# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name _publ_author_footnote _publ_author_address 'Martin Cowie' . ; Department of Chemistry University of Alberta Edmonton, Alberta T6G 2G2 Canada ; 'Michael J Ferguson' 'X-ray Crystallography Laboratory' ; Department of Chemistry University of Alberta Edmonton, Alberta T6G 2G2 Canada ; 'Robert McDonald' 'X-ray Crystallography Laboratory' ; Department of Chemistry University of Alberta Edmonton, Alberta T6G 2G2 Canada ; 'Matt Zamora' . ; Department of Chemistry University of Alberta Edmonton, Alberta T6G 2G2 Canada ; _publ_contact_author_name 'Martin Cowie' _publ_contact_author_email MARTIN.COWIE@UALBERTA.CA _publ_section_title ; Carbene-Anchored/Pendent-Imidazolium Species as Precursors to Di-N-Heterocyclic Carbene-Bridged Mixed-Metal Complexes ; _publ_contact_author_address ; Department of Chemistry University of Alberta Edmonton, Alberta T6G 2G2 Canada ; _publ_contact_author_fax 1(780)4928231 _publ_contact_author_phone 1(780)4925581 _publ_contact_letter ; To: Cambridge Crystallographic Data Centre Please accept the following CIF data for a structure we hope to publish in Dalton Transactions. Please forward any questions concerning this CIF to Bob McDonald (Bob.McDonald@ualberta.ca). ; _publ_requested_journal 'Dalton Transactions' # Attachment 'cowdalt.cif' data_2c _database_code_depnum_ccdc_archive 'CCDC 726822' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H27 Br N4 Rh, Br' _chemical_formula_sum 'C18 H27 Br2 N4 Rh' _chemical_formula_weight 562.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 23.748(2) _cell_length_b 6.9405(7) _cell_length_c 12.3794(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.4800(10) _cell_angle_gamma 90.00 _cell_volume 2039.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 6655 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.19 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.831 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 4.764 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2717 _exptl_absorpt_correction_T_max 0.7966 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 16813 _diffrn_reflns_av_R_equivalents 0.0370 _diffrn_reflns_av_sigmaI/netI 0.0319 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 27.53 _reflns_number_total 4660 _reflns_number_gt 3703 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0421P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4660 _refine_ls_number_parameters 228 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0314 _refine_ls_wR_factor_ref 0.0753 _refine_ls_wR_factor_gt 0.0697 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.164675(9) 0.35528(3) 0.194243(19) 0.02230(7) Uani 1 1 d . . . Br1 Br 0.210108(14) 0.06409(5) 0.11454(3) 0.03518(10) Uani 1 1 d . . . Br2 Br 0.424941(14) 0.65660(5) 0.42979(3) 0.03663(10) Uani 1 1 d . . . N11 N 0.28308(10) 0.5131(4) 0.2371(2) 0.0262(6) Uani 1 1 d . . . N12 N 0.25468(11) 0.5762(4) 0.0755(2) 0.0266(6) Uani 1 1 d . . . N13 N 0.35631(12) 0.1779(4) 0.3100(2) 0.0313(6) Uani 1 1 d . . . N14 N 0.44579(12) 0.1249(4) 0.3008(2) 0.0306(6) Uani 1 1 d . . . C1 C 0.10133(13) 0.1819(5) 0.2779(3) 0.0296(7) Uani 1 1 d . . . H1 H 0.1107 0.0418 0.2838 0.036 Uiso 1 1 calc R . . C2 C 0.07787(13) 0.2357(5) 0.1791(2) 0.0285(7) Uani 1 1 d . . . H2 H 0.0739 0.1276 0.1261 0.034 Uiso 1 1 calc R . . C3 C 0.03523(13) 0.3968(5) 0.1616(3) 0.0355(8) Uani 1 1 d . . . H3A H 0.0136 0.4143 0.2282 0.043 Uiso 1 1 calc R . . H3B H 0.0084 0.3603 0.1026 0.043 Uiso 1 1 calc R . . C4 C 0.06381(14) 0.5881(5) 0.1328(3) 0.0354(8) Uani 1 1 d . . . H4A H 0.0688 0.5928 0.0537 0.043 Uiso 1 1 calc R . . H4B H 0.0387 0.6957 0.1523 0.043 Uiso 1 1 calc R . . C5 C 0.12019(14) 0.6171(4) 0.1887(3) 0.0308(7) Uani 1 1 d . . . H5 H 0.1423 0.7272 0.1595 0.037 Uiso 1 1 calc R . . C6 C 0.13339(13) 0.5731(5) 0.2971(3) 0.0306(7) Uani 1 1 d . . . H6 H 0.1635 0.6570 0.3297 0.037 Uiso 1 1 calc R . . C7 C 0.09185(15) 0.4993(5) 0.3785(3) 0.0370(8) Uani 1 1 d . . . H7A H 0.0536 0.5457 0.3582 0.044 Uiso 1 1 calc R . . H7B H 0.1019 0.5523 0.4508 0.044 Uiso 1 1 calc R . . C8 C 0.09135(14) 0.2796(5) 0.3845(3) 0.0350(8) Uani 1 1 d . . . H8A H 0.1208 0.2373 0.4374 0.042 Uiso 1 1 calc R . . H8B H 0.0545 0.2371 0.4115 0.042 Uiso 1 1 calc R . . C10 C 0.23803(12) 0.4936(4) 0.1684(2) 0.0248(6) Uani 1 1 d . . . C11 C 0.32732(13) 0.6050(5) 0.1863(3) 0.0331(8) Uani 1 1 d . . . H11 H 0.3633 0.6340 0.2175 0.040 Uiso 1 1 calc R . . C12 C 0.30965(14) 0.6446(5) 0.0859(3) 0.0329(7) Uani 1 1 d . . . H12 H 0.3305 0.7075 0.0318 0.040 Uiso 1 1 calc R . . C13 C 0.28654(14) 0.4392(5) 0.3467(3) 0.0327(7) Uani 1 1 d . . . H13A H 0.2499 0.4602 0.3813 0.039 Uiso 1 1 calc R . . H13B H 0.3154 0.5135 0.3882 0.039 Uiso 1 1 calc R . . C14 C 0.30116(14) 0.2275(5) 0.3534(3) 0.0359(8) Uani 1 1 d . . . H14A H 0.3005 0.1868 0.4300 0.043 Uiso 1 1 calc R . . H14B H 0.2717 0.1534 0.3134 0.043 Uiso 1 1 calc R . . C15 C 0.40508(15) 0.1774(4) 0.3653(3) 0.0312(7) Uani 1 1 d . . . H15 H 0.4099 0.2098 0.4395 0.037 Uiso 1 1 calc R . . C16 C 0.36691(16) 0.1214(5) 0.2058(3) 0.0378(8) Uani 1 1 d . . . H16 H 0.3398 0.1083 0.1484 0.045 Uiso 1 1 calc R . . C17 C 0.42255(16) 0.0882(5) 0.2001(3) 0.0386(8) Uani 1 1 d . . . H17 H 0.4421 0.0471 0.1382 0.046 Uiso 1 1 calc R . . C18 C 0.21825(15) 0.5989(5) -0.0201(3) 0.0362(8) Uani 1 1 d . . . H18A H 0.1993 0.4765 -0.0364 0.043 Uiso 1 1 calc R . . H18B H 0.2409 0.6371 -0.0816 0.043 Uiso 1 1 calc R . . H18C H 0.1900 0.6985 -0.0067 0.043 Uiso 1 1 calc R . . C19 C 0.50435(15) 0.0938(6) 0.3351(3) 0.0409(9) Uani 1 1 d . . . H19A H 0.5290 0.1210 0.2747 0.049 Uiso 1 1 calc R . . H19B H 0.5094 -0.0403 0.3581 0.049 Uiso 1 1 calc R . . H19C H 0.5140 0.1800 0.3955 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.01756(12) 0.02353(13) 0.02583(13) -0.00204(9) 0.00117(9) -0.00172(9) Br1 0.03204(19) 0.02868(18) 0.0450(2) -0.00907(14) 0.00505(15) 0.00001(14) Br2 0.02981(19) 0.0467(2) 0.03344(19) -0.00335(15) 0.00150(14) -0.00348(15) N11 0.0180(13) 0.0307(14) 0.0299(13) 0.0015(11) 0.0016(10) -0.0007(10) N12 0.0239(14) 0.0252(13) 0.0309(14) 