# 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 'Maravanji Balakrishna' 'Chelladurai Ganesamoorthy' 'Joel Mague' _publ_contact_author_name 'Maravanji Balakrishna' _publ_contact_author_email KRISHNA@CHEM.IITB.AC.IN _publ_section_title ; Di-, tetra- and polynuclear RhI complexes containing phenylenediaminotetra(phosphonite), p-C6H4[N{P(OC6H4OMe-o)2}2]2 and their catalytic investigation towards transfer hydrogenation reactions ; # Attachment 'Compound_4.cif' data_msb329_0m _database_code_depnum_ccdc_archive 'CCDC 701818' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Dichlorobis(acetonitrile)(\m-1,4-Bis[bis(bis(o- methoxyphenoxy)phosphino)amino]benzene-1\k^2^P,P'; 2\k^2^P",P"')dirhodium(I) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H66 Cl2 N4 O16 P4 Rh2' _chemical_formula_sum 'C66 H66 Cl2 N4 O16 P4 Rh2' _chemical_formula_weight 1571.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2409(5) _cell_length_b 11.0859(6) _cell_length_c 17.0064(9) _cell_angle_alpha 84.207(1) _cell_angle_beta 77.819(1) _cell_angle_gamma 88.350(1) _cell_volume 1694.23(16) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7047 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 28.62 _exptl_crystal_description Plate _exptl_crystal_colour clear _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 802 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9194 _exptl_absorpt_correction_T_max 0.9527 _exptl_absorpt_process_details 'SADABS, (Sheldrick, 2004)' _exptl_special_details ; The diffraction data were collected in three sets of 606 frames having a width of 0.3 \% in omega and phi having values of 0, 120 and 240 \%. ; _diffrn_ambient_temperature 100(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-AXS Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15149 _diffrn_reflns_av_R_equivalents 0.0223 _diffrn_reflns_av_sigmaI/netI 0.0350 _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 -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7829 _reflns_number_gt 6968 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2006)' _publ_section_references ; Bruker-AXS (2006). APEX2, Version 2.1-0, Madison, WI. Bruker-AXS (2006a). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2004). SADABS, Version 2004/2. University of G\"ottingen, Germany. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. ; _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^)+(0.0339P)^2^+1.4007P] 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 7829 _refine_ls_number_parameters 429 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0810 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _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 0.870930(19) 0.379324(16) 0.202677(10) 0.01593(6) Uani 1 1 d . . . Cl Cl 0.83828(6) 0.20041(5) 0.14060(3) 0.02283(12) Uani 1 1 d . . . P1 P 0.92129(6) 0.30334(5) 0.31652(3) 0.01420(11) Uani 1 1 d . . . P2 P 0.89876(6) 0.52338(5) 0.27295(3) 0.01554(12) Uani 1 1 d . . . O1 O 0.80625(17) 0.24193(13) 0.39325(9) 0.0157(3) Uani 1 1 d . . . O2 O 0.8379(2) 0.12212(15) 0.53046(10) 0.0265(4) Uani 1 1 d . . . O3 O 1.05857(17) 0.21347(14) 0.32473(10) 0.0181(3) Uani 1 1 d . . . O4 O 1.31103(18) 0.30130(16) 0.34311(11) 0.0253(4) Uani 1 1 d . . . O5 O 0.76587(17) 0.60121(15) 0.32099(9) 0.0204(3) Uani 1 1 d . . . O6 O 0.50091(18) 0.60086(15) 0.40958(10) 0.0218(3) Uani 1 1 d . . . O7 O 1.01769(18) 0.63151(14) 0.24611(10) 0.0206(3) Uani 1 1 d . . . O8 O 1.0280(2) 0.7669(2) 0.10866(15) 0.0582(8) Uani 1 1 d . . . N1 N 0.9494(2) 0.43758(16) 0.35091(11) 0.0143(4) Uani 1 1 d . . . N2 N 0.8386(2) 0.48613(19) 0.09921(12) 0.0222(4) Uani 1 1 d . . . C1 C 0.7712(2) 0.11778(19) 0.40517(14) 0.0189(5) Uani 1 1 d . . . C2 C 0.7214(3) 0.0617(2) 0.34783(16) 0.0267(5) Uani 1 1 d . . . H2 H 0.7164 0.1045 0.2972 0.032 Uiso 1 1 calc R . . C3 C 0.6780(4) -0.0594(3) 0.36498(19) 0.0400(7) Uani 1 1 d . . . H3 H 0.6422 -0.0995 0.3262 0.048 Uiso 1 1 calc R . . C4 C 0.6873(4) -0.1204(3) 0.43817(19) 0.0443(8) Uani 1 1 d . . . H4 H 0.6577 -0.2027 0.4495 0.053 Uiso 1 1 calc R . . C5 C 0.7390(3) -0.0640(2) 0.49570(17) 