# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Martin Cowie' 'Matthias Bierenstiel' 'Michael J Ferguson' 'Lindsay J. Hounjet' 'Robert McDonald' _publ_contact_author_name 'Martin Cowie' _publ_contact_author_email MARTIN.COWIE@UALBERTA.CA _publ_section_title ; Mono- and Binuclear Complexes of Rhodium Involving a New Series of Hemilabile o-Phosphinoaniline Ligands ; # Attachment 'b822170g.cif' data_compound(5) _database_code_depnum_ccdc_archive 'CCDC 713707' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 Cl N O P Rh, 0.25(C H2 Cl2)' _chemical_formula_sum 'C20.25 H18.5 Cl1.5 N O P Rh' _chemical_formula_weight 478.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.2776(8) _cell_length_b 34.571(3) _cell_length_c 11.5554(9) _cell_angle_alpha 90.00 _cell_angle_beta 103.2770(10) _cell_angle_gamma 90.00 _cell_volume 3996.0(5) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6862 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 26.38 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.592 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1924 _exptl_absorpt_coefficient_mu 1.144 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6390 _exptl_absorpt_correction_T_max 0.9041 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30586 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0236 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 26.39 _reflns_number_total 8169 _reflns_number_gt 7347 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0325P)^2^+2.5251P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8169 _refine_ls_number_parameters 451 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0356 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0746 _refine_ls_wR_factor_gt 0.0728 _refine_ls_goodness_of_fit_ref 1.137 _refine_ls_restrained_S_all 1.137 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh1A Rh 0.43053(2) 0.310648(6) 0.363552(16) 0.02837(6) Uani 1 1 d . . . Cl1A Cl 0.45688(7) 0.33817(2) 0.55763(5) 0.03943(15) Uani 1 1 d . . . P1A P 0.36924(6) 0.286556(19) 0.18365(5) 0.02758(13) Uani 1 1 d . . . O1A O 0.7156(2) 0.30572(8) 0.3538(2) 0.0601(6) Uani 1 1 d . . . N1A N 0.2219(2) 0.30870(6) 0.3570(2) 0.0329(5) Uani 1 1 d . . . H1NA H 0.2004 0.3317 0.3897 0.039 Uiso 1 1 calc R . . C1A C 0.6063(3) 0.30857(9) 0.3596(2) 0.0385(6) Uani 1 1 d . . . C2A C 0.1935(3) 0.27690(10) 0.4344(3) 0.0479(7) Uani 1 1 d . . . H2AA H 0.0977 0.2764 0.4323 0.058 Uiso 1 1 calc R . . H2BA H 0.2440 0.2812 0.5162 0.058 Uiso 1 1 calc R . . H2CA H 0.2201 0.2521 0.4056 0.058 Uiso 1 1 calc R . . C11A C 0.1898(3) 0.29491(7) 0.1444(2) 0.0317(5) Uani 1 1 d . . . C12A C 0.1341(3) 0.30566(8) 0.2377(2) 0.0340(6) Uani 1 1 d . . . C13A C -0.0021(3) 0.31282(9) 0.2200(3) 0.0495(8) Uani 1 1 d . . . H13A H -0.0399 0.3198 0.2848 0.059 Uiso 1 1 calc R . . C14A C -0.0819(3) 0.30958(10) 0.1058(3) 0.0586(9) Uani 1 1 d . . . H14A H -0.1751 0.3146 0.0925 0.070 Uiso 1 1 calc R . . C15A C -0.0278(3) 0.29921(10) 0.0114(3) 0.0534(8) Uani 1 1 d . . . H15A H -0.0834 0.2973 -0.0664 0.064 Uiso 1 1 calc R . . C16A C 0.1073(3) 0.29164(8) 0.0304(3) 0.0407(6) Uani 1 1 d . . . H16A H 0.1445 0.2842 -0.0344 0.049 Uiso 1 1 calc R . . C21A C 0.4358(3) 0.30555(8) 0.0619(2) 0.0307(5) Uani 1 1 d . . . C22A C 0.4119(3) 0.28654(8) -0.0481(2) 0.0368(6) Uani 1 1 d . . . H22A H 0.3615 0.2633 -0.0597 0.044 Uiso 1 1 calc R . . C23A C 0.4621(3) 0.30179(9) -0.1398(2) 0.0426(7) Uani 1 1 d . . . H23A H 0.4441 0.2893 -0.2150 0.051 Uiso 1 1 calc R . . C24A C 0.5380(3) 0.33503(9) -0.1224(3) 0.0449(7) Uani 1 1 d . . . H24A H 0.5730 0.3452 -0.1854 0.054 Uiso 1 1 calc R . . C25A C 0.5632(3) 0.35356(9) -0.0141(3) 0.0419(7) Uani 1 1 d . . . H25A H 0.6166 0.3763 -0.0023 0.050 Uiso 1 1 calc R . . C26A C 0.5112(3) 0.33932(8) 0.0779(2) 0.0343(6) Uani 1 1 d . . . H26A H 0.5271 0.3526 0.1518 0.041 Uiso 1 1 calc R . . C31A C 0.3911(3) 0.23464(7) 0.1700(2) 0.0295(5) Uani 1 1 d . . . C32A C 0.5196(3) 0.22078(8) 0.1726(2) 0.0366(6) Uani 1 1 d . . . H32A H 0.5923 0.2384 0.1818 0.044 Uiso 1 1 calc R . . C33A C 0.5414(3) 0.18163(9) 0.1619(3) 0.0436(7) Uani 1 1 d . . . H33A H 0.6285 0.1725 0.1617 0.052 Uiso 1 1 calc R . . C34A C 0.4372(3) 0.15589(9) 0.1517(3) 0.0435(7) Uani 1 1 d . . . H34A H 0.4526 0.1290 0.1449 0.052 Uiso 1 1 calc R . . C35A C 0.3106(3) 0.16903(8) 0.1512(2) 0.0408(6) Uani 1 1 d . . . H35A H 0.2392 0.1511 0.1450 0.049 Uiso 1 1 calc R . . C36A C 0.2868(3) 0.20843(8) 0.1596(2) 0.0338(6) Uani 1 1 d . . . H36A H 0.1991 0.2174 0.1583 0.041 Uiso 1 1 calc R . . Rh1B Rh 0.31038(2) -0.082015(6) 0.203965(18) 0.03272(6) Uani 1 1 d . . . Cl1B Cl 0.39226(7) -0.11137(2) 0.04884(6) 0.04206(16) Uani 1 1 d . . . P1B P 0.21216(7) -0.05098(2) 0.32567(6) 0.03083(14) Uani 1 1 d . . . O1B O 0.5588(2) -0.09141(10) 0.3892(2) 0.0801(9) Uani 1 1 d . . . N1B N 0.1158(3) -0.07958(7) 0.0876(2) 0.0451(6) Uani 1 1 d . . . H1NB H 0.1026 -0.1031 0.0474 0.054 Uiso 1 1 calc R . . C1B C 0.4648(3) -0.08698(10) 0.3157(3) 0.0482(7) Uani 1 1 d . . . C2B C 0.1078(4) -0.04883(12) -0.0044(3) 0.0705(11) Uani 1 1 d . . . H2AB H 0.0183 -0.0489 -0.0573 0.085 Uiso 1 1 calc R . . H2BB H 0.1746 -0.0539 -0.0510 0.085 Uiso 1 1 calc R . . H2CB H 0.1252 -0.0236 0.0345 0.085 Uiso 1 1 calc R . . C11B C 0.0368(3) -0.06055(8) 0.2635(3) 0.0376(6) Uani 1 1 d . . . C12B C 0.0073(3) -0.07547(9) 0.1496(3) 0.0482(7) Uani 1 1 d . . . C13B C -0.1226(4) -0.08684(12) 0.0966(4) 0.0745(12) Uani 1 1 d . . . H13B H -0.1431 -0.0973 0.0185 0.089 Uiso 1 1 calc R . . C14B C -0.2214(4) -0.08266(14) 0.1592(5) 0.0928(16) Uani 1 1 d . . . H14B H -0.3100 -0.0907 0.1240 0.111 Uiso 1 1 calc R . . C15B C -0.1932(4) -0.06700(13) 0.2715(5) 0.0764(12) Uani 1 1 d . . . H15B H -0.2627 -0.0636 0.3124 0.092 Uiso 1 1 calc R . . C16B C -0.0646(3) -0.05630(10) 0.3249(3) 0.0525(8) Uani 1 1 d . . . H16B H -0.0448 -0.0460 0.4033 0.063 Uiso 1 1 calc R . . C21B C 0.2387(3) -0.06418(8) 0.4816(2) 0.0346(6) Uani 1 1 d . . . C22B C 0.2293(3) -0.03792(10) 0.5698(3) 0.0525(8) Uani 1 1 d . . . H22B H 0.2128 -0.0114 0.5506 0.063 Uiso 1 1 calc R . . C23B C 0.2439(4) -0.05042(12) 0.6858(3) 0.0609(10) Uani 1 1 d . . . H23B H 0.2377 -0.0324 0.7463 0.073 Uiso 1 1 calc R . . C24B C 0.2673(3) -0.08900(12) 0.7141(3) 0.0582(9) Uani 1 1 d . . . H24B H 0.2764 -0.0975 0.7937 0.070 Uiso 1 1 calc R . . C25B C 0.2775(3) -0.11497(10) 0.6270(3) 0.0512(8) Uani 1 1 d . . . H25B H 0.2937 -0.1415 0.6466 0.061 Uiso 1 1 calc R . . C26B C 0.2644(3) -0.10301(9) 0.5114(3) 0.0410(6) Uani 1 1 d . . . H26B H 0.2728 -0.1212 0.4518 0.049 Uiso 1 1 calc R . . C31B C 0.2311(3) 0.00127(8) 0.3271(2) 0.0341(6) Uani 1 1 d . . . C32B C 0.1237(3) 0.02654(9) 0.3055(3) 0.0440(7) Uani 1 1 d . . . H32B H 0.0352 0.0166 0.2895 0.053 Uiso 1 1 calc R . . C33B C 0.1444(4) 0.06613(9) 0.3069(3) 0.0542(8) Uani 1 1 d . . . H33B H 0.0700 0.0832 0.2919 0.065 Uiso 1 1 calc R . . C34B C 0.2723(4) 0.08078(9) 0.3302(3) 0.0567(9) Uani 1 1 d . . . H34B H 0.2863 0.1079 0.3307 0.068 Uiso 1 1 calc R . . C35B C 0.3791(4) 0.05609(10) 0.3524(4) 0.0625(9) Uani 1 1 d . . . H35B H 0.4674 0.0662 0.3698 0.075 Uiso 1 1 calc R . . C36B C 0.3597(3) 0.01650(10) 0.3500(3) 0.0531(8) Uani 1 1 d . . . H36B H 0.4346 -0.0004 0.3640 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1A 0.02828(11) 0.03564(11) 0.02256(10) 0.00155(7) 0.00864(7) 0.00071(8) Cl1A 0.0445(4) 0.0502(4) 0.0229(3) -0.0004(3) 0.0063(3) 0.0021(3) P1A 0.0288(3) 0.0312(3) 0.0243(3) 0.0014(2) 0.0093(2) 0.0027(3) O1A 0.0314(12) 0.100(2) 0.0495(13) 0.0002(12) 0.0115(10) 0.0045(11) N1A 0.0328(12) 0.0354(12) 0.0341(12) -0.0032(9) 0.0156(9) -0.0007(9) C1A 0.0357(16) 0.0554(18) 0.0242(13) -0.0001(11) 0.0065(11) -0.0004(12) C2A 0.0504(18) 0.0563(19) 0.0437(17) 0.0032(14) 0.0245(14) -0.0122(15) C11A 0.0308(13) 0.0274(13) 0.0368(14) -0.0005(10) 0.0072(11) 0.0011(10) C12A 0.0299(13) 0.0332(14) 0.0392(14) -0.0050(11) 0.0086(11) 0.0002(10) C13A 0.0336(16) 0.056(2) 0.060(2) -0.0160(15) 0.0123(14) 0.0009(13) C14A 0.0295(16) 0.065(2) 0.076(2) -0.0169(18) 0.0009(16) 0.0053(14) C15A 0.0411(17) 0.059(2) 0.0509(18) -0.0079(16) -0.0072(14) 0.0023(15) C16A 0.0418(16) 0.0396(15) 0.0374(15) -0.0041(12) 0.0024(12) 0.0016(12) C21A 0.0324(13) 0.0360(14) 0.0260(12) 0.0065(10) 0.0111(10) 0.0089(10) C22A 0.0438(16) 0.0371(15) 0.0313(13) 0.0013(11) 0.0121(12) 0.0046(12) C23A 0.0591(19) 0.0447(16) 0.0272(13) 0.0036(12) 0.0167(13) 0.0107(14) C24A 0.0566(18) 0.0497(18) 0.0341(15) 0.0117(13) 0.0221(13) 0.0064(14) C25A 0.0472(17) 0.0406(15) 0.0417(16) 0.0068(12) 0.0177(13) -0.0015(13) C26A 0.0380(14) 0.0379(14) 0.0281(13) 0.0041(11) 0.0100(11) 0.0041(11) C31A 0.0362(13) 0.0325(13) 0.0214(11) 0.0031(9) 0.0102(10) 0.0046(10) C32A 0.0359(14) 0.0418(15) 0.0356(14) 0.0057(12) 0.0151(11) 0.0039(12) C33A 0.0482(17) 0.0456(17) 0.0413(16) 0.0096(13) 0.0193(13) 0.0163(13) C34A 0.0584(19) 0.0349(15) 0.0388(15) 0.0035(12) 0.0143(13) 0.0121(13) C35A 0.0495(17) 0.0326(14) 0.0378(15) 0.0012(12) 0.0048(12) -0.0012(12) C36A 0.0345(14) 0.0365(14) 0.0300(13) 0.0025(11) 0.0066(11) 0.0050(11) Rh1B 0.03371(12) 0.03620(12) 0.03000(11) -0.00158(8) 0.01094(8) 0.00029(8) Cl1B 0.0501(4) 0.0438(4) 0.0381(3) -0.0034(3) 0.0220(3) -0.0005(3) P1B 0.0305(3) 0.0329(3) 0.0305(3) -0.0010(3) 0.0098(3) -0.0002(3) O1B 0.0392(14) 0.142(3) 0.0551(15) -0.0078(16) 0.0033(12) 0.0070(15) N1B 0.0482(15) 0.0438(14) 0.0386(13) -0.0120(11) 0.0005(11) 0.0076(11) C1B 0.0376(16) 0.068(2) 0.0433(17) -0.0053(15) 0.0175(14) -0.0006(14) C2B 0.082(3) 0.084(3) 0.0410(18) 0.0102(18) 0.0053(17) 0.030(2) C11B 0.0309(14) 0.0315(14) 0.0500(16) -0.0022(12) 0.0088(12) -0.0005(11) C12B 0.0336(15) 0.0469(18) 0.0592(19) -0.0117(15) 0.0006(14) 0.0044(13) C13B 0.047(2) 0.070(3) 0.095(3) -0.036(2) -0.010(2) 0.0027(18) C14B 0.0318(19) 0.087(3) 0.150(5) -0.036(3) 0.003(2) -0.0062(19) C15B 0.0363(19) 0.076(3) 0.122(4) -0.014(3) 0.027(2) -0.0055(18) C16B 0.0396(17) 0.0489(18) 0.072(2) -0.0014(16) 0.0196(16) -0.0011(14) C21B 0.0318(13) 0.0434(15) 0.0308(13) 0.0023(11) 0.0118(11) 0.0020(11) C22B 0.063(2) 0.058(2) 0.0402(16) 0.0019(14) 0.0191(15) 0.0200(16) C23B 0.071(2) 0.081(3) 0.0342(16) 0.0017(16) 0.0191(15) 0.026(2) C24B 0.0514(19) 0.086(3) 0.0386(17) 0.0179(17) 0.0125(15) 0.0079(18) C25B 0.0529(19) 0.055(2) 0.0429(17) 0.0135(15) 0.0058(14) -0.0056(15) C26B 0.0410(16) 0.0411(16) 0.0403(15) 0.0026(12) 0.0077(12) -0.0055(12) C31B 0.0425(15) 0.0324(13) 0.0282(12) -0.0013(10) 0.0098(11) -0.0034(11) C32B 0.0448(17) 0.0391(16) 0.0446(16) -0.0029(13) 0.0029(13) -0.0009(13) C33B 0.066(2) 0.0362(16) 0.0543(19) -0.0039(14) 0.0010(16) 0.0056(15) C34B 0.084(3) 0.0351(16) 0.0507(19) -0.0028(14) 0.0141(18) -0.0108(17) C35B 0.058(2) 0.049(2) 0.083(3) -0.0126(18) 0.0231(19) -0.0177(17) C36B 0.0432(17) 0.0459(18) 0.071(2) -0.0057(16) 0.0142(16) -0.0053(14) _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 Rh1A C1A 1.819(3) . ? Rh1A N1A 2.129(2) . ? Rh1A P1A 2.1933(7) . ? Rh1A Cl1A 2.3936(7) . ? P1A C11A 1.819(3) . ? P1A C31A 1.820(3) . ? P1A C21A 1.823(2) . ? O1A C1A 1.145(3) . ? N1A C12A 1.468(3) . ? N1A C2A 1.488(4) . ? C11A C12A 1.383(4) . ? C11A C16A 1.398(4) . ? C12A C13A 1.390(4) . ? C13A C14A 1.389(5) . ? C14A C15A 1.381(5) . ? C15A C16A 1.381(4) . ? C21A C26A 1.390(4) . ? C21A C22A 1.401(4) . ? C22A C23A 1.385(4) . ? C23A C24A 1.377(5) . ? C24A C25A 1.377(4) . ? C25A C26A 1.385(4) . ? C31A C36A 1.387(4) . ? C31A C32A 1.399(4) . ? C32A C33A 1.382(4) . ? C33A C34A 1.376(4) . ? C34A C35A 1.377(4) . ? C35A C36A 1.391(4) . ? Rh1B C1B 1.809(3) . ? Rh1B N1B 2.140(2) . ? Rh1B P1B 2.1909(7) . ? Rh1B Cl1B 2.3757(7) . ? P1B C11B 1.811(3) . ? P1B C31B 1.816(3) . ? P1B C21B 1.818(3) . ? O1B C1B 1.141(4) . ? N1B C12B 1.465(4) . ? N1B C2B 1.492(4) . ? C11B C12B 1.381(4) . ? C11B C16B 1.397(4) . ? C12B C13B 1.391(5) . ? C13B C14B 1.383(6) . ? C14B C15B 1.374(7) . ? C15B C16B 1.374(5) . ? C21B C22B 1.384(4) . ? C21B C26B 1.396(4) . ? C22B C23B 1.384(4) . ? C23B C24B 1.381(5) . ? C24B C25B 1.371(5) . ? C25B C26B 1.375(4) . ? C31B C32B 1.384(4) . ? C31B C36B 1.391(4) . ? C32B C33B 1.385(4) . ? C33B C34B 1.377(5) . ? C34B C35B 1.368(5) . ? C35B C36B 1.382(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 C1A Rh1A N1A 174.70(11) . . ? C1A Rh1A P1A 91.83(9) . . ? N1A Rh1A P1A 83.49(6) . . ? C1A Rh1A Cl1A 98.04(9) . . ? N1A Rh1A Cl1A 86.69(6) . . ? P1A Rh1A Cl1A 170.08(3) . . ? C11A P1A C31A 105.87(12) . . ? C11A P1A C21A 106.83(12) . . ? C31A P1A C21A 102.27(11) . . ? C11A P1A Rh1A 103.30(9) . . ? C31A P1A Rh1A 116.25(8) . . ? C21A P1A Rh1A 121.19(9) . . ? C12A N1A C2A 110.4(2) . . ? C12A N1A Rh1A 115.65(16) . . ? C2A N1A Rh1A 109.70(18) . . ? O1A C1A Rh1A 176.7(3) . . ? C12A C11A C16A 119.2(2) . . ? C12A C11A P1A 115.2(2) . . ? C16A C11A P1A 125.6(2) . . ? C11A C12A C13A 121.1(3) . . ? C11A C12A N1A 118.4(2) . . ? C13A C12A N1A 120.5(3) . . ? C14A C13A C12A 118.7(3) . . ? C15A C14A C13A 121.0(3) . . ? C16A C15A C14A 119.8(3) . . ? C15A C16A C11A 120.3(3) . . ? C26A C21A C22A 119.4(2) . . ? C26A C21A P1A 119.75(19) . . ? C22A C21A P1A 120.8(2) . . ? C23A C22A C21A 119.8(3) . . ? C24A C23A C22A 120.2(3) . . ? C23A C24A C25A 120.2(3) . . ? C24A C25A C26A 120.5(3) . . ? C25A C26A C21A 119.8(3) . . ? C36A C31A C32A 119.0(2) . . ? C36A C31A P1A 122.9(2) . . ? C32A C31A P1A 118.1(2) . . ? C33A C32A C31A 120.4(3) . . ? C34A C33A C32A 120.1(3) . . ? C33A C34A C35A 120.2(3) . . ? C34A C35A C36A 120.2(3) . . ? C31A C36A C35A 120.1(3) . . ? C1B Rh1B N1B 172.77(12) . . ? C1B Rh1B P1B 92.65(10) . . ? N1B Rh1B P1B 83.24(7) . . ? C1B Rh1B Cl1B 95.36(10) . . ? N1B Rh1B Cl1B 89.11(7) . . ? P1B Rh1B Cl1B 171.41(3) . . ? C11B P1B C31B 106.25(13) . . ? C11B P1B C21B 104.87(13) . . ? C31B P1B C21B 104.43(12) . . ? C11B P1B Rh1B 102.67(9) . . ? C31B P1B Rh1B 115.39(9) . . ? C21B P1B Rh1B 121.81(9) . . ? C12B N1B C2B 110.8(3) . . ? C12B N1B Rh1B 113.79(18) . . ? C2B N1B Rh1B 111.5(2) . . ? O1B C1B Rh1B 176.5(3) . . ? C12B C11B C16B 119.8(3) . . ? C12B C11B P1B 115.3(2) . . ? C16B C11B P1B 124.8(2) . . ? C11B C12B C13B 120.3(3) . . ? C11B C12B N1B 118.5(3) . . ? C13B C12B N1B 121.2(3) . . ? C14B C13B C12B 119.0(4) . . ? C15B C14B C13B 120.9(4) . . ? C16B C15B C14B 120.2(4) . . ? C15B C16B C11B 119.8(4) . . ? C22B C21B C26B 119.4(3) . . ? C22B C21B P1B 123.0(2) . . ? C26B C21B P1B 117.5(2) . . ? C23B C22B C21B 119.9(3) . . ? C24B C23B C22B 120.3(3) . . ? C25B C24B C23B 119.8(3) . . ? C24B C25B C26B 120.6(3) . . ? C25B C26B C21B 120.0(3) . . ? C32B C31B C36B 118.6(3) . . ? C32B C31B P1B 123.2(2) . . ? C36B C31B P1B 118.2(2) . . ? C31B C32B C33B 120.6(3) . . ? C34B C33B C32B 120.2(3) . . ? C35B C34B C33B 119.8(3) . . ? C34B C35B C36B 120.6(3) . . ? C35B C36B C31B 120.3(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 C1A Rh1A P1A C11A -167.34(13) . . . . ? N1A Rh1A P1A C11A 15.16(10) . . . . ? Cl1A Rh1A P1A C11A 7.39(18) . . . . ? C1A Rh1A P1A C31A 77.21(13) . . . . ? N1A Rh1A P1A C31A -100.30(11) . . . . ? Cl1A Rh1A P1A C31A -108.07(17) . . . . ? C1A Rh1A P1A C21A -47.94(13) . . . . ? N1A Rh1A P1A C21A 134.56(11) . . . . ? Cl1A Rh1A P1A C21A 126.79(17) . . . . ? C1A Rh1A N1A C12A -46.7(12) . . . . ? P1A Rh1A N1A C12A -18.59(16) . . . . ? Cl1A Rh1A N1A C12A 160.08(17) . . . . ? C1A Rh1A N1A C2A 78.9(12) . . . . ? P1A Rh1A N1A C2A 107.03(18) . . . . ? Cl1A Rh1A N1A C2A -74.31(18) . . . . ? N1A Rh1A C1A O1A -4(6) . . . . ? P1A Rh1A C1A O1A -32(5) . . . . ? Cl1A Rh1A C1A O1A 149(5) . . . . ? C31A P1A C11A C12A 110.0(2) . . . . ? C21A P1A C11A C12A -141.5(2) . . . . ? Rh1A P1A C11A C12A -12.6(2) . . . . ? C31A P1A C11A C16A -70.5(3) . . . . ? C21A P1A C11A C16A 37.9(3) . . . . ? Rh1A P1A C11A C16A 166.8(2) . . . . ? C16A C11A C12A C13A 0.7(4) . . . . ? P1A C11A C12A C13A -179.8(2) . . . . ? C16A C11A C12A N1A 179.6(2) . . . . ? P1A C11A C12A N1A -0.9(3) . . . . ? C2A N1A C12A C11A -109.7(3) . . . . ? Rh1A N1A C12A C11A 15.6(3) . . . . ? C2A N1A C12A C13A 69.2(3) . . . . ? Rh1A N1A C12A C13A -165.5(2) . . . . ? C11A C12A C13A C14A -1.0(5) . . . . ? N1A C12A C13A C14A -179.9(3) . . . . ? C12A C13A C14A C15A 0.4(5) . . . . ? C13A C14A C15A C16A 0.5(6) . . . . ? C14A C15A C16A C11A -0.8(5) . . . . ? C12A C11A C16A C15A 0.2(4) . . . . ? P1A C11A C16A C15A -179.2(2) . . . . ? C11A P1A C21A C26A 108.1(2) . . . . ? C31A P1A C21A C26A -140.9(2) . . . . ? Rh1A P1A C21A C26A -9.5(2) . . . . ? C11A P1A C21A C22A -71.8(2) . . . . ? C31A P1A C21A C22A 39.2(2) . . . . ? Rh1A P1A C21A C22A 170.53(18) . . . . ? C26A C21A C22A C23A -0.8(4) . . . . ? P1A C21A C22A C23A 179.2(2) . . . . ? C21A C22A C23A C24A 1.5(4) . . . . ? C22A C23A C24A C25A -0.7(5) . . . . ? C23A C24A C25A C26A -0.9(5) . . . . ? C24A C25A C26A C21A 1.6(4) . . . . ? C22A C21A C26A C25A -0.8(4) . . . . ? P1A C21A C26A C25A 179.3(2) . . . . ? C11A P1A C31A C36A -13.5(2) . . . . ? C21A P1A C31A C36A -125.2(2) . . . . ? Rh1A P1A C31A C36A 100.5(2) . . . . ? C11A P1A C31A C32A 167.88(19) . . . . ? C21A P1A C31A C32A 56.2(2) . . . . ? Rh1A P1A C31A C32A -78.1(2) . . . . ? C36A C31A C32A C33A 1.7(4) . . . . ? P1A C31A C32A C33A -179.6(2) . . . . ? C31A C32A C33A C34A -1.7(4) . . . . ? C32A C33A C34A C35A 0.4(4) . . . . ? C33A C34A C35A C36A 0.7(4) . . . . ? C32A C31A C36A C35A -0.5(4) . . . . ? P1A C31A C36A C35A -179.1(2) . . . . ? C34A C35A C36A C31A -0.7(4) . . . . ? C1B Rh1B P1B C11B -155.30(14) . . . . ? N1B Rh1B P1B C11B 18.72(12) . . . . ? Cl1B Rh1B P1B C11B 45.9(2) . . . . ? C1B Rh1B P1B C31B 89.60(15) . . . . ? N1B