0.0015(11) 0.0038(11) 0.0003(11) N13 0.0320(15) 0.0299(15) 0.0318(15) 0.0045(11) -0.0036(12) -0.0027(11) N14 0.0345(16) 0.0263(14) 0.0307(14) -0.0017(11) -0.0018(12) -0.0008(11) C1 0.0240(16) 0.0342(18) 0.0308(17) 0.0019(13) 0.0037(13) -0.0067(13) C2 0.0189(15) 0.0361(18) 0.0304(17) -0.0018(14) 0.0000(12) -0.0099(13) C3 0.0178(16) 0.054(2) 0.0345(18) 0.0013(15) -0.0039(13) -0.0028(14) C4 0.0239(17) 0.042(2) 0.0403(19) 0.0051(15) -0.0019(14) 0.0074(14) C5 0.0266(17) 0.0251(17) 0.0409(19) -0.0018(13) 0.0055(14) 0.0034(13) C6 0.0232(16) 0.0291(16) 0.0395(19) -0.0097(14) -0.0014(14) 0.0018(13) C7 0.0284(18) 0.055(2) 0.0281(17) -0.0089(15) -0.0006(14) 0.0094(16) C8 0.0237(17) 0.054(2) 0.0275(17) 0.0032(15) 0.0005(13) -0.0003(16) C10 0.0209(16) 0.0249(16) 0.0286(16) -0.0032(12) 0.0018(12) 0.0004(12) C11 0.0198(16) 0.0318(18) 0.048(2) 0.0018(14) 0.0028(14) -0.0069(13) C12 0.0280(17) 0.0293(17) 0.042(2) 0.0059(14) 0.0085(14) -0.0021(14) C13 0.0235(17) 0.049(2) 0.0260(16) -0.0008(14) 0.0008(13) -0.0020(15) C14 0.0288(18) 0.046(2) 0.0324(18) 0.0122(15) -0.0013(14) -0.0059(15) C15 0.0378(19) 0.0293(17) 0.0263(16) 0.0002(13) -0.0027(14) -0.0013(14) C16 0.045(2) 0.040(2) 0.0281(18) -0.0014(14) -0.0079(15) -0.0035(16) C17 0.049(2) 0.0366(19) 0.0304(18) -0.0028(14) 0.0001(16) 0.0002(16) C18 0.038(2) 0.041(2) 0.0296(17) 0.0037(14) 0.0011(14) 0.0078(15) C19 0.0317(19) 0.049(2) 0.042(2) -0.0029(16) -0.0021(16) 0.0003(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Rh C10 2.022(3) . ? Rh C5 2.102(3) . ? Rh C6 2.123(3) . ? Rh C1 2.205(3) . ? Rh C2 2.226(3) . ? Rh Br1 2.5054(4) . ? N11 C10 1.356(4) . ? N11 C11 1.393(4) . ? N11 C13 1.452(4) . ? N12 C10 1.354(4) . ? N12 C12 1.392(4) . ? N12 C18 1.457(4) . ? N13 C15 1.330(4) . ? N13 C16 1.378(4) . ? N13 C14 1.469(4) . ? N14 C15 1.321(4) . ? N14 C17 1.374(4) . ? N14 C19 1.460(4) . ? C1 C2 1.382(4) . ? C1 C8 1.508(5) . ? C2 C3 1.520(5) . ? C3 C4 1.537(5) . ? C4 C5 1.504(4) . ? C5 C6 1.404(5) . ? C6 C7 1.517(5) . ? C7 C8 1.527(5) . ? C11 C12 1.330(5) . ? C13 C14 1.512(5) . ? C16 C17 1.345(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 C10 Rh C5 91.08(12) . . ? C10 Rh C6 94.19(12) . . ? C5 Rh C6 38.82(13) . . ? C10 Rh C1 159.12(12) . . ? C5 Rh C1 97.97(13) . . ? C6 Rh C1 81.57(12) . . ? C10 Rh C2 164.53(12) . . ? C5 Rh C2 81.71(13) . . ? C6 Rh C2 88.76(12) . . ? C1 Rh C2 36.34(11) . . ? C10 Rh Br1 86.51(8) . . ? C5 Rh Br1 154.89(9) . . ? C6 Rh Br1 166.28(9) . . ? C1 Rh Br1 92.91(9) . . ? C2 Rh Br1 94.21(9) . . ? C10 N11 C11 110.8(3) . . ? C10 N11 C13 125.1(3) . . ? C11 N11 C13 124.0(3) . . ? C10 N12 C12 111.1(3) . . ? C10 N12 C18 123.8(3) . . ? C12 N12 C18 125.0(3) . . ? C15 N13 C16 107.6(3) . . ? C15 N13 C14 125.9(3) . . ? C16 N13 C14 126.5(3) . . ? C15 N14 C17 108.4(3) . . ? C15 N14 C19 124.9(3) . . ? C17 N14 C19 126.4(3) . . ? C2 C1 C8 125.8(3) . . ? C2 C1 Rh 72.63(18) . . ? C8 C1 Rh 106.9(2) . . ? C1 C2 C3 125.2(3) . . ? C1 C2 Rh 71.03(17) . . ? C3 C2 Rh 110.5(2) . . ? C2 C3 C4 111.8(3) . . ? C5 C4 C3 113.7(3) . . ? C6 C5 C4 125.8(3) . . ? C6 C5 Rh 71.40(18) . . ? C4 C5 Rh 109.9(2) . . ? C5 C6 C7 125.1(3) . . ? C5 C6 Rh 69.77(17) . . ? C7 C6 Rh 113.7(2) . . ? C6 C7 C8 112.0(3) . . ? C1 C8 C7 113.9(3) . . ? N12 C10 N11 104.3(3) . . ? N12 C10 Rh 127.4(2) . . ? N11 C10 Rh 128.2(2) . . ? C12 C11 N11 107.0(3) . . ? C11 C12 N12 106.8(3) . . ? N11 C13 C14 113.7(3) . . ? N13 C14 C13 114.4(3) . . ? N14 C15 N13 109.4(3) . . ? C17 C16 N13 107.6(3) . . ? C16 C17 N14 107.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 Rh C1 C2 179.0(3) . . . . ? C5 Rh C1 C2 64.2(2) . . . . ? C6 Rh C1 C2 99.5(2) . . . . ? Br1 Rh C1 C2 -93.16(19) . . . . ? C10 Rh C1 C8 56.0(4) . . . . ? C5 Rh C1 C8 -58.9(2) . . . . ? C6 Rh C1 C8 -23.5(2) . . . . ? C2 Rh C1 C8 -123.0(3) . . . . ? Br1 Rh C1 C8 143.8(2) . . . . ? C8 C1 C2 C3 -3.5(5) . . . . ? Rh C1 C2 C3 -102.1(3) . . . . ? C8 C1 C2 Rh 98.6(3) . . . . ? C10 Rh C2 C1 -178.7(4) . . . . ? C5 Rh C2 C1 -115.8(2) . . . . ? C6 Rh C2 C1 -77.4(2) . . . . ? Br1 Rh C2 C1 89.18(19) . . . . ? C10 Rh C2 C3 -57.2(5) . . . . ? C5 Rh C2 C3 5.7(2) . . . . ? C6 Rh C2 C3 44.1(2) . . . . ? C1 Rh C2 C3 121.5(3) . . . . ? Br1 Rh C2 C3 -149.3(2) . . . . ? C1 C2 C3 C4 94.1(4) . . . . ? Rh C2 C3 C4 13.4(3) . . . . ? C2 C3 C4 C5 -34.8(4) . . . . ? C3 C4 C5 C6 -41.6(5) . . . . ? C3 C4 C5 Rh 39.3(3) . . . . ? C10 Rh C5 C6 -95.3(2) . . . . ? C1 Rh C5 C6 65.8(2) . . . . ? C2 Rh C5 C6 98.4(2) . . . . ? Br1 Rh C5 C6 -179.41(16) . . . . ? C10 Rh C5 C4 142.4(2) . . . . ? C6 Rh C5 C4 -122.3(3) . . . . ? C1 Rh C5 C4 -56.5(2) . . . . ? C2 Rh C5 C4 -23.9(2) . . . . ? Br1 Rh C5 C4 58.3(3) . . . . ? C4 C5 C6 C7 -3.8(5) . . . . ? Rh C5 C6 C7 -105.3(3) . . . . ? C4 C5 C6 Rh 101.5(3) . . . . ? C10 Rh C6 C5 86.5(2) . . . . ? C1 Rh C6 C5 -114.1(2) . . . . ? C2 Rh C6 C5 -78.3(2) . . . . ? Br1 Rh C6 C5 179(14) . . . . ? C10 Rh C6 C7 -153.0(2) . . . . ? C5 Rh C6 C7 120.5(3) . . . . ? C1 Rh C6 C7 6.5(2) . . . . ? C2 Rh C6 C7 42.2(2) . . . . ? Br1 Rh C6 C7 -60.5(5) . . . . ? C5 C6 C7 C8 93.5(4) . . . . ? Rh C6 C7 C8 12.3(3) . . . . ? C2 C1 C8 C7 -42.6(4) . . . . ? Rh C1 C8 C7 37.8(3) . . . . ? C6 C7 C8 C1 -34.2(4) . . . . ? C12 N12 C10 N11 0.6(3) . . . . ? C18 N12 C10 N11 -176.2(3) . . . . ? C12 N12 C10 Rh -175.3(2) . . . . ? C18 N12 C10 Rh 7.9(4) . . . . ? C11 N11 C10 N12 -0.7(3) . . . . ? C13 N11 C10 N12 -177.4(3) . . . . ? C11 N11 C10 Rh 175.2(2) . . . . ? C13 N11 C10 Rh -1.5(4) . . . . ? C5 Rh C10 N12 -71.8(3) . . . . ? C6 Rh C10 N12 -110.6(3) . . . . ? C1 Rh C10 N12 172.2(3) . . . . ? C2 Rh C10 N12 -10.0(6) . . . . ? Br1 Rh C10 N12 83.2(3) . . . . ? C5 Rh C10 N11 113.3(3) . . . . ? C6 Rh C10 N11 74.5(3) . . . . ? C1 Rh C10 N11 -2.8(5) . . . . ? C2 Rh C10 N11 175.1(4) . . . . ? Br1 Rh C10 N11 -91.8(3) . . . . ? C10 N11 C11 C12 0.5(4) . . . . ? C13 N11 C11 C12 177.3(3) . . . . ? N11 C11 C12 N12 -0.2(4) . . . . ? C10 N12 C12 C11 -0.2(4) . . . . ? C18 N12 C12 C11 176.5(3) . . . . ? C10 N11 C13 C14 80.9(4) . . . . ? C11 N11 C13 C14 -95.3(4) . . . . ? C15 N13 C14 C13 88.7(4) . . . . ? C16 N13 C14 C13 -92.1(4) . . . . ? N11 C13 C14 N13 61.7(4) . . . . ? C17 N14 C15 N13 -0.5(4) . . . . ? C19 N14 C15 N13 -175.1(3) . . . . ? C16 N13 C15 N14 0.5(4) . . . . ? C14 N13 C15 N14 179.7(3) . . . . ? C15 N13 C16 C17 -0.2(4) . . . . ? C14 N13 C16 C17 -179.5(3) . . . . ? N13 C16 C17 N14 -0.1(4) . . . . ? C15 N14 C17 C16 0.4(4) . . . . ? C19 N14 C17 C16 174.