0.0345(6) Uani 1 1 d . . . H5 H 0.7450 -0.1076 0.5460 0.041 Uiso 1 1 calc R . . C6 C 0.7822(3) 0.0570(2) 0.47979(15) 0.0234(5) Uani 1 1 d . . . C7 C 0.8571(3) 0.0594(3) 0.60562(16) 0.0343(6) Uani 1 1 d . . . H7A H 0.7604 0.0338 0.6383 0.051 Uiso 1 1 calc R . . H7B H 0.9035 0.1136 0.6350 0.051 Uiso 1 1 calc R . . H7C H 0.9205 -0.0120 0.5950 0.051 Uiso 1 1 calc R . . C8 C 1.1842(2) 0.2000(2) 0.26391(14) 0.0192(5) Uani 1 1 d . . . C9 C 1.1778(3) 0.1375(2) 0.19880(15) 0.0249(5) Uani 1 1 d . . . H9 H 1.0857 0.1091 0.1918 0.030 Uiso 1 1 calc R . . C10 C 1.3076(3) 0.1164(3) 0.14342(16) 0.0316(6) Uani 1 1 d . . . H10 H 1.3044 0.0734 0.0982 0.038 Uiso 1 1 calc R . . C11 C 1.4410(3) 0.1575(3) 0.15384(16) 0.0310(6) Uani 1 1 d . . . H11 H 1.5293 0.1427 0.1158 0.037 Uiso 1 1 calc R . . C12 C 1.4471(3) 0.2206(2) 0.21968(17) 0.0280(6) Uani 1 1 d . . . H12 H 1.5395 0.2490 0.2263 0.034 Uiso 1 1 calc R . . C13 C 1.3185(3) 0.2425(2) 0.27597(15) 0.0214(5) Uani 1 1 d . . . C14 C 1.4489(3) 0.3281(3) 0.3633(2) 0.0364(7) Uani 1 1 d . . . H14A H 1.5054 0.2528 0.3696 0.055 Uiso 1 1 calc R . . H14B H 1.4297 0.3663 0.4140 0.055 Uiso 1 1 calc R . . H14C H 1.5060 0.3834 0.3200 0.055 Uiso 1 1 calc R . . C15 C 0.6581(2) 0.6641(2) 0.28638(14) 0.0185(4) Uani 1 1 d . . . C16 C 0.6890(3) 0.7282(2) 0.21112(15) 0.0235(5) Uani 1 1 d . . . H16 H 0.7860 0.7267 0.1785 0.028 Uiso 1 1 calc R . . C17 C 0.5769(3) 0.7953(2) 0.18330(16) 0.0285(6) Uani 1 1 d . . . H17 H 0.5973 0.8401 0.1316 0.034 Uiso 1 1 calc R . . C18 C 0.4368(3) 0.7965(2) 0.23067(17) 0.0303(6) Uani 1 1 d . . . H18 H 0.3606 0.8425 0.2116 0.036 Uiso 1 1 calc R . . C19 C 0.4053(3) 0.7304(2) 0.30708(16) 0.0263(5) Uani 1 1 d . . . H19 H 0.3079 0.7308 0.3393 0.032 Uiso 1 1 calc R . . C20 C 0.5166(3) 0.6646(2) 0.33521(14) 0.0192(5) Uani 1 1 d . . . C21 C 0.3550(3) 0.5992(3) 0.46012(16) 0.0299(6) Uani 1 1 d . . . H21A H 0.3236 0.6822 0.4708 0.045 Uiso 1 1 calc R . . H21B H 0.3562 0.5504 0.5113 0.045 Uiso 1 1 calc R . . H21C H 0.2856 0.5638 0.4327 0.045 Uiso 1 1 calc R . . C22 C 1.1428(3) 0.6197(2) 0.18442(14) 0.0205(5) Uani 1 1 d . . . C23 C 1.2576(3) 0.5422(2) 0.19488(16) 0.0256(5) Uani 1 1 d . . . H23 H 1.2514 0.4913 0.2439 0.031 Uiso 1 1 calc R . . C24 C 1.3832(3) 0.5388(3) 0.13304(18) 0.0323(6) Uani 1 1 d . . . H24 H 1.4634 0.4858 0.1395 0.039 Uiso 1 1 calc R . . C25 C 1.3897(3) 0.6139(3) 0.06175(17) 0.0349(6) Uani 1 1 d . . . H25 H 1.4749 0.6117 0.0194 0.042 Uiso 1 1 calc R . . C26 C 1.2741(3) 0.6916(3) 0.05167(17) 0.0359(7) Uani 1 1 d . . . H26 H 1.2800 0.7425 0.0027 0.043 Uiso 1 1 calc R . . C27 C 1.1493(3) 0.6951(3) 0.11315(16) 0.0286(6) Uani 1 1 d . . . C28 C 1.0480(4) 0.8824(3) 0.0682(2) 0.0484(8) Uani 1 1 d . . . H28A H 1.1306 0.9216 0.0833 0.073 Uiso 1 1 calc R . . H28B H 0.9576 0.9306 0.0831 0.073 Uiso 1 1 calc R . . H28C H 1.0701 0.8766 0.0098 0.073 Uiso 1 1 calc R . . C29 C 1.0190(2) 0.3806(2) 0.48089(14) 0.0168(4) Uani 1 1 d . . . H29 H 1.0325 0.2991 0.4680 0.020 Uiso 1 1 calc R . . C30 C 0.9760(2) 0.46922(19) 0.42614(13) 0.0150(4) Uani 1 1 d . . . C31 C 0.9578(2) 0.5886(2) 0.44569(13) 0.0168(4) Uani 1 1 d . . . H31 H 0.9293 0.6495 0.4084 0.020 Uiso 1 1 calc R . . C32 C 0.8307(3) 0.5543(2) 0.04558(14) 0.0216(5) Uani 1 1 d . . . C33 C 0.8218(3) 0.6436(2) -0.02218(16) 0.0288(6) Uani 1 1 d . . . H33A H 0.7369 0.6976 -0.0069 0.043 Uiso 1 1 calc R . . H33B H 0.8097 0.6020 -0.0685 0.043 Uiso 1 1 calc R . . H33C H 0.9129 0.6912 -0.0367 0.043 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 0.01395(9) 0.01879(10) 0.01486(9) 0.00025(6) -0.00346(6) -0.00033(6) Cl 0.0226(3) 0.0252(3) 0.0219(3) -0.0034(2) -0.0064(2) -0.0036(2) P1 0.0123(3) 0.0145(3) 0.0155(3) 0.0008(2) -0.0032(2) -0.0012(2) P2 0.0143(3) 0.0171(3) 0.0143(3) 0.0015(2) -0.0026(2) 0.0010(2) O1 0.0163(8) 0.0123(7) 0.0171(8) 0.0009(6) -0.0012(6) -0.0020(6) O2 0.0364(10) 0.0203(9) 0.0230(9) 0.0050(7) -0.0104(8) 0.0003(7) O3 0.0132(7) 0.0191(8) 0.0206(8) 0.0028(6) -0.0027(6) 0.0016(6) O4 0.0179(8) 0.0253(9) 0.0349(10) -0.0062(7) -0.0091(7) 0.0000(7) O5 0.0174(8) 0.0260(9) 0.0171(8) -0.0004(7) -0.0041(6) 0.0064(6) O6 0.0169(8) 0.0239(9) 