) O3W 0.053(3) 0.044(4) 0.092(5) 0.009(4) 0.030(4) -0.008(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 C1 1.819(3) . ? Rh1 P1 2.3056(9) . ? Rh1 P2 2.3228(8) . ? Rh1 Cl1 2.3764(8) . ? P1 C8' 1.785(10) . ? P1 C40 1.800(3) . ? P1 C2 1.831(3) . ? P1 C8 1.842(2) . ? C1 O1 1.137(4) . ? C2 C3 1.384(4) . ? C2 C7 1.392(5) . ? P2 C14 1.807(3) . ? P2 C26 1.823(3) . ? P2 C20 1.833(3) . ? C7 C6 1.387(5) . ? O2 C31 1.380(3) . ? O2 C34 1.422(3) . ? C6 C5 1.389(6) . ? O3 C35 1.369(4) . ? O3 C34 1.455(3) . ? C5 C4 1.367(5) . ? C4 C3 1.402(5) . ? C8 C9 1.3900 . ? C8 C13 1.3900 . ? C9 C10 1.3900 . ? C10 C11 1.3900 . ? C11 C12 1.3900 . ? C12 C13 1.3900 . ? C8' C9' 1.369(17) . ? C8' C13' 1.443(16) . ? C9' C10' 1.451(19) . ? C10' C11' 1.371(19) . ? C11' C12' 1.45(2) . ? C12' C13' 1.34(2) . ? C14 C19 1.386(5) . ? C14 C15 1.406(5) . ? C15 C16 1.388(6) . ? C16 C17 1.380(7) . ? C17 C18 1.365(6) . ? C18 C19 1.391(5) . ? C20 C21 1.393(4) . ? C20 C25 1.396(5) . ? C21 C22 1.388(5) . ? C22 C23 1.396(6) . ? C23 C24 1.394(5) . ? C24 C25 1.392(4) . ? C26 C31 1.384(4) . ? C26 C27 1.412(4) . ? C27 C28 1.405(5) . ? C28 C29 1.402(4) . ? C28 C32 1.500(4) . ? C29 C30 1.372(4) . ? C30 C31 1.393(4) . ? C30 C33 1.502(4) . ? C33 C36 1.503(4) . ? C33 C34 1.547(4) . ? C35 C36 1.387(4) . ? C35 C40 1.400(4) 3_667 ? C36 C37 1.382(4) . ? C37 C38 1.402(4) . ? C38 C39 1.391(4) . ? C38 C41 1.509(5) . ? C39 C40 1.411(4) 3_667 ? C40 C35 1.400(4) 3_667 ? C40 C39 1.411(4) 3_667 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh1 P1 89.21(11) . . ? C1 Rh1 P2 92.93(11) . . ? P1 Rh1 P2 162.88(3) . . ? C1 Rh1 Cl1 177.23(10) . . ? P1 Rh1 Cl1 89.28(3) . . ? P2 Rh1 Cl1 89.20(3) . . ? C8' P1 C40 113.0(4) . . ? C8' P1 C2 98.4(4) . . ? C40 P1 C2 103.50(14) . . ? C8' P1 C8 8.5(4) . . ? C40 P1 C8 104.58(14) . . ? C2 P1 C8 100.30(14) . . ? C8' P1 Rh1 117.1(4) . . ? C40 P1 Rh1 103.91(10) . . ? C2 P1 Rh1 120.49(11) . . ? C8 P1 Rh1 121.80(10) . . ? O1 C1 Rh1 177.0(3) . . ? C3 C2 C7 119.3(3) . . ? C3 C2 P1 122.4(3) . . ? C7 C2 P1 117.9(2) . . ? C14 P2 C26 104.32(14) . . ? C14 P2 C20 104.70(14) . . ? C26 P2 C20 104.72(13) . . ? C14 P2 Rh1 117.02(11) . . ? C26 P2 Rh1 115.65(10) . . ? C20 P2 Rh1 109.23(11) . . ? C6 C7 C2 120.5(3) . . ? C31 O2 C34 107.4(2) . . ? C7 C6 C5 119.8(4) . . ? C35 O3 C34 107.3(2) . . ? C4 C5 C6 119.9(3) . . ? C5 C4 C3 120.6(3) . . ? C2 C3 C4 119.8(3) . . ? C9 C8 C13 120.0 . . ? C9 C8 P1 121.84(15) . . ? C13 C8 P1 117.87(15) . . ? C10 C9 C8 120.0 . . ? C9 C10 C11 120.0 . . ? C10 C11 C12 120.0 . . ? C11 C12 C13 120.0 . . ? C12 C13 C8 120.0 . . ? C9' C8' C13' 118.2(10) . . ? C9' C8' P1 120.5(8) . . ? C13' C8' P1 121.2(9) . . ? C8' C9' C10' 118.6(11) . . ? C11' C10' C9' 123.4(14) . . ? C10' C11' C12' 116.1(13) . . ? C13' C12' C11' 120.9(14) . . ? C12' C13' C8' 122.5(14) . . ? C19 C14 C15 118.5(3) . . ? C19 C14 P2 122.4(2) . . ? C15 C14 P2 119.1(3) . . ? C16 C15 C14 120.0(4) . . ? C17 C16 C15 120.2(4) . . ? C18 C17 C16 120.5(4) . . ? C17 C18 C19 120.0(4) . . ? C14 C19 C18 120.9(3) . . ? C21 C20 C25 119.0(3) . . ? C21 C20 P2 122.9(3) . . ? C25 C20 P2 118.0(2) . . ? C22 C21 C20 120.8(3) . . ? C21 C22 C23 120.1(3) . . ? C24 C23 C22 119.3(3) . . ? C25 C24 C23 120.3(3) . . ? C24 C25 C20 120.4(3) . . ? C31 C26 C27 115.9(3) . . ? C31 C26 P2 120.3(2) . . ? C27 C26 P2 123.1(2) . . ? C28 C27 C26 122.2(3) . . ? C29 C28 C27 118.7(3) . . ? C29 C28 C32 119.9(3) . . ? C27 C28 C32 121.4(3) . . ? C30 C29 C28 120.2(3) . . ? C29 C30 C31 119.6(2) . . ? C29 C30 C33 132.0(3) . . ? C31 C30 C33 108.3(2) . . ? O2 C31 C26 123.6(3) . . ? O2 C31 C30 113.0(2) . . ? C26 C31 C30 123.1(3) . . ? C30 C33 C36 115.7(2) . . ? C30 C33 C34 101.1(2) . . ? C36 C33 C34 102.2(2) . . ? O2 C34 O3 108.2(2) . . ? O2 C34 C33 108.6(2) . . ? O3 C34 C33 106.2(2) . . ? O3 C35 C36 113.5(2) . . ? O3 C35 C40 123.6(3) . 3_667 ? C36 C35 C40 122.9(3) . 3_667 ? C37 C36 C35 120.6(3) . . ? C37 C36 C33 131.5(3) . . ? C35 C36 C33 107.9(2) . . ? C36 C37 C38 118.8(3) . . ? C39 C38 C37 119.7(3) . . ? C39 C38 C41 120.5(3) . . ? C37 C38 C41 119.8(3) . . ? C38 C39 C40 122.8(3) . 3_667 ? C35 C40 C39 115.2(3) 3_667 3_667 ? C35 C40 P1 119.0(2) 3_667 . ? C39 C40 P1 125.4(2) 3_667 . ? 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 C1 Rh1 P1 C8' 121.5(4) . . . . ? P2 Rh1 P1 C8' -141.2(4) . . . . ? Cl1 Rh1 P1 C8' -56.2(4) . . . . ? C1 Rh1 P1 C40 -113.12(13) . . . . ? P2 Rh1 P1 C40 -15.74(14) . . . . ? Cl1 Rh1 P1 C40 69.19(9) . . . . ? C1 Rh1 P1 C2 2.03(14) . . . . ? P2 Rh1 P1 C2 99.41(14) . . . . ? Cl1 Rh1 P1 C2 -175.65(11) . . . . ? C1 Rh1 P1 C8 129.57(15) . . . . ? P2 Rh1 P1 C8 -133.05(14) . . . . ? Cl1 Rh1 P1 C8 -48.12(12) . . . . ? P1 Rh1 C1 O1 -18(6) . . . . ? P2 Rh1 C1 O1 179(100) . . . . ? Cl1 Rh1 C1 O1 39(7) . . . . ? C8' P1 C2 C3 105.4(5) . . . . ? C40 P1 C2 C3 -10.8(3) . . . . ? C8 P1 C2 C3 97.0(3) . . . . ? Rh1 P1 C2 C3 -126.2(3) . . . . ? C8' P1 C2 C7 -67.3(5) . . . . ? C40 P1 C2 C7 176.5(3) . . . . ? C8 P1 C2 C7 -75.7(3) . . . . ? Rh1 P1 C2 C7 61.1(3) . . . . ? C1 Rh1 P2 C14 -138.76(16) . . . . ? P1 Rh1 P2 C14 124.41(15) . . . . ? Cl1 Rh1 P2 C14 39.47(13) . . . . ? C1 Rh1 P2 C26 -15.19(13) . . . . ? P1 Rh1 P2 C26 -112.02(13) . . . . ? Cl1 Rh1 P2 C26 163.04(10) . . . . ? C1 Rh1 P2 C20 102.58(14) . . . . ? P1 Rh1 P2 C20 5.76(15) . . . . ? Cl1 Rh1 P2 C20 -79.19(10) . . . . ? C3 C2 C7 C6 -1.2(6) . . . . ? P1 C2 C7 C6 171.8(3) . . . . ? C2 C7 C6 C5 0.0(6) . . . . ? C7 C6 C5 C4 1.2(6) . . . . ? C6 C5 C4 C3 -1.3(6) . . . . ? C7 C2 C3 C4 1.1(5) . . . . ? P1 C2 C3 C4 -171.5(3) . . . . ? C5 C4 C3 C2 0.2(6) . . . . ? C8' P1 C8 C9 -121(3) . . . . ? C40 P1 C8 C9 63.7(2) . . . . ? C2 P1 C8 C9 -43.3(2) . . . . ? Rh1 P1 C8 C9 -179.35(17) . . . . ? C8' P1 C8 C13 53(3) . . . . ? C40 P1 C8 C13 -122.5(2) . . . . ? C2 P1 C8 C13 130.5(2) . . . . ? Rh1 P1 C8 C13 -5.5(2) . . . . ? C13 C8 C9 C10 0.0 . . . . ? P1 C8 C9 C10 173.68(19) . . . . ? C8 C9 C10 C11 0.0 . . . . ? C9 C10 C11 C12 0.0 . . . . ? C10 C11 C12 C13 0.0 . . . . ? C11 C12 C13 C8 0.0 . . . . ? C9 C8 C13 C12 0.0 . . . . ? P1 C8 C13 C12 -173.93(19) . . . . ? C40 P1 C8' C9' 60.9(11) . . . . ? C2 P1 C8' C9' -47.7(11) . . . . ? C8 P1 C8' C9' 56(2) . . . . ? Rh1 P1 C8' C9' -178.3(9) . . . . ? C40 P1 C8' C13' -122.0(10) . . . . ? C2 P1 C8' C13' 129.4(10) . . . . ? C8 P1 C8' C13' -127(3) . . . . ? Rh1 P1 C8' C13' -1.3(12) . . . . ? C13' C8' C9' C10' -1(2) . . . . ? P1 C8' C9' C10' 175.9(11) . . . . ? C8' C9' C10' C11' 5(2) . . . . ? C9' C10' C11' C12' -6(2) . . . . ? C10' C11' C12' C13' 5(2) . . . . ? C11' C12' C13' C8' -2(3) . . . . ? C9' C8' C13' C12' 0(2) . . . . ? P1 C8' C13' C12' -176.8(13) . . . . ? C26 P2 C14 C19 90.9(3) . . . . ? C20 P2 C14 C19 -18.8(3) . . . . ? Rh1 P2 C14 C19 -139.9(3) . . . . ? C26 P2 C14 C15 -88.7(3) . . . . ? C20 P2 C14 C15 161.6(3) . . . . ? Rh1 P2 C14 C15 40.5(4) . . . . ? C19 C14 C15 C16 -0.5(6) . . . . ? P2 C14 C15 C16 179.2(4) . . . . ? C14 C15 C16 C17 1.0(7) . . . . ? C15 C16 C17 C18 -0.2(7) . . . . ? C16 C17 C18 C19 -1.2(7) . . . . ? C15 C14 C19 C18 -0.9(6) . . . . ? P2 C14 C19 C18 179.4(3) . . . . ? C17 C18 C19 C14 1.8(6) . . . . ? C14 P2 C20 C21 100.6(3) . . . . ? C26 P2 C20 C21 -8.8(3) . . . . ? Rh1 P2 C20 C21 -133.3(3) . . . . ? C14 P2 C20 C25 -82.3(3) . . . . ? C26 P2 C20 C25 168.3(2) . . . . ? Rh1 P2 C20 C25 43.8(3) . . . . ? C25 C20 C21 C22 -3.0(5) . . . . ? P2 C20 C21 C22 174.1(3) . . . . ? C20 C21 C22 C23 1.5(5) . . . . ? C21 C22 C23 C24 1.6(5) . . . . ? C22 C23 C24 C25 -3.2(5) . . . . ? C23 C24 C25 C20 1.7(5) . . . . ? C21 C20 C25 C24 1.4(5) . . . . ? P2 C20 C25 C24 -175.8(2) . . . . ? C14 P2 C26 C31 -169.8(2) . . . . ? C20 P2 C26 C31 -60.0(3) . . . . ? Rh1 P2 C26 C31 60.2(3) . . . . ? C14 P2 C26 C27 20.7(3) . . . . ? C20 P2 C26 C27 130.4(3) . . . . ? Rh1 P2 C26 C27 -109.3(3) . . . . ? C31 C26 C27 C28 -0.9(4) . . . . ? P2 C26 C27 C28 169.1(2) . . . . ? C26 C27 C28 C29 -2.3(5) . . . . ? C26 C27 C28 C32 -179.3(3) . . . . ? C27 C28 C29 C30 1.3(5) . . . . ? C32 C28 C29 C30 178.3(3) . . . . ? C28 C29 C30 C31 2.8(4) . . . . ? C28 C29 C30 C33 -174.3(3) . . . . ? C34 O2 C31 C26 -179.6(3) . . . . ? C34 O2 C31 C30 -4.9(3) . . . . ? C27 C26 C31 O2 179.4(3) . . . . ? P2 C26 C31 O2 9.1(4) . . . . ? C27 C26 C31 C30 5.2(4) . . . . ? P2 C26 C31 C30 -165.1(2) . . . . ? C29 C30 C31 O2 178.9(3) . . . . ? C33 C30 C31 O2 -3.3(3) . . . . ? C29 C30 C31 C26 -6.4(4) . . . . ? C33 C30 C31 C26 171.4(3) . . . . ? C29 C30 C33 C36 -63.9(4) . . . . ? C31 C30 C33 C36 118.7(3) . . . . ? C29 C30 C33 C34 -173.4(3) . . . . ? C31 C30 C33 C34 9.2(3) . . . . ? C31 O2 C34 O3 -103.9(2) . . . . ? C31 O2 C34 C33 10.9(3) . . . . ? C35 O3 C34 O2 133.1(2) . . . . ? C35 O3 C34 C33 16.7(3) . . . . ? C30 C33 C34 O2 -12.2(3) . . . . ? C36 C33 C34 O2 -131.9(2) . . . . ? C30 C33 C34 O3 103.9(2) . . . . ? C36 C33 C34 O3 -15.8(3) . . . . ? C34 O3 C35 C36 -11.0(3) . . . . ? C34 O3 C35 C40 168.9(3) . . . 3_667 ? O3 C35 C36 C37 -178.3(3) . . . . ? C40 C35 C36 C37 1.7(4) 3_667 . . . ? O3 C35 C36 C33 0.3(3) . . . . ? C40 C35 C36 C33 -179.6(3) 3_667 . . . ? C30 C33 C36 C37 79.2(4) . . . . ? C34 C33 C36 C37 -171.9(3) . . . . ? C30 C33 C36 C35 -99.2(3) . . . . ? C34 C33 C36 C35 9.6(3) . . . . ? C35 C36 C37 C38 -0.7(4) . . . . ? C33 C36 C37 C38 -179.0(3) . . . . ? C36 C37 C38 C39 -0.3(4) . . . . ? C36 C37 C38 C41 -179.5(3) . . . . ? C37 C38 C39 C40 0.5(5) . . . 