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.53 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.227 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.115 #===END data_2d _database_code_depnum_ccdc_archive 'CCDC 726823' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H39 Br N4 Rh, 2(C H2 Cl2), Br' _chemical_formula_sum 'C26 H43 Br2 Cl4 N4 Rh' _chemical_formula_weight 816.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21' _symmetry_space_group_name_Hall 'P 2yb' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.5243(10) _cell_length_b 13.8891(16) _cell_length_c 14.5876(17) _cell_angle_alpha 90.00 _cell_angle_beta 101.093(2) _cell_angle_gamma 90.00 _cell_volume 1694.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5922 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 27.42 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 3.199 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3270 _exptl_absorpt_correction_T_max 0.6455 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14567 _diffrn_reflns_av_R_equivalents 0.0163 _diffrn_reflns_av_sigmaI/netI 0.0273 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 27.44 _reflns_number_total 7648 _reflns_number_gt 7288 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART (Bruker, 1997)' _computing_cell_refinement 'Bruker SAINT (Bruker, 1997)' _computing_data_reduction 'Bruker SAINT (Bruker, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL (Bruker, 1997)' _computing_publication_material 'Bruker SHELXTL (Bruker, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0504P)^2^+0.2277P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881. 3641 Friedel pairs.' _refine_ls_abs_structure_Flack 0.364(6) _refine_ls_number_reflns 7648 _refine_ls_number_parameters 335 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0294 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Rh Rh 0.64721(2) 0.553501(17) 0.929564(15) 0.02277(6) Uani 1 1 d . . . Br1 Br 0.83518(4) 0.62485(2) 0.83264(2) 0.03204(8) Uani 1 1 d . . . Br2 Br 0.77381(4) 0.12361(3) 0.66496(2) 0.03771(9) Uani 1 1 d . . . N11 N 0.7577(3) 0.35927(18) 0.87499(16) 0.0223(5) Uani 1 1 d . . . N12 N 0.8936(3) 0.39169(18) 1.01126(17) 0.0227(5) Uani 1 1 d . . . N13 N 0.6686(4) 0.4068(2) 0.61991(18) 0.0292(6) Uani 1 1 d . . . N14 N 0.5423(4) 0.3803(2) 0.47853(19) 0.0309(6) Uani 1 1 d . . . C1 C 0.5677(5) 0.6959(3) 0.9662(3) 0.0406(8) Uani 1 1 d . . . H1 H 0.6453 0.7488 0.9613 0.049 Uiso 1 1 calc R . . C2 C 0.4722(5) 0.6708(3) 0.8819(3) 0.0408(9) Uani 1 1 d . . . H2 H 0.4938 0.7082 0.8271 0.049 Uiso 1 1 calc R . . C3 C 0.3015(5) 0.6349(4) 0.8717(3) 0.0496(10) Uani 1 1 d . . . H3A H 0.2377 0.6589 0.8122 0.060 Uiso 1 1 calc R . . H3B H 0.2540 0.6611 0.9233 0.060 Uiso 1 1 calc R . . C4 C 0.2931(5) 0.5241(3) 0.8731(3) 0.0467(10) Uani 1 1 d . . . H4A H 0.1944 0.5044 0.8944 0.056 Uiso 1 1 calc R . . H4B H 0.2866 0.4996 0.8088 0.056 Uiso 1 1 calc R . . C5 C 0.4355(4) 0.4787(3) 0.9362(2) 0.0312(7) Uani 1 1 d . . . H5 H 0.4437 0.4077 0.9270 0.037 Uiso 1 1 calc R . . C6 C 0.5042(4) 0.5095(3) 1.0266(2) 0.0310(7) Uani 1 1 d . . . H6 H 0.5523 0.4563 1.0691 0.037 Uiso 1 1 calc R . . C7 C 0.4433(5) 0.5937(3) 1.0766(3) 0.0433(9) Uani 1 1 d . . . H7A H 0.4641 0.5805 1.1446 0.052 Uiso 1 1 calc R . . H7B H 0.3262 0.5993 1.0552 0.052 Uiso 1 1 calc R . . C8 C 0.5213(5) 0.6893(3) 1.0595(3) 0.0477(10) Uani 1 1 d . . . H8A H 0.4461 0.7423 1.0654 0.057 Uiso 1 1 calc R . . H8B H 0.6179 0.6986 1.1086 0.057 Uiso 1 1 calc R . . C10 C 0.7765(3) 0.4279(2) 0.94208(19) 0.0207(5) Uani 1 1 d . . . C11 C 0.8578(4) 0.2821(2) 0.9001(2) 0.0277(6) Uani 1 1 d . . . H11 H 0.8659 0.2261 0.8639 0.033 Uiso 1 1 calc R . . C12 C 0.9415(4) 0.3014(2) 0.9858(2) 0.0273(6) Uani 1 1 d . . . H12 H 1.0192 0.2610 1.0223 0.033 Uiso 1 1 calc R . . C13 C 0.6579(4) 0.3695(2) 0.7823(2) 0.0245(6) Uani 1 1 d . . . H13A H 0.5811 0.4230 0.7821 0.029 Uiso 1 1 calc R . . H13B H 0.5967 0.3096 0.7646 0.029 Uiso 1 1 calc R . . C14 C 0.7664(4) 0.3901(2) 0.7131(2) 0.0272(6) Uani 1 1 d . . . H14A H 0.8326 0.4477 0.7334 0.033 Uiso 1 1 calc R . . H14B H 0.8389 0.3349 0.7109 0.033 Uiso 1 1 calc R . . C15 C 0.6364(4) 0.3406(2) 0.5533(2) 0.0310(7) Uani 1 1 d . . . H15 H 0.6736 0.2760 0.5578 0.037 Uiso 1 1 calc R . . C16 C 0.5949(5) 0.4909(3) 0.5881(2) 0.0384(8) Uani 1 1 d . . . H16 H 0.5990 0.5497 0.6217 0.046 Uiso 1 1 calc R . . C17 C 0.5147(5) 0.4750(3) 0.4995(2) 0.0381(8) Uani 1 1 d . . . H17 H 0.4518 0.5203 0.4596 0.046 Uiso 1 1 calc R . . C18 C 0.9679(4) 0.4376(2) 1.1021(2) 0.0274(6) Uani 1 1 d . . . C19 C 0.9434(4) 0.5469(3) 1.0968(2) 0.0410(8) Uani 1 1 d . . . H19A H 0.9949 0.5734 1.0478 0.062 Uiso 1 1 calc R . . H19B H 0.9910 0.5759 1.1570 0.062 Uiso 1 1 calc R . . H19C H 0.8288 0.5613 1.0823 0.062 Uiso 1 1 calc R . . C20 C 0.8953(5) 0.3935(3) 1.1792(2) 0.0446(10) Uani 1 1 d . . . H20A H 0.9438 0.4226 1.2392 0.067 Uiso 1 1 calc R . . H20B H 0.9152 0.3240 1.1817 0.067 Uiso 1 1 calc R . . H20C H 0.7798 0.4054 1.1667 0.067 Uiso 1 1 calc R . . C21 C 1.1485(4) 0.4175(3) 1.1198(3) 0.0369(8) Uani 1 1 d . . . H21A H 1.1951 0.4473 1.0704 0.055 Uiso 1 1 calc R . . H21B H 1.1667 0.3478 1.1200 0.055 Uiso 1 1 calc R . . H21C H 1.1988 0.4444 1.1805 0.055 Uiso 1 1 calc R . . C22 C 0.4794(5) 0.3306(3) 0.3878(2) 0.0413(9) Uani 1 1 d . . . C23 C 0.5229(5) 0.3903(3) 0.3101(2) 0.0431(9) Uani 1 1 d . . . H23A H 0.6391 0.3894 0.3147 0.065 Uiso 1 1 calc R . . H23B H 0.4871 0.4568 0.3154 0.065 Uiso 1 1 calc R . . H23C H 0.4708 0.3636 0.2497 0.065 Uiso 1 1 calc R . . C24 C 0.2964(7) 0.3268(5) 0.3777(3) 0.0729(17) Uani 1 1 d . . . H24A H 0.2685 0.2852 0.4265 0.109 Uiso 1 1 calc R . . H24B H 0.2488 0.3009 0.3162 0.109 Uiso 1 1 calc R . . H24C H 0.2553 0.3919 0.3841 0.109 Uiso 1 1 calc R . . C25 C 0.5545(10) 0.2320(3) 0.3909(3) 0.087(2) Uani 