0.0228(9) 0.0005(7) -0.0014(7) -0.0002(6) O7 0.0223(8) 0.0174(8) 0.0191(8) 0.0015(6) 0.0012(7) -0.0023(6) O8 0.0258(11) 0.0665(16) 0.0663(16) 0.0486(13) -0.0003(10) 0.0020(10) N1 0.0154(9) 0.0127(8) 0.0145(9) 0.0023(7) -0.0039(7) -0.0023(7) N2 0.0206(10) 0.0260(11) 0.0198(10) -0.0020(8) -0.0037(8) -0.0019(8) C1 0.0180(11) 0.0111(10) 0.0251(12) 0.0006(9) -0.0002(9) -0.0013(8) C2 0.0347(14) 0.0186(12) 0.0254(13) -0.0007(10) -0.0034(11) -0.0046(10) C3 0.061(2) 0.0234(14) 0.0361(16) -0.0076(12) -0.0064(14) -0.0151(13) C4 0.070(2) 0.0159(13) 0.0435(18) -0.0011(12) -0.0021(16) -0.0134(13) C5 0.0517(18) 0.0169(12) 0.0300(14) 0.0056(10) -0.0010(13) -0.0018(11) C6 0.0268(13) 0.0163(11) 0.0245(12) -0.0004(9) -0.0005(10) 0.0014(9) C7 0.0441(17) 0.0304(14) 0.0268(14) 0.0097(11) -0.0112(12) 0.0077(12) C8 0.0153(11) 0.0169(11) 0.0230(12) 0.0023(9) -0.0012(9) 0.0050(8) C9 0.0248(13) 0.0238(12) 0.0273(13) -0.0010(10) -0.0087(10) 0.0021(10) C10 0.0339(15) 0.0350(15) 0.0259(13) -0.0073(11) -0.0059(11) 0.0108(12) C11 0.0245(13) 0.0352(15) 0.0278(14) 0.0023(11) 0.0033(11) 0.0081(11) C12 0.0174(12) 0.0268(13) 0.0365(15) 0.0046(11) -0.0017(10) 0.0005(10) C13 0.0192(11) 0.0157(11) 0.0280(13) 0.0034(9) -0.0051(10) 0.0019(9) C14 0.0240(14) 0.0339(15) 0.0556(19) -0.0116(13) -0.0142(13) -0.0032(11) C15 0.0174(11) 0.0171(11) 0.0235(12) -0.0043(9) -0.0087(9) 0.0029(8) C16 0.0220(12) 0.0250(12) 0.0224(12) -0.0017(10) -0.0031(10) 0.0030(9) C17 0.0357(15) 0.0271(13) 0.0229(13) 0.0031(10) -0.0100(11) 0.0028(11) C18 0.0281(14) 0.0300(14) 0.0365(15) -0.0022(11) -0.0169(12) 0.0078(11) C19 0.0199(12) 0.0270(13) 0.0328(14) -0.0029(11) -0.0077(10) 0.0029(10) C20 0.0192(11) 0.0158(11) 0.0239(12) -0.0043(9) -0.0064(9) -0.0009(8) C21 0.0210(13) 0.0346(14) 0.0296(14) -0.0002(11) 0.0032(10) 0.0027(10) C22 0.0188(11) 0.0232(12) 0.0188(11) -0.0012(9) -0.0018(9) -0.0064(9) C23 0.0235(13) 0.0229(12) 0.0295(13) 0.0012(10) -0.0050(10) -0.0032(10) C24 0.0220(13) 0.0299(14) 0.0433(16) -0.0064(12) -0.0017(11) -0.0020(10) C25 0.0243(14) 0.0442(17) 0.0331(15) -0.0115(13) 0.0061(11) -0.0123(12) C26 0.0284(14) 0.0548(19) 0.0224(13) 0.0077(12) -0.0037(11) -0.0149(13) C27 0.0205(12) 0.0381(15) 0.0252(13) 0.0091(11) -0.0052(10) -0.0051(11) C28 0.053(2) 0.0334(17) 0.057(2) -0.0073(15) -0.0070(17) 0.0008(14) C29 0.0158(10) 0.0133(10) 0.0215(11) 0.0001(8) -0.0051(9) -0.0015(8) C30 0.0127(10) 0.0165(10) 0.0155(10) 0.0006(8) -0.0028(8) -0.0035(8) C31 0.0180(11) 0.0145(10) 0.0187(11) 0.0032(8) -0.0072(9) -0.0015(8) C32 0.0192(11) 0.0261(12) 0.0196(12) -0.0021(10) -0.0041(9) -0.0018(9) C33 0.0295(14) 0.0315(14) 0.0241(13) 0.0070(11) -0.0072(11) -0.0027(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh N2 2.090(2) . ? Rh P2 2.1410(6) . ? Rh P1 2.1686(6) . ? Rh Cl 2.3939(6) . ? P1 O1 1.6041(16) . ? P1 O3 1.6110(16) . ? P1 N1 1.6988(19) . ? P1 P2 2.4928(8) . ? P2 O5 1.6055(17) . ? P2 O7 1.6146(17) . ? P2 N1 1.6920(18) . ? O1 C1 1.408(3) . ? O2 C6 1.365(3) . ? O2 C7 1.435(3) . ? O3 C8 1.398(3) . ? O4 C13 1.360(3) . ? O4 C14 1.434(3) . ? O5 C15 1.396(3) . ? O6 C20 1.366(3) . ? O6 C21 1.438(3) . ? O7 C22 1.400(3) . ? O8 C27 1.368(3) . ? O8 C28 1.389(4) . ? N1 C30 1.431(3) . ? N2 C32 1.138(3) . ? C1 C2 1.370(3) . ? C1 C6 1.397(3) . ? C2 C3 1.397(4) . ? C2 H2 0.9500 . ? C3 C4 1.373(4) . ? C3 H3 0.9500 . ? C4 C5 1.383(4) . ? C4 H4 0.9500 . ? C5 C6 1.394(3) . ? C5 H5 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.377(3) . ? C8 C13 1.402(3) . ? C9 C10 1.390(4) . ? C9 H9 0.9500 . ? C10 C11 1.378(4) . ? C10 H10 0.9500 . ? C11 C12 1.390(4) . ? C11 H11 0.9500 . ? C12 C13 1.392(3) . ? C12 H12 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.378(3) . ? C15 C20 1.393(3) . ? C16 C17 1.394(3) . ? C16 H16 0.9500 . ? C17 C18 1.373(4) . ? C17 H17 0.9500 . ? C18 C19 1.404(4) . ? C18 H18 0.9500 . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.376(3) . ? C22 C27 1.392(3) . ? C23 C24 1.395(4) . ? C23 H23 0.9500 . ? C24 C25 1.391(4) . ? C24 H24 0.9500 . ? C25 C26 1.381(4) . ? C25 H25 0.9500 . ? C26 C27 1.386(4) . ? C26 H26 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.387(3) 2_766 ? C29 C30 1.392(3) . ? C29 H29 0.9500 . ? C30 C31 1.394(3) . ? C31 C29 1.387(3) 2_766 ? C31 H31 0.9500 . ? C32 C33 1.456(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? 