3_667 ? C41 C38 C39 C40 179.6(3) . . . 3_667 ? C8' P1 C40 C35 178.8(4) . . . 3_667 ? C2 P1 C40 C35 -75.9(3) . . . 3_667 ? C8 P1 C40 C35 179.5(2) . . . 3_667 ? Rh1 P1 C40 C35 50.8(2) . . . 3_667 ? C8' P1 C40 C39 5.5(5) . . . 3_667 ? C2 P1 C40 C39 110.8(3) . . . 3_667 ? C8 P1 C40 C39 6.2(3) . . . 3_667 ? Rh1 P1 C40 C39 -122.5(3) . . . 3_667 ? _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 36.54 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 3.597 _refine_diff_density_min -1.773 _refine_diff_density_rms 0.206 #===END data_jm147_0m_20 _database_code_depnum_ccdc_archive 'CCDC 762012' #TrackingRef '1764_web_deposit_cif_file_0_EduardoC.Escudero-Adan_1279182185.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H76 Cl10 O6 P4 Rh2' _chemical_formula_weight 1913.69 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' _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 12.7468(5) _cell_length_b 18.3066(7) _cell_length_c 19.1337(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.1580(10) _cell_angle_gamma 90.00 _cell_volume 4309.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8038 _cell_measurement_theta_min 3.28 _cell_measurement_theta_max 39.41 _exptl_crystal_description block _exptl_crystal_colour colourless _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 1.475 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.819 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 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 70 _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_reflns_number 65761 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 37.50 _reflns_number_total 21725 _reflns_number_gt 18426 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. 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. Two dichloromethane molecules are present in the asymmetric unit. The molecules are disordered in two positions with occupation ratio of 61:39. Anisotropic displacements and distances retrains have been applied to these solvent 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^)+(0.0654P)^2^+5.9236P] 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 21725 _refine_ls_number_parameters 538 _refine_ls_number_restraints 57 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1385 _refine_ls_wR_factor_gt 0.1284 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.089 _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 0.165828(8) 0.435370(6) 0.180232(6) 0.01451(2) Uani 1 1 d . . . Cl1 Cl 0.21405(4) 0.53280(2) 0.26589(2) 0.02645(8) Uani 1 1 d . . . P1 P 0.03545(3) 0.40578(2) 0.24076(2) 0.01497(6) Uani 1 1 d . . . O1 O 0.11671(14) 0.30457(8) 0.08688(9) 0.0335(3) Uani 1 1 d . . . C1 C 0.13475(14) 0.35601(9) 0.12184(9) 0.0220(3) Uani 1 1 d . . . O2 O -0.04899(10) 0.50973(6) 0.12632(6) 0.01849(19) Uani 1 1 d . . . P2 P 0.29189(3) 0.48076(2) 0.12234(2) 0.01611(6) Uani 1 1 d . . . C2 C -0.07269(12) 0.33935(8) 0.20644(8) 0.0172(2) Uani 1 1 d . . . O3 O -0.12049(8) 0.55474(6) 0.01070(6) 0.01684(18) Uani 1 1 d . . . C3 C -0.18274(13) 0.35688(10) 0.19400(10) 0.0236(3) Uani 1 1 d . . . H3 H -0.2039 0.4061 0.1985 0.028 Uiso 1 1 calc R . . C4 C -0.26142(15) 0.30247(12) 0.17508(12) 0.0308(4) Uani 1 1 d . . . H4 H -0.3361 0.3147 0.1669 0.037 Uiso 1 1 calc R . . C5 C -0.23168(16) 0.23055(11) 0.16812(13) 0.0317(4) Uani 1 1 d . . . H5 H -0.2857 0.1936 0.1554 0.038 Uiso 1 1 calc R . . C6 C -0.12183(16) 0.21262(10) 0.17988(12) 0.0291(4) Uani 1 1 d . . . H6 H -0.1009 0.1634 0.1753 0.035 Uiso 1 1 calc R . . C7 C -0.04356(14) 0.26689(9) 0.19825(10) 0.0227(3) Uani 1 1 d . . . H7 H 0.0309 0.2546 0.2054 0.027 Uiso 1 1 calc R . . C8 C 0.09288(12) 0.37192(8) 0.33242(8) 0.0178(2) Uani 1 1 d . . . C9 C 0.02719(14) 0.34516(9) 0.37530(9) 0.0208(3) Uani 1 1 d . . . H9 H -0.0497 0.3452 0.3571 0.025 Uiso 1 1 calc R . . C10 C 0.07491(16) 0.31851(9) 0.44448(9) 0.0239(3) Uani 1 1 d . . . H10 H 0.0305 0.3017 0.4740 0.029 Uiso 1 1 calc R . . C11 C 0.18717(17) 0.31641(10) 0.47038(9) 0.0264(3) Uani 1 1 d . . . H11 H 0.2193 0.2972 0.5172 0.032 Uiso 1 1 calc R . . C12 C 0.25264(15) 0.34218(10) 0.42832(9) 0.0257(3) Uani 1 1 d . . . H12 H 0.3295 0.3408 0.4464 0.031 Uiso 1 1 calc R . . C13 C 0.20578(13) 0.37012(9) 0.35946(9) 0.0218(3) Uani 1 1 d . . . H13 H 0.2508 0.3880 0.3308 0.026 Uiso 1 1 calc R . . C14 C -0.03875(12) 0.48862(8) 0.25022(8) 0.0166(2) Uani 1 1 d . . . C15 C -0.06287(13) 0.51119(9) 0.31400(8) 0.0197(2) Uani 1 1 d . . . H15 H -0.0438 0.4806 0.3555 0.024 Uiso 1 1 calc R . . C16 C -0.11453(14) 0.57794(9) 0.31791(9) 0.0212(3) Uani 1 1 d . . . C17 C -0.13745(12) 0.62368(8) 0.25768(8) 0.0189(2) Uani 1 1 d . . . H17 H -0.1709 0.6696 0.2602 0.023 Uiso 1 1 calc R . . C18 C -0.11238(11) 0.60355(8) 0.19390(8) 0.0166(2) Uani 1 1 d . . . C19 C -0.06754(11) 0.53478(8) 0.18978(8) 0.0162(2) Uani 1 1 d . . . C20 C -0.12405(11) 0.65256(8) 0.12909(8) 0.0174(2) Uani 1 1 d . . . H20 H -0.1269 0.7048 0.1436 0.021 Uiso 1 1 calc R . . C21 C -0.02271(12) 0.63900(9) 0.10189(9) 0.0192(2) Uani 1 1 d . . . H21A H -0.0200 0.6738 0.0628 0.023 Uiso 1 1 calc R . . H21B H 0.0441 0.6449 0.1418 0.023 Uiso 1 1 calc R . . C22 C -0.03239(11) 0.56172(8) 0.07379(8) 0.0169(2) Uani 1 1 d . . . H22 H 0.0363 0.5488 0.0608 0.020 Uiso 1 1 calc R . . C23 C -0.1437(2) 0.60113(12) 0.38614(11) 0.0329(4) Uani 1 1 d . . . H23A H -0.1261 0.6529 0.3955 0.049 Uiso 1 1 calc R . . H23B H -0.1022 0.5719 0.4270 0.049 Uiso 1 1 calc R . . H23C H -0.2216 0.5936 0.3803 0.049 Uiso 1 1 calc R . . C24 C 0.30816(11) 0.42892(8) 0.04395(8) 0.0167(2) Uani 1 1 d . . . C25 C 0.21701(11) 0.41313(8) -0.01364(8) 0.0161(2) Uani 1 1 d . . . C26 C 0.22453(11) 0.36644(8) -0.06961(8) 0.0167(2) Uani 1 1 d . . . C27 C 0.32547(12) 0.33663(8) -0.06899(9) 0.0190(2) Uani 1 1 d . . . H27 H 0.3313 0.3057 -0.1077 0.023 Uiso 1 1 calc R . . C28 C 0.41803(12) 0.35091(9) -0.01311(9) 0.0208(3) Uani 1 1 d . . . C29 C 0.40763(12) 0.39687(9) 0.04291(9) 0.0194(2) Uani 1 1 d . . . H29 H 0.4699 0.4067 0.0815 0.023 Uiso 1 1 calc R . . C30 C 0.52508(14) 0.31571(12) -0.01219(11) 0.0292(4) Uani 1 1 d . . . H30A H 0.5846 0.3487 0.0110 0.044 Uiso 1 1 calc R . . H30B H 0.5280 0.3058 -0.0620 0.044 Uiso 1 1 calc R . . H30C H 0.5323 0.2698 0.0150 0.044 Uiso 1 1 calc R . . C31 C 0.42901(12) 0.48075(9) 0.18226(9) 0.0203(3) Uani 1 1 d . . . C32 C 0.51307(14) 0.52189(11) 0.16782(11) 0.0275(3) Uani 1 1 d . . . H32 H 0.4988 0.5538 0.1272 0.033 Uiso 1 1 calc R . . C33 C 0.61803(15) 0.51621(13) 0.21298(14) 0.0350(4) Uani 1 1 d . . . H33 H 0.6753 0.5439 0.2027 0.042 Uiso 1 1 calc R . . C34 C 0.63936(16) 0.47059(15) 0.27259(13) 0.0369(5) Uani 1 1 d . . . H34 H 0.7108 0.4676 0.3036 0.044 Uiso 1 1 calc R . . C35 C 0.55657(17) 0.42929(16) 0.28711(13) 0.0396(5) Uani 1 1 d . . . H35 H 0.5713 0.3974 0.3277 0.048 Uiso 1 1 calc R . . C36 C 0.45149(15) 0.43458(12) 0.24208(11) 0.0302(4) Uani 1 1 d . . . H36 H 0.3947 0.4064 0.2523 0.036 Uiso 1 1 calc R . . C37 C 0.26906(12) 0.57638(8) 0.09323(9) 0.0200(3) Uani 1 1 d . . . C38 C 0.22044(13) 0.59660(9) 0.02149(10) 0.0232(3) Uani 1 1 d . . . H38 H 0.2038 0.5604 -0.0153 0.028 Uiso 1 1 calc R . . C39 C 0.19627(14) 0.66967(10) 0.00384(12) 0.0278(3) Uani 1 1 d . . . H39 H 0.1623 0.6828 -0.0449 0.033 Uiso 1 1 calc R . . C40 C 0.22146(16) 0.72343(10) 0.05697(13) 0.0313(4) Uani 1 1 d . . . H40 H 0.2047 0.7731 0.0447 0.038 Uiso 1 1 calc R . . C41 C 0.27108(18) 0.70407(10) 0.12784(13) 0.0320(4) Uani 1 1 d . . . H41 H 0.2891 0.7407 0.1642 0.038 Uiso 1 1 calc R . . C42 C 0.29476(16) 0.63106(10) 0.14631(11) 0.0266(3) Uani 1 1 d . . . H42 H 0.3285 0.6183 0.1951 0.032 Uiso 1 1 calc R . . C1V C 0.4043(7) 0.2497(3) 0.6781(2) 0.082(2) Uani 0.606(2) 1 d PDU A 1 H1VA H 0.3262 0.2439 0.6533 0.098 Uiso 0.606(2) 1 calc PR A 1 H1VB H 0.4409 0.2029 0.6738 0.098 Uiso 0.606(2) 1 calc PR A 1 Cl1V Cl 0.41766(17) 0.26788(11) 0.76853(9) 0.0770(5) Uani 0.606(2) 1 d PDU A 1 Cl2V Cl 0.4584(2) 0.31745(17) 0.63435(16) 0.0988(7) Uani 0.606(2) 1 d PDU A 1 C1V' C 0.4780(13) 0.3518(5) 0.6653(5) 0.161(4) Uani 0.394(2) 1 d PDU A 2 H1V1 H 0.4225 0.3794 0.6821 0.193 Uiso 0.394(2) 1 calc PR A 2 H1V2 H 0.5450 0.3470 0.7053 0.193 Uiso 0.394(2) 1 calc PR A 2 Cl1' Cl 0.4294(5) 0.2669(4) 0.6278(3) 0.1403(19) Uani 0.394(2) 1 d PDU A 2 Cl2' Cl 0.5031(7) 0.3896(5) 0.5875(5) 0.258(4) Uani 0.394(2) 1 d PDU A 2 Cl1W Cl 0.13851(13) 0.57372(6) 0.49708(7) 0.0888(4) Uani 1 1 d D . . C1W C 0.2212(5) 0.5243(6) 0.4574(3) 0.0775(16) Uani 0.394(2) 1 d PDU A 2 H1WA H 0.2335 0.5509 0.4152 0.093 Uiso 0.394(2) 1 calc PR A 2 H1WB H 0.1879 0.4764 0.4407 0.093 Uiso 0.394(2) 1 calc PR A 2 Cl2W Cl 0.3432(2) 0.51227(19) 0.52282(16) 0.0813(9) Uani 0.394(2) 1 d PD A 2 C1W' C 0.2505(3) 0.5486(3) 0.4649(4) 0.0775(16) Uani 0.606(2) 1 d PDU A 1 H1WC H 0.2264 0.5488 0.4114 0.093 Uiso 0.606(2) 1 calc PR A 1 H1WD H 0.2692 0.4975 0.4801 0.093 Uiso 0.606(2) 1 calc PR A 1 Cl3W Cl 0.3710(3) 0.60040(18) 0.49078(14) 0.1169(10) Uani 0.606(2) 1 d PD A 1 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 0.01432(4) 0.01498(4) 0.01556(4) -0.00032(3) 0.00626(3) -0.00019(3) Cl1 0.02909(17) 0.02484(16) 0.02797(17) -0.00589(13) 0.01199(14) -0.00516(13) P1 0.01545(13) 0.01602(14) 0.01457(13) 0.00054(11) 0.00594(11) 0.00031(11) O1 0.0492(8) 0.0234(6) 0.0352(7) -0.0046(5) 0.0239(6) -0.0065(6) C1 0.0247(6) 0.0223(6) 0.0223(6) 