# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email brookhar@email.unc.edu _publ_contact_author_name 'Marc Walter' loop_ _publ_author_name 'Marc Walter' 'Peter White' 'Cynthia Schauer' 'Maurice Brookhart' data_IrMe _database_code_depnum_ccdc_archive 'CCDC 834658' #TrackingRef '- IrMe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H49 Ir N2 O2 P2' _chemical_formula_weight 759.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ir Ir -4.7710 6.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1882(3) _cell_length_b 12.8593(3) _cell_length_c 23.2460(6) _cell_angle_alpha 90.00 _cell_angle_beta 94.8910(10) _cell_angle_gamma 90.00 _cell_volume 3332.28(15) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9994 _cell_measurement_theta_min 3.82 _cell_measurement_theta_max 69.77 _exptl_crystal_description block _exptl_crystal_colour black _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 8.896 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.6174 _exptl_absorpt_correction_T_max 0.7762 _exptl_absorpt_process_details '(Bruker SADABS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22893 _diffrn_reflns_av_R_equivalents 0.0303 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 70.12 _reflns_number_total 6154 _reflns_number_gt 5415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0405P)^2^+0.0398P] 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 6154 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0641 _refine_ls_wR_factor_gt 0.0616 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 C1 C 0.9070(3) -0.1490(3) 0.39431(14) 0.0200(6) Uani 1 1 d . . . C2 C 0.9858(3) -0.0982(3) 0.44420(15) 0.0245(7) Uani 1 1 d . . . H2A H 0.9395 -0.0914 0.4780 0.037 Uiso 1 1 calc R . . H2B H 1.0114 -0.0292 0.4323 0.037 Uiso 1 1 calc R . . H2C H 1.0565 -0.1416 0.4541 0.037 Uiso 1 1 calc R . . C3 C 0.9838(3) -0.1635(3) 0.34312(15) 0.0296(8) Uani 1 1 d . . . H3A H 1.0101 -0.0953 0.3301 0.044 Uiso 1 1 calc R . . H3B H 0.9362 -0.1982 0.3114 0.044 Uiso 1 1 calc R . . H3C H 1.0542 -0.2060 0.3552 0.044 Uiso 1 1 calc R . . C4 C 0.8626(3) -0.2541(3) 0.41416(16) 0.0304(8) Uani 1 1 d . . . H4A H 0.9314 -0.2970 0.4282 0.046 Uiso 1 1 calc R . . H4B H 0.8177 -0.2892 0.3817 0.046 Uiso 1 1 calc R . . H4C H 0.8102 -0.2436 0.4454 0.046 Uiso 1 1 calc R . . C5 C 0.6551(3) -0.1097(3) 0.33126(15) 0.0231(7) Uani 1 1 d . . . C6 C 0.5717(3) -0.0169(3) 0.31611(17) 0.0344(9) Uani 1 1 d . . . H6A H 0.6141 0.0348 0.2945 0.052 Uiso 1 1 calc R . . H6B H 0.5475 0.0146 0.3517 0.052 Uiso 1 1 calc R . . H6C H 0.5003 -0.0409 0.2925 0.052 Uiso 1 1 calc R . . C7 C 0.6970(3) -0.1560(3) 0.27581(16) 0.0352(9) Uani 1 1 d . . . H7A H 0.7438 -0.2191 0.2851 0.053 Uiso 1 1 calc R . . H7B H 0.7469 -0.1052 0.2575 0.053 Uiso 1 1 calc R . . H7C H 0.6270 -0.1734 0.2493 0.053 Uiso 1 1 calc R . . C8 C 0.5849(3) -0.1903(3) 0.36335(17) 0.0392(10) Uani 1 1 d . . . H8A H 0.5146 -0.2130 0.3385 0.059 Uiso 1 1 calc R . . H8B H 0.5586 -0.1591 0.3986 0.059 Uiso 1 1 calc R . . H8C H 0.6365 -0.2503 0.3735 0.059 Uiso 1 1 calc R . . C9 C 0.7280(2) 0.0508(2) 0.46478(13) 0.0164(6) Uani 1 1 d . . . C10 C 0.6944(3) 0.0609(2) 0.52087(13) 0.0168(6) Uani 1 1 d . . . C11 C 0.6708(3) -0.0290(2) 0.55825(13) 0.0167(6) Uani 1 1 d . . . C12 C 0.6001(3) -0.1128(2) 0.53917(14) 0.0205(6) Uani 1 1 d . . . H12 H 0.5671 -0.1158 0.5002 0.025 Uiso 1 1 calc R . . C13 C 0.5778(3) -0.1923(3) 0.57708(15) 0.0228(7) Uani 1 1 d . . . H13 H 0.5278 -0.2487 0.5641 0.027 Uiso 1 1 calc R . . C14 C 0.6278(3) -0.1902(3) 0.63369(14) 0.0224(7) Uani 1 1 d . . . H14 H 0.6124 -0.2452 0.6593 0.027 Uiso 1 1 calc R . . C15 C 0.7006(3) -0.1075(3) 0.65295(15) 0.0241(7) Uani 1 1 d . . . H15 H 0.7364 -0.1064 0.6915 0.029 Uiso 1 1 calc R . . C16 C 0.7206(3) -0.0264(3) 0.61543(14) 0.0211(7) Uani 1 1 d . . . H16 H 0.7684 0.0312 0.6288 0.025 Uiso 1 1 calc R . . C17 C 0.7146(3) 0.2401(2) 0.51427(13) 0.0182(6) Uani 1 1 d . . . C18 C 0.6967(3) 0.3416(3) 0.54291(14) 0.0203(6) Uani 1 1 d . . . C19 C 0.6987(3) 0.3444(3) 0.60315(15) 0.0269(7) Uani 1 1 d . . . H19 H 0.7168 0.2828 0.6247 0.032 Uiso 1 1 calc R . . C20 C 0.6749(3) 0.4347(3) 0.63151(16) 0.0319(8) Uani 1 1 d . . . H20 H 0.6781 0.4354 0.6725 0.038 Uiso 1 1 calc R . . C21 C 0.6464(3) 0.5246(3) 0.60081(17) 0.0303(8) Uani 1 1 d . . . H21 H 0.6286 0.5867 0.6205 0.036 Uiso 1 1 calc R . . C22 C 0.6441(3) 0.5238(3) 0.54078(16) 0.0279(8) Uani 1 1 d . . . H22 H 0.6250 0.5856 0.5196 0.033 Uiso 1 1 calc R . . C23 C 0.6694(3) 0.4335(3) 0.51199(15) 0.0240(7) Uani 1 1 d . . . H23 H 0.6682 0.4336 0.4711 0.029 Uiso 1 1 calc R . . C24 C 0.7571(3) 0.2282(2) 0.45975(13) 0.0177(6) Uani 1 1 d . . . C25 C 1.0044(3) 0.3469(3) 0.38368(14) 0.0215(7) Uani 1 1 d . . . C26 C 1.0718(3) 0.2691(3) 0.42512(15) 0.0292(8) Uani 1 1 d . . . H26A H 1.1539 0.2939 0.4349 0.044 Uiso 1 1 calc R . . H26B H 1.0742 0.2010 0.4064 0.044 Uiso 1 1 calc R . . H26C H 1.0302 0.2630 0.4604 0.044 Uiso 1 1 calc R . . C27 C 1.0045(3) 0.4533(3) 0.41352(17) 0.0341(9) Uani 1 1 d . . . H27A H 1.0865 0.4710 0.4286 0.051 Uiso 1 1 calc R . . H27B H 0.9527 0.4506 0.4454 0.051 Uiso 1 1 calc R . . H27C H 0.9745 0.5062 0.3856 0.051 Uiso 1 1 calc R . . C28 C 1.0667(3) 0.3518(3) 0.32781(15) 0.0297(8) Uani 1 1 d . . . H28A H 1.0245 0.4012 0.3012 0.045 Uiso 1 1 calc R . . H28B H 1.0658 0.2827 0.3100 0.045 Uiso 1 1 calc R . . H28C H 1.1499 0.3746 0.3364 0.045 Uiso 1 1 calc R . . C29 C 0.7506(3) 0.3711(3) 0.31902(15) 0.0229(7) Uani 1 1 d . . . C30 C 0.7576(3) 0.4874(3) 0.33140(18) 0.0363(9) Uani 1 1 d . . . H30A H 0.6918 0.5230 0.3089 0.055 Uiso 1 1 calc R . . H30B H 0.8345 0.5145 0.3207 0.055 Uiso 1 1 calc R . . H30C H 0.7511 0.4995 0.3726 0.055 Uiso 1 1 calc R . . C31 C 0.7745(3) 0.3496(3) 0.25612(15) 0.0354(9) Uani 1 1 d . . . H31A H 0.7645 0.2752 0.2480 0.053 Uiso 1 1 calc R . . H31B H 0.8566 0.3706 0.2499 0.053 Uiso 1 1 calc R . . H31C H 0.7176 0.3893 0.2303 0.053 Uiso 1 1 calc R . . C32 C 0.6242(3) 0.3318(3) 0.32789(16) 0.0311(8) Uani 1 1 d . . . H32A H 0.6052 0.3478 0.3673 0.047 Uiso 1 1 calc R . . H32B H 0.6206 0.2564 0.3218 0.047 Uiso 1 1 calc R . . H32C H 0.5660 0.3661 0.3003 0.047 Uiso 1 1 calc R . . C33 C 0.9198(3) 0.0941(3) 0.28077(15) 0.0276(8) Uani 1 1 d . . . H33A H 1.0053 0.0797 0.2900 0.041 Uiso 1 1 calc R . . H33B H 0.9106 0.1575 0.2574 0.041 Uiso 1 1 calc R . . H33C H 0.8825 0.0356 0.2591 0.041 Uiso 1 1 calc R . . N1 N 0.7642(2) 0.13353(19) 0.43445(11) 0.0152(5) Uani 1 1 d . . . N2 N 0.6876(2) 0.1557(2) 0.54431(11) 0.0185(5) Uani 1 1 d . . . O1 O 0.72906(18) -0.04331(17) 0.43918(9) 0.0190(4) Uani 1 1 d . . . O2 O 0.79576(19) 0.31029(17) 0.43055(9) 0.0191(4) Uani 1 1 d . . . P1 P 0.78783(7) -0.05105(6) 0.37428(3) 0.01662(15) Uani 1 1 d . . . P2 P 0.85380(7) 0.28683(6) 0.36636(3) 0.01738(16) Uani 1 1 d . . . Ir1 Ir 0.836125(11) 0.114647(10) 0.357830(5) 0.01675(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0199(15) 0.0194(16) 0.0206(15) -0.0008(13) 0.0010(13) 0.0041(12) C2 0.0236(16) 0.0250(18) 0.0241(17) -0.0008(14) -0.0031(14) 0.0016(13) C3 0.0259(17) 0.036(2) 0.0269(18) -0.0013(16) 0.0037(14) 0.0108(15) C4 0.0346(19) 0.0229(18) 0.033(2) 0.0017(15) -0.0014(16) 0.0015(14) C5 0.0147(14) 0.0290(18) 0.0254(17) -0.0063(14) 0.0005(13) -0.0012(12) C6 0.0199(16) 0.039(2) 0.043(2) -0.0137(18) -0.0070(16) 0.0040(15) C7 0.0252(17) 0.050(2) 0.0290(19) -0.0180(18) -0.0028(15) -0.0007(16) C8 0.0307(19) 0.046(2) 0.042(2) -0.0111(19) 0.0058(17) -0.0178(17) C9 0.0127(13) 0.0177(15) 0.0189(15) 0.0020(12) 0.0021(11) -0.0007(11) C10 0.0126(13) 0.0203(16) 0.0177(14) -0.0013(13) 0.0021(11) -0.0009(11) C11 0.0128(13) 0.0171(16) 0.0211(15) 0.0003(12) 0.0062(12) 0.0023(11) C12 0.0179(14) 0.0221(16) 0.0219(16) -0.0014(13) 0.0047(12) 0.0012(12) C13 0.0207(15) 0.0195(16) 0.0292(17) -0.0022(14) 0.0071(13) -0.0004(12) C14 0.0232(15) 0.0201(17) 0.0253(17) 0.0038(13) 0.0110(13) 0.0027(13) C15 0.0231(16) 0.0285(19) 0.0210(16) 0.0025(14) 0.0039(13) 0.0029(13) C16 0.0189(15) 0.0217(17) 0.0232(16) -0.0021(13) 0.0041(13) -0.0009(12) C17 0.0157(14) 0.0198(16) 0.0195(16) -0.0011(13) 0.0030(12) 0.0016(11) C18 0.0145(13) 0.0215(16) 0.0255(16) -0.0047(14) 0.0041(12) -0.0011(12) C19 0.0293(17) 0.0266(18) 0.0259(17) 0.0006(15) 0.0076(14) -0.0015(14) C20 0.0330(19) 0.035(2) 0.0283(19) -0.0107(16) 0.0096(15) -0.0042(16) C21 0.0244(17) 0.0234(19) 0.044(2) -0.0116(16) 0.0088(16) 0.0005(14) C22 0.0249(16) 0.0192(17) 0.040(2) -0.0021(15) 0.0045(15) 0.0026(13) C23 0.0227(16) 0.0243(18) 0.0252(17) -0.0002(14) 0.0023(13) 0.0016(13) C24 0.0132(13) 0.0188(16) 0.0212(16) -0.0017(13) 0.0029(12) 0.0004(11) C25 0.0143(14) 0.0266(17) 0.0243(16) 0.0033(14) 0.0050(12) 0.0006(12) C26 0.0228(17) 0.036(2) 0.0283(18) 0.0107(16) -0.0021(14) -0.0041(14) C27 0.0221(17) 0.033(2) 0.047(2) -0.0099(18) 0.0040(16) -0.0044(15) C28 0.0220(16) 0.041(2) 0.0271(18) 0.0016(16) 0.0068(14) -0.0074(15) C29 0.0187(15) 0.0271(19) 0.0230(16) 0.0086(14) 0.0026(13) 0.0037(13) C30 0.038(2) 0.024(2) 0.046(2) 0.0093(17) -0.0038(18) 0.0031(15) C31 0.0285(18) 0.053(3) 0.0239(18) 0.0087(18) -0.0001(15) 0.0075(17) C32 0.0198(16) 0.042(2) 0.0315(19) 0.0106(17) 0.0020(14) 0.0032(15) C33 0.0380(19) 0.0257(19) 0.0204(16) -0.0023(14) 0.0101(15) 0.0002(15) N1 0.0142(11) 0.0176(13) 0.0141(12) -0.0004(10) 0.0033(10) -0.0006(9) N2 0.0166(12) 0.0198(13) 0.0194(13) -0.0006(11) 0.0042(10) 0.0011(10) O1 0.0200(10) 0.0194(11) 0.0185(11) -0.0024(9) 0.0067(9) -0.0032(8) O2 0.0208(10) 0.0182(11) 0.0194(11) 0.0003(9) 0.0078(9) 0.0002(8) P1 0.0152(3) 0.0189(4) 0.0161(4) -0.0024(3) 0.0032(3) 0.0000(3) P2 0.0160(3) 0.0190(4) 0.0175(4) 0.0026(3) 0.0037(3) 0.0004(3) Ir1 0.01667(8) 0.01883(8) 0.01526(8) 0.00001(5) 0.00433(5) 0.00013(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C4 1.525(5) . ? C1 C3 1.537(4) . ? C1 C2 1.541(4) . ? C1 P1 1.864(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.529(5) . ? C5 C8 1.532(5) . ? C5 C6 1.538(5) . ? C5 P1 1.877(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O1 1.349(4) . ? C9 N1 1.358(4) . ? C9 C10 1.394(4) . ? C10 N2 1.340(4) . ? C10 C11 1.482(4) . ? C11 C12 1.388(4) . ? C11 C16 1.397(4) . ? C12 C13 1.386(5) . ? C12 H12 0.9500 . ? C13 C14 1.386(5) . ? C13 H13 0.9500 . ? C14 C15 1.390(5) . ? C14 H14 0.9500 . ? C15 C16 1.389(5) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N2 1.339(4) . ? C17 C24 1.399(4) . ? C17 C18 1.487(4) . ? C18 C19 1.399(5) . ? C18 C23 1.402(5) . ? C19 C20 1.373(5) . ? C19 H19 0.9500 . ? C20 C21 1.382(5) . ? C20 H20 0.9500 . ? C21 C22 1.393(5) . ? C21 H21 0.9500 . ? C22 C23 1.382(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O2 1.346(4) . ? C24 N1 1.358(4) . ? C25 C28 1.527(4) . ? C25 C27 1.533(5) . ? C25 C26 1.541(4) . ? C25 P2 1.867(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C30 1.524(5) . ? C29 C32 1.532(4) . ? C29 C31 1.534(5) . ? C29 P2 1.871(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 Ir1 2.107(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? N1 Ir1 2.030(3) . ? O1 P1 1.699(2) . ? O2 P2 1.704(2) . ? P1 Ir1 2.2391(8) . ? P2 Ir1 2.2302(8) . ? 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 C4 C1 C3 110.2(3) . . ? C4 C1 C2 109.2(3) . . ? C3 C1 C2 108.2(3) . . ? C4 C1 P1 115.5(2) . . ? C3 C1 P1 108.9(2) . . ? C2 C1 P1 104.6(2) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 C8 110.7(3) . . ? C7 C5 C6 109.4(3) . . ? C8 C5 C6 108.1(3) . . ? C7 C5 P1 108.7(2) . . ? C8 C5 P1 115.3(2) . . ? C6 C5 P1 104.3(2) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 N1 117.4(3) . . ? O1 C9 C10 120.7(3) . . ? N1 C9 C10 121.9(3) . . ? N2 C10 C9 119.6(3) . . ? N2 C10 C11 116.8(3) . . ? C9 C10 C11 123.4(3) . . ? C12 C11 C16 119.5(3) . . ? C12 C11 C10 122.9(3) . . ? C16 C11 C10 117.6(3) . . ? C13 C12 C11 119.9(3) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C12 C13 C14 120.7(3) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C13 C14 C15 119.9(3) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 119.6(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C11 120.5(3) . . ? C15 C16 H16 119.8 . . ? C11 C16 H16 119.8 . . ? N2 C17 C24 119.6(3) . . ? N2 C17 C18 115.7(3) . . ? C24 C17 C18 124.7(3) . . ? C19 C18 C23 118.4(3) . . ? C19 C18 C17 118.6(3) . . ? C23 C18 C17 122.8(3) . . ? C20 C19 C18 121.0(4) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C22 119.6(3) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.3(3) . . ? C23 C22 H22 119.9 . . ? C21 C22 H22 119.9 . . ? C22 C23 C18 120.3(3) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? O2 C24 N1 116.8(3) . . ? O2 C24 C17 121.3(3) . . ? N1 C24 C17 121.8(3) . . ? C28 C25 C27 111.5(3) . . ? C28 C25 C26 108.9(3) . . ? C27 C25 C26 108.4(3) . . ? C28 C25 P2 107.6(2) . . ? C27 C25 P2 115.6(2) . . ? C26 C25 P2 104.5(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C30 C29 C32 109.4(3) . . ? C30 C29 C31 110.3(3) . . ? C32 C29 C31 107.9(3) . . ? C30 C29 P2 116.0(2) . . ? C32 C29 P2 105.1(2) . . ? C31 C29 P2 107.9(2) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Ir1 C33 H33A 109.5 . . ? Ir1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Ir1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C24 N1 C9 116.6(3) . . ? C24 