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 N2 Rh P2 97.77(6) . . ? N2 Rh P1 168.02(6) . . ? P2 Rh P1 70.68(2) . . ? N2 Rh Cl 89.88(6) . . ? P2 Rh Cl 172.23(2) . . ? P1 Rh Cl 101.76(2) . . ? O1 P1 O3 96.78(8) . . ? O1 P1 N1 100.16(9) . . ? O3 P1 N1 109.16(9) . . ? O1 P1 Rh 126.55(6) . . ? O3 P1 Rh 124.55(6) . . ? N1 P1 Rh 96.51(6) . . ? O1 P1 P2 119.94(6) . . ? O3 P1 P2 134.18(6) . . ? N1 P1 P2 42.58(6) . . ? Rh P1 P2 54.143(19) . . ? O5 P2 O7 97.47(9) . . ? O5 P2 N1 100.45(9) . . ? O7 P2 N1 106.56(9) . . ? O5 P2 Rh 124.74(7) . . ? O7 P2 Rh 126.04(7) . . ? N1 P2 Rh 97.76(7) . . ? O5 P2 P1 119.26(7) . . ? O7 P2 P1 133.09(7) . . ? N1 P2 P1 42.79(6) . . ? Rh P2 P1 55.181(19) . . ? C1 O1 P1 124.05(14) . . ? C6 O2 C7 117.0(2) . . ? C8 O3 P1 125.17(14) . . ? C13 O4 C14 116.8(2) . . ? C15 O5 P2 124.87(15) . . ? C20 O6 C21 116.39(19) . . ? C22 O7 P2 120.67(14) . . ? C27 O8 C28 119.0(2) . . ? C30 N1 P2 131.18(15) . . ? C30 N1 P1 133.07(15) . . ? P2 N1 P1 94.64(9) . . ? C32 N2 Rh 171.9(2) . . ? C2 C1 C6 122.0(2) . . ? C2 C1 O1 121.3(2) . . ? C6 C1 O1 116.6(2) . . ? C1 C2 C3 119.0(2) . . ? C1 C2 H2 120.5 . . ? C3 C2 H2 120.5 . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 121.2(3) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C6 119.9(3) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? O2 C6 C5 125.7(2) . . ? O2 C6 C1 116.2(2) . . ? C5 C6 C1 118.2(2) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 O3 120.9(2) . . ? C9 C8 C13 121.6(2) . . ? O3 C8 C13 117.2(2) . . ? C8 C9 C10 119.2(2) . . ? C8 C9 H9 120.4 . . ? C10 C9 H9 120.4 . . ? C11 C10 C9 120.2(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.4(2) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C13 120.3(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? O4 C13 C12 125.6(2) . . ? O4 C13 C8 116.2(2) . . ? C12 C13 C8 118.2(2) . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 121.3(2) . . ? C16 C15 O5 123.1(2) . . ? C20 C15 O5 115.5(2) . . ? C15 C16 C17 119.4(2) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C18 C17 C16 119.9(2) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.5(2) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 119.7(2) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? O6 C20 C19 125.1(2) . . ? O6 C20 C15 115.8(2) . . ? C19 C20 C15 119.1(2) . . ? O6 C21 H21A 109.5 . . ? O6 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O6 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 C27 121.3(2) . . ? C23 C22 O7 121.9(2) . . ? C27 C22 O7 116.8(2) . . ? C22 C23 C24 119.5(2) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C25 C24 C23 119.2(3) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C26 C25 C24 120.9(2) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C27 119.9(3) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? O8 C27 C26 124.4(2) . . ? O8 C27 C22 116.4(2) . . ? C26 C27 C22 119.2(3) . . ? O8 C28 H28A 109.5 . . ? O8 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O8 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C30 120.0(2) 2_766 . ? C31 C29 H29 120.0 2_766 . ? C30 C29 H29 120.0 . . ? C29 C30 C31 119.3(2) . . ? C29 C30 N1 120.2(2) . . ? C31 C30 N1 120.44(19) . . ? C29 C31 C30 120.7(2) 2_766 . ? C29 C31 H31 119.7 2_766 . ? C30 C31 H31 119.7 . . ? N2 C32 C33 178.7(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.931 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.931 _refine_diff_density_max 0.685 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.081 # Attachment 'Compound_6.cif' data_msb368_0m _database_code_depnum_ccdc_archive 'CCDC 701819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; catena-Poly{dichloro(\m-1,4-bis(bis(bis(2- methoxyphenoxy)phospino)amino)benzene-1\k^2^ P,P':2\k^2^P",P"')(\m-pyrazine-1\kN:2\kN') dirhodium(I)} ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H64 Cl2 N4 O16 P4 Rh2' _chemical_formula_sum 'C66 H64 Cl2 N4 