Rh1B P1B C31B -96.37(12) . . . . ? Cl1B Rh1B P1B C31B -69.2(2) . . . . ? C1B Rh1B P1B C21B -38.63(15) . . . . ? N1B Rh1B P1B C21B 135.40(13) . . . . ? Cl1B Rh1B P1B C21B 162.58(19) . . . . ? C1B Rh1B N1B C12B 31.5(11) . . . . ? P1B Rh1B N1B C12B -24.18(19) . . . . ? Cl1B Rh1B N1B C12B 159.7(2) . . . . ? C1B Rh1B N1B C2B 157.7(10) . . . . ? P1B Rh1B N1B C2B 102.1(2) . . . . ? Cl1B Rh1B N1B C2B -74.0(2) . . . . ? N1B Rh1B C1B O1B 14(6) . . . . ? P1B Rh1B C1B O1B 69(6) . . . . ? Cl1B Rh1B C1B O1B -114(6) . . . . ? C31B P1B C11B C12B 107.4(2) . . . . ? C21B P1B C11B C12B -142.3(2) . . . . ? Rh1B P1B C11B C12B -14.1(2) . . . . ? C31B P1B C11B C16B -76.9(3) . . . . ? C21B P1B C11B C16B 33.3(3) . . . . ? Rh1B P1B C11B C16B 161.5(2) . . . . ? C16B C11B C12B C13B -1.0(5) . . . . ? P1B C11B C12B C13B 174.8(3) . . . . ? C16B C11B C12B N1B -180.0(3) . . . . ? P1B C11B C12B N1B -4.1(4) . . . . ? C2B N1B C12B C11B -104.6(3) . . . . ? Rh1B N1B C12B C11B 22.0(4) . . . . ? C2B N1B C12B C13B 76.4(4) . . . . ? Rh1B N1B C12B C13B -157.0(3) . . . . ? C11B C12B C13B C14B 0.5(6) . . . . ? N1B C12B C13B C14B 179.5(4) . . . . ? C12B C13B C14B C15B 1.0(7) . . . . ? C13B C14B C15B C16B -2.0(8) . . . . ? C14B C15B C16B C11B 1.5(6) . . . . ? C12B C11B C16B C15B 0.0(5) . . . . ? P1B C11B C16B C15B -175.4(3) . . . . ? C11B P1B C21B C22B -92.8(3) . . . . ? C31B P1B C21B C22B 18.7(3) . . . . ? Rh1B P1B C21B C22B 151.6(2) . . . . ? C11B P1B C21B C26B 84.5(2) . . . . ? C31B P1B C21B C26B -163.9(2) . . . . ? Rh1B P1B C21B C26B -31.1(3) . . . . ? C26B C21B C22B C23B -0.7(5) . . . . ? P1B C21B C22B C23B 176.6(3) . . . . ? C21B C22B C23B C24B -0.2(6) . . . . ? C22B C23B C24B C25B 0.6(6) . . . . ? C23B C24B C25B C26B 0.0(5) . . . . ? C24B C25B C26B C21B -0.9(5) . . . . ? C22B C21B C26B C25B 1.2(4) . . . . ? P1B C21B C26B C25B -176.2(2) . . . . ? C11B P1B C31B C32B 11.1(3) . . . . ? C21B P1B C31B C32B -99.4(2) . . . . ? Rh1B P1B C31B C32B 124.1(2) . . . . ? C11B P1B C31B C36B -168.3(2) . . . . ? C21B P1B C31B C36B 81.2(3) . . . . ? Rh1B P1B C31B C36B -55.3(3) . . . . ? C36B C31B C32B C33B -0.1(4) . . . . ? P1B C31B C32B C33B -179.5(2) . . . . ? C31B C32B C33B C34B -0.1(5) . . . . ? C32B C33B C34B C35B -0.4(5) . . . . ? C33B C34B C35B C36B 1.0(6) . . . . ? C34B C35B C36B C31B -1.3(6) . . . . ? C32B C31B C36B C35B 0.8(5) . . . . ? P1B C31B C36B C35B -179.8(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1NA Cl1B 0.93 2.36 3.284(2) 169.9 2 N1B H1NB Cl1A 0.93 2.37 3.299(3) 173.7 2_545 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.879 _refine_diff_density_min -0.449 _refine_diff_density_rms 0.072 data_compound(6) _database_code_depnum_ccdc_archive 'CCDC 713708' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H21 Cl N2 O P Rh, 0.5(C H2 Cl2)' _chemical_formula_sum 'C21.5 H22 Cl2 N2 O P Rh' _chemical_formula_weight 529.19 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' N N 0.0061 0.0033 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.768(2) _cell_length_b 13.306(2) _cell_length_c 14.389(2) _cell_angle_alpha 84.988(2) _cell_angle_beta 76.837(2) _cell_angle_gamma 74.965(2) _cell_volume 2297.7(6) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 4201 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 25.54 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1068 _exptl_absorpt_coefficient_mu 1.060 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6193 _exptl_absorpt_correction_T_max 0.8404 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2002)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 17407 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0524 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.59 _diffrn_reflns_theta_max 27.59 _reflns_number_total 17407 _reflns_number_gt 12537 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'DIRDIF-96 (Beurskens et al., 1996)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0467P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17407 _refine_ls_number_parameters 519 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0626 _refine_ls_R_factor_gt 0.0400 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0885 _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_restrained_S_all 0.971 _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 RhA Rh 0.194955(18) 0.034320(17) 0.190101(15) 0.02706(6) Uani 1 1 d . . . ClA Cl 0.38489(6) -0.03126(6) 0.19755(5) 0.03407(17) Uani 1 1 d . . . P0A P 0.01334(6) 0.09672(6) 0.20682(5) 0.02737(16) Uani 1 1 d . . . O0A O 0.2430(2) -0.0019(2) -0.01723(16) 0.0646(8) Uani 1 1 d . . . N1A N 0.15913(19) 0.05794(17) 0.33980(16) 0.0295(5) Uani 1 1 d . . . H1NA H 0.2183 0.0784 0.3533 0.035 Uiso 1 1 calc R . . N2A N 0.1020(2) 0.2790(2) 0.10411(18) 0.0415(6) Uani 1 1 d . . . H2NA H 0.1247 0.2406 0.1521 0.050 Uiso 1 1 calc R . . C1A C 0.2228(2) 0.0131(2) 0.0623(2) 0.0374(7) Uani 1 1 d . . . C11A C -0.0235(2) 0.1617(2) 0.32033(19) 0.0276(6) Uani 1 1 d . . . C12A C 0.0585(2) 0.1385(2) 0.37382(19) 0.0295(6) Uani 1 1 d . . . C13A C 0.0430(3) 0.1880(2) 0.4587(2) 0.0368(7) Uani 1 1 d . . . H13A H 0.0995 0.1723 0.4945 0.044 Uiso 1 1 calc R . . C14A C -0.0557(3) 0.2604(3) 0.4906(2) 0.0431(8) Uani 1 1 d . . . H14A H -0.0668 0.2952 0.5482 0.052 Uiso 1 1 calc R . . C15A C -0.1376(3) 0.2821(2) 0.4391(2) 0.0413(8) Uani 1 1 d . . . H15A H -0.2057 0.3308 0.4625 0.050 Uiso 1 1 calc R . . C16A C -0.1229(2) 0.2344(2) 0.3542(2) 0.0367(7) Uani 1 1 d . . . H16A H -0.1800 0.2509 0.3191 0.044 Uiso 1 1 calc R . . C17A C 0.1529(3) -0.0424(2) 0.3934(2) 0.0409(8) Uani 1 1 d . . . H17A H 0.1396 -0.0317 0.4621 0.049 Uiso 1 1 calc R . . H17B H 0.2231 -0.0945 0.3736 0.049 Uiso 1 1 calc R . . H17C H 0.0920 -0.0668 0.3798 0.049 Uiso 1 1 calc R . . C21A C -0.0472(2) 0.1924(2) 0.12335(19) 0.0295(6) Uani 1 1 d . . . C22A C 0.0055(2) 0.2728(2) 0.0826(2) 0.0338(7) Uani 1 1 d . . . C23A C -0.0457(3) 0.3457(2) 0.0203(2) 0.0411(8) Uani 1 1 d . . . H23A H -0.0137 0.4016 -0.0060 0.049 Uiso 1 1 calc R . . C24A C -0.1422(3) 0.3377(3) -0.0036(2) 0.0470(9) Uani 1 1 d . . . H24A H -0.1748 0.3878 -0.0466 0.056 Uiso 1 1 calc R . . C25A C -0.1913(3) 0.2590(3) 0.0337(2) 0.0450(8) Uani 1 1 d . . . H25A H -0.2568 0.2533 0.0160 0.054 Uiso 1 1 calc R . . C26A C -0.1436(2) 0.1873(2) 0.0979(2) 0.0364(7) Uani 1 1 d . . . H26A H -0.1784 0.1333 0.1251 0.044 Uiso 1 1 calc R . . C27A C 0.1686(3) 0.3467(3) 0.0510(3) 0.0578(10) Uani 1 1 d . . . H27A H 0.1800 0.3364 -0.0176 0.069 Uiso 1 1 calc R . . H27B H 0.2406 0.3300 0.0694 0.069 Uiso 1 1 calc R . . H27C H 0.1303 0.4194 0.0652 0.069 Uiso 1 1 calc R . . C31A C -0.0644(2) -0.0023(2) 0.2221(2) 0.0294(6) Uani 1 1 d . . . C32A C -0.1423(3) -0.0141(3) 0.3038(2) 0.0410(8) Uani 1 1 d . . . H32A H -0.1591 0.0324 0.3546 0.049 Uiso 1 1 calc R . . C33A C -0.1961(3) -0.0936(3) 0.3118(2) 0.0540(10) Uani 1 1 d . . . H33A H -0.2495 -0.1012 0.3682 0.065 Uiso 1 1 calc R . . C34A C -0.1728(3) -0.1613(3) 0.2390(3) 0.0514(9) Uani 1 1 d . . . H34A H -0.2098 -0.2157 0.2451 0.062 Uiso 1 1 calc R . . C35A C -0.0964(3) -0.1504(3) 0.1576(3) 0.0517(9) Uani 1 1 d . . . H35A H -0.0811 -0.1967 0.1069 0.062 Uiso 1 1 calc R . . C36A C -0.0412(3) -0.0715(2) 0.1489(2) 0.0396(8) Uani 1 1 d . . . H36A H 0.0127 -0.0650 0.0926 0.047 Uiso 1 1 calc R . . RhB Rh 0.362431(19) 0.265332(17) 0.360120(15) 0.02861(6) Uani 1 1 d . . . ClB Cl 0.34497(6) 0.10458(6) 0.44062(5) 0.03670(17) Uani 1 1 d . . . P0B P 0.40297(6) 0.39654(6) 0.26700(5) 0.02915(17) Uani 1 1 d . . . O0B O 0.2166(2) 0.4014(2) 0.51479(17) 0.0641(7) Uani 1 1 d . . . N1B N 0.45945(19) 0.17612(18) 0.23944(16) 0.0319(6) Uani 1 1 d . . . H1NB H 0.4254 0.1230 0.2364 0.038 Uiso 1 1 calc R . . N2B N 0.1534(2) 0.4433(2) 0.27010(19) 0.0417(7) Uani 1 1 d . . . H2NB H 0.2010 0.3821 0.2620 0.050 Uiso 1 1 calc R . . C1B C 0.2748(3) 0.3481(2) 0.4565(2) 0.0379(7) Uani 1 1 d . . . C11B C 0.4352(2) 0.3424(2) 0.14912(19) 0.0280(6) Uani 1 1 d . . . C12B C 0.4615(2) 0.2341(2) 0.1479(2) 0.0303(6) Uani 1 1 d . . . C13B C 0.4891(3) 0.1838(2) 0.0621(2) 0.0404(8) Uani 1 1 d . . . H13B H 0.5081 0.1099 0.0612 0.048 Uiso 1 1 calc R . . C14B C 0.4888(3) 0.2423(3) -0.0222(2) 0.0461(8) Uani 1 1 d . . . H14B H 0.5069 0.2081 -0.0811 0.055 Uiso 1 1 calc R . . C15B C 0.4628(3) 0.3489(3) -0.0221(2) 0.0423(8) Uani 1 1 d . . . H15B H 0.4633 0.3879 -0.0806 0.051 Uiso 1 1 calc R . . C16B C 0.4358(3) 0.3999(2) 0.0633(2) 0.0358(7) Uani 1 1 d . . . H16B H 0.4177 0.4738 0.0633 0.043 Uiso 1 1 calc R . . C17B C 0.5740(2) 0.1243(3) 0.2519(2) 0.0444(8) Uani 1 1 d . . . H17D H 0.6122 0.0774 0.1991 0.053 Uiso 1 1 calc R . . H17E H 0.5703 0.0843 0.3125 0.053 Uiso 1 1 calc R . . H17F H 0.6149 0.1772 0.2521 0.053 Uiso 1 1 calc R . . C21B C 0.3067(2) 0.5224(2) 0.26070(19) 0.0318(7) Uani 1 1 d . . . C22B C 0.1929(3) 0.5305(2) 0.2640(2) 0.0343(7) Uani 1 1 d . . . C23B C 0.1234(3) 0.6301(3) 0.2572(2) 0.0439(8) Uani 1 1 d . . . H23B H 0.0468 0.6374 0.2596 0.053 Uiso 1 1 calc R . . C24B C 0.1641(3) 0.7180(3) 0.2471(2) 0.0496(9) Uani 1 1 d . . . H24B H 0.1155 0.7847 0.2415 0.060 Uiso 1 1 calc R . . C25B C 0.2739(3) 0.7102(3) 0.2451(2) 0.0502(9) Uani 1 1 d . . . H25B H 0.3010 0.7710 0.2386 0.060 Uiso 1 1 calc R . . C26B C 0.3445(3) 0.6134(2) 0.2526(2) 0.0416(8) Uani 1 1 d . . . H26B H 0.4203 0.6083 0.2522 0.050 Uiso 1 1 calc R . . C27B C 0.0354(3) 0.4488(3) 0.2895(3) 0.0581(10) Uani 1 1 d . . . H27D H -0.0014 0.4861 0.3486 0.070 Uiso 1 1 calc R . . H27E H 0.0241 0.3782 0.2966 0.070 Uiso 1 1 calc R . . H27F H 0.0038 0.4859 0.2364 0.070 Uiso 1 1 calc R . . C31B C 0.5300(2) 0.4274(2) 0.2787(2) 0.0329(7) Uani 1 1 d . . . C32B C 0.6165(2) 0.4325(2) 0.2031(2) 0.0394(8) Uani 1 1 d . . . H32B H 0.6133 0.4156 0.1411 0.047 Uiso 1 1 calc R . . C33B C 0.7086(3) 0.4620(3) 0.2164(3) 0.0493(9) Uani 1 1 d . . . H33B H 0.7675 0.4658 0.1633 0.059 Uiso 1 1 calc R . . C34B C 0.7153(3) 0.4854(3) 0.3047(3) 0.0481(9) Uani 1 1 d . . . H34B H 0.7769 0.5086 0.3128 0.058 Uiso 1 1 calc R . . C35B C 0.6332(3) 0.4755(3) 0.3812(3) 0.0640(11) Uani 1 1 d . . . H35B H 0.6391 0.4890 0.4434 0.077 Uiso 1 1 calc R . . C36B C 0.5411(3) 0.4459(3) 0.3690(2) 0.0567(10) Uani 1 1 d . . . H36B H 0.4848 0.4381 0.4231 0.068 Uiso 1 1 calc R . . Cl1S Cl 0.43630(11) 0.25853(11) 0.66385(14) 0.1282(6) Uani 1 1 d . . . Cl2S Cl 0.61196(11) 0.19557(12) 0.49936(11) 0.1136(5) Uani 1 1 d . . . C1S C 0.5151(3) 0.1565(3) 0.5917(3) 0.0595(10) Uani 1 1 d . . . H1SA H 0.4654 0.1272 0.5643 0.071 Uiso 1 1 calc R . . H1SB H 0.5544 0.1010 0.6310 0.071 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 RhA 0.02566(12) 0.02803(13) 0.02708(12) -0.00098(9) -0.00588(9) -0.00566(9) ClA 0.0275(4) 0.0298(4) 0.0451(4) -0.0045(3) -0.0092(3) -0.0050(3) P0A 0.0267(4) 0.0300(4) 0.0253(4) -0.0012(3) -0.0066(3) -0.0056(3) O0A 0.0585(17) 0.098(2) 0.0335(14) -0.0184(14) -0.0083(12) -0.0079(15) N1A 0.0307(13) 0.0310(14) 0.0304(13) 0.0013(10) -0.0112(10) -0.0104(10) N2A 0.0437(16) 0.0396(16) 0.0450(16) 0.0115(12) -0.0144(13) -0.0169(13) C1A 0.0276(16) 0.045(2) 0.0378(18) -0.0066(14) -0.0067(14) -0.0045(14) C11A 0.0292(15) 0.0299(16) 0.0247(14) -0.0030(12) -0.0032(12) -0.0101(12) C12A 0.0345(16) 0.0265(16) 0.0285(15) 0.0017(12) -0.0038(13) -0.0127(12) C13A 0.0443(19) 0.0426(19) 0.0257(15) -0.0017(13) -0.0078(14) -0.0139(15) C14A 0.056(2) 0.044(2) 0.0307(17) -0.0085(14) -0.0031(15) -0.0179(17) C15A 0.0442(19) 0.0356(19) 0.0405(18) -0.0048(14) -0.0032(15) -0.0075(15) C16A 0.0347(17) 0.0356(18) 0.0388(17) -0.0038(14) -0.0059(14) -0.0080(14) C17A 0.049(2) 0.0363(19) 0.0357(17) 0.0050(14) -0.0122(15) -0.0077(15) C21A 0.0292(16) 0.0323(17) 0.0235(14) -0.0030(12) -0.0063(12) -0.0003(12) C22A 0.0374(17) 0.0333(17) 0.0283(15) -0.0037(13) -0.0055(13) -0.0050(14) C23A 0.051(2) 0.0315(18) 0.0356(18) 0.0010(14) -0.0058(15) -0.0044(15) C24A 0.055(2) 0.045(2) 0.0353(18) 0.0022(15) -0.0178(16) 0.0043(17) C25A 0.0388(19) 0.050(2) 0.046(2) -0.0064(16) -0.0190(16) 0.0006(16) C26A 0.0303(17) 0.0347(18) 0.0412(18) -0.0028(14) -0.0068(14) -0.0031(13) C27A 0.060(2) 0.055(2) 0.063(3) 0.0155(19) -0.017(2) -0.0261(19) C31A 0.0270(15) 0.0302(16) 0.0309(15) 0.0004(12) -0.0105(12) -0.0035(12) C32A 0.046(2) 0.050(2) 0.0310(17) -0.0025(14) -0.0070(14) -0.0197(16) C33A 0.056(2) 0.071(3) 0.043(2) 0.0040(18) -0.0034(17) -0.036(2) C34A 0.054(2) 0.045(2) 0.066(2) 0.0020(18) -0.019(2) -0.0261(17) C35A 0.053(2) 0.046(2) 0.059(2) -0.0175(18) -0.0115(19) -0.0144(17) C36A 0.0385(18) 0.0408(19) 0.0386(18) -0.0095(14) -0.0023(14) -0.0107(14) RhB 0.02985(13) 0.02919(13) 0.02706(12) -0.00017(9) -0.00256(9) -0.01103(10) ClB 0.0436(4) 0.0392(4) 0.0331(4) 0.0083(3) -0.0127(3) -0.0195(3) P0B 0.0317(4) 0.0272(4) 0.0287(4) -0.0036(3) -0.0010(3) -0.0115(3) O0B 0.0607(17) 0.0749(19) 0.0497(15) -0.0290(14) 0.0046(13) -0.0097(14) N1B 0.0327(14) 0.0246(13) 0.0370(14) 0.0000(10) -0.0032(11) -0.0083(10) N2B 0.0353(15) 0.0344(16) 0.0574(18) -0.0056(13) -0.0117(13) -0.0090(12) C1B 0.0390(18) 0.044(2) 0.0330(17) 0.0002(14) -0.0062(14) -0.0161(15) C11B 0.0287(15) 0.0286(16) 0.0265(14) -0.0031(12) 0.0009(12) -0.0120(12) C12B 0.0299(16) 0.0299(16) 0.0311(16) -0.0029(12) 0.0016(12) -0.0136(12) C13B 0.048(2) 0.0311(18) 0.0392(18) -0.0079(14) 0.0025(15) -0.0120(14) C14B 0.058(2) 0.048(2) 0.0326(18) -0.0098(15) 0.0031(15) -0.0204(17) C15B 0.057(2) 0.044(2) 0.0259(16) 0.0013(14) 0.0013(15) -0.0231(16) C16B 0.0438(19) 0.0319(17) 0.0335(17) 0.0024(13) -0.0040(14) -0.0170(14) C17B 0.0320(18) 0.046(2) 0.047(2) -0.0032(16) -0.0033(15) 0.0007(15) C21B 0.0416(18) 0.0263(16) 0.0267(15) -0.0024(12) -0.0026(13) -0.0106(13) C22B 0.0403(18) 0.0351(18) 0.0259(15) -0.0026(12) -0.0036(13) -0.0092(14) C23B 0.048(2) 0.044(2) 0.0383(18) -0.0055(15) -0.0145(15) -0.0034(16) C24B 0.072(3) 0.031(2) 0.0384(19) -0.0013(14) -0.0137(18) 0.0014(17) C25B 0.067(3) 0.0272(19) 0.048(2) -0.0014(15) 0.0030(18) -0.0107(17) C26B 0.048(2) 0.0316(18) 0.0407(18) -0.0072(14) 0.0078(15) -0.0145(15) C27B 0.044(2) 0.058(3) 0.075(3) -0.005(2) -0.011(2) -0.0177(18) C31B 0.0357(17) 0.0263(16) 0.0376(17) -0.0043(13) -0.0048(14) -0.0110(13) C32B 0.0324(17) 0.047(2) 0.0386(18) -0.0045(15) -0.0041(14) -0.0114(14) C33B 0.0328(18) 0.056(2) 0.058(2) -0.0065(18) -0.0008(16) -0.0145(16) C34B 0.0377(19) 0.046(2) 0.065(2) -0.0117(18) -0.0120(18) -0.0151(16) C35B 0.048(2) 0.095(3) 0.057(2) -0.033(2) -0.0059(19) -0.025(2) C36B 0.048(2) 0.086(3) 0.043(2) -0.0234(19) 0.0037(17) -0.032(2) Cl1S 0.0765(9) 0.0755(9) 0.2307(19) -0.0512(11) -0.0381(11) 0.0043(7) Cl2S 0.0878(10) 0.1407(13) 0.1272(12) 0.0740(10) -0.0455(9) -0.0601(9) C1S 0.063(3) 0.046(2) 0.080(3) 0.0153(19) -0.037(2) -0.0187(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 RhA C1A 1.825(3) . ? RhA N1A 2.131(2) . ? RhA P0A 2.2150(8) . ? RhA ClA 2.3786(8) . ? P0A C31A 1.816(3) . ? P0A C21A 1.818(3) . ? P0A C11A 1.823(3) . ? O0A C1A 1.137(3) . ? N1A C12A 1.460(3) . ? N1A C17A 1.494(4) . ? N2A C22A 1.361(4) . ? N2A C27A 1.449(4) . ? C11A C12A 1.393(4) . ? C11A C16A 1.395(4) . ? C12A C13A 1.388(4) . ? C13A C14A 1.381(4) . ? C14A C15A 1.373(4) . ? C15A C16A 1.378(4) . ? C21A C26A 1.381(4) . ? C21A C22A 1.423(4) . ? C22A C23A 1.399(4) . ? C23A C24A 1.383(5) . ? C24A C25A 1.367(5) . ? C25A C26A 1.392(4) . ? C31A C32A 1.383(4) . ? C31A C36A 1.390(4) . ? C32A C33A 1.386(4) . ? C33A C34A 1.372(5) . ? C34A C35A 1.366(5) . ? C35A C36A 1.391(4) . ? RhB C1B 1.819(3) . ? RhB N1B 2.139(2) . ? RhB P0B 2.2035(8) . ? RhB ClB 2.3797(8) . ? P0B C21B 1.811(3) . ? P0B C11B 1.819(3) . ? P0B C31B 1.820(3) . ? O0B C1B 1.142(4) . ? N1B C12B 1.466(3) . ? N1B C17B 1.490(4) . ? N2B C22B 1.368(4) . ? N2B C27B 1.452(4) . ? C11B C12B 1.393(4) . ? C11B C16B 1.394(4) . ? C12B C13B 1.386(4) . ? C13B C14B 1.384(4) . ? C14B C15B 1.370(4) . ? C15B C16B 1.385(4) . ? C21B C26B 1.402(4) . ? C21B C22B 1.419(4) . ? C22B C23B 1.400(4) . ? C23B C24B 1.382(5) . ? C24B C25B 1.372(5) . ? C25B C26B 1.379(4) . ? C31B C32B 1.374(4) . ? C31B C36B 1.387(4) . ? C32B C33B 1.389(4) . ? C33B C34B 1.360(4) . ? C34B C35B 1.360(5) . ? C35B C36B 1.384(5) . ? Cl1S C1S 1.730(4) . ? Cl2S C1S 1.740(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 C1A RhA N1A 178.69(12) . . ? C1A RhA P0A 95.71(9) . . ? N1A RhA P0A 83.28(6) . . ? C1A RhA ClA 92.87(9) . . ? N1A RhA ClA 88.13(6) . . ? P0A RhA ClA 171.38(3) . . ? C31A P0A C21A 104.76(13) . . ? C31A P0A C11A 106.50(13) . . ? C21A P0A C11A 105.66(13) . . ? C31A P0A RhA 114.32(9) . . ? C21A P0A RhA 122.44(10) . . ? C11A P0A RhA 101.84(9) . . ? C12A N1A C17A 110.1(2) . . ? C12A N1A RhA 114.31(17) . . ? C17A N1A RhA 109.87(17) . . ? C22A N2A C27A 122.4(3) . . ? O0A C1A RhA 178.1(3) . . ? C12A C11A C16A 118.9(3) . . ? C12A C11A P0A 115.5(2) . . ? C16A C11A P0A 125.5(2) . . ? C13A C12A C11A 120.9(3) . . ? C13A C12A N1A 121.1(3) . . ? C11A C12A N1A 118.0(2) . . ? C14A C13A C12A 119.3(3) . . ? C15A C14A C13A 120.1(3) . . ? C14A C15A C16A 121.2(3) . . ? C15A C16A C11A 119.5(3) . . ? C26A C21A C22A 119.3(3) . . ? C26A C21A P0A 120.6(2) . . ? C22A C21A P0A 120.0(2) . . ? N2A C22A C23A 121.1(3) . . ? N2A C22A C21A 121.1(3) . . ? C23A C22A C21A 117.8(3) . . ? C24A C23A C22A 121.1(3) . . ? C25A C24A C23A 121.1(3) . . ? C24A C25A C26A 118.8(3) . . ? C21A C26A C25A 121.9(3) . . ? C32A C31A C36A 118.8(3) . . ? C32A C31A P0A 123.3(2) . . ? C36A C31A P0A 117.9(2) . . ? C31A C32A C33A 120.3(3) . . ? C34A C33A C32A 120.5(3) . . ? C35A C34A C33A 120.0(3) . . ? C34A C35A C36A 120.1(3) . . ? C31A C36A C35A 