1 1 d . . . H25A H 0.5253 0.1947 0.4422 0.131 Uiso 1 1 calc R . . H25B H 0.6710 0.2384 0.4009 0.131 Uiso 1 1 calc R . . H25C H 0.5158 0.1987 0.3316 0.131 Uiso 1 1 calc R . . Cl1S Cl 0.9861(3) 0.0880(2) 0.38893(16) 0.1254(9) Uani 1 1 d . . . Cl2S Cl 1.0523(2) -0.0639(2) 0.52575(17) 0.1326(10) Uani 1 1 d . . . Cl3S Cl 0.63735(19) 0.67172(12) 0.35268(13) 0.0835(4) Uani 1 1 d . . . Cl4S Cl 0.8162(2) 0.81654(16) 0.27873(19) 0.1133(8) Uani 1 1 d . . . C1S C 0.9117(8) 0.0176(6) 0.4651(5) 0.095(3) Uani 1 1 d . . . H1SA H 0.8193 -0.0189 0.4305 0.114 Uiso 1 1 calc R . . H1SB H 0.8724 0.0593 0.5109 0.114 Uiso 1 1 calc R . . C2S C 0.8265(7) 0.7122(6) 0.3474(6) 0.102(3) Uani 1 1 d . . . H2SA H 0.8852 0.6614 0.3203 0.123 Uiso 1 1 calc R . . H2SB H 0.8857 0.7262 0.4113 0.123 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rh 0.02561(10) 0.01788(10) 0.02541(10) 0.00022(9) 0.00641(8) 0.00154(10) Br1 0.03872(17) 0.02622(15) 0.03359(16) -0.00095(13) 0.01301(13) -0.00505(13) Br2 0.04607(19) 0.02964(17) 0.03320(17) 0.00022(14) -0.00296(14) -0.00059(15) N11 0.0266(12) 0.0219(12) 0.0181(12) -0.0001(9) 0.0035(10) 0.0004(10) N12 0.0255(12) 0.0200(12) 0.0213(12) 0.0011(9) 0.0014(10) -0.0013(10) N13 0.0394(15) 0.0254(14) 0.0211(12) -0.0011(10) 0.0020(11) 0.0024(11) N14 0.0428(16) 0.0263(14) 0.0208(12) 0.0018(10) -0.0004(11) -0.0012(12) C1 0.0418(19) 0.0194(15) 0.065(2) -0.0042(16) 0.0220(18) 0.0023(14) C2 0.041(2) 0.0302(19) 0.054(2) 0.0118(16) 0.0156(17) 0.0136(15) C3 0.039(2) 0.051(3) 0.056(2) 0.006(2) 0.0035(17) 0.0110(19) C4 0.0279(18) 0.048(2) 0.062(3) -0.0048(18) 0.0027(17) 0.0040(15) C5 0.0292(15) 0.0239(15) 0.0426(18) -0.0023(13) 0.0125(14) -0.0002(13) C6 0.0307(16) 0.0291(17) 0.0357(17) 0.0013(13) 0.0126(14) -0.0027(13) C7 0.046(2) 0.042(2) 0.047(2) -0.0082(17) 0.0200(18) -0.0035(16) C8 0.052(2) 0.039(2) 0.058(2) -0.0162(19) 0.0249(19) -0.0024(18) C10 0.0225(13) 0.0203(13) 0.0189(13) -0.0004(10) 0.0031(10) -0.0023(11) C11 0.0318(16) 0.0207(15) 0.0299(16) -0.0013(12) 0.0041(13) 0.0049(12) C12 0.0306(15) 0.0228(15) 0.0270(15) 0.0013(12) 0.0017(12) 0.0043(12) C13 0.0273(15) 0.0242(14) 0.0202(14) -0.0031(11) 0.0004(11) 0.0017(11) C14 0.0323(16) 0.0288(16) 0.0183(14) -0.0011(11) -0.0005(12) 0.0007(12) C15 0.0455(19) 0.0244(15) 0.0214(14) 0.0008(12) 0.0019(13) 0.0037(14) C16 0.056(2) 0.0288(17) 0.0271(16) -0.0033(14) -0.0007(15) 0.0077(16) C17 0.055(2) 0.0298(18) 0.0272(16) 0.0033(14) 0.0012(15) 0.0103(16) C18 0.0312(15) 0.0275(16) 0.0212(14) -0.0021(12) -0.0009(12) -0.0043(12) C19 0.0468(18) 0.0318(18) 0.0369(17) -0.0110(17) -0.0110(14) 0.0019(18) C20 0.049(2) 0.065(3) 0.0197(15) -0.0014(16) 0.0066(15) -0.0103(19) C21 0.0331(17) 0.040(2) 0.0331(18) -0.0012(15) -0.0059(14) -0.0060(15) C22 0.064(3) 0.0326(19) 0.0230(16) -0.0019(14) -0.0021(16) -0.0067(17) C23 0.060(2) 0.045(2) 0.0226(16) -0.0002(15) 0.0016(16) -0.0027(18) C24 0.068(3) 0.107(5) 0.037(2) -0.002(3) -0.005(2) -0.041(3) C25 0.182(7) 0.034(2) 0.030(2) -0.0106(18) -0.021(3) 0.022(3) Cl1S 0.1077(14) 0.169(3) 0.1082(15) 0.0416(15) 0.0409(12) 0.0371(14) Cl2S 0.0881(13) 0.208(3) 0.1130(15) 0.0546(17) 0.0486(12) 0.0505(15) Cl3S 0.0693(8) 0.0786(10) 0.1052(12) 0.0173(9) 0.0230(8) -0.0039(7) Cl4S 0.0693(10) 0.1036(14) 0.1599(19) 0.0515(13) 0.0043(11) -0.0191(9) C1S 0.068(4) 0.147(8) 0.073(4) -0.017(4) 0.019(3) 0.015(4) C2S 0.050(3) 0.120(6) 0.142(7) 0.055(5) 0.030(4) 0.023(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 Rh C10 2.053(3) . ? Rh C5 2.101(3) . ? Rh C6 2.127(3) . ? Rh C1 2.190(4) . ? Rh C2 2.229(3) . ? Rh Br1 2.5338(4) . ? N11 C10 1.353(4) . ? N11 C11 1.375(4) . ? N11 C13 1.460(4) . ? N12 C10 1.371(4) . ? N12 C12 1.391(4) . ? N12 C18 1.497(4) . ? N13 C15 1.327(4) . ? N13 C16 1.365(5) . ? N13 C14 1.470(4) . ? N14 C15 1.341(4) . ? N14 C17 1.381(5) . ? N14 C22 1.497(4) . ? C1 C2 1.383(6) . ? C1 C8 1.491(6) . ? C2 C3 1.518(6) . ? C3 C4 1.541(7) . ? C4 C5 1.512(5) . ? C5 C6 1.403(5) . ? C6 C7 1.523(5) . ? C7 C8 1.527(6) . ? C11 C12 1.342(5) . ? C13 C14 1.521(4) . ? C16 C17 1.359(5) . ? C18 C20 1.514(5) . ? C18 C19 1.532(5) . ? C18 C21 1.536(5) . ? C22 C23 1.508(5) . ? C22 C25 1.508(7) . ? C22 C24 1.540(7) . ? Cl1S C1S 1.692(8) . ? Cl2S C1S 1.759(8) . ? Cl3S C2S 1.723(7) . ? Cl4S C2S 1.755(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 C10 Rh C5 91.57(13) . . ? C10 Rh C6 93.62(13) . . ? C5 Rh C6 38.74(13) . . ? C10 Rh C1 158.71(14) . . ? C5 Rh C1 97.25(14) . . ? C6 Rh C1 81.57(14) . . ? C10 Rh C2 164.80(14) . . ? C5 Rh C2 81.15(14) . . ? C6 Rh C2 89.02(14) . . ? C1 Rh C2 36.46(16) . . ? C10 Rh Br1 89.74(8) . . ? C5 Rh Br1 149.33(10) . . ? C6 Rh Br1 171.25(10) . . ? C1 Rh Br1 92.39(11) . . ? C2 Rh Br1 89.85(11) . . ? C10 N11 C11 112.1(2) . . ? C10 N11 C13 124.6(2) . . ? C11 N11 C13 123.0(3) . . ? C10 N12 C12 110.1(2) . . ? C10 N12 C18 128.3(3) . . ? C12 N12 C18 121.7(2) . . ? C15 N13 C16 109.1(3) . . ? C15 N13 C14 124.7(3) . . ? C16 N13 C14 126.2(3) . . ? C15 N14 C17 108.2(3) . . ? C15 N14 C22 125.8(3) . . ? C17 N14 C22 126.0(3) . . ? C2 C1 C8 125.6(4) . . ? C2 C1 Rh 73.3(2) . . ? C8 C1 Rh 108.4(3) . . ? C1 C2 C3 124.0(4) . . ? C1 C2 Rh 70.3(2) . . ? C3 C2 Rh 111.2(3) . . ? C2 C3 C4 111.9(3) . . ? C5 C4 C3 113.0(3) . . ? C6 C5 C4 125.9(3) . . ? C6 C5 Rh 71.66(19) . . ? C4 C5 Rh 111.2(3) . . ? C5 C6 C7 124.4(3) . . ? C5 C6 Rh 69.60(19) . . ? C7 C6 Rh 112.9(2) . . ? C6 C7 C8 113.0(3) . . ? C1 C8 C7 113.7(3) . . ? N11 C10 N12 104.0(2) . . ? N11 C10 Rh 123.2(2) . . ? N12 C10 Rh 132.8(2) . . ? C12 C11 N11 106.5(3) . . ? C11 C12 N12 107.4(3) . . ? N11 C13 C14 108.2(2) . . ? N13 C14 C13 109.5(3) . . ? N13 C15 N14 108.5(3) . . ? C17 C16 N13 107.4(3) . . ? C16 C17 N14 106.8(3) . . ? N12 C18 C20 108.8(3) . . ? N12 C18 C19 110.3(3) . . ? C20 C18 C19 111.5(3) . . ? N12 C18 C21 108.1(3) . . ? C20 C18 C21 109.9(3) . . ? C19 C18 C21 108.1(3) . . ? N14 C22 C23 108.2(3) . . ? N14 C22 C25 108.4(3) . . ? C23 C22 C25 111.0(4) . . ? N14 C22 C24 106.5(4) . . ? C23 C22 C24 109.8(4) . . ? C25 C22 C24 112.8(5) . . ? Cl1S C1S Cl2S 113.4(4) . . ? Cl3S C2S Cl4S 110.5(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 C10 Rh C1 