0.0006(5) 0.0121(5) -0.0021(5) O2 0.0237(4) 0.0176(4) 0.0163(4) 0.0004(3) 0.0089(4) 0.0038(4) P2 0.01387(13) 0.01687(14) 0.01880(15) 0.00116(11) 0.00641(11) -0.00032(11) C2 0.0171(5) 0.0176(5) 0.0180(5) 0.0007(4) 0.0062(4) -0.0005(4) O3 0.0132(4) 0.0202(4) 0.0183(4) 0.0002(3) 0.0063(3) 0.0026(3) C3 0.0174(5) 0.0238(7) 0.0300(7) -0.0024(6) 0.0069(5) 0.0000(5) C4 0.0189(6) 0.0317(8) 0.0419(10) -0.0027(7) 0.0079(6) -0.0042(6) C5 0.0267(7) 0.0273(8) 0.0410(10) -0.0009(7) 0.0084(7) -0.0096(6) C6 0.0281(7) 0.0191(6) 0.0394(9) -0.0001(6) 0.0075(7) -0.0038(5) C7 0.0215(6) 0.0171(6) 0.0293(7) 0.0011(5) 0.0060(5) 0.0003(5) C8 0.0196(5) 0.0183(5) 0.0163(5) 0.0010(4) 0.0061(4) 0.0014(4) C9 0.0253(6) 0.0204(6) 0.0186(6) 0.0007(5) 0.0092(5) 0.0007(5) C10 0.0349(8) 0.0213(6) 0.0179(6) 0.0004(5) 0.0111(6) 0.0027(6) C11 0.0368(8) 0.0251(7) 0.0164(6) 0.0006(5) 0.0052(6) 0.0074(6) C12 0.0261(7) 0.0282(7) 0.0207(6) 0.0003(5) 0.0022(5) 0.0048(6) C13 0.0207(6) 0.0249(7) 0.0197(6) 0.0010(5) 0.0050(5) 0.0024(5) C14 0.0175(5) 0.0167(5) 0.0169(5) -0.0009(4) 0.0068(4) 0.0006(4) C15 0.0230(6) 0.0195(6) 0.0181(5) -0.0016(4) 0.0082(5) 0.0007(5) C16 0.0249(6) 0.0209(6) 0.0201(6) -0.0040(5) 0.0100(5) 0.0002(5) C17 0.0197(5) 0.0175(5) 0.0212(6) -0.0038(4) 0.0084(5) 0.0000(4) C18 0.0156(5) 0.0162(5) 0.0189(5) -0.0015(4) 0.0063(4) -0.0001(4) C19 0.0165(5) 0.0168(5) 0.0166(5) -0.0012(4) 0.0069(4) 0.0010(4) C20 0.0162(5) 0.0156(5) 0.0217(6) -0.0007(4) 0.0072(4) -0.0001(4) C21 0.0161(5) 0.0198(6) 0.0237(6) 0.0002(5) 0.0084(5) -0.0018(4) C22 0.0142(5) 0.0194(5) 0.0182(5) 0.0015(4) 0.0064(4) 0.0014(4) C23 0.0493(11) 0.0295(8) 0.0254(7) -0.0046(6) 0.0195(8) 0.0064(8) C24 0.0144(5) 0.0181(5) 0.0191(5) 0.0017(4) 0.0072(4) 0.0006(4) C25 0.0140(4) 0.0168(5) 0.0193(5) 0.0016(4) 0.0078(4) 0.0013(4) C26 0.0149(5) 0.0163(5) 0.0205(5) 0.0011(4) 0.0076(4) 0.0009(4) C27 0.0167(5) 0.0197(6) 0.0228(6) 0.0001(5) 0.0091(5) 0.0020(4) C28 0.0151(5) 0.0240(6) 0.0255(6) 0.0014(5) 0.0092(5) 0.0030(4) C29 0.0141(5) 0.0234(6) 0.0222(6) 0.0016(5) 0.0073(4) 0.0010(4) C30 0.0177(6) 0.0385(9) 0.0338(8) -0.0014(7) 0.0109(6) 0.0082(6) C31 0.0159(5) 0.0229(6) 0.0228(6) -0.0010(5) 0.0061(5) -0.0009(4) C32 0.0180(6) 0.0273(7) 0.0371(9) -0.0008(6) 0.0073(6) -0.0050(5) C33 0.0180(6) 0.0371(10) 0.0487(12) -0.0083(8) 0.0069(7) -0.0060(6) C34 0.0177(6) 0.0500(12) 0.0394(10) -0.0094(9) 0.0013(7) 0.0020(7) C35 0.0221(7) 0.0590(14) 0.0345(10) 0.0093(9) 0.0016(7) 0.0074(8) C36 0.0180(6) 0.0419(10) 0.0296(8) 0.0096(7) 0.0041(6) 0.0015(6) C37 0.0185(5) 0.0173(5) 0.0266(7) 0.0022(5) 0.0102(5) -0.0005(4) C38 0.0207(6) 0.0209(6) 0.0289(7) 0.0056(5) 0.0083(5) -0.0009(5) C39 0.0224(6) 0.0235(7) 0.0391(9) 0.0112(6) 0.0111(6) 0.0016(5) C40 0.0291(7) 0.0197(6) 0.0507(11) 0.0070(7) 0.0203(8) 0.0030(6) C41 0.0393(9) 0.0188(7) 0.0439(10) -0.0010(6) 0.0216(8) 0.0000(6) C42 0.0327(8) 0.0198(6) 0.0308(8) -0.0004(6) 0.0145(6) -0.0014(6) C1V 0.107(4) 0.083(4) 0.059(3) -0.001(3) 0.029(3) 0.000(3) Cl1V 0.0939(11) 0.0758(10) 0.0689(9) -0.0116(7) 0.0352(8) 0.0209(9) Cl2V 0.0815(11) 0.1081(14) 0.1136(13) 0.0003(11) 0.0375(10) -0.0002(10) C1V' 0.160(4) 0.162(4) 0.161(4) -0.0041(19) 0.0419(19) 0.0015(19) Cl1' 0.126(3) 0.144(3) 0.144(3) -0.016(3) 0.024(3) 0.026(3) Cl2' 0.253(6) 0.256(6) 0.256(6) 0.000(4) 0.052(4) 0.000(4) Cl1W 0.1307(11) 0.0533(5) 0.0819(7) 0.0007(5) 0.0268(7) -0.0206(6) C1W 0.105(3) 0.064(3) 0.056(2) -0.011(2) 0.008(2) -0.003(2) Cl2W 0.0634(14) 0.103(2) 0.0735(16) -0.0137(15) 0.0102(12) -0.0074(14) C1W' 0.105(3) 0.064(3) 0.056(2) -0.011(2) 0.008(2) -0.003(2) Cl3W 0.137(2) 0.127(2) 0.0888(15) 0.0330(15) 0.0326(15) 0.0177(18) _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 C1 1.8123(17) . ? Rh1 P1 2.3245(4) . ? Rh1 P2 2.3304(4) . ? Rh1 Cl1 2.3914(4) . ? P1 C14 1.8211(15) . ? P1 C8 1.8234(15) . ? P1 C2 1.8268(15) . ? O1 C1 1.143(2) . ? O2 C19 1.3751(18) . ? O2 C22 1.4395(19) . ? P2 C31 1.8225(15) . ? P2 C24 1.8320(16) . ? P2 C37 1.8368(16) . ? C2 C7 1.397(2) . ? C2 C3 1.397(2) . ? O3 C25 1.3780(17) 3_565 ? O3 C22 1.4233(18) . ? C3 C4 1.393(3) . ? C4 C5 1.386(3) . ? C5 C6 1.398(3) . ? C6 C7 1.387(2) . ? C8 C13 1.397(2) . ? C8 C9 1.405(2) . ? C9 C10 1.392(2) . ? C10 C11 1.387(3) . ? C11 C12 1.385(3) . ? C12 C13 1.394(2) . ? C14 C15 1.397(2) . ? C14 C19 1.401(2) . ? C15 C16 1.399(2) . ? C16 C17 1.392(2) . ? C16 C23 1.508(2) . ? C17 C18 1.390(2) . ? C18 C19 1.393(2) . ? C18 C20 1.506(2) . ? C20 C26 1.515(2) 3_565 ? C20 C21 1.534(2) . ? C21 C22 1.507(2) . ? C24 C29 1.402(2) . ? C24 C25 1.406(2) . ? C25 O3 1.3780(17) 3_565 ? C25 C26 1.393(2) . ? C26 C27 1.395(2) . ? C26 C20 1.515(2) 3_565 ? C27 C28 1.394(2) . ? C28 C29 1.396(2) . ? C28 C30 1.505(2) . ? C31 C36 1.391(3) . ? C31 C32 1.395(2) . ? C32 C33 1.394(3) . ? C33 C34 1.382(4) . ? C34 C35 1.384(4) . ? C35 C36 1.394(3) . ? C37 C38 1.400(2) . ? C37 C42 1.403(2) . ? C38 C39 1.394(2) . ? C39 C40 1.391(3) . ? C40 C41 1.384(3) . ? C41 C42 1.395(3) . ? C1V Cl1V 1.727(4) . ? C1V Cl2V 1.736(4) . ? C1V' Cl2' 1.746(5) . ? C1V' Cl1' 1.755(5) . ? Cl1W C1W 1.711(5) . ? Cl1W C1W' 1.757(4) . ? C1W Cl2W 1.736(4) . ? C1W' Cl3W 1.762(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 C1 Rh1 P1 92.91(5) . . ? C1 Rh1 P2 93.42(5) . . ? P1 Rh1 P2 172.581(14) . . ? C1 Rh1 Cl1 174.89(6) . . ? P1 Rh1 Cl1 85.496(15) . . ? P2 Rh1 Cl1 88.521(15) . . ? C14 P1 C8 106.01(7) . . ? C14 P1 C2 103.14(7) . . ? C8 P1 C2 101.24(7) . . ? C14 P1 Rh1 108.24(5) . . ? C8 P1 Rh1 113.51(5) . . ? C2 P1 Rh1 123.14(5) . . ? O1 C1 Rh1 177.80(17) . . ? C19 O2 C22 119.12(12) . . ? C31 P2 C24 102.69(7) . . ? C31 P2 C37 103.93(7) . . ? C24 P2 C37 106.75(7) . . ? C31 P2 Rh1 111.59(6) . . ? C24 P2 Rh1 116.37(5) . . ? C37 P2 Rh1 114.19(5) . . ? C7 C2 C3 118.91(14) . . ? C7 C2 P1 118.33(11) . . ? C3 C2 P1 122.53(12) . . ? C25 O3 C22 116.23(12) 3_565 . ? C4 C3 C2 120.17(16) . . ? C5 C4 C3 120.53(17) . . ? C4 C5 C6 119.68(17) . . ? C7 C6 C5 119.78(17) . . ? C6 C7 C2 120.92(16) . . ? C13 C8 C9 119.29(14) . . ? C13 C8 P1 118.68(12) . . ? C9 C8 P1 121.98(12) . . ? C10 C9 C8 119.89(16) . . ? C11 C10 C9 120.19(17) . . ? C12 C11 C10 120.33(16) . . ? C11 C12 C13 120.00(17) . . ? C12 C13 C8 120.28(16) . . ? C15 C14 C19 118.20(13) . . ? C15 C14 P1 124.88(11) . . ? C19 C14 P1 116.80(11) . . ? C14 C15 C16 121.28(14) . . ? C17 C16 C15 118.73(15) . . ? C17 C16 C23 120.08(15) . . ? C15 C16 C23 121.18(16) . . ? C18 C17 C16 121.39(14) . . ? C17 C18 C19 118.76(14) . . ? C17 C18 C20 124.70(13) . . ? C19 C18 C20 116.45(13) . . ? O2 C19 C18 121.27(13) . . ? O2 C19 C14 117.33(12) . . ? C18 C19 C14 121.40(13) . . ? C18 C20 C26 111.35(12) . 3_565 ? C18 C20 C21 105.81(12) . . ? C26 C20 C21 109.24(12) 3_565 . ? C22 C21 C20 105.98(12) . . ? O3 C22 O2 107.77(11) . . ? O3 C22 C21 111.09(12) . . ? O2 C22 C21 112.64(12) . . ? C29 C24 C25 117.89(14) . . ? C29 C24 P2 121.66(11) . . ? C25 C24 P2 120.05(11) . . ? O3 C25 C26 122.34(12) 3_565 . ? O3 C25 C24 116.34(13) 3_565 . ? C26 C25 C24 121.31(13) . . ? C25 C26 C27 118.84(13) . . ? C25 C26 C20 120.26(12) . 3_565 ? C27 C26 C20 120.89(13) . 3_565 ? C28 C27 C26 121.79(14) . . ? C27 C28 C29 118.08(14) . . ? C27 C28 C30 120.76(15) . . ? C29 C28 C30 121.13(15) . . ? C28 C29 C24 122.07(14) . . ? C36 C31 C32 119.16(15) . . ? C36 C31 P2 118.37(13) . . ? C32 C31 P2 122.36(13) . . ? C33 C32 C31 119.96(19) . . ? C34 C33 C32 120.43(19) . . ? C33 C34 C35 120.00(18) . . ? C34 C35 C36 119.9(2) . . ? C31 C36 C35 120.59(19) . . ? C38 C37 C42 118.75(15) . . ? C38 C37 P2 122.93(13) . . ? C42 C37 P2 118.17(13) . . ? C39 C38 C37 120.29(17) . . ? C40 C39 C38 120.50(18) . . ? C41 C40 C39 119.60(17) . . ? C40 C41 C42 120.44(19) . . ? C41 C42 C37 120.41(18) . . ? Cl1V C1V Cl2V 113.4(3) . . ? Cl2' C1V' Cl1' 97.2(6) . . ? C1W Cl1W C1W' 19.0(4) . . ? Cl1W C1W Cl2W 106.6(3) . . ? Cl1W C1W' Cl3W 119.3(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 C1 Rh1 P1 C14 -135.57(7) . . . . ? P2 Rh1 P1 C14 12.95(12) . . . . ? Cl1 Rh1 P1 C14 49.30(5) . . . . ? C1 Rh1 P1 C8 107.03(8) . . . . ? P2 Rh1 P1 C8 -104.45(12) . . . . ? Cl1 Rh1 P1 C8 -68.10(6) . . . . ? C1 Rh1 P1 C2 -15.50(8) . . . . ? P2 Rh1 P1 C2 133.02(11) . . . . ? Cl1 Rh1 P1 C2 169.36(6) . . . . ? P1 Rh1 C1 O1 -72(4) . . . . ? P2 Rh1 C1 O1 112(4) . . . . ? Cl1 Rh1 C1 O1 -1(5) . . . . ? C1 Rh1 P2 C31 -114.50(8) . . . . ? P1 Rh1 P2 C31 97.00(12) . . . . ? Cl1 Rh1 P2 C31 60.77(6) . . . . ? C1 Rh1 P2 C24 2.89(8) . . . . ? P1 Rh1 P2 C24 -145.62(11) . . . . ? Cl1 Rh1 P2 C24 178.15(5) . . . . ? C1 Rh1 P2 C37 128.02(8) . . . . ? P1 Rh1 P2 C37 -20.49(13) . . . . ? Cl1 Rh1 P2 C37 -56.72(6) . . . . ? C14 P1 C2 C7 -175.01(13) . . . . ? C8 P1 C2 C7 -65.43(14) . . . . ? Rh1 P1 C2 C7 62.56(14) . . . . ? C14 P1 C2 C3 -0.55(15) . . . . ? C8 P1 C2 C3 109.04(14) . . . . ? Rh1 P1 C2 C3 -122.98(13) . . . . ? C7 C2 C3 C4 1.2(3) . . . . ? P1 C2 C3 C4 -173.27(15) . . . . ? C2 C3 C4 C5 -0.2(3) . . . . ? C3 C4 C5 C6 -0.3(3) . . . . ? C4 C5 C6 C7 -0.1(3) . . . . ? C5 C6 C7 C2 1.1(3) . . . . ? C3 C2 C7 C6 -1.6(3) . . . . ? P1 C2 C7 C6 173.07(15) . . . . ? C14 P1 C8 C13 -115.43(13) . . . . ? C2 P1 C8 C13 137.22(13) . . . . ? Rh1 P1 C8 C13 3.25(14) . . . . ? C14 P1 C8 C9 67.04(14) . . . . ? C2 P1 C8 C9 -40.31(14) . . . . ? Rh1 P1 C8 C9 -174.27(11) . . . . ? C13 C8 C9 C10 1.2(2) . . . . ? P1 C8 C9 C10 178.72(12) . . . . ? C8 C9 C10 C11 -1.8(2) . . . . ? C9 C10 C11 C12 1.4(3) . . . . ? C10 C11 C12 C13 -0.3(3) . . . . ? C11 C12 C13 C8 -0.3(3) . . . . ? C9 C8 C13 C12 -0.1(2) . . . . ? P1 C8 C13 C12 -177.72(13) . . . . ? C8 P1 C14 C15 -11.43(15) . . . . ? C2 P1 C14 C15 94.55(14) . . . . ? Rh1 P1 C14 C15 -133.54(12) . . . . ? C8 P1 C14 C19 164.54(11) . . . . ? C2 P1 C14 C19 -89.48(12) . . . . ? Rh1 P1 C14 C19 42.43(12) . . . . ? C19 C14 C15 C16 0.1(2) . . . . ? P1 C14 C15 C16 176.03(12) . . . . ? C14 C15 C16 C17 -2.9(2) . . . . ? C14 C15 C16 C23 178.06(17) . . . . ? C15 C16 C17 C18 1.5(2) . . . . ? C23 C16 C17 C18 -179.47(17) . . . . ? C16 C17 C18 C19 2.7(2) . . . . ? C16 C17 C18 C20 -173.58(14) . . . . ? C22 O2 C19 C18 25.6(2) . . . . ? C22 O2 C19 C14 -153.88(13) . . . . ? C17 C18 C19 O2 174.88(13) . . . . ? C20 C18 C19 O2 -8.5(2) . . . . ? C17 C18 C19 C14 -5.6(2) . . . . ? C20 C18 C19 C14 170.95(13) . . . . ? C15 C14 C19 O2 -176.25(13) . . . . ? P1 C14 C19 O2 7.50(18) . . . . ? C15 C14 C19 C18 4.2(2) . . . . ? P1 C14 C19 C18 -172.01(11) . . . . ? C17 C18 C20 C26 -102.84(16) . . . 