120.4(3) . . ? C1B RhB N1B 175.66(12) . . ? C1B RhB P0B 94.07(10) . . ? N1B RhB P0B 82.83(7) . . ? C1B RhB ClB 96.06(10) . . ? N1B RhB ClB 87.16(7) . . ? P0B RhB ClB 169.63(3) . . ? C21B P0B C11B 106.32(13) . . ? C21B P0B C31B 104.16(14) . . ? C11B P0B C31B 105.02(13) . . ? C21B P0B RhB 124.00(10) . . ? C11B P0B RhB 101.78(9) . . ? C31B P0B RhB 113.89(10) . . ? C12B N1B C17B 111.1(2) . . ? C12B N1B RhB 114.13(16) . . ? C17B N1B RhB 112.22(18) . . ? C22B N2B C27B 122.0(3) . . ? O0B C1B RhB 177.2(3) . . ? C12B C11B C16B 119.4(3) . . ? C12B C11B P0B 115.1(2) . . ? C16B C11B P0B 125.5(2) . . ? C13B C12B C11B 120.4(3) . . ? C13B C12B N1B 121.7(3) . . ? C11B C12B N1B 118.0(2) . . ? C14B C13B C12B 119.3(3) . . ? C15B C14B C13B 121.0(3) . . ? C14B C15B C16B 120.1(3) . . ? C15B C16B C11B 119.8(3) . . ? C26B C21B C22B 119.2(3) . . ? C26B C21B P0B 119.9(2) . . ? C22B C21B P0B 120.9(2) . . ? N2B C22B C23B 121.2(3) . . ? N2B C22B C21B 120.9(3) . . ? C23B C22B C21B 117.9(3) . . ? C24B C23B C22B 121.3(3) . . ? C25B C24B C23B 120.8(3) . . ? C24B C25B C26B 119.6(3) . . ? C25B C26B C21B 121.2(3) . . ? C32B C31B C36B 118.0(3) . . ? C32B C31B P0B 123.6(2) . . ? C36B C31B P0B 118.4(2) . . ? C31B C32B C33B 120.5(3) . . ? C34B C33B C32B 120.6(3) . . ? C35B C34B C33B 119.7(3) . . ? C34B C35B C36B 120.2(3) . . ? C35B C36B C31B 120.8(3) . . ? Cl1S C1S Cl2S 112.1(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 C1A RhA P0A C31A 83.43(14) . . . . ? N1A RhA P0A C31A -95.73(12) . . . . ? ClA RhA P0A C31A -91.0(2) . . . . ? C1A RhA P0A C21A -44.78(16) . . . . ? N1A RhA P0A C21A 136.06(13) . . . . ? ClA RhA P0A C21A 140.8(2) . . . . ? C1A RhA P0A C11A -162.16(14) . . . . ? N1A RhA P0A C11A 18.67(11) . . . . ? ClA RhA P0A C11A 23.4(2) . . . . ? C1A RhA N1A C12A -65(5) . . . . ? P0A RhA N1A C12A -25.59(18) . . . . ? ClA RhA N1A C12A 155.11(18) . . . . ? C1A RhA N1A C17A 59(5) . . . . ? P0A RhA N1A C17A 98.71(18) . . . . ? ClA RhA N1A C17A -80.58(17) . . . . ? N1A RhA C1A O0A -126(9) . . . . ? P0A RhA C1A O0A -166(10) . . . . ? ClA RhA C1A O0A 14(10) . . . . ? C31A P0A C11A C12A 107.2(2) . . . . ? C21A P0A C11A C12A -141.7(2) . . . . ? RhA P0A C11A C12A -12.8(2) . . . . ? C31A P0A C11A C16A -75.8(3) . . . . ? C21A P0A C11A C16A 35.2(3) . . . . ? RhA P0A C11A C16A 164.1(2) . . . . ? C16A C11A C12A C13A -1.2(4) . . . . ? P0A C11A C12A C13A 176.0(2) . . . . ? C16A C11A C12A N1A 176.5(2) . . . . ? P0A C11A C12A N1A -6.3(3) . . . . ? C17A N1A C12A C13A 78.0(3) . . . . ? RhA N1A C12A C13A -157.8(2) . . . . ? C17A N1A C12A C11A -99.7(3) . . . . ? RhA N1A C12A C11A 24.5(3) . . . . ? C11A C12A C13A C14A 0.6(4) . . . . ? N1A C12A C13A C14A -177.0(3) . . . . ? C12A C13A C14A C15A 0.7(5) . . . . ? C13A C14A C15A C16A -1.4(5) . . . . ? C14A C15A C16A C11A 0.8(5) . . . . ? C12A C11A C16A C15A 0.5(4) . . . . ? P0A C11A C16A C15A -176.4(2) . . . . ? C31A P0A C21A C26A 9.7(3) . . . . ? C11A P0A C21A C26A -102.6(2) . . . . ? RhA P0A C21A C26A 141.9(2) . . . . ? C31A P0A C21A C22A -169.5(2) . . . . ? C11A P0A C21A C22A 78.2(2) . . . . ? RhA P0A C21A C22A -37.3(3) . . . . ? C27A N2A C22A C23A -12.6(5) . . . . ? C27A N2A C22A C21A 168.0(3) . . . . ? C26A C21A C22A N2A -178.5(3) . . . . ? P0A C21A C22A N2A 0.7(4) . . . . ? C26A C21A C22A C23A 2.1(4) . . . . ? P0A C21A C22A C23A -178.7(2) . . . . ? N2A C22A C23A C24A 178.3(3) . . . . ? C21A C22A C23A C24A -2.3(4) . . . . ? C22A C23A C24A C25A 0.7(5) . . . . ? C23A C24A C25A C26A 1.1(5) . . . . ? C22A C21A C26A C25A -0.3(4) . . . . ? P0A C21A C26A C25A -179.5(2) . . . . ? C24A C25A C26A C21A -1.4(5) . . . . ? C21A P0A C31A C32A -106.5(3) . . . . ? C11A P0A C31A C32A 5.2(3) . . . . ? RhA P0A C31A C32A 116.8(2) . . . . ? C21A P0A C31A C36A 75.7(3) . . . . ? C11A P0A C31A C36A -172.6(2) . . . . ? RhA P0A C31A C36A -61.0(3) . . . . ? C36A C31A C32A C33A -0.2(5) . . . . ? P0A C31A C32A C33A -177.9(3) . . . . ? C31A C32A C33A C34A -0.1(5) . . . . ? C32A C33A C34A C35A -0.3(6) . . . . ? C33A C34A C35A C36A 0.8(6) . . . . ? C32A C31A C36A C35A 0.7(5) . . . . ? P0A C31A C36A C35A 178.6(3) . . . . ? C34A C35A C36A C31A -1.0(5) . . . . ? C1B RhB P0B C21B -35.53(15) . . . . ? N1B RhB P0B C21B 141.41(13) . . . . ? ClB RhB P0B C21B 156.60(17) . . . . ? C1B RhB P0B C11B -154.66(13) . . . . ? N1B RhB P0B C11B 22.28(11) . . . . ? ClB RhB P0B C11B 37.47(19) . . . . ? C1B RhB P0B C31B 92.89(14) . . . . ? N1B RhB P0B C31B -90.16(12) . . . . ? ClB RhB P0B C31B -74.97(19) . . . . ? C1B RhB N1B C12B 18.3(17) . . . . ? P0B RhB N1B C12B -26.34(18) . . . . ? ClB RhB N1B C12B 156.36(19) . . . . ? C1B RhB N1B C17B 145.8(15) . . . . ? P0B RhB N1B C17B 101.23(19) . . . . ? ClB RhB N1B C17B -76.06(19) . . . . ? N1B RhB C1B O0B 29(7) . . . . ? P0B RhB C1B O0B 73(6) . . . . ? ClB RhB C1B O0B -109(6) . . . . ? C21B P0B C11B C12B -150.7(2) . . . . ? C31B P0B C11B C12B 99.3(2) . . . . ? RhB P0B C11B C12B -19.6(2) . . . . ? C21B P0B C11B C16B 29.7(3) . . . . ? C31B P0B C11B C16B -80.4(3) . . . . ? RhB P0B C11B C16B 160.7(2) . . . . ? C16B C11B C12B C13B 0.7(4) . . . . ? P0B C11B C12B C13B -179.0(2) . . . . ? C16B C11B C12B N1B -179.7(3) . . . . ? P0B C11B C12B N1B 0.6(3) . . . . ? C17B N1B C12B C13B 72.3(4) . . . . ? RhB N1B C12B C13B -159.6(2) . . . . ? C17B N1B C12B C11B -107.3(3) . . . . ? RhB N1B C12B C11B 20.8(3) . . . . ? C11B C12B C13B C14B -0.9(5) . . . . ? N1B C12B C13B C14B 179.5(3) . . . . ? C12B C13B C14B C15B 0.7(5) . . . . ? C13B C14B C15B C16B -0.3(5) . . . . ? C14B C15B C16B C11B 0.0(5) . . . . ? C12B C11B C16B C15B -0.2(4) . . . . ? P0B C11B C16B C15B 179.4(2) . . . . ? C11B P0B C21B C26B -102.2(2) . . . . ? C31B P0B C21B C26B 8.4(3) . . . . ? RhB P0B C21B C26B 140.8(2) . . . . ? C11B P0B C21B C22B 77.8(2) . . . . ? C31B P0B C21B C22B -171.5(2) . . . . ? RhB P0B C21B C22B -39.2(3) . . . . ? C27B N2B C22B C23B -12.8(5) . . . . ? C27B N2B C22B C21B 169.5(3) . . . . ? C26B C21B C22B N2B 178.8(3) . . . . ? P0B C21B C22B N2B -1.3(4) . . . . ? C26B C21B C22B C23B 1.1(4) . . . . ? P0B C21B C22B C23B -179.0(2) . . . . ? N2B C22B C23B C24B -177.3(3) . . . . ? C21B C22B C23B C24B 0.3(4) . . . . ? C22B C23B C24B C25B -1.1(5) . . . . ? C23B C24B C25B C26B 0.4(5) . . . . ? C24B C25B C26B C21B 1.0(5) . . . . ? C22B C21B C26B C25B -1.8(4) . . . . ? P0B C21B C26B C25B 178.3(2) . . . . ? C21B P0B C31B C32B -96.6(3) . . . . ? C11B P0B C31B C32B 15.0(3) . . . . ? RhB P0B C31B C32B 125.5(2) . . . . ? C21B P0B C31B C36B 84.2(3) . . . . ? C11B P0B C31B C36B -164.2(3) . . . . ? RhB P0B C31B C36B -53.8(3) . . . . ? C36B C31B C32B C33B -4.2(5) . . . . ? P0B C31B C32B C33B 176.5(2) . . . . ? C31B C32B C33B C34B 0.6(5) . . . . ? C32B C33B C34B C35B 2.9(5) . . . . ? C33B C34B C35B C36B -2.7(6) . . . . ? C34B C35B C36B C31B -1.0(6) . . . . ? C32B C31B C36B C35B 4.4(5) . . . . ? P0B C31B C36B C35B -176.3(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1A H1NA ClB 0.93 2.37 3.257(2) 159.7 . N1B H1NB ClA 0.93 2.38 3.286(3) 164.1 . _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 27.59 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.143 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.123 data_compound(7) _database_code_depnum_ccdc_archive 'CCDC 713709' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H24 Cl N3 O P Rh' _chemical_formula_sum 'C22 H24 Cl N3 O P Rh' _chemical_formula_weight 515.77 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' N N 0.0061 0.0033 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3726(8) _cell_length_b 11.3968(10) _cell_length_c 11.4388(10) _cell_angle_alpha 85.0063(12) _cell_angle_beta 77.9072(12) _cell_angle_gamma 72.8739(11) _cell_volume 1141.36(17) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5134 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 27.44 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.501 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 524 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.6848 _exptl_absorpt_correction_T_max 0.7898 _exptl_absorpt_process_details 'Bruker SHELXTL (Bruker, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10067 _diffrn_reflns_av_R_equivalents 0.0119 _diffrn_reflns_av_sigmaI/netI 0.0171 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5172 _reflns_number_gt 4964 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0327P)^2^+0.3460P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5172 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0576 _refine_ls_wR_factor_gt 0.0569 _refine_ls_goodness_of_fit_ref 1.104 _refine_ls_restrained_S_all 1.104 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.218969(12) 0.099411(9) 0.311255(9) 0.02336(5) Uani 1 1 d . . . Cl Cl 0.22942(5) -0.08655(4) 0.42549(4) 0.03919(10) Uani 1 1 d . . . P P 0.18144(4) 0.26610(3) 0.19276(3) 0.02262(8) Uani 1 1 d . . . O O 0.53144(16) 0.09286(15) 0.32820(18) 0.0625(4) Uani 1 1 d . . . N1 N -0.01518(14) 0.11800(12) 0.31343(12) 0.0280(3) Uani 1 1 d . . . H1N H -0.0581 0.1027 0.3921 0.034 Uiso 1 1 calc R . . N2 N 0.50875(17) 0.18390(15) 0.04350(14) 0.0425(3) Uani 1 1 d . . . H2N H 0.4834 0.2189 0.1133 0.051 Uiso 1 1 calc R . . N3 N 0.16847(18) 0.37321(14) 0.43168(12) 0.0371(3) Uani 1 1 d . . . H3N H 0.1291 0.3148 0.4206 0.044 Uiso 1 1 calc R . . C1 C 0.4121(2) 0.09443(15) 0.31940(17) 0.0363(4) Uani 1 1 d . . . C11 C -0.02507(17) 0.32143(13) 0.21866(13) 0.0253(3) Uani 1 1 d . . . C12 C -0.10300(17) 0.24147(14) 0.28091(13) 0.0270(3) Uani 1 1 d . . . C13 C -0.26087(19) 0.27761(17) 0.31050(17) 0.0375(4) Uani 1 1 d . . . H13 H -0.3137 0.2233 0.3544 0.045 Uiso 1 1 calc R . . C14 C -0.34075(19) 0.39375(18) 0.27538(18) 0.0415(4) Uani 1 1 d . . . H14 H -0.4488 0.4186 0.2946 0.050 Uiso 1 1 calc R . . C15 C -0.2641(2) 0.47418(16) 0.21226(16) 0.0364(4) Uani 1 1 d . . . H15 H -0.3196 0.5534 0.1882 0.044 Uiso 1 1 calc R . . C16 C -0.10687(19) 0.43856(14) 0.18455(14) 0.0310(3) Uani 1 1 d . . . H16 H -0.0543 0.4938 0.1422 0.037 Uiso 1 1 calc R . . C17 C -0.0349(2) 0.02350(17) 0.2406(2) 0.0446(4) Uani 1 1 d . . . H17A H 0.0248 -0.0581 0.2636 0.053 Uiso 1 1 calc R . . H17B H 0.0002 0.0402 0.1556 0.053 Uiso 1 1 calc R . . H17C H -0.1427 0.0264 0.2547 0.053 Uiso 1 1 calc R . . C21 C 0.24048(19) 0.23863(13) 0.03292(13) 0.0287(3) Uani 1 1 d . . . C22 C 0.3971(2) 0.19516(14) -0.02082(15) 0.0338(3) Uani 1 1 d . . . C23 C 0.4336(2) 0.16478(16) -0.14237(16) 0.0438(4) Uani 1 1 d . . . H23 H 0.5374 0.1350 -0.1801 0.053 Uiso 1 1 calc R . . C24 C 0.3219(3) 0.17738(17) -0.20731(16) 0.0492(5) Uani 1 1 d . . . H24 H 0.3499 0.1568 -0.2893 0.059 Uiso 1 1 calc R . . C25 C 0.1695(3) 0.21948(17) -0.15559(16) 0.0451(4) Uani 1 1 d . . . H25 H 0.0932 0.2277 -0.2013 0.054 Uiso 1 1 calc R . . C26 C 0.1300(2) 0.24951(15) -0.03564(14) 0.0346(3) Uani 1 1 d . . . H26 H 0.0255 0.2781 0.0005 0.041 Uiso 1 1 calc R . . C27 C 0.6671(2) 0.11668(19) 0.0016(2) 0.0517(5) Uani 1 1 d . . . H27A H 0.6733 0.0335 -0.0194 0.062 Uiso 1 1 calc R . . H27B H 0.7248 0.1120 0.0649 0.062 Uiso 1 1 calc R . . H27C H 0.7099 0.1593 -0.0691 0.062 Uiso 1 1 calc R . . C31 C 0.23699(17) 0.40036(13) 0.21693(13) 0.0255(3) Uani 1 1 d . . . C32 C 0.21933(17) 0.43943(14) 0.33494(14) 0.0291(3) Uani 1 1 d . . . C33 C 0.2489(2) 0.55127(16) 0.34831(17) 0.0385(4) Uani 1 1 d . . . H33 H 0.2352 0.5806 0.4263 0.046 Uiso 1 1 calc R . . C34 C 0.2974(2) 0.61896(16) 0.2504(2) 0.0446(4) Uani 1 1 d . . . H34 H 0.3153 0.6946 0.2619 0.054 Uiso 1 1 calc R . . C35 C 0.3204(2) 0.57835(16) 0.13609(19) 0.0441(4) Uani 1 1 d . . . H35 H 0.3575 0.6240 0.0692 0.053 Uiso 1 1 calc R . . C36 C 0.2889(2) 0.46997(15) 0.11961(15) 0.0343(3) Uani 1 1 d . . . H36 H 0.3029 0.4427 0.0408 0.041 Uiso 1 1 calc R . . C37 C 0.1775(3) 0.3966(2) 0.55215(17) 0.0532(5) Uani 1 1 d . . . H37A H 0.2830 0.3908 0.5555 0.064 Uiso 1 1 calc R . . H37B H 0.1432 0.3356 0.6079 0.064 Uiso 1 1 calc R . . H37C H 0.1125 0.4791 0.5745 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.02334(7) 0.02142(7) 0.02472(7) 0.00264(4) -0.00366(4) -0.00704(5) Cl 0.0374(2) 0.03023(19) 0.0415(2) 0.01369(16) -0.00094(17) -0.00554(16) P 0.02537(17) 0.02111(17) 0.02144(17) 0.00091(13) -0.00212(13) -0.00879(13) O 0.0357(7) 0.0580(9) 0.1022(13) -0.0021(9) -0.0260(8) -0.0170(7) N1 0.0267(6) 0.0257(6) 0.0322(7) 0.0050(5) -0.0046(5) -0.0109(5) N2 0.0345(8) 0.0450(8) 0.0407(8) -0.0046(7) 0.0047(6) -0.0073(6) N3 0.0487(8) 0.0382(7) 0.0238(6) -0.0028(5) -0.0059(6) -0.0117(6) C1 0.0332(8) 0.0281(8) 0.0480(10) 0.0004(7) -0.0093(7) -0.0083(6) C11 0.0265(7) 0.0260(7) 0.0236(7) 0.0005(5) -0.0048(5) -0.0082(5) C12 0.0267(7) 0.0264(7) 0.0285(7) 0.0025(6) -0.0074(6) -0.0082(6) C13 0.0282(8) 0.0393(9) 0.0462(10) 0.0071(7) -0.0077(7) -0.0133(7) C14 0.0261(8) 0.0443(10) 0.0506(10) 0.0027(8) -0.0098(7) -0.0042(7) C15 0.0371(8) 0.0301(8) 0.0394(9) 0.0012(7) -0.0144(7) -0.0015(6) C16 0.0362(8) 0.0267(7) 0.0298(7) 0.0032(6) -0.0078(6) -0.0085(6) C17 0.0423(10) 0.0329(9) 0.0658(13) -0.0049(8) -0.0194(9) -0.0146(7) C21 0.0401(8) 0.0220(6) 0.0231(7) 0.0000(5) -0.0011(6) -0.0108(6) C22 0.0436(9) 0.0221(7) 0.0308(8) -0.0002(6) 0.0041(7) -0.0098(6) C23 0.0600(12) 0.0277(8) 0.0326(9) -0.0036(7) 0.0114(8) -0.0089(8) C24 0.0850(15) 0.0331(9) 0.0246(8) -0.0044(7) -0.0005(9) -0.0150(9) C25 0.0757(14) 0.0363(9) 0.0282(8) 0.0003(7) -0.0151(9) -0.0200(9) C26 0.0503(10) 0.0279(7) 0.0275(8) 0.0011(6) -0.0082(7) -0.0142(7) C27 0.0371(10) 0.0384(10) 0.0649(13) 0.0092(9) 0.0083(9) -0.0041(8) C31 0.0260(7) 0.0223(6) 0.0279(7) -0.0011(5) -0.0026(5) -0.0080(5) C32 0.0256(7) 0.0287(7) 0.0314(8) -0.0044(6) -0.0057(6) -0.0042(6) C33 0.0356(8) 0.0345(8) 0.0462(10) -0.0152(7) -0.0075(7) -0.0077(7) C34 0.0411(9) 0.0277(8) 0.0670(13) -0.0098(8) -0.0057(9) -0.0137(7) C35 0.0481(10) 0.0280(8) 0.0548(11) 0.0019(7) 0.0029(8) -0.0184(7) C36 0.0410(9) 0.0273(7) 0.0336(8) 0.0003(6) -0.0006(7) -0.0134(6) C37 0.0620(13) 0.0636(13) 0.0276(9) -0.0070(8) -0.0122(8) -0.0041(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh C1 1.8160(17) . ? Rh N1 2.1368(13) . ? Rh P 2.2199(4) . ? Rh Cl 2.3787(4) . ? P C31 1.8143(15) . ? P C11 1.8180(15) . ? P C21 1.8223(15) . ? O C1 1.139(2) . ? N1 C12 1.4666(19) . ? N1 C17 1.492(2) . ? N2 C22 1.371(2) . ? N2 C27 1.455(2) . ? N3 C32 1.366(2) . ? N3 C37 1.450(2) . ? C11 C12 1.390(2) . ? C11 C16 1.398(2) . ? C12 C13 1.389(2) . ? C13 C14 1.387(2) . ? C14 C15 1.390(3) . ? C15 C16 1.382(2) . ? C21 C26 1.396(2) . ? C21 C22 1.423(2) . ? C22 C23 1.409(2) . ? C23 C24 1.374(3) . ? C24 C25 1.383(3) . ? C25 C26 1.390(2) . ? C31 C36 1.397(2) . ? C31 C32 1.420(2) . ? C32 C33 1.409(2) . ? C33 C34 1.378(3) . ? C34 C35 1.378(3) . ? C35 C36 1.388(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 Rh N1 174.80(6) . . ? C1 Rh P 95.00(6) . . ? N1 Rh P 84.05(4) . . ? C1 Rh Cl 93.16(5) . . ? N1 Rh Cl 88.16(4) . . ? P Rh Cl 171.011(16) . . ? C31 P C11 103.35(7) . . ? C31 P C21 106.04(7) . . ? C11 P C21 105.07(7) . . ? C31 P Rh 122.75(5) . . ? C11 P Rh 101.89(5) . . ? C21 P Rh 115.52(5) . . ? C12 N1 C17 110.83(13) . . ? C12 N1 Rh 114.46(9) . . ? C17 N1 Rh 112.21(10) . . ? C22 N2 C27 122.99(17) . . ? C32 N3 C37 121.80(17) . . ? O C1 Rh 177.73(19) . . ? C12 C11 C16 119.50(14) . . ? C12 C11 P 116.19(11) . . ? C16 C11 P 124.26(12) . . ? C13 C12 C11 120.54(14) . . ? C13 C12 N1 120.82(14) . . ? C11 C12 N1 118.63(13) . . ? C14 C13 C12 119.40(16) . . ? C13 C14 C15 120.58(16) . . ? C16 C15 C14 119.86(15) . . ? C15 C16 C11 120.12(15) . . ? C26 C21 C22 119.38(15) . . ? C26 C21 P 119.30(12) . . ? C22 C21 P 121.04(13) . . ? N2 C22 C23 121.15(17) . . ? N2 C22 C21 121.03(15) . . ? C23 C22 C21 117.81(17) . . ? C24 C23 C22 121.22(18) . . ? C23 C24 C25 121.24(17) . . ? C24 C25 C26 118.83(19) . . ? C25 C26 C21 121.50(18) . . ? C36 C31 C32 119.56(14) . . ? C36 C31 P 120.27(12) . . ? C32 C31 P 120.06(11) . . ? N3 C32 C33 121.43(15) . . ? N3 C32 C31 120.75(14) . . ? C33 C32 C31 117.75(15) . . ? C34 C33 C32 121.25(16) . . ? C35 C34 C33 120.88(16) . . ? C34 C35 C36 119.32(17) . . ? C35 C36 C31 121.15(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh P C31 -44.49(8) . . . . ? N1 Rh P C31 130.38(7) . . . . ? Cl Rh P C31 160.42(10) . . . . ? C1 Rh P C11 -159.07(8) . . . . ? N1 Rh P C11 15.80(6) . . . . ? Cl Rh P C11 45.84(11) . . . . ? C1 Rh P C21 87.67(8) . . . . ? N1 Rh P C21 -97.47(7) . . . . ? Cl Rh P C21 -67.42(11) . . . . ? C1 Rh N1 C12 58.9(7) . . . . ? P Rh N1 C12 -20.84(10) . . . . ? Cl Rh N1 C12 163.64(10) . . . . ? C1 Rh N1 C17 -173.7(7) . . . . ? P Rh N1 C17 106.57(11) . . . . ? Cl Rh N1 C17 -68.94(11) . . . . ? N1 Rh C1 O 24(5) . . . . ? P Rh C1 O 103(4) . . . . ? Cl Rh C1 O -81(4) . . . . ? C31 P C11 C12 -139.78(12) . . . . ? C21 P C11 C12 109.24(12) . . . . ? Rh P C11 C12 -11.61(12) . . . . ? C31 P C11 C16 37.53(15) . . . . ? C21 P C11 C16 -73.45(14) . . . . ? Rh P C11 C16 165.71(12) . . . . ? C16 C11 C12 C13 -0.8(2) . . . . ? P C11 C12 C13 176.69(13) . . . . ? C16 C11 C12 N1 178.60(14) . . . . ? P C11 C12 N1 -3.95(19) . . . . ? C17 N1 C12 C13 70.5(2) . . . . ? Rh N1 C12 C13 -161.39(13) . . . . ? C17 N1 C12 C11 -108.87(16) . . . . ? Rh N1 C12 C11 19.26(17) . . . . ? C11 C12 C13 C14 1.2(3) . . . . ? N1 C12 C13 C14 -178.12(16) . . . . ? C12 C13 C14 C15 -0.7(3) . . . . ? C13 C14 C15 C16 -0.3(3) . . . . ? C14 C15 C16 C11 0.7(3) . . . . ? C12 C11 C16 C15 -0.2(2) . . . . ? P C11 C16 C15 -177.46(13) . . . . ? C31 P C21 C26 -115.61(12) . . . . ? C11 P C21 C26 -6.57(14) . . . . ? Rh P C21 C26 104.84(12) . . . . ? C31 