C2 -178.1(3) . . . . ? C5 Rh C1 C2 -64.3(2) . . . . ? C6 Rh C1 C2 -99.9(2) . . . . ? Br1 Rh C1 C2 86.5(2) . . . . ? C10 Rh C1 C8 -55.3(5) . . . . ? C5 Rh C1 C8 58.4(3) . . . . ? C6 Rh C1 C8 22.9(3) . . . . ? C2 Rh C1 C8 122.7(4) . . . . ? Br1 Rh C1 C8 -150.8(3) . . . . ? C8 C1 C2 C3 1.8(6) . . . . ? Rh C1 C2 C3 102.8(4) . . . . ? C8 C1 C2 Rh -101.0(4) . . . . ? C10 Rh C2 C1 177.3(4) . . . . ? C5 Rh C2 C1 115.2(2) . . . . ? C6 Rh C2 C1 77.1(2) . . . . ? Br1 Rh C2 C1 -94.2(2) . . . . ? C10 Rh C2 C3 57.5(6) . . . . ? C5 Rh C2 C3 -4.7(3) . . . . ? C6 Rh C2 C3 -42.8(3) . . . . ? C1 Rh C2 C3 -119.9(4) . . . . ? Br1 Rh C2 C3 145.9(3) . . . . ? C1 C2 C3 C4 -93.9(5) . . . . ? Rh C2 C3 C4 -14.0(5) . . . . ? C2 C3 C4 C5 33.8(5) . . . . ? C3 C4 C5 C6 44.4(5) . . . . ? C3 C4 C5 Rh -37.8(4) . . . . ? C10 Rh C5 C6 93.8(2) . . . . ? C1 Rh C5 C6 -66.7(2) . . . . ? C2 Rh C5 C6 -99.6(2) . . . . ? Br1 Rh C5 C6 -174.03(16) . . . . ? C10 Rh C5 C4 -143.9(3) . . . . ? C6 Rh C5 C4 122.3(4) . . . . ? C1 Rh C5 C4 55.5(3) . . . . ? C2 Rh C5 C4 22.7(3) . . . . ? Br1 Rh C5 C4 -51.8(4) . . . . ? C4 C5 C6 C7 1.1(6) . . . . ? Rh C5 C6 C7 104.4(3) . . . . ? C4 C5 C6 Rh -103.3(4) . . . . ? C10 Rh C6 C5 -88.0(2) . . . . ? C1 Rh C6 C5 112.9(2) . . . . ? C2 Rh C6 C5 77.0(2) . . . . ? Br1 Rh C6 C5 159.6(5) . . . . ? C10 Rh C6 C7 152.2(3) . . . . ? C5 Rh C6 C7 -119.8(4) . . . . ? C1 Rh C6 C7 -7.0(3) . . . . ? C2 Rh C6 C7 -42.8(3) . . . . ? Br1 Rh C6 C7 39.8(8) . . . . ? C5 C6 C7 C8 -90.5(5) . . . . ? Rh C6 C7 C8 -10.2(4) . . . . ? C2 C1 C8 C7 46.9(6) . . . . ? Rh C1 C8 C7 -35.4(4) . . . . ? C6 C7 C8 C1 31.0(5) . . . . ? C11 N11 C10 N12 0.3(3) . . . . ? C13 N11 C10 N12 -172.9(3) . . . . ? C11 N11 C10 Rh -179.8(2) . . . . ? C13 N11 C10 Rh 7.0(4) . . . . ? C12 N12 C10 N11 -1.1(3) . . . . ? C18 N12 C10 N11 178.1(3) . . . . ? C12 N12 C10 Rh 179.1(2) . . . . ? C18 N12 C10 Rh -1.8(5) . . . . ? C5 Rh C10 N11 68.0(3) . . . . ? C6 Rh C10 N11 106.7(3) . . . . ? C1 Rh C10 N11 -177.3(3) . . . . ? C2 Rh C10 N11 7.1(6) . . . . ? Br1 Rh C10 N11 -81.4(2) . . . . ? C5 Rh C10 N12 -112.2(3) . . . . ? C6 Rh C10 N12 -73.4(3) . . . . ? C1 Rh C10 N12 2.5(5) . . . . ? C2 Rh C10 N12 -173.1(4) . . . . ? Br1 Rh C10 N12 98.5(3) . . . . ? C10 N11 C11 C12 0.6(4) . . . . ? C13 N11 C11 C12 173.9(3) . . . . ? N11 C11 C12 N12 -1.2(4) . . . . ? C10 N12 C12 C11 1.5(4) . . . . ? C18 N12 C12 C11 -177.7(3) . . . . ? C10 N11 C13 C14 102.3(3) . . . . ? C11 N11 C13 C14 -70.1(4) . . . . ? C15 N13 C14 C13 -97.3(4) . . . . ? C16 N13 C14 C13 81.8(4) . . . . ? N11 C13 C14 N13 -176.6(2) . . . . ? C16 N13 C15 N14 -0.2(4) . . . . ? C14 N13 C15 N14 179.0(3) . . . . ? C17 N14 C15 N13 -0.1(4) . . . . ? C22 N14 C15 N13 179.5(3) . . . . ? C15 N13 C16 C17 0.4(5) . . . . ? C14 N13 C16 C17 -178.8(3) . . . . ? N13 C16 C17 N14 -0.4(5) . . . . ? C15 N14 C17 C16 0.3(4) . . . . ? C22 N14 C17 C16 -179.2(4) . . . . ? C10 N12 C18 C20 101.8(4) . . . . ? C12 N12 C18 C20 -79.2(4) . . . . ? C10 N12 C18 C19 -20.8(4) . . . . ? C12 N12 C18 C19 158.2(3) . . . . ? C10 N12 C18 C21 -138.9(3) . . . . ? C12 N12 C18 C21 40.2(4) . . . . ? C15 N14 C22 C23 -126.6(4) . . . . ? C17 N14 C22 C23 52.8(5) . . . . ? C15 N14 C22 C25 -6.3(6) . . . . ? C17 N14 C22 C25 173.2(5) . . . . ? C15 N14 C22 C24 115.4(4) . . . . ? C17 N14 C22 C24 -65.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.989 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.099 #===END data_11b _database_code_depnum_ccdc_archive 'CCDC 726824' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H36 I2 N4 P Pd, I' _chemical_formula_sum 'C23 H36 I3 N4 P Pd' _chemical_formula_weight 886.63 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.4861(11) _cell_length_b 12.0320(13) _cell_length_c 14.0083(16) _cell_angle_alpha 91.9746(12) _cell_angle_beta 100.9332(12) _cell_angle_gamma 103.9630(12) _cell_volume 1518.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9866 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.53 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.940 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 3.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2626 _exptl_absorpt_correction_T_max 0.6405 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11967 _diffrn_reflns_av_R_equivalents 0.0148 _diffrn_reflns_av_sigmaI/netI 0.0222 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 26.40 _reflns_number_total 6159 _reflns_number_gt 5815 _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^)+(0.0310P)^2^+4.1569P] 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 SHELXL _refine_ls_extinction_coef 0.00110(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6159 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0266 _refine_ls_R_factor_gt 0.0251 _refine_ls_wR_factor_ref 0.0764 _refine_ls_wR_factor_gt 0.0757 _refine_ls_goodness_of_fit_ref 1.157 _refine_ls_restrained_S_all 1.157 _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 I1 I 0.41463(3) 0.25196(2) 0.320636(19) 0.02614(8) Uani 1 1 d . . . I2 I -0.14776(3) 0.22052(2) 0.30385(2) 0.03133(8) Uani 1 1 d . . . I3 I -0.13572(3) 0.65748(3) 0.06535(2) 0.03669(9) Uani 1 1 d . . . Pd Pd 0.13349(3) 0.22879(2) 0.32139(2) 0.01982(8) Uani 1 1 d . . . P P 0.08586(13) 0.04213(9) 0.25440(8) 0.0305(2) Uani 1 1 d . . . N11 N 0.2072(3) 0.4500(3) 0.4645(2) 0.0200(6) Uani 1 1 d . . . N12 N 0.1723(3) 0.4834(3) 0.3137(2) 0.0200(6) Uani 1 1 d . . . N13 N 0.2566(3) 0.5365(3) 0.1669(2) 0.0213(6) Uani 1 1 d . . . N14 N 0.3707(3) 0.6593(3) 0.0811(2) 0.0209(6) Uani 1 1 d . . . C1A C 0.2059(5) 0.4677(4) 0.6405(3) 0.0328(9) Uani 1 1 d . . . H1AA H 0.2761 0.5436 0.6503 0.039 Uiso 1 1 calc R . . H1AB H 0.2165 0.4294 0.7011 0.039 Uiso 1 1 calc R . . H1AC H 0.1044 0.4764 0.6222 0.039 Uiso 1 1 calc R . . C1B C 0.4012(5) 0.3937(4) 0.5804(3) 0.0342(10) Uani 1 1 d . . . H1BA H 0.4633 0.4725 0.5958 0.041 Uiso 1 1 calc R . . H1BB H 0.4244 0.3590 0.5229 0.041 Uiso 1 1 calc R . . H1BC H 0.4207 0.3485 0.6360 0.041 Uiso 1 1 calc R . . C1C C 0.1371(7) 0.2749(4) 0.5510(3) 0.0484(13) Uani 1 1 d . . . H1CA H 0.1552 0.2408 0.6133 0.058 Uiso 1 1 calc R . . H1CB H 0.1578 