O16 P4 Rh2' _chemical_formula_weight 1569.81 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 P2(1)/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 16.9519(9) _cell_length_b 11.3413(6) _cell_length_c 18.325(1) _cell_angle_alpha 90.00 _cell_angle_beta 110.072(1) _cell_angle_gamma 90.00 _cell_volume 3309.1(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6709 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 24.79 _exptl_crystal_description Block _exptl_crystal_colour orange _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 0.748 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9071 _exptl_absorpt_correction_T_max 0.9364 _exptl_absorpt_process_details 'sadabs (Sheldrick, 2007)' _exptl_special_details ; The diffraction data were obtained from 3 sets of 606 frames, each of width 0.3 deg. in omega, colllected at phi = 0.00, 120.00 and 240.00 deg. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart APEX CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23110 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_sigmaI/netI 0.0642 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 24.83 _reflns_number_total 5711 _reflns_number_gt 4024 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_data_reduction 'Bruker SAINT+ (Bruker-AXS, 2006a)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker APEX2 (Bruker-AXS, 2006)' _computing_publication_material 'Bruker APEX2 (Bruker-AXS, 2006)' _publ_section_references ; Bruker-AXS (2006). APEX2, Version 2.1-0, Madison, WI. Bruker-AXS (2006a). SAINT+, Version 7.34A, Madison, WI Sheldrick, G. M. (1997). SHELXS-97 and SHELXL-97. University of G\"ottingen, Germany. Sheldrick, G, M. (2007). SADABS, Version 2007/2. University of G\"ottingen, Germany. ; _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. H-atoms were placed in calculated positions (C---H = 0.95 - 0.98 \%A) and included as riding contributions with isotropic displacement parameters 1.2 - 1.5 times those of the attached carbon atoms. The methoxy group containing O8 and C31 is disordered over two sites in a 60/40 ratio. These atoms were refined with restraints to approximate the same geometry. ; _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^)+(0.0619P)^2^] 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 5711 _refine_ls_number_parameters 436 _refine_ls_number_restraints 27 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0467 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1051 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.021 _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 0.68657(2) 0.66180(3) 0.01752(2) 0.02631(14) Uani 1 1 d . . . Cl1 Cl 0.60681(7) 0.83857(11) -0.00126(8) 0.0340(3) Uani 1 1 d . . . P1 P 0.80631(7) 0.72449(10) 0.01298(8) 0.0223(3) Uani 1 1 d . . . P2 P 0.76656(7) 0.51440(11) 0.02234(8) 0.0261(3) Uani 1 1 d . . . O1 O 0.81799(19) 0.8020(3) -0.05603(19) 0.0261(8) Uani 1 1 d . . . O2 O 0.8829(2) 0.7026(3) -0.1515(2) 0.0351(9) Uani 1 1 d . . . O3 O 0.87895(18) 0.7904(3) 0.08219(18) 0.0231(7) Uani 1 1 d . . . O4 O 1.0217(2) 0.8972(3) 0.0931(2) 0.0335(8) Uani 1 1 d . . . O5 O 0.7416(2) 0.4157(3) -0.0447(2) 0.0340(9) Uani 1 1 d . . . O6 O 0.6394(2) 0.2479(3) -0.0376(2) 0.0439(10) Uani 1 1 d . . . O7 O 0.8086(2) 0.4231(3) 0.0923(2) 0.0332(9) Uani 1 1 d . . . O8 O 0.7378(7) 0.3351(10) 0.1847(7) 0.049(3) Uani 0.603(17) 1 d PDU A 1 O8A O 0.7579(12) 0.3092(15) 0.1986(11) 0.049(3) Uani 0.397(17) 1 d PDU A 2 N1 N 0.8488(2) 0.5896(3) 0.0118(2) 0.0217(9) Uani 1 1 d . . . N2 N 0.5737(3) 0.5664(4) 0.0110(3) 0.0365(11) Uani 1 1 d . . . C1 C 0.7673(3) 0.7951(4) -0.1342(3) 0.0268(11) Uani 1 1 d . . . C2 C 0.6882(3) 0.8400(5) -0.1611(3) 0.0439(14) Uani 1 1 d . . . H2 H 0.6634 0.8720 -0.1262 0.053 Uiso 1 1 calc R . . C3 C 0.6438(4) 0.8381(6) -0.2415(4) 0.0590(18) Uani 1 1 d . . . H3 H 0.5877 0.8666 -0.2611 0.071 Uiso 1 1 calc R . . C4 C 0.6809(4) 0.7957(6) -0.2913(4) 0.0602(19) Uani 1 1 d . . . H4 H 0.6514 0.7981 -0.3457 0.072 Uiso 1 1 calc R . . C5 C 0.7607(4) 0.7495(5) -0.2636(3) 0.0479(15) Uani 1 1 d . . . H5 H 0.7858 0.7193 -0.2988 0.057 