P C21 C22 70.38(13) . . . . ? C11 P C21 C22 179.42(12) . . . . ? Rh P C21 C22 -69.17(13) . . . . ? C27 N2 C22 C23 -13.7(3) . . . . ? C27 N2 C22 C21 166.65(16) . . . . ? C26 C21 C22 N2 179.64(15) . . . . ? P C21 C22 N2 -6.4(2) . . . . ? C26 C21 C22 C23 0.0(2) . . . . ? P C21 C22 C23 174.00(12) . . . . ? N2 C22 C23 C24 -179.22(17) . . . . ? C21 C22 C23 C24 0.4(2) . . . . ? C22 C23 C24 C25 -0.5(3) . . . . ? C23 C24 C25 C26 0.1(3) . . . . ? C24 C25 C26 C21 0.3(3) . . . . ? C22 C21 C26 C25 -0.4(2) . . . . ? P C21 C26 C25 -174.47(13) . . . . ? C11 P C31 C36 -100.71(13) . . . . ? C21 P C31 C36 9.56(15) . . . . ? Rh P C31 C36 145.44(11) . . . . ? C11 P C31 C32 75.53(13) . . . . ? C21 P C31 C32 -174.20(12) . . . . ? Rh P C31 C32 -38.32(14) . . . . ? C37 N3 C32 C33 -15.4(2) . . . . ? C37 N3 C32 C31 167.65(16) . . . . ? C36 C31 C32 N3 179.86(15) . . . . ? P C31 C32 N3 3.6(2) . . . . ? C36 C31 C32 C33 2.8(2) . . . . ? P C31 C32 C33 -173.42(12) . . . . ? N3 C32 C33 C34 -178.75(16) . . . . ? C31 C32 C33 C34 -1.8(2) . . . . ? C32 C33 C34 C35 -0.9(3) . . . . ? C33 C34 C35 C36 2.3(3) . . . . ? C34 C35 C36 C31 -1.2(3) . . . . ? C32 C31 C36 C35 -1.4(2) . . . . ? P C31 C36 C35 174.82(14) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N Cl 0.93 2.38 3.2870(14) 164.7 2_556 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.484 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.090 data_compound(9) _database_code_depnum_ccdc_archive 'CCDC 713710' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H30 Cl N3 O P Rh' _chemical_formula_sum 'C25 H30 Cl N3 O P Rh' _chemical_formula_weight 557.85 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' N N 0.0061 0.0033 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.3735(9) _cell_length_b 15.9907(15) _cell_length_c 17.1786(16) _cell_angle_alpha 90.00 _cell_angle_beta 100.0340(10) _cell_angle_gamma 90.00 _cell_volume 2535.5(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5831 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 26.37 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 0.864 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7024 _exptl_absorpt_correction_T_max 0.9034 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18416 _diffrn_reflns_av_R_equivalents 0.0304 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 26.39 _reflns_number_total 5195 _reflns_number_gt 4574 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0349P)^2^+1.4201P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5195 _refine_ls_number_parameters 289 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0247 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0629 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 Rh Rh 0.423583(16) 0.344948(10) 0.101460(9) 0.02116(6) Uani 1 1 d . . . Cl Cl 0.45713(6) 0.48130(3) 0.15933(3) 0.03261(13) Uani 1 1 d . . . P P 0.41389(6) 0.21471(3) 0.05925(3) 0.02182(11) Uani 1 1 d . . . O1 O 0.11315(19) 0.35493(13) 0.11112(14) 0.0564(6) Uani 1 1 d . . . N1 N 0.64303(19) 0.34358(11) 0.07413(10) 0.0244(4) Uani 1 1 d . . . N2 N 0.22131(19) 0.17856(13) 0.18050(11) 0.0294(4) Uani 1 1 d . . . N3 N 0.2932(2) 0.29201(13) -0.09738(11) 0.0346(4) Uani 1 1 d . . . C1 C 0.2350(3) 0.34783(15) 0.11032(16) 0.0366(6) Uani 1 1 d . . . C11 C 0.5754(2) 0.20577(13) 0.01400(12) 0.0244(4) Uani 1 1 d . . . C12 C 0.6762(2) 0.26967(13) 0.02944(12) 0.0236(4) Uani 1 1 d . . . C13 C 0.8062(2) 0.26475(16) 0.00080(14) 0.0341(5) Uani 1 1 d . . . H13 H 0.8768 0.3076 0.0130 0.041 Uiso 1 1 calc R . . C14 C 0.8324(3) 0.19766(17) -0.04518(15) 0.0390(6) Uani 1 1 d . . . H14 H 0.9216 0.1943 -0.0642 0.047 Uiso 1 1 calc R . . C15 C 0.7303(3) 0.13549(16) -0.06377(15) 0.0370(5) Uani 1 1 d . . . H15 H 0.7476 0.0904 -0.0969 0.044 Uiso 1 1 calc R . . C16 C 0.6028(3) 0.13906(14) -0.03393(14) 0.0334(5) Uani 1 1 d . . . H16 H 0.5330 0.0958 -0.0461 0.040 Uiso 1 1 calc R . . C17 C 0.6519(4) 0.41878(16) 0.02367(19) 0.0560(8) Uani 1 1 d . . . H17A H 0.7483 0.4217 0.0091 0.067 Uiso 1 1 calc R . . H17B H 0.6348 0.4693 0.0531 0.067 Uiso 1 1 calc R . . H17C H 0.5783 0.4148 -0.0243 0.067 Uiso 1 1 calc R . . C18 C 0.7493(3) 0.3500(2) 0.14876(16) 0.0580(9) Uani 1 1 d . . . H18A H 0.8478 0.3491 0.1368 0.070 Uiso 1 1 calc R . . H18B H 0.7365 0.3026 0.1831 0.070 Uiso 1 1 calc R . . H18C H 0.7338 0.4024 0.1756 0.070 Uiso 1 1 calc R . . C21 C 0.4420(2) 0.13208(14) 0.13545(12) 0.0253(4) Uani 1 1 d . . . C22 C 0.3393(2) 0.11994(14) 0.18459(12) 0.0277(4) Uani 1 1 d . . . C23 C 0.3537(3) 0.05309(16) 0.23675(14) 0.0372(5) Uani 1 1 d . . . H23 H 0.2825 0.0442 0.2690 0.045 Uiso 1 1 calc R . . C24 C 0.4702(3) -0.00080(17) 0.24241(15) 0.0441(6) Uani 1 1 d . . . H24 H 0.4781 -0.0469 0.2778 0.053 Uiso 1 1 calc R . . C25 C 0.5751(3) 0.01247(17) 0.19653(15) 0.0433(6) Uani 1 1 d . . . H25 H 0.6570 -0.0234 0.2014 0.052 Uiso 1 1 calc R . . C26 C 0.5609(3) 0.07814(15) 0.14337(14) 0.0342(5) Uani 1 1 d . . . H26 H 0.6332 0.0867 0.1117 0.041 Uiso 1 1 calc R . . C27 C 0.0777(3) 0.13936(18) 0.16330(17) 0.0423(6) Uani 1 1 d . . . H27A H 0.0708 0.1048 0.1157 0.051 Uiso 1 1 calc R . . H27B H 0.0030 0.1829 0.1547 0.051 Uiso 1 1 calc R . . H27C H 0.0633 0.1042 0.2080 0.051 Uiso 1 1 calc R . . C28 C 0.2364(3) 0.22720(19) 0.25387(16) 0.0470(7) Uani 1 1 d . . . H28A H 0.3338 0.2515 0.2656 0.056 Uiso 1 1 calc R . . H28B H 0.2215 0.1905 0.2974 0.056 Uiso 1 1 calc R . . H28C H 0.1641 0.2721 0.2477 0.056 Uiso 1 1 calc R . . C31 C 0.2769(2) 0.16755(13) -0.01746(12) 0.0244(4) Uani 1 1 d . . . C32 C 0.2348(2) 0.21011(14) -0.08893(12) 0.0264(4) Uani 1 1 d . . . C33 C 0.1410(2) 0.17106(16) -0.15018(13) 0.0321(5) Uani 1 1 d . . . H33 H 0.1117 0.1999 -0.1987 0.038 Uiso 1 1 calc R . . C34 C 0.0901(2) 0.09133(16) -0.14148(14) 0.0350(5) Uani 1 1 d . . . H34 H 0.0263 0.0656 -0.1837 0.042 Uiso 1 1 calc R . . C35 C 0.1322(3) 0.04906(15) -0.07127(14) 0.0353(5) Uani 1 1 d . . . H35 H 0.0975 -0.0059 -0.0651 0.042 Uiso 1 1 calc R . . C36 C 0.2249(2) 0.08677(14) -0.00994(13) 0.0313(5) Uani 1 1 d . . . H36 H 0.2538 0.0572 0.0382 0.038 Uiso 1 1 calc R . . C37 C 0.3744(4) 0.2981(2) -0.16229(18) 0.0580(8) Uani 1 1 d . . . H37A H 0.4104 0.3553 -0.1653 0.070 Uiso 1 1 calc R . . H37B H 0.3109 0.2839 -0.2121 0.070 Uiso 1 1 calc R . . H37C H 0.4564 0.2592 -0.1531 0.070 Uiso 1 1 calc R . . C38 C 0.1830(4) 0.35649(18) -0.1029(2) 0.0601(9) Uani 1 1 d . . . H38A H 0.1293 0.3504 -0.0591 0.072 Uiso 1 1 calc R . . H38B H 0.1160 0.3510 -0.1533 0.072 Uiso 1 1 calc R . . H38C H 0.2291 0.4117 -0.1001 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.01987(9) 0.02021(10) 0.02316(10) -0.00304(6) 0.00309(6) -0.00111(6) Cl 0.0472(3) 0.0230(3) 0.0292(3) -0.0063(2) 0.0111(2) -0.0041(2) P 0.0207(2) 0.0206(3) 0.0248(3) -0.0029(2) 0.0056(2) -0.0028(2) O1 0.0236(9) 0.0597(13) 0.0876(16) -0.0151(11) 0.0140(10) 0.0029(8) N1 0.0234(9) 0.0264(9) 0.0235(9) -0.0024(7) 0.0044(7) -0.0060(7) N2 0.0238(9) 0.0327(10) 0.0332(10) -0.0030(8) 0.0092(8) -0.0050(8) N3 0.0420(11) 0.0296(10) 0.0313(10) 0.0027(8) 0.0037(8) -0.0075(9) C1 0.0318(13) 0.0319(13) 0.0460(14) -0.0110(10) 0.0064(11) 0.0000(10) C11 0.0245(10) 0.0240(10) 0.0257(10) 0.0010(8) 0.0070(8) 0.0014(8) C12 0.0231(10) 0.0261(11) 0.0216(9) 0.0023(8) 0.0042(8) 0.0018(8) C13 0.0250(11) 0.0397(13) 0.0387(12) -0.0001(10) 0.0086(9) -0.0021(10) C14 0.0330(12) 0.0453(15) 0.0437(14) 0.0044(11) 0.0205(11) 0.0083(11) C15 0.0460(14) 0.0305(12) 0.0387(13) -0.0013(10) 0.0193(11) 0.0088(11) C16 0.0414(13) 0.0254(12) 0.0364(12) -0.0032(9) 0.0152(10) -0.0003(10) C17 0.086(2) 0.0249(13) 0.072(2) 0.0038(13) 0.0539(18) -0.0035(14) C18 0.0246(12) 0.107(3) 0.0389(15) -0.0343(16) -0.0032(11) -0.0028(14) C21 0.0276(11) 0.0241(10) 0.0236(10) -0.0014(8) 0.0028(8) -0.0034(9) C22 0.0261(11) 0.0298(11) 0.0265(10) -0.0034(9) 0.0026(8) -0.0053(9) C23 0.0371(13) 0.0441(15) 0.0320(12) 0.0048(11) 0.0100(10) -0.0050(11) C24 0.0533(16) 0.0411(15) 0.0380(14) 0.0127(11) 0.0083(12) 0.0054(12) C25 0.0457(15) 0.0431(15) 0.0424(14) 0.0115(12) 0.0111(12) 0.0144(12) C26 0.0360(12) 0.0345(13) 0.0338(12) 0.0039(10) 0.0107(10) 0.0057(10) C27 0.0265(12) 0.0505(16) 0.0503(15) 0.0015(12) 0.0080(11) -0.0081(11) C28 0.0454(15) 0.0527(17) 0.0459(15) -0.0149(13) 0.0159(12) 0.0006(13) C31 0.0221(10) 0.0239(11) 0.0277(10) -0.0049(8) 0.0055(8) -0.0027(8) C32 0.0244(10) 0.0268(11) 0.0296(11) -0.0033(9) 0.0089(8) -0.0013(9) C33 0.0281(11) 0.0412(13) 0.0268(11) -0.0026(10) 0.0044(9) -0.0013(10) C34 0.0273(11) 0.0435(14) 0.0343(12) -0.0156(11) 0.0054(9) -0.0085(10) C35 0.0376(13) 0.0285(12) 0.0408(13) -0.0105(10) 0.0095(10) -0.0110(10) C36 0.0347(12) 0.0263(12) 0.0324(12) -0.0021(9) 0.0048(9) -0.0071(9) C37 0.073(2) 0.0554(19) 0.0489(16) 0.0042(14) 0.0206(15) -0.0300(16) C38 0.074(2) 0.0319(15) 0.069(2) 0.0017(14) -0.0002(17) 0.0041(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh C1 1.801(3) . ? Rh N1 2.1883(18) . ? Rh P 2.2019(6) . ? Rh Cl 2.3941(6) . ? P C11 1.824(2) . ? P C31 1.834(2) . ? P C21 1.846(2) . ? O1 C1 1.150(3) . ? N1 C12 1.472(3) . ? N1 C18 1.484(3) . ? N1 C17 1.493(3) . ? N2 C22 1.442(3) . ? N2 C28 1.467(3) . ? N2 C27 1.468(3) . ? N3 C32 1.437(3) . ? N3 C38 1.451(4) . ? N3 C37 1.459(3) . ? C11 C12 1.386(3) . ? C11 C16 1.398(3) . ? C12 C13 1.394(3) . ? C13 C14 1.379(4) . ? C14 C15 1.378(4) . ? C15 C16 1.382(3) . ? C21 C26 1.397(3) . ? C21 C22 1.400(3) . ? C22 C23 1.386(3) . ? C23 C24 1.382(4) . ? C24 C25 1.379(4) . ? C25 C26 1.383(3) . ? C31 C36 1.394(3) . ? C31 C32 1.399(3) . ? C32 C33 1.396(3) . ? C33 C34 1.378(3) . ? C34 C35 1.379(4) . ? C35 C36 1.382(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Rh N1 172.53(10) . . ? C1 Rh P 93.86(8) . . ? N1 Rh P 84.62(5) . . ? C1 Rh Cl 90.08(7) . . ? N1 Rh Cl 92.17(5) . . ? P Rh Cl 173.21(2) . . ? C11 P C31 101.00(10) . . ? C11 P C21 102.70(10) . . ? C31 P C21 102.16(10) . . ? C11 P Rh 102.99(7) . . ? C31 P Rh 127.51(7) . . ? C21 P Rh 116.80(7) . . ? C12 N1 C18 109.57(19) . . ? C12 N1 C17 107.80(17) . . ? C18 N1 C17 110.5(2) . . ? C12 N1 Rh 114.31(12) . . ? C18 N1 Rh 109.18(15) . . ? C17 N1 Rh 105.42(16) . . ? C22 N2 C28 110.15(19) . . ? C22 N2 C27 113.63(19) . . ? C28 N2 C27 110.3(2) . . ? C32 N3 C38 112.0(2) . . ? C32 N3 C37 113.4(2) . . ? C38 N3 C37 111.3(2) . . ? O1 C1 Rh 174.1(3) . . ? C12 C11 C16 119.1(2) . . ? C12 C11 P 116.71(16) . . ? C16 C11 P 124.17(17) . . ? C11 C12 C13 120.0(2) . . ? C11 C12 N1 119.55(18) . . ? C13 C12 N1 120.4(2) . . ? C14 C13 C12 120.0(2) . . ? C15 C14 C13 120.5(2) . . ? C14 C15 C16 119.7(2) . . ? C15 C16 C11 120.6(2) . . ? C26 C21 C22 118.5(2) . . ? C26 C21 P 121.56(17) . . ? C22 C21 P 119.92(17) . . ? C23 C22 C21 119.8(2) . . ? C23 C22 N2 121.4(2) . . ? C21 C22 N2 118.8(2) . . ? C24 C23 C22 120.9(2) . . ? C25 C24 C23 119.8(2) . . ? C24 C25 C26 119.8(2) . . ? C25 C26 C21 121.1(2) . . ? C36 C31 C32 118.83(19) . . ? C36 C31 P 121.75(17) . . ? C32 C31 P 119.06(16) . . ? C33 C32 C31 119.2(2) . . ? C33 C32 N3 122.2(2) . . ? C31 C32 N3 118.54(19) . . ? C34 C33 C32 121.1(2) . . ? C33 C34 C35 119.8(2) . . ? C34 C35 C36 119.9(2) . . ? C35 C36 C31 121.1(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 C1 Rh P C11 161.63(11) . . . . ? N1 Rh P C11 -11.03(8) . . . . ? Cl Rh P C11 -73.04(18) . . . . ? C1 Rh P C31 46.55(12) . . . . ? N1 Rh P C31 -126.11(10) . . . . ? Cl Rh P C31 171.88(17) . . . . ? C1 Rh P C21 -86.70(12) . . . . ? N1 Rh P C21 100.64(9) . . . . ? Cl Rh P C21 38.63(19) . . . . ? C1 Rh N1 C12 -68.2(7) . . . . ? P Rh N1 C12 10.39(13) . . . . ? Cl Rh N1 C12 -175.61(13) . . . . ? C1 Rh N1 C18 168.7(6) . . . . ? P Rh N1 C18 -112.73(18) . . . . ? Cl Rh N1 C18 61.27(18) . . . . ? C1 Rh N1 C17 50.0(7) . . . . ? P Rh N1 C17 128.60(16) . . . . ? Cl Rh N1 C17 -57.40(16) . . . . ? N1 Rh C1 O1 -39(3) . . . . ? P Rh C1 O1 -117(2) . . . . ? Cl Rh C1 O1 69(2) . . . . ? C31 P C11 C12 145.61(16) . . . . ? C21 P C11 C12 -109.10(17) . . . . ? Rh P C11 C12 12.66(17) . . . . ? C31 P C11 C16 -34.8(2) . . . . ? C21 P C11 C16 70.4(2) . . . . ? Rh P C11 C16 -167.80(18) . . . . ? C16 C11 C12 C13 -3.4(3) . . . . ? P C11 C12 C13 176.18(17) . . . . ? C16 C11 C12 N1 174.83(19) . . . . ? P C11 C12 N1 -5.6(3) . . . . ? C18 N1 C12 C11 117.9(2) . . . . ? C17 N1 C12 C11 -121.8(2) . . . . ? Rh N1 C12 C11 -5.0(2) . . . . ? C18 N1 C12 C13 -63.9(3) . . . . ? C17 N1 C12 C13 56.4(3) . . . . ? Rh N1 C12 C13 173.21(16) . . . . ? C11 C12 C13 C14 2.2(3) . . . . ? N1 C12 C13 C14 -176.0(2) . . . . ? C12 C13 C14 C15 0.6(4) . . . . ? C13 C14 C15 C16 -2.1(4) . . . . ? C14 C15 C16 C11 0.9(4) . . . . ? C12 C11 C16 C15 1.8(3) . . . . ? P C11 C16 C15 -177.71(18) . . . . ? C11 P C21 C26 -3.8(2) . . . . ? C31 P C21 C26 100.58(19) . . . . ? Rh P C21 C26 -115.65(18) . . . . ? C11 P C21 C22 179.10(17) . . . . ? C31 P C21 C22 -76.51(19) . . . . ? Rh P C21 C22 67.26(18) . . . . ? C26 C21 C22 C23 -3.1(3) . . . . ? P C21 C22 C23 174.08(17) . . . . ? C26 C21 C22 N2 175.9(2) . . . . ? P C21 C22 N2 -6.9(3) . . . . ? C28 N2 C22 C23 67.3(3) . . . . ? C27 N2 C22 C23 -57.1(3) . . . . ? C28 N2 C22 C21 -111.8(2) . . . . ? C27 N2 C22 C21 123.9(2) . . . . ? C21 C22 C23 C24 1.6(4) . . . . ? N2 C22 C23 C24 -177.4(2) . . . . ? C22 C23 C24 C25 1.0(4) . . . . ? C23 C24 C25 C26 -1.9(4) . . . . ? C24 C25 C26 C21 0.4(4) . . . . ? C22 C21 C26 C25 2.1(3) . . . . ? P C21 C26 C25 -175.0(2) . . . . ? C11 P C31 C36 103.56(19) . . . . ? C21 P C31 C36 -2.2(2) . . . . ? Rh P C31 C36 -140.47(16) . . . . ? C11 P C31 C32 -69.52(18) . . . . ? C21 P C31 C32 -175.24(17) . . . . ? Rh P C31 C32 46.4(2) . . . . ? C36 C31 C32 C33 0.7(3) . . . . ? P C31 C32 C33 174.00(17) . . . . ? C36 C31 C32 N3 -177.6(2) . . . . ? P C31 C32 N3 -4.3(3) . . . . ? C38 N3 C32 C33 69.2(3) . . . . ? C37 N3 C32 C33 -57.8(3) . . . . ? C38 N3 C32 C31 -112.6(2) . . . . ? C37 N3 C32 C31 120.4(2) . . . . ? C31 C32 C33 C34 -0.4(3) . . . . ? N3 C32 C33 C34 177.8(2) . . . . ? C32 C33 C34 C35 0.0(4) . . . . ? C33 C34 C35 C36 0.1(4) . . . . ? C34 C35 C36 C31 0.3(4) . . . . ? C32 C31 C36 C35 -0.7(3) . . . . ? P C31 C36 C35 -173.77(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.691 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.066 data_compound(10) _database_code_depnum_ccdc_archive 'CCDC 713711' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H34 Cl2 N4 O2 P2 Rh2 0.75(C H2 Cl2)' _chemical_formula_sum 'C31.75 H35.5 Cl3.5 N4 O2 P2 Rh2' _chemical_formula_weight 896.98 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' N N 0.0061 0.0033 '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 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.6270(8) _cell_length_b 18.1593(12) _cell_length_c 17.4024(12) _cell_angle_alpha 90.00 _cell_angle_beta 104.6430(11) _cell_angle_gamma 90.00 _cell_volume 3555.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 7195 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 25.53 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1798 _exptl_absorpt_coefficient_mu 1.317 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6704 _exptl_absorpt_correction_T_max 0.8907 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 25488 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_sigmaI/netI 0.0366 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.65 _diffrn_reflns_theta_max 26.40 _reflns_number_total 7269 _reflns_number_gt 5696 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0477P)^2^+0.2493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7269 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0504 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0824 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 0.35769(2) 0.134845(14) 0.104032(15) 0.02982(8) Uani 1 1 d . . . Rh2 Rh 0.18752(2) 0.065878(14) 0.223692(19) 0.04019(9) Uani 1 1 d . . . Cl1 Cl 0.27501(8) 0.05470(5) -0.00410(6) 0.0482(2) Uani 1 1 d . . . Cl2 Cl 0.20637(10) -0.05867(5) 0.18369(9) 0.0735(4) Uani 1 1 d . . . P1 P 0.42900(7) 0.19490(4) 0.21542(5) 0.02763(18) Uani 1 1 d . . . P2 P 0.17798(7) 0.18437(4) 0.24334(5) 0.02841(18) Uani 1 1 d . . . O1 O 0.2578(2) 0.26858(16) 0.01444(17) 0.0595(7) Uani 1 1 d . . . O2 O 0.3147(3) 0.0417(2) 0.3920(2) 0.0807(10) Uani 1 1 d . . . N1 N 0.4452(2) 0.04109(14) 0.16726(16) 0.0341(6) Uani 1 1 d . . . H1N H 0.3880 0.0045 0.1634 0.041 Uiso 1 1 calc R . . N2 N 0.6387(2) 0.19678(18) 0.14257(18) 0.0465(8) Uani 1 1 d . . . H2N H 0.5838 0.1626 0.1379 0.056 Uiso 1 1 calc R . . N3 N 0.0766(2) 0.08963(16) 0.10658(19) 0.0449(8) Uani 1 1 d . . . H3N H 0.1204 0.0754 0.0712 0.054 Uiso 1 1 calc R . . N4 N -0.0465(2) 0.12677(16) 0.2828(2) 0.0454(8) Uani 1 1 d . . . H4N H -0.0104 0.1086 0.2482 0.054 Uiso 1 1 calc R . . C1 C 0.2945(3) 0.2167(2) 0.0499(2) 0.0370(8) Uani 1 1 d . . . C2 C 0.2677(4) 0.0501(2) 0.3261(3) 0.0522(10) Uani 1 1 d . . . C10 C 0.3186(2) 0.23531(17) 0.26265(19) 0.0295(7) Uani 1 1 d . . . H10A H 0.3533 0.2375 0.3207 0.035 Uiso 1 1 calc R . . H10B H 0.3019 0.2865 0.2434 0.035 Uiso 1 1 calc R . . C11 C 0.5037(3) 0.12306(17) 0.28262(19) 0.0309(7) Uani 1 1 d . . . C12 C 0.5000(3) 0.05231(18) 0.2521(2) 0.0347(8) Uani 1 1 d . . . C13 C 0.5493(3) -0.0059(2) 0.3010(2) 0.0463(9) Uani 1 1 d . . . H13 H 0.5439 -0.0547 0.2808 0.056 Uiso 1 1 calc R . . C14 C 0.6067(3) 0.0082(2) 0.3796(2) 0.0529(10) Uani 1 1 d . . . H14 H 0.6410 -0.0315 0.4132 0.064 Uiso 1 1 calc R . . C15 C 0.6148(3) 0.0789(2) 0.4101(2) 0.0503(10) Uani 1 1 d . . . H15 H 0.6553 0.0879 0.4640 0.060 Uiso 1 1 calc R . . C16 C 