N1 Ir1 122.0(2) . . ? C9 N1 Ir1 121.3(2) . . ? C17 N2 C10 120.2(3) . . ? C9 O1 P1 117.6(2) . . ? C24 O2 P2 117.7(2) . . ? O1 P1 C1 98.08(13) . . ? O1 P1 C5 98.52(13) . . ? C1 P1 C5 112.21(15) . . ? O1 P1 Ir1 102.31(8) . . ? C1 P1 Ir1 120.52(11) . . ? C5 P1 Ir1 118.89(11) . . ? O2 P2 C25 98.18(13) . . ? O2 P2 C29 98.65(13) . . ? C25 P2 C29 112.79(15) . . ? O2 P2 Ir1 102.48(8) . . ? C25 P2 Ir1 120.13(11) . . ? C29 P2 Ir1 118.50(11) . . ? N1 Ir1 C33 176.93(12) . . ? N1 Ir1 P2 80.91(7) . . ? C33 Ir1 P2 99.06(10) . . ? N1 Ir1 P1 81.06(7) . . ? C33 Ir1 P1 99.04(10) . . ? P2 Ir1 P1 161.88(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 O1 C9 C10 N2 -176.4(2) . . . . ? N1 C9 C10 N2 5.7(4) . . . . ? O1 C9 C10 C11 6.9(4) . . . . ? N1 C9 C10 C11 -171.1(3) . . . . ? N2 C10 C11 C12 136.3(3) . . . . ? C9 C10 C11 C12 -46.9(4) . . . . ? N2 C10 C11 C16 -42.2(4) . . . . ? C9 C10 C11 C16 134.6(3) . . . . ? C16 C11 C12 C13 1.1(5) . . . . ? C10 C11 C12 C13 -177.4(3) . . . . ? C11 C12 C13 C14 -1.5(5) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C13 C14 C15 C16 1.3(5) . . . . ? C14 C15 C16 C11 -1.8(5) . . . . ? C12 C11 C16 C15 0.6(5) . . . . ? C10 C11 C16 C15 179.1(3) . . . . ? N2 C17 C18 C19 23.7(4) . . . . ? C24 C17 C18 C19 -155.9(3) . . . . ? N2 C17 C18 C23 -151.6(3) . . . . ? C24 C17 C18 C23 28.8(5) . . . . ? C23 C18 C19 C20 -0.2(5) . . . . ? C17 C18 C19 C20 -175.7(3) . . . . ? C18 C19 C20 C21 1.1(5) . . . . ? C19 C20 C21 C22 -1.2(5) . . . . ? C20 C21 C22 C23 0.4(5) . . . . ? C21 C22 C23 C18 0.5(5) . . . . ? C19 C18 C23 C22 -0.6(5) . . . . ? C17 C18 C23 C22 174.7(3) . . . . ? N2 C17 C24 O2 -173.7(3) . . . . ? C18 C17 C24 O2 5.9(5) . . . . ? N2 C17 C24 N1 4.6(4) . . . . ? C18 C17 C24 N1 -175.7(3) . . . . ? O2 C24 N1 C9 178.4(2) . . . . ? C17 C24 N1 C9 0.0(4) . . . . ? O2 C24 N1 Ir1 2.6(4) . . . . ? C17 C24 N1 Ir1 -175.8(2) . . . . ? O1 C9 N1 C24 176.9(2) . . . . ? C10 C9 N1 C24 -5.0(4) . . . . ? O1 C9 N1 Ir1 -7.2(3) . . . . ? C10 C9 N1 Ir1 170.8(2) . . . . ? C24 C17 N2 C10 -4.1(4) . . . . ? C18 C17 N2 C10 176.3(2) . . . . ? C9 C10 N2 C17 -0.9(4) . . . . ? C11 C10 N2 C17 176.1(3) . . . . ? N1 C9 O1 P1 5.6(3) . . . . ? C10 C9 O1 P1 -172.4(2) . . . . ? N1 C24 O2 P2 -2.1(3) . . . . ? C17 C24 O2 P2 176.3(2) . . . . ? C9 O1 P1 C1 121.9(2) . . . . ? C9 O1 P1 C5 -124.0(2) . . . . ? C9 O1 P1 Ir1 -1.9(2) . . . . ? C4 C1 P1 O1 60.7(3) . . . . ? C3 C1 P1 O1 -174.8(2) . . . . ? C2 C1 P1 O1 -59.3(2) . . . . ? C4 C1 P1 C5 -42.0(3) . . . . ? C3 C1 P1 C5 82.5(3) . . . . ? C2 C1 P1 C5 -162.0(2) . . . . ? C4 C1 P1 Ir1 170.2(2) . . . . ? C3 C1 P1 Ir1 -65.3(2) . . . . ? C2 C1 P1 Ir1 50.2(2) . . . . ? C7 C5 P1 O1 -162.5(3) . . . . ? C8 C5 P1 O1 -37.5(3) . . . . ? C6 C5 P1 O1 80.9(3) . . . . ? C7 C5 P1 C1 -60.1(3) . . . . ? C8 C5 P1 C1 64.9(3) . . . . ? C6 C5 P1 C1 -176.7(2) . . . . ? C7 C5 P1 Ir1 88.3(3) . . . . ? C8 C5 P1 Ir1 -146.7(2) . . . . ? C6 C5 P1 Ir1 -28.3(3) . . . . ? C24 O2 P2 C25 -122.7(2) . . . . ? C24 O2 P2 C29 122.7(2) . . . . ? C24 O2 P2 Ir1 0.8(2) . . . . ? C28 C25 P2 O2 -170.4(2) . . . . ? C27 C25 P2 O2 -45.1(3) . . . . ? C26 C25 P2 O2 73.9(2) . . . . ? C28 C25 P2 C29 -67.4(3) . . . . ? C27 C25 P2 C29 57.9(3) . . . . ? C26 C25 P2 C29 176.9(2) . . . . ? C28 C25 P2 Ir1 80.0(2) . . . . ? C27 C25 P2 Ir1 -154.7(2) . . . . ? C26 C25 P2 Ir1 -35.7(3) . . . . ? C30 C29 P2 O2 64.1(3) . . . . ? C32 C29 P2 O2 -56.7(3) . . . . ? C31 C29 P2 O2 -171.6(2) . . . . ? C30 C29 P2 C25 -38.6(3) . . . . ? C32 C29 P2 C25 -159.4(2) . . . . ? C31 C29 P2 C25 85.7(3) . . . . ? C30 C29 P2 Ir1 173.5(2) . . . . ? C32 C29 P2 Ir1 52.6(3) . . . . ? C31 C29 P2 Ir1 -62.3(3) . . . . ? C24 N1 Ir1 C33 88(2) . . . . ? C9 N1 Ir1 C33 -87(2) . . . . ? C24 N1 Ir1 P2 -1.6(2) . . . . ? C9 N1 Ir1 P2 -177.2(2) . . . . ? C24 N1 Ir1 P1 -179.8(2) . . . . ? C9 N1 Ir1 P1 4.6(2) . . . . ? O2 P2 Ir1 N1 0.35(10) . . . . ? C25 P2 Ir1 N1 107.62(14) . . . . ? C29 P2 Ir1 N1 -106.82(14) . . . . ? O2 P2 Ir1 C33 -176.54(13) . . . . ? C25 P2 Ir1 C33 -69.28(16) . . . . ? C29 P2 Ir1 C33 76.28(16) . . . . ? O2 P2 Ir1 P1 6.13(13) . . . . ? C25 P2 Ir1 P1 113.40(14) . . . . ? C29 P2 Ir1 P1 -101.04(15) . . . . ? O1 P1 Ir1 N1 -1.24(10) . . . . ? C1 P1 Ir1 N1 -108.44(14) . . . . ? C5 P1 Ir1 N1 105.83(14) . . . . ? O1 P1 Ir1 C33 175.66(13) . . . . ? C1 P1 Ir1 C33 68.46(16) . . . . ? C5 P1 Ir1 C33 -77.27(16) . . . . ? O1 P1 Ir1 P2 -7.02(13) . . . . ? C1 P1 Ir1 P2 -114.21(14) . . . . ? C5 P1 Ir1 P2 100.05(15) . . . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 70.12 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 0.985 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.095 # Attachment '- PdMe.cif' data_PdMe _database_code_depnum_ccdc_archive 'CCDC 834659' #TrackingRef '- PdMe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H56 B Cl2 F24 N O2 P2 Pd' _chemical_formula_weight 1469.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7687(5) _cell_length_b 23.5697(9) _cell_length_c 19.7027(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.591(2) _cell_angle_gamma 90.00 _cell_volume 6322.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4193 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 69.79 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.543 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 4.631 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.3372 _exptl_absorpt_correction_T_max 0.8015 _exptl_absorpt_process_details '(Bruker SADABS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59378 _diffrn_reflns_av_R_equivalents 0.0310 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 70.14 _reflns_number_total 11956 _reflns_number_gt 10879 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0703P)^2^+12.2747P] 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 11956 _refine_ls_number_parameters 806 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0502 _refine_ls_R_factor_gt 0.0463 _refine_ls_wR_factor_ref 0.1273 _refine_ls_wR_factor_gt 0.1241 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0229(3) 0.42758(14) 0.73004(19) 0.0342(8) Uani 1 1 d . . . C2 C 0.9438(4) 0.40874(17) 0.6717(2) 0.0555(12) Uani 1 1 d . . . H2A H 0.9531 0.3686 0.6616 0.083 Uiso 1 1 calc R . . H2B H 0.9487 0.4314 0.6306 0.083 Uiso 1 1 calc R . . H2C H 0.8788 0.4142 0.6853 0.083 Uiso 1 1 calc R . . C3 C 1.0187(3) 0.38959(15) 0.7928(2) 0.0412(9) Uani 1 1 d . . . H3A H 0.9541 0.3932 0.8076 0.062 Uiso 1 1 calc R . . H3B H 1.0698 0.4013 0.8303 0.062 Uiso 1 1 calc R . . H3C H 1.0295 0.3500 0.7807 0.062 Uiso 1 1 calc R . . C4 C 1.1245(4) 0.42314(19) 0.7071(3) 0.0594(13) Uani 1 1 d . . . H4A H 1.1345 0.3844 0.6915 0.089 Uiso 1 1 calc R . . H4B H 1.1754 0.4324 0.7458 0.089 Uiso 1 1 calc R . . H4C H 1.1283 0.4498 0.6694 0.089 Uiso 1 1 calc R . . C5 C 1.1251(3) 0.50489(18) 0.8710(2) 0.0516(11) Uani 1 1 d . . . H5A H 1.1635 0.4728 0.8577 0.077 Uiso 1 1 calc R . . H5B H 1.0694 0.4906 0.8916 0.077 Uiso 1 1 calc R . . H5C H 1.1668 0.5285 0.9044 0.077 Uiso 1 1 calc R . . C6 C 1.0870(3) 0.54042(15) 0.80719(19) 0.0343(8) Uani 1 1 d . . . C7 C 1.1729(3) 0.55799(18) 0.7703(3) 0.0508(11) Uani 1 1 d . . . H7A H 1.2202 0.5803 0.8017 0.076 Uiso 1 1 calc R . . H7B H 1.1481 0.5809 0.7300 0.076 Uiso 1 1 calc R . . H7C H 1.2053 0.5240 0.7559 0.076 Uiso 1 1 calc R . . C8 C 1.0349(3) 0.59406(17) 0.8283(2) 0.0475(10) Uani 1 1 d . . . H8A H 1.0822 0.6178 0.8577 0.071 Uiso 1 1 calc R . . H8B H 0.9817 0.5831 0.8536 0.071 Uiso 1 1 calc R . . H8C H 1.0076 0.6154 0.7872 0.071 Uiso 1 1 calc R . . C9 C 0.8219(2) 0.52882(13) 0.77503(16) 0.0237(6) Uani 1 1 d . . . C10 C 0.7526(2) 0.53047(13) 0.81853(16) 0.0268(6) Uani 1 1 d . . . H10 H 0.7591 0.5079 0.8589 0.032 Uiso 1 1 calc R . . C11 C 0.6729(2) 0.56624(14) 0.80139(17) 0.0275(7) Uani 1 1 d . . . H11 H 0.6240 0.5684 0.8306 0.033 Uiso 1 1 calc R . . C12 C 0.6632(2) 0.59900(13) 0.74241(16) 0.0253(6) Uani 1 1 d . . . H12 H 0.6092 0.6241 0.7309 0.030 Uiso 1 1 calc R . . C13 C 0.7351(2) 0.59374(13) 0.70119(15) 0.0218(6) Uani 1 1 d . . . C14 C 0.7267(3) 0.57393(17) 0.51712(18) 0.0358(8) Uani 1 1 d . . . C15 C 0.6853(3) 0.52240(18) 0.5512(2) 0.0487(10) Uani 1 1 d . . . H15A H 0.6429 0.5355 0.5838 0.073 Uiso 1 1 calc R . . H15B H 0.7396 0.5000 0.5756 0.073 Uiso 1 1 calc R . . H15C H 0.6470 0.4988 0.5159 0.073 Uiso 1 1 calc R . . C16 C 0.7914(4) 0.5523(2) 0.4655(2) 0.0601(13) Uani 1 1 d . . . H16A H 0.7514 0.5297 0.4300 0.090 Uiso 1 1 calc R . . H16B H 0.8443 0.5287 0.4894 0.090 Uiso 1 1 calc R . . H16C H 0.8197 0.5846 0.4441 0.090 Uiso 1 1 calc R . . C17 C 0.6415(3) 0.6100(2) 0.4822(2) 0.0573(12) Uani 1 1 d . . . H17A H 0.6671 0.6408 0.4565 0.086 Uiso 1 1 calc R . . H17B H 0.6056 0.6261 0.5171 0.086 Uiso 1 1 calc R . . H17C H 0.5970 0.5863 0.4506 0.086 Uiso 1 1 calc R . . C18 C 0.8386(2) 0.68498(14) 0.56652(18) 0.0300(7) Uani 1 1 d . . . C19 C 0.9128(3) 0.70401(16) 0.6281(2) 0.0434(9) Uani 1 1 d . . . H19A H 0.9325 0.7433 0.6213 0.065 Uiso 1 1 calc R . . H19B H 0.9707 0.6794 0.6324 0.065 Uiso 1 1 calc R . . H19C H 0.8826 0.7015 0.6700 0.065 Uiso 1 1 calc R . . C20 C 0.8879(3) 0.68631(19) 0.5014(2) 0.0481(10) Uani 1 1 d . . . H20A H 0.8391 0.6776 0.4612 0.072 Uiso 1 1 calc R . . H20B H 0.9407 0.6580 0.5054 0.072 Uiso 1 1 calc R . . H20C H 0.9155 0.7241 0.4961 0.072 Uiso 1 1 calc R . . C21 C 0.7503(3) 0.72526(15) 0.5590(2) 0.0379(8) Uani 1 1 d . . . H21A H 0.7184 0.7230 0.6002 0.057 Uiso 1 1 calc R . . H21B H 0.7033 0.7143 0.5187 0.057 Uiso 1 1 calc R . . H21C H 0.7726 0.7642 0.5532 0.057 Uiso 1 1 calc R . . C22 C 1.0274(3) 0.55346(18) 0.5913(2) 0.0410(9) Uani 1 1 d . . . H22A H 1.0242 0.5880 0.5633 0.062 Uiso 1 1 calc R . . H22B H 1.0165 0.5202 0.5612 0.062 Uiso 1 1 calc R . . H22C H 1.0922 0.5507 0.6194 0.062 Uiso 1 1 calc R . . C23 C 0.4271(2) 0.18488(12) 0.60386(14) 0.0188(5) Uani 1 1 d . . . C24 C 0.3635(2) 0.15289(12) 0.55564(15) 0.0219(6) Uani 1 1 d . . . H24 H 0.3908 0.1303 0.5233 0.026 Uiso 1 1 calc R . . C25 C 0.2620(2) 0.15334(13) 0.55389(16) 0.0253(6) Uani 1 1 d . . . C26 C 0.1994(3) 0.11667(16) 0.50236(19) 0.0363(8) Uani 1 1 d . . . C27 C 0.2186(2) 0.18655(14) 0.59889(16) 0.0263(6) Uani 1 1 d . . . H27 H 0.1493 0.1871 0.5975 0.032 Uiso 1 1 calc R . . C28 C 0.2795(2) 0.21900(13) 0.64609(16) 0.0252(6) Uani 1 1 d . . . C29 C 0.2366(3) 0.25587(16) 0.69609(18) 0.0345(8) Uani 1 1 d . . . C30 C 0.3811(2) 0.21763(12) 0.64889(15) 0.0218(6) Uani 1 1 d . . . H30 H 0.4207 0.2398 0.6826 0.026 Uiso 1 1 calc R . . C31 C 0.6102(2) 0.22733(12) 0.65254(14) 0.0193(6) Uani 1 1 d . . . C32 C 0.5829(2) 0.28442(12) 0.64602(16) 0.0238(6) Uani 1 1 d . . . H32 H 0.5242 0.2943 0.6166 0.029 Uiso 1 1 calc R . . C33 C 0.6392(2) 0.32742(13) 0.68145(17) 0.0284(7) Uani 1 1 d . . . C34 C 0.6034(3) 0.38747(15) 0.6738(2) 0.0471(10) Uani 1 1 d . . . C35 C 0.7254(2) 0.31492(13) 0.72464(16) 0.0258(6) Uani 1 1 d . . . H35 H 0.7630 0.3440 0.7495 0.031 Uiso 1 1 calc R . . C36 C 0.7553(2) 0.25895(13) 0.73059(15) 0.0231(6) Uani 1 1 d . . . C37 C 0.8478(2) 0.24331(14) 0.77709(18) 0.0299(7) Uani 1 1 d . . . C38 C 0.6994(2) 0.21630(12) 0.69478(15) 0.0203(6) Uani 1 1 d . . . H38 H 0.7226 0.1783 0.6992 0.024 Uiso 1 1 calc R . . C39 C 0.56465(19) 0.11501(12) 0.65055(14) 0.0182(5) Uani 1 1 d . . . C40 C 0.5745(2) 0.11128(12) 0.72243(15) 0.0187(5) Uani 1 1 d . . . H40 H 0.5776 0.1453 0.7485 0.022 Uiso 1 1 calc R . . C41 C 0.5799(2) 0.05957(13) 0.75675(16) 0.0232(6) Uani 1 1 d . . . C42 C 0.5947(3) 0.05862(14) 0.83382(18) 0.0304(7) Uani 1 1 d . . . C43 C 0.5743(2) 0.00887(13) 0.72081(16) 0.0252(6) Uani 1 1 d . . . H43 H 0.5774 -0.0265 0.7441 0.030 Uiso 1 1 calc R . . C44 C 0.5640(2) 0.01132(13) 0.64975(16) 0.0247(6) Uani 1 1 d . . . C45 C 0.5532(3) -0.04258(14) 0.6091(2) 0.0381(8) Uani 1 1 d . . . C46 C 0.5594(2) 0.06332(12) 0.61560(15) 0.0203(6) Uani 1 1 d . . . H46 H 0.5525 0.0636 0.5669 0.024 Uiso 1 1 calc R . . C47 C 0.5834(2) 0.17526(12) 0.53500(14) 0.0193(6) Uani 1 1 d . . . C48 C 0.5360(2) 0.20732(12) 0.47975(15) 0.0226(6) Uani 1 1 d . . . H48 H 0.4784 0.2280 0.4853 0.027 Uiso 1 1 calc R . . C49 C 0.5708(2) 0.20967(13) 0.41704(16) 0.0271(6) Uani 1 1 d . . . C50 C 0.5158(3) 0.24277(17) 0.35876(19) 0.0430(9) Uani 1 1 d . . . C51 C 0.6541(2) 0.17998(13) 0.40665(16) 0.0277(7) Uani 1 1 d . . . H51 H 0.6775 0.1814 0.3637 0.033 Uiso 1 1 calc R . . C52 C 0.7022(2) 0.14836(13) 0.46025(16) 0.0256(6) Uani 1 1 d . . . C53 C 0.7917(3) 0.11428(16) 0.45083(19) 0.0378(8) Uani 1 1 d . . . C54 C 0.6680(2) 0.14652(12) 0.52320(15) 0.0220(6) Uani 1 1 d . . . H54 H 0.7034 0.1249 0.5594 0.026 Uiso 1 1 calc R . . C100 C 0.7895(5) 0.2874(3) 0.5278(4) 0.101(2) Uani 1 1 d . . . H10A H 0.7752 0.2646 0.4852 0.122 Uiso 1 1 calc R . . H10B H 0.7330 0.2828 0.5531 0.122 Uiso 1 1 calc R . . B1 B 0.5466(2) 0.17608(13) 0.61034(16) 0.0179(6) Uani 1 1 d . . . N1 N 0.81358(18) 0.55975(10) 0.71696(13) 0.0200(5) Uani 1 1 d . . . O1 O 0.90241(16) 0.49544(9) 0.78910(11) 0.0271(5) Uani 1 1 d . . . O2 O 0.72871(15) 0.62380(9) 0.64199(11) 0.0244(4) Uani 1 1 d . . . F1 F 0.2134(3) 0.06236(11) 0.51485(15) 0.0810(11) Uani 1 1 d . . . F2 F 0.2211(2) 0.12276(11) 0.43930(12) 0.0600(7) Uani 1 1 d . . . F3 F 0.10604(19) 0.1278(2) 