3_565 ? C19 C18 C20 C26 80.80(16) . . . 3_565 ? C17 C18 C20 C21 138.58(15) . . . . ? C19 C18 C20 C21 -37.77(16) . . . . ? C18 C20 C21 C22 67.15(14) . . . . ? C26 C20 C21 C22 -52.82(15) 3_565 . . . ? C25 O3 C22 O2 78.04(15) 3_565 . . . ? C25 O3 C22 C21 -45.79(17) 3_565 . . . ? C19 O2 C22 O3 -114.93(13) . . . . ? C19 O2 C22 C21 7.96(18) . . . . ? C20 C21 C22 O3 67.41(15) . . . . ? C20 C21 C22 O2 -53.60(15) . . . . ? C31 P2 C24 C29 3.77(14) . . . . ? C37 P2 C24 C29 112.76(13) . . . . ? Rh1 P2 C24 C29 -118.42(12) . . . . ? C31 P2 C24 C25 176.32(12) . . . . ? C37 P2 C24 C25 -74.68(13) . . . . ? Rh1 P2 C24 C25 54.14(13) . . . . ? C29 C24 C25 O3 179.70(13) . . . 3_565 ? P2 C24 C25 O3 6.86(18) . . . 3_565 ? C29 C24 C25 C26 0.8(2) . . . . ? P2 C24 C25 C26 -172.03(11) . . . . ? O3 C25 C26 C27 179.42(14) 3_565 . . . ? C24 C25 C26 C27 -1.8(2) . . . . ? O3 C25 C26 C20 -1.8(2) 3_565 . . 3_565 ? C24 C25 C26 C20 177.03(13) . . . 3_565 ? C25 C26 C27 C28 1.6(2) . . . . ? C20 C26 C27 C28 -177.19(15) 3_565 . . . ? C26 C27 C28 C29 -0.5(2) . . . . ? C26 C27 C28 C30 177.56(16) . . . . ? C27 C28 C29 C24 -0.5(2) . . . . ? C30 C28 C29 C24 -178.55(16) . . . . ? C25 C24 C29 C28 0.4(2) . . . . ? P2 C24 C29 C28 173.07(13) . . . . ? C24 P2 C31 C36 -104.26(16) . . . . ? C37 P2 C31 C36 144.62(15) . . . . ? Rh1 P2 C31 C36 21.10(17) . . . . ? C24 P2 C31 C32 71.81(16) . . . . ? C37 P2 C31 C32 -39.31(17) . . . . ? Rh1 P2 C31 C32 -162.82(14) . . . . ? C36 C31 C32 C33 0.2(3) . . . . ? P2 C31 C32 C33 -175.82(16) . . . . ? C31 C32 C33 C34 -0.7(3) . . . . ? C32 C33 C34 C35 1.0(4) . . . . ? C33 C34 C35 C36 -0.9(4) . . . . ? C32 C31 C36 C35 -0.1(3) . . . . ? P2 C31 C36 C35 176.14(19) . . . . ? C34 C35 C36 C31 0.4(4) . . . . ? C31 P2 C37 C38 136.59(14) . . . . ? C24 P2 C37 C38 28.47(15) . . . . ? Rh1 P2 C37 C38 -101.60(14) . . . . ? C31 P2 C37 C42 -47.95(15) . . . . ? C24 P2 C37 C42 -156.07(13) . . . . ? Rh1 P2 C37 C42 73.85(14) . . . . ? C42 C37 C38 C39 -1.3(2) . . . . ? P2 C37 C38 C39 174.15(13) . . . . ? C37 C38 C39 C40 0.9(3) . . . . ? C38 C39 C40 C41 0.1(3) . . . . ? C39 C40 C41 C42 -0.7(3) . . . . ? C40 C41 C42 C37 0.3(3) . . . . ? C38 C37 C42 C41 0.7(3) . . . . ? P2 C37 C42 C41 -174.96(15) . . . . ? C1W' Cl1W C1W Cl2W 57.8(9) . . . . ? C1W Cl1W C1W' Cl3W -168.7(15) . . . . ? _diffrn_measured_fraction_theta_max 0.957 _diffrn_reflns_theta_full 37.50 _diffrn_measured_fraction_theta_full 0.957 _refine_diff_density_max 1.854 _refine_diff_density_min -2.240 _refine_diff_density_rms 0.112 #===END data_jm-044_0m_22 _database_code_depnum_ccdc_archive 'CCDC 762013' #TrackingRef '1764_web_deposit_cif_file_0_EduardoC.Escudero-Adan_1279182185.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H37 Cl5 O4 P2 Rh2' _chemical_formula_weight 1086.76 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 11.2602(16) _cell_length_b 14.114(4) _cell_length_c 14.469(2) _cell_angle_alpha 87.046(10) _cell_angle_beta 76.892(8) _cell_angle_gamma 79.328(9) _cell_volume 2200.8(8) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7071 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 32.50 _exptl_crystal_description Block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.640 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.169 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8190 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS Version 2008/1 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 Due to the formation of ice no better data completeness could be obtained (91%). ; _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 70 _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_reflns_number 30226 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0363 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 32.50 _reflns_number_total 14497 _reflns_number_gt 12283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. 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^)+(0.0824P)^2^+6.4811P] 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 14497 _refine_ls_number_parameters 527 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0609 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1473 _refine_ls_wR_factor_gt 0.1327 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _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 -0.403959(19) -0.925405(15) -0.272816(17) 0.01426(6) Uani 1 1 d . . . Cl1 Cl -0.56273(6) -0.81601(5) -0.32901(5) 0.01604(12) Uani 1 1 d . . . P1 P -0.49849(7) -1.05355(5) -0.25613(6) 0.01434(13) Uani 1 1 d . . . C1 C -0.8238(3) -0.84906(19) -0.1112(2) 0.0148(5) Uani 1 1 d . . . O1 O -0.7242(2) -0.92738(15) -0.14250(17) 0.0163(4) Uani 1 1 d . . . Rh2 Rh -0.496121(19) -0.683783(15) -0.270791(16) 0.01315(6) Uani 1 1 d . . . Cl2 Cl -0.29709(6) -0.78993(5) -0.30581(6) 0.01853(13) Uani 1 1 d . . . P2 P -0.67872(7) -0.58297(5) -0.23898(6) 0.01358(13) Uani 1 1 d . . . C2 C -0.7418(3) -0.96333(19) -0.2234(2) 0.0139(5) Uani 1 1 d . . . O2 O -0.7768(2) -0.76115(15) -0.14173(17) 0.0165(4) Uani 1 1 d . . . C3 C -0.6500(3) -1.02600(19) -0.2842(2) 0.0146(5) Uani 1 1 d . . . O3 O -0.1902(3) -1.0475(2) -0.2151(3) 0.0386(8) Uani 1 1 d . . . C4 C -0.6828(3) -1.05669(19) -0.3640(2) 0.0162(5) Uani 1 1 d . . . H4 H -0.6225 -1.0985 -0.4076 0.019 Uiso 1 1 calc R . . O4 O -0.3847(3) -0.5210(2) -0.2311(2) 0.0298(6) Uani 1 1 d . . . C5 C -0.8018(3) -1.0278(2) -0.3816(2) 0.0187(5) Uani 1 1 d . . . C6 C -0.8891(3) -0.9629(2) -0.3197(2) 0.0182(5) Uani 1 1 d . . . H6 H -0.9693 -0.9410 -0.3316 0.022 Uiso 1 1 calc R . . C7 C -0.8581(3) -0.93063(19) -0.2410(2) 0.0148(5) Uani 1 1 d . . . C8 C -0.9268(3) -0.8544(2) -0.1684(2) 0.0160(5) Uani 1 1 d . . . C9 C -0.9371(3) -0.75636(19) -0.2172(2) 0.0150(5) Uani 1 1 d . . . C10 C -1.0158(3) -0.7131(2) -0.2738(2) 0.0173(5) Uani 1 1 d . . . H10 H -1.0813 -0.7431 -0.2826 0.021 Uiso 1 1 calc R . . C11 C -0.9982(3) -0.6245(2) -0.3183(2) 0.0176(5) Uani 1 1 d . . . C12 C -0.8972(3) -0.5842(2) -0.3078(2) 0.0159(5) Uani 1 1 d . . . H12 H -0.8836 -0.5253 -0.3397 0.019 Uiso 1 1 calc R . . C13 C -0.8153(3) -0.62828(19) -0.2513(2) 0.0146(5) Uani 1 1 d . . . C14 C -0.8414(3) -0.71321(19) -0.2047(2) 0.0138(5) Uani 1 1 d . . . C15 C -0.8577(3) -0.8497(2) -0.0046(2) 0.0219(6) Uani 1 1 d . . . H15A H -0.7863 -0.8406 0.0200 0.033 Uiso 1 1 calc R . . H15B H -0.8813 -0.9116 0.0183 0.033 Uiso 1 1 calc R . . H15C H -0.9274 -0.7974 0.0175 0.033 Uiso 1 1 calc R . . C16 C -1.0496(3) -0.8774(3) -0.1095(3) 0.0252(7) Uani 1 1 d . . . H16A H -1.0349 -0.9412 -0.0797 0.038 Uiso 1 1 calc R . . H16B H -1.1076 -0.8771 -0.1508 0.038 Uiso 1 1 calc R . . H16C H -1.0850 -0.8287 -0.0602 0.038 Uiso 1 1 calc R . . C17 C -0.8338(4) -1.0649(3) -0.4669(3) 0.0272(7) Uani 1 1 d . . . H17A H -0.8664 -1.0104 -0.5042 0.041 Uiso 1 1 calc R . . H17B H -0.8966 -1.1058 -0.4459 0.041 Uiso 1 1 calc R . . H17C H -0.7592 -1.1027 -0.5061 0.041 Uiso 1 1 calc R . . C18 C -1.0839(3) -0.5743(3) -0.3792(3) 0.0272(7) Uani 1 1 d . . . H18A H -1.1309 -0.6202 -0.3960 0.041 Uiso 1 1 calc R . . H18B H -1.0351 -0.5495 -0.4371 0.041 Uiso 1 1 calc R . . H18C H -1.1414 -0.5207 -0.3439 0.041 Uiso 1 1 calc R . . C19 C -0.5327(3) -1.1148(2) -0.1420(2) 0.0174(5) Uani 1 1 d . . . C20 C -0.4744(3) -1.1022(2) -0.0692(3) 0.0233(6) Uani 1 1 d . . . H20 H -0.4171 -1.0591 -0.0780 0.028 Uiso 1 1 calc R . . C21 C -0.5001(4) -1.1527(3) 0.0167(3) 0.0304(7) Uani 1 1 d . . . H21 H -0.4598 -1.1442 0.0659 0.036 Uiso 1 1 calc R . . C22 C -0.5845(4) -1.2154(3) 0.0304(3) 0.0294(7) Uani 1 1 d . . . H22 H -0.6026 -1.2488 0.0891 0.035 Uiso 1 1 calc R . . C23 C -0.6424(3) -1.2291(3) -0.0419(3) 0.0258(7) Uani 1 1 d . . . H23 H -0.6986 -1.2731 -0.0331 0.031 Uiso 1 1 calc R . . C24 C -0.6181(3) -1.1785(2) -0.1269(3) 0.0211(6) Uani 1 1 d . . . H24 H -0.6595 -1.1869 -0.1754 0.025 Uiso 1 1 calc R . . C25 C -0.4085(3) -1.1489(2) -0.3371(2) 0.0158(5) Uani 1 1 d . . . C26 C -0.3835(3) -1.2458(2) -0.3083(3) 0.0252(7) Uani 1 1 d . . . H26 H -0.4174 -1.2646 -0.2453 0.030 Uiso 1 1 calc R . . C27 C -0.3088(4) -1.3138(3) -0.3726(4) 0.0345(9) Uani 1 1 d . . . H27 H -0.2929 -1.3795 -0.3534 0.041 Uiso 1 1 calc R . . C28 C -0.2575(3) -1.2870(3) -0.4638(3) 0.0286(7) Uani 1 1 d . . . H28 H -0.2058 -1.3341 -0.5068 0.034 Uiso 1 1 calc R . . C29 C -0.2813(3) -1.1908(3) -0.4934(3) 0.0250(6) Uani 1 1 d . . . H29 H -0.2467 -1.1723 -0.5564 0.030 Uiso 1 1 calc R . . C30 C -0.3562(3) -1.1226(2) -0.4294(3) 0.0219(6) Uani 1 1 d . . . H30 H -0.3721 -1.0570 -0.4489 0.026 Uiso 1 1 calc R . . C31 C -0.7273(3) -0.5318(2) -0.1210(2) 0.0179(5) Uani 1 1 d . . . C32 C -0.6583(4) -0.5596(3) -0.0524(3) 0.0291(7) Uani 1 1 d . . . H32 H -0.5833 -0.6050 -0.0681 0.035 Uiso 1 1 calc R . . C33 C -0.6970(5) -0.5224(4) 0.0380(3) 0.0415(10) Uani 1 1 d . . . H33 H -0.6484 -0.5420 0.0837 0.050 Uiso 1 1 calc R . . C34 C -0.8072(5) -0.4561(3) 0.0625(3) 0.0392(9) Uani 1 1 d . . . H34 H -0.8336 -0.4298 0.1245 0.047 Uiso 1 1 calc R . . C35 C -0.8777(4) -0.4290(3) -0.0049(3) 0.0332(8) Uani 1 1 d . . . H35 H -0.9528 -0.3839 0.0113 0.040 Uiso 1 1 calc R . . C36 C -0.8400(3) -0.4668(2) -0.0953(3) 0.0255(6) Uani 1 1 d . . . H36 H -0.8903 -0.4489 -0.1402 0.031 Uiso 1 1 calc R . . C37 C -0.6705(3) -0.4812(2) -0.3217(2) 0.0168(5) Uani 1 1 d . . . C38 C -0.6582(3) -0.4983(2) -0.4176(2) 0.0206(6) Uani 1 1 d . . . H38 H -0.6610 -0.5607 -0.4376 0.025 Uiso 1 1 calc R . . C39 C -0.6419(3) -0.4247(3) -0.4843(3) 0.0255(7) Uani 1 1 d . . . H39 H -0.6362 -0.4366 -0.5493 0.031 Uiso 1 1 calc R . . C40 C -0.6340(3) -0.3340(3) -0.4565(3) 0.0290(8) Uani 1 1 d . . . H40 H -0.6226 -0.2836 -0.5020 0.035 Uiso 1 1 calc R . . C41 C -0.6429(4) -0.3180(3) -0.3620(3) 0.0314(8) Uani 1 1 d . . . H41 H -0.6357 -0.2564 -0.3427 0.038 Uiso 1 1 calc R . . C42 C -0.6623(4) -0.3909(2) -0.2937(3) 0.0258(7) Uani 1 1 d . . . H42 H -0.6698 -0.3783 -0.2286 0.031 Uiso 1 1 calc R . . C43 C -0.2749(3) -1.0016(2) -0.2363(3) 0.0236(6) Uani 1 1 d . . . C44 C -0.4299(3) -0.5844(2) -0.2432(2) 0.0197(5) Uani 1 1 d . . . C1S C -0.9565(4) -0.7404(3) -0.7269(3) 0.0340(8) Uani 1 1 d . . . H1S H -0.8903 -0.7934 -0.7130 0.041 Uiso 1 1 calc R . . Cl1S Cl -0.88559(11) -0.65977(9) -0.80834(10) 0.0440(3) Uani 1 1 d . . . Cl2S Cl -1.03511(11) -0.68223(8) -0.61907(9) 0.0417(2) Uani 1 1 d . . . Cl3S Cl -1.05998(11) -0.79219(8) -0.77499(10) 0.0421(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 Rh1 0.01555(10) 0.01382(10) 0.01356(12) 0.00161(7) -0.00359(8) -0.00307(7) Cl1 0.0187(3) 0.0157(3) 0.0156(3) 0.0043(2) -0.0060(2) -0.0062(2) P1 0.0179(3) 0.0126(3) 0.0123(4) 0.0028(2) -0.0039(3) -0.0022(2) C1 0.0182(11) 0.0128(10) 0.0120(13) 0.0026(9) 0.0002(9) -0.0039(8) O1 0.0191(9) 0.0153(9) 0.0140(11) 0.0003(7) -0.0033(8) -0.0026(7) Rh2 0.01597(10) 0.01459(10) 0.00989(11) 0.00385(7) -0.00332(7) -0.00581(7) Cl2 0.0162(3) 0.0179(3) 0.0222(4) 0.0012(2) -0.0040(2) -0.0055(2) P2 0.0187(3) 0.0123(3) 0.0106(3) 0.0044(2) -0.0039(2) -0.0053(2) C2 0.0167(11) 0.0123(10) 0.0125(13) 0.0026(8) -0.0020(9) -0.0047(8) O2 0.0218(9) 0.0156(9) 0.0138(11) 0.0069(7) -0.0059(8) -0.0074(7) C3 0.0184(11) 0.0107(10) 0.0143(14) 0.0027(8) -0.0038(10) -0.0024(8) O3 0.0291(13) 0.0282(13) 0.060(2) 0.0029(13) -0.0198(14) 0.0018(10) C4 0.0231(12) 0.0111(10) 0.0147(14) 0.0022(9) -0.0052(10) -0.0031(9) O4 0.0350(13) 0.0314(13) 0.0286(16) -0.0021(10) -0.0100(12) -0.0164(10) C5 0.0250(13) 0.0144(11) 0.0188(15) 0.0031(10) -0.0084(11) -0.0053(9) C6 0.0197(12) 0.0149(11) 0.0213(16) 0.0031(10) -0.0072(11) -0.0042(9) C7 0.0163(11) 0.0118(10) 0.0164(14) 0.0026(9) -0.0029(10) -0.0046(8) C8 0.0165(11) 0.0149(11) 0.0157(14) 0.0020(9) -0.0004(10) -0.0047(9) C9 0.0148(10) 0.0143(11) 0.0143(14) 0.0008(9) -0.0001(9) -0.0030(8) C10 0.0137(10) 0.0180(12) 0.0202(16) 0.0006(10) -0.0039(10) -0.0024(9) C11 0.0155(11) 0.0194(12) 0.0176(15) 0.0010(10) -0.0043(10) -0.0018(9) C12 0.0172(11) 0.0163(11) 0.0137(14) 0.0034(9) -0.0034(10) -0.0022(9) C13 0.0173(11) 0.0147(11) 0.0112(13) 0.0028(9) -0.0021(9) -0.0037(8) C14 0.0161(10) 0.0137(10) 0.0109(13) 0.0023(8) -0.0008(9) -0.0044(8) C15 0.0300(15) 0.0220(13) 0.0112(15) 0.0040(10) 0.0005(11) -0.0054(11) C16 0.0200(13) 0.0259(15) 0.0277(19) 0.0045(12) 0.0022(12) -0.0094(11) C17 0.0321(16) 0.0278(15) 0.0247(19) -0.0044(13) -0.0141(15) -0.0025(12) C18 0.0232(14) 0.0282(15) 0.032(2) 0.0079(13) -0.0142(14) -0.0029(12) C19 0.0223(12) 0.0163(11) 0.0116(14) 0.0024(9) -0.0023(10) -0.0010(9) C20 0.0285(15) 0.0259(14) 0.0154(16) 0.0021(11) -0.0071(12) -0.0028(11) C21 0.0389(18) 0.0344(18) 0.0169(18) 0.0038(13) -0.0096(15) -0.0007(14) C22 0.0362(17) 0.0293(16) 0.0170(18) 0.0077(12) -0.0018(14) 0.0010(13) C23 0.0301(15) 0.0247(14) 0.0175(17) 0.0088(12) 0.0021(12) -0.0032(12) C24 0.0233(13) 0.0224(13) 0.0158(16) 0.0053(11) -0.0013(11) -0.0045(10) C25 0.0178(11) 0.0161(11) 0.0129(14) 0.0022(9) -0.0025(10) -0.0031(9) C26 0.0311(15) 0.0151(12) 0.0217(18) 0.0029(11) 0.0053(13) 0.0010(11) C27 0.0380(19) 0.0186(14) 0.037(2) 0.0010(14) 0.0045(16) 0.0028(13) C28 0.0280(15) 0.0274(16) 0.027(2) -0.0082(13) 0.0010(14) -0.0027(12) C29 0.0291(15) 0.0293(16) 0.0157(17) -0.0011(12) -0.0018(12) -0.0063(12) C30 0.0293(14) 0.0199(13) 0.0139(15) 0.0024(10) -0.0004(12) -0.0040(11) C31 0.0237(13) 0.0156(11) 0.0145(15) 0.0024(9) -0.0024(11) -0.0065(9) C32 0.0350(17) 0.0385(19) 0.0118(17) 0.0003(13) -0.0057(13) -0.0013(14) C33 0.058(3) 0.052(3) 0.015(2) -0.0034(16) -0.0101(19) -0.009(2) C34 0.055(3) 0.042(2) 0.019(2) -0.0080(15) 0.0020(18) -0.0136(19) C35 0.0374(19) 0.0284(17) 0.028(2) -0.0084(14) 0.0055(15) -0.0038(14) C36 0.0280(15) 0.0233(14) 0.0228(19) -0.0036(12) -0.0019(13) -0.0021(11) C37 0.0198(12) 0.0166(11) 0.0146(14) 0.0068(9) -0.0049(10) -0.0053(9) C38 0.0219(13) 0.0223(13) 0.0145(15) 0.0070(10) -0.0010(11) -0.0021(10) C39 0.0253(14) 0.0333(16) 0.0147(16) 0.0111(12) -0.0014(12) -0.0036(12) C40 0.0283(15) 0.0277(15) 0.029(2) 0.0178(14) -0.0044(14) -0.0066(12) C41 0.046(2) 0.0202(14) 0.030(2) 0.0123(13) -0.0105(17) -0.0121(14) C42 0.0403(18) 0.0199(13) 0.0205(18) 0.0074(11) -0.0100(14) -0.0121(12) C43 0.0229(13) 0.0207(13) 0.0285(19) -0.0010(12) -0.0080(13) -0.0039(10) C44 0.0239(13) 0.0206(13) 0.0166(16) 0.0024(10) -0.0063(11) -0.0075(10) C1S 0.0347(18) 0.0294(17) 0.031(2) 0.0039(14) 0.0019(16) -0.0015(14) Cl1S 0.0412(5) 0.0479(6) 0.0414(7) 0.0158(5) -0.0063(5) -0.0125(4) Cl2S 0.0438(5) 0.0386(5) 0.0370(7) -0.0016(4) -0.0016(4) -0.0018(4) Cl3S 0.0411(5) 0.0383(5) 0.0408(7) -0.0039(4) 0.0046(4) -0.0068(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 Rh1 C43 1.805(3) . ? Rh1 P1 2.2391(9) . ? Rh1 Cl1 2.3977(8) . ? Rh1 Cl2 2.4145(9) . ? Cl1 Rh2 2.3920(8) . ? P1 C3 1.811(3) . ? P1 C19 1.820(3) . ? P1 C25 1.825(3) . ? C1 O1 1.431(3) . ? C1 O2 1.447(3) . ? C1 C15 1.503(5) . ? C1 C8 1.585(4) . ? O1 C2 1.368(4) . ? Rh2 C44 1.806(3) . ? Rh2 P2 2.2402(8) . ? Rh2 Cl2 2.4173(8) . ? P2 C31 1.814(3) . ? P2 C13 1.818(3) . ? P2 C37 1.824(3) . ? C2 C7 1.381(4) . ? C2 C3 1.397(4) . ? O2 C14 1.368(3) . ? C3 C4 1.401(4) . ? O3 C43 1.144(4) . ? C4 C5 1.404(4) . ? O4 C44 1.147(4) . ? C5 C6 1.400(5) . ? C5 C17 1.504(5) . ? C6 C7 1.384(4) . ? C7 C8 1.516(4) . ? C8 C9 1.518(4) . ? C8 C16 1.533(4) . ? C9 C10 1.381(4) . ? C9 C14 1.381(4) . ? C10 C11 1.404(4) . ? C11 C12 1.403(4) . ? C11 C18 1.508(4) . ? C12 C13 1.407(4) . ? C13 C14 1.391(4) . ? C19 C20 1.395(4) . ? C19 C24 1.408(4) . ? C20 C21 1.401(5) . ? C21 C22 1.389(6) . ? C22 C23 1.391(6) . ? C23 C24 1.388(5) . ? C25 C30 1.393(5) . ? C25 C26 1.405(4) . ? C26 C27 1.390(5) . ? C27 C28 1.380(6) . ? C28 C29 1.398(5) . ? C29 C30 1.391(5) . ? C31 C32 1.393(5) . ? C31 C36 1.406(5) . ? C32 C33 1.380(6) . ? C33 C34 1.395(7) . ? C34 C35 1.388(7) . ? C35 C36 1.384(6) . ? C37 C42 1.382(4) . ? C37 C38 1.392(5) . ? C38 C39 1.389(4) . ? C39 C40 1.386(6) . ? C40 C41 1.375(6) . ? C41 C42 1.401(5) . ? C1S Cl1S 1.759(4) . ? C1S Cl3S 1.764(5) . ? C1S Cl2S 1.768(5) . ? 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 C43 Rh1 P1 88.01(11) . . ? C43 Rh1 Cl1 175.00(12) . . ? P1 Rh1 Cl1 96.39(3) . . ? C43 Rh1 Cl2 92.89(11) . . ? P1 Rh1 Cl2 174.89(3) . . ? Cl1 Rh1 Cl2 82.52(3) . . ? Rh2 Cl1 Rh1 89.61(3) . . ? C3 P1 C19 101.47(14) . . ? C3 P1 C25 106.07(14) . . ? C19 P1 C25 104.09(14) . . ? C3 P1 Rh1 112.58(9) . . ? C19 P1 Rh1 120.84(10) . . ? C25 P1 Rh1 110.46(10) . . ? O1 C1 O2 106.8(2) . . ? O1 C1 C15 108.9(2) . . ? O2 C1 C15 107.7(2) . . ? O1 C1 C8 107.0(2) . . ? O2 C1 C8 106.5(2) . . ? C15 C1 C8 119.3(3) . . ? C2 O1 C1 108.0(2) . . ? C44 Rh2 P2 86.26(11) . . ? C44 Rh2 Cl1 171.68(11) . . ? P2 Rh2 Cl1 98.36(3) . . ? C44 Rh2 Cl2 92.74(11) . . ? P2 Rh2 Cl2 178.90(2) . . ? Cl1 Rh2 Cl2 82.58(3) . . ? Rh1 Cl2 Rh2 88.62(3) . . ? C31 P2 C13 102.28(14) . . ? C31 P2 C37 106.19(14) . . ? C13 P2 C37 104.42(13) . . ? C31 P2 Rh2 116.43(10) . . ? C13 P2 Rh2 117.85(10) . . ? C37 P2 Rh2 108.48(10) . . ? O1 C2 C7 114.0(3) . . ? O1 C2 C3 123.3(2) . . ? C7 C2 C3 122.7(3) . . ? C14 O2 C1 109.0(2) . . ? C2 C3 C4 116.4(3) . . ? C2 C3 P1 117.0(2) . . ? C4 C3 P1 126.5(2) . . ? C3 C4 C5 122.2(3) . . ? C6 C5 C4 118.9(3) . . ? C6 C5 C17 120.8(3) . . ? C4 C5 C17 120.2(3) . . ? C7 C6 C5 119.8(3) . . ? C2 C7 C6 119.9(3) . . ? C2 C7 C8 108.4(2) . . ? C6 C7 C8 131.5(3) . . ? C7 C8 C9 109.0(3) . . ? C7 C8 C16 113.8(2) . . ? C9 C8 C16 114.6(2) . . ? C7 C8 C1 100.9(2) . . ? C9 C8 C1 101.2(2) . . ? C16 C8 C1 115.8(3) . . ? C10 C9 C14 120.5(3) . . ? C10 C9 C8 130.7(3) . . ? C14 C9 C8 108.5(2) . . ? C9 C10 C11 119.4(3) . . ? C12 C11 C10 119.0(3) . . ? C12 C11 C18 120.2(3) . . ? C10 C11 C18 120.8(3) . . ? C11 C12 C13 122.1(3) . . ? C14 C13 C12 116.4(2) . . ? C14 C13 P2 119.3(2) . . ? C12 C13 P2 124.3(2) . . ? O2 C14 C9 113.7(2) . . ? O2 C14 C13 123.8(2) . . ? C9 C14 C13 122.5(3) . . ? C20 C19 C24 118.8(3) . . ? C20 C19 P1 121.7(2) . . ? C24 C19 P1 119.5(2) . . ? C19 C20 C21 120.3(3) . . ? C22 C21 C20 120.2(3) . . ? C21 C22 C23 120.1(3) . . ? C24 C23 C22 119.9(3) . . ? C23 C24 C19 120.8(3) . . ? C30 C25 C26 119.2(3) . . ? C30 C25 P1 118.0(2) . . ? C26 C25 P1 122.7(3) . . ? C27 C26 C25 119.6(3) . . ? C28 C27 C26 120.7(3) . . ? C27 C28 C29 120.3(3) . . ? C30 C29 C28 119.1(3) . . ? C29 C30 C25 121.0(3) . . ? C32 C31 C36 118.5(3) . . ? C32 C31 P2 121.2(3) . . ? C36 C31 P2 120.3(3) . . ? C33 C32 C31 121.1(4) . . ? C32 C33 C34 120.3(4) . . ? C35 C34 C33 119.1(4) . . ? C36 C35 C34 120.9(4) . . ? C35 C36 C31 120.1(4) . . ? C42 C37 C38 119.3(3) . . ? C42 C37 P2 122.0(3) . . ? C38 C37 P2 118.4(2) . . ? C39 C38 C37 120.5(3) . . ? C40 C39 C38 120.3(4) . . ? C41 C40 C39 119.0(3) . . ? C40 C41 C42 121.2(4) . . ? C37 C42 C41 119.6(4) . . ? O3 C43 Rh1 177.3(3) . . ? O4 C44 Rh2 176.1(3) . . ? Cl1S C1S Cl3S 110.9(3) . . ? Cl1S C1S Cl2S 111.0(2) . . ? Cl3S C1S Cl2S 110.1(2) . . ? 