0.2275 0.4996 0.058 Uiso 1 1 calc R . . H1CC H 0.0332 0.2784 0.5346 0.058 Uiso 1 1 calc R . . C1D C 0.2660(5) 0.7982(4) -0.0161(3) 0.0325(9) Uani 1 1 d . . . H1DA H 0.1809 0.7380 -0.0512 0.039 Uiso 1 1 calc R . . H1DB H 0.2878 0.8615 -0.0575 0.039 Uiso 1 1 calc R . . H1DC H 0.2428 0.8267 0.0439 0.039 Uiso 1 1 calc R . . C1E C 0.5375(5) 0.8421(4) 0.0591(4) 0.0375(10) Uani 1 1 d . . . H1EA H 0.5643 0.8989 0.0128 0.045 Uiso 1 1 calc R . . H1EB H 0.6202 0.8072 0.0806 0.045 Uiso 1 1 calc R . . H1EC H 0.5158 0.8800 0.1156 0.045 Uiso 1 1 calc R . . C1F C 0.4292(6) 0.6896(4) -0.0800(3) 0.0370(10) Uani 1 1 d . . . H1FA H 0.3378 0.6341 -0.1133 0.044 Uiso 1 1 calc R . . H1FB H 0.5069 0.6494 -0.0597 0.044 Uiso 1 1 calc R . . H1FC H 0.4614 0.7471 -0.1245 0.044 Uiso 1 1 calc R . . C10 C 0.2379(5) 0.3955(3) 0.5594(3) 0.0275(8) Uani 1 1 d . . . C11 C 0.1772(4) 0.3974(3) 0.3736(3) 0.0192(7) Uani 1 1 d . . . C12 C 0.2224(4) 0.5677(3) 0.4605(3) 0.0251(8) Uani 1 1 d . . . H12 H 0.2451 0.6232 0.5147 0.030 Uiso 1 1 calc R . . C13 C 0.1991(4) 0.5882(3) 0.3663(3) 0.0249(8) Uani 1 1 d . . . H13 H 0.2008 0.6604 0.3406 0.030 Uiso 1 1 calc R . . C14 C 0.1369(4) 0.4673(3) 0.2076(3) 0.0233(8) Uani 1 1 d . . . H14A H 0.0437 0.4897 0.1828 0.028 Uiso 1 1 calc R . . H14B H 0.1214 0.3851 0.1864 0.028 Uiso 1 1 calc R . . C15 C 0.2421(4) 0.6199(3) 0.1083(3) 0.0223(7) Uani 1 1 d . . . H15 H 0.1552 0.6465 0.0894 0.027 Uiso 1 1 calc R . . C16 C 0.3979(4) 0.5208(4) 0.1751(3) 0.0266(8) Uani 1 1 d . . . H16 H 0.4373 0.4662 0.2116 0.032 Uiso 1 1 calc R . . C17 C 0.4690(4) 0.5978(4) 0.1217(3) 0.0269(8) Uani 1 1 d . . . H17 H 0.5683 0.6078 0.1134 0.032 Uiso 1 1 calc R . . C18 C 0.4004(4) 0.7488(3) 0.0094(3) 0.0252(8) Uani 1 1 d . . . C21 C 0.2139(5) -0.0365(3) 0.3145(3) 0.0298(9) Uani 1 1 d . . . C22 C 0.3199(6) -0.0669(4) 0.2706(3) 0.0426(11) Uani 1 1 d . . . H22 H 0.3214 -0.0533 0.2043 0.051 Uiso 1 1 calc R . . C23 C 0.4245(7) -0.1175(5) 0.3235(4) 0.0504(13) Uani 1 1 d . . . H23 H 0.4965 -0.1387 0.2929 0.060 Uiso 1 1 calc R . . C24 C 0.4240(6) -0.1369(4) 0.4190(4) 0.0429(11) Uani 1 1 d . . . H24 H 0.4966 -0.1701 0.4549 0.052 Uiso 1 1 calc R . . C25 C 0.3188(6) -0.1083(4) 0.4630(3) 0.0421(11) Uani 1 1 d . . . H25 H 0.3174 -0.1229 0.5291 0.051 Uiso 1 1 calc R . . C26 C 0.2140(5) -0.0579(4) 0.4111(3) 0.0362(10) Uani 1 1 d . . . H26 H 0.1418 -0.0379 0.4421 0.043 Uiso 1 1 calc R . . C27 C 0.0990(8) 0.0389(5) 0.1274(3) 0.0552(16) Uani 1 1 d . . . H27A H 0.0801 -0.0410 0.1010 0.066 Uiso 1 1 calc R . . H27B H 0.1987 0.0812 0.1216 0.066 Uiso 1 1 calc R . . H27C H 0.0253 0.0746 0.0908 0.066 Uiso 1 1 calc R . . C28 C -0.0942(6) -0.0551(4) 0.2528(5) 0.0559(15) Uani 1 1 d . . . H28A H -0.0968 -0.1313 0.2244 0.067 Uiso 1 1 calc R . . H28B H -0.1720 -0.0256 0.2134 0.067 Uiso 1 1 calc R . . H28C H -0.1107 -0.0607 0.3196 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.02546(14) 0.02594(14) 0.03019(14) 0.00518(10) 0.00945(10) 0.00919(10) I2 0.02293(14) 0.03406(16) 0.03529(16) -0.00280(11) 0.00543(10) 0.00515(11) I3 0.01953(14) 0.04208(18) 0.04960(19) -0.00187(13) 0.00751(11) 0.01038(11) Pd 0.02245(15) 0.01730(15) 0.01954(15) 0.00105(10) 0.00419(11) 0.00488(11) P 0.0371(6) 0.0221(5) 0.0290(5) -0.0045(4) -0.0024(4) 0.0094(4) N11 0.0205(15) 0.0205(15) 0.0189(15) 0.0016(12) 0.0045(11) 0.0045(12) N12 0.0186(15) 0.0186(15) 0.0232(16) 0.0032(12) 0.0064(12) 0.0032(11) N13 0.0186(15) 0.0247(16) 0.0213(15) 0.0046(12) 0.0052(12) 0.0056(12) N14 0.0190(15) 0.0220(16) 0.0235(16) 0.0052(12) 0.0072(12) 0.0061(12) C1A 0.034(2) 0.041(2) 0.024(2) 0.0012(17) 0.0115(17) 0.0068(18) C1B 0.044(3) 0.039(2) 0.024(2) 0.0024(17) 0.0041(18) 0.023(2) C1C 0.069(4) 0.035(3) 0.028(2) 0.0092(19) 0.005(2) -0.010(2) C1D 0.035(2) 0.038(2) 0.032(2) 0.0153(18) 0.0127(18) 0.0181(19) C1E 0.033(2) 0.030(2) 0.049(3) 0.0099(19) 0.012(2) 0.0044(18) C1F 0.050(3) 0.052(3) 0.019(2) 0.0118(18) 0.0182(18) 0.023(2) C10 0.036(2) 0.024(2) 0.0205(19) 0.0042(15) 0.0062(16) 0.0035(16) C11 0.0155(16) 0.0181(17) 0.0238(18) 0.0023(13) 0.0058(13) 0.0023(13) C12 0.0250(19) 0.0191(18) 0.030(2) -0.0015(15) 0.0071(15) 0.0034(14) C13 0.0235(19) 0.0178(18) 0.034(2) 0.0032(15) 0.0069(15) 0.0048(14) C14 0.0197(18) 0.0261(19) 0.0214(18) 0.0052(14) 0.0027(14) 0.0012(14) C15 0.0183(17) 0.0269(19) 0.0226(18) 0.0040(14) 0.0040(14) 0.0075(14) C16 0.0243(19) 0.030(2) 0.028(2) 0.0077(16) 0.0047(15) 0.0112(16) C17 0.0186(18) 0.033(2) 0.033(2) 0.0067(16) 0.0074(15) 0.0116(15) C18 0.0238(19) 0.0224(19) 0.034(2) 0.0108(16) 0.0120(16) 0.0085(15) C21 0.038(2) 0.0193(19) 0.030(2) -0.0012(15) 0.0019(17) 0.0073(16) C22 0.063(3) 0.043(3) 0.030(2) 0.0055(19) 0.010(2) 0.028(2) C23 0.059(3) 0.052(3) 0.050(3) 0.006(2) 0.011(3) 0.032(3) C24 0.054(3) 0.025(2) 0.045(3) 0.0062(19) -0.005(2) 0.014(2) C25 0.056(3) 0.032(2) 0.032(2) 0.0107(18) 0.002(2) 0.004(2) C26 0.041(2) 0.033(2) 0.034(2) 0.0050(18) 0.0086(19) 0.0071(19) C27 0.092(4) 0.057(3) 0.021(2) -0.005(2) -0.008(2) 0.043(3) C28 0.044(3) 0.025(2) 0.085(4) -0.010(2) -0.008(3) 0.002(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Pd 2.6158(5) . ? I2 Pd 2.6095(5) . ? Pd C11 2.049(4) . ? Pd P 2.3093(11) . ? P C27 1.806(5) . ? P C21 1.816(4) . ? P C28 1.818(5) . ? N11 C11 1.350(5) . ? N11 C12 1.393(5) . ? N11 C10 1.513(5) . ? N12 C11 1.359(5) . ? N12 C13 1.380(5) . ? N12 C14 1.456(5) . ? N13 C15 1.334(5) . ? N13 C16 1.382(5) . ? N13 C14 1.459(4) . ? N14 C15 1.329(5) . ? N14 C17 1.379(5) . ? N14 C18 1.511(5) . ? C1A C10 1.525(6) . ? C1B C10 1.527(6) . ? C1C C10 1.520(6) . ? C1D C18 1.521(5) . ? C1E C18 1.527(6) . ? C1F C18 1.520(6) . ? C12 C13 1.339(6) . ? C16 C17 1.346(6) . ? C21 C26 1.385(6) . ? C21 C22 1.386(7) . ? C22 C23 1.395(7) . ? C23 C24 1.367(7) . ? C24 C25 1.371(8) . ? C25 C26 1.389(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pd P 176.92(10) . . ? C11 Pd I2 87.45(10) . . ? P Pd I2 93.00(3) . . ? C11 Pd I1 90.49(10) . . ? P Pd I1 88.70(3) . . ? I2 Pd I1 173.030(14) . . ? C27 P C21 106.6(2) . . ? C27 P C28 103.3(3) . . ? C21 P C28 102.7(2) . . ? C27 P Pd 111.01(19) . . ? C21 P Pd 113.35(13) . . ? C28 P Pd 118.78(19) . . ? C11 N11 C12 