0.4974(2) 0.1210(18) Uani 1 1 d . . . F4 F 0.13958(16) 0.26062(13) 0.68239(14) 0.0607(7) Uani 1 1 d . . . F5 F 0.2580(2) 0.23690(12) 0.76022(11) 0.0568(7) Uani 1 1 d . . . F6 F 0.27217(19) 0.30870(10) 0.69776(14) 0.0556(6) Uani 1 1 d . . . F7 F 0.5145(3) 0.39379(12) 0.6891(2) 0.0870(11) Uani 1 1 d . . . F8 F 0.5902(3) 0.40463(11) 0.60800(17) 0.0757(9) Uani 1 1 d . . . F9 F 0.6640(3) 0.42434(11) 0.7051(2) 0.1209(19) Uani 1 1 d . . . F10 F 0.92487(19) 0.24075(18) 0.74467(15) 0.0848(11) Uani 1 1 d . . . F11 F 0.87218(19) 0.27963(11) 0.82761(14) 0.0606(7) Uani 1 1 d . . . F12 F 0.8429(2) 0.19337(12) 0.80628(18) 0.0871(12) Uani 1 1 d . . . F13 F 0.68925(18) 0.06245(13) 0.86038(12) 0.0594(7) Uani 1 1 d . . . F14 F 0.5514(2) 0.10142(11) 0.86109(11) 0.0578(7) Uani 1 1 d . . . F15 F 0.5613(2) 0.01165(11) 0.85925(12) 0.0650(8) Uani 1 1 d . . . F16 F 0.5958(3) -0.08615(10) 0.64195(14) 0.0882(12) Uani 1 1 d . . . F17 F 0.4595(2) -0.05537(14) 0.5887(2) 0.0951(13) Uani 1 1 d . . . F18 F 0.5897(2) -0.03899(10) 0.55047(13) 0.0616(7) Uani 1 1 d . . . F19 F 0.46489(18) 0.28573(11) 0.37809(12) 0.0521(6) Uani 1 1 d . . . F20 F 0.4545(4) 0.21108(15) 0.31775(19) 0.129(2) Uani 1 1 d . . . F21 F 0.5762(3) 0.26608(15) 0.31983(17) 0.0919(13) Uani 1 1 d . . . F22 F 0.87132(19) 0.13216(17) 0.4883(2) 0.1038(15) Uani 1 1 d . . . F23 F 0.7823(2) 0.05964(10) 0.46773(15) 0.0609(7) Uani 1 1 d . . . F24 F 0.8060(2) 0.11126(13) 0.38579(14) 0.0689(9) Uani 1 1 d . . . P1 P 0.99586(5) 0.50314(3) 0.74425(4) 0.02183(16) Uani 1 1 d . . . P2 P 0.80753(5) 0.61116(3) 0.58645(4) 0.02212(16) Uani 1 1 d . . . Cl1 Cl 0.7958(2) 0.35611(10) 0.50550(14) 0.1419(10) Uani 1 1 d . . . Cl2 Cl 0.89199(12) 0.25906(6) 0.57722(8) 0.0796(4) Uani 1 1 d . . . Pd1 Pd 0.920659(15) 0.556506(9) 0.654112(11) 0.02121(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0408(19) 0.0227(15) 0.041(2) 0.0021(14) 0.0117(16) 0.0065(14) C2 0.089(3) 0.0288(19) 0.045(2) -0.0064(17) -0.003(2) 0.000(2) C3 0.050(2) 0.0239(16) 0.050(2) 0.0093(16) 0.0103(18) 0.0027(15) C4 0.068(3) 0.042(2) 0.078(3) 0.018(2) 0.043(3) 0.027(2) C5 0.059(3) 0.041(2) 0.046(2) 0.0086(18) -0.022(2) -0.0072(19) C6 0.0314(17) 0.0306(17) 0.0368(19) 0.0063(15) -0.0084(15) -0.0049(14) C7 0.0284(19) 0.049(2) 0.072(3) 0.017(2) -0.0040(19) -0.0131(16) C8 0.059(3) 0.035(2) 0.043(2) -0.0070(17) -0.0074(19) -0.0050(18) C9 0.0227(14) 0.0244(15) 0.0243(15) 0.0025(12) 0.0047(12) 0.0004(11) C10 0.0294(16) 0.0281(16) 0.0245(15) 0.0043(12) 0.0086(13) -0.0002(13) C11 0.0254(15) 0.0316(16) 0.0277(16) -0.0029(13) 0.0110(13) -0.0014(13) C12 0.0207(14) 0.0277(15) 0.0286(16) -0.0014(13) 0.0071(12) 0.0020(12) C13 0.0190(13) 0.0239(14) 0.0227(15) -0.0016(12) 0.0032(11) 0.0007(11) C14 0.0341(18) 0.046(2) 0.0254(17) -0.0096(15) -0.0003(14) -0.0024(15) C15 0.046(2) 0.045(2) 0.053(2) -0.0138(19) 0.0015(19) -0.0142(18) C16 0.060(3) 0.084(4) 0.039(2) -0.030(2) 0.014(2) -0.012(2) C17 0.048(2) 0.069(3) 0.046(2) -0.006(2) -0.023(2) -0.001(2) C18 0.0289(16) 0.0278(16) 0.0339(18) 0.0084(13) 0.0074(14) 0.0026(13) C19 0.0358(19) 0.0320(18) 0.060(3) 0.0001(18) -0.0010(17) -0.0043(15) C20 0.050(2) 0.049(2) 0.051(2) 0.0191(19) 0.026(2) 0.0087(18) C21 0.0367(18) 0.0311(17) 0.047(2) 0.0117(16) 0.0091(16) 0.0078(15) C22 0.0364(19) 0.058(2) 0.0341(19) 0.0128(17) 0.0230(16) 0.0176(17) C23 0.0220(13) 0.0166(13) 0.0180(13) 0.0027(10) 0.0037(11) 0.0013(11) C24 0.0249(14) 0.0216(14) 0.0196(14) -0.0007(11) 0.0050(11) 0.0013(11) C25 0.0262(15) 0.0235(14) 0.0249(15) 0.0018(12) -0.0002(12) 0.0001(12) C26 0.0288(17) 0.041(2) 0.0373(19) -0.0054(16) -0.0010(14) -0.0053(14) C27 0.0208(14) 0.0311(16) 0.0272(16) 0.0067(13) 0.0044(12) 0.0031(12) C28 0.0271(15) 0.0263(15) 0.0227(15) 0.0024(12) 0.0057(12) 0.0066(12) C29 0.0292(17) 0.042(2) 0.0336(19) -0.0032(15) 0.0098(14) 0.0104(14) C30 0.0254(14) 0.0216(14) 0.0182(14) 0.0001(11) 0.0028(11) 0.0018(11) C31 0.0219(13) 0.0213(14) 0.0161(13) 0.0004(11) 0.0079(11) -0.0025(11) C32 0.0266(15) 0.0208(14) 0.0232(15) 0.0007(11) 0.0011(12) -0.0008(12) C33 0.0331(16) 0.0195(15) 0.0318(17) -0.0015(12) 0.0020(13) -0.0004(12) C34 0.045(2) 0.0225(17) 0.068(3) -0.0039(17) -0.013(2) 0.0025(15) C35 0.0291(15) 0.0212(14) 0.0270(16) -0.0039(12) 0.0034(13) -0.0054(12) C36 0.0227(14) 0.0260(15) 0.0211(15) -0.0012(12) 0.0053(12) -0.0019(12) C37 0.0265(15) 0.0243(15) 0.0370(18) -0.0036(13) -0.0018(14) -0.0012(12) C38 0.0231(14) 0.0193(13) 0.0199(14) 0.0000(11) 0.0084(11) 0.0003(11) C39 0.0153(12) 0.0195(13) 0.0202(14) -0.0002(11) 0.0037(10) -0.0001(10) C40 0.0170(13) 0.0195(13) 0.0197(14) -0.0014(11) 0.0032(11) -0.0003(10) C41 0.0213(14) 0.0245(15) 0.0235(16) 0.0041(12) 0.0027(12) -0.0020(11) C42 0.0376(18) 0.0283(17) 0.0248(16) 0.0068(13) 0.0028(14) -0.0004(13) C43 0.0248(15) 0.0204(14) 0.0304(16) 0.0050(12) 0.0038(12) -0.0006(11) C44 0.0224(14) 0.0214(14) 0.0305(16) -0.0018(12) 0.0053(12) -0.0003(11) C45 0.051(2) 0.0212(16) 0.042(2) -0.0057(15) 0.0089(17) -0.0035(15) C46 0.0203(14) 0.0210(14) 0.0197(14) -0.0029(11) 0.0034(11) -0.0010(11) C47 0.0226(13) 0.0178(13) 0.0175(13) -0.0021(11) 0.0032(11) -0.0038(11) C48 0.0258(14) 0.0206(14) 0.0220(15) -0.0002(11) 0.0054(12) 0.0003(11) C49 0.0346(17) 0.0246(15) 0.0231(15) 0.0038(12) 0.0076(13) -0.0022(13) C50 0.061(2) 0.041(2) 0.0287(19) 0.0120(16) 0.0113(18) 0.0092(18) C51 0.0388(17) 0.0269(15) 0.0204(15) 0.0004(12) 0.0141(13) -0.0037(13) C52 0.0291(15) 0.0234(15) 0.0263(16) -0.0022(12) 0.0107(13) -0.0015(12) C53 0.042(2) 0.042(2) 0.0335(19) 0.0013(15) 0.0184(16) 0.0096(16) C54 0.0254(14) 0.0209(14) 0.0200(14) -0.0002(11) 0.0045(11) -0.0017(11) C100 0.094(5) 0.086(5) 0.119(6) 0.004(4) 0.000(4) -0.046(4) B1 0.0208(15) 0.0173(14) 0.0160(15) -0.0016(12) 0.0038(12) 0.0001(12) N1 0.0189(12) 0.0244(12) 0.0178(12) 0.0006(9) 0.0063(10) 0.0002(9) O1 0.0245(10) 0.0312(11) 0.0271(11) 0.0099(9) 0.0089(9) 0.0055(9) O2 0.0217(10) 0.0296(11) 0.0227(10) 0.0042(9) 0.0055(8) 0.0059(8) F1 0.136(3) 0.0352(13) 0.0577(17) 0.0052(11) -0.0314(18) -0.0348(16) F2 0.0834(19) 0.0574(15) 0.0335(12) -0.0067(11) -0.0094(12) -0.0270(14) F3 0.0247(13) 0.187(4) 0.147(3) -0.121(3) -0.0025(16) -0.0084(18) F4 0.0296(11) 0.090(2) 0.0633(16) -0.0305(14) 0.0102(11) 0.0152(12) F5 0.0762(17) 0.0696(16) 0.0282(11) -0.0013(11) 0.0195(11) 0.0276(14) F6 0.0625(15) 0.0363(12) 0.0742(17) -0.0171(12) 0.0304(13) 0.0067(11) F7 0.095(2) 0.0385(14) 0.138(3) 0.0055(16) 0.051(2) 0.0315(15) F8 0.100(2) 0.0381(14) 0.085(2) 0.0246(14) -0.0014(18) 0.0121(14) F9 0.118(3) 0.0213(12) 0.187(4) -0.0272(18) -0.098(3) 0.0113(15) F10 0.0370(13) 0.163(3) 0.0526(16) -0.0072(19) 0.0002(12) 0.0345(17) F11 0.0545(14) 0.0544(15) 0.0619(16) -0.0213(12) -0.0271(12) 0.0106(12) F12 0.0694(18) 0.0528(16) 0.117(3) 0.0395(16) -0.0591(18) -0.0249(14) F13 0.0435(13) 0.101(2) 0.0296(12) 0.0048(12) -0.0078(10) -0.0025(13) F14 0.0925(19) 0.0600(15) 0.0216(10) 0.0037(10) 0.0109(11) 0.0317(14) F15 0.113(2) 0.0503(14) 0.0312(12) 0.0118(10) 0.0101(13) -0.0336(15) F16 0.185(4) 0.0240(12) 0.0511(16) -0.0017(11) 0.0028(19) 0.0280(17) F17 0.068(2) 0.074(2) 0.145(3) -0.070(2) 0.022(2) -0.0347(16) F18 0.110(2) 0.0313(11) 0.0482(14) -0.0157(10) 0.0272(15) 0.0011(13) F19 0.0515(13) 0.0651(15) 0.0430(13) 0.0251(11) 0.0182(11) 0.0274(12) F20 0.203(5) 0.065(2) 0.082(2) 0.0182(18) -0.096(3) -0.008(2) F21 0.108(2) 0.104(2) 0.082(2) 0.0715(19) 0.0713(19) 0.067(2) F22 0.0282(13) 0.123(3) 0.157(3) -0.088(3) 0.0014(17) 0.0155(15) F23 0.0788(19) 0.0444(14) 0.0678(17) 0.0147(12) 0.0387(15) 0.0285(12) F24 0.088(2) 0.0778(18) 0.0526(15) 0.0180(13) 0.0488(15) 0.0425(16) P1 0.0193(3) 0.0214(3) 0.0254(4) 0.0032(3) 0.0054(3) 0.0019(3) P2 0.0216(3) 0.0267(4) 0.0184(4) 0.0002(3) 0.0041(3) 0.0021(3) Cl1 0.154(2) 0.1114(15) 0.1430(19) 0.0559(14) -0.0351(16) -0.0516(15) Cl2 0.0885(10) 0.0730(8) 0.0828(9) -0.0099(7) 0.0313(8) -0.0173(7) Pd1 0.01961(12) 0.02469(13) 0.02058(13) 0.00198(8) 0.00704(9) 0.00358(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.527(6) . ? C1 C3 1.535(5) . ? C1 C4 1.537(5) . ? C1 P1 1.849(3) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C6 1.536(5) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.535(6) . ? C6 C8 1.542(6) . ? C6 P1 1.849(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 N1 1.347(4) . ? C9 O1 1.354(4) . ? C9 C10 1.376(4) . ? C10 C11 1.385(5) . ? C10 H10 0.9500 . ? C11 C12 1.385(5) . ? C11 H11 0.9500 . ? C12 C13 1.376(4) . ? C12 H12 0.9500 . ? C13 N1 1.344(4) . ? C13 O2 1.356(4) . ? C14 C17 1.527(6) . ? C14 C16 1.536(6) . ? C14 C15 1.538(6) . ? C14 P2 1.850(3) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C21 1.532(5) . ? C18 C19 1.533(5) . ? C18 C20 1.540(5) . ? C18 P2 1.848(3) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 Pd1 2.060(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C30 1.397(4) . ? C23 C24 1.410(4) . ? C23 B1 1.644(4) . ? C24 C25 1.393(4) . ? C24 H24 0.9500 . ? C25 C27 1.384(5) . ? C25 C26 1.503(5) . ? C26 F3 1.302(5) . ? C26 F1 1.312(5) . ? C26 F2 1.328(5) . ? C27 C28 1.385(5) . ? C27 H27 0.9500 . ? C28 C30 1.393(4) . ? C28 C29 1.500(4) . ? C29 F4 1.327(4) . ? C29 F5 1.331(4) . ? C29 F6 1.337(4) . ? C30 H30 0.9500 . ? C31 C32 1.398(4) . ? C31 C38 1.402(4) . ? C31 B1 1.643(4) . ? C32 C33 1.398(4) . ? C32 H32 0.9500 . ? C33 C35 1.385(5) . ? C33 C34 1.499(5) . ? C34 F9 1.295(5) . ? C34 F7 1.312(5) . ? C34 F8 1.344(6) . ? C35 C36 1.382(4) . ? C35 H35 0.9500 . ? C36 C38 1.392(4) . ? C36 C37 1.499(4) . ? C37 F12 1.316(4) . ? C37 F11 1.318(4) . ? C37 F10 1.319(4) . ? C38 H38 0.9500 . ? C39 C46 1.396(4) . ? C39 C40 1.405(4) . ? C39 B1 1.644(4) . ? C40 C41 1.390(4) . ? C40 H40 0.9500 . ? C41 C43 1.385(4) . ? C41 C42 1.502(5) . ? C42 F14 1.325(4) . ? C42 F15 1.326(4) . ? C42 F13 1.332(4) . ? C43 C44 1.387(5) . ? C43 H43 0.9500 . ? C44 C46 1.395(4) . ? C44 C45 1.498(4) . ? C45 F16 1.305(5) . ? C45 F17 1.328(5) . ? C45 F18 1.328(5) . ? C46 H46 0.9500 . ? C47 C54 1.396(4) . ? C47 C48 1.403(4) . ? C47 B1 1.639(4) . ? C48 C49 1.392(4) . ? C48 H48 0.9500 . ? C49 C51 1.384(5) . ? C49 C50 1.497(5) . ? C50 F20 1.311(5) . ? C50 F19 1.320(5) . ? C50 F21 1.331(5) . ? C51 C52 1.378(5) . ? C51 H51 0.9500 . ? C52 C54 1.392(4) . ? C52 C53 1.506(5) . ? C53 F22 1.297(5) . ? C53 F24 1.327(4) . ? C53 F23 1.341(4) . ? C54 H54 0.9500 . ? C100 Cl1 1.685(7) . ? C100 Cl2 1.725(8) . ? C100 H10A 0.9900 . ? C100 H10B 0.9900 . ? N1 Pd1 2.064(2) . ? O1 P1 1.676(2) . ? O2 P2 1.679(2) . ? P1 Pd1 2.2932(8) . ? P2 Pd1 2.2896(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C3 109.2(3) . . ? C2 C1 C4 109.7(4) . . ? C3 C1 C4 110.0(3) . . ? C2 C1 P1 104.9(3) . . ? C3 C1 P1 114.0(3) . . ? C4 C1 P1 108.8(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C6 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C6 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C5 109.9(3) . . ? C7 C6 C8 109.2(3) . . ? C5 C6 C8 110.0(3) . . ? C7 C6 P1 107.7(3) . . ? C5 C6 P1 113.9(3) . . ? C8 C6 P1 105.9(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 O1 116.9(3) . . ? N1 C9 C10 122.3(3) . . ? O1 C9 C10 120.8(3) . . ? C9 C10 C11 117.6(3) . . ? C9 C10 H10 121.2 . . ? C11 C10 H10 121.2 . . ? C10 C11 C12 121.2(3) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 117.2(3) . . ? C13 C12 H12 121.4 . . ? C11 C12 H12 121.4 . . ? N1 C13 O2 117.2(3) . . ? N1 C13 C12 122.8(3) . . ? O2 C13 C12 120.0(3) . . ? C17 C14 C16 111.7(4) . . ? C17 C14 C15 109.1(3) . . ? C16 C14 C15 108.4(4) . . ? C17 C14 P2 113.9(3) . . ? C16 C14 P2 107.6(3) . . ? C15 C14 P2 105.9(2) . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C14 C17 H17A 109.5 . . ? C14 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C14 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C21 C18 C19 108.7(3) . . ? C21 C18 C20 110.4(3) . . ? C19 C18 C20 109.2(3) . . ? C21 C18 P2 113.5(2) . . ? C19 C18 P2 104.8(2) . . ? C20 C18 P2 109.9(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Pd1 C22 H22A 109.5 . . ? Pd1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Pd1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C30 C23 C24 115.4(3) . . ? C30 C23 B1 124.3(3) . . ? C24 C23 B1 119.9(2) . . ? C25 C24 C23 122.2(3) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C27 C25 C24 121.1(3) . . ? C27 C25 C26 119.9(3) . . ? C24 C25 C26 119.0(3) . . ? F3 C26 F1 109.1(4) . . ? F3 C26 F2 105.4(4) . . ? F1 C26 F2 103.5(3) . . ? F3 C26 C25 113.3(3) . . ? F1 C26 C25 112.4(3) . . ? F2 C26 C25 112.5(3) . . ? C25 C27 C28 117.8(3) . . ? C25 C27 H27 121.1 . . ? C28 C27 H27 121.1 . . ? C27 C28 C30 121.2(3) . . ? C27 C28 C29 120.2(3) . . ? C30 C28 C29 118.7(3) . . ? F4 C29 F5 107.2(3) . . ? F4 C29 F6 106.3(3) . . ? F5 C29 F6 105.1(3) . . ? F4 C29 C28 113.5(3) . . ? F5 C29 C28 112.1(3) . . ? F6 C29 C28 112.1(3) . . ? C28 C30 C23 122.4(3) . . ? C28 C30 H30 118.8 . . ? C23 C30 H30 118.8 . . ? C32 C31 C38 115.6(3) . . ? C32 C31 B1 123.1(3) . . ? C38 C31 B1 121.2(3) . . ? C31 C32 C33 122.0(3) . . ? C31 C32 H32 119.0 . . ? C33 C32 H32 119.0 . . ? C35 C33 C32 120.9(3) . . ? C35 C33 C34 120.1(3) . . ? C32 C33 C34 119.0(3) . . ? F9 C34 F7 111.8(4) . . ? F9 C34 F8 104.0(4) . . ? F7 C34 F8 101.0(3) . . ? F9 C34 C33 114.0(3) . . ? F7 C34 C33 112.8(3) . . ? F8 C34 C33 112.1(4) . . ? C36 C35 C33 118.2(3) . . ? C36 C35 H35 120.9 . . ? C33 C35 H35 120.9 . . ? C35 C36 C38 120.7(3) . . ? C35 C36 C37 120.1(3) . . ? C38 C36 C37 119.1(3) . . ? F12 C37 F11 105.9(3) . . ? F12 C37 F10 105.5(3) . . ? F11 C37 F10 105.2(3) . . ? F12 C37 C36 113.1(3) . . ? F11 C37 C36 113.5(3) . . ? F10 C37 C36 112.7(3) . . ? C36 C38 C31 122.4(3) . . ? C36 C38 H38 118.8 . . ? C31 C38 H38 118.8 . . ? C46 C39 C40 115.6(3) . . ? C46 C39 B1 122.2(2) . . ? C40 C39 B1 121.7(2) . . ? C41 C40 C39 122.4(3) . . ? C41 C40 H40 118.8 . . ? C39 C40 H40 118.8 . . ? C43 C41 C40 120.8(3) . . ? C43 C41 C42 119.5(3) . . ? C40 C41 C42 119.6(3) . . ? F14 C42 F15 106.2(3) . . ? F14 C42 F13 105.1(3) . . ? F15 C42 F13 106.4(3) . . ? F14 C42 C41 113.4(3) . . ? F15 C42 C41 113.1(3) . . ? F13 C42 C41 111.9(3) . . ? C41 C43 C44 118.0(3) . . ? C41 C43 H43 121.0 . . ? C44 C43 H43 121.0 . . ? C43 C44 C46 120.9(3) . . ? C43 C44 C45 119.5(3) . . ? C46 C44 C45 119.6(3) . . ? F16 C45 F17 108.3(4) . . ? F16 C45 F18 106.4(3) . . ? F17 C45 F18 103.2(4) . . ? F16 C45 C44 113.6(3) . . ? F17 C45 C44 111.6(3) . . ? F18 C45 C44 113.0(3) . . ? C44 C46 C39 122.2(3) . . ? C44 C46 H46 118.9 . . ? C39 C46 H46 118.9 . . ? C54 C47 C48 115.8(3) . . ? C54 C47 B1 122.3(3) . . ? C48 C47 B1 121.7(3) . . ? C49 C48 C47 121.8(3) . . ? C49 C48 H48 119.1 . . ? C47 C48 H48 119.1 . . ? C51 C49 C48 121.0(3) . . ? C51 C49 C50 119.0(3) . . ? C48 C49 C50 120.0(3) . . ? F20 C50 F19 107.1(4) . . ? F20 C50 F21 106.3(4) . . ? F19 C50 F21 104.7(3) . . ? F20 C50 C49 112.4(3) . . ? F19 C50 C49 114.1(3) . . ? F21 C50 C49 111.7(3) . . ? C52 C51 C49 118.3(3) . . ? C52 C51 H51 120.9 . . ? C49 C51 H51 120.9 . . ? C51 C52 C54 120.8(3) . . ? C51 C52 C53 120.1(3) . . ? C54 C52 C53 119.0(3) . . ? F22 C53 F24 109.3(4) . . ? F22 C53 F23 106.0(4) . . ? F24 C53 F23 102.8(3) . . ? F22 C53 C52 113.2(3) . . ? F24 C53 C52 113.0(3) . . ? F23 C53 C52 111.7(3) . . ? C52 C54 C47 122.3(3) . . ? C52 C54 H54 118.8 . . ? C47 C54 H54 118.8 . . ? Cl1 C100 Cl2 116.7(4) . . ? Cl1 C100 H10A 108.1 . . ? Cl2 C100 H10A 108.1 . . ? Cl1 C100 H10B 108.1 . . ? Cl2 C100 H10B 108.1 . . ? H10A C100 H10B 107.3 . . ? C47 B1 C31 104.7(2) . . ? C47 B1 C39 112.4(2) . . ? C31 B1 C39 111.7(2) . . ? C47 B1 C23 111.9(2) . . ? C31 B1 C23 113.4(2) . . ? C39 B1 C23 103.0(2) . . ? C13 N1 C9 118.9(3) . . ? C13 N1 Pd1 120.3(2) . . ? C9 N1 Pd1 120.8(2) . . ? C9 O1 P1 119.91(19) . . ? C13 O2 P2 120.17(18) . . ? O1 P1 C6 101.26(15) . . ? O1 P1 C1 99.39(14) . . ? C6 P1 C1 115.32(17) . . ? O1 P1 Pd1 100.04(8) . . ? C6 P1 Pd1 116.19(11) . . ? C1 P1 Pd1 119.26(12) . . ? O2 P2 C18 99.43(13) . . ? O2 P2 C14 100.91(14) . . ? C18 P2 C14 114.99(17) . . ? O2 P2 Pd1 99.80(8) . . ? C18 P2 Pd1 119.65(11) . . ? C14 P2 Pd1 116.44(13) . . ? C22 Pd1 N1 179.86(14) . . ? C22 Pd1 P2 98.86(11) . . ? N1 Pd1 P2 81.01(7) . . ? C22 Pd1 P1 99.57(11) . . ? N1 Pd1 P1 80.56(7) . . ? P2 Pd1 P1 161.57(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 N1 C9 C10 C11 -1.1(5) . . . . ? O1 C9 C10 C11 179.0(3) . . . . ? C9 C10 C11 C12 0.3(5) . . . . ? C10 C11 C12 C13 1.1(5) . . . . ? C11 C12 C13 N1 -1.7(5) . . . . ? C11 C12 C13 O2 178.6(3) . . . . ? C30 C23 C24 C25 -1.0(4) . . . . ? B1 C23 C24 C25 171.7(3) . . . . ? C23 C24 C25 C27 1.5(5) . . . . ? C23 C24 C25 C26 -178.1(3) . . . . ? C27 C25 C26 F3 11.6(5) . . . . ? C24 C25 C26 F3 -168.8(4) . . . . ? C27 C25 C26 F1 -112.5(4) . . . . ? C24 C25 C26 F1 67.1(4) . . . . ? C27 C25 C26 F2 131.1(3) . . . . ? C24 C25 C26 F2 -49.3(4) . . . . ? C24 C25 C27 C28 -0.5(5) . . . . ? C26 C25 C27 C28 179.1(3) . . . . ? C25 C27 C28 C30 -0.9(5) . . . . ? C25 C27 C28 C29 179.9(3) . . . . ? C27 C28 C29 F4 -10.4(5) . . . . ? C30 C28 C29 F4 170.4(3) . . . . ? C27 C28 C29 F5 111.2(4) . . . . ? C30 C28 C29 F5 -68.0(4) . . . . ? C27 C28 C29 F6 -130.9(3) . . . . ? C30 C28 C29 F6 49.9(4) . . . . ? C27 C28 C30 C23 1.5(5) . . . . ? C29 C28 C30 C23 -179.4(3) . . . . ? C24 C23 C30 C28 -0.5(4) . . . . ? B1 C23 C30 C28 -172.8(3) . . . . ? C38 C31 C32 C33 -2.3(4) . . . . ? B1 C31 C32 C33 -178.7(3) . . . . ? C31 C32 C33 C35 0.3(5) . . . . ? C31 C32 C33 C34 -177.9(3) . . . . ? C35 C33 C34 F9 6.1(6) . . . . ? C32 C33 C34 F9 -175.8(4) . . . . ? C35 C33 C34 F7 -122.8(4) . . . . ? C32 C33 C34 F7 55.4(5) . . . . ? C35 C33 C34 F8 124.0(4) . . . . ? C32 C33 C34 F8 -57.9(5) . . . . ? C32 C33 C35 C36 1.4(5) . . . . ? C34 C33 C35 C36 179.5(3) . . . . ? C33 C35 C36 C38 -0.9(5) . . . . ? C33 C35 C36 C37 -179.6(3) . . . . ? C35 C36 C37 F12 146.0(4) . . . . ? C38 C36 C37 F12 -32.7(5) . . . . ? C35 C36 C37 F11 25.3(5) . . . . ? C38 C36 C37 F11 -153.5(3) . . . . ? C35 C36 C37 F10 -94.3(4) . . . . ? C38 C36 C37 F10 87.0(4) . . . . ? C35 C36 C38 C31 -1.3(5) . . . . ? C37 C36 C38 C31 177.4(3) . . . . ? C32 C31 C38 C36 2.9(4) . . . . ? B1 C31 C38 C36 179.3(3) . . . . ? C46 C39 C40 C41 0.7(4) . . . . ? B1 C39 C40 C41 173.4(3) . . . . ? C39 C40 C41 C43 -0.9(4) . . . . ? C39 C40 C41 C42 177.4(3) . . . . ? C43 C41 C42 F14 -147.6(3) . . . . ? C40 C41 C42 F14 34.1(4) . . . . ? C43 C41 C42 F15 -26.5(5) . . . . ? C40 C41 C42 F15 155.1(3) . . . . ? C43 C41 C42 F13 93.7(4) . . . . ? C40 C41 C42 F13 -84.7(4) . . . . ? C40 C41 C43 C44 0.5(4) . . . . ? C42 C41 C43 C44 -177.8(3) . . . . ? C41 C43 C44 C46 0.0(4) . . . . ? C41 C43 C44 C45 -177.3(3) . . . . ? C43 C44 C45 F16 -28.4(5) . . . . ? C46 C44 C45 F16 154.2(4) . . . . ? C43 C44 C45 F17 94.4(4) . . . . ? C46 C44 C45 F17 -83.0(4) . . . . ? C43 C44 C45 F18 -149.8(3) . . . . ? C46 C44 C45 F18 32.9(5) . . . . ? C43 C44 C46 C39 -0.1(5) . . . . ? C45 C44 C46 C39 177.2(3) . . . . ? C40 C39 C46 C44 -0.2(4) . . . . ? B1 C39 C46 C44 -172.8(3) . . . . ? C54 C47 C48 C49 0.6(4) . . . . ? B1 C47 C48 C49 175.7(3) . . . . ? C47 C48 C49 C51 0.3(5) . . . . ? C47 C48 C49 C50 177.8(3) . . . . ? C51 C49 C50 F20 83.4(5) . . . . ? C48 C49 C50 F20 -94.1(5) . . . . ? C51 C49 C50 F19 -154.4(3) . . . . ? C48 C49 C50 F19 28.0(5) . . . . ? C51 C49 C50 F21 -35.9(5) . . . . ? C48 C49 C50 F21 146.5(4) . . . . ? C48 C49 C51 C52 -0.5(5) . . . . ? C50 C49 C51 C52 -178.1(3) . . . . ? C49 C51 C52 C54 -0.2(5) . . . . ? C49 C51 C52 C53 178.6(3) . . . . ? C51 C52 C53 F22 114.6(4) . . . . ? C54 C52 C53 F22 -66.7(5) . . . . ? C51 C52 C53 F24 -10.4(5) . . . . ? C54 C52 C53 F24 168.3(3) . . . . ? C51 C52 C53 F23 -125.8(3) . . . . ? C54 C52 C53 F23 53.0(4) . . . . ? C51 C52 C54 C47 1.2(5) . . . . ? C53 C52 C54 C47 -177.6(3) . . . . ? C48 C47 C54 C52 -1.4(4) . . . . ? B1 C47 C54 C52 -176.4(3) . . . . ? C54 C47 B1 C31 83.7(3) . . . . ? C48 C47 B1 C31 -91.0(3) . . . . ? C54 C47 B1 C39 -37.7(4) . . . . ? C48 C47 B1 C39 147.6(3) . . . . ? C54 C47 B1 C23 -153.0(3) . . . . ? C48 C47 B1 C23 32.2(4) . . . . ? C32 C31 B1 C47 83.3(3) . . . . ? C38 C31 B1 C47 -92.9(3) . . . . ? C32 C31 B1 C39 -154.9(3) . . . . ? C38 C31 B1 C39 29.0(4) . . . . ? C32 C31 B1 C23 -39.0(4) . . . . ? C38 C31 B1 C23 144.9(3) . . . . ? C46 C39 B1 C47 -32.4(4) . . . . ? C40 C39 B1 C47 155.5(2) . . . . ? C46 C39 B1 C31 -149.7(3) . . . . ? C40 C39 B1 C31 38.2(3) . . . . ? C46 C39 B1 C23 88.2(3) . . . . ? C40 C39 B1 C23 -83.9(3) . . . . ? C30 C23 B1 C47 -141.8(3) . . . . ? C24 C23 B1 C47 46.2(3) . . . . ? C30 C23 B1 C31 -23.7(4) . . . . ? C24 C23 B1 C31 164.3(2) . . . . ? C30 C23 B1 C39 97.2(3) . . . . ? C24 C23 B1 C39 -74.8(3) . . . . ? O2 C13 N1 C9 -179.4(3) . . . . ? C12 C13 N1 C9 1.0(4) . . . . ? O2 C13 N1 Pd1 1.9(4) . . . . ? C12 C13 N1 Pd1 -177.8(2) . . . . ? O1 C9 N1 C13 -179.6(3) . . . . ? C10 C9 N1 C13 0.5(4) . . . . ? O1 C9 N1 Pd1 -0.9(4) . . . . ? C10 C9 N1 Pd1 179.2(2) . . . . ? N1 C9 O1 P1 11.8(4) . . . . ? C10 C9 O1 P1 -168.3(2) . . . . ? N1 C13 O2 P2 8.5(4) . . . . ? C12 C13 O2 P2 -171.8(2) . . . . ? C9 O1 P1 C6 104.8(2) . . . . ? C9 O1 P1 C1 -136.9(2) . . . . ? C9 O1 P1 Pd1 -14.7(2) . . . . ? C7 C6 P1 O1 -172.4(2) . . . . ? C5 C6 P1 O1 65.4(3) . . . . ? C8 C6 P1 O1 -55.6(3) . . . . ? C7 C6 P1 C1 81.4(3) . . . . ? C5 C6 P1 C1 -40.8(4) . . . . ? C8 C6 P1 C1 -161.8(3) . . . . ? C7 C6 P1 Pd1 -65.2(3) . . . . ? C5 C6 P1 Pd1 172.6(3) . . . . ? C8 C6 P1 Pd1 51.6(3) . . . . ? C2 C1 P1 O1 78.3(3) . . . . ? C3 C1 P1 O1 -41.2(3) . . . . ? C4 C1 P1 O1 -164.4(3) . . . . ? C2 C1 P1 C6 -174.4(3) . . . . ? C3 C1 P1 C6 66.1(3) . . . . ? C4 C1 P1 C6 -57.1(3) . . . . ? C2 C1 P1 Pd1 -28.9(3) . . . . ? C3 C1 P1 Pd1 -148.3(2) . . . . ? C4 C1 P1 Pd1 88.5(3) . . . . ? C13 O2 P2 C18 -135.2(2) . . . . ? C13 O2 P2 C14 106.9(2) . . . . ? C13 O2 P2 Pd1 -12.7(2) . . . . ? C21 C18 P2 O2 -40.0(3) . . . . ? C19 C18 P2 O2 78.5(2) . . . . ? C20 C18 P2 O2 -164.3(2) . . . . ? C21 C18 P2 C14 66.8(3) . . . . ? C19 C18 P2 C14 -174.7(2) . . . . ? C20 C18 P2 C14 -57.5(3) . . . . ? C21 C18 P2 Pd1 -147.0(2) . . . . ? C19 C18 P2 Pd1 -28.5(3) . . . . ? C20 C18 P2 Pd1 88.7(3) . . . . ? C17 C14 P2 O2 62.8(3) . . . . ? C16 C14 P2 O2 -172.8(3) . . . . ? C15 C14 P2 O2 -57.0(3) . . . . ? C17 C14 P2 C18 -43.1(4) . . . . ? C16 C14 P2 C18 81.3(3) . . . . ? C15 C14 P2 C18 -162.9(2) . . . . ? C17 C14 P2 Pd1 169.6(3) . . . . ? C16 C14 P2 Pd1 -66.0(3) . . . . ? C15 C14 P2 Pd1 49.8(3) . . . . ? C13 N1 Pd1 P2 -7.7(2) . . . . ? C9 N1 Pd1 P2 173.6(2) . . . . ? C13 N1 Pd1 P1 172.2(2) . . . . ? C9 N1 Pd1 P1 -6.5(2) . . . . ? O2 P2 Pd1 C22 -170.61(15) . . . . ? C18 P2 Pd1 C22 -63.77(18) . . . . ? C14 P2 Pd1 C22 81.92(19) . . . . ? O2 P2 Pd1 N1 9.34(11) . . . . ? C18 P2 Pd1 N1 116.17(15) . . . . ? C14 P2 Pd1 N1 -98.14(15) . . . . ? O2 P2 Pd1 P1 9.01(13) . . . . ? C18 P2 Pd1 P1 115.84(15) . . . . ? C14 P2 Pd1 P1 -98.47(16) . . . . ? O1 P1 Pd1 C22 -170.32(16) . . . . ? C6 P1 Pd1 C22 81.74(19) . . . . ? C1 P1 Pd1 C22 -63.52(19) . . . . ? O1 P1 Pd1 N1 9.73(11) . . . . ? C6 P1 Pd1 N1 -98.20(16) . . . . ? C1 P1 Pd1 N1 116.53(15) . . . . ? O1 P1 Pd1 P2 10.07(14) . . . . ? C6 P1 Pd1 P2 -97.87(16) . . . . ? C1 P1 Pd1 P2 116.87(16) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 70.14 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.278 _refine_diff_density_min -0.755 _refine_diff_density_rms 0.085 # Attachment '- RhI.cif' data_RhI _database_code_depnum_ccdc_archive 'CCDC 834660' #TrackingRef '- RhI.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C71 H99 I2 N4 O4 P4 Rh2' _chemical_formula_weight 1656.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1948(4) _cell_length_b 12.7179(5) _cell_length_c 14.3447(9) _cell_angle_alpha 100.145(2) _cell_angle_beta 102.482(2) _cell_angle_gamma 110.4030(10) _cell_volume 1796.98(15) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9874 _cell_measurement_theta_min 4.32 _cell_measurement_theta_max 69.95 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.530 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 841 _exptl_absorpt_coefficient_mu 11.679 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.2414 _exptl_absorpt_correction_T_max 0.3598 _exptl_absorpt_process_details '(Bruker SADABS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29205 _diffrn_reflns_av_R_equivalents 0.0285 _diffrn_reflns_av_sigmaI/netI 0.0221 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.28 _diffrn_reflns_theta_max 70.18 _reflns_number_total 6587 _reflns_number_gt 6427 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0416P)^2^+1.8546P] 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 6587 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0704 _refine_ls_wR_factor_gt 0.0699 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0419(3) 0.6484(3) 0.4396(2) 0.0317(7) Uani 1 1 d . . . H1A H 0.1154 0.6585 0.4966 0.048 Uiso 1 1 calc R . . H1B H 0.0781 0.6894 0.3937 0.048 Uiso 1 1 calc R . . H1C H -0.0083 0.5651 0.4055 0.048 Uiso 1 1 calc R . . C2 C -0.1030(3) 0.6372(3) 0.5503(2) 0.0359(7) Uani 1 1 d . . . H2A H -0.1598 0.5549 0.5165 0.054 Uiso 1 1 calc R . . H2B H -0.1552 0.6744 0.5789 0.054 Uiso 1 1 calc R . . H2C H -0.0273 0.6431 0.6034 0.054 Uiso 1 1 calc R . . C3 C -0.0512(3) 0.6986(2) 0.47575(18) 0.0195(5) Uani 1 1 d . . . C4 C 0.0270(3) 0.8294(2) 0.5255(2) 0.0300(6) Uani 1 1 d . . . H4A H -0.0262 0.8594 0.5597 0.045 Uiso 1 1 calc R . . H4B H 0.0460 0.8701 0.4749 0.045 Uiso 1 1 calc R . . H4C H 0.1112 0.8427 0.5736 0.045 Uiso 1 1 calc R . . C5 C -0.3782(3) 0.6916(3) 0.4541(2) 0.0273(6) Uani 1 1 d . . . H5A H -0.4490 0.7202 0.4541 0.041 Uiso 1 1 calc R . . H5B H -0.3135 0.7215 0.5206 0.041 Uiso 1 1 calc R . . H5C H -0.4174 0.6062 0.4355 0.041 Uiso 1 1 calc R . . C6 C -0.2381(3) 0.8675(2) 0.4096(2) 0.0271(6) Uani 1 1 d . . . H6A H -0.1888 0.8927 0.3632 0.041 Uiso 1 1 calc R . . H6B H -0.1760 0.8947 0.4769 0.041 Uiso 1 1 calc R . . H6C H -0.3055 0.9004 0.4081 0.041 Uiso 1 1 calc R . . C7 C -0.4110(3) 0.6930(3) 0.2763(2) 0.0290(6) Uani 1 1 d . . . H7A H -0.4770 0.7268 0.2793 0.043 Uiso 1 1 calc R . . H7B H -0.4561 0.6077 0.2565 0.043 Uiso 1 1 calc R . . H7C H -0.3661 0.7184 0.2277 0.043 Uiso 1 1 calc R . . C8 C -0.3071(3) 0.7341(2) 0.3791(2) 0.0191(5) Uani 1 1 d . . . C9 C -0.1207(2) 0.6895(2) 0.20440(18) 0.0145(5) Uani 1 1 d . . . C10 C -0.0668(2) 0.7555(2) 0.14345(18) 0.0147(5) Uani 1 1 d . . . C11 C 0.0146(2) 0.8834(2) 0.18017(18) 0.0150(5) Uani 1 1 d . . . C12 C 0.1167(3) 