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 C43 Rh1 Cl1 Rh2 -53.7(14) . . . . ? P1 Rh1 Cl1 Rh2 154.67(3) . . . . ? Cl2 Rh1 Cl1 Rh2 -30.36(3) . . . . ? C43 Rh1 P1 C3 179.92(17) . . . . ? Cl1 Rh1 P1 C3 -2.45(12) . . . . ? Cl2 Rh1 P1 C3 -79.9(3) . . . . ? C43 Rh1 P1 C19 59.97(17) . . . . ? Cl1 Rh1 P1 C19 -122.40(12) . . . . ? Cl2 Rh1 P1 C19 160.2(3) . . . . ? C43 Rh1 P1 C25 -61.72(16) . . . . ? Cl1 Rh1 P1 C25 115.91(10) . . . . ? Cl2 Rh1 P1 C25 38.5(3) . . . . ? O2 C1 O1 C2 -100.2(2) . . . . ? C15 C1 O1 C2 143.8(2) . . . . ? C8 C1 O1 C2 13.5(3) . . . . ? Rh1 Cl1 Rh2 C44 86.4(7) . . . . ? Rh1 Cl1 Rh2 P2 -150.27(3) . . . . ? Rh1 Cl1 Rh2 Cl2 30.32(3) . . . . ? C43 Rh1 Cl2 Rh2 -151.96(13) . . . . ? P1 Rh1 Cl2 Rh2 108.1(3) . . . . ? Cl1 Rh1 Cl2 Rh2 30.02(3) . . . . ? C44 Rh2 Cl2 Rh1 156.82(11) . . . . ? P2 Rh2 Cl2 Rh1 -179(100) . . . . ? Cl1 Rh2 Cl2 Rh1 -30.09(3) . . . . ? C44 Rh2 P2 C31 -58.59(15) . . . . ? Cl1 Rh2 P2 C31 128.37(11) . . . . ? Cl2 Rh2 P2 C31 -83.2(15) . . . . ? C44 Rh2 P2 C13 179.32(15) . . . . ? Cl1 Rh2 P2 C13 6.28(11) . . . . ? Cl2 Rh2 P2 C13 154.7(15) . . . . ? C44 Rh2 P2 C37 61.05(15) . . . . ? Cl1 Rh2 P2 C37 -111.99(11) . . . . ? Cl2 Rh2 P2 C37 36.5(15) . . . . ? C1 O1 C2 C7 -12.9(3) . . . . ? C1 O1 C2 C3 165.9(2) . . . . ? O1 C1 O2 C14 116.8(3) . . . . ? C15 C1 O2 C14 -126.4(3) . . . . ? C8 C1 O2 C14 2.7(3) . . . . ? O1 C2 C3 C4 179.7(3) . . . . ? C7 C2 C3 C4 -1.6(4) . . . . ? O1 C2 C3 P1 -3.9(4) . . . . ? C7 C2 C3 P1 174.8(2) . . . . ? C19 P1 C3 C2 63.5(2) . . . . ? C25 P1 C3 C2 172.0(2) . . . . ? Rh1 P1 C3 C2 -67.1(2) . . . . ? C19 P1 C3 C4 -120.6(3) . . . . ? C25 P1 C3 C4 -12.1(3) . . . . ? Rh1 P1 C3 C4 108.8(2) . . . . ? C2 C3 C4 C5 -1.1(4) . . . . ? P1 C3 C4 C5 -177.0(2) . . . . ? C3 C4 C5 C6 2.8(4) . . . . ? C3 C4 C5 C17 -178.3(3) . . . . ? C4 C5 C6 C7 -1.9(4) . . . . ? C17 C5 C6 C7 179.2(3) . . . . ? O1 C2 C7 C6 -178.7(3) . . . . ? C3 C2 C7 C6 2.5(4) . . . . ? O1 C2 C7 C8 6.3(3) . . . . ? C3 C2 C7 C8 -172.5(2) . . . . ? C5 C6 C7 C2 -0.7(4) . . . . ? C5 C6 C7 C8 173.0(3) . . . . ? C2 C7 C8 C9 108.3(3) . . . . ? C6 C7 C8 C9 -65.9(4) . . . . ? C2 C7 C8 C16 -122.5(3) . . . . ? C6 C7 C8 C16 63.3(4) . . . . ? C2 C7 C8 C1 2.3(3) . . . . ? C6 C7 C8 C1 -171.9(3) . . . . ? O1 C1 C8 C7 -9.5(3) . . . . ? O2 C1 C8 C7 104.5(2) . . . . ? C15 C1 C8 C7 -133.5(3) . . . . ? O1 C1 C8 C9 -121.5(2) . . . . ? O2 C1 C8 C9 -7.6(3) . . . . ? C15 C1 C8 C9 114.4(3) . . . . ? O1 C1 C8 C16 113.9(3) . . . . ? O2 C1 C8 C16 -132.1(3) . . . . ? C15 C1 C8 C16 -10.2(4) . . . . ? C7 C8 C9 C10 78.2(4) . . . . ? C16 C8 C9 C10 -50.6(5) . . . . ? C1 C8 C9 C10 -176.0(3) . . . . ? C7 C8 C9 C14 -95.8(3) . . . . ? C16 C8 C9 C14 135.4(3) . . . . ? C1 C8 C9 C14 10.0(3) . . . . ? C14 C9 C10 C11 -0.3(5) . . . . ? C8 C9 C10 C11 -173.8(3) . . . . ? C9 C10 C11 C12 3.0(5) . . . . ? C9 C10 C11 C18 -178.8(3) . . . . ? C10 C11 C12 C13 -2.2(5) . . . . ? C18 C11 C12 C13 179.7(3) . . . . ? C11 C12 C13 C14 -1.3(5) . . . . ? C11 C12 C13 P2 177.0(2) . . . . ? C31 P2 C13 C14 -76.2(3) . . . . ? C37 P2 C13 C14 173.3(2) . . . . ? Rh2 P2 C13 C14 52.9(3) . . . . ? C31 P2 C13 C12 105.5(3) . . . . ? C37 P2 C13 C12 -5.0(3) . . . . ? Rh2 P2 C13 C12 -125.4(2) . . . . ? C1 O2 C14 C9 4.2(4) . . . . ? C1 O2 C14 C13 -176.6(3) . . . . ? C10 C9 C14 O2 175.8(3) . . . . ? C8 C9 C14 O2 -9.5(4) . . . . ? C10 C9 C14 C13 -3.4(5) . . . . ? C8 C9 C14 C13 171.3(3) . . . . ? C12 C13 C14 O2 -175.0(3) . . . . ? P2 C13 C14 O2 6.6(4) . . . . ? C12 C13 C14 C9 4.2(5) . . . . ? P2 C13 C14 C9 -174.3(2) . . . . ? C3 P1 C19 C20 -142.6(3) . . . . ? C25 P1 C19 C20 107.4(3) . . . . ? Rh1 P1 C19 C20 -17.3(3) . . . . ? C3 P1 C19 C24 38.9(3) . . . . ? C25 P1 C19 C24 -71.1(3) . . . . ? Rh1 P1 C19 C24 164.2(2) . . . . ? C24 C19 C20 C21 0.5(5) . . . . ? P1 C19 C20 C21 -178.0(3) . . . . ? C19 C20 C21 C22 -0.4(6) . . . . ? C20 C21 C22 C23 0.9(6) . . . . ? C21 C22 C23 C24 -1.5(6) . . . . ? C22 C23 C24 C19 1.6(5) . . . . ? C20 C19 C24 C23 -1.1(5) . . . . ? P1 C19 C24 C23 177.5(3) . . . . ? C3 P1 C25 C30 80.2(3) . . . . ? C19 P1 C25 C30 -173.2(2) . . . . ? Rh1 P1 C25 C30 -42.0(3) . . . . ? C3 P1 C25 C26 -104.0(3) . . . . ? C19 P1 C25 C26 2.6(3) . . . . ? Rh1 P1 C25 C26 133.7(3) . . . . ? C30 C25 C26 C27 -0.9(5) . . . . ? P1 C25 C26 C27 -176.6(3) . . . . ? C25 C26 C27 C28 1.0(6) . . . . ? C26 C27 C28 C29 -0.8(6) . . . . ? C27 C28 C29 C30 0.6(6) . . . . ? C28 C29 C30 C25 -0.6(5) . . . . ? C26 C25 C30 C29 0.8(5) . . . . ? P1 C25 C30 C29 176.7(3) . . . . ? C13 P2 C31 C32 125.5(3) . . . . ? C37 P2 C31 C32 -125.3(3) . . . . ? Rh2 P2 C31 C32 -4.4(3) . . . . ? C13 P2 C31 C36 -50.9(3) . . . . ? C37 P2 C31 C36 58.3(3) . . . . ? Rh2 P2 C31 C36 179.2(2) . . . . ? C36 C31 C32 C33 -2.0(6) . . . . ? P2 C31 C32 C33 -178.4(3) . . . . ? C31 C32 C33 C34 0.4(7) . . . . ? C32 C33 C34 C35 0.7(7) . . . . ? C33 C34 C35 C36 0.0(7) . . . . ? C34 C35 C36 C31 -1.6(6) . . . . ? C32 C31 C36 C35 2.6(5) . . . . ? P2 C31 C36 C35 179.0(3) . . . . ? C31 P2 C37 C42 19.3(3) . . . . ? C13 P2 C37 C42 127.0(3) . . . . ? Rh2 P2 C37 C42 -106.5(3) . . . . ? C31 P2 C37 C38 -168.0(2) . . . . ? C13 P2 C37 C38 -60.4(3) . . . . ? Rh2 P2 C37 C38 66.1(2) . . . . ? C42 C37 C38 C39 -2.1(5) . . . . ? P2 C37 C38 C39 -175.0(2) . . . . ? C37 C38 C39 C40 1.9(5) . . . . ? C38 C39 C40 C41 -0.2(5) . . . . ? C39 C40 C41 C42 -1.4(6) . . . . ? C38 C37 C42 C41 0.6(5) . . . . ? P2 C37 C42 C41 173.1(3) . . . . ? C40 C41 C42 C37 1.2(6) . . . . ? P1 Rh1 C43 O3 155(8) . . . . ? Cl1 Rh1 C43 O3 4(9) . . . . ? Cl2 Rh1 C43 O3 -20(8) . . . . ? P2 Rh2 C44 O4 -110(4) . . . . ? Cl1 Rh2 C44 O4 14(5) . . . . ? Cl2 Rh2 C44 O4 69(4) . . . . ? _diffrn_measured_fraction_theta_max 0.910 _diffrn_reflns_theta_full 32.50 _diffrn_measured_fraction_theta_full 0.910 _refine_diff_density_max 2.896 _refine_diff_density_min -2.848 _refine_diff_density_rms 0.176 #===END data_jm236b_0m_24 _database_code_depnum_ccdc_archive 'CCDC 762014' #TrackingRef '1764_web_deposit_cif_file_0_EduardoC.Escudero-Adan_1279182185.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42.25 H33.50 Cl2.50 O4 P2 Rh2' _chemical_formula_weight 961.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I-4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'y, -x, -z' '-y, x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' _cell_length_a 28.7585(6) _cell_length_b 28.7585(6) _cell_length_c 9.2270(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7631.2(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9920 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 32.52 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.674 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3852 _exptl_absorpt_coefficient_mu 1.167 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details ; SADABS Version 2008/1 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 70 _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_reflns_number 41695 _diffrn_reflns_av_R_equivalents 0.0597 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 33.17 _reflns_number_total 12617 _reflns_number_gt 10915 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2 v2009.1-0' _computing_cell_refinement 'Bruker APEX2 v2009.1-0' _computing_data_reduction 'Bruker SAINT V7.60A' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXS-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. 