110.4(3) . . ? C11 N11 C10 126.6(3) . . ? C12 N11 C10 122.6(3) . . ? C11 N12 C13 111.3(3) . . ? C11 N12 C14 124.7(3) . . ? C13 N12 C14 123.9(3) . . ? C15 N13 C16 108.9(3) . . ? C15 N13 C14 124.6(3) . . ? C16 N13 C14 126.4(3) . . ? C15 N14 C17 109.0(3) . . ? C15 N14 C18 125.7(3) . . ? C17 N14 C18 125.0(3) . . ? N11 C10 C1C 109.8(3) . . ? N11 C10 C1A 108.8(3) . . ? C1C C10 C1A 108.9(4) . . ? N11 C10 C1B 107.7(3) . . ? C1C C10 C1B 111.3(4) . . ? C1A C10 C1B 110.3(3) . . ? N11 C11 N12 104.5(3) . . ? N11 C11 Pd 133.0(3) . . ? N12 C11 Pd 122.4(3) . . ? C13 C12 N11 107.3(3) . . ? C12 C13 N12 106.4(3) . . ? N12 C14 N13 110.6(3) . . ? N14 C15 N13 108.0(3) . . ? C17 C16 N13 106.9(3) . . ? C16 C17 N14 107.2(3) . . ? N14 C18 C1F 107.3(3) . . ? N14 C18 C1D 108.8(3) . . ? C1F C18 C1D 111.5(4) . . ? N14 C18 C1E 107.3(3) . . ? C1F C18 C1E 110.9(4) . . ? C1D C18 C1E 110.8(4) . . ? C26 C21 C22 118.6(4) . . ? C26 C21 P 118.5(3) . . ? C22 C21 P 122.6(3) . . ? C21 C22 C23 120.1(5) . . ? C24 C23 C22 120.5(5) . . ? C23 C24 C25 120.0(5) . . ? C24 C25 C26 120.1(4) . . ? C21 C26 C25 120.7(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Pd P C27 1.2(19) . . . . ? I2 Pd P C27 99.5(2) . . . . ? I1 Pd P C27 -73.7(2) . . . . ? C11 Pd P C21 121.1(19) . . . . ? I2 Pd P C21 -140.57(16) . . . . ? I1 Pd P C21 46.20(16) . . . . ? C11 Pd P C28 -118.3(19) . . . . ? I2 Pd P C28 -19.9(2) . . . . ? I1 Pd P C28 166.8(2) . . . . ? C11 N11 C10 C1C -38.8(5) . . . . ? C12 N11 C10 C1C 148.3(4) . . . . ? C11 N11 C10 C1A -157.9(3) . . . . ? C12 N11 C10 C1A 29.2(5) . . . . ? C11 N11 C10 C1B 82.6(4) . . . . ? C12 N11 C10 C1B -90.3(4) . . . . ? C12 N11 C11 N12 -0.7(4) . . . . ? C10 N11 C11 N12 -174.3(3) . . . . ? C12 N11 C11 Pd -177.3(3) . . . . ? C10 N11 C11 Pd 9.1(6) . . . . ? C13 N12 C11 N11 0.1(4) . . . . ? C14 N12 C11 N11 -177.3(3) . . . . ? C13 N12 C11 Pd 177.2(2) . . . . ? C14 N12 C11 Pd -0.2(5) . . . . ? P Pd C11 N11 -168.0(16) . . . . ? I2 Pd C11 N11 93.6(3) . . . . ? I1 Pd C11 N11 -93.1(3) . . . . ? P Pd C11 N12 16(2) . . . . ? I2 Pd C11 N12 -82.6(3) . . . . ? I1 Pd C11 N12 90.8(3) . . . . ? C11 N11 C12 C13 1.0(4) . . . . ? C10 N11 C12 C13 174.9(3) . . . . ? N11 C12 C13 N12 -0.9(4) . . . . ? C11 N12 C13 C12 0.5(4) . . . . ? C14 N12 C13 C12 178.0(3) . . . . ? C11 N12 C14 N13 -123.2(4) . . . . ? C13 N12 C14 N13 59.6(5) . . . . ? C15 N13 C14 N12 -118.5(4) . . . . ? C16 N13 C14 N12 67.5(5) . . . . ? C17 N14 C15 N13 1.3(4) . . . . ? C18 N14 C15 N13 175.7(3) . . . . ? C16 N13 C15 N14 -1.4(4) . . . . ? C14 N13 C15 N14 -176.4(3) . . . . ? C15 N13 C16 C17 1.0(5) . . . . ? C14 N13 C16 C17 175.8(4) . . . . ? N13 C16 C17 N14 -0.2(5) . . . . ? C15 N14 C17 C16 -0.7(5) . . . . ? C18 N14 C17 C16 -175.2(4) . . . . ? C15 N14 C18 C1F -113.3(4) . . . . ? C17 N14 C18 C1F 60.3(5) . . . . ? C15 N14 C18 C1D 7.5(5) . . . . ? C17 N14 C18 C1D -178.9(4) . . . . ? C15 N14 C18 C1E 127.5(4) . . . . ? C17 N14 C18 C1E -59.0(5) . . . . ? C27 P C21 C26 -173.1(4) . . . . ? C28 P C21 C26 -64.8(4) . . . . ? Pd P C21 C26 64.5(4) . . . . ? C27 P C21 C22 12.7(5) . . . . ? C28 P C21 C22 120.9(4) . . . . ? Pd P C21 C22 -109.7(4) . . . . ? C26 C21 C22 C23 -0.3(7) . . . . ? P C21 C22 C23 173.9(4) . . . . ? C21 C22 C23 C24 -0.4(8) . . . . ? C22 C23 C24 C25 1.1(8) . . . . ? C23 C24 C25 C26 -1.0(8) . . . . ? C22 C21 C26 C25 0.4(7) . . . . ? P C21 C26 C25 -174.1(4) . . . . ? C24 C25 C26 C21 0.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.40 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.306 _refine_diff_density_min -0.697 _refine_diff_density_rms 0.134 #===END data_13b _database_code_depnum_ccdc_archive 'CCDC 726825' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H47 I N4 P2 Pd, 1.5(C2 H3 N), 2(I)' _chemical_formula_sum 'C34 H51.50 I3 N5.50 P2 Pd' _chemical_formula_weight 1086.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 15.060(2) _cell_length_b 13.1140(17) _cell_length_c 22.022(3) _cell_angle_alpha 90.00 _cell_angle_beta 96.159(2) _cell_angle_gamma 90.00 _cell_volume 4324.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9089 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 28.39 _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2116 _exptl_absorpt_coefficient_mu 2.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3564 _exptl_absorpt_correction_T_max 0.5437 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 36366 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0282 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9905 _reflns_number_gt 8875 _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^)+(0.0281P)^2^+2.5400P] 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 9905 _refine_ls_number_parameters 426 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0283 _refine_ls_R_factor_gt 0.0241 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 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 I1 I 0.406332(10) 0.451846(12) 0.314654(7) 0.02819(4) Uani 1 1 d . . . I2 I -0.084995(11) 0.323306(13) 0.353326(7) 0.03046(5) Uani 1 1 d . . . I3 I 0.329487(13) 0.269998(15) 0.504550(8) 0.04085(5) Uani 1 1 d . . . Pd Pd 0.296870(11) 0.302282(13) 0.274416(7) 0.02020(4) Uani 1 1 d . . . P1 P 0.19230(4) 0.18037(5) 0.24745(3) 0.02534(12) Uani 1 1 d . . . P2 P 0.41796(4) 0.19174(5) 0.28791(3) 0.02840(13) Uani 1 1 d . . . N11 N 0.17480(13) 0.48164(15) 0.22151(8) 0.0245(4) Uani 1 1 d . . . N12 N 0.15708(12) 0.44265(14) 0.31402(8) 0.0227(4) Uani 1 1 d . . . N13 N 0.17742(13) 0.45708(15) 0.42270(8) 0.0242(4) Uani 1 1 d . . . N14 N 0.24879(13) 0.55297(16) 0.49124(9) 0.0264(4) Uani 1 1 d . . . C1A C 0.2705(2) 0.5794(2) 0.15993(13) 0.0410(6) Uani 1 1 d . . . H1AA H 0.3230 0.5646 0.1888 0.049 Uiso 1 1 calc R . . H1AB H 0.2414 0.6416 0.1726 0.049 Uiso 1 1 calc R . . H1AC H 0.2891 0.5893 0.1190 0.049 Uiso 1 1 calc R . . C1B C 0.1235(2) 0.5111(2) 0.11368(12) 0.0435(7) Uani 1 1 d . . . H1BA H 0.0952 0.5749 0.1245 0.052 Uiso 1 1 calc R . . H1BB H 0.0810 0.4547 0.1152 0.052 Uiso 1 1 calc R . . H1BC H 0.1415 0.5166 0.0723 0.052 Uiso 1 1 calc R . . C1C C 0.2497(2) 0.3928(2) 0.14119(13) 0.0476(8) Uani 1 1 d . . . H1CA