0.9316(2) 0.27065(19) 0.0188(5) Uani 1 1 d . . . H12 H 0.1303 0.8830 0.3114 0.023 Uiso 1 1 calc R . . C13 C 0.1979(3) 1.0496(2) 0.3012(2) 0.0221(5) Uani 1 1 d . . . H13 H 0.2686 1.0811 0.3619 0.027 Uiso 1 1 calc R . . C14 C 0.1766(3) 1.1221(2) 0.2435(2) 0.0212(5) Uani 1 1 d . . . H14 H 0.2317 1.2033 0.2650 0.025 Uiso 1 1 calc R . . C15 C 0.0744(3) 1.0755(2) 0.1541(2) 0.0222(5) Uani 1 1 d . . . H15 H 0.0591 1.1249 0.1147 0.027 Uiso 1 1 calc R . . C16 C -0.0058(2) 0.9563(2) 0.12219(19) 0.0187(5) Uani 1 1 d . . . H16 H -0.0747 0.9246 0.0606 0.022 Uiso 1 1 calc R . . C17 C -0.1557(2) 0.5867(2) 0.01316(18) 0.0153(5) Uani 1 1 d . . . C18 C -0.1833(2) 0.5323(2) -0.09393(18) 0.0165(5) Uani 1 1 d . . . C19 C -0.2318(2) 0.5831(2) -0.16395(19) 0.0186(5) Uani 1 1 d . . . H19 H -0.2455 0.6518 -0.1424 0.022 Uiso 1 1 calc R . . C20 C -0.2599(3) 0.5336(2) -0.26453(19) 0.0208(5) Uani 1 1 d . . . H20 H -0.2953 0.5673 -0.3117 0.025 Uiso 1 1 calc R . . C21 C -0.2367(3) 0.4351(2) -0.29659(19) 0.0218(5) Uani 1 1 d . . . H21 H -0.2548 0.4020 -0.3655 0.026 Uiso 1 1 calc R . . C22 C -0.1866(3) 0.3852(2) -0.2273(2) 0.0222(5) Uani 1 1 d . . . H22 H -0.1693 0.3185 -0.2491 0.027 Uiso 1 1 calc R . . C23 C -0.1617(3) 0.4322(2) -0.1264(2) 0.0195(5) Uani 1 1 d . . . H23 H -0.1300 0.3962 -0.0797 0.023 Uiso 1 1 calc R . . C24 C -0.2007(2) 0.5210(2) 0.07628(18) 0.0151(5) Uani 1 1 d . . . C25 C -0.2341(4) 0.1700(4) 0.0303(2) 0.0456(10) Uani 1 1 d . . . H25A H -0.1672 0.1368 0.0429 0.068 Uiso 1 1 calc R . . H25B H -0.2104 0.2242 -0.0101 0.068 Uiso 1 1 calc R . . H25C H -0.3221 0.1071 -0.0052 0.068 Uiso 1 1 calc R . . C26 C -0.2925(5) 0.1520(4) 0.1880(4) 0.0613(13) Uani 1 1 d . . . H26A H -0.3847 0.0982 0.1508 0.092 Uiso 1 1 calc R . . H26B H -0.2904 0.1966 0.2518 0.092 Uiso 1 1 calc R . . H26C H -0.2374 0.1075 0.1996 0.092 Uiso 1 1 calc R . . C28 C -0.2380(3) 0.2352(2) 0.1288(2) 0.0200(5) Uani 1 1 d . . . C29 C -0.5931(3) 0.1803(4) 0.0873(3) 0.0541(11) Uani 1 1 d . . . H29A H -0.5801 0.2287 0.1530 0.081 Uiso 1 1 calc R . . H29B H -0.5683 0.1149 0.0948 0.081 Uiso 1 1 calc R . . H29C H -0.6871 0.1502 0.0478 0.081 Uiso 1 1 calc R . . C30 C -0.5186(3) 0.1810(3) -0.0664(2) 0.0323(7) Uani 1 1 d . . . H30A H -0.4965 0.1144 -0.0582 0.048 Uiso 1 1 calc R . . H30B H -0.4571 0.2291 -0.0964 0.048 Uiso 1 1 calc R . . H30C H -0.6105 0.1526 -0.1096 0.048 Uiso 1 1 calc R . . C031 C -0.0946(3) 0.3190(3) 0.1883(3) 0.0398(8) Uani 1 1 d . . . H03A H -0.0945 0.3667 0.2499 0.060 Uiso 1 1 calc R . . H03B H -0.0563 0.3698 0.1489 0.060 Uiso 1 1 calc R . . H03C H -0.0410 0.2742 0.2041 0.060 Uiso 1 1 calc R . . C31 C -0.5511(3) 0.3517(3) 0.0182(3) 0.0359(7) Uani 1 1 d . . . H31A H -0.6452 0.3174 -0.0220 0.054 Uiso 1 1 calc R . . H31B H -0.4965 0.3987 -0.0166 0.054 Uiso 1 1 calc R . . H31C H -0.5407 0.4015 0.0824 0.054 Uiso 1 1 calc R . . C32 C -0.5055(2) 0.2538(2) 0.0348(2) 0.0205(5) Uani 1 1 d . . . N1 N -0.1887(2) 0.57212(17) 0.17118(15) 0.0138(4) Uani 1 1 d . . . N2 N -0.0892(2) 0.70308(18) 0.04758(15) 0.0154(4) Uani 1 1 d . . . O1 O -0.10925(17) 0.74185(14) 0.29713(12) 0.0160(3) Uani 1 1 d . . . O2 O -0.26199(17) 0.40423(14) 0.04404(13) 0.0170(3) Uani 1 1 d . . . P1 P -0.19364(6) 0.65922(5) 0.36221(4) 0.01375(12) Uani 1 1 d . . . P2 P -0.33125(6) 0.33126(5) 0.12043(4) 0.01436(12) Uani 1 1 d . . . Rh1 Rh -0.278805(17) 0.480228(14) 0.254291(12) 0.01345(6) Uani 1 1 d . . . I1 I -0.407314(18) 0.362185(14) 0.361333(13) 0.02623(7) Uani 1 1 d . . . C100 C 0.4132(4) 0.8969(3) 0.4339(3) 0.0484(10) Uani 1 1 d . . . H100 H 0.3524 0.8249 0.3872 0.058 Uiso 1 1 calc R . . C101 C 0.4276(4) 0.9083(3) 0.5320(4) 0.0498(10) Uani 1 1 d . . . H101 H 0.3778 0.8450 0.5535 0.060 Uiso 1 1 calc R . . C102 C 0.4845(4) 0.9872(4) 0.3997(3) 0.0481(9) Uani 1 1 d . . . C103 C 0.4687(10) 0.9736(10) 0.2983(7) 0.063(3) Uani 0.50 1 d P . . H10A H 0.4779 1.0477 0.2832 0.094 Uiso 0.50 1 calc PR . . H10B H 0.3800 0.9136 0.2599 0.094 Uiso 0.50 1 calc PR . . H10C H 0.5373 0.9500 0.2808 0.094 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0295(15) 0.0394(17) 0.0270(15) 0.0009(12) 0.0007(12) 0.0234(13) C2 0.0402(17) 0.0434(19) 0.0236(15) 0.0189(13) 0.0096(13) 0.0115(15) C3 0.0234(12) 0.0195(12) 0.0152(12) 0.0045(10) 0.0053(10) 0.0087(10) C4 0.0333(15) 0.0213(14) 0.0253(14) -0.0009(11) -0.0010(12) 0.0086(12) C5 0.0318(15) 0.0240(14) 0.0357(16) 0.0105(12) 0.0230(13) 0.0137(12) C6 0.0292(14) 0.0148(13) 0.0415(17) 0.0071(11) 0.0154(13) 0.0112(11) C7 0.0253(14) 0.0344(16) 0.0303(15) 0.0078(12) 0.0070(12) 0.0170(12) C8 0.0211(12) 0.0169(12) 0.0236(13) 0.0069(10) 0.0115(10) 0.0091(10) C9 0.0137(11) 0.0135(11) 0.0159(11) 0.0026(9) 0.0053(9) 0.0051(9) C10 0.0150(11) 0.0131(11) 0.0161(11) 0.0033(9) 0.0052(9) 0.0059(9) C11 0.0146(11) 0.0128(11) 0.0184(12) 0.0042(9) 0.0086(9) 0.0045(9) C12 0.0205(12) 0.0147(12) 0.0192(12) 0.0042(9) 0.0062(10) 0.0050(10) C13 0.0214(12) 0.0177(12) 0.0198(13) 0.0004(10) 0.0036(10) 0.0031(10) C14 0.0225(12) 0.0115(11) 0.0265(13) 0.0021(10) 0.0120(11) 0.0022(10) C15 0.0264(13) 0.0171(12) 0.0271(14) 0.0108(10) 0.0127(11) 0.0083(10) C16 0.0186(12) 0.0162(12) 0.0194(12) 0.0055(9) 0.0053(10) 0.0046(10) C17 0.0150(11) 0.0139(11) 0.0175(12) 0.0030(9) 0.0067(9) 0.0059(9) C18 0.0145(11) 0.0152(11) 0.0175(12) 0.0033(9) 0.0073(9) 0.0023(9) C19 0.0208(12) 0.0155(12) 0.0207(12) 0.0051(10) 0.0103(10) 0.0061(10) C20 0.0201(12) 0.0209(13) 0.0190(12) 0.0069(10) 0.0061(10) 0.0049(10) C21 0.0213(12) 0.0219(13) 0.0162(12) -0.0010(10) 0.0073(10) 0.0039(10) C22 0.0235(13) 0.0198(13) 0.0223(13) 0.0009(10) 0.0098(11) 0.0081(10) C23 0.0206(12) 0.0175(12) 0.0217(13) 0.0049(10) 0.0093(10) 0.0077(10) C24 0.0145(11) 0.0120(11) 0.0186(12) 0.0029(9) 0.0055(9) 0.0055(9) C25 0.0461(19) 0.061(2) 0.0315(17) -0.0108(16) -0.0002(15) 0.0417(18) C26 0.083(3) 0.044(2) 0.114(4) 0.057(3) 0.073(3) 0.049(2) C28 0.0220(12) 0.0136(12) 0.0240(13) 0.0035(10) 0.0069(10) 0.0075(10) C29 0.0229(16) 0.069(3) 0.041(2) 0.0255(19) 0.0010(14) -0.0156(16) C30 0.0288(15) 0.0289(15) 0.0286(15) -0.0046(12) -0.0045(12) 0.0133(12) C031 0.0278(15) 0.0297(16) 0.049(2) -0.0028(14) -0.0091(14) 0.0161(13) C31 0.0246(14) 0.0328(16) 0.0433(18) -0.0037(14) -0.0003(13) 0.0164(13) C32 0.0142(11) 0.0180(12) 0.0227(13) 0.0030(10) 0.0029(10) 0.0016(10) N1 0.0146(9) 0.0111(9) 0.0147(9) 0.0034(7) 0.0064(8) 0.0029(7) N2 0.0151(9) 0.0138(10) 0.0161(10) 0.0034(8) 0.0050(8) 0.0045(8) O1 0.0203(8) 0.0101(8) 0.0144(8) 0.0017(6) 0.0077(7) 0.0018(7) O2 0.0210(8) 0.0093(8) 0.0173(8) 0.0008(6) 0.0075(7) 0.0024(7) P1 0.0176(3) 0.0104(3) 0.0139(3) 0.0033(2) 0.0071(2) 0.0050(2) P2 0.0151(3) 0.0094(3) 0.0161(3) 0.0022(2) 0.0053(2) 0.0024(2) Rh1 0.01661(10) 0.00905(9) 0.01467(10) 0.00343(7) 0.00717(7) 0.00358(7) I1 0.03821(11) 0.01639(10) 0.02706(10) 0.01028(7) 0.02010(8) 0.00623(7) C100 0.0326(17) 0.0205(15) 0.074(3) -0.0006(15) -0.0070(17) 0.0097(13) C101 0.0352(18) 0.0359(19) 0.082(3) 0.0282(19) 0.0086(18) 0.0185(15) C102 0.045(2) 0.058(2) 0.051(2) 0.0090(18) 0.0039(17) 0.0405(19) C103 0.076(6) 0.105(8) 0.068(6) 0.058(6) 0.053(5) 0.071(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C3 1.530(4) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.528(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.530(4) . ? C3 P1 1.866(3) . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C8 1.535(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C8 1.531(3) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.537(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 P1 1.864(3) . ? C9 O1 1.335(3) . ? C9 N1 1.355(3) . ? C9 C10 1.402(4) . ? C10 N2 1.345(3) . ? C10 C11 1.486(3) . ? C11 C16 1.393(3) . ? C11 C12 1.399(4) . ? C12 C13 1.384(4) . ? C12 H12 0.9500 . ? C13 C14 1.389(4) . ? C13 H13 0.9500 . ? C14 C15 1.389(4) . ? C14 H14 0.9500 . ? C15 C16 1.394(4) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N2 1.343(3) . ? C17 C24 1.394(4) . ? C17 C18 1.485(3) . ? C18 C23 1.396(4) . ? C18 C19 1.400(4) . ? C19 C20 1.386(4) . ? C19 H19 0.9500 . ? C20 C21 1.387(4) . ? C20 H20 0.9500 . ? C21 C22 1.391(4) . ? C21 H21 0.9500 . ? C22 C23 1.390(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O2 1.342(3) . ? C24 N1 1.357(3) . ? C25 C28 1.524(4) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C28 1.518(4) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C28 C031 1.528(4) . ? C28 P2 1.867(3) . ? C29 C32 1.527(4) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.526(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C031 H03A 0.9800 . ? C031 H03B 0.9800 . ? C031 H03C 0.9800 . ? C31 C32 1.538(4) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 P2 1.866(2) . ? N1 Rh1 1.998(2) . ? O1 P1 1.7038(18) . ? O2 P2 1.6991(19) . ? P1 Rh1 2.2572(6) . ? P2 Rh1 2.2532(6) . ? Rh1 I1 2.6348(2) . ? C100 C101 1.357(6) . ? C100 C102 1.387(6) . ? C100 H100 0.9500 . ? C101 C102 1.381(6) 2_676 ? C101 H101 0.9500 . ? C102 C101 1.381(6) 2_676 ? C102 C103 1.398(10) . ? C103 H10A 0.9800 . ? C103 H10B 0.9800 . ? C103 H10C 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 C3 C1 H1A 109.5 . . ? C3 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C3 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C2 C3 C4 109.9(2) . . ? C2 C3 C1 109.1(2) . . ? C4 C3 C1 109.0(2) . . ? C2 C3 P1 108.96(19) . . ? C4 C3 P1 115.24(18) . . ? C1 C3 P1 104.44(17) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C8 C5 H5A 109.5 . . ? C8 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C8 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C8 C6 H6A 109.5 . . ? C8 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C8 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 C5 110.6(2) . . ? C6 C8 C7 108.9(2) . . ? C5 C8 C7 109.0(2) . . ? C6 C8 P1 114.17(18) . . ? C5 C8 P1 109.64(18) . . ? C7 C8 P1 104.20(18) . . ? O1 C9 N1 117.8(2) . . ? O1 C9 C10 120.4(2) . . ? N1 C9 C10 121.8(2) . . ? N2 C10 C9 119.8(2) . . ? N2 C10 C11 117.6(2) . . ? C9 C10 C11 122.5(2) . . ? C16 C11 C12 119.0(2) . . ? C16 C11 C10 120.1(2) . . ? C12 C11 C10 120.8(2) . . ? C13 C12 C11 120.5(2) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C12 C13 C14 120.3(2) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C15 C14 C13 119.7(2) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C14 C15 C16 120.1(2) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C11 C16 C15 120.4(2) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? N2 C17 C24 120.2(2) . . ? N2 C17 C18 117.9(2) . . ? C24 C17 C18 121.8(2) . . ? C23 C18 C19 119.3(2) . . ? C23 C18 C17 121.8(2) . . ? C19 C18 C17 119.0(2) . . ? C20 C19 C18 120.4(2) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 120.3(2) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C22 119.6(2) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C23 C22 C21 120.5(2) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C18 119.9(2) . . ? C22 C23 H23 120.0 . . ? C18 C23 H23 120.0 . . ? O2 C24 N1 117.4(2) . . ? O2 C24 C17 120.9(2) . . ? N1 C24 C17 121.7(2) . . ? C28 C25 H25A 109.5 . . ? C28 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C28 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 H26A 109.5 . . ? C28 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C28 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C26 C28 C25 111.4(3) . . ? C26 C28 C031 108.7(3) . . ? C25 C28 C031 107.5(3) . . ? C26 C28 P2 108.8(2) . . ? C25 C28 P2 115.9(2) . . ? C031 C28 P2 104.18(18) . . ? C32 C29 H29A 109.5 . . ? C32 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C32 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 H30A 109.5 . . ? C32 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C32 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C031 H03A 109.5 . . ? C28 C031 H03B 109.5 . . ? H03A C031 H03B 109.5 . . ? C28 C031 H03C 109.5 . . ? H03A C031 H03C 109.5 . . ? H03B C031 H03C 109.5 . . ? C32 C31 H31A 109.5 . . ? C32 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C32 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C30 C32 C29 111.4(3) . . ? C30 C32 C31 107.9(2) . . ? C29 C32 C31 108.8(3) . . ? C30 C32 P2 114.89(19) . . ? C29 C32 P2 108.9(2) . . ? C31 C32 P2 104.66(18) . . ? C9 N1 C24 116.8(2) . . ? C9 N1 Rh1 121.56(16) . . ? C24 N1 Rh1 121.49(16) . . ? C17 N2 C10 119.3(2) . . ? C9 O1 P1 118.07(15) . . ? C24 O2 P2 118.15(16) . . ? O1 P1 C8 98.48(10) . . ? O1 P1 C3 98.45(10) . . ? C8 P1 C3 113.63(12) . . ? O1 P1 Rh1 100.68(6) . . ? C8 P1 Rh1 119.03(9) . . ? C3 P1 Rh1 119.76(8) . . ? O2 P2 C32 97.78(11) . . ? O2 P2 C28 98.90(11) . . ? C32 P2 C28 113.12(12) . . ? O2 P2 Rh1 100.90(6) . . ? C32 P2 Rh1 121.10(9) . . ? C28 P2 Rh1 118.19(8) . . ? N1 Rh1 P2 81.66(6) . . ? N1 Rh1 P1 81.65(6) . . ? P2 Rh1 P1 163.28(2) . . ? N1 Rh1 I1 177.21(6) . . ? P2 Rh1 I1 98.862(17) . . ? P1 Rh1 I1 97.854(17) . . ? C101 C100 C102 122.0(3) . . ? C101 C100 H100 119.0 . . ? C102 C100 H100 119.0 . . ? C100 C101 C102 119.4(4) . 2_676 ? C100 C101 H101 120.3 . . ? C102 C101 H101 120.3 2_676 . ? C101 C102 C100 118.7(4) 2_676 . ? C101 C102 C103 120.2(6) 2_676 . ? C100 C102 C103 121.2(6) . . ? C102 C103 H10A 109.5 . . ? C102 C103 H10B 109.5 . . ? H10A C103 H10B 109.5 . . ? C102 C103 H10C 109.5 . . ? H10A C103 H10C 109.5 . . ? H10B C103 H10C 109.5 . . ? 