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. C1s-Cl1s distance as well as anisotropic displacement of atom C1s have been restrained. Small deviations from the standard geometry of the dichloromethane molecule could be found since it is highly disordered over a 4-fold axis. ; _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^)+(0.0448P)^2^+17.1153P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _chemical_absolute_configuration ad _refine_ls_abs_structure_Flack 0.49(2) _refine_ls_number_reflns 12617 _refine_ls_number_parameters 491 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0411 _refine_ls_wR_factor_ref 0.0989 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.025 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.22534(10) 0.65712(10) 0.5289(4) 0.0145(6) Uani 1 1 d . . . H1 H 0.2228 0.6472 0.6325 0.017 Uiso 1 1 calc R . . Cl1 Cl 0.22582(2) 0.65257(3) 0.10613(10) 0.01488(14) Uani 1 1 d . . . O1 O 0.18248(7) 0.65006(7) 0.4540(4) 0.0151(5) Uani 1 1 d . . . P1 P 0.10855(3) 0.64368(3) 0.20429(11) 0.01248(16) Uani 1 1 d . . . Rh1 Rh 0.156545(7) 0.610567(8) 0.04207(3) 0.01276(5) Uani 1 1 d . . . C2 C 0.29010(10) 0.66142(10) 0.3884(4) 0.0135(6) Uani 1 1 d . . . Cl2 Cl 0.20770(3) 0.57703(3) -0.13729(11) 0.01946(17) Uani 1 1 d . . . O2 O 0.26014(7) 0.63097(7) 0.4546(3) 0.0162(5) Uani 1 1 d . . . P2 P 0.32282(3) 0.58977(3) 0.21262(11) 0.01269(16) Uani 1 1 d . . . Rh2 Rh 0.265468(7) 0.581284(8) 0.05030(3) 0.01280(5) Uani 1 1 d . . . C3 C 0.32408(10) 0.64767(10) 0.2906(4) 0.0133(6) Uani 1 1 d . . . O4 O 0.30160(10) 0.48925(9) -0.0366(4) 0.0302(7) Uani 1 1 d . . . C4 C 0.35296(11) 0.68317(11) 0.2373(4) 0.0161(7) Uani 1 1 d . . . H4 H 0.3769 0.6753 0.1707 0.019 Uiso 1 1 calc R . . O3 O 0.07853(9) 0.55330(9) -0.0666(4) 0.0256(7) Uani 1 1 d . . . C5 C 0.34792(11) 0.72962(11) 0.2785(5) 0.0164(7) Uani 1 1 d . . . C6 C 0.31202(11) 0.74159(11) 0.3732(4) 0.0155(7) Uani 1 1 d . . . H6 H 0.3076 0.7732 0.4002 0.019 Uiso 1 1 calc R . . C7 C 0.28259(10) 0.70717(10) 0.4283(4) 0.0134(7) Uani 1 1 d . . . C8 C 0.23838(11) 0.70981(11) 0.5172(4) 0.0155(7) Uani 1 1 d . . . H8 H 0.2421 0.7258 0.6127 0.019 Uiso 1 1 calc R . . C9 C 0.19883(10) 0.72833(10) 0.4261(4) 0.0135(7) Uani 1 1 d . . . C10 C 0.19061(11) 0.77193(11) 0.3690(4) 0.0156(7) Uani 1 1 d . . . H10 H 0.2097 0.7975 0.3954 0.019 Uiso 1 1 calc R . . C11 C 0.15401(11) 0.77786(11) 0.2723(4) 0.0159(7) Uani 1 1 d . . . C12 C 0.12715(11) 0.73946(11) 0.2302(4) 0.0150(7) Uani 1 1 d . . . H12 H 0.1029 0.7438 0.1615 0.018 Uiso 1 1 calc R . . C13 C 0.13494(10) 0.69481(10) 0.2865(4) 0.0132(6) Uani 1 1 d . . . H13 H 0.1102 0.6978 0.3620 0.016 Uiso 1 1 calc R . . C14 C 0.17054(10) 0.69092(10) 0.3874(4) 0.0138(6) Uani 1 1 d . . . C15 C 0.38045(12) 0.76572(12) 0.2188(5) 0.0224(8) Uani 1 1 d . . . H15A H 0.4103 0.7639 0.2695 0.034 Uiso 1 1 calc R . . H15B H 0.3670 0.7967 0.2328 0.034 Uiso 1 1 calc R . . H15C H 0.3853 0.7602 0.1151 0.034 Uiso 1 1 calc R . . C16 C 0.14384(13) 0.82501(11) 0.2053(5) 0.0207(8) Uani 1 1 d . . . H16A H 0.1156 0.8380 0.2488 0.031 Uiso 1 1 calc R . . H16B H 0.1393 0.8214 0.1006 0.031 Uiso 1 1 calc R . . H16C H 0.1700 0.8460 0.2233 0.031 Uiso 1 1 calc R . . C17 C 0.38055(10) 0.58550(10) 0.1315(4) 0.0142(6) Uani 1 1 d . . . C18 C 0.38524(11) 0.59141(11) -0.0182(4) 0.0166(7) Uani 1 1 d . . . H18 H 0.3583 0.5960 -0.0762 0.020 Uiso 1 1 calc R . . C19 C 0.42884(12) 0.59069(12) -0.0827(5) 0.0228(9) Uani 1 1 d . . . H19 H 0.4317 0.5949 -0.1845 0.027 Uiso 1 1 calc R . . C20 C 0.46843(11) 0.58385(12) 0.0016(5) 0.0209(8) Uani 1 1 d . . . H20 H 0.4982 0.5826 -0.0426 0.025 Uiso 1 1 calc R . . C21 C 0.46412(12) 0.57889(13) 0.1494(5) 0.0230(8) Uani 1 1 d . . . H21 H 0.4912 0.5747 0.2069 0.028 Uiso 1 1 calc R . . C22 C 0.42037(11) 0.57986(12) 0.2163(5) 0.0184(7) Uani 1 1 d . . . H22 H 0.4178 0.5767 0.3185 0.022 Uiso 1 1 calc R . . C23 C 0.32543(10) 0.55033(11) 0.3675(4) 0.0148(6) Uani 1 1 d . . . C24 C 0.31062(12) 0.50373(12) 0.3516(5) 0.0219(8) Uani 1 1 d . . . H24 H 0.2995 0.4930 0.2606 0.026 Uiso 1 1 calc R . . C25 C 0.31231(13) 0.47389(11) 0.4686(6) 0.0256(9) Uani 1 1 d . . . H25 H 0.3031 0.4424 0.4566 0.031 Uiso 1 1 calc R . . C26 C 0.32722(13) 0.48911(12) 0.6032(5) 0.0223(8) Uani 1 1 d . . . H26 H 0.3274 0.4685 0.6836 0.027 Uiso 1 1 calc R . . C27 C 0.34189(14) 0.53485(12) 0.6197(5) 0.0225(8) Uani 1 1 d . . . H27 H 0.3522 0.5456 0.7116 0.027 Uiso 1 1 calc R . . C28 C 0.34146(12) 0.56484(12) 0.5018(4) 0.0193(7) Uani 1 1 d . . . H28 H 0.3523 0.5958 0.5133 0.023 Uiso 1 1 calc R . . C29 C 0.08865(11) 0.60733(11) 0.3532(4) 0.0138(6) Uani 1 1 d . . . C30 C 0.08103(12) 0.56023(12) 0.3293(5) 0.0189(7) Uani 1 1 d . . . H30 H 0.0874 0.5473 0.2367 0.023 Uiso 1 1 calc R . . C31 C 0.06427(13) 0.53196(12) 0.4395(6) 0.0245(8) Uani 1 1 d . . . H31 H 0.0589 0.4999 0.4214 0.029 Uiso 1 1 calc R . . C32 C 0.05528(13) 0.55016(13) 0.5760(5) 0.0242(9) Uani 1 1 d . . . H32 H 0.0442 0.5306 0.6514 0.029 Uiso 1 1 calc R . . C33 C 0.06261(13) 0.59756(14) 0.6017(5) 0.0244(8) Uani 1 1 d . . . H33 H 0.0565 0.6105 0.6945 0.029 Uiso 1 1 calc R . . C34 C 0.07890(12) 0.62543(13) 0.4897(4) 0.0205(8) Uani 1 1 d . . . H34 H 0.0835 0.6577 0.5067 0.025 Uiso 1 1 calc R . . C35 C 0.05465(10) 0.66554(11) 0.1259(5) 0.0156(7) Uani 1 1 d . . . C36 C 0.01621(12) 0.67790(12) 0.2136(5) 0.0175(7) Uani 1 1 d . . . H36 H 0.0181 0.6754 0.3161 0.021 Uiso 1 1 calc R . . C37 C -0.02413(12) 0.69367(13) 0.1482(5) 0.0218(8) Uani 1 1 d . . . H37 H -0.0500 0.7019 0.2070 0.026 Uiso 1 1 calc R . . C38 C -0.02766(12) 0.69767(13) -0.0004(5) 0.0219(8) Uani 1 1 d . . . H38 H -0.0557 0.7083 -0.0433 0.026 Uiso 1 1 calc R . . C39 C 0.00999(13) 0.68606(14) -0.0867(5) 0.0220(8) Uani 1 1 d . . . H39 H 0.0077 0.6888 -0.1890 0.026 Uiso 1 1 calc R . . C40 C 0.05111(11) 0.67046(12) -0.0242(5) 0.0192(8) Uani 1 1 d . . . H40 H 0.0770 0.6631 -0.0840 0.023 Uiso 1 1 calc R . . C42 C 0.28888(12) 0.52518(13) -0.0017(5) 0.0213(8) Uani 1 1 d . . . C41 C 0.10818(11) 0.57590(11) -0.0217(5) 0.0180(7) Uani 1 1 d . . . C1S C 0.5057(7) 0.4999(4) 0.546(3) 0.066(6) Uani 0.25 1 d PDU A -1 H1SA H 0.5063 0.4844 0.6376 0.080 Uiso 0.25 1 d PR A -1 H1SB H 0.5342 0.4945 0.4945 0.080 Uiso 0.25 1 d PR A -1 Cl1S Cl 0.48127(9) 0.55529(12) 0.5600(3) 0.0523(7) Uani 0.50 1 d PD A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0146(12) 0.0185(13) 0.0105(18) 0.0007(11) -0.0021(12) 0.0019(10) Cl1 0.0128(3) 0.0150(3) 0.0168(4) -0.0005(3) -0.0007(3) 0.0005(3) O1 0.0145(9) 0.0121(8) 0.0188(14) 0.0002(10) -0.0043(10) 0.0009(7) P1 0.0121(3) 0.0118(3) 0.0135(5) -0.0001(3) -0.0008(3) 0.0004(2) Rh1 0.01172(9) 0.01319(9) 0.01337(13) -0.00057(9) -0.00082(9) 0.00073(7) C2 0.0140(12) 0.0114(12) 0.0149(19) 0.0009(11) -0.0016(11) 0.0000(9) Cl2 0.0163(3) 0.0290(4) 0.0131(5) -0.0064(3) -0.0012(3) 0.0029(3) O2 0.0161(9) 0.0132(9) 0.0194(14) -0.0001(10) 0.0027(10) 0.0016(7) P2 0.0115(3) 0.0120(3) 0.0145(5) -0.0019(3) -0.0007(3) 0.0008(2) Rh2 0.01088(9) 0.01454(9) 0.01298(13) -0.00188(9) -0.00070(9) 0.00031(7) C3 0.0146(12) 0.0091(11) 0.0161(19) -0.0015(11) -0.0012(11) 0.0011(9) O4 0.0335(13) 0.0244(12) 0.033(2) -0.0120(13) -0.0014(14) 0.0058(10) C4 0.0141(13) 0.0155(13) 0.019(2) 0.0010(12) -0.0013(12) -0.0009(10) O3 0.0237(11) 0.0259(12) 0.027(2) -0.0059(11) -0.0002(11) -0.0082(9) C5 0.0138(13) 0.0155(13) 0.020(2) 0.0004(12) -0.0066(12) -0.0031(10) C6 0.0183(13) 0.0132(12) 0.0149(19) -0.0022(11) -0.0056(12) 0.0007(10) C7 0.0135(11) 0.0126(12) 0.014(2) -0.0012(10) -0.0016(11) 0.0012(9) C8 0.0182(13) 0.0151(12) 0.013(2) -0.0013(11) -0.0022(11) 0.0016(10) C9 0.0133(12) 0.0143(12) 0.013(2) -0.0021(10) 0.0005(11) 0.0011(9) C10 0.0163(13) 0.0133(12) 0.017(2) -0.0033(12) -0.0021(12) 0.0020(10) C11 0.0171(13) 0.0140(13) 0.016(2) 0.0000(12) 0.0026(12) 0.0014(10) C12 0.0159(13) 0.0128(12) 0.016(2) 0.0012(11) 0.0013(12) 0.0025(10) C13 0.0125(12) 0.0119(12) 0.0152(19) -0.0001(11) 0.0025(11) 0.0023(9) C14 0.0139(12) 0.0120(12) 0.015(2) 0.0010(11) 0.0030(11) 0.0024(9) C15 0.0208(15) 0.0166(14) 0.030(3) -0.0001(14) 0.0001(15) -0.0051(12) C16 0.0246(16) 0.0112(13) 0.026(2) 0.0009(13) -0.0022(14) 0.0039(11) C17 0.0120(12) 0.0125(12) 0.0181(19) -0.0015(12) 0.0017(11) -0.0016(9) C18 0.0137(12) 0.0172(13) 0.019(2) 0.0032(12) -0.0003(11) 0.0013(10) C19 0.0215(15) 0.0202(15) 0.027(3) 0.0054(13) 0.0049(14) -0.0002(12) C20 0.0124(13) 0.0199(15) 0.030(2) -0.0012(13) 0.0038(12) -0.0013(11) C21 0.0147(14) 0.0227(16) 0.032(3) -0.0056(15) -0.0023(14) -0.0023(11) C22 0.0152(13) 0.0199(14) 0.020(2) -0.0025(13) -0.0017(12) 0.0026(11) C23 0.0136(12) 0.0151(13) 0.0156(19) 0.0000(12) -0.0015(11) 0.0026(10) C24 0.0240(16) 0.0179(14) 0.024(2) -0.0039(14) -0.0091(14) -0.0044(12) C25 0.0307(17) 0.0149(13) 0.031(3) 0.0046(15) -0.0064(17) -0.0063(12) C26 0.0257(16) 0.0203(15) 0.021(2) 0.0061(13) 0.0014(14) 0.0022(13) C27 0.0345(18) 0.0198(15) 0.013(2) 0.0016(13) -0.0036(15) 0.0018(13) C28 0.0252(15) 0.0159(13) 0.017(2) -0.0020(12) -0.0038(13) 0.0019(12) C29 0.0157(13) 0.0156(13) 0.0099(18) 0.0015(11) -0.0010(11) -0.0011(10) C30 0.0226(15) 0.0192(14) 0.015(2) 0.0008(12) 0.0025(13) -0.0013(12) C31 0.0281(16) 0.0177(14) 0.028(3) 0.0033(15) 0.0034(16) -0.0029(12) C32 0.0261(16) 0.0255(16) 0.021(3) 0.0050(14) 0.0006(14) -0.0038(13) C33 0.0251(17) 0.0283(17) 0.020(2) 0.0002(15) 0.0022(14) -0.0020(13) C34 0.0242(15) 0.0222(15) 0.015(2) -0.0026(12) 0.0023(13) -0.0026(12) C35 0.0124(12) 0.0150(13) 0.019(2) 0.0013(12) -0.0013(12) 0.0004(10) C36 0.0190(14) 0.0231(15) 0.0106(19) -0.0010(13) 0.0013(12) 0.0015(11) C37 0.0159(14) 0.0252(16) 0.024(2) 0.0006(15) 0.0052(13) 0.0039(12) C38 0.0160(14) 0.0262(16) 0.023(2) 0.0006(14) -0.0046(12) 0.0077(12) C39 0.0226(16) 0.0322(18) 0.011(2) 0.0020(13) -0.0006(13) 0.0032(14) C40 0.0142(13) 0.0239(15) 0.019(2) 0.0021(13) -0.0003(12) 0.0038(11) C42 0.0161(14) 0.0256(16) 0.022(2) -0.0049(13) -0.0020(12) -0.0004(12) C41 0.0168(13) 0.0188(13) 0.018(2) -0.0024(12) 0.0029(12) 0.0011(10) C1S 0.065(7) 0.069(6) 0.066(7) -0.001(5) 0.000(5) -0.008(4) Cl1S 0.0418(11) 0.094(2) 0.0208(16) 0.0139(14) -0.0153(10) -0.0140(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.427(4) . ? C1 O1 1.427(4) . ? C1 C8 1.565(4) . ? Cl1 Rh2 2.4017(8) . ? Cl1 Rh1 2.4037(8) . ? O1 C14 1.370(4) . ? P1 C29 1.819(4) . ? P1 C13 1.820(3) . ? P1 C35 1.822(3) . ? P1 Rh1 2.2477(9) . ? Rh1 C41 1.810(3) . ? Rh1 Cl2 2.4152(9) . ? C2 O2 1.372(4) . ? C2 C7 1.383(4) . ? C2 C3 1.388(5) . ? Cl2 Rh2 2.4024(9) . ? P2 C3 1.814(3) . ? P2 C17 1.825(3) . ? P2 C23 1.826(4) . ? P2 Rh2 2.2411(9) . ? Rh2 C42 1.813(4) . ? C3 C4 1.405(5) . ? O4 C42 1.142(4) . ? C4 C5 1.396(5) . ? O3 C41 1.149(4) . ? C5 C6 1.396(5) . ? C5 C15 1.502(5) . ? C6 C7 1.398(5) . ? C7 C8 1.515(5) . ? C8 C9 1.511(5) . ? C9 C10 1.381(4) . ? C9 C14 1.396(4) . ? C10 C11 1.390(5) . ? C11 C12 1.403(5) . ? C11 C16 1.519(5) . ? C12 C13 1.403(4) . ? C13 C14 1.388(5) . ? C17 C22 1.397(5) . ? C17 C18 1.398(5) . ? C18 C19 1.388(5) . ? C19 C20 1.393(5) . ? C20 C21 1.376(6) . ? C21 C22 1.402(5) . ? C23 C28 1.386(5) . ? C23 C24 1.414(5) . ? C24 C25 1.380(6) . ? C25 C26 1.385(6) . ? C26 C27 1.390(5) . ? C27 C28 1.389(6) . ? C29 C30 1.390(5) . ? C29 C34 1.391(5) . ? C30 C31 1.389(6) . ? C31 C32 1.388(6) . ? C32 C33 1.400(5) . ? C33 C34 1.389(6) . ? C35 C40 1.396(6) . ? C35 C36 1.415(5) . ? C36 C37 1.384(5) . ? C37 C38 1.380(7) . ? C38 C39 1.385(5) . ? C39 C40 1.390(5) . ? C1S Cl1S 1.744(5) . ? 