0.5638(3) 0.1355(2) 0.3617(2) 0.0394(8) Uani 1 1 d . . . H16 H 0.5693 0.1842 0.3822 0.047 Uiso 1 1 calc R . . C17 C 0.5370(3) 0.0121(2) 0.1269(2) 0.0436(9) Uani 1 1 d . . . H17A H 0.4996 0.0037 0.0705 0.052 Uiso 1 1 calc R . . H17B H 0.5697 -0.0343 0.1519 0.052 Uiso 1 1 calc R . . H17C H 0.6011 0.0482 0.1323 0.052 Uiso 1 1 calc R . . C21 C 0.5416(3) 0.26603(18) 0.2275(2) 0.0337(7) Uani 1 1 d . . . C22 C 0.6357(3) 0.2563(2) 0.1896(2) 0.0420(8) Uani 1 1 d . . . C23 C 0.7271(4) 0.3086(3) 0.2053(3) 0.0671(13) Uani 1 1 d . . . H23 H 0.7911 0.3038 0.1809 0.080 Uiso 1 1 calc R . . C24 C 0.7258(4) 0.3668(3) 0.2555(3) 0.0856(17) Uani 1 1 d . . . H24 H 0.7893 0.4013 0.2654 0.103 Uiso 1 1 calc R . . C25 C 0.6351(4) 0.3763(3) 0.2917(3) 0.0748(15) Uani 1 1 d . . . H25 H 0.6354 0.4170 0.3261 0.090 Uiso 1 1 calc R . . C26 C 0.5432(3) 0.3260(2) 0.2772(2) 0.0516(10) Uani 1 1 d . . . H26 H 0.4798 0.3325 0.3019 0.062 Uiso 1 1 calc R . . C27 C 0.7306(3) 0.1883(3) 0.0998(3) 0.0664(13) Uani 1 1 d . . . H27A H 0.7166 0.1429 0.0685 0.080 Uiso 1 1 calc R . . H27B H 0.8086 0.1859 0.1379 0.080 Uiso 1 1 calc R . . H27C H 0.7284 0.2305 0.0644 0.080 Uiso 1 1 calc R . . C31 C 0.0900(3) 0.21794(19) 0.14828(19) 0.0336(7) Uani 1 1 d . . . C32 C 0.0475(3) 0.1666(2) 0.0899(2) 0.0377(8) Uani 1 1 d . . . C33 C -0.0254(3) 0.1900(3) 0.0166(2) 0.0533(11) Uani 1 1 d . . . H33 H -0.0565 0.1552 -0.0241 0.064 Uiso 1 1 calc R . . C34 C -0.0513(3) 0.2635(3) 0.0044(2) 0.0593(12) Uani 1 1 d . . . H34 H -0.1008 0.2788 -0.0451 0.071 Uiso 1 1 calc R . . C35 C -0.0081(3) 0.3151(2) 0.0612(2) 0.0526(10) Uani 1 1 d . . . H35 H -0.0268 0.3657 0.0509 0.063 Uiso 1 1 calc R . . C36 C 0.0638(3) 0.2931(2) 0.1346(2) 0.0388(8) Uani 1 1 d . . . H36 H 0.0946 0.3285 0.1748 0.047 Uiso 1 1 calc R . . C37 C -0.0324(3) 0.0417(2) 0.0883(3) 0.0631(13) Uani 1 1 d . . . H37A H -0.0090 -0.0098 0.0999 0.076 Uiso 1 1 calc R . . H37B H -0.0739 0.0466 0.0321 0.076 Uiso 1 1 calc R . . H37C H -0.0854 0.0570 0.1212 0.076 Uiso 1 1 calc R . . C41 C 0.1020(3) 0.22345(17) 0.31320(18) 0.0304(7) Uani 1 1 d . . . C42 C -0.0045(3) 0.19074(19) 0.3218(2) 0.0383(8) Uani 1 1 d . . . C43 C -0.0694(4) 0.2279(2) 0.3683(3) 0.0546(11) Uani 1 1 d . . . H43 H -0.1412 0.2071 0.3751 0.066 Uiso 1 1 calc R . . C44 C -0.0301(4) 0.2934(2) 0.4037(3) 0.0561(11) Uani 1 1 d . . . H44 H -0.0770 0.3186 0.4329 0.067 Uiso 1 1 calc R . . C45 C 0.0762(3) 0.3240(2) 0.3980(2) 0.0479(9) Uani 1 1 d . . . H45 H 0.1044 0.3684 0.4252 0.057 Uiso 1 1 calc R . . C46 C 0.1408(3) 0.28900(18) 0.3522(2) 0.0366(8) Uani 1 1 d . . . H46 H 0.2133 0.3102 0.3473 0.044 Uiso 1 1 calc R . . C47 C -0.1494(4) 0.0878(2) 0.2970(3) 0.0624(12) Uani 1 1 d . . . H47A H -0.1661 0.0442 0.2627 0.075 Uiso 1 1 calc R . . H47B H -0.2187 0.1205 0.2849 0.075 Uiso 1 1 calc R . . H47C H -0.1323 0.0726 0.3527 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02241(13) 0.03754(15) 0.02985(14) -0.00666(11) 0.00722(10) -0.00152(10) Rh2 0.03214(15) 0.02851(15) 0.0660(2) -0.00558(13) 0.02373(14) -0.00186(11) Cl1 0.0369(5) 0.0632(6) 0.0437(5) -0.0237(4) 0.0089(4) -0.0097(4) Cl2 0.0625(7) 0.0299(5) 0.1448(12) -0.0176(6) 0.0572(7) -0.0053(4) P1 0.0222(4) 0.0324(4) 0.0288(4) -0.0038(3) 0.0074(3) -0.0014(3) P2 0.0243(4) 0.0287(4) 0.0340(5) -0.0033(3) 0.0106(3) 0.0005(3) O1 0.0543(16) 0.0720(19) 0.0552(18) 0.0222(15) 0.0193(14) 0.0184(15) O2 0.062(2) 0.100(3) 0.083(3) 0.036(2) 0.0247(19) 0.0144(18) N1 0.0258(13) 0.0344(15) 0.0437(17) -0.0063(13) 0.0118(12) -0.0009(11) N2 0.0279(14) 0.068(2) 0.0472(19) -0.0119(16) 0.0169(13) -0.0082(14) N3 0.0326(15) 0.0513(18) 0.057(2) -0.0242(15) 0.0227(14) -0.0126(13) N4 0.0340(15) 0.0490(18) 0.061(2) -0.0052(15) 0.0266(15) -0.0090(13) C1 0.0267(16) 0.052(2) 0.0340(19) -0.0036(17) 0.0113(14) -0.0006(15) C2 0.045(2) 0.044(2) 0.074(3) 0.016(2) 0.029(2) 0.0084(17) C10 0.0248(15) 0.0311(16) 0.0331(17) -0.0039(13) 0.0080(13) -0.0008(12) C11 0.0196(14) 0.0406(18) 0.0327(18) 0.0012(14) 0.0071(13) 0.0026(12) C12 0.0241(16) 0.0418(19) 0.039(2) 0.0001(15) 0.0104(14) 0.0022(13) C13 0.0364(19) 0.041(2) 0.066(3) 0.0057(18) 0.0199(18) 0.0099(15) C14 0.042(2) 0.059(3) 0.056(3) 0.019(2) 0.0083(18) 0.0112(18) C15 0.039(2) 0.070(3) 0.037(2) 0.0057(19) 0.0023(16) 0.0085(19) C16 0.0320(17) 0.048(2) 0.038(2) -0.0033(16) 0.0085(15) 0.0027(15) C17 0.0367(18) 0.044(2) 0.053(2) -0.0107(18) 0.0171(17) 0.0085(16) C21 0.0283(16) 0.0368(17) 0.0349(18) -0.0053(15) 0.0059(14) -0.0068(13) C22 0.0281(17) 0.057(2) 0.040(2) -0.0049(17) 0.0081(15) -0.0095(15) C23 0.044(2) 0.087(3) 0.077(3) -0.021(3) 0.027(2) -0.030(2) C24 0.061(3) 0.105(4) 0.096(4) -0.039(3) 0.030(3) -0.055(3) C25 0.067(3) 0.073(3) 0.091(4) -0.039(3) 0.031(3) -0.035(2) C26 0.044(2) 0.053(2) 0.061(3) -0.015(2) 0.0187(19) -0.0143(18) C27 0.034(2) 0.111(4) 0.059(3) -0.013(3) 0.022(2) -0.006(2) C31 0.0238(15) 0.0457(19) 0.0328(18) -0.0035(15) 0.0101(13) -0.0002(14) C32 0.0251(16) 0.055(2) 0.0352(19) -0.0098(16) 0.0121(14) -0.0034(15) C33 0.036(2) 0.086(3) 0.039(2) -0.019(2) 0.0124(17) -0.011(2) C34 0.038(2) 0.103(4) 0.035(2) 0.005(2) 0.0064(17) 0.003(2) C35 0.047(2) 0.071(3) 0.044(2) 0.012(2) 0.0185(18) 0.014(2) C36 0.0399(19) 0.046(2) 0.0335(19) 0.0033(16) 0.0144(15) 0.0043(15) C37 0.043(2) 0.064(3) 0.089(3) -0.035(2) 0.028(2) -0.025(2) C41 0.0297(16) 0.0342(17) 0.0296(17) 0.0034(14) 0.0115(13) 0.0066(13) C42 0.0365(18) 0.0397(19) 0.044(2) 0.0091(16) 0.0204(16) 0.0063(15) C43 0.055(2) 0.053(2) 0.069(3) 0.008(2) 0.041(2) 0.0088(19) C44 0.071(3) 0.052(2) 0.059(3) -0.006(2) 0.041(2) 0.011(2) C45 0.063(2) 0.041(2) 0.046(2) -0.0039(17) 0.0243(19) 0.0075(18) C46 0.0407(18) 0.0333(18) 0.038(2) 0.0000(15) 0.0137(15) 0.0045(14) C47 0.044(2) 0.059(3) 0.095(4) -0.005(2) 0.038(2) -0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 1.813(4) . ? Rh1 N1 2.140(3) . ? Rh1 P1 2.1958(8) . ? Rh1 Cl1 2.3810(9) . ? Rh2 C2 1.813(5) . ? Rh2 N3 2.162(3) . ? Rh2 P2 2.1859(8) . ? Rh2 Cl2 2.3927(10) . ? P1 C21 1.814(3) . ? P1 C11 1.819(3) . ? P1 C10 1.842(3) . ? P2 C31 1.816(3) . ? P2 C41 1.818(3) . ? P2 C10 1.834(3) . ? O1 C1 1.147(4) . ? O2 C2 1.149(5) . ? N1 C12 1.467(4) . ? N1 C17 1.512(4) . ? N2 C22 1.362(5) . ? N2 C27 1.456(4) . ? N3 C32 1.449(5) . ? N3 C37 1.503(4) . ? N4 C42 1.372(4) . ? N4 C47 1.464(4) . ? C11 C12 1.387(5) . ? C11 C16 1.395(5) . ? C12 C13 1.386(5) . ? C13 C14 1.387(6) . ? C14 C15 1.383(6) . ? C15 C16 1.366(5) . ? C21 C26 1.388(5) . ? C21 C22 1.423(5) . ? C22 C23 1.400(5) . ? C23 C24 1.373(6) . ? C24 C25 1.369(6) . ? C25 C26 1.380(5) . ? C31 C32 1.376(5) . ? C31 C36 1.406(5) . ? C32 C33 1.407(5) . ? C33 C34 1.373(6) . ? C34 C35 1.362(6) . ? C35 C36 1.397(5) . ? C41 C46 1.388(5) . ? C41 C42 1.415(4) . ? C42 C43 1.410(5) . ? C43 C44 1.365(6) . ? C44 C45 1.382(5) . ? C45 C46 1.382(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 C1 Rh1 N1 175.65(12) . . ? C1 Rh1 P1 93.68(11) . . ? N1 Rh1 P1 85.23(8) . . ? C1 Rh1 Cl1 93.51(11) . . ? N1 Rh1 Cl1 87.97(8) . . ? P1 Rh1 Cl1 171.19(4) . . ? C2 Rh2 N3 173.77(14) . . ? C2 Rh2 P2 92.03(13) . . ? N3 Rh2 P2 84.79(8) . . ? C2 Rh2 Cl2 94.28(13) . . ? N3 Rh2 Cl2 89.49(9) . . ? P2 Rh2 Cl2 171.10(4) . . ? C21 P1 C11 102.88(14) . . ? C21 P1 C10 103.23(14) . . ? C11 P1 C10 105.80(15) . . ? C21 P1 Rh1 123.79(11) . . ? C11 P1 Rh1 102.93(11) . . ? C10 P1 Rh1 116.20(10) . . ? C31 P2 C41 102.79(14) . . ? C31 P2 C10 105.55(15) . . ? C41 P2 C10 103.99(14) . . ? C31 P2 Rh2 103.13(11) . . ? C41 P2 Rh2 122.78(11) . . ? C10 P2 Rh2 116.55(10) . . ? C12 N1 C17 109.7(2) . . ? C12 N1 Rh1 115.86(19) . . ? C17 N1 Rh1 109.7(2) . . ? C22 N2 C27 121.6(3) . . ? C32 N3 C37 112.0(3) . . ? C32 N3 Rh2 115.8(2) . . ? C37 N3 Rh2 110.7(3) . . ? C42 N4 C47 122.0(3) . . ? O1 C1 Rh1 177.6(3) . . ? O2 C2 Rh2 177.1(4) . . ? P2 C10 P1 113.99(16) . . ? C12 C11 C16 119.1(3) . . ? C12 C11 P1 117.1(2) . . ? C16 C11 P1 123.8(3) . . ? C13 C12 C11 120.3(3) . . ? C13 C12 N1 121.2(3) . . ? C11 C12 N1 118.5(3) . . ? C12 C13 C14 119.0(4) . . ? C15 C14 C13 121.3(4) . . ? C16 C15 C14 119.0(4) . . ? C15 C16 C11 121.2(3) . . ? C26 C21 C22 119.7(3) . . ? C26 C21 P1 121.7(3) . . ? C22 C21 P1 118.4(2) . . ? N2 C22 C23 121.5(3) . . ? N2 C22 C21 121.1(3) . . ? C23 C22 C21 117.4(3) . . ? C24 C23 C22 121.1(4) . . ? C25 C24 C23 121.6(4) . . ? C24 C25 C26 118.9(4) . . ? C25 C26 C21 121.4(4) . . ? C32 C31 C36 120.7(3) . . ? C32 C31 P2 117.4(3) . . ? C36 C31 P2 121.9(3) . . ? C31 C32 C33 119.1(4) . . ? C31 C32 N3 118.9(3) . . ? C33 C32 N3 122.0(3) . . ? C34 C33 C32 119.5(4) . . ? C35 C34 C33 122.1(4) . . ? C34 C35 C36 119.4(4) . . ? C35 C36 C31 119.1(3) . . ? C46 C41 C42 119.5(3) . . ? C46 C41 P2 120.6(2) . . ? C42 C41 P2 119.5(2) . . ? N4 C42 C43 120.9(3) . . ? N4 C42 C41 121.0(3) . . ? C43 C42 C41 118.0(3) . . ? C44 C43 C42 120.6(3) . . ? C43 C44 C45 121.5(3) . . ? C46 C45 C44 118.9(4) . . ? C45 C46 C41 121.4(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 C21 -63.20(16) . . . . ? N1 Rh1 P1 C21 112.58(15) . . . . ? Cl1 Rh1 P1 C21 152.2(2) . . . . ? C1 Rh1 P1 C11 -178.58(14) . . . . ? N1 Rh1 P1 C11 -2.81(12) . . . . ? Cl1 Rh1 P1 C11 36.8(2) . . . . ? C1 Rh1 P1 C10 66.32(15) . . . . ? N1 Rh1 P1 C10 -117.91(14) . . . . ? Cl1 Rh1 P1 C10 -78.3(2) . . . . ? C2 Rh2 P2 C31 -176.53(15) . . . . ? N3 Rh2 P2 C31 -1.90(12) . . . . ? Cl2 Rh2 P2 C31 48.3(3) . . . . ? C2 Rh2 P2 C41 -61.66(17) . . . . ? N3 Rh2 P2 C41 112.97(14) . . . . ? Cl2 Rh2 P2 C41 163.2(3) . . . . ? C2 Rh2 P2 C10 68.37(17) . . . . ? N3 Rh2 P2 C10 -117.00(14) . . . . ? Cl2 Rh2 P2 C10 -66.8(3) . . . . ? C1 Rh1 N1 C12 81.4(17) . . . . ? P1 Rh1 N1 C12 5.73(19) . . . . ? Cl1 Rh1 N1 C12 -168.7(2) . . . . ? C1 Rh1 N1 C17 -43.5(17) . . . . ? P1 Rh1 N1 C17 -119.2(2) . . . . ? Cl1 Rh1 N1 C17 66.4(2) . . . . ? C2 Rh2 N3 C32 61.3(14) . . . . ? P2 Rh2 N3 C32 1.7(2) . . . . ? Cl2 Rh2 N3 C32 -171.4(2) . . . . ? C2 Rh2 N3 C37 -67.5(14) . . . . ? P2 Rh2 N3 C37 -127.1(2) . . . . ? Cl2 Rh2 N3 C37 59.8(2) . . . . ? N1 Rh1 C1 O1 28(9) . . . . ? P1 Rh1 C1 O1 103(8) . . . . ? Cl1 Rh1 C1 O1 -82(8) . . . . ? N3 Rh2 C2 O2 -5(9) . . . . ? P2 Rh2 C2 O2 54(8) . . . . ? Cl2 Rh2 C2 O2 -132(8) . . . . ? C31 P2 C10 P1 -84.4(2) . . . . ? C41 P2 C10 P1 167.81(17) . . . . ? Rh2 P2 C10 P1 29.4(2) . . . . ? C21 P1 C10 P2 168.53(17) . . . . ? C11 P1 C10 P2 -83.7(2) . . . . ? Rh1 P1 C10 P2 29.7(2) . . . . ? C21 P1 C11 C12 -129.7(2) . . . . ? C10 P1 C11 C12 122.3(2) . . . . ? Rh1 P1 C11 C12 -0.1(3) . . . . ? C21 P1 C11 C16 50.0(3) . . . . ? C10 P1 C11 C16 -57.9(3) . . . . ? Rh1 P1 C11 C16 179.7(2) . . . . ? C16 C11 C12 C13 3.8(5) . . . . ? P1 C11 C12 C13 -176.4(2) . . . . ? C16 C11 C12 N1 -175.0(3) . . . . ? P1 C11 C12 N1 4.8(4) . . . . ? C17 N1 C12 C13 -61.3(4) . . . . ? Rh1 N1 C12 C13 173.8(2) . . . . ? C17 N1 C12 C11 117.5(3) . . . . ? Rh1 N1 C12 C11 -7.4(3) . . . . ? C11 C12 C13 C14 -2.8(5) . . . . ? N1 C12 C13 C14 176.0(3) . . . . ? C12 C13 C14 C15 0.4(5) . . . . ? C13 C14 C15 C16 0.9(6) . . . . ? C14 C15 C16 C11 0.2(5) . . . . ? C12 C11 C16 C15 -2.5(5) . . . . ? P1 C11 C16 C15 177.7(3) . . . . ? C11 P1 C21 C26 -98.0(3) . . . . ? C10 P1 C21 C26 11.9(4) . . . . ? Rh1 P1 C21 C26 146.6(3) . . . . ? C11 P1 C21 C22 76.9(3) . . . . ? C10 P1 C21 C22 -173.2(3) . . . . ? Rh1 P1 C21 C22 -38.5(3) . . . . ? C27 N2 C22 C23 -6.4(6) . . . . ? C27 N2 C22 C21 176.4(4) . . . . ? C26 C21 C22 N2 177.8(4) . . . . ? P1 C21 C22 N2 2.8(5) . . . . ? C26 C21 C22 C23 0.4(6) . . . . ? P1 C21 C22 C23 -174.5(3) . . . . ? N2 C22 C23 C24 -177.2(5) . . . . ? C21 C22 C23 C24 0.1(7) . . . . ? C22 C23 C24 C25 -0.4(9) . . . . ? C23 C24 C25 C26 0.2(9) . . . . ? C24 C25 C26 C21 0.4(8) . . . . ? C22 C21 C26 C25 -0.7(6) . . . . ? P1 C21 C26 C25 174.1(4) . . . . ? C41 P2 C31 C32 -126.3(3) . . . . ? C10 P2 C31 C32 125.0(2) . . . . ? Rh2 P2 C31 C32 2.3(3) . . . . ? C41 P2 C31 C36 52.5(3) . . . . ? C10 P2 C31 C36 -56.2(3) . . . . ? Rh2 P2 C31 C36 -179.0(2) . . . . ? C36 C31 C32 C33 -1.6(5) . . . . ? P2 C31 C32 C33 177.2(2) . . . . ? C36 C31 C32 N3 -179.9(3) . . . . ? P2 C31 C32 N3 -1.1(4) . . . . ? C37 N3 C32 C31 127.5(3) . . . . ? Rh2 N3 C32 C31 -0.7(4) . . . . ? C37 N3 C32 C33 -50.8(4) . . . . ? Rh2 N3 C32 C33 -179.0(2) . . . . ? C31 C32 C33 C34 0.9(5) . . . . ? N3 C32 C33 C34 179.1(3) . . . . ? C32 C33 C34 C35 0.3(6) . . . . ? C33 C34 C35 C36 -0.7(6) . . . . ? C34 C35 C36 C31 0.0(5) . . . . ? C32 C31 C36 C35 1.2(5) . . . . ? P2 C31 C36 C35 -177.6(2) . . . . ? C31 P2 C41 C46 -95.7(3) . . . . ? C10 P2 C41 C46 14.2(3) . . . . ? Rh2 P2 C41 C46 149.3(2) . . . . ? C31 P2 C41 C42 77.9(3) . . . . ? C10 P2 C41 C42 -172.2(3) . . . . ? Rh2 P2 C41 C42 -37.1(3) . . . . ? C47 N4 C42 C43 -9.8(5) . . . . ? C47 N4 C42 C41 173.6(3) . . . . ? C46 C41 C42 N4 178.7(3) . . . . ? P2 C41 C42 N4 5.0(4) . . . . ? C46 C41 C42 C43 2.0(5) . . . . ? P2 C41 C42 C43 -171.7(3) . . . . ? N4 C42 C43 C44 -176.7(4) . . . . ? C41 C42 C43 C44 0.0(6) . . . . ? C42 C43 C44 C45 -2.7(7) . . . . ? C43 C44 C45 C46 3.2(6) . . . . ? C44 C45 C46 C41 -1.1(5) . . . . ? C42 C41 C46 C45 -1.4(5) . . . . ? P2 C41 C46 C45 172.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.670 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.083 data_compound(11) _database_code_depnum_ccdc_archive 'CCDC 713712' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H42 Cl2 N4 O2 P2 Rh2' _chemical_formula_weight 889.39 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' N N 0.0061 0.0033 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 17.363(3) _cell_length_b 20.180(3) _cell_length_c 20.910(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7326.5(18) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6637 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 26.36 _exptl_crystal_description fragment _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.613 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3600 _exptl_absorpt_coefficient_mu 1.171 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6645 _exptl_absorpt_correction_T_max 0.8347 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 62099 _diffrn_reflns_av_R_equivalents 0.0826 _diffrn_reflns_av_sigmaI/netI 0.0672 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 27.60 _reflns_number_total 16892 _reflns_number_gt 14226 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _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^)+(0.0418P)^2^+1.0655P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(2) _refine_ls_number_reflns 16892 _refine_ls_number_parameters 847 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0578 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.0980 _refine_ls_wR_factor_gt 0.0910 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Rh1A Rh 0.31453(2) 0.340007(18) 0.37494(2) 0.02606(9) Uani 1 1 d . . . Rh2A Rh 0.34377(2) 0.413092(19) 0.557359(18) 0.02486(9) Uani 1 1 d . . . Cl1A Cl 0.39832(9) 0.24884(7) 0.35099(8) 0.0458(4) Uani 1 1 d . . . Cl2A Cl 0.47679(8) 0.39988(7) 0.58509(7) 0.0400(3) Uani 1 1 d . . . P1A P 0.24228(7) 0.42747(6) 0.38837(5) 0.0210(2) Uani 1 1 d . . . P2A P 0.22011(7) 0.41962(6) 0.53772(6) 0.0235(3) Uani 1 1 d . . . O1A O 0.1896(3) 0.24376(19) 0.3989(2) 0.0534(12) Uani 1 1 d . . . O2A O 0.3725(3) 0.5566(2) 0.5389(2) 0.0481(11) Uani 1 1 d . . . N10A N 0.4078(2) 0.4108(2) 0.36008(18) 0.0257(9) Uani 1 1 d . . . N20A N 0.0682(2) 0.3857(2) 0.3624(2) 0.0306(10) Uani 1 1 d . . . N30A N 0.3234(2) 0.3068(2) 0.57318(19) 0.0293(9) Uani 1 1 d . . . N40A N 0.0979(3) 0.3940(2) 0.6558(2) 0.0390(11) Uani 1 1 d . . . C1A C 0.2361(3) 0.2816(2) 0.3892(3) 0.0328(12) Uani 1 1 d . . . C2A C 0.3597(3) 0.5012(3) 0.5457(3) 0.0323(12) Uani 1 1 d . . . C3A C 0.1818(3) 0.4425(2) 0.4577(2) 0.0218(9) Uani 1 1 d . . . H3AA H 0.1329 0.4182 0.4513 0.026 Uiso 1 1 calc R . . H3BA H 0.1691 0.4903 0.4585 0.026 Uiso 1 1 calc R . . C11A C 0.3112(3) 0.4959(2) 0.3874(2) 0.0221(10) Uani 1 1 d . . . C12A C 0.3863(3) 0.4805(2) 0.3721(2) 0.0251(10) Uani 1 1 d . . . C13A C 0.4418(3) 0.5308(3) 0.3675(3) 0.0335(12) Uani 1 1 d . . . H13A H 0.4936 0.5203 0.3568 0.040 Uiso 1 1 calc R . . C14A C 0.4209(3) 0.5953(3) 0.3785(3) 0.0362(12) Uani 1 1 d . . . H14A H 0.4584 0.6294 0.3758 0.043 Uiso 1 1 calc R . . C15A C 0.3454(3) 0.6110(2) 0.3934(2) 0.0335(12) Uani 1 1 d . . . H15A H 0.3314 0.6559 0.4008 0.040 Uiso 1 1 calc R . . C16A C 0.2909(3) 0.5620(2) 0.3978(2) 0.0301(11) Uani 1 1 d . . . H16A H 0.2391 0.5731 0.4078 0.036 Uiso 1 1 calc R . . C17A C 0.4331(4) 0.4047(3) 0.2912(3) 0.0410(14) Uani 1 1 d . . . H17A H 0.4750 0.4361 0.2828 0.049 Uiso 1 1 calc R . . H17B H 0.3896 0.4147 0.2629 0.049 Uiso 1 1 calc R . . H17C H 0.4512 0.3595 0.2830 0.049 Uiso 1 1 calc R . . C18A C 0.4749(3) 0.3924(3) 0.4016(3) 0.0354(13) Uani 1 1 d . . . H18A H 0.5167 0.4244 0.3951 0.042 Uiso 1 1 calc R . . H18B H 0.4929 0.3480 0.3901 0.042 Uiso 1 1 calc R . . H18C H 0.4590 0.3930 0.4465 0.042 Uiso 1 1 calc R . . C21A C 0.1797(3) 0.4477(2) 0.3201(2) 0.0223(9) Uani 1 1 d . . . C22A C 0.1036(3) 0.4247(2) 0.3133(2) 0.0245(10) Uani 1 1 d . . . C23A C 0.0632(3) 0.4402(3) 0.2570(2) 0.0292(11) Uani 1 1 d . . . H23A H 0.0116 0.4252 0.2524 0.035 Uiso 1 1 calc R . . C24A C 0.0962(3) 0.4764(3) 0.2085(3) 0.0354(12) Uani 1 1 d . . . H24A H 0.0673 0.4870 0.1713 0.043 Uiso 1 1 calc R . . C25A C 0.1716(3) 0.4974(3) 0.2141(2) 0.0313(11) Uani 1 1 d . . . H25A H 0.1955 0.5211 0.1802 0.038 Uiso 1 1 calc R . . C26A C 0.2122(3) 0.4837(2) 0.2699(2) 0.0271(11) Uani 1 1 d . . . H26A H 0.2636 0.4992 0.2740 0.033 Uiso 1 1 calc R . . C27A C 0.0457(4) 0.3202(3) 0.3390(3) 0.0514(17) Uani 1 1 d . . . H27A H 0.0906 0.2981 0.3202 0.062 Uiso 1 1 calc R . . H27B H 0.0055 0.3250 0.3065 0.062 Uiso 1 1 calc R . . H27C H 0.0260 0.2936 0.3747 0.062 Uiso 1 1 calc R . . C28A C 0.0013(3) 0.4197(3) 0.3904(3) 0.0477(15) Uani 1 1 d . . . H28A H 0.0171 0.4633 0.4063 0.057 Uiso 1 1 calc R . . H28B H -0.0191 0.3932 0.4259 0.057 Uiso 1 1 calc R . . H28C H -0.0386 0.4251 0.3577 0.057 Uiso 1 1 calc R . . C31A C 0.1878(3) 0.3338(2) 0.5456(2) 0.0288(11) Uani 1 1 d . . . C32A C 0.2433(3) 0.2873(2) 0.5623(2) 0.0308(11) Uani 1 1 d . . . C33A C 0.2213(4) 0.2204(3) 0.5670(3) 0.0401(14) Uani 1 1 d . . . H33A H 0.2588 0.1879 0.5773 0.048 Uiso 1 1 calc R . . C34A C 0.1470(4) 0.2016(3) 0.5569(3) 0.0507(16) Uani 1 1 d . . . H34A H 0.1330 0.1563 0.5612 0.061 Uiso 1 1 calc R . . C35A C 0.0908(4) 0.2483(3) 0.5403(3) 0.0495(16) Uani 1 1 d . . . H35A H 0.0391 0.2349 0.5329 0.059 Uiso 1 1 calc R . . C36A C 0.1115(3) 0.3142(3) 0.5348(3) 0.0374(13) Uani 1 1 d . . . H36A H 0.0738 0.3463 0.5237 0.045 Uiso 1 1 calc R . . C37A C 0.3762(3) 0.2693(3) 0.5295(3) 0.0399(13) Uani 1 1 d . . . H37A H 0.3683 0.2216 0.5354 0.048 Uiso 1 1 calc R . . H37B H 0.4298 0.2805 0.5395 0.048 Uiso 1 1 calc R . . H37C H 0.3651 0.2812 0.4850 0.048 Uiso 1 1 calc R . . C38A C 0.3451(4) 0.2903(3) 0.6404(2) 0.0384(13) Uani 1 1 d . . . H38A H 0.3365 0.2430 0.6481 0.046 Uiso 1 1 calc R . . H38B H 0.3135 0.3163 0.6699 0.046 Uiso 1 1 calc R . . H38C H 0.3996 0.3008 0.6472 0.046 Uiso 1 1 calc R . . C41A C 0.1581(3) 0.4759(2) 0.5851(2) 0.0282(10) Uani 1 1 d . . . C42A C 0.1007(3) 0.4585(3) 0.6302(3) 0.0344(12) Uani 1 1 d . . . C43A C 0.0469(3) 0.5058(3) 0.6485(3) 0.0408(14) Uani 1 1 d . . . H43A H 0.0052 0.4933 0.6753 0.049 Uiso 1 1 calc R . . C44A C 0.0532(4) 0.5712(3) 0.6282(3) 0.0500(16) Uani 1 1 d . . . H44A H 0.0157 0.6027 0.6410 0.060 Uiso 1 1 calc R . . C45A C 0.1129(4) 0.5905(3) 0.5900(3) 0.0475(15) Uani 1 1 d . . . H45A H 0.1194 0.6357 0.5785 0.057 Uiso 1 1 calc R . . C46A C 0.1637(3) 0.5426(2) 0.5685(2) 0.0325(11) Uani 1 1 d . . . H46A H 0.2045 0.5559 0.5410 0.039 Uiso 1 1 calc R . . C47A C 0.1626(4) 0.3726(3) 0.6927(3) 0.0462(14) Uani 1 1 d . . . H47A H 0.2103 0.3874 0.6721 0.055 Uiso 1 1 calc R . . H47B H 0.1625 0.3241 0.6955 0.055 Uiso 1 1 calc R . . H47C H 0.1594 0.3915 0.7358 0.055 Uiso 1 1 calc R . . C48A C 0.0248(4) 0.3743(4) 0.6855(4) 0.061(2) Uani 1 1 d . . . H48A H -0.0182 0.3900 0.6592 0.074 Uiso 1 1 calc R . . H48B H 0.0211 0.3939 0.7283 0.074 Uiso 1 1 calc R . . H48C H 0.0227 0.3259 0.6889 0.074 Uiso 1 1 calc R . . Rh1B Rh 0.33742(2) 0.182762(18) -0.021333(18) 0.02425(9) Uani 1 1 d . . . Rh2B Rh 0.24601(2) 0.052200(18) 0.123635(18) 0.02407(8) Uani 1 1 d . . . Cl1B Cl 0.46613(8) 0.21866(7) 0.00469(7) 0.0417(3) Uani 1 1 d . . . Cl2B Cl 0.34396(8) -0.02110(7) 0.16436(7) 0.0411(3) Uani 1 1 d . . . P1B P 0.22406(7) 0.14627(6) -0.05100(6) 0.0210(2) Uani 1 1 d . . . P2B P 0.15902(7) 0.12364(6) 0.09137(6) 0.0212(2) Uani 1 1 d . . . O1B O 0.2703(3) 0.31461(19) 0.0035(2) 0.0484(11) Uani 1 1 d . . . O2B O 0.1737(3) -0.0622(2) 0.0585(2) 0.0530(11) Uani 1 1 d . . . N10B N 0.3761(2) 0.0803(2) -0.04235(18) 0.0271(9) Uani 1 1 d . . . N20B N 0.2886(2) 0.1561(2) -0.18548(19) 0.0294(9) Uani 1 1 d . . . N30B N 0.2960(2) 0.1371(2) 0.1751(2) 0.0284(9) Uani 1 1 d . . . N40B N 0.1046(2) 0.1118(2) 0.22671(19) 0.0263(9) Uani 1 1 d . . . C1B C 0.2974(3) 0.2635(3) -0.0054(3) 0.0343(12) Uani 1 1 d . . . C2B C 0.2012(3) -0.0172(3) 0.0827(3) 0.0330(12) Uani 1 1 d . . . C3B C 0.1438(3) 0.1438(2) 0.0068(2) 0.0243(10) Uani 1 1 d . . . H3AB H 0.1187 0.1878 0.0054 0.029 Uiso 1 1 calc R . . H3BB H 0.1059 0.1115 -0.0099 0.029 Uiso 1 1 calc R . . C11B C 0.2403(3) 0.0597(2) -0.0695(2) 0.0208(9) Uani 1 1 d . . . C12B C 0.3138(3) 0.0355(2) -0.0599(2) 0.0244(10) Uani 1 1 d . . . C13B C 0.3278(3) -0.0321(3) -0.0694(3) 0.0369(13) Uani 1 1 d . . . H13B H 0.3781 -0.0496 -0.0635 0.044 Uiso 1 1 calc R . . C14B C 0.2679(4) -0.0733(3) -0.0873(3) 0.0402(14) Uani 1 1 d . . . H14B H 0.2773 -0.1194 -0.0916 0.048 Uiso 1 1 calc R . . C15B C 0.1962(4) -0.0496(3) -0.0988(3) 0.0385(13) Uani 1 1 d . . . H15B H 0.1567 -0.0785 -0.1131 0.046 Uiso 1 1 calc R . . C16B C 0.1810(3) 0.0173(2) -0.0896(2) 0.0296(11) Uani 1 1 d . . . H16B H 0.1307 0.0343 -0.0968 0.035 Uiso 1 1 calc R . . C17B C 0.4315(3) 0.0844(3) -0.0968(3) 0.0366(12) Uani 1 1 d . . . H17D H 0.4509 0.0399 -0.1068 0.044 Uiso 1 1 calc R . . H17E H 0.4747 0.1131 -0.0849 0.044 Uiso 1 1 calc R . . H17F H 0.4054 0.1027 -0.1344 0.044 Uiso 1 1 calc R . . C18B C 0.4188(3) 0.0534(3) 0.0140(3) 0.0349(12) Uani 1 1 d . . . H18D H 0.4367 0.0084 0.0044 0.042 Uiso 1 1 calc R . . H18E H 0.3846 0.0523 0.0512 0.042 Uiso 1 1 calc R . . H18F H 0.4633 0.0818 0.0232 0.042 Uiso 1 1 calc R . . C21B C 0.1735(3) 0.1790(2) -0.1222(2) 0.0234(9) Uani 1 1 d . . . C22B C 0.2097(3) 0.1741(2) -0.1824(2) 0.0286(11) Uani 1 1 d . . . C23B C 0.1657(4) 0.1874(3) -0.2370(2) 0.0370(12) Uani 1 1 d . . . H23B H 0.1882 0.1810 -0.2779 0.044 Uiso 1 1 calc R . . C24B C 0.0915(4) 0.2093(3) -0.2334(3) 0.0414(14) Uani 1 1 d . . . H24B H 0.0632 0.2178 -0.2714 0.050 Uiso 1 1 calc R . . C25B C 0.0575(3) 0.2190(3) -0.1745(3) 0.0377(13) Uani 1 1 d . . . H25B H 0.0067 0.2362 -0.1717 0.045 Uiso 1 1 calc R . . C26B C 0.0982(3) 0.2033(2) -0.1190(3) 0.0288(11) Uani 1 1 d . . . H26B H 0.0744 0.2092 -0.0784 0.035 Uiso 1 1 calc R . . C27B C 0.3374(4) 0.2154(3) -0.1866(3) 0.0419(13) Uani 1 1 d . . . H27D H 0.3238 0.2443 -0.1507 0.050 Uiso 1 1 calc R . . H27E H 0.3296 0.2392 -0.2269 0.050 Uiso 1 1 calc R . . H27F H 0.3916 0.2023 -0.1829 0.050 Uiso 1 1 calc R . . C28B C 0.3068(4) 0.1139(3) -0.2404(3) 0.0499(16) Uani 1 1 d . . . H28D H 0.2738 0.0745 -0.2396 0.060 Uiso 1 1 calc R . . H28E H 0.3609 0.1004 -0.2383 0.060 Uiso 1 1 calc R . . H28F H 0.2977 0.1387 -0.2800 0.060 Uiso 1 1 calc R . . C31B C 0.1894(3) 0.2010(2) 0.1267(2) 0.0264(10) Uani 1 1 d . . . C32B C 0.2523(3) 0.1993(2) 0.1672(2) 0.0287(11) Uani 1 1 d . . . C33B C 0.2748(3) 0.2565(3) 0.1993(3) 0.0396(13) Uani 1 1 d . . . H33B H 0.3184 0.2558 0.2268 0.048 Uiso 1 1 calc R . . C34B C 0.2337(4) 0.3144(3) 0.1910(3) 0.0502(17) Uani 1 1 d . . . H34B H 0.2488 0.3533 0.2134 0.060 Uiso 1 1 calc R . . C35B C 0.1707(4) 0.3166(3) 0.1503(3) 0.0431(14) Uani 1 1 d . . . H35B H 0.1437 0.3571 0.1440 0.052 Uiso 1 1 calc R . . C36B C 0.1474(3) 0.2601(2) 0.1189(3) 0.0334(12) Uani 1 1 d . . . H36B H 0.1031 0.2610 0.0922 0.040 Uiso 1 1 calc R . . C37B C 0.2993(3) 0.1189(3) 0.2447(3) 0.0378(13) Uani 1 1 d . . . H37D H 0.3212 0.1558 0.2691 0.045 Uiso 1 1 calc R . . H37E H 0.3316 0.0795 0.2502 0.045 Uiso 1 1 calc R . . H37F H 0.2472 0.1095 0.2602 0.045 Uiso 1 1 calc R . . C38B C 0.3761(3) 0.1471(3) 0.1538(3) 0.0379(13) Uani 1 1 d . . . H38D H 0.3984 0.1850 0.1765 0.045 Uiso 1 1 calc R . . H38E H 0.3768 0.1557 0.1077 0.045 Uiso 1 1 calc R . . H38F H 0.4063 0.1072 0.1631 0.045 Uiso 1 1 calc R . . C41B C 0.0575(3) 0.1174(2) 0.1163(2) 0.0256(10) Uani 1 1 d . . . C42B C 0.0409(3) 0.1138(2) 0.1824(2) 0.0263(11) Uani 1 1 d . . . C43B C -0.0343(3) 0.1126(3) 0.2023(3) 0.0346(12) Uani 1 1 d . . . H43B H -0.0450 0.1100 0.2468 0.042 Uiso 1 1 calc R . . C44B C -0.0948(3) 0.1150(3) 0.1597(3) 0.0377(13) Uani 1 1 d . . . H44B H -0.1465 0.1152 0.1747 0.045 Uiso 1 1 calc R . . C45B C -0.0798(3) 0.1170(3) 0.0955(3) 0.0379(13) Uani 1 1 d . . . H45B H -0.1211 0.1173 0.0658 0.046 Uiso 1 1 calc R . . C46B C -0.0042(3) 0.1188(3) 0.0739(3) 0.0322(12) Uani 1 1 d . . . H46B H 0.0056 0.1209 0.0292 0.039 Uiso 1 1 calc R . . C47B C 0.1093(4) 0.0475(3) 0.2576(3) 0.0414(14) Uani 1 1 d . . . H47D H 0.1134 0.0128 0.2249 0.050 Uiso 1 1 calc R . . H47E H 0.0629 0.0401 0.2833 0.050 Uiso 1 1 calc R . . H47F H 0.1548 0.0462 0.2853 0.050 Uiso 1 1 calc R . . C48B C 0.0996(4) 0.1674(3) 0.2727(3) 0.0454(15) Uani 1 1 d . . . H48D H 0.0972 0.2094 0.2492 0.054 Uiso 1 1 calc R . . H48E H 0.1451 0.1671 0.3004 0.054 Uiso 1 1 calc R . . H48F H 0.0531 0.1624 0.2988 0.054 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1A 0.0309(2) 0.02318(18) 0.02408(19) -0.00281(16) -0.00464(17) 0.00459(15) Rh2A 0.02617(19) 0.02968(19) 0.01873(18) 0.00255(15) -0.00358(16) -0.00206(17) Cl1A 0.0487(9) 0.0372(7) 0.0514(9) -0.0145(7) -0.0102(7) 0.0170(7) Cl2A 0.0279(7) 0.0526(9) 0.0395(8) 0.0060(6) -0.0085(6) -0.0037(6) P1A 0.0244(6) 0.0212(6) 0.0173(6) -0.0005(4) -0.0031(5) 0.0005(5) P2A 0.0272(6) 0.0260(6) 0.0173(6) 0.0022(5) -0.0016(5) -0.0005(5) O1A 0.062(3) 0.032(2) 0.066(3) -0.001(2) -0.006(2) -0.017(2) O2A 0.067(3) 0.035(2) 0.042(3) 0.0034(19) -0.010(2) -0.015(2) N10A 0.025(2) 0.033(2) 0.018(2) -0.0030(17) -0.0021(16) 0.0031(18) N20A 0.027(2) 0.033(2) 0.032(2) 0.0009(19) -0.0054(18) -0.0060(18) N30A 0.029(2) 0.036(2) 0.023(2) 0.0044(17) -0.0022(17) 0.0038(19) N40A 0.042(3) 0.039(3) 0.036(3) 0.007(2) 0.000(2) -0.007(2) C1A 0.043(3) 0.022(2) 0.033(3) -0.007(2) -0.007(2) 0.002(2) C2A 0.035(3) 0.038(3) 0.024(3) 0.001(2) -0.009(2) 0.000(2) C3A 0.022(2) 0.025(2) 0.018(2) 0.0006(18) -0.0032(18) 0.0017(19) C11A 0.025(2) 0.021(2) 0.020(2) -0.0010(18) -0.0036(19) 0.0014(18) C12A 0.027(3) 0.032(2) 0.016(2) 0.002(2) -0.005(2) 0.003(2) C13A 0.026(3) 0.042(3) 0.032(3) 0.002(2) 0.003(2) -0.002(2) C14A 0.039(3) 0.033(3) 0.037(3) 0.005(3) -0.005(3) -0.008(2) C15A 0.041(3) 0.024(2) 0.035(3) -0.004(2) -0.007(2) 0.000(2) C16A 0.033(3) 0.027(3) 0.030(3) 0.002(2) -0.003(2) 0.001(2) C17A 0.054(4) 0.046(3) 0.023(3) -0.002(2) 0.008(2) 0.007(3) C18A 0.030(3) 0.038(3) 0.038(3) 0.006(2) -0.005(2) 0.005(2) C21A 0.026(2) 0.022(2) 0.018(2) 0.0006(18) -0.0038(18) 0.002(2) C22A 0.025(2) 0.023(2) 0.025(2) -0.0043(19) 0.001(2) 0.0012(19) C23A 0.026(3) 0.031(3) 0.031(3) -0.004(2) -0.006(2) 0.000(2) C24A 0.043(3) 0.038(3) 0.026(3) 0.000(2) -0.010(2) 0.006(3) C25A 0.037(3) 0.035(3) 0.021(2) 0.002(2) 0.001(2) 0.001(2) C26A 0.028(3) 0.030(3) 0.023(3) 0.001(2) -0.002(2) -0.001(2) C27A 0.060(4) 0.036(3) 0.058(4) 0.006(3) -0.013(3) -0.018(3) C28A 0.035(3) 0.067(4) 0.041(3) 0.008(3) 0.005(3) 0.008(3) C31A 0.032(3) 0.030(3) 0.025(3) 0.005(2) 0.004(2) -0.005(2) C32A 0.033(3) 0.032(3) 0.027(3) 0.007(2) 0.002(2) -0.001(2) C33A 0.047(3) 0.028(3) 0.045(3) 0.010(3) 0.000(3) -0.002(3) C34A 0.060(4) 0.033(3) 0.059(4) 0.012(3) 0.006(3) -0.017(3) C35A 0.042(3) 0.045(4) 0.061(4) 0.008(3) -0.005(3) -0.018(3) C36A 0.040(3) 0.035(3) 0.038(3) 0.005(2) -0.004(2) -0.003(2) C37A 0.040(3) 0.038(3) 0.041(3) -0.004(3) 0.005(3) 0.007(2) C38A 0.048(3) 0.041(3) 0.027(3) 0.010(2) -0.002(3) 0.005(3) C41A 0.037(3) 0.027(2) 0.021(2) -0.0008(19) -0.003(2) 0.003(2) C42A 0.036(3) 0.040(3) 0.027(3) -0.003(2) -0.004(2) 0.001(2) C43A 0.043(3) 0.051(4) 0.028(3) -0.003(3) 0.010(3) 0.003(3) C44A 0.062(4) 0.044(3) 0.044(4) -0.008(3) 0.010(3) 0.015(3) C45A 0.078(5) 0.027(3) 0.037(3) 0.000(3) 0.001(3) 0.007(3) C46A 0.048(3) 0.028(2) 0.022(2) 0.0008(19) 0.007(2) 0.003(2) C47A 0.051(4) 0.048(3) 0.039(3) 0.010(3) 0.006(3) -0.002(3) C48A 0.052(4) 0.059(4) 0.073(5) 0.013(4) 0.013(4) -0.013(4) Rh1B 0.02526(19) 0.02590(18) 0.02160(18) 0.00097(15) -0.00153(16) -0.00255(16) Rh2B 0.02506(19) 0.02341(17) 0.02375(18) 0.00238(15) 0.00211(16) 0.00224(15) Cl1B 0.0338(7) 0.0464(8) 0.0449(8) 0.0060(7) -0.0088(6) -0.0131(6) Cl2B 0.0350(7) 0.0398(7) 0.0485(8) 0.0162(6) 0.0034(7) 0.0101(6) P1B 0.0238(6) 0.0215(6) 0.0176(6) -0.0005(5) -0.0007(5) 0.0014(5) P2B 0.0222(6) 0.0214(5) 0.0200(6) -0.0005(5) 0.0007(5) 0.0006(5) O1B 0.061(3) 0.029(2) 0.056(3) -0.0054(19) 0.005(2) 0.000(2) O2B 0.069(3) 0.036(2) 0.054(3) -0.013(2) 0.011(2) -0.013(2) N10B 0.032(2) 0.032(2) 0.018(2) 0.0047(17) 0.0012(17) 0.0025(18) N20B 0.036(2) 0.034(2) 0.019(2) 0.0015(18) -0.0021(18) -0.001(2) N30B 0.030(2) 0.034(2) 0.022(2) 0.0005(18) -0.0012(17) -0.0036(18) N40B 0.034(2) 0.025(2) 0.020(2) -0.0042(16) 0.0043(17) -0.0043(18) C1B 0.044(3) 0.028(3) 0.031(3) -0.005(2) 0.002(2) -0.008(2) C2B 0.036(3) 0.030(3) 0.034(3) -0.002(2) 0.011(2) 0.007(2) C3B 0.024(2) 0.028(2) 0.020(2) 0.0023(19) 0.0022(19) 0.002(2) C11B 0.027(2) 0.024(2) 0.012(2) -0.0020(17) 0.0010(18) 0.003(2) C12B 0.031(3) 0.027(2) 0.015(2) 0.0044(19) 0.002(2) 0.000(2) C13B 0.041(3) 0.033(3) 0.037(3) 0.003(2) 0.008(3) 0.011(2) C14B 0.059(4) 0.024(3) 0.037(3) -0.005(2) 0.011(3) 0.004(3) C15B 0.053(4) 0.029(3) 0.034(3) -0.008(2) 0.002(3) -0.010(3) C16B 0.031(3) 0.032(3) 0.026(3) -0.007(2) 0.003(2) -0.005(2) C17B 0.033(3) 0.049(3) 0.029(3) 0.001(3) 0.009(2) 0.006(3) C18B 0.039(3) 0.040(3) 0.026(3) 0.005(2) -0.006(2) 0.008(2) C21B 0.031(3) 0.0171(19) 0.022(2) 0.0010(18) -0.006(2) 0.0014(19) C22B 0.040(3) 0.020(2) 0.026(3) 0.002(2) -0.005(2) 0.000(2) C23B 0.050(3) 0.040(3) 0.022(3) 0.005(2) -0.006(2) 0.000(3) C24B 0.052(4) 0.038(3) 0.034(3) 0.007(3) -0.015(3) 0.001(3) C25B 0.032(3) 0.032(3) 0.050(4) 0.007(3) -0.013(3) 0.005(2) C26B 0.028(3) 0.027(2) 0.031(3) 0.005(2) -0.004(2) 0.000(2) C27B 0.044(3) 0.049(3) 0.033(3) 0.012(3) 0.000(3) -0.008(3) C28B 0.053(4) 0.057(4) 0.040(4) -0.015(3) 0.001(3) 0.007(3) C31B 0.035(3) 0.023(2) 0.021(2) 0.0010(19) 0.003(2) -0.001(2) C32B 0.034(3) 0.029(3) 0.023(2) -0.0023(19) 0.006(2) -0.007(2) C33B 0.048(4) 0.036(3) 0.035(3) -0.006(2) -0.004(3) -0.006(3) C34B 0.073(5) 0.032(3) 0.046(4) -0.010(3) 0.001(3) -0.016(3) C35B 0.065(4) 0.032(3) 0.032(3) -0.003(2) 0.006(3) 0.009(3) C36B 0.048(3) 0.026(2) 0.026(3) -0.001(2) 0.004(2) 0.004(2) C37B 0.043(3) 0.045(3) 0.026(3) 0.004(2) -0.005(2) -0.003(3) C38B 0.030(3) 0.046(3) 0.037(3) 0.000(3) -0.006(2) -0.004(3) C41B 0.024(2) 0.021(2) 0.031(3) 0.003(2) 0.006(2) 0.0041(19) C42B 0.032(3) 0.016(2) 0.030(3) 0.0020(19) 0.005(2) 0.002(2) C43B 0.038(3) 0.035(3) 0.031(3) 0.003(2) 0.010(2) -0.002(2) C44B 0.026(3) 0.042(3) 0.045(3) 0.009(3) 0.007(2) -0.002(2) C45B 0.024(3) 0.042(3) 0.048(4) 0.010(3) -0.007(2) -0.003(2) C46B 0.028(3) 0.039(3) 0.030(3) 0.007(2) -0.003(2) 0.000(2) C47B 0.050(4) 0.039(3) 0.035(3) 0.010(3) -0.006(3) -0.011(3) C48B 0.058(4) 0.041(3) 0.037(3) -0.009(3) 0.010(3) -0.012(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 Rh1A C1A 1.825(6) . ? Rh1A N10A 2.181(4) . ? Rh1A P1A 2.1835(12) . ? Rh1A Cl1A 2.3984(14) . ? Rh2A C2A 1.816(6) . ? Rh2A P2A 2.1899(13) . ? Rh2A N30A 2.200(4) . ? Rh2A Cl2A 2.3963(14) . ? P1A C3A 1.816(5) . ? P1A C11A 1.826(5) . ? P1A C21A 1.839(5) . ? P2A C31A 1.828(5) . ? P2A C41A 1.852(5) . ? P2A C3A 1.859(4) . ? O1A C1A 1.130(6) . ? O2A C2A 1.149(6) . ? N10A C12A 1.476(6) . ? N10A C18A 1.499(6) . ? N10A C17A 1.512(6) . ? N20A C22A 1.432(6) . ? N20A C27A 1.463(7) . ? N20A C28A 1.470(7) . ? N30A C32A 1.464(7) . ? N30A C38A 1.492(6) . ? N30A C37A 1.498(7) . ? N40A C42A 1.408(7) . ? N40A C47A 1.430(8) . ? N40A C48A 1.469(8) . ? C11A C12A 1.379(7) . ? C11A C16A 1.397(7) . ? C12A C13A 1.404(7) . ? C13A C14A 1.369(8) . ? C14A C15A 1.384(8) . ? C15A C16A 1.372(7) . ? C21A C26A 1.395(7) . ? C21A C22A 1.407(7) . ? C22A C23A 1.405(7) . ? C23A C24A 1.376(8) . ? C24A C25A 1.381(8) . ? C25A C26A 1.391(7) . ? C31A C32A 1.390(7) . ? C31A C36A 1.401(7) . ? C32A C33A 1.406(7) . ? C33A C34A 1.362(8) . ? C34A C35A 1.399(9) . ? C35A C36A 1.382(8) . ? C41A C46A 1.395(7) . ? C41A C42A 1.415(7) . ? C42A C43A 1.390(8) . ? C43A C44A 1.390(9) . ? C44A C45A 1.365(9) . ? C45A C46A 1.383(8) . ? Rh1B C1B 1.801(6) . ? Rh1B P1B 2.1911(13) . ? Rh1B N10B 2.217(4) . ? Rh1B Cl1B 2.4115(14) . ? Rh2B C2B 1.817(6) . ? Rh2B P2B 2.1943(13) . ? Rh2B N30B 2.202(4) . ? Rh2B Cl2B 2.4094(14) . ? P1B C11B 1.812(5) . ? P1B C3B 1.844(5) . ? P1B C21B 1.850(5) . ? P2B C31B 1.805(5) . ? P2B C3B 1.834(5) . ? P2B C41B 1.843(5) . ? O1B C1B 1.149(6) . ? O2B C2B 1.144(6) . ? N10B C12B 1.458(6) . ? N10B C17B 1.493(6) . ? N10B C18B 1.495(6) . ? N20B C22B 1.419(6) . ? N20B C28B 1.463(7) . ? N20B C27B 1.467(7) . ? N30B C38B 1.473(6) . ? N30B C32B 1.476(7) . ? N30B C37B 1.502(7) . ? N40B C42B 1.443(7) . ? N40B C47B 1.452(7) . ? N40B C48B 1.479(7) . ? C11B C12B 1.381(7) . ? C11B C16B 1.402(7) . ? C12B C13B 1.401(7) . ? C13B C14B 1.382(8) . ? C14B C15B 1.355(8) . ? C15B C16B 1.389(7) . ? C21B C26B 1.398(7) . ? C21B C22B 1.411(7) . ? C22B C23B 1.400(7) . ? C23B C24B 1.363(8) . ? C24B C25B 1.381(9) . ? C25B C26B 1.395(7) . ? C31B C32B 1.383(7) . ? C31B C36B 1.408(7) . ? C32B C33B 1.391(7) . ? C33B C34B 1.380(9) . ? C34B C35B 1.387(9) . ? C35B C36B 1.376(8) . ? C41B C46B 1.392(7) . ? C41B C42B 1.413(7) . ? C42B C43B 1.370(7) . ? C43B C44B 1.380(8) . ? C44B C45B 1.367(8) . ? C45B C46B 1.389(7) . ? 