Uiso 1 1 calc R . . C6 C 0.8043(3) 0.7468(4) -0.1847(3) 0.0298(12) Uani 1 1 d . . . C7 C 0.9218(4) 0.6482(6) -0.2009(4) 0.0560(17) Uani 1 1 d . . . H7A H 0.8857 0.5848 -0.2307 0.084 Uiso 1 1 calc R . . H7B H 0.9763 0.6153 -0.1691 0.084 Uiso 1 1 calc R . . H7C H 0.9302 0.7070 -0.2366 0.084 Uiso 1 1 calc R . . C8 C 0.8819(3) 0.9152(4) 0.0866(3) 0.0263(11) Uani 1 1 d . . . C9 C 0.8125(3) 0.9799(5) 0.0856(3) 0.0366(13) Uani 1 1 d . . . H9 H 0.7614 0.9415 0.0817 0.044 Uiso 1 1 calc R . . C10 C 0.8186(4) 1.1029(5) 0.0905(3) 0.0450(15) Uani 1 1 d . . . H10 H 0.7712 1.1489 0.0889 0.054 Uiso 1 1 calc R . . C11 C 0.8928(4) 1.1563(5) 0.0974(3) 0.0431(15) Uani 1 1 d . . . H11 H 0.8968 1.2398 0.1011 0.052 Uiso 1 1 calc R . . C12 C 0.9624(4) 1.0911(5) 0.0990(3) 0.0396(14) Uani 1 1 d . . . H12 H 1.0135 1.1301 0.1038 0.048 Uiso 1 1 calc R . . C13 C 0.9578(3) 0.9692(4) 0.0937(3) 0.0270(11) Uani 1 1 d . . . C14 C 1.1010(3) 0.9522(5) 0.1029(3) 0.0429(15) Uani 1 1 d . . . H14A H 1.0930 1.0146 0.0640 0.064 Uiso 1 1 calc R . . H14B H 1.1402 0.8932 0.0962 0.064 Uiso 1 1 calc R . . H14C H 1.1239 0.9864 0.1550 0.064 Uiso 1 1 calc R . . C15 C 0.9260(3) 0.5445(4) 0.0064(3) 0.0196(10) Uani 1 1 d . . . C16 C 0.9940(3) 0.6197(4) 0.0160(3) 0.0231(11) Uani 1 1 d . . . H16 H 0.9902 0.7010 0.0269 0.028 Uiso 1 1 calc R . . C17 C 0.9331(3) 0.4259(4) -0.0095(3) 0.0251(11) Uani 1 1 d . . . H17 H 0.8867 0.3749 -0.0160 0.030 Uiso 1 1 calc R . . C18 C 0.6597(3) 0.4189(5) -0.1001(3) 0.0315(12) Uani 1 1 d . . . C19 C 0.6336(4) 0.5051(5) -0.1552(3) 0.0431(14) Uani 1 1 d . . . H19 H 0.6721 0.5642 -0.1582 0.052 Uiso 1 1 calc R . . C20 C 0.5516(4) 0.5075(6) -0.2070(3) 0.0544(17) Uani 1 1 d . . . H20 H 0.5330 0.5684 -0.2446 0.065 Uiso 1 1 calc R . . C21 C 0.4979(4) 0.4185(6) -0.2020(4) 0.0528(17) Uani 1 1 d . . . H21 H 0.4416 0.4188 -0.2370 0.063 Uiso 1 1 calc R . . C22 C 0.5236(3) 0.3291(5) -0.1478(3) 0.0402(14) Uani 1 1 d . . . H22 H 0.4854 0.2688 -0.1461 0.048 Uiso 1 1 calc R . . C23 C 0.6068(3) 0.3277(5) -0.0950(3) 0.0363(13) Uani 1 1 d . . . C24 C 0.5929(3) 0.1410(5) -0.0425(4) 0.0520(17) Uani 1 1 d . . . H24A H 0.5389 0.1589 -0.0365 0.078 Uiso 1 1 calc R . . H24B H 0.6249 0.0871 -0.0012 0.078 Uiso 1 1 calc R . . H24C H 0.5831 0.1039 -0.0932 0.078 Uiso 1 1 calc R . . C25 C 0.8426(3) 0.4570(4) 0.1713(3) 0.0341(13) Uani 1 1 d . A . C26 C 0.9075(3) 0.5363(5) 0.1980(3) 0.0399(14) Uani 1 1 d . . . H26 H 0.9283 0.5757 0.1626 0.048 Uiso 1 1 calc R . . C27 C 0.9423(3) 0.5583(6) 0.2769(3) 0.0475(16) Uani 1 1 d . . . H27 H 0.9872 0.6130 0.2954 0.057 Uiso 1 1 calc R . . C28 C 0.9130(4) 0.5022(6) 0.3287(4) 0.0536(18) Uani 1 1 d . . . H28 H 0.9373 0.5179 0.3827 0.064 Uiso 1 1 calc R . . C29 C 0.8473(4) 0.4221(5) 0.3017(4) 0.0489(16) Uani 1 1 d . A . H29 H 0.8273 0.3823 0.3375 0.059 Uiso 1 1 calc R . . C30 C 0.8110(4) 0.4002(5) 0.2230(4) 0.0429(15) Uani 1 1 d D . . C31 C 0.6994(10) 0.2763(13) 0.2345(9) 0.070(3) Uani 0.603(17) 1 d PDU A 1 H31A H 0.7425 0.2330 0.2753 0.104 Uiso 0.603(17) 1 calc PR A 1 H31B H 0.6564 0.2212 0.2035 0.104 Uiso 0.603(17) 1 calc PR A 1 H31C H 0.6734 0.3352 0.2582 0.104 Uiso 0.603(17) 1 calc PR A 1 C31A C 0.7439(16) 0.2372(18) 0.2584(13) 0.070(3) Uani 0.397(17) 1 d PDU A 2 H31D H 0.7970 0.2010 0.2904 0.104 Uiso 0.397(17) 1 calc PR A 2 H31E H 0.7030 0.1753 0.2340 0.104 Uiso 0.397(17) 1 calc PR A 2 H31F H 0.7223 0.2867 0.2911 0.104 Uiso 0.397(17) 1 calc PR A 2 C32 C 0.5742(3) 0.4693(5) 0.0546(3) 0.0350(13) Uani 1 1 d . . . H32 H 0.6251 0.4457 0.0935 0.042 Uiso 1 1 calc R . . C33 C 0.4978(3) 0.5956(5) -0.0435(3) 0.0365(13) Uani 1 1 d . . . H33 H 0.4947 0.6634 -0.0749 0.044 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 0.0200(2) 0.0200(2) 0.0452(3) -0.00356(19) 0.01927(18) -0.00243(17) Cl1 0.0238(6) 0.0257(6) 0.0560(9) -0.0057(6) 0.0183(6) 0.0014(6) P1 0.0179(6) 0.0180(7) 0.0338(8) -0.0009(6) 0.0125(6) -0.0016(5) P2 0.0205(6) 0.0186(6) 0.0453(8) -0.0029(6) 0.0192(6) -0.0038(5) O1 0.0243(18) 0.0237(18) 0.033(2) -0.0009(15) 0.0131(16) -0.0050(14) O2 0.029(2) 0.039(2) 0.041(2) -0.0018(17) 0.0174(17) 0.0026(16) O3 0.0188(17) 0.0184(17) 