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 O2 C1 O1 107.3(3) . . ? O2 C1 C8 108.0(3) . . ? O1 C1 C8 108.1(2) . . ? Rh2 Cl1 Rh1 84.94(2) . . ? C14 O1 C1 108.2(2) . . ? C29 P1 C13 106.30(17) . . ? C29 P1 C35 103.32(16) . . ? C13 P1 C35 103.96(15) . . ? C29 P1 Rh1 116.93(11) . . ? C13 P1 Rh1 111.33(11) . . ? C35 P1 Rh1 113.84(14) . . ? C41 Rh1 P1 88.74(12) . . ? C41 Rh1 Cl1 173.66(12) . . ? P1 Rh1 Cl1 97.60(3) . . ? C41 Rh1 Cl2 91.45(12) . . ? P1 Rh1 Cl2 178.20(4) . . ? Cl1 Rh1 Cl2 82.21(3) . . ? O2 C2 C7 113.0(3) . . ? O2 C2 C3 123.4(3) . . ? C7 C2 C3 123.6(3) . . ? Rh2 Cl2 Rh1 84.67(3) . . ? C2 O2 C1 108.5(2) . . ? C3 P2 C17 101.89(14) . . ? C3 P2 C23 105.00(17) . . ? C17 P2 C23 103.99(15) . . ? C3 P2 Rh2 112.31(11) . . ? C17 P2 Rh2 112.82(13) . . ? C23 P2 Rh2 119.06(11) . . ? C42 Rh2 P2 90.03(12) . . ? C42 Rh2 Cl1 173.09(11) . . ? P2 Rh2 Cl1 96.49(3) . . ? C42 Rh2 Cl2 91.19(12) . . ? P2 Rh2 Cl2 174.86(3) . . ? Cl1 Rh2 Cl2 82.52(3) . . ? C2 C3 C4 115.9(3) . . ? C2 C3 P2 120.3(2) . . ? C4 C3 P2 122.7(3) . . ? C5 C4 C3 122.6(3) . . ? C4 C5 C6 118.9(3) . . ? C4 C5 C15 119.8(3) . . ? C6 C5 C15 121.3(3) . . ? C5 C6 C7 120.0(3) . . ? C2 C7 C6 118.8(3) . . ? C2 C7 C8 108.8(3) . . ? C6 C7 C8 132.0(3) . . ? C9 C8 C7 110.4(3) . . ? C9 C8 C1 101.5(2) . . ? C7 C8 C1 101.0(2) . . ? C10 C9 C14 120.2(3) . . ? C10 C9 C8 131.4(3) . . ? C14 C9 C8 108.0(3) . . ? C9 C10 C11 119.1(3) . . ? C10 C11 C12 119.9(3) . . ? C10 C11 C16 121.1(3) . . ? C12 C11 C16 119.0(3) . . ? C11 C12 C13 122.0(3) . . ? C14 C13 C12 116.1(3) . . ? C14 C13 P1 121.4(2) . . ? C12 C13 P1 121.2(3) . . ? O1 C14 C13 123.7(3) . . ? O1 C14 C9 113.6(3) . . ? C13 C14 C9 122.7(3) . . ? C22 C17 C18 119.3(3) . . ? C22 C17 P2 121.6(3) . . ? C18 C17 P2 119.0(3) . . ? C19 C18 C17 120.6(3) . . ? C18 C19 C20 120.0(4) . . ? C21 C20 C19 119.6(3) . . ? C20 C21 C22 121.0(4) . . ? C17 C22 C21 119.4(4) . . ? C28 C23 C24 118.6(3) . . ? C28 C23 P2 121.7(2) . . ? C24 C23 P2 119.7(3) . . ? C25 C24 C23 119.8(4) . . ? C24 C25 C26 121.1(3) . . ? C25 C26 C27 119.4(4) . . ? C28 C27 C26 119.9(4) . . ? C23 C28 C27 121.1(3) . . ? C30 C29 C34 118.5(3) . . ? C30 C29 P1 119.3(3) . . ? C34 C29 P1 122.2(2) . . ? C31 C30 C29 120.6(4) . . ? C32 C31 C30 120.6(3) . . ? C31 C32 C33 119.5(4) . . ? C34 C33 C32 119.1(4) . . ? C33 C34 C29 121.7(3) . . ? C40 C35 C36 119.0(3) . . ? C40 C35 P1 119.4(3) . . ? C36 C35 P1 121.6(3) . . ? C37 C36 C35 119.2(4) . . ? C38 C37 C36 121.5(4) . . ? C37 C38 C39 119.6(3) . . ? C38 C39 C40 120.3(4) . . ? C39 C40 C35 120.4(3) . . ? O4 C42 Rh2 176.8(3) . . ? O3 C41 Rh1 177.3(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 C14 -110.6(3) . . . . ? C8 C1 O1 C14 5.7(4) . . . . ? C29 P1 Rh1 C41 70.15(17) . . . . ? C13 P1 Rh1 C41 -167.43(17) . . . . ? C35 P1 Rh1 C41 -50.32(17) . . . . ? C29 P1 Rh1 Cl1 -110.11(12) . . . . ? C13 P1 Rh1 Cl1 12.32(13) . . . . ? C35 P1 Rh1 Cl1 129.42(12) . . . . ? C29 P1 Rh1 Cl2 166.1(10) . . . . ? C13 P1 Rh1 Cl2 -71.5(10) . . . . ? C35 P1 Rh1 Cl2 45.6(10) . . . . ? Rh2 Cl1 Rh1 C41 -37.4(11) . . . . ? Rh2 Cl1 Rh1 P1 144.88(3) . . . . ? Rh2 Cl1 Rh1 Cl2 -36.92(3) . . . . ? C41 Rh1 Cl2 Rh2 -143.13(12) . . . . ? P1 Rh1 Cl2 Rh2 121.0(10) . . . . ? Cl1 Rh1 Cl2 Rh2 36.93(3) . . . . ? C7 C2 O2 C1 8.7(4) . . . . ? C3 C2 O2 C1 -170.7(3) . . . . ? O1 C1 O2 C2 110.9(3) . . . . ? C8 C1 O2 C2 -5.5(4) . . . . ? C3 P2 Rh2 C42 171.14(18) . . . . ? C17 P2 Rh2 C42 56.66(17) . . . . ? C23 P2 Rh2 C42 -65.61(18) . . . . ? C3 P2 Rh2 Cl1 -11.14(13) . . . . ? C17 P2 Rh2 Cl1 -125.62(11) . . . . ? C23 P2 Rh2 Cl1 112.10(13) . . . . ? C3 P2 Rh2 Cl2 67.4(4) . . . . ? C17 P2 Rh2 Cl2 -47.1(4) . . . . ? C23 P2 Rh2 Cl2 -169.3(3) . . . . ? Rh1 Cl1 Rh2 C42 12.7(11) . . . . ? Rh1 Cl1 Rh2 P2 -147.96(3) . . . . ? Rh1 Cl1 Rh2 Cl2 37.12(3) . . . . ? Rh1 Cl2 Rh2 C42 140.22(13) . . . . ? Rh1 Cl2 Rh2 P2 -116.1(3) . . . . ? Rh1 Cl2 Rh2 Cl1 -36.93(3) . . . . ? O2 C2 C3 C4 -177.6(3) . . . . ? C7 C2 C3 C4 3.1(5) . . . . ? O2 C2 C3 P2 13.8(5) . . . . ? C7 C2 C3 P2 -165.5(3) . . . . ? C17 P2 C3 C2 -166.8(3) . . . . ? C23 P2 C3 C2 -58.6(3) . . . . ? Rh2 P2 C3 C2 72.2(3) . . . . ? C17 P2 C3 C4 25.4(3) . . . . ? C23 P2 C3 C4 133.6(3) . . . . ? Rh2 P2 C3 C4 -95.6(3) . . . . ? C2 C3 C4 C5 -0.5(5) . . . . ? P2 C3 C4 C5 167.7(3) . . . . ? C3 C4 C5 C6 -1.8(6) . . . . ? C3 C4 C5 C15 179.2(4) . . . . ? C4 C5 C6 C7 1.7(5) . . . . ? C15 C5 C6 C7 -179.3(3) . . . . ? O2 C2 C7 C6 177.4(3) . . . . ? C3 C2 C7 C6 -3.2(5) . . . . ? O2 C2 C7 C8 -8.3(4) . . . . ? C3 C2 C7 C8 171.1(3) . . . . ? C5 C6 C7 C2 0.6(5) . . . . ? C5 C6 C7 C8 -172.1(4) . . . . ? C2 C7 C8 C9 -102.5(3) . . . . ? C6 C7 C8 C9 70.8(5) . . . . ? C2 C7 C8 C1 4.2(4) . . . . ? C6 C7 C8 C1 177.5(4) . . . . ? O2 C1 C8 C9 114.4(3) . . . . ? O1 C1 C8 C9 -1.5(4) . . . . ? O2 C1 C8 C7 0.7(3) . . . . ? O1 C1 C8 C7 -115.1(3) . . . . ? C7 C8 C9 C10 -69.4(5) . . . . ? C1 C8 C9 C10 -175.8(4) . . . . ? C7 C8 C9 C14 103.2(3) . . . . ? C1 C8 C9 C14 -3.2(4) . . . . ? C14 C9 C10 C11 -0.3(5) . . . . ? C8 C9 C10 C11 171.6(4) . . . . ? C9 C10 C11 C12 -2.3(5) . . . . ? C9 C10 C11 C16 -179.4(3) . . . . ? C10 C11 C12 C13 2.2(6) . . . . ? C16 C11 C12 C13 179.3(3) . . . . ? C11 C12 C13 C14 0.6(5) . . . . ? C11 C12 C13 P1 -166.9(3) . . . . ? C29 P1 C13 C14 55.2(3) . . . . ? C35 P1 C13 C14 163.9(3) . . . . ? Rh1 P1 C13 C14 -73.2(3) . . . . ? C29 P1 C13 C12 -138.0(3) . . . . ? C35 P1 C13 C12 -29.3(3) . . . . ? Rh1 P1 C13 C12 93.6(3) . . . . ? C1 O1 C14 C13 169.4(3) . . . . ? C1 O1 C14 C9 -8.3(4) . . . . ? C12 C13 C14 O1 179.3(3) . . . . ? P1 C13 C14 O1 -13.2(5) . . . . ? C12 C13 C14 C9 -3.2(5) . . . . ? P1 C13 C14 C9 164.2(3) . . . . ? C10 C9 C14 O1 -179.2(3) . . . . ? C8 C9 C14 O1 7.3(4) . . . . ? C10 C9 C14 C13 3.2(5) . . . . ? C8 C9 C14 C13 -170.4(3) . . . . ? C3 P2 C17 C22 73.3(3) . . . . ? C23 P2 C17 C22 -35.7(3) . . . . ? Rh2 P2 C17 C22 -166.1(2) . . . . ? C3 P2 C17 C18 -102.0(3) . . . . ? C23 P2 C17 C18 149.0(3) . . . . ? Rh2 P2 C17 C18 18.6(3) . . . . ? C22 C17 C18 C19 1.4(5) . . . . ? P2 C17 C18 C19 176.8(3) . . . . ? C17 C18 C19 C20 0.3(5) . . . . ? C18 C19 C20 C21 -1.5(5) . . . . ? C19 C20 C21 C22 1.0(5) . . . . ? C18 C17 C22 C21 -1.8(5) . . . . ? P2 C17 C22 C21 -177.1(3) . . . . ? C20 C21 C22 C17 0.6(5) . . . . ? C3 P2 C23 C28 -19.7(3) . . . . ? C17 P2 C23 C28 87.0(3) . . . . ? Rh2 P2 C23 C28 -146.4(2) . . . . ? C3 P2 C23 C24 160.1(3) . . . . ? C17 P2 C23 C24 -93.2(3) . . . . ? Rh2 P2 C23 C24 33.3(3) . . . . ? C28 C23 C24 C25 0.1(5) . . . . ? P2 C23 C24 C25 -179.7(3) . . . . ? C23 C24 C25 C26 1.6(6) . . . . ? C24 C25 C26 C27 -1.7(6) . . . . ? C25 C26 C27 C28 0.1(6) . . . . ? C24 C23 C28 C27 -1.8(5) . . . . ? P2 C23 C28 C27 178.0(3) . . . . ? C26 C27 C28 C23 1.7(6) . . . . ? C13 P1 C29 C30 -159.1(3) . . . . ? C35 P1 C29 C30 91.8(3) . . . . ? Rh1 P1 C29 C30 -34.1(3) . . . . ? C13 P1 C29 C34 23.6(3) . . . . ? C35 P1 C29 C34 -85.5(3) . . . . ? Rh1 P1 C29 C34 148.6(2) . . . . ? C34 C29 C30 C31 -0.3(5) . . . . ? P1 C29 C30 C31 -177.7(3) . . . . ? C29 C30 C31 C32 -0.7(6) . . . . ? C30 C31 C32 C33 0.9(6) . . . . ? C31 C32 C33 C34 -0.2(6) . . . . ? C32 C33 C34 C29 -0.8(6) . . . . ? C30 C29 C34 C33 1.0(5) . . . . ? P1 C29 C34 C33 178.4(3) . . . . ? C29 P1 C35 C40 -142.4(3) . . . . ? C13 P1 C35 C40 106.7(3) . . . . ? Rh1 P1 C35 C40 -14.6(3) . . . . ? C29 P1 C35 C36 37.9(3) . . . . ? C13 P1 C35 C36 -73.0(3) . . . . ? Rh1 P1 C35 C36 165.7(2) . . . . ? C40 C35 C36 C37 1.2(5) . . . . ? P1 C35 C36 C37 -179.1(3) . . . . ? C35 C36 C37 C38 -0.1(6) . . . . ? C36 C37 C38 C39 -0.5(6) . . . . ? C37 C38 C39 C40 0.0(6) . . . . ? C38 C39 C40 C35 1.1(6) . . . . ? C36 C35 C40 C39 -1.7(5) . . . . ? P1 C35 C40 C39 178.5(3) . . . . ? P2 Rh2 C42 O4 155(7) . . . . ? Cl1 Rh2 C42 O4 -6(8) . . . . ? Cl2 Rh2 C42 O4 -30(7) . . . . ? P1 Rh1 C41 O3 172(100) . . . . ? Cl1 Rh1 C41 O3 -6(9) . . . . ? Cl2 Rh1 C41 O3 -6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.940 _diffrn_reflns_theta_full 33.17 _diffrn_measured_fraction_theta_full 0.940 _refine_diff_density_max 2.473 _refine_diff_density_min -0.644 _refine_diff_density_rms 0.133 #===END