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 C1A Rh1A N10A 178.6(2) . . ? C1A Rh1A P1A 94.14(16) . . ? N10A Rh1A P1A 85.14(11) . . ? C1A Rh1A Cl1A 89.51(17) . . ? N10A Rh1A Cl1A 91.28(11) . . ? P1A Rh1A Cl1A 174.51(6) . . ? C2A Rh2A P2A 93.75(17) . . ? C2A Rh2A N30A 179.0(2) . . ? P2A Rh2A N30A 85.97(11) . . ? C2A Rh2A Cl2A 89.69(17) . . ? P2A Rh2A Cl2A 175.62(5) . . ? N30A Rh2A Cl2A 90.55(11) . . ? C3A P1A C11A 105.1(2) . . ? C3A P1A C21A 103.9(2) . . ? C11A P1A C21A 102.2(2) . . ? C3A P1A Rh1A 124.76(15) . . ? C11A P1A Rh1A 103.48(15) . . ? C21A P1A Rh1A 114.75(15) . . ? C31A P2A C41A 110.7(2) . . ? C31A P2A C3A 101.9(2) . . ? C41A P2A C3A 97.0(2) . . ? C31A P2A Rh2A 103.13(17) . . ? C41A P2A Rh2A 120.46(17) . . ? C3A P2A Rh2A 122.32(15) . . ? C12A N10A C18A 109.5(4) . . ? C12A N10A C17A 108.2(4) . . ? C18A N10A C17A 107.8(4) . . ? C12A N10A Rh1A 114.3(3) . . ? C18A N10A Rh1A 109.4(3) . . ? C17A N10A Rh1A 107.4(3) . . ? C22A N20A C27A 111.8(4) . . ? C22A N20A C28A 111.6(4) . . ? C27A N20A C28A 110.1(5) . . ? C32A N30A C38A 109.1(4) . . ? C32A N30A C37A 110.5(4) . . ? C38A N30A C37A 107.9(4) . . ? C32A N30A Rh2A 113.0(3) . . ? C38A N30A Rh2A 108.6(3) . . ? C37A N30A Rh2A 107.6(3) . . ? C42A N40A C47A 117.3(5) . . ? C42A N40A C48A 116.2(5) . . ? C47A N40A C48A 111.6(5) . . ? O1A C1A Rh1A 177.4(5) . . ? O2A C2A Rh2A 177.6(5) . . ? P1A C3A P2A 118.0(2) . . ? C12A C11A C16A 119.3(4) . . ? C12A C11A P1A 116.9(3) . . ? C16A C11A P1A 123.7(4) . . ? C11A C12A C13A 120.2(5) . . ? C11A C12A N10A 119.6(4) . . ? C13A C12A N10A 120.3(4) . . ? C14A C13A C12A 119.6(5) . . ? C13A C14A C15A 120.5(5) . . ? C16A C15A C14A 120.2(5) . . ? C15A C16A C11A 120.3(5) . . ? C26A C21A C22A 118.3(4) . . ? C26A C21A P1A 117.4(3) . . ? C22A C21A P1A 124.1(4) . . ? C23A C22A C21A 118.8(4) . . ? C23A C22A N20A 120.5(4) . . ? C21A C22A N20A 120.7(4) . . ? C24A C23A C22A 121.8(5) . . ? C23A C24A C25A 119.7(5) . . ? C24A C25A C26A 119.4(5) . . ? C25A C26A C21A 122.0(5) . . ? C32A C31A C36A 120.3(5) . . ? C32A C31A P2A 116.8(4) . . ? C36A C31A P2A 123.0(4) . . ? C31A C32A C33A 118.6(5) . . ? C31A C32A N30A 121.1(4) . . ? C33A C32A N30A 120.3(5) . . ? C34A C33A C32A 120.9(5) . . ? C33A C34A C35A 120.7(5) . . ? C36A C35A C34A 119.1(6) . . ? C35A C36A C31A 120.3(5) . . ? C46A C41A C42A 117.0(5) . . ? C46A C41A P2A 114.7(4) . . ? C42A C41A P2A 127.9(4) . . ? C43A C42A N40A 120.4(5) . . ? C43A C42A C41A 119.2(5) . . ? N40A C42A C41A 120.4(5) . . ? C44A C43A C42A 120.9(5) . . ? C45A C44A C43A 120.6(5) . . ? C44A C45A C46A 118.4(5) . . ? C45A C46A C41A 123.2(5) . . ? C1B Rh1B P1B 90.54(18) . . ? C1B Rh1B N10B 174.9(2) . . ? P1B Rh1B N10B 84.41(11) . . ? C1B Rh1B Cl1B 92.54(18) . . ? P1B Rh1B Cl1B 175.79(5) . . ? N10B Rh1B Cl1B 92.53(11) . . ? C2B Rh2B P2B 93.83(17) . . ? C2B Rh2B N30B 177.76(19) . . ? P2B Rh2B N30B 84.86(12) . . ? C2B Rh2B Cl2B 89.75(17) . . ? P2B Rh2B Cl2B 176.26(5) . . ? N30B Rh2B Cl2B 91.53(12) . . ? C11B P1B C3B 103.4(2) . . ? C11B P1B C21B 104.2(2) . . ? C3B P1B C21B 100.3(2) . . ? C11B P1B Rh1B 104.17(16) . . ? C3B P1B Rh1B 120.14(16) . . ? C21B P1B Rh1B 122.28(15) . . ? C31B P2B C3B 104.2(2) . . ? C31B P2B C41B 102.9(2) . . ? C3B P2B C41B 98.7(2) . . ? C31B P2B Rh2B 103.95(17) . . ? C3B P2B Rh2B 122.75(15) . . ? C41B P2B Rh2B 121.76(16) . . ? C12B N10B C17B 108.7(4) . . ? C12B N10B C18B 110.0(4) . . ? C17B N10B C18B 107.5(4) . . ? C12B N10B Rh1B 113.8(3) . . ? C17B N10B Rh1B 107.2(3) . . ? C18B N10B Rh1B 109.5(3) . . ? C22B N20B C28B 113.1(4) . . ? C22B N20B C27B 110.5(4) . . ? C28B N20B C27B 109.7(5) . . ? C38B N30B C32B 109.6(4) . . ? C38B N30B C37B 106.9(4) . . ? C32B N30B C37B 109.6(4) . . ? C38B N30B Rh2B 109.3(3) . . ? C32B N30B Rh2B 113.9(3) . . ? C37B N30B Rh2B 107.3(3) . . ? C42B N40B C47B 110.7(4) . . ? C42B N40B C48B 110.6(4) . . ? C47B N40B C48B 113.1(4) . . ? O1B C1B Rh1B 178.1(5) . . ? O2B C2B Rh2B 177.8(5) . . ? P2B C3B P1B 122.0(3) . . ? C12B C11B C16B 120.4(4) . . ? C12B C11B P1B 117.0(3) . . ? C16B C11B P1B 122.5(4) . . ? C11B C12B C13B 119.0(5) . . ? C11B C12B N10B 120.2(4) . . ? C13B C12B N10B 120.8(4) . . ? C14B C13B C12B 119.5(5) . . ? C15B C14B C13B 121.8(5) . . ? C14B C15B C16B 119.6(5) . . ? C15B C16B C11B 119.6(5) . . ? C26B C21B C22B 118.9(4) . . ? C26B C21B P1B 122.0(4) . . ? C22B C21B P1B 118.8(4) . . ? C23B C22B C21B 118.2(5) . . ? C23B C22B N20B 122.6(5) . . ? C21B C22B N20B 119.2(4) . . ? C24B C23B C22B 122.2(5) . . ? C23B C24B C25B 120.0(5) . . ? C24B C25B C26B 119.6(5) . . ? C25B C26B C21B 120.9(5) . . ? C32B C31B C36B 120.0(5) . . ? C32B C31B P2B 117.5(4) . . ? C36B C31B P2B 122.3(4) . . ? C31B C32B C33B 119.9(5) . . ? C31B C32B N30B 119.6(4) . . ? C33B C32B N30B 120.5(5) . . ? C34B C33B C32B 119.8(6) . . ? C33B C34B C35B 120.8(5) . . ? C36B C35B C34B 119.9(6) . . ? C35B C36B C31B 119.7(5) . . ? C46B C41B C42B 117.9(5) . . ? C46B C41B P2B 123.6(4) . . ? C42B C41B P2B 118.4(4) . . ? C43B C42B C41B 119.5(5) . . ? C43B C42B N40B 122.3(5) . . ? C41B C42B N40B 118.2(4) . . ? C42B C43B C44B 122.0(5) . . ? C45B C44B C43B 119.3(5) . . ? C44B C45B C46B 120.1(5) . . ? C45B C46B C41B 121.2(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1A Rh1A P1A C3A 52.8(2) . . . . ? N10A Rh1A P1A C3A -126.1(2) . . . . ? Cl1A Rh1A P1A C3A -175.6(5) . . . . ? C1A Rh1A P1A C11A 172.4(2) . . . . ? N10A Rh1A P1A C11A -6.50(18) . . . . ? Cl1A Rh1A P1A C11A -56.0(6) . . . . ? C1A Rh1A P1A C21A -77.2(2) . . . . ? N10A Rh1A P1A C21A 104.0(2) . . . . ? Cl1A Rh1A P1A C21A 54.5(6) . . . . ? C2A Rh2A P2A C31A 179.4(2) . . . . ? N30A Rh2A P2A C31A -1.6(2) . . . . ? Cl2A Rh2A P2A C31A -39.1(7) . . . . ? C2A Rh2A P2A C41A -56.7(2) . . . . ? N30A Rh2A P2A C41A 122.3(2) . . . . ? Cl2A Rh2A P2A C41A 84.9(7) . . . . ? C2A Rh2A P2A C3A 65.9(2) . . . . ? N30A Rh2A P2A C3A -115.1(2) . . . . ? Cl2A Rh2A P2A C3A -152.6(7) . . . . ? C1A Rh1A N10A C12A -52(9) . . . . ? P1A Rh1A N10A C12A 6.5(3) . . . . ? Cl1A Rh1A N10A C12A -177.7(3) . . . . ? C1A Rh1A N10A C18A 72(9) . . . . ? P1A Rh1A N10A C18A 129.7(3) . . . . ? Cl1A Rh1A N10A C18A -54.5(3) . . . . ? C1A Rh1A N10A C17A -172(9) . . . . ? P1A Rh1A N10A C17A -113.6(3) . . . . ? Cl1A Rh1A N10A C17A 62.2(3) . . . . ? C2A Rh2A N30A C32A 76(11) . . . . ? P2A Rh2A N30A C32A 2.1(3) . . . . ? Cl2A Rh2A N30A C32A 179.4(3) . . . . ? C2A Rh2A N30A C38A -45(11) . . . . ? P2A Rh2A N30A C38A -119.1(3) . . . . ? Cl2A Rh2A N30A C38A 58.2(3) . . . . ? C2A Rh2A N30A C37A -161(11) . . . . ? P2A Rh2A N30A C37A 124.4(3) . . . . ? Cl2A Rh2A N30A C37A -58.3(3) . . . . ? N10A Rh1A C1A O1A -94(14) . . . . ? P1A Rh1A C1A O1A -152(11) . . . . ? Cl1A Rh1A C1A O1A 32(11) . . . . ? P2A Rh2A C2A O2A 177(100) . . . . ? N30A Rh2A C2A O2A 103(16) . . . . ? Cl2A Rh2A C2A O2A -1(12) . . . . ? C11A P1A C3A P2A -79.2(3) . . . . ? C21A P1A C3A P2A 173.8(3) . . . . ? Rh1A P1A C3A P2A 39.6(3) . . . . ? C31A P2A C3A P1A -89.6(3) . . . . ? C41A P2A C3A P1A 157.4(3) . . . . ? Rh2A P2A C3A P1A 24.5(3) . . . . ? C3A P1A C11A C12A 139.3(4) . . . . ? C21A P1A C11A C12A -112.4(4) . . . . ? Rh1A P1A C11A C12A 7.0(4) . . . . ? C3A P1A C11A C16A -44.4(5) . . . . ? C21A P1A C11A C16A 63.9(5) . . . . ? Rh1A P1A C11A C16A -176.6(4) . . . . ? C16A C11A C12A C13A 0.5(7) . . . . ? P1A C11A C12A C13A 177.0(4) . . . . ? C16A C11A C12A N10A -179.0(4) . . . . ? P1A C11A C12A N10A -2.5(6) . . . . ? C18A N10A C12A C11A -126.9(5) . . . . ? C17A N10A C12A C11A 115.9(5) . . . . ? Rh1A N10A C12A C11A -3.7(5) . . . . ? C18A N10A C12A C13A 53.6(6) . . . . ? C17A N10A C12A C13A -63.6(6) . . . . ? Rh1A N10A C12A C13A 176.8(4) . . . . ? C11A C12A C13A C14A 0.2(8) . . . . ? N10A C12A C13A C14A 179.7(5) . . . . ? C12A C13A C14A C15A -0.6(9) . . . . ? C13A C14A C15A C16A 0.4(9) . . . . ? C14A C15A C16A C11A 0.4(8) . . . . ? C12A C11A C16A C15A -0.8(7) . . . . ? P1A C11A C16A C15A -177.1(4) . . . . ? C3A P1A C21A C26A 137.6(4) . . . . ? C11A P1A C21A C26A 28.4(4) . . . . ? Rh1A P1A C21A C26A -82.8(4) . . . . ? C3A P1A C21A C22A -47.6(4) . . . . ? C11A P1A C21A C22A -156.8(4) . . . . ? Rh1A P1A C21A C22A 92.0(4) . . . . ? C26A C21A C22A C23A -1.4(7) . . . . ? P1A C21A C22A C23A -176.1(4) . . . . ? C26A C21A C22A N20A 178.0(4) . . . . ? P1A C21A C22A N20A 3.2(6) . . . . ? C27A N20A C22A C23A 59.9(6) . . . . ? C28A N20A C22A C23A -63.9(6) . . . . ? C27A N20A C22A C21A -119.5(5) . . . . ? C28A N20A C22A C21A 116.8(5) . . . . ? C21A C22A C23A C24A 0.7(7) . . . . ? N20A C22A C23A C24A -178.7(5) . . . . ? C22A C23A C24A C25A 1.2(8) . . . . ? C23A C24A C25A C26A -2.4(8) . . . . ? C24A C25A C26A C21A 1.6(8) . . . . ? C22A C21A C26A C25A 0.2(7) . . . . ? P1A C21A C26A C25A 175.3(4) . . . . ? C41A P2A C31A C32A -128.9(4) . . . . ? C3A P2A C31A C32A 128.8(4) . . . . ? Rh2A P2A C31A C32A 1.2(4) . . . . ? C41A P2A C31A C36A 52.1(5) . . . . ? C3A P2A C31A C36A -50.2(5) . . . . ? Rh2A P2A C31A C36A -177.8(4) . . . . ? C36A C31A C32A C33A 0.9(8) . . . . ? P2A C31A C32A C33A -178.1(4) . . . . ? C36A C31A C32A N30A 179.4(5) . . . . ? P2A C31A C32A N30A 0.4(6) . . . . ? C38A N30A C32A C31A 119.0(5) . . . . ? C37A N30A C32A C31A -122.6(5) . . . . ? Rh2A N30A C32A C31A -1.9(6) . . . . ? C38A N30A C32A C33A -62.5(6) . . . . ? C37A N30A C32A C33A 55.9(6) . . . . ? Rh2A N30A C32A C33A 176.6(4) . . . . ? C31A C32A C33A C34A -1.4(9) . . . . ? N30A C32A C33A C34A -180.0(5) . . . . ? C32A C33A C34A C35A 1.3(10) . . . . ? C33A C34A C35A C36A -0.7(10) . . . . ? C34A C35A C36A C31A 0.1(10) . . . . ? C32A C31A C36A C35A -0.3(8) . . . . ? P2A C31A C36A C35A 178.7(5) . . . . ? C31A P2A C41A C46A -162.8(4) . . . . ? C3A P2A C41A C46A -57.2(4) . . . . ? Rh2A P2A C41A C46A 77.0(4) . . . . ? C31A P2A C41A C42A 9.7(5) . . . . ? C3A P2A C41A C42A 115.3(5) . . . . ? Rh2A P2A C41A C42A -110.5(5) . . . . ? C47A N40A C42A C43A -117.7(6) . . . . ? C48A N40A C42A C43A 18.0(8) . . . . ? C47A N40A C42A C41A 62.8(7) . . . . ? C48A N40A C42A C41A -161.5(5) . . . . ? C46A C41A C42A C43A 9.0(8) . . . . ? P2A C41A C42A C43A -163.4(4) . . . . ? C46A C41A C42A N40A -171.5(5) . . . . ? P2A C41A C42A N40A 16.2(7) . . . . ? N40A C42A C43A C44A 174.0(6) . . . . ? C41A C42A C43A C44A -6.5(9) . . . . ? C42A C43A C44A C45A -0.4(10) . . . . ? C43A C44A C45A C46A 4.4(10) . . . . ? C44A C45A C46A C41A -1.6(9) . . . . ? C42A C41A C46A C45A -5.1(8) . . . . ? P2A C41A C46A C45A 168.2(5) . . . . ? C1B Rh1B P1B C11B -178.0(2) . . . . ? N10B Rh1B P1B C11B 1.35(18) . . . . ? Cl1B Rh1B P1B C11B 44.8(7) . . . . ? C1B Rh1B P1B C3B -63.0(3) . . . . ? N10B Rh1B P1B C3B 116.3(2) . . . . ? Cl1B Rh1B P1B C3B 159.8(7) . . . . ? C1B Rh1B P1B C21B 64.6(2) . . . . ? N10B Rh1B P1B C21B -116.0(2) . . . . ? Cl1B Rh1B P1B C21B -72.6(7) . . . . ? C2B Rh2B P2B C31B 179.7(2) . . . . ? N30B Rh2B P2B C31B 1.5(2) . . . . ? Cl2B Rh2B P2B C31B 17.0(8) . . . . ? C2B Rh2B P2B C3B -63.0(3) . . . . ? N30B Rh2B P2B C3B 118.9(2) . . . . ? Cl2B Rh2B P2B C3B 134.4(8) . . . . ? C2B Rh2B P2B C41B 64.6(3) . . . . ? N30B Rh2B P2B C41B -113.6(2) . . . . ? Cl2B Rh2B P2B C41B -98.0(8) . . . . ? C1B Rh1B N10B C12B 2(2) . . . . ? P1B Rh1B N10B C12B -4.6(3) . . . . ? Cl1B Rh1B N10B C12B 178.3(3) . . . . ? C1B Rh1B N10B C17B 123(2) . . . . ? P1B Rh1B N10B C17B 115.6(3) . . . . ? Cl1B Rh1B N10B C17B -61.5(3) . . . . ? C1B Rh1B N10B C18B -121(2) . . . . ? P1B Rh1B N10B C18B -128.1(3) . . . . ? Cl1B Rh1B N10B C18B 54.8(3) . . . . ? C2B Rh2B N30B C38B -176(37) . . . . ? P2B Rh2B N30B C38B -121.9(3) . . . . ? Cl2B Rh2B N30B C38B 59.1(3) . . . . ? C2B Rh2B N30B C32B -53(5) . . . . ? P2B Rh2B N30B C32B 1.0(3) . . . . ? Cl2B Rh2B N30B C32B -178.0(3) . . . . ? C2B Rh2B N30B C37B 69(5) . . . . ? P2B Rh2B N30B C37B 122.5(3) . . . . ? Cl2B Rh2B N30B C37B -56.4(3) . . . . ? P1B Rh1B C1B O1B -27(17) . . . . ? N10B Rh1B C1B O1B -34(19) . . . . ? Cl1B Rh1B C1B O1B 150(17) . . . . ? P2B Rh2B C2B O2B -144(13) . . . . ? N30B Rh2B C2B O2B -91(14) . . . . ? Cl2B Rh2B C2B O2B 34(13) . . . . ? C31B P2B C3B P1B 82.6(3) . . . . ? C41B P2B C3B P1B -171.7(3) . . . . ? Rh2B P2B C3B P1B -34.7(4) . . . . ? C11B P1B C3B P2B 79.4(3) . . . . ? C21B P1B C3B P2B -173.1(3) . . . . ? Rh1B P1B C3B P2B -36.0(4) . . . . ? C3B P1B C11B C12B -124.2(4) . . . . ? C21B P1B C11B C12B 131.3(4) . . . . ? Rh1B P1B C11B C12B 2.1(4) . . . . ? C3B P1B C11B C16B 52.5(4) . . . . ? C21B P1B C11B C16B -52.0(4) . . . . ? Rh1B P1B C11B C16B 178.8(4) . . . . ? C16B C11B C12B C13B -1.1(7) . . . . ? P1B C11B C12B C13B 175.7(4) . . . . ? C16B C11B C12B N10B 176.8(4) . . . . ? P1B C11B C12B N10B -6.5(6) . . . . ? C17B N10B C12B C11B -111.8(5) . . . . ? C18B N10B C12B C11B 130.8(4) . . . . ? Rh1B N10B C12B C11B 7.5(5) . . . . ? C17B N10B C12B C13B 66.0(6) . . . . ? C18B N10B C12B C13B -51.4(6) . . . . ? Rh1B N10B C12B C13B -174.6(4) . . . . ? C11B C12B C13B C14B -0.8(7) . . . . ? N10B C12B C13B C14B -178.7(4) . . . . ? C12B C13B C14B C15B 3.0(8) . . . . ? C13B C14B C15B C16B -3.1(9) . . . . ? C14B C15B C16B C11B 1.1(8) . . . . ? C12B C11B C16B C15B 1.0(7) . . . . ? P1B C11B C16B C15B -175.6(4) . . . . ? C11B P1B C21B C26B 116.3(4) . . . . ? C3B P1B C21B C26B 9.5(4) . . . . ? Rh1B P1B C21B C26B -126.4(3) . . . . ? C11B P1B C21B C22B -58.3(4) . . . . ? C3B P1B C21B C22B -165.0(4) . . . . ? Rh1B P1B C21B C22B 59.1(4) . . . . ? C26B C21B C22B C23B -6.4(7) . . . . ? P1B C21B C22B C23B 168.3(4) . . . . ? C26B C21B C22B N20B 173.5(4) . . . . ? P1B C21B C22B N20B -11.8(6) . . . . ? C28B N20B C22B C23B -36.5(7) . . . . ? C27B N20B C22B C23B 86.9(6) . . . . ? C28B N20B C22B C21B 143.6(5) . . . . ? C27B N20B C22B C21B -93.0(5) . . . . ? C21B C22B C23B C24B 4.7(8) . . . . ? N20B C22B C23B C24B -175.2(5) . . . . ? C22B C23B C24B C25B 0.0(9) . . . . ? C23B C24B C25B C26B -3.0(9) . . . . ? C24B C25B C26B C21B 1.1(8) . . . . ? C22B C21B C26B C25B 3.6(7) . . . . ? P1B C21B C26B C25B -170.9(4) . . . . ? C3B P2B C31B C32B -134.0(4) . . . . ? C41B P2B C31B C32B 123.5(4) . . . . ? Rh2B P2B C31B C32B -4.4(4) . . . . ? C3B P2B C31B C36B 52.1(5) . . . . ? C41B P2B C31B C36B -50.5(5) . . . . ? Rh2B P2B C31B C36B -178.3(4) . . . . ? C36B C31B C32B C33B -1.4(8) . . . . ? P2B C31B C32B C33B -175.5(4) . . . . ? C36B C31B C32B N30B 179.9(5) . . . . ? P2B C31B C32B N30B 5.9(6) . . . . ? C38B N30B C32B C31B 118.5(5) . . . . ? C37B N30B C32B C31B -124.5(5) . . . . ? Rh2B N30B C32B C31B -4.3(6) . . . . ? C38B N30B C32B C33B -60.2(6) . . . . ? C37B N30B C32B C33B 56.8(6) . . . . ? Rh2B N30B C32B C33B 177.1(4) . . . . ? C31B C32B C33B C34B 0.8(8) . . . . ? N30B C32B C33B C34B 179.5(5) . . . . ? C32B C33B C34B C35B -1.0(9) . . . . ? C33B C34B C35B C36B 1.7(9) . . . . ? C34B C35B C36B C31B -2.3(9) . . . . ? C32B C31B C36B C35B 2.1(8) . . . . ? P2B C31B C36B C35B 175.9(4) . . . . ? C31B P2B C41B C46B 115.2(4) . . . . ? C3B P2B C41B C46B 8.4(5) . . . . ? Rh2B P2B C41B C46B -129.2(4) . . . . ? C31B P2B C41B C42B -62.0(4) . . . . ? C3B P2B C41B C42B -168.8(4) . . . . ? Rh2B P2B C41B C42B 53.6(4) . . . . ? C46B C41B C42B C43B -0.7(7) . . . . ? P2B C41B C42B C43B 176.7(4) . . . . ? C46B C41B C42B N40B 179.5(4) . . . . ? P2B C41B C42B N40B -3.1(6) . . . . ? C47B N40B C42B C43B 68.7(6) . . . . ? C48B N40B C42B C43B -57.4(6) . . . . ? C47B N40B C42B C41B -111.4(5) . . . . ? C48B N40B C42B C41B 122.4(5) . . . . ? C41B C42B C43B C44B -0.3(8) . . . . ? N40B C42B C43B C44B 179.5(5) . . . . ? C42B C43B C44B C45B 1.7(9) . . . . ? C43B C44B C45B C46B -2.0(9) . . . . ? C44B C45B C46B C41B 1.0(9) . . . . ? C42B C41B C46B C45B 0.3(8) . . . . ? P2B C41B C46B C45B -176.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.516 _refine_diff_density_min -0.778 _refine_diff_density_rms 0.126 data_compound(14) _database_code_depnum_ccdc_archive 'CCDC 713713' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C39 H48 N4 O7 P2 Rh2' _chemical_formula_weight 952.57 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2965(5) _cell_length_b 25.9075(11) _cell_length_c 14.7517(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.5840(10) _cell_angle_gamma 90.00 _cell_volume 4092.