0.033(2) -0.0021(14) 0.0106(15) -0.0019(13) O4 0.0231(18) 0.035(2) 0.046(2) -0.0068(17) 0.0168(17) -0.0127(16) O5 0.0224(18) 0.0260(19) 0.059(2) -0.0157(17) 0.0202(18) -0.0048(15) O6 0.025(2) 0.027(2) 0.077(3) 0.001(2) 0.015(2) -0.0057(17) O7 0.037(2) 0.0209(18) 0.050(2) 0.0048(17) 0.0259(18) 0.0047(16) O8 0.067(5) 0.031(5) 0.061(4) 0.013(3) 0.038(4) 0.000(4) O8A 0.067(5) 0.031(5) 0.061(4) 0.013(3) 0.038(4) 0.000(4) N1 0.0166(19) 0.014(2) 0.037(2) 0.0010(17) 0.0128(18) -0.0013(16) N2 0.031(2) 0.030(3) 0.059(3) -0.006(2) 0.028(2) 0.002(2) C1 0.026(3) 0.021(2) 0.035(3) 0.003(2) 0.013(2) -0.001(2) C2 0.042(3) 0.043(3) 0.048(4) 0.006(3) 0.018(3) 0.013(3) C3 0.045(4) 0.064(4) 0.061(5) 0.010(4) 0.010(3) 0.019(3) C4 0.061(5) 0.075(5) 0.040(4) 0.008(3) 0.011(3) 0.017(4) C5 0.057(4) 0.053(4) 0.038(4) 0.004(3) 0.021(3) 0.004(3) C6 0.030(3) 0.024(3) 0.034(3) 0.003(2) 0.009(2) -0.005(2) C7 0.048(4) 0.068(5) 0.064(4) -0.019(4) 0.033(3) -0.001(3) C8 0.031(3) 0.018(3) 0.029(3) -0.003(2) 0.008(2) -0.004(2) C9 0.027(3) 0.028(3) 0.052(4) -0.012(3) 0.010(3) -0.005(2) C10 0.040(3) 0.030(3) 0.053(4) -0.011(3) -0.001(3) 0.009(3) C11 0.057(4) 0.018(3) 0.043(3) -0.001(3) 0.003(3) 0.002(3) C12 0.042(3) 0.027(3) 0.043(4) 0.000(3) 0.006(3) -0.012(3) C13 0.027(3) 0.025(3) 0.030(3) 0.003(2) 0.011(2) 0.002(2) C14 0.035(3) 0.045(4) 0.053(4) -0.003(3) 0.021(3) -0.019(3) C15 0.012(2) 0.024(3) 0.023(3) 0.002(2) 0.006(2) 0.0013(19) C16 0.017(2) 0.018(2) 0.035(3) -0.003(2) 0.010(2) -0.0014(19) C17 0.016(2) 0.025(3) 0.039(3) -0.005(2) 0.015(2) -0.005(2) C18 0.024(3) 0.032(3) 0.042(3) -0.017(3) 0.016(3) -0.003(2) C19 0.050(4) 0.040(4) 0.043(4) -0.007(3) 0.021(3) -0.009(3) C20 0.062(4) 0.068(5) 0.032(3) -0.004(3) 0.015(3) -0.003(4) C21 0.043(4) 0.064(5) 0.047(4) -0.017(3) 0.010(3) 0.001(3) C22 0.025(3) 0.040(3) 0.055(4) -0.015(3) 0.013(3) -0.005(3) C23 0.030(3) 0.028(3) 0.055(4) -0.009(3) 0.019(3) -0.001(2) C24 0.035(3) 0.028(3) 0.101(5) -0.003(3) 0.033(4) -0.011(3) C25 0.037(3) 0.022(3) 0.048(4) 0.009(3) 0.022(3) 0.016(2) C26 0.030(3) 0.047(4) 0.047(4) 0.009(3) 0.018(3) 0.008(3) C27 0.030(3) 0.070(5) 0.043(4) 0.000(3) 0.013(3) 0.008(3) C28 0.049(4) 0.068(5) 0.048(4) 0.011(3) 0.022(3) 0.032(4) C29 0.063(4) 0.042(4) 0.053(4) 0.020(3) 0.034(4) 0.024(3) C30 0.048(4) 0.028(3) 0.063(4) 0.003(3) 0.032(3) 0.004(3) C31 0.083(7) 0.064(6) 0.067(6) 0.021(4) 0.032(5) -0.018(5) C31A 0.083(7) 0.064(6) 0.067(6) 0.021(4) 0.032(5) -0.018(5) C32 0.022(3) 0.032(3) 0.057(4) -0.004(3) 0.023(3) 0.002(2) C33 0.028(3) 0.033(3) 0.051(4) -0.006(3) 0.018(3) 0.000(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 P2 2.1350(13) . ? Rh1 N2 2.165(4) . ? Rh1 P1 2.1790(12) . ? Rh1 Cl1 2.3763(13) . ? P1 O1 1.607(3) . ? P1 O3 1.616(3) . ? P1 N1 1.695(4) . ? P1 P2 2.4980(17) . ? P2 O5 1.608(3) . ? P2 O7 1.611(4) . ? P2 N1 1.702(4) . ? O1 C1 1.397(6) . ? O2 C6 1.356(6) . ? O2 C7 1.429(6) . ? O3 C8 1.418(5) . ? O4 C13 1.360(6) . ? O4 C14 1.437(5) . ? O5 C18 1.412(6) . ? O6 C23 1.353(6) . ? O6 C24 1.432(6) . ? O7 C25 1.415(6) . ? O8 C30 1.406(10) . ? O8 C31 1.451(11) . ? O8A C30 1.341(13) . ? O8A C31A 1.449(15) . ? N1 C15 1.439(5) . ? N2 C32 1.360(7) . ? N2 C33 1.371(7) . ? C1 C2 1.358(7) . ? C1 C6 1.397(7) . ? C2 C3 1.407(8) . ? C2 H2 0.9500 . ? C3 C4 1.362(9) . ? C3 H3 0.9500 . ? C4 C5 1.375(8) . ? C4 H4 0.9500 . ? C5 C6 1.380(7) . ? C5 H5 0.9500 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.380(7) . ? C8 C13 1.390(6) . ? C9 C10 1.399(7) . ? C9 H9 0.9500 . ? C10 C11 1.363(8) . ? C10 H10 0.9500 . ? C11 C12 1.384(8) . ? C11 H11 0.9500 . ? C12 C13 1.386(7) . ? C12 H12 0.9500 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C17 1.391(6) . ? C15 C16 1.395(6) . ? C16 C17 1.382(6) 3_765 ? C16 H16 0.9500 . ? C17 C16 1.382(6) 3_765 ? C17 H17 0.9500 . ? C18 C19 1.365(7) . ? C18 C23 1.392(7) . ? C19 C20 1.388(8) . ? C19 H19 0.9500 . ? C20 C21 1.384(9) . ? C20 H20 0.9500 . ? C21 C22 1.381(8) . ? C21 H21 0.9500 . ? C22 C23 1.410(7) . ? C22 H22 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.374(7) . ? C25 C30 1.397(7) . ? C26 C27 1.384(8) . ? C26 H26 0.9500 . ? C27 C28 1.369(8) . ? C27 H27 0.9500 . ? C28 C29 1.389(8) . ? C28 H28 0.9500 . ? C29 C30 1.382(8) . ? C29 H29 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C32 C33 1.380(7) 3_665 ? C32 H32 0.9500 . ? C33 C32 1.380(7) 3_665 ? C33 H33 0.9500 . ? 