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 O1 C9 C10 N2 -174.1(2) . . . . ? N1 C9 C10 N2 4.1(3) . . . . ? O1 C9 C10 C11 5.4(3) . . . . ? N1 C9 C10 C11 -176.4(2) . . . . ? N2 C10 C11 C16 42.4(3) . . . . ? C9 C10 C11 C16 -137.1(3) . . . . ? N2 C10 C11 C12 -134.5(2) . . . . ? C9 C10 C11 C12 46.1(3) . . . . ? C16 C11 C12 C13 -1.2(4) . . . . ? C10 C11 C12 C13 175.6(2) . . . . ? C11 C12 C13 C14 1.7(4) . . . . ? C12 C13 C14 C15 -0.9(4) . . . . ? C13 C14 C15 C16 -0.5(4) . . . . ? C12 C11 C16 C15 -0.1(4) . . . . ? C10 C11 C16 C15 -177.0(2) . . . . ? C14 C15 C16 C11 0.9(4) . . . . ? N2 C17 C18 C23 134.4(2) . . . . ? C24 C17 C18 C23 -47.9(3) . . . . ? N2 C17 C18 C19 -45.4(3) . . . . ? C24 C17 C18 C19 132.3(3) . . . . ? C23 C18 C19 C20 0.9(4) . . . . ? C17 C18 C19 C20 -179.3(2) . . . . ? C18 C19 C20 C21 -1.8(4) . . . . ? C19 C20 C21 C22 0.9(4) . . . . ? C20 C21 C22 C23 1.0(4) . . . . ? C21 C22 C23 C18 -1.9(4) . . . . ? C19 C18 C23 C22 0.9(4) . . . . ? C17 C18 C23 C22 -178.9(2) . . . . ? N2 C17 C24 O2 -177.0(2) . . . . ? C18 C17 C24 O2 5.4(3) . . . . ? N2 C17 C24 N1 5.2(3) . . . . ? C18 C17 C24 N1 -172.4(2) . . . . ? O1 C9 N1 C24 179.1(2) . . . . ? C10 C9 N1 C24 0.8(3) . . . . ? O1 C9 N1 Rh1 3.6(3) . . . . ? C10 C9 N1 Rh1 -174.59(17) . . . . ? O2 C24 N1 C9 176.8(2) . . . . ? C17 C24 N1 C9 -5.4(3) . . . . ? O2 C24 N1 Rh1 -7.8(3) . . . . ? C17 C24 N1 Rh1 170.04(17) . . . . ? C24 C17 N2 C10 -0.1(3) . . . . ? C18 C17 N2 C10 177.6(2) . . . . ? C9 C10 N2 C17 -4.4(3) . . . . ? C11 C10 N2 C17 176.1(2) . . . . ? N1 C9 O1 P1 -5.9(3) . . . . ? C10 C9 O1 P1 172.31(17) . . . . ? N1 C24 O2 P2 5.4(3) . . . . ? C17 C24 O2 P2 -172.51(17) . . . . ? C9 O1 P1 C8 -116.79(18) . . . . ? C9 O1 P1 C3 127.62(18) . . . . ? C9 O1 P1 Rh1 5.03(17) . . . . ? C6 C8 P1 O1 -44.3(2) . . . . ? C5 C8 P1 O1 -169.08(18) . . . . ? C7 C8 P1 O1 74.41(19) . . . . ? C6 C8 P1 C3 58.8(2) . . . . ? C5 C8 P1 C3 -65.9(2) . . . . ? C7 C8 P1 C3 177.56(18) . . . . ? C6 C8 P1 Rh1 -151.58(17) . . . . ? C5 C8 P1 Rh1 83.6(2) . . . . ? C7 C8 P1 Rh1 -32.9(2) . . . . ? C2 C3 P1 O1 177.9(2) . . . . ? C4 C3 P1 O1 53.8(2) . . . . ? C1 C3 P1 O1 -65.7(2) . . . . ? C2 C3 P1 C8 74.7(2) . . . . ? C4 C3 P1 C8 -49.4(2) . . . . ? C1 C3 P1 C8 -168.85(19) . . . . ? C2 C3 P1 Rh1 -74.6(2) . . . . ? C4 C3 P1 Rh1 161.31(18) . . . . ? C1 C3 P1 Rh1 41.8(2) . . . . ? C24 O2 P2 C32 122.80(18) . . . . ? C24 O2 P2 C28 -122.21(18) . . . . ? C24 O2 P2 Rh1 -1.07(17) . . . . ? C30 C32 P2 O2 55.2(2) . . . . ? C29 C32 P2 O2 -179.1(3) . . . . ? C31 C32 P2 O2 -63.0(2) . . . . ? C30 C32 P2 C28 -48.0(2) . . . . ? C29 C32 P2 C28 77.7(3) . . . . ? C31 C32 P2 C28 -166.2(2) . . . . ? C30 C32 P2 Rh1 162.94(18) . . . . ? C29 C32 P2 Rh1 -71.4(3) . . . . ? C31 C32 P2 Rh1 44.8(2) . . . . ? C26 C28 P2 O2 -175.2(3) . . . . ? C25 C28 P2 O2 -48.8(3) . . . . ? C031 C28 P2 O2 69.0(2) . . . . ? C26 C28 P2 C32 -72.7(3) . . . . ? C25 C28 P2 C32 53.6(3) . . . . ? C031 C28 P2 C32 171.4(2) . . . . ? C26 C28 P2 Rh1 77.3(3) . . . . ? C25 C28 P2 Rh1 -156.4(2) . . . . ? C031 C28 P2 Rh1 -38.6(2) . . . . ? C9 N1 Rh1 P2 -179.29(19) . . . . ? C24 N1 Rh1 P2 5.50(17) . . . . ? C9 N1 Rh1 P1 -0.23(17) . . . . ? C24 N1 Rh1 P1 -175.44(18) . . . . ? O2 P2 Rh1 N1 -2.03(9) . . . . ? C32 P2 Rh1 N1 -108.12(12) . . . . ? C28 P2 Rh1 N1 104.36(11) . . . . ? O2 P2 Rh1 P1 -5.26(11) . . . . ? C32 P2 Rh1 P1 -111.36(12) . . . . ? C28 P2 Rh1 P1 101.12(12) . . . . ? O2 P2 Rh1 I1 175.20(6) . . . . ? C32 P2 Rh1 I1 69.11(10) . . . . ? C28 P2 Rh1 I1 -78.41(10) . . . . ? O1 P1 Rh1 N1 -2.25(8) . . . . ? C8 P1 Rh1 N1 103.79(11) . . . . ? C3 P1 Rh1 N1 -108.51(12) . . . . ? O1 P1 Rh1 P2 0.99(11) . . . . ? C8 P1 Rh1 P2 107.02(12) . . . . ? C3 P1 Rh1 P2 -105.28(12) . . . . ? O1 P1 Rh1 I1 -179.48(6) . . . . ? C8 P1 Rh1 I1 -73.44(10) . . . . ? C3 P1 Rh1 I1 74.26(10) . . . . ? C102 C100 C101 C102 0.2(6) . . . 2_676 ? C101 C100 C102 C101 -0.2(6) . . . 2_676 ? C101 C100 C102 C103 179.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 70.18 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.087 _refine_diff_density_min -0.983 _refine_diff_density_rms 0.085 # Attachment '- RhMe.cif' data_RhMe _database_code_depnum_ccdc_archive 'CCDC 834661' #TrackingRef '- RhMe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H49 N2 O2 P2 Rh' _chemical_formula_weight 670.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1771(2) _cell_length_b 12.8681(3) _cell_length_c 23.2854(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.7390(10) _cell_angle_gamma 90.00 _cell_volume 3337.64(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9827 _cell_measurement_theta_min 3.81 _cell_measurement_theta_max 67.68 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 5.275 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.3006 _exptl_absorpt_correction_T_max 0.7784 _exptl_absorpt_process_details '(Bruker SADABS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49137 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 68.01 _reflns_number_total 5872 _reflns_number_gt 5610 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0351P)^2^+2.1536P] 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 5872 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.34470(18) -0.10943(15) 0.16841(8) 0.0218(4) Uani 1 1 d . . . C2 C 0.4265(2) -0.01613(18) 0.18439(10) 0.0345(5) Uani 1 1 d . . . H2A H 0.3828 0.0345 0.2062 0.052 Uiso 1 1 calc R . . H2B H 0.4509 0.0165 0.1492 0.052 Uiso 1 1 calc R . . H2C H 0.4979 -0.0399 0.2080 0.052 Uiso 1 1 calc R . . C3 C 0.3031(2) -0.15713(19) 0.22349(9) 0.0332(5) Uani 1 1 d . . . H3A H 0.2563 -0.2201 0.2139 0.050 Uiso 1 1 calc R . . H3B H 0.2531 -0.1069 0.2422 0.050 Uiso 1 1 calc R . . H3C H 0.3732 -0.1750 0.2497 0.050 Uiso 1 1 calc R . . C4 C 0.4170(2) -0.18894(19) 0.13675(10) 0.0372(5) Uani 1 1 d . . . H4A H 0.4867 -0.2114 0.1620 0.056 Uiso 1 1 calc R . . H4B H 0.4444 -0.1572 0.1019 0.056 Uiso 1 1 calc R . . H4C H 0.3663 -0.2492 0.1261 0.056 Uiso 1 1 calc R . . C5 C 0.09363(17) -0.15062(14) 0.10541(8) 0.0195(4) Uani 1 1 d . . . C6 C 0.01669(19) -0.16611(18) 0.15624(9) 0.0286(5) Uani 1 1 d . . . H6A H -0.0082 -0.0983 0.1702 0.043 Uiso 1 1 calc R . . H6B H 0.0636 -0.2028 0.1873 0.043 Uiso 1 1 calc R . . H6C H -0.0546 -0.2071 0.1437 0.043 Uiso 1 1 calc R . . C7 C 0.1395(2) -0.25497(15) 0.08481(9) 0.0280(4) Uani 1 1 d . . . H7A H 0.1808 -0.2921 0.1174 0.042 Uiso 1 1 calc R . . H7B H 0.1955 -0.2431 0.0553 0.042 Uiso 1 1 calc R . . H7C H 0.0716 -0.2967 0.0685 0.042 Uiso 1 1 calc R . . C8 C 0.01484(18) -0.09887(15) 0.05604(8) 0.0233(4) Uani 1 1 d . . . H8A H -0.0552 -0.1427 0.0455 0.035 Uiso 1 1 calc R . . H8B H 0.0616 -0.0903 0.0225 0.035 Uiso 1 1 calc R . . H8C H -0.0119 -0.0307 0.0687 0.035 Uiso 1 1 calc R . . C9 C 0.27269(16) 0.05065(13) 0.03556(7) 0.0151(3) Uani 1 1 d . . . C10 C 0.30547(15) 0.06121(13) -0.02056(7) 0.0149(3) Uani 1 1 d . . . C11 C 0.32831(16) -0.02846(13) -0.05836(7) 0.0159(3) Uani 1 1 d . . . C12 C 0.39883(17) -0.11303(13) -0.03931(8) 0.0179(4) Uani 1 1 d . . . H12 H 0.4319 -0.1161 -0.0004 0.021 Uiso 1 1 calc R . . C13 C 0.42074(17) -0.19284(14) -0.07721(8) 0.0205(4) Uani 1 1 d . . . H13 H 0.4703 -0.2496 -0.0644 0.025 Uiso 1 1 calc R . . C14 C 0.37045(18) -0.18994(14) -0.13371(8) 0.0212(4) Uani 1 1 d . . . H14 H 0.3851 -0.2450 -0.1594 0.025 Uiso 1 1 calc R . . C15 C 0.29888(19) -0.10689(14) -0.15270(8) 0.0211(4) Uani 1 1 d . . . H15 H 0.2636 -0.1053 -0.1912 0.025 Uiso 1 1 calc R . . C16 C 0.27883(17) -0.02602(14) -0.11526(8) 0.0189(4) Uani 1 1 d . . . H16 H 0.2310 0.0315 -0.1285 0.023 Uiso 1 1 calc R . . C17 C 0.28622(16) 0.24020(13) -0.01379(7) 0.0153(3) Uani 1 1 d . . . C18 C 0.30405(16) 0.34164(14) -0.04253(8) 0.0175(4) Uani 1 1 d . . . C19 C 0.30166(18) 0.34391(15) -0.10266(8) 0.0238(4) Uani 1 1 d . . . H19 H 0.2832 0.2824 -0.1241 0.029 Uiso 1 1 calc R . . C20 C 0.3259(2) 0.43485(17) -0.13115(9) 0.0289(5) Uani 1 1 d . . . H20 H 0.3231 0.4356 -0.1720 0.035 Uiso 1 1 calc R . . C21 C 0.35418(19) 0.52464(16) -0.10036(10) 0.0284(4) Uani 1 1 d . . . H21 H 0.3723 0.5867 -0.1200 0.034 Uiso 1 1 calc R . . C22 C 0.35596(18) 0.52392(15) -0.04086(9) 0.0264(4) Uani 1 1 d . . . H22 H 0.3746 0.5857 -0.0197 0.032 Uiso 1 1 calc R . . C23 C 0.33062(17) 0.43323(15) -0.01207(8) 0.0221(4) Uani 1 1 d . . . H23 H 0.3314 0.4335 0.0288 0.026 Uiso 1 1 calc R . . C24 C 0.24407(16) 0.22806(13) 0.04076(7) 0.0152(3) Uani 1 1 d . . . C25 C 0.24961(18) 0.37154(15) 0.18136(8) 0.0218(4) Uani 1 1 d . . . C26 C 0.2452(2) 0.48777(17) 0.16807(10) 0.0356(5) Uani 1 1 d . . . H26A H 0.1702 0.5171 0.1800 0.053 Uiso 1 1 calc R . . H26B H 0.2490 0.4984 0.1266 0.053 Uiso 1 1 calc R . . H26C H 0.3136 0.5224 0.1891 0.053 Uiso 1 1 calc R . . C27 C 0.2240(2) 0.3528(2) 0.24407(9) 0.0337(5) Uani 1 1 d . . . H27A H 0.2841 0.3893 0.2697 0.051 Uiso 1 1 calc R . . H27B H 0.2278 0.2782 0.2523 0.051 Uiso 1 1 calc R . . H27C H 0.1438 0.3791 0.2503 0.051 Uiso 1 1 calc R . . C28 C 0.37570(19) 0.33072(18) 0.17285(9) 0.0295(5) Uani 1 1 d . . . H28A H 0.3950 0.3451 0.1333 0.044 Uiso 1 1 calc R . . H28B H 0.3784 0.2556 0.1797 0.044 Uiso 1 1 calc R . . H28C H 0.4343 0.3654 0.2000 0.044 Uiso 1 1 calc R . . C29 C -0.00344(17) 0.34728(15) 0.11660(8) 0.0198(4) Uani 1 1 d . . . C30 C -0.0037(2) 0.45309(17) 0.08652(10) 0.0328(5) Uani 1 1 d . . . H30A H -0.0856 0.4704 0.0714 0.049 Uiso 1 1 calc R . . H30B H 0.0485 0.4502 0.0547 0.049 Uiso 1 1 calc R . . H30C H 0.0260 0.5064 0.1142 0.049 Uiso 1 1 calc R . . C31 C -0.06774(19) 0.35303(18) 0.17205(9) 0.0288(4) Uani 1 1 d . . . H31A H -0.0276 0.4042 0.1982 0.043 Uiso 1 1 calc R . . H31B H -0.0654 0.2847 0.1907 0.043 Uiso 1 1 calc R . . H31C H -0.1514 0.3738 0.1628 0.043 Uiso 1 1 calc R . . C32 C -0.07042(19) 0.26887(17) 0.07544(9) 0.0279(4) Uani 1 1 d . . . H32A H -0.0722 0.2008 0.0943 0.042 Uiso 1 1 calc R . . H32B H -0.0288 0.2629 0.0401 0.042 Uiso 1 1 calc R . . H32C H -0.1527 0.2931 0.0658 0.042 Uiso 1 1 calc R . . C33 C 0.07651(19) 0.09417(14) 0.22081(8) 0.0222(4) Uani 1 1 d . . . H33A H 0.0811 0.1591 0.2429 0.033 Uiso 1 1 calc R . . H33B H 0.1166 0.0386 0.2438 0.033 Uiso 1 1 calc R . . H33C H -0.0079 0.0757 0.2113 0.033 Uiso 1 1 calc R . . N1 N 0.23742(13) 0.13364(11) 0.06546(6) 0.0147(3) Uani 1 1 d . . . N2 N 0.31252(13) 0.15558(11) -0.04376(6) 0.0160(3) Uani 1 1 d . . . O1 O 0.27137(11) -0.04273(9) 0.06120(5) 0.0169(3) Uani 1 1 d . . . O2 O 0.20551(11) 0.30991(9) 0.07022(5) 0.0175(3) Uani 1 1 d . . . P1 P 0.21169(4) -0.05161(3) 0.126109(18) 0.01499(10) Uani 1 1 d . . . P2 P 0.14651(4) 0.28672(3) 0.134368(18) 0.01570(10) Uani 1 1 d . . . Rh1 Rh 0.164030(12) 0.114517(10) 0.142293(5) 0.01517(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0166(10) 0.0277(10) 0.0208(9) 0.0078(7) 0.0003(7) 0.0011(7) C2 0.0212(12) 0.0417(13) 0.0387(12) 0.0093(10) -0.0083(9) -0.0071(9) C3 0.0241(12) 0.0493(14) 0.0255(10) 0.0179(10) -0.0021(8) -0.0010(9) C4 0.0280(13) 0.0452(13) 0.0383(12) 0.0082(10) 0.0025(9) 0.0178(10) C5 0.0182(10) 0.0208(9) 0.0194(9) 0.0014(7) 0.0008(7) -0.0032(7) C6 0.0224(11) 0.0386(12) 0.0251(10) 0.0033(9) 0.0042(8) -0.0115(9) C7 0.0359(13) 0.0178(9) 0.0297(11) 0.0000(8) -0.0004(9) -0.0015(8) C8 0.0195(11) 0.0262(10) 0.0234(10) -0.0002(8) -0.0032(8) -0.0014(7) C9 0.0109(9) 0.0160(8) 0.0182(8) 0.0011(7) 0.0007(6) 0.0002(6) C10 0.0103(9) 0.0175(8) 0.0169(8) 0.0008(7) 0.0014(6) 0.0001(6) C11 0.0134(9) 0.0166(8) 0.0183(8) 0.0000(7) 0.0056(7) -0.0029(6) C12 0.0150(10) 0.0200(9) 0.0190(9) 0.0009(7) 0.0032(7) -0.0009(7) C13 0.0194(10) 0.0168(9) 0.0259(9) 0.0004(7) 0.0049(7) 0.0014(7) C14 0.0223(10) 0.0180(9) 0.0243(9) -0.0053(7) 0.0084(7) -0.0041(7) C15 0.0215(11) 0.0240(10) 0.0179(9) -0.0011(7) 0.0029(7) -0.0036(7) C16 0.0175(10) 0.0197(9) 0.0198(9) 0.0018(7) 0.0032(7) 0.0010(7) C17 0.0100(9) 0.0175(9) 0.0184(8) 0.0002(7) 0.0008(6) -0.0007(6) C18 0.0108(9) 0.0184(9) 0.0236(9) 0.0030(7) 0.0035(7) 0.0017(6) C19 0.0258(11) 0.0211(10) 0.0250(10) 0.0017(8) 0.0061(8) -0.0003(8) C20 0.0333(13) 0.0285(11) 0.0257(10) 0.0089(8) 0.0070(8) 0.0027(8) C21 0.0234(11) 0.0219(10) 0.0406(12) 0.0121(9) 0.0067(9) 0.0000(8) C22 0.0217(11) 0.0194(9) 0.0379(11) 0.0013(8) 0.0023(8) -0.0021(8) C23 0.0186(10) 0.0214(9) 0.0264(10) 0.0012(8) 0.0031(7) -0.0021(7) C24 0.0100(9) 0.0167(8) 0.0188(8) -0.0008(7) -0.0001(6) -0.0006(6) C25 0.0178(10) 0.0252(10) 0.0222(10) -0.0075(7) 0.0012(7) -0.0014(7) C26 0.0353(13) 0.0268(11) 0.0436(13) -0.0097(9) -0.0038(10) -0.0054(9) C27 0.0276(12) 0.0521(14) 0.0213(10) -0.0104(10) 0.0019(8) -0.0094(10) C28 0.0174(11) 0.0381(12) 0.0326(11) -0.0114(9) -0.0004(8) -0.0004(8) C29 0.0155(10) 0.0223(9) 0.0219(9) -0.0014(7) 0.0027(7) 0.0015(7) C30 0.0231(12) 0.0295(11) 0.0457(13) 0.0104(9) 0.0023(9) 0.0054(8) C31 0.0197(11) 0.0421(12) 0.0252(10) -0.0043(9) 0.0049(8) 0.0075(9) C32 0.0194(11) 0.0361(11) 0.0276(10) -0.0077(9) -0.0024(8) 0.0010(8) C33 0.0269(11) 0.0157(8) 0.0244(10) 0.0013(7) 0.0054(8) 0.0006(7) N1 0.0123(8) 0.0171(7) 0.0145(7) 0.0000(6) 0.0010(5) -0.0006(6) N2 0.0127(8) 0.0170(7) 0.0182(7) 0.0012(6) 0.0015(6) -0.0001(6) O1 0.0193(7) 0.0155(6) 0.0164(6) 0.0022(5) 0.0049(5) 0.0022(5) O2 0.0194(7) 0.0156(6) 0.0181(6) -0.0011(5) 0.0053(5) 0.0000(5) P1 0.0141(2) 0.0169(2) 0.0141(2) 0.00218(16) 0.00206(16) 0.00017(16) P2 0.0152(2) 0.0165(2) 0.0157(2) -0.00228(16) 0.00322(16) -0.00011(16) Rh1 0.01624(9) 0.01637(8) 0.01330(8) -0.00003(4) 0.00368(5) -0.00003(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 C1 C3 1.529(3) . ? C1 C4 1.531(3) . ? C1 C2 1.536(3) . ? C1 P1 1.869(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.528(3) . ? C5 C6 1.533(3) . ? C5 C8 1.540(3) . ? C5 P1 1.8686(19) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O1 1.342(2) . ? C9 N1 1.351(2) . ? C9 C10 1.393(2) . ? C10 N2 1.334(2) . ? C10 C11 1.486(2) . ? C11 C16 1.393(3) . ? C11 C12 1.394(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N2 1.339(2) . ? C17 C24 1.400(2) . ? C17 C18 1.488(2) . ? C18 C23 1.395(3) . ? C18 C19 1.398(3) . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 C21 1.382(3) . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O2 1.347(2) . ? C24 N1 1.349(2) . ? C25 C26 1.527(3) . ? C25 C27 1.530(3) . ? C25 C28 1.532(3) . ? C25 P2 1.8730(19) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.530(3) . ? C29 C30 1.531(3) . ? C29 C32 1.542(3) . ? C29 P2 1.8636(19) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 Rh1 2.1596(19) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? N1 Rh1 2.0437(15) . ? O1 P1 1.7055(12) . ? O2 P2 1.7082(12) . ? P1 Rh1 2.2425(5) . ? P2 Rh1 2.2308(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 C3 C1 C4 110.19(17) . . ? C3 C1 C2 109.07(18) . . ? C4 C1 C2 108.17(18) . . ? C3 C1 P1 108.56(14) . . ? C4 C1 P1 116.19(14) . . ? C2 C1 P1 104.36(13) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 C6 110.62(16) . . ? C7 C5 C8 109.36(16) . . ? C6 C5 C8 108.05(16) . . ? C7 C5 P1 115.60(14) . . ? C6 C5 P1 108.59(13) . . ? C8 C5 P1 104.23(12) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 N1 117.63(15) . . ? O1 C9 C10 121.21(15) . . ? N1 C9 C10 121.13(16) . . ? N2 C10 C9 119.84(16) . . ? N2 C10 C11 116.64(15) . . ? C9 C10 C11 123.46(15) . . ? C16 C11 C12 119.31(16) . . ? C16 C11 C10 118.14(16) . . ? C12 C11 C10 122.54(16) . . ? C13 C12 C11 119.98(17) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.24(17) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.08(17) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.80(18) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.57(17) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? N2 C17 C24 119.15(16) . . ? N2 C17 C18 115.84(15) . . ? C24 C17 C18 125.02(16) . . ? C23 C18 C19 118.50(17) . . ? C23 C18 C17 122.91(17) . . ? C19 C18 C17 118.45(16) . . ? C20 C19 C18 120.64(19) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 120.26(19) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.81(18) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 120.20(19) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 120.57(18) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? O2 C24 N1 117.13(15) . . ? O2 C24 C17 121.38(15) . . ? N1 C24 C17 121.47(16) . . ? C26 C25 C27 109.99(18) . . ? C26 C25 C28 108.91(18) . . ? C27 C25 C28 108.42(17) . . ? C26 C25 P2 116.38(15) . . ? C27 C25 P2 108.15(14) . . ? C28 C25 P2 104.64(13) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C30 111.09(17) . . ? C31 C29 C32 108.56(17) . . ? C30 C29 C32 108.37(17) . . ? C31 C29 P2 108.02(13) . . ? C30 C29 P2 116.16(14) . . ? C32 C29 P2 104.23(13) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Rh1 C33 H33A 109.5 . . ? Rh1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Rh1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C24 N1 C9 117.61(15) . . ? C24 N1 Rh1 121.46(12) . . ? C9 N1 Rh1 120.74(12) . . ? C10 N2 C17 120.43(15) . . ? C9 O1 P1 118.27(11) . . ? C24 O2 P2 118.14(11) . . ? O1 P1 C5 97.85(7) . . ? O1 P1 C1 98.13(8) . . ? C5 P1 C1 112.25(9) . . ? O1 P1 Rh1 101.58(4) . . ? C5 P1 Rh1 121.39(6) . . ? C1 P1 Rh1 118.73(6) . . ? O2 P2 C29 97.93(7) . . ? O2 P2 C25 98.38(8) . . ? C29 P2 C25 112.62(9) . . ? O2 P2 Rh1 102.02(4) . . ? C29 P2 Rh1 120.33(6) . . ? C25 P2 Rh1 119.01(6) . . ? N1 Rh1 C33 176.73(7) . . ? N1 Rh1 P2 81.19(4) . . ? C33 Rh1 P2 98.49(5) . . ? N1 Rh1 P1 81.35(4) . . ? C33 Rh1 P1 99.05(5) . . ? P2 Rh1 P1 162.447(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 O1 C9 C10 N2 -176.21(15) . . . . ? N1 C9 C10 N2 5.9(3) . . . . ? O1 C9 C10 C11 6.8(3) . . . . ? N1 C9 C10 C11 -171.07(16) . . . . ? N2 C10 C11 C16 -42.1(2) . . . . ? C9 C10 C11 C16 134.98(18) . . . . ? N2 C10 C11 C12 136.58(18) . . . . ? C9 C10 C11 C12 -46.3(3) . . . . ? C16 C11 C12 C13 1.1(3) . . . . ? C10 C11 C12 C13 -177.59(16) . . . . ? C11 C12 C13 C14 -1.5(3) . . . . ? C12 C13 C14 C15 0.5(3) . . . . ? C13 C14 C15 C16 0.8(3) . . . . ? C14 C15 C16 C11 -1.2(3) . . . . ? C12 C11 C16 C15 0.2(3) . . . . ? C10 C11 C16 C15 178.96(16) . . . . ? N2 C17 C18 C23 -152.25(17) . . . . ? C24 C17 C18 C23 28.3(3) . . . . ? N2 C17 C18 C19 23.5(2) . . . . ? C24 C17 C18 C19 -155.96(18) . . . . ? C23 C18 C19 C20 0.4(3) . . . . ? C17 C18 C19 C20 -175.54(18) . . . . ? C18 C19 C20 C21 0.7(3) . . . . ? C19 C20 C21 C22 -1.2(3) . . . . ? C20 C21 C22 C23 0.6(3) . . . . ? C21 C22 C23 C18 0.5(3) . . . . ? C19 C18 C23 C22 -1.0(3) . . . . ? C17 C18 C23 C22 174.74(17) . . . . ? N2 C17 C24 O2 -173.53(15) . . . . ? C18 C17 C24 O2 5.9(3) . . . . ? N2 C17 C24 N1 4.7(3) . . . . ? C18 C17 C24 N1 -175.78(16) . . . . ? O2 C24 N1 C9 178.17(15) . . . . ? C17 C24 N1 C9 -0.2(2) . . . . ? O2 C24 N1 Rh1 3.1(2) . . . . ? C17 C24 N1 Rh1 -175.27(13) . . . . ? O1 C9 N1 C24 176.98(15) . . . . ? C10 C9 N1 C24 -5.1(2) . . . . ? O1 C9 N1 Rh1 -7.9(2) . . . . ? C10 C9 N1 Rh1 170.05(13) . . . . ? C9 C10 N2 C17 -1.2(2) . . . . ? C11 C10 N2 C17 176.01(16) . . . . ? C24 C17 N2 C10 -4.0(2) . . . . ? C18 C17 N2 C10 176.53(15) . . . . ? N1 C9 O1 P1 6.4(2) . . . . ? C10 C9 O1 P1 -171.56(13) . . . . ? N1 C24 O2 P2 -2.5(2) . . . . ? C17 C24 O2 P2 175.80(13) . . . . ? C9 O1 P1 C5 122.15(13) . . . . ? C9 O1 P1 C1 -123.91(13) . . . . ? C9 O1 P1 Rh1 -2.25(13) . . . . ? C7 C5 P1 O1 60.20(14) . . . . ? C6 C5 P1 O1 -174.84(13) . . . . ? C8 C5 P1 O1 -59.84(13) . . . . ? C7 C5 P1 C1 -41.96(16) . . . . ? C6 C5 P1 C1 83.00(15) . . . . ? C8 C5 P1 C1 -162.00(12) . . . . ? C7 C5 P1 Rh1 168.96(11) . . . . ? C6 C5 P1 Rh1 -66.08(15) . . . . ? C8 C5 P1 Rh1 48.92(14) . . . . ? C3 C1 P1 O1 -162.25(14) . . . . ? C4 C1 P1 O1 -37.45(17) . . . . ? C2 C1 P1 O1 81.53(14) . . . . ? C3 C1 P1 C5 -60.27(17) . . . . ? C4 C1 P1 C5 64.53(18) . . . . ? C2 C1 P1 C5 -176.49(13) . . . . ? C3 C1 P1 Rh1 89.72(15) . . . . ? C4 C1 P1 Rh1 -145.48(14) . . . . ? C2 C1 P1 Rh1 -26.50(16) . . . . ? C24 O2 P2 C29 -122.45(13) . . . . ? C24 O2 P2 C25 123.16(13) . . . . ? C24 O2 P2 Rh1 0.98(13) . . . . ? C31 C29 P2 O2 -170.42(13) . . . . ? C30 C29 P2 O2 -44.87(16) . . . . ? C32 C29 P2 O2 74.26(13) . . . . ? C31 C29 P2 C25 -67.86(16) . . . . ? C30 C29 P2 C25 57.69(17) . . . . ? C32 C29 P2 C25 176.82(13) . . . . ? C31 C29 P2 Rh1 80.61(14) . . . . ? C30 C29 P2 Rh1 -153.84(13) . . . . ? C32 C29 P2 Rh1 -34.71(15) . . . . ? C26 C25 P2 O2 62.83(16) . . . . ? C27 C25 P2 O2 -172.82(14) . . . . ? C28 C25 P2 O2 -57.40(14) . . . . ? C26 C25 P2 C29 -39.43(18) . . . . ? C27 C25 P2 C29 84.92(16) . . . . ? C28 C25 P2 C29 -159.66(13) . . . . ? C26 C25 P2 Rh1 171.64(13) . . . . ? C27 C25 P2 Rh1 -64.01(16) . . . . ? C28 C25 P2 Rh1 51.41(15) . . . . ? C24 N1 Rh1 P2 -1.90(12) . . . . ? C9 N1 Rh1 P2 -176.83(14) . . . . ? C24 N1 Rh1 P1 179.89(13) . . . . ? C9 N1 Rh1 P1 4.95(13) . . . . ? O2 P2 Rh1 N1 0.40(6) . . . . ? C29 P2 Rh1 N1 107.14(8) . . . . ? C25 P2 Rh1 N1 -106.36(8) . . . . ? O2 P2 Rh1 C33 -176.31(7) . . . . ? C29 P2 Rh1 C33 -69.58(9) . . . . ? C25 P2 Rh1 C33 76.92(9) . . . . ? O2 P2 Rh1 P1 6.26(8) . . . . ? C29 P2 Rh1 P1 112.99(9) . . . . ? C25 P2 Rh1 P1 -100.51(9) . . . . ? O1 P1 Rh1 N1 -1.22(6) . . . . ? C5 P1 Rh1 N1 -107.98(8) . . . . ? C1 P1 Rh1 N1 104.86(8) . . . . ? O1 P1 Rh1 C33 175.50(7) . . . . ? C5 P1 Rh1 C33 68.74(9) . . . . ? C1 P1 Rh1 C33 -78.42(9) . . . . ? O1 P1 Rh1 P2 -7.07(8) . . . . ? C5 P1 Rh1 P2 -113.84(8) . . . . ? C1 P1 Rh1 P2 99.00(9) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 68.01 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.481 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.058 # Attachment '- RhMe.cif' data_RhMe_2 _database_code_depnum_ccdc_archive 'CCDC 834662' #TrackingRef '- RhMe.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H49 N2 O2 P2 Rh' _chemical_formula_weight 670.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh 0.0927 3.6045 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1771(2) _cell_length_b 12.8681(3) _cell_length_c 23.2854(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.7390(10) _cell_angle_gamma 90.00 _cell_volume 3337.64(12) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9827 _cell_measurement_theta_min 3.81 _cell_measurement_theta_max 67.68 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 5.275 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.3006 _exptl_absorpt_correction_T_max 0.7784 _exptl_absorpt_process_details '(Bruker SADABS, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49137 _diffrn_reflns_av_R_equivalents 0.0289 _diffrn_reflns_av_sigmaI/netI 0.0151 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.81 _diffrn_reflns_theta_max 68.01 _reflns_number_total 5872 _reflns_number_gt 5610 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _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^)+(0.0351P)^2^+2.1536P] 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 5872 _refine_ls_number_parameters 374 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0244 _refine_ls_R_factor_gt 0.0232 _refine_ls_wR_factor_ref 0.0613 _refine_ls_wR_factor_gt 0.0604 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.34470(18) -0.10943(15) 0.16841(8) 0.0218(4) Uani 1 1 d . . . C2 C 0.4265(2) -0.01613(18) 0.18439(10) 0.0345(5) Uani 1 1 d . . . H2A H 0.3828 0.0345 0.2062 0.052 Uiso 1 1 calc R . . H2B H 0.4509 0.0165 0.1492 0.052 Uiso 1 1 calc R . . H2C H 0.4979 -0.0399 0.2080 0.052 Uiso 1 1 calc R . . C3 C 0.3031(2) -0.15713(19) 0.22349(9) 0.0332(5) Uani 1 1 d . . . H3A H 0.2563 -0.2201 0.2139 0.050 Uiso 1 1 calc R . . H3B H 0.2531 -0.1069 0.2422 0.050 Uiso 1 1 calc R . . H3C H 0.3732 -0.1750 0.2497 0.050 Uiso 1 1 calc R . . C4 C 0.4170(2) -0.18894(19) 0.13675(10) 0.0372(5) Uani 1 1 d . . . H4A H 0.4867 -0.2114 0.1620 0.056 Uiso 1 1 calc R . . H4B H 0.4444 -0.1572 0.1019 0.056 Uiso 1 1 calc R . . H4C H 0.3663 -0.2492 0.1261 0.056 Uiso 1 1 calc R . . C5 C 0.09363(17) -0.15062(14) 0.10541(8) 0.0195(4) Uani 1 1 d . . . C6 C 0.01669(19) -0.16611(18) 0.15624(9) 0.0286(5) Uani 1 1 d . . . H6A H -0.0082 -0.0983 0.1702 0.043 Uiso 1 1 calc R . . H6B H 0.0636 -0.2028 0.1873 0.043 Uiso 1 1 calc R . . H6C H -0.0546 -0.2071 0.1437 0.043 Uiso 1 1 calc R . . C7 C 0.1395(2) -0.25497(15) 0.08481(9) 0.0280(4) Uani 1 1 d . . . H7A H 0.1808 -0.2921 0.1174 0.042 Uiso 1 1 calc R . . H7B H 0.1955 -0.2431 0.0553 0.042 Uiso 1 1 calc R . . H7C H 0.0716 -0.2967 0.0685 0.042 Uiso 1 1 calc R . . C8 C 0.01484(18) -0.09887(15) 0.05604(8) 0.0233(4) Uani 1 1 d . . . H8A H -0.0552 -0.1427 0.0455 0.035 Uiso 1 1 calc R . . H8B H 0.0616 -0.0903 0.0225 0.035 Uiso 1 1 calc R . . H8C H -0.0119 -0.0307 0.0687 0.035 Uiso 1 1 calc R . . C9 C 0.27269(16) 0.05065(13) 0.03556(7) 0.0151(3) Uani 1 1 d . . . C10 C 0.30547(15) 0.06121(13) -0.02056(7) 0.0149(3) Uani 1 1 d . . . C11 C 0.32831(16) -0.02846(13) -0.05836(7) 0.0159(3) Uani 1 1 d . . . C12 C 0.39883(17) -0.11303(13) -0.03931(8) 0.0179(4) Uani 1 1 d . . . H12 H 0.4319 -0.1161 -0.0004 0.021 Uiso 1 1 calc R . . C13 C 0.42074(17) -0.19284(14) -0.07721(8) 0.0205(4) Uani 1 1 d . . . H13 H 0.4703 -0.2496 -0.0644 0.025 Uiso 1 1 calc R . . C14 C 0.37045(18) -0.18994(14) -0.13371(8) 0.0212(4) Uani 1 1 d . . . H14 H 0.3851 -0.2450 -0.1594 0.025 Uiso 1 1 calc R . . C15 C 0.29888(19) -0.10689(14) -0.15270(8) 0.0211(4) Uani 1 1 d . . . H15 H 0.2636 -0.1053 -0.1912 0.025 Uiso 1 1 calc R . . C16 C 0.27883(17) -0.02602(14) -0.11526(8) 0.0189(4) Uani 1 1 d . . . H16 H 0.2310 0.0315 -0.1285 0.023 Uiso 1 1 calc R . . C17 C 0.28622(16) 0.24020(13) -0.01379(7) 0.0153(3) Uani 1 1 d . . . C18 C 0.30405(16) 0.34164(14) -0.04253(8) 0.0175(4) Uani 1 1 d . . . C19 C 0.30166(18) 0.34391(15) -0.10266(8) 0.0238(4) Uani 1 1 d . . . H19 H 0.2832 0.2824 -0.1241 0.029 Uiso 1 1 calc R . . C20 C 0.3259(2) 0.43485(17) -0.13115(9) 0.0289(5) Uani 1 1 d . . . H20 H 0.3231 0.4356 -0.1720 0.035 Uiso 1 1 calc R . . C21 C 0.35418(19) 0.52464(16) -0.10036(10) 0.0284(4) Uani 1 1 d . . . H21 H 0.3723 0.5867 -0.1200 0.034 Uiso 1 1 calc R . . C22 C 0.35596(18) 0.52392(15) -0.04086(9) 0.0264(4) Uani 1 1 d . . . H22 H 0.3746 0.5857 -0.0197 0.032 Uiso 1 1 calc R . . C23 C 0.33062(17) 0.43323(15) -0.01207(8) 0.0221(4) Uani 1 1 d . . . H23 H 0.3314 0.4335 0.0288 0.026 Uiso 1 1 calc R . . C24 C 0.24407(16) 0.22806(13) 0.04076(7) 0.0152(3) Uani 1 1 d . . . C25 C 0.24961(18) 0.37154(15) 0.18136(8) 0.0218(4) Uani 1 1 d . . . C26 C 0.2452(2) 0.48777(17) 