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9897 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.59 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.546 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 0.937 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6356 _exptl_absorpt_correction_T_max 0.7934 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 35647 _diffrn_reflns_av_R_equivalents 0.0165 _diffrn_reflns_av_sigmaI/netI 0.0137 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9382 _reflns_number_gt 8686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-97 (Altomare et al, 1999)' _computing_structure_refinement 'SHELXL-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^)+(0.0288P)^2^+2.8749P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9382 _refine_ls_number_parameters 493 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0251 _refine_ls_R_factor_gt 0.0227 _refine_ls_wR_factor_ref 0.0598 _refine_ls_wR_factor_gt 0.0582 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.003 _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 0.359199(12) 0.119636(5) 0.746383(9) 0.02193(4) Uani 1 1 d . . . Rh2 Rh 0.624201(13) 0.091429(5) 0.720105(10) 0.02565(4) Uani 1 1 d . . . P1 P 0.45570(4) 0.190935(16) 0.80943(3) 0.02067(8) Uani 1 1 d . . . P2 P 0.62263(4) 0.173840(17) 0.68331(3) 0.02167(9) Uani 1 1 d . . . O1 O 0.21219(13) 0.17345(6) 0.56858(10) 0.0389(3) Uani 1 1 d . . . O2 O 0.81850(17) 0.10816(9) 0.90790(13) 0.0681(6) Uani 1 1 d . . . O3 O 0.28057(15) 0.04642(5) 0.71269(11) 0.0379(3) Uani 1 1 d . . . O4 O 0.27765(16) 0.04118(6) 0.56099(11) 0.0453(4) Uani 1 1 d . . . O5 O 0.59466(16) 0.01165(5) 0.72128(11) 0.0412(3) Uani 1 1 d . . . O6 O 0.5906(2) 0.00359(6) 0.87062(12) 0.0589(5) Uani 1 1 d . . . N1 N 0.44641(16) 0.08736(6) 0.88501(11) 0.0310(3) Uani 1 1 d . . . H1N H 0.4897 0.0585 0.8753 0.037 Uiso 1 1 calc R . . N2 N 0.21294(16) 0.19128(7) 0.86006(13) 0.0380(4) Uani 1 1 d . . . H2N H 0.2529 0.1644 0.8476 0.046 Uiso 1 1 calc R . . N3 N 0.51480(14) 0.08198(5) 0.57455(10) 0.0247(3) Uani 1 1 d . . . H3N H 0.4472 0.0612 0.5735 0.030 Uiso 1 1 calc R . . N4 N 0.85585(18) 0.12885(9) 0.64269(16) 0.0503(5) Uani 1 1 d . . . H4N H 0.7899 0.1116 0.6453 0.060 Uiso 1 1 calc R . . C1 C 0.27119(16) 0.15167(7) 0.63461(13) 0.0257(3) Uani 1 1 d . . . C2 C 0.7394(2) 0.10069(10) 0.83817(15) 0.0411(5) Uani 1 1 d . . . C3 C 0.2525(2) 0.02523(7) 0.63127(16) 0.0370(4) Uani 1 1 d . . . C4 C 0.1780(3) -0.02432(9) 0.6223(2) 0.0618(8) Uani 1 1 d . . . H4A H 0.1843 -0.0443 0.5676 0.074 Uiso 1 1 calc R . . H4B H 0.0902 -0.0160 0.6127 0.074 Uiso 1 1 calc R . . H4C H 0.2113 -0.0447 0.6809 0.074 Uiso 1 1 calc R . . C5 C 0.5814(2) -0.01384(8) 0.79096(16) 0.0447(5) Uani 1 1 d . . . C6 C 0.5520(4) -0.07028(10) 0.7717(2) 0.0720(10) Uani 1 1 d . . . H6A H 0.5408 -0.0864 0.8285 0.086 Uiso 1 1 calc R . . H6B H 0.6210 -0.0872 0.7566 0.086 Uiso 1 1 calc R . . H6C H 0.4751 -0.0740 0.7175 0.086 Uiso 1 1 calc R . . C10 C 0.56246(16) 0.22028(7) 0.75251(12) 0.0248(3) Uani 1 1 d . . . H10A H 0.6338 0.2359 0.8026 0.030 Uiso 1 1 calc R . . H10B H 0.5180 0.2483 0.7094 0.030 Uiso 1 1 calc R . . C11 C 0.55584(17) 0.17002(7) 0.92644(12) 0.0270(4) Uani 1 1 d . . . C12 C 0.53900(19) 0.11990(8) 0.95228(13) 0.0316(4) Uani 1 1 d . . . C13 C 0.6117(2) 0.10076(10) 1.04128(15) 0.0456(5) Uani 1 1 d . . . H13 H 0.6003 0.0664 1.0595 0.055 Uiso 1 1 calc R . . C14 C 0.7001(2) 0.13231(11) 1.10237(16) 0.0522(6) Uani 1 1 d . . . H14 H 0.7499 0.1193 1.1627 0.063 Uiso 1 1 calc R . . C15 C 0.7174(2) 0.18226(11) 1.07751(15) 0.0464(6) Uani 1 1 d . . . H15 H 0.7788 0.2034 1.1205 0.056 Uiso 1 1 calc R . . C16 C 0.64522(18) 0.20171(9) 0.98956(14) 0.0354(4) Uani 1 1 d . . . H16 H 0.6564 0.2363 0.9723 0.043 Uiso 1 1 calc R . . C17 C 0.3509(2) 0.06747(9) 0.92717(16) 0.0455(5) Uani 1 1 d . . . H17A H 0.3922 0.0464 0.9836 0.055 Uiso 1 1 calc R . . H17B H 0.2896 0.0463 0.8797 0.055 Uiso 1 1 calc R . . H17C H 0.3084 0.0966 0.9458 0.055 Uiso 1 1 calc R . . C21 C 0.37378(17) 0.24639(7) 0.83579(12) 0.0253(3) Uani 1 1 d . . . C22 C 0.26241(18) 0.23935(7) 0.85938(13) 0.0297(4) Uani 1 1 d . . . C23 C 0.2071(2) 0.28320(9) 0.88526(16) 0.0404(5) Uani 1 1 d . . . H23 H 0.1317 0.2795 0.9001 0.049 Uiso 1 1 calc R . . C24 C 0.2595(2) 0.33120(8) 0.88953(17) 0.0455(5) Uani 1 1 d . . . H24 H 0.2201 0.3601 0.9075 0.055 Uiso 1 1 calc R . . C25 C 0.3687(2) 0.33822(8) 0.86809(16) 0.0426(5) Uani 1 1 d . . . H25 H 0.4049 0.3715 0.8717 0.051 Uiso 1 1 calc R . . C26 C 0.4245(2) 0.29588(7) 0.84129(14) 0.0333(4) Uani 1 1 d . . . H26 H 0.4995 0.3006 0.8262 0.040 Uiso 1 1 calc R . . C27 C 0.0971(2) 0.18276(10) 0.88055(18) 0.0474(6) Uani 1 1 d . . . H27A H 0.0766 0.1459 0.8746 0.057 Uiso 1 1 calc R . . H27B H 0.0298 0.2023 0.8351 0.057 Uiso 1 1 calc R . . H27C H 0.1067 0.1943 0.9458 0.057 Uiso 1 1 calc R . . C31 C 0.50815(15) 0.17620(7) 0.56432(12) 0.0217(3) Uani 1 1 d . . . C32 C 0.46442(16) 0.12900(7) 0.52293(12) 0.0233(3) Uani 1 1 d . . . C33 C 0.37326(18) 0.12669(8) 0.43326(13) 0.0314(4) Uani 1 1 d . . . H33 H 0.3417 0.0943 0.4060 0.038 Uiso 1 1 calc R . . C34 C 0.32931(19) 0.17175(9) 0.38455(14) 0.0362(4) Uani 1 1 d . . . H34 H 0.2672 0.1704 0.3235 0.043 Uiso 1 1 calc R . . C35 C 0.37534(18) 0.21910(8) 0.42420(14) 0.0329(4) Uani 1 1 d . . . H35 H 0.3462 0.2500 0.3895 0.039 Uiso 1 1 calc R . . C36 C 0.46347(17) 0.22153(7) 0.51410(13) 0.0273(4) Uani 1 1 d . . . H36 H 0.4936 0.2541 0.5416 0.033 Uiso 1 1 calc R . . C37 C 0.5900(2) 0.05303(7) 0.52402(14) 0.0331(4) Uani 1 1 d . . . H37A H 0.5364 0.0436 0.4597 0.040 Uiso 1 1 calc R . . H37B H 0.6241 0.0216 0.5600 0.040 Uiso 1 1 calc R . . H37C H 0.6587 0.0748 0.5193 0.040 Uiso 1 1 calc R . . C41 C 0.75575(17) 0.20793(8) 0.66793(13) 0.0315(4) Uani 1 1 d . . . C42 C 0.85339(19) 0.18130(10) 0.64664(15) 0.0406(5) Uani 1 1 d . . . C43 C 0.9469(2) 0.21152(12) 0.62770(19) 0.0578(7) Uani 1 1 d . . . H43 H 1.0145 0.1947 0.6146 0.069 Uiso 1 1 calc R . . C44 C 0.9429(3) 0.26420(13) 0.6278(2) 0.0692(9) Uani 1 1 d . . . H44 H 1.0073 0.2832 0.6143 0.083 Uiso 1 1 calc R . . C45 C 0.8477(3) 0.29023(11) 0.6468(2) 0.0602(8) Uani 1 1 d . . . H45 H 0.8456 0.3269 0.6467 0.072 Uiso 1 1 calc R . . C46 C 0.7546(2) 0.26172(9) 0.66612(15) 0.0419(5) Uani 1 1 d . . . H46 H 0.6878 0.2795 0.6786 0.050 Uiso 1 1 calc R . . C47 C 0.9622(2) 0.10004(13) 0.6343(2) 0.0658(8) Uani 1 1 d . . . H47A H 0.9458 0.0630 0.6361 0.079 Uiso 1 1 calc R . . H47B H 1.0368 0.1090 0.6876 0.079 Uiso 1 1 calc R . . H47C H 0.9757 0.1087 0.5737 0.079 Uiso 1 1 calc R . . O1S O 0.1053(4) 0.11547(17) 0.2082(3) 0.1341(13) Uani 1 1 d . . . C1S C 0.0771(6) 0.0715(4) 0.2523(4) 0.174(4) Uani 1 1 d . . . H1SA H 0.0043 0.0789 0.2738 0.208 Uiso 1 1 calc R . . H1SB H 0.1488 0.0633 0.3096 0.208 Uiso 1 1 calc R . . C2S C 0.0503(9) 0.0284(3) 0.1913(7) 0.193(3) Uani 1 1 d . . . H2SA H -0.0322 0.0135 0.1865 0.232 Uiso 1 1 calc R . . H2SB H 0.1151 0.0015 0.2136 0.232 Uiso 1 1 calc R . . C3S C 0.0503(8) 0.0503(2) 0.0994(5) 0.185(4) Uani 1 1 d . . . H3SA H 0.1179 0.0346 0.0793 0.222 Uiso 1 1 calc R . . H3SB H -0.0305 0.0433 0.0494 0.222 Uiso 1 1 calc R . . C4S C 0.0702(6) 0.1060(2) 0.1132(4) 0.140(2) Uani 1 1 d . . . H4SA H 0.1360 0.1176 0.0867 0.168 Uiso 1 1 calc R . . H4SB H -0.0078 0.1249 0.0799 0.168 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh1 0.02818(7) 0.01876(7) 0.02261(7) -0.00048(5) 0.01341(5) -0.00143(5) Rh2 0.02965(8) 0.02823(8) 0.02175(7) 0.00450(5) 0.01199(6) 0.00814(5) P1 0.0243(2) 0.0204(2) 0.02025(19) -0.00094(15) 0.01123(16) 0.00017(15) P2 0.02025(19) 0.0269(2) 0.01976(19) -0.00184(16) 0.00902(16) -0.00176(16) O1 0.0313(7) 0.0500(9) 0.0364(8) 0.0104(7) 0.0123(6) 0.0084(6) O2 0.0466(10) 0.1149(17) 0.0332(9) -0.0027(10) -0.0006(8) 0.0224(11) O3 0.0543(9) 0.0252(7) 0.0408(8) -0.0033(6) 0.0246(7) -0.0108(6) O4 0.0554(9) 0.0453(9) 0.0437(9) -0.0136(7) 0.0279(8) -0.0194(7) O5 0.0655(10) 0.0286(7) 0.0385(8) 0.0086(6) 0.0293(7) 0.0125(7) O6 0.1081(15) 0.0407(9) 0.0379(9) 0.0158(7) 0.0372(10) 0.0303(9) N1 0.0459(9) 0.0248(7) 0.0271(8) 0.0037(6) 0.0184(7) 0.0030(7) N2 0.0381(9) 0.0364(9) 0.0510(11) -0.0091(8) 0.0302(8) -0.0021(7) N3 0.0316(8) 0.0215(7) 0.0244(7) -0.0003(6) 0.0136(6) -0.0001(6) N4 0.0318(9) 0.0674(14) 0.0609(13) -0.0070(10) 0.0277(9) 0.0037(9) C1 0.0245(8) 0.0267(8) 0.0301(9) -0.0024(7) 0.0148(7) -0.0019(7) C2 0.0375(11) 0.0588(14) 0.0283(10) 0.0073(9) 0.0124(9) 0.0195(10) C3 0.0435(11) 0.0244(9) 0.0520(12) -0.0059(8) 0.0277(10) -0.0051(8) C4 0.087(2) 0.0364(12) 0.0777(19) -0.0201(12) 0.0482(16) -0.0287(13) C5 0.0687(15) 0.0342(11) 0.0416(12) 0.0127(9) 0.0322(11) 0.0235(10) C6 0.142(3) 0.0328(12) 0.0654(18) 0.0110(12) 0.068(2) 0.0112(15) C10 0.0286(8) 0.0260(8) 0.0239(8) -0.0039(7) 0.0140(7) -0.0048(7) C11 0.0285(9) 0.0345(9) 0.0210(8) -0.0006(7) 0.0120(7) 0.0053(7) C12 0.0394(10) 0.0357(10) 0.0231(9) 0.0025(7) 0.0147(8) 0.0098(8) C13 0.0600(14) 0.0492(13) 0.0286(10) 0.0116(9) 0.0157(10) 0.0174(11) C14 0.0529(14) 0.0752(18) 0.0248(10) 0.0062(11) 0.0073(10) 0.0184(12) C15 0.0368(11) 0.0732(17) 0.0266(10) -0.0091(10) 0.0061(8) 0.0041(11) C16 0.0325(10) 0.0488(12) 0.0272(9) -0.0064(8) 0.0125(8) -0.0003(8) C17 0.0631(15) 0.0444(12) 0.0369(11) 0.0106(9) 0.0269(11) -0.0068(11) C21 0.0302(9) 0.0241(8) 0.0236(8) -0.0017(6) 0.0114(7) 0.0038(7) C22 0.0324(9) 0.0329(9) 0.0266(9) -0.0019(7) 0.0134(7) 0.0047(7) C23 0.0422(11) 0.0433(12) 0.0433(12) -0.0025(9) 0.0242(10) 0.0118(9) C24 0.0624(14) 0.0328(11) 0.0482(13) -0.0034(9) 0.0274(11) 0.0163(10) C25 0.0634(14) 0.0232(9) 0.0469(12) -0.0037(8) 0.0254(11) 0.0032(9) C26 0.0431(11) 0.0257(9) 0.0360(10) -0.0025(8) 0.0194(9) 0.0011(8) C27 0.0425(12) 0.0562(14) 0.0552(14) -0.0089(11) 0.0322(11) -0.0061(10) C31 0.0211(7) 0.0265(8) 0.0203(7) 0.0007(6) 0.0106(6) -0.0010(6) C32 0.0251(8) 0.0261(8) 0.0215(8) -0.0002(6) 0.0116(7) 0.0002(6) C33 0.0337(10) 0.0363(10) 0.0236(9) -0.0049(7) 0.0084(7) -0.0046(8) C34 0.0332(10) 0.0499(12) 0.0231(9) 0.0042(8) 0.0054(7) 0.0012(9) C35 0.0315(9) 0.0377(10) 0.0308(9) 0.0125(8) 0.0118(8) 0.0069(8) C36 0.0291(9) 0.0267(9) 0.0297(9) 0.0025(7) 0.0144(7) -0.0012(7) C37 0.0443(11) 0.0278(9) 0.0337(10) -0.0030(8) 0.0215(9) 0.0040(8) C41 0.0256(9) 0.0473(11) 0.0242(8) -0.0080(8) 0.0117(7) -0.0127(8) C42 0.0269(9) 0.0649(15) 0.0328(10) -0.0118(10) 0.0137(8) -0.0088(9) C43 0.0370(12) 0.095(2) 0.0517(14) -0.0210(14) 0.0281(11) -0.0207(13) C44 0.0641(17) 0.097(2) 0.0629(17) -0.0293(16) 0.0427(15) -0.0501(17) C45 0.0738(18) 0.0623(16) 0.0594(16) -0.0228(13) 0.0421(14) -0.0416(14) C46 0.0474(12) 0.0497(13) 0.0359(11) -0.0139(9) 0.0235(9) -0.0224(10) C47 0.0404(13) 0.094(2) 0.0714(19) -0.0119(16) 0.0297(13) 0.0158(14) O1S 0.129(3) 0.167(3) 0.093(2) -0.046(2) 0.016(2) -0.054(2) C1S 0.139(5) 0.291(10) 0.096(4) -0.041(5) 0.045(4) -0.126(6) C2S 0.216(9) 0.142(6) 0.217(9) 0.024(6) 0.063(8) 0.052(6) C3S 0.262(9) 0.115(5) 0.109(4) -0.041(4) -0.038(5) 0.036(5) C4S 0.152(5) 0.148(5) 0.083(3) -0.023(3) -0.014(3) -0.027(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 C1 1.8306(18) . ? Rh1 O3 2.0864(13) . ? Rh1 N1 2.1373(16) . ? Rh1 P1 2.1953(4) . ? Rh2 C2 1.828(2) . ? Rh2 O5 2.0946(15) . ? Rh2 N3 2.1228(15) . ? Rh2 P2 2.2017(5) . ? P1 C21 1.8169(17) . ? P1 C11 1.8188(18) . ? P1 C10 1.8394(17) . ? P2 C31 1.8194(17) . ? P2 C41 1.8194(18) . ? P2 C10 1.8422(17) . ? O1 C1 1.139(2) . ? O2 C2 1.144(3) . ? O3 C3 1.265(3) . ? O4 C3 1.230(3) . ? O5 C5 1.270(2) . ? O6 C5 1.232(3) . ? N1 C12 1.459(3) . ? N1 C17 1.498(3) . ? N2 C22 1.366(3) . ? N2 C27 1.450(2) . ? N3 C32 1.453(2) . ? N3 C37 1.498(2) . ? N4 C42 1.361(3) . ? N4 C47 1.452(3) . ? C3 C4 1.518(3) . ? C5 C6 1.506(3) . ? C11 C12 1.383(3) . ? C11 C16 1.400(3) . ? C12 C13 1.399(3) . ? C13 C14 1.380(4) . ? C14 C15 1.376(4) . ? C15 C16 1.389(3) . ? C21 C26 1.396(3) . ? C21 C22 1.420(2) . ? C22 C23 1.407(3) . ? C23 C24 1.370(3) . ? C24 C25 1.379(3) . ? C25 C26 1.384(3) . ? C31 C32 1.385(2) . ? C31 C36 1.395(2) . ? C32 C33 1.395(2) . ? C33 C34 1.378(3) . ? C34 C35 1.387(3) . ? C35 C36 1.383(3) . ? C41 C46 1.394(3) . ? C41 C42 1.418(3) . ? C42 C43 1.413(3) . ? C43 C44 1.366(4) . ? C44 C45 1.372(4) . ? C45 C46 1.387(3) . ? O1S C4S 1.353(5) . ? O1S C1S 1.397(8) . ? C1S C2S 1.406(9) . ? C2S C3S 1.468(9) . ? C3S C4S 1.466(7) . ? 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 O3 97.46(7) . . ? C1 Rh1 N1 172.59(7) . . ? O3 Rh1 N1 84.47(6) . . ? C1 Rh1 P1 93.09(6) . . ? O3 Rh1 P1 169.17(4) . . ? N1 Rh1 P1 84.76(5) . . ? C2 Rh2 O5 100.87(9) . . ? C2 Rh2 N3 170.85(8) . . ? O5 Rh2 N3 81.47(6) . . ? C2 Rh2 P2 93.15(8) . . ? O5 Rh2 P2 165.97(5) . . ? N3 Rh2 P2 84.61(4) . . ? C21 P1 C11 103.75(8) . . ? C21 P1 C10 102.92(8) . . ? C11 P1 C10 104.85(8) . . ? C21 P1 Rh1 122.55(6) . . ? C11 P1 Rh1 103.07(6) . . ? C10 P1 Rh1 117.62(6) . . ? C31 P2 C41 103.01(8) . . ? C31 P2 C10 103.79(8) . . ? C41 P2 C10 102.57(8) . . ? C31 P2 Rh2 102.58(6) . . ? C41 P2 Rh2 124.02(7) . . ? C10 P2 Rh2 118.17(6) . . ? C3 O3 Rh1 125.40(13) . . ? C5 O5 Rh2 125.45(14) . . ? C12 N1 C17 111.81(16) . . ? C12 N1 Rh1 115.89(11) . . ? C17 N1 Rh1 111.00(13) . . ? C22 N2 C27 122.57(18) . . ? C32 N3 C37 110.40(13) . . ? C32 N3 Rh2 115.97(11) . . ? C37 N3 Rh2 108.75(12) . . ? C42 N4 C47 123.1(2) . . ? O1 C1 Rh1 175.28(16) . . ? O2 C2 Rh2 173.9(2) . . ? O4 C3 O3 126.78(18) . . ? O4 C3 C4 118.8(2) . . ? O3 C3 C4 114.43(19) . . ? O6 C5 O5 125.8(2) . . ? O6 C5 C6 118.8(2) . . ? O5 C5 C6 115.3(2) . . ? P1 C10 P2 113.24(9) . . ? C12 C11 C16 120.03(18) . . ? C12 C11 P1 116.26(14) . . ? C16 C11 P1 123.71(15) . . ? C11 C12 C13 120.0(2) . . ? C11 C12 N1 119.14(16) . . ? C13 C12 N1 120.84(19) . . ? C14 C13 C12 119.3(2) . . ? C15 C14 C13 121.2(2) . . ? C14 C15 C16 120.0(2) . . ? C15 C16 C11 119.5(2) . . ? C26 C21 C22 118.88(16) . . ? C26 C21 P1 120.74(14) . . ? C22 C21 P1 120.15(14) . . ? N2 C22 C23 121.07(18) . . ? N2 C22 C21 121.01(16) . . ? C23 C22 C21 117.88(18) . . ? C24 C23 C22 121.5(2) . . ? C23 C24 C25 120.95(19) . . ? C24 C25 C26 118.9(2) . . ? C25 C26 C21 121.90(19) . . ? C32 C31 C36 119.43(16) . . ? C32 C31 P2 116.07(13) . . ? C36 C31 P2 124.50(13) . . ? C31 C32 C33 120.51(16) . . ? C31 C32 N3 118.94(15) . . ? C33 C32 N3 120.56(16) . . ? C34 C33 C32 119.51(18) . . ? C33 C34 C35 120.34(18) . . ? C36 C35 C34 120.21(18) . . ? C35 C36 C31 119.95(17) . . ? C46 C41 C42 119.02(18) . . ? C46 C41 P2 119.00(15) . . ? C42 C41 P2 121.55(16) . . ? N4 C42 C43 121.2(2) . . ? N4 C42 C41 121.55(19) . . ? C43 C42 C41 117.2(2) . . ? C44 C43 C42 121.8(2) . . ? C43 C44 C45 121.3(2) . . ? C44 C45 C46 118.4(3) . . ? C45 C46 C41 122.2(2) . . ? C4S O1S C1S 107.4(4) . . ? O1S C1S C2S 112.6(6) . . ? C1S C2S C3S 102.8(6) . . ? C4S C3S C2S 107.3(5) . . ? O1S C4S C3S 107.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Rh1 P1 C21 64.50(9) . . . . ? O3 Rh1 P1 C21 -102.5(2) . . . . ? N1 Rh1 P1 C21 -108.39(8) . . . . ? C1 Rh1 P1 C11 -179.54(8) . . . . ? O3 Rh1 P1 C11 13.4(2) . . . . ? N1 Rh1 P1 C11 7.57(7) . . . . ? C1 Rh1 P1 C10 -64.80(9) . . . . ? O3 Rh1 P1 C10 128.2(2) . . . . ? N1 Rh1 P1 C10 122.31(8) . . . . ? C2 Rh2 P2 C31 -178.99(8) . . . . ? O5 Rh2 P2 C31 2.71(19) . . . . ? N3 Rh2 P2 C31 9.91(7) . . . . ? C2 Rh2 P2 C41 65.62(10) . . . . ? O5 Rh2 P2 C41 -112.68(19) . . . . ? N3 Rh2 P2 C41 -105.48(8) . . . . ? C2 Rh2 P2 C10 -65.63(9) . . . . ? O5 Rh2 P2 C10 116.07(19) . . . . ? N3 Rh2 P2 C10 123.27(8) . . . . ? C1 Rh1 O3 C3 38.41(18) . . . . ? N1 Rh1 O3 C3 -148.79(18) . . . . ? P1 Rh1 O3 C3 -154.68(18) . . . . ? C2 Rh2 O5 C5 43.5(2) . . . . ? N3 Rh2 O5 C5 -145.5(2) . . . . ? P2 Rh2 O5 C5 -138.25(18) . . . . ? C1 Rh1 N1 C12 -81.8(6) . . . . ? O3 Rh1 N1 C12 172.69(13) . . . . ? P1 Rh1 N1 C12 -8.42(12) . . . . ? C1 Rh1 N1 C17 47.2(6) . . . . ? O3 Rh1 N1 C17 -58.35(14) . . . . ? P1 Rh1 N1 C17 120.54(13) . . . . ? C2 Rh2 N3 C32 -89.2(5) . . . . ? O5 Rh2 N3 C32 165.23(12) . . . . ? P2 Rh2 N3 C32 -13.01(11) . . . . ? C2 Rh2 N3 C37 35.9(6) . . . . ? O5 Rh2 N3 C37 -69.67(11) . . . . ? P2 Rh2 N3 C37 112.09(11) . . . . ? O3 Rh1 C1 O1 110(2) . . . . ? N1 Rh1 C1 O1 6(2) . . . . ? P1 Rh1 C1 O1 -67(2) . . . . ? O5 Rh2 C2 O2 120(2) . . . . ? N3 Rh2 C2 O2 16(3) . . . . ? P2 Rh2 C2 O2 -59(2) . . . . ? Rh1 O3 C3 O4 8.0(3) . . . . ? Rh1 O3 C3 C4 -170.72(17) . . . . ? Rh2 O5 C5 O6 -4.3(4) . . . . ? Rh2 O5 C5 C6 175.78(19) . . . . ? C21 P1 C10 P2 -161.59(10) . . . . ? C11 P1 C10 P2 90.16(11) . . . . ? Rh1 P1 C10 P2 -23.59(12) . . . . ? C31 P2 C10 P1 89.51(11) . . . . ? C41 P2 C10 P1 -163.50(10) . . . . ? Rh2 P2 C10 P1 -23.18(12) . . . . ? C21 P1 C11 C12 121.41(14) . . . . ? C10 P1 C11 C12 -130.94(14) . . . . ? Rh1 P1 C11 C12 -7.31(15) . . . . ? C21 P1 C11 C16 -57.91(17) . . . . ? C10 P1 C11 C16 49.73(17) . . . . ? Rh1 P1 C11 C16 173.37(14) . . . . ? C16 C11 C12 C13 -0.3(3) . . . . ? P1 C11 C12 C13 -179.67(15) . . . . ? C16 C11 C12 N1 -179.29(16) . . . . ? P1 C11 C12 N1 1.4(2) . . . . ? C17 N1 C12 C11 -122.59(19) . . . . ? Rh1 N1 C12 C11 6.0(2) . . . . ? C17 N1 C12 C13 58.5(2) . . . . ? Rh1 N1 C12 C13 -172.98(15) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? N1 C12 C13 C14 178.7(2) . . . . ? C12 C13 C14 C15 0.4(4) . . . . ? C13 C14 C15 C16 0.0(4) . . . . ? C14 C15 C16 C11 -0.5(3) . . . . ? C12 C11 C16 C15 0.7(3) . . . . ? P1 C11 C16 C15 180.00(15) . . . . ? C11 P1 C21 C26 88.44(17) . . . . ? C10 P1 C21 C26 -20.64(17) . . . . ? Rh1 P1 C21 C26 -155.94(13) . . . . ? C11 P1 C21 C22 -86.00(16) . . . . ? C10 P1 C21 C22 164.91(15) . . . . ? Rh1 P1 C21 C22 29.62(17) . . . . ? C27 N2 C22 C23 4.4(3) . . . . ? C27 N2 C22 C21 -177.8(2) . . . . ? C26 C21 C22 N2 -176.45(19) . . . . ? P1 C21 C22 N2 -1.9(3) . . . . ? C26 C21 C22 C23 1.4(3) . . . . ? P1 C21 C22 C23 175.93(15) . . . . ? N2 C22 C23 C24 176.6(2) . . . . ? C21 C22 C23 C24 -1.2(3) . . . . ? C22 C23 C24 C25 0.3(4) . . . . ? C23 C24 C25 C26 0.5(4) . . . . ? C24 C25 C26 C21 -0.3(3) . . . . ? C22 C21 C26 C25 -0.7(3) . . . . ? P1 C21 C26 C25 -175.18(17) . . . . ? C41 P2 C31 C32 122.27(14) . . . . ? C10 P2 C31 C32 -131.07(13) . . . . ? Rh2 P2 C31 C32 -7.51(13) . . . . ? C41 P2 C31 C36 -57.70(16) . . . . ? C10 P2 C31 C36 48.95(16) . . . . ? Rh2 P2 C31 C36 172.51(13) . . . . ? C36 C31 C32 C33 -2.3(2) . . . . ? P2 C31 C32 C33 177.76(13) . . . . ? C36 C31 C32 N3 177.90(15) . . . . ? P2 C31 C32 N3 -2.1(2) . . . . ? C37 N3 C32 C31 -112.47(17) . . . . ? Rh2 N3 C32 C31 11.77(19) . . . . ? C37 N3 C32 C33 67.7(2) . . . . ? Rh2 N3 C32 C33 -168.07(13) . . . . ? C31 C32 C33 C34 1.9(3) . . . . ? N3 C32 C33 C34 -178.26(17) . . . . ? C32 C33 C34 C35 0.1(3) . . . . ? C33 C34 C35 C36 -1.7(3) . . . . ? C34 C35 C36 C31 1.3(3) . . . . ? C32 C31 C36 C35 0.7(2) . . . . ? P2 C31 C36 C35 -179.36(13) . . . . ? C31 P2 C41 C46 79.15(17) . . . . ? C10 P2 C41 C46 -28.44(18) . . . . ? Rh2 P2 C41 C46 -165.66(13) . . . . ? C31 P2 C41 C42 -93.37(17) . . . . ? C10 P2 C41 C42 159.04(16) . . . . ? Rh2 P2 C41 C42 21.82(19) . . . . ? C47 N4 C42 C43 10.1(4) . . . . ? C47 N4 C42 C41 -171.2(2) . . . . ? C46 C41 C42 N4 -176.7(2) . . . . ? P2 C41 C42 N4 -4.2(3) . . . . ? C46 C41 C42 C43 2.0(3) . . . . ? P2 C41 C42 C43 174.54(17) . . . . ? N4 C42 C43 C44 177.4(3) . . . . ? C41 C42 C43 C44 -1.3(4) . . . . ? C42 C43 C44 C45 0.4(5) . . . . ? C43 C44 C45 C46 -0.1(4) . . . . ? C44 C45 C46 C41 0.8(4) . . . . ? C42 C41 C46 C45 -1.8(3) . . . . ? P2 C41 C46 C45 -174.54(19) . . . . ? C4S O1S C1S C2S 13.8(9) . . . . ? O1S C1S C2S C3S -6.0(10) . . . . ? C1S C2S C3S C4S -3.4(10) . . . . ? C1S O1S C4S C3S -15.3(8) . . . . ? C2S C3S C4S O1S 11.8(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1N O6 0.93 1.84 2.762(2) 172.6 . N2 H2N Rh1 0.88 2.48 3.2792(16) 151.0 . N3 H3N O4 0.93 1.94 2.827(2) 159.8 . N4 H4N Rh2 0.88 2.51 3.3161(19) 152.2 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.723 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.058