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 P2 Rh1 N2 98.49(11) . . ? P2 Rh1 P1 70.76(4) . . ? N2 Rh1 P1 167.94(11) . . ? P2 Rh1 Cl1 171.22(5) . . ? N2 Rh1 Cl1 88.01(11) . . ? P1 Rh1 Cl1 102.14(5) . . ? O1 P1 O3 95.61(17) . . ? O1 P1 N1 108.40(18) . . ? O3 P1 N1 102.41(18) . . ? O1 P1 Rh1 125.20(13) . . ? O3 P1 Rh1 126.16(13) . . ? N1 P1 Rh1 96.43(13) . . ? O1 P1 P2 133.22(14) . . ? O3 P1 P2 122.57(13) . . ? N1 P1 P2 42.76(12) . . ? Rh1 P1 P2 53.80(4) . . ? O5 P2 O7 95.11(19) . . ? O5 P2 N1 105.80(18) . . ? O7 P2 N1 104.88(18) . . ? O5 P2 Rh1 121.11(14) . . ? O7 P2 Rh1 129.58(14) . . ? N1 P2 Rh1 97.87(13) . . ? O5 P2 P1 128.16(15) . . ? O7 P2 P1 127.72(14) . . ? N1 P2 P1 42.56(13) . . ? Rh1 P2 P1 55.44(4) . . ? C1 O1 P1 125.2(3) . . ? C6 O2 C7 118.2(4) . . ? C8 O3 P1 120.6(3) . . ? C13 O4 C14 116.9(4) . . ? C18 O5 P2 117.9(3) . . ? C23 O6 C24 116.6(4) . . ? C25 O7 P2 123.6(3) . . ? C30 O8 C31 115.9(9) . . ? C30 O8A C31A 116.5(14) . . ? C15 N1 P1 136.2(3) . . ? C15 N1 P2 129.1(3) . . ? P1 N1 P2 94.68(18) . . ? C32 N2 C33 116.1(4) . . ? C32 N2 Rh1 123.0(3) . . ? C33 N2 Rh1 120.7(4) . . ? C2 C1 O1 122.3(5) . . ? C2 C1 C6 121.2(5) . . ? O1 C1 C6 116.3(4) . . ? C1 C2 C3 118.8(6) . . ? C1 C2 H2 120.6 . . ? C3 C2 H2 120.6 . . ? C4 C3 C2 120.2(6) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.7(6) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 120.0(6) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? O2 C6 C5 124.6(5) . . ? O2 C6 C1 116.4(4) . . ? C5 C6 C1 119.0(5) . . ? O2 C7 H7A 109.5 . . ? O2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 121.6(5) . . ? C9 C8 O3 121.2(4) . . ? C13 C8 O3 117.3(4) . . ? C8 C9 C10 119.1(5) . . ? C8 C9 H9 120.5 . . ? C10 C9 H9 120.5 . . ? C11 C10 C9 119.6(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 121.2(5) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C13 120.3(5) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? O4 C13 C12 125.0(5) . . ? O4 C13 C8 116.7(4) . . ? C12 C13 C8 118.3(5) . . ? O4 C14 H14A 109.5 . . ? O4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C17 C15 C16 119.4(4) . . ? C17 C15 N1 120.3(4) . . ? C16 C15 N1 120.4(4) . . ? C17 C16 C15 119.0(4) 3_765 . ? C17 C16 H16 120.5 3_765 . ? C15 C16 H16 120.5 . . ? C16 C17 C15 121.6(4) 3_765 . ? C16 C17 H17 119.2 3_765 . ? C15 C17 H17 119.2 . . ? C19 C18 C23 121.9(5) . . ? C19 C18 O5 122.6(5) . . ? C23 C18 O5 115.5(5) . . ? C18 C19 C20 121.0(6) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 117.8(6) . . ? C21 C20 H20 121.1 . . ? C19 C20 H20 121.1 . . ? C22 C21 C20 122.1(6) . . ? C22 C21 H21 119.0 . . ? C20 C21 H21 119.0 . . ? C21 C22 C23 119.8(5) . . ? C21 C22 H22 120.1 . . ? C23 C22 H22 120.1 . . ? O6 C23 C18 116.6(5) . . ? O6 C23 C22 125.9(5) . . ? C18 C23 C22 117.4(5) . . ? O6 C24 H24A 109.5 . . ? O6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 120.4(6) . . ? C26 C25 O7 122.6(5) . . ? C30 C25 O7 116.9(5) . . ? C25 C26 C27 119.5(5) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C28 C27 C26 120.9(6) . . ? C28 C27 H27 119.6 . . ? C26 C27 H27 119.6 . . ? C27 C28 C29 119.6(6) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 120.3(6) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? O8A C30 C29 119.6(9) . . ? O8A C30 C25 119.9(10) . . ? C29 C30 C25 119.2(6) . . ? O8A C30 O8 18.9(11) . . ? C29 C30 O8 128.0(7) . . ? C25 C30 O8 112.4(7) . . ? O8A C31A H31D 109.5 . . ? O8A C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? O8A C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? N2 C32 C33 121.3(5) . 3_665 ? N2 C32 H32 119.4 . . ? C33 C32 H32 119.4 3_665 . ? N2 C33 C32 122.7(5) . 3_665 ? N2 C33 H33 118.7 . . ? C32 C33 H33 118.7 3_665 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.83 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.338 _refine_diff_density_min -0.404 _refine_diff_density_rms 0.103