0.16807(10) 0.0356(5) Uani 1 1 d . . . H26A H 0.1702 0.5171 0.1800 0.053 Uiso 1 1 calc R . . H26B H 0.2490 0.4984 0.1266 0.053 Uiso 1 1 calc R . . H26C H 0.3136 0.5224 0.1891 0.053 Uiso 1 1 calc R . . C27 C 0.2240(2) 0.3528(2) 0.24407(9) 0.0337(5) Uani 1 1 d . . . H27A H 0.2841 0.3893 0.2697 0.051 Uiso 1 1 calc R . . H27B H 0.2278 0.2782 0.2523 0.051 Uiso 1 1 calc R . . H27C H 0.1438 0.3791 0.2503 0.051 Uiso 1 1 calc R . . C28 C 0.37570(19) 0.33072(18) 0.17285(9) 0.0295(5) Uani 1 1 d . . . H28A H 0.3950 0.3451 0.1333 0.044 Uiso 1 1 calc R . . H28B H 0.3784 0.2556 0.1797 0.044 Uiso 1 1 calc R . . H28C H 0.4343 0.3654 0.2000 0.044 Uiso 1 1 calc R . . C29 C -0.00344(17) 0.34728(15) 0.11660(8) 0.0198(4) Uani 1 1 d . . . C30 C -0.0037(2) 0.45309(17) 0.08652(10) 0.0328(5) Uani 1 1 d . . . H30A H -0.0856 0.4704 0.0714 0.049 Uiso 1 1 calc R . . H30B H 0.0485 0.4502 0.0547 0.049 Uiso 1 1 calc R . . H30C H 0.0260 0.5064 0.1142 0.049 Uiso 1 1 calc R . . C31 C -0.06774(19) 0.35303(18) 0.17205(9) 0.0288(4) Uani 1 1 d . . . H31A H -0.0276 0.4042 0.1982 0.043 Uiso 1 1 calc R . . H31B H -0.0654 0.2847 0.1907 0.043 Uiso 1 1 calc R . . H31C H -0.1514 0.3738 0.1628 0.043 Uiso 1 1 calc R . . C32 C -0.07042(19) 0.26887(17) 0.07544(9) 0.0279(4) Uani 1 1 d . . . H32A H -0.0722 0.2008 0.0943 0.042 Uiso 1 1 calc R . . H32B H -0.0288 0.2629 0.0401 0.042 Uiso 1 1 calc R . . H32C H -0.1527 0.2931 0.0658 0.042 Uiso 1 1 calc R . . C33 C 0.07651(19) 0.09417(14) 0.22081(8) 0.0222(4) Uani 1 1 d . . . H33A H 0.0811 0.1591 0.2429 0.033 Uiso 1 1 calc R . . H33B H 0.1166 0.0386 0.2438 0.033 Uiso 1 1 calc R . . H33C H -0.0079 0.0757 0.2113 0.033 Uiso 1 1 calc R . . N1 N 0.23742(13) 0.13364(11) 0.06546(6) 0.0147(3) Uani 1 1 d . . . N2 N 0.31252(13) 0.15558(11) -0.04376(6) 0.0160(3) Uani 1 1 d . . . O1 O 0.27137(11) -0.04273(9) 0.06120(5) 0.0169(3) Uani 1 1 d . . . O2 O 0.20551(11) 0.30991(9) 0.07022(5) 0.0175(3) Uani 1 1 d . . . P1 P 0.21169(4) -0.05161(3) 0.126109(18) 0.01499(10) Uani 1 1 d . . . P2 P 0.14651(4) 0.28672(3) 0.134368(18) 0.01570(10) Uani 1 1 d . . . Rh1 Rh 0.164030(12) 0.114517(10) 0.142293(5) 0.01517(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0166(10) 0.0277(10) 0.0208(9) 0.0078(7) 0.0003(7) 0.0011(7) C2 0.0212(12) 0.0417(13) 0.0387(12) 0.0093(10) -0.0083(9) -0.0071(9) C3 0.0241(12) 0.0493(14) 0.0255(10) 0.0179(10) -0.0021(8) -0.0010(9) C4 0.0280(13) 0.0452(13) 0.0383(12) 0.0082(10) 0.0025(9) 0.0178(10) C5 0.0182(10) 0.0208(9) 0.0194(9) 0.0014(7) 0.0008(7) -0.0032(7) C6 0.0224(11) 0.0386(12) 0.0251(10) 0.0033(9) 0.0042(8) -0.0115(9) C7 0.0359(13) 0.0178(9) 0.0297(11) 0.0000(8) -0.0004(9) -0.0015(8) C8 0.0195(11) 0.0262(10) 0.0234(10) -0.0002(8) -0.0032(8) -0.0014(7) C9 0.0109(9) 0.0160(8) 0.0182(8) 0.0011(7) 0.0007(6) 0.0002(6) C10 0.0103(9) 0.0175(8) 0.0169(8) 0.0008(7) 0.0014(6) 0.0001(6) C11 0.0134(9) 0.0166(8) 0.0183(8) 0.0000(7) 0.0056(7) -0.0029(6) C12 0.0150(10) 0.0200(9) 0.0190(9) 0.0009(7) 0.0032(7) -0.0009(7) C13 0.0194(10) 0.0168(9) 0.0259(9) 0.0004(7) 0.0049(7) 0.0014(7) C14 0.0223(10) 0.0180(9) 0.0243(9) -0.0053(7) 0.0084(7) -0.0041(7) C15 0.0215(11) 0.0240(10) 0.0179(9) -0.0011(7) 0.0029(7) -0.0036(7) C16 0.0175(10) 0.0197(9) 0.0198(9) 0.0018(7) 0.0032(7) 0.0010(7) C17 0.0100(9) 0.0175(9) 0.0184(8) 0.0002(7) 0.0008(6) -0.0007(6) C18 0.0108(9) 0.0184(9) 0.0236(9) 0.0030(7) 0.0035(7) 0.0017(6) C19 0.0258(11) 0.0211(10) 0.0250(10) 0.0017(8) 0.0061(8) -0.0003(8) C20 0.0333(13) 0.0285(11) 0.0257(10) 0.0089(8) 0.0070(8) 0.0027(8) C21 0.0234(11) 0.0219(10) 0.0406(12) 0.0121(9) 0.0067(9) 0.0000(8) C22 0.0217(11) 0.0194(9) 0.0379(11) 0.0013(8) 0.0023(8) -0.0021(8) C23 0.0186(10) 0.0214(9) 0.0264(10) 0.0012(8) 0.0031(7) -0.0021(7) C24 0.0100(9) 0.0167(8) 0.0188(8) -0.0008(7) -0.0001(6) -0.0006(6) C25 0.0178(10) 0.0252(10) 0.0222(10) -0.0075(7) 0.0012(7) -0.0014(7) C26 0.0353(13) 0.0268(11) 0.0436(13) -0.0097(9) -0.0038(10) -0.0054(9) C27 0.0276(12) 0.0521(14) 0.0213(10) -0.0104(10) 0.0019(8) -0.0094(10) C28 0.0174(11) 0.0381(12) 0.0326(11) -0.0114(9) -0.0004(8) -0.0004(8) C29 0.0155(10) 0.0223(9) 0.0219(9) -0.0014(7) 0.0027(7) 0.0015(7) C30 0.0231(12) 0.0295(11) 0.0457(13) 0.0104(9) 0.0023(9) 0.0054(8) C31 0.0197(11) 0.0421(12) 0.0252(10) -0.0043(9) 0.0049(8) 0.0075(9) C32 0.0194(11) 0.0361(11) 0.0276(10) -0.0077(9) -0.0024(8) 0.0010(8) C33 0.0269(11) 0.0157(8) 0.0244(10) 0.0013(7) 0.0054(8) 0.0006(7) N1 0.0123(8) 0.0171(7) 0.0145(7) 0.0000(6) 0.0010(5) -0.0006(6) N2 0.0127(8) 0.0170(7) 0.0182(7) 0.0012(6) 0.0015(6) -0.0001(6) O1 0.0193(7) 0.0155(6) 0.0164(6) 0.0022(5) 0.0049(5) 0.0022(5) O2 0.0194(7) 0.0156(6) 0.0181(6) -0.0011(5) 0.0053(5) 0.0000(5) P1 0.0141(2) 0.0169(2) 0.0141(2) 0.00218(16) 0.00206(16) 0.00017(16) P2 0.0152(2) 0.0165(2) 0.0157(2) -0.00228(16) 0.00322(16) -0.00011(16) Rh1 0.01624(9) 0.01637(8) 0.01330(8) -0.00003(4) 0.00368(5) -0.00003(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 C1 C3 1.529(3) . ? C1 C4 1.531(3) . ? C1 C2 1.536(3) . ? C1 P1 1.869(2) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 C7 1.528(3) . ? C5 C6 1.533(3) . ? C5 C8 1.540(3) . ? C5 P1 1.8686(19) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 O1 1.342(2) . ? C9 N1 1.351(2) . ? C9 C10 1.393(2) . ? C10 N2 1.334(2) . ? C10 C11 1.486(2) . ? C11 C16 1.393(3) . ? C11 C12 1.394(3) . ? C12 C13 1.389(3) . ? C12 H12 0.9500 . ? C13 C14 1.388(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.388(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N2 1.339(2) . ? C17 C24 1.400(2) . ? C17 C18 1.488(2) . ? C18 C23 1.395(3) . ? C18 C19 1.398(3) . ? C19 C20 1.383(3) . ? C19 H19 0.9500 . ? C20 C21 1.382(3) . ? C20 H20 0.9500 . ? C21 C22 1.384(3) . ? C21 H21 0.9500 . ? C22 C23 1.387(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 O2 1.347(2) . ? C24 N1 1.349(2) . ? C25 C26 1.527(3) . ? C25 C27 1.530(3) . ? C25 C28 1.532(3) . ? C25 P2 1.8730(19) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.530(3) . ? C29 C30 1.531(3) . ? C29 C32 1.542(3) . ? C29 P2 1.8636(19) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 Rh1 2.1596(19) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? N1 Rh1 2.0437(15) . ? O1 P1 1.7055(12) . ? O2 P2 1.7082(12) . ? P1 Rh1 2.2425(5) . ? P2 Rh1 2.2308(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 C3 C1 C4 110.19(17) . . ? C3 C1 C2 109.07(18) . . ? C4 C1 C2 108.17(18) . . ? C3 C1 P1 108.56(14) . . ? C4 C1 P1 116.19(14) . . ? C2 C1 P1 104.36(13) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C7 C5 C6 110.62(16) . . ? C7 C5 C8 109.36(16) . . ? C6 C5 C8 108.05(16) . . ? C7 C5 P1 115.60(14) . . ? C6 C5 P1 108.59(13) . . ? C8 C5 P1 104.23(12) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O1 C9 N1 117.63(15) . . ? O1 C9 C10 121.21(15) . . ? N1 C9 C10 121.13(16) . . ? N2 C10 C9 119.84(16) . . ? N2 C10 C11 116.64(15) . . ? C9 C10 C11 123.46(15) . . ? C16 C11 C12 119.31(16) . . ? C16 C11 C10 118.14(16) . . ? C12 C11 C10 122.54(16) . . ? C13 C12 C11 119.98(17) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.24(17) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.08(17) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.80(18) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 120.57(17) . . ? C15 C16 H16 119.7 . . ? C11 C16 H16 119.7 . . ? N2 C17 C24 119.15(16) . . ? N2 C17 C18 115.84(15) . . ? C24 C17 C18 125.02(16) . . ? C23 C18 C19 118.50(17) . . ? C23 C18 C17 122.91(17) . . ? C19 C18 C17 118.45(16) . . ? C20 C19 C18 120.64(19) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 120.26(19) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C22 119.81(18) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 120.20(19) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 120.57(18) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? O2 C24 N1 117.13(15) . . ? O2 C24 C17 121.38(15) . . ? N1 C24 C17 121.47(16) . . ? C26 C25 C27 109.99(18) . . ? C26 C25 C28 108.91(18) . . ? C27 C25 C28 108.42(17) . . ? C26 C25 P2 116.38(15) . . ? C27 C25 P2 108.15(14) . . ? C28 C25 P2 104.64(13) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C30 111.09(17) . . ? C31 C29 C32 108.56(17) . . ? C30 C29 C32 108.37(17) . . ? C31 C29 P2 108.02(13) . . ? C30 C29 P2 116.16(14) . . ? C32 C29 P2 104.23(13) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Rh1 C33 H33A 109.5 . . ? Rh1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Rh1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C24 N1 C9 117.61(15) . . ? C24 N1 Rh1 121.46(12) . . ? C9 N1 Rh1 120.74(12) . . ? C10 N2 C17 120.43(15) . . ? C9 O1 P1 118.27(11) . . ? C24 O2 P2 118.14(11) . . ? O1 P1 C5 97.85(7) . . ? O1 P1 C1 98.13(8) . . ? C5 P1 C1 112.25(9) . . ? O1 P1 Rh1 101.58(4) . . ? C5 P1 Rh1 121.39(6) . . ? C1 P1 Rh1 118.73(6) . . ? O2 P2 C29 97.93(7) . . ? O2 P2 C25 98.38(8) . . ? C29 P2 C25 112.62(9) . . ? O2 P2 Rh1 102.02(4) . . ? C29 P2 Rh1 120.33(6) . . ? C25 P2 Rh1 119.01(6) . . ? N1 Rh1 C33 176.73(7) . . ? N1 Rh1 P2 81.19(4) . . ? C33 Rh1 P2 98.49(5) . . ? N1 Rh1 P1 81.35(4) . . ? C33 Rh1 P1 99.05(5) . . ? P2 Rh1 P1 162.447(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 O1 C9 C10 N2 -176.21(15) . . . . ? N1 C9 C10 N2 5.9(3) . . . . ? O1 C9 C10 C11 6.8(3) . . . . ? N1 C9 C10 C11 -171.07(16) . . . . ? N2 C10 C11 C16 -42.1(2) . . . . ? C9 C10 C11 C16 134.98(18) . . . . ? N2 C10 C11 C12 136.58(18) . . . . ? C9 C10 C11 C12 -46.3(3) . . . . ? C16 C11 C12 C13 1.1(3) . . . . ? C10 C11 C12 C13 -177.59(16) . . . . ? C11 C12 C13 C14 -1.5(3) . . . . ? C12 C13 C14 C15 0.5(3) . . . . ? C13 C14 C15 C16 0.8(3) . . . . ? C14 C15 C16 C11 -1.2(3) . . . . ? C12 C11 C16 C15 0.2(3) . . . . ? C10 C11 C16 C15 178.96(16) . . . . ? N2 C17 C18 C23 -152.25(17) . . . . ? C24 C17 C18 C23 28.3(3) . . . . ? N2 C17 C18 C19 23.5(2) . . . . ? C24 C17 C18 C19 -155.96(18) . . . . ? C23 C18 C19 C20 0.4(3) . . . . ? C17 C18 C19 C20 -175.54(18) . . . . ? C18 C19 C20 C21 0.7(3) . . . . ? C19 C20 C21 C22 -1.2(3) . . . . ? C20 C21 C22 C23 0.6(3) . . . . ? C21 C22 C23 C18 0.5(3) . . . . ? C19 C18 C23 C22 -1.0(3) . . . . ? C17 C18 C23 C22 174.74(17) . . . . ? N2 C17 C24 O2 -173.53(15) . . . . ? C18 C17 C24 O2 5.9(3) . . . . ? N2 C17 C24 N1 4.7(3) . . . . ? C18 C17 C24 N1 -175.78(16) . . . . ? O2 C24 N1 C9 178.17(15) . . . . ? C17 C24 N1 C9 -0.2(2) . . . . ? O2 C24 N1 Rh1 3.1(2) . . . . ? C17 C24 N1 Rh1 -175.27(13) . . . . ? O1 C9 N1 C24 176.98(15) . . . . ? C10 C9 N1 C24 -5.1(2) . . . . ? O1 C9 N1 Rh1 -7.9(2) . . . . ? C10 C9 N1 Rh1 170.05(13) . . . . ? C9 C10 N2 C17 -1.2(2) . . . . ? C11 C10 N2 C17 176.01(16) . . . . ? C24 C17 N2 C10 -4.0(2) . . . . ? C18 C17 N2 C10 176.53(15) . . . . ? N1 C9 O1 P1 6.4(2) . . . . ? C10 C9 O1 P1 -171.56(13) . . . . ? N1 C24 O2 P2 -2.5(2) . . . . ? C17 C24 O2 P2 175.80(13) . . . . ? C9 O1 P1 C5 122.15(13) . . . . ? C9 O1 P1 C1 -123.91(13) . . . . ? C9 O1 P1 Rh1 -2.25(13) . . . . ? C7 C5 P1 O1 60.20(14) . . . . ? C6 C5 P1 O1 -174.84(13) . . . . ? C8 C5 P1 O1 -59.84(13) . . . . ? C7 C5 P1 C1 -41.96(16) . . . . ? C6 C5 P1 C1 83.00(15) . . . . ? C8 C5 P1 C1 -162.00(12) . . . . ? C7 C5 P1 Rh1 168.96(11) . . . . ? C6 C5 P1 Rh1 -66.08(15) . . . . ? C8 C5 P1 Rh1 48.92(14) . . . . ? C3 C1 P1 O1 -162.25(14) . . . . ? C4 C1 P1 O1 -37.45(17) . . . . ? C2 C1 P1 O1 81.53(14) . . . . ? C3 C1 P1 C5 -60.27(17) . . . . ? C4 C1 P1 C5 64.53(18) . . . . ? C2 C1 P1 C5 -176.49(13) . . . . ? C3 C1 P1 Rh1 89.72(15) . . . . ? C4 C1 P1 Rh1 -145.48(14) . . . . ? C2 C1 P1 Rh1 -26.50(16) . . . . ? C24 O2 P2 C29 -122.45(13) . . . . ? C24 O2 P2 C25 123.16(13) . . . . ? C24 O2 P2 Rh1 0.98(13) . . . . ? C31 C29 P2 O2 -170.42(13) . . . . ? C30 C29 P2 O2 -44.87(16) . . . . ? C32 C29 P2 O2 74.26(13) . . . . ? C31 C29 P2 C25 -67.86(16) . . . . ? C30 C29 P2 C25 57.69(17) . . . . ? C32 C29 P2 C25 176.82(13) . . . . ? C31 C29 P2 Rh1 80.61(14) . . . . ? C30 C29 P2 Rh1 -153.84(13) . . . . ? C32 C29 P2 Rh1 -34.71(15) . . . . ? C26 C25 P2 O2 62.83(16) . . . . ? C27 C25 P2 O2 -172.82(14) . . . . ? C28 C25 P2 O2 -57.40(14) . . . . ? C26 C25 P2 C29 -39.43(18) . . . . ? C27 C25 P2 C29 84.92(16) . . . . ? C28 C25 P2 C29 -159.66(13) . . . . ? C26 C25 P2 Rh1 171.64(13) . . . . ? C27 C25 P2 Rh1 -64.01(16) . . . . ? C28 C25 P2 Rh1 51.41(15) . . . . ? C24 N1 Rh1 P2 -1.90(12) . . . . ? C9 N1 Rh1 P2 -176.83(14) . . . . ? C24 N1 Rh1 P1 179.89(13) . . . . ? C9 N1 Rh1 P1 4.95(13) . . . . ? O2 P2 Rh1 N1 0.40(6) . . . . ? C29 P2 Rh1 N1 107.14(8) . . . . ? C25 P2 Rh1 N1 -106.36(8) . . . . ? O2 P2 Rh1 C33 -176.31(7) . . . . ? C29 P2 Rh1 C33 -69.58(9) . . . . ? C25 P2 Rh1 C33 76.92(9) . . . . ? O2 P2 Rh1 P1 6.26(8) . . . . ? C29 P2 Rh1 P1 112.99(9) . . . . ? C25 P2 Rh1 P1 -100.51(9) . . . . ? O1 P1 Rh1 N1 -1.22(6) . . . . ? C5 P1 Rh1 N1 -107.98(8) . . . . ? C1 P1 Rh1 N1 104.86(8) . . . . ? O1 P1 Rh1 C33 175.50(7) . . . . ? C5 P1 Rh1 C33 68.74(9) . . . . ? C1 P1 Rh1 C33 -78.42(9) . . . . ? O1 P1 Rh1 P2 -7.07(8) . . . . ? C5 P1 Rh1 P2 -113.84(8) . . . . ? C1 P1 Rh1 P2 99.00(9) . . . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 68.01 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 0.481 _refine_diff_density_min -0.395 _refine_diff_density_rms 0.058