H 0.3028 0.3798 0.1699 0.057 Uiso 1 1 calc R . . H1CB H 0.2672 0.3993 0.0998 0.057 Uiso 1 1 calc R . . H1CC H 0.2076 0.3361 0.1425 0.057 Uiso 1 1 calc R . . C1D C 0.3330(2) 0.5661(2) 0.59162(12) 0.0405(6) Uani 1 1 d . . . H1DA H 0.2779 0.5764 0.6108 0.049 Uiso 1 1 calc R . . H1DB H 0.3827 0.5999 0.6161 0.049 Uiso 1 1 calc R . . H1DC H 0.3454 0.4929 0.5893 0.049 Uiso 1 1 calc R . . C1E C 0.4068(2) 0.5976(3) 0.49660(15) 0.0493(8) Uani 1 1 d . . . H1EA H 0.3984 0.6275 0.4556 0.059 Uiso 1 1 calc R . . H1EB H 0.4202 0.5248 0.4935 0.059 Uiso 1 1 calc R . . H1EC H 0.4566 0.6319 0.5208 0.059 Uiso 1 1 calc R . . C1F C 0.2934(2) 0.7219(2) 0.52816(15) 0.0493(8) Uani 1 1 d . . . H1FA H 0.2390 0.7278 0.5486 0.059 Uiso 1 1 calc R . . H1FB H 0.2816 0.7469 0.4861 0.059 Uiso 1 1 calc R . . H1FC H 0.3410 0.7627 0.5502 0.059 Uiso 1 1 calc R . . C10 C 0.20541(18) 0.49092(19) 0.15879(11) 0.0305(5) Uani 1 1 d . . . C11 C 0.20137(14) 0.41448(17) 0.26604(10) 0.0209(4) Uani 1 1 d . . . C12 C 0.11658(18) 0.5532(2) 0.24225(11) 0.0323(5) Uani 1 1 d . . . H12 H 0.0898 0.6090 0.2197 0.039 Uiso 1 1 calc R . . C13 C 0.10541(17) 0.5282(2) 0.30017(11) 0.0315(5) Uani 1 1 d . . . H13 H 0.0692 0.5627 0.3264 0.038 Uiso 1 1 calc R . . C14 C 0.16171(16) 0.38789(18) 0.37154(10) 0.0242(5) Uani 1 1 d . . . H14A H 0.1050 0.3508 0.3742 0.029 Uiso 1 1 calc R . . H14B H 0.2106 0.3371 0.3733 0.029 Uiso 1 1 calc R . . C15 C 0.25571(16) 0.50003(19) 0.44088(10) 0.0259(5) Uani 1 1 d . . . H15 H 0.3083 0.4937 0.4209 0.031 Uiso 1 1 calc R . . C16 C 0.11817(17) 0.4812(2) 0.46439(12) 0.0367(6) Uani 1 1 d . . . H16 H 0.0576 0.4601 0.4630 0.044 Uiso 1 1 calc R . . C17 C 0.16272(18) 0.5401(2) 0.50719(12) 0.0387(6) Uani 1 1 d . . . H17 H 0.1396 0.5680 0.5421 0.046 Uiso 1 1 calc R . . C18 C 0.32214(17) 0.6112(2) 0.52749(11) 0.0318(5) Uani 1 1 d . . . C21 C 0.18320(16) 0.08398(19) 0.30599(11) 0.0291(5) Uani 1 1 d . . . C22 C 0.21876(18) 0.1022(2) 0.36613(12) 0.0341(6) Uani 1 1 d . . . H22 H 0.2502 0.1637 0.3762 0.041 Uiso 1 1 calc R . . C23 C 0.2084(2) 0.0305(2) 0.41135(14) 0.0444(7) Uani 1 1 d . . . H23 H 0.2320 0.0437 0.4523 0.053 Uiso 1 1 calc R . . C24 C 0.1637(2) -0.0600(2) 0.39690(16) 0.0498(8) Uani 1 1 d . . . H24 H 0.1572 -0.1093 0.4277 0.060 Uiso 1 1 calc R . . C25 C 0.1289(2) -0.0779(2) 0.33758(16) 0.0490(7) Uani 1 1 d . . . H25 H 0.0981 -0.1399 0.3277 0.059 Uiso 1 1 calc R . . C26 C 0.13801(19) -0.0073(2) 0.29193(14) 0.0399(6) Uani 1 1 d . . . H26 H 0.1136 -0.0209 0.2512 0.048 Uiso 1 1 calc R . . C27 C 0.07904(16) 0.2282(2) 0.23285(12) 0.0334(6) Uani 1 1 d . . . H27A H 0.0383 0.1713 0.2216 0.040 Uiso 1 1 calc R . . H27B H 0.0757 0.2776 0.1993 0.040 Uiso 1 1 calc R . . H27C H 0.0619 0.2614 0.2697 0.040 Uiso 1 1 calc R . . C28 C 0.2060(2) 0.1120(2) 0.17749(12) 0.0384(6) Uani 1 1 d . . . H28A H 0.1582 0.0614 0.1698 0.046 Uiso 1 1 calc R . . H28B H 0.2640 0.0774 0.1815 0.046 Uiso 1 1 calc R . . H28C H 0.2032 0.1602 0.1433 0.046 Uiso 1 1 calc R . . C31 C 0.50162(16) 0.23183(18) 0.23912(11) 0.0276(5) Uani 1 1 d . . . C32 C 0.47666(18) 0.2373(2) 0.17639(12) 0.0359(6) Uani 1 1 d . . . H32 H 0.4177 0.2192 0.1603 0.043 Uiso 1 1 calc R . . C33 C 0.5374(2) 0.2691(2) 0.13756(13) 0.0447(7) Uani 1 1 d . . . H33 H 0.5199 0.2733 0.0949 0.054 Uiso 1 1 calc R . . C34 C 0.6238(2) 0.2950(2) 0.16061(15) 0.0474(7) Uani 1 1 d . . . H34 H 0.6655 0.3166 0.1338 0.057 Uiso 1 1 calc R . . C35 C 0.64903(19) 0.2894(2) 0.22243(15) 0.0418(7) Uani 1 1 d . . . H35 H 0.7083 0.3067 0.2382 0.050 Uiso 1 1 calc R . . C36 C 0.58795(17) 0.2586(2) 0.26190(12) 0.0323(5) Uani 1 1 d . . . H36 H 0.6054 0.2558 0.3046 0.039 Uiso 1 1 calc R . . C37 C 0.4055(2) 0.0563(2) 0.27133(17) 0.0489(8) Uani 1 1 d . . . H37A H 0.4635 0.0225 0.2798 0.059 Uiso 1 1 calc R . . H37B H 0.3832 0.0470 0.2282 0.059 Uiso 1 1 calc R . . H37C H 0.3630 0.0265 0.2970 0.059 Uiso 1 1 calc R . . C38 C 0.4716(2) 0.1908(3) 0.36554(13) 0.0453(7) Uani 1 1 d . . . H38A H 0.5219 0.1431 0.3686 0.054 Uiso 1 1 calc R . . H38B H 0.4284 0.1694 0.3933 0.054 Uiso 1 1 calc R . . H38C H 0.4934 0.2594 0.3767 0.054 Uiso 1 1 calc R . . N1S N -0.0087(3) 0.2038(4) 0.08411(18) 0.0915(13) Uani 1 1 d D . . C1S C 0.0219(3) 0.2450(3) 0.04649(18) 0.0627(10) Uani 1 1 d D . . C2S C 0.0621(3) 0.2985(3) -0.00189(17) 0.0698(11) Uani 1 1 d D . . H2SA H 0.1253 0.2798 -0.0005 0.084 Uiso 1 1 calc R . . H2SB H 0.0569 0.3723 0.0039 0.084 Uiso 1 1 calc R . . H2SC H 0.0311 0.2793 -0.0416 0.084 Uiso 1 1 calc R . . N2S N 0.6144(7) 0.0551(7) 0.4874(5) 0.120(4) Uani 0.50 1 d PD A -1 C3S C 0.5524(15) 0.0178(18) 0.5025(16) 0.114(10) Uani 0.50 1 d PD A -1 C4S C 0.4626(14) -0.024(2) 0.5052(14) 0.088(7) Uani 0.50 1 d PD A -1 H4SA H 0.4181 0.0299 0.4970 0.106 Uiso 0.50 1 calc PR A -1 H4SB H 0.4582 -0.0528 0.5459 0.106 Uiso 0.50 1 calc PR A -1 H4SC H 0.4515 -0.0782 0.4745 0.106 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.02102(8) 0.02913(9) 0.03497(9) -0.00723(6) 0.00553(6) -0.00601(6) I2 0.02892(9) 0.03314(9) 0.02996(8) -0.00308(6) 0.00611(6) 0.00203(6) I3 0.04552(11) 0.04245(11) 0.03344(9) 0.00447(7) -0.00107(8) 0.00272(8) Pd 0.01682(8) 0.01921(9) 0.02497(8) -0.00365(6) 0.00404(6) -0.00008(6) P1 0.0240(3) 0.0242(3) 0.0284(3) -0.0081(2) 0.0055(2) -0.0043(2) P2 0.0231(3) 0.0262(3) 0.0371(3) 0.0008(3) 0.0087(3) 0.0053(2) N11 0.0255(10) 0.0248(10) 0.0233(9) -0.0016(7) 0.0025(7) 0.0039(8) N12 0.0197(9) 0.0259(10) 0.0222(9) -0.0028(7) 0.0013(7) 0.0030(7) N13 0.0224(10) 0.0297(11) 0.0205(9) -0.0030(7) 0.0028(7) 0.0018(8) N14 0.0240(10) 0.0321(11) 0.0234(9) -0.0033(8) 0.0038(8) -0.0003(8) C1A 0.0402(16) 0.0446(16) 0.0392(14) 0.0065(12) 0.0081(12) -0.0057(13) C1B 0.0525(18) 0.0498(18) 0.0265(12) -0.0008(12) -0.0033(12) 0.0000(14) C1C 0.074(2) 0.0393(16) 0.0330(14) 0.0025(12) 0.0246(14) 0.0153(15) C1D 0.0403(16) 0.0490(17) 0.0308(13) -0.0027(12) -0.0028(11) -0.0094(13) C1E 0.0338(15) 0.066(2) 0.0502(17) -0.0186(15) 0.0117(13) -0.0197(14) C1F 0.064(2) 0.0316(15) 0.0509(18) -0.0055(13) -0.0006(15) -0.0050(14) C10 0.0421(15) 0.0279(13) 0.0227(11) 0.0000(9) 0.0082(10) 0.0006(11) C11 0.0180(10) 0.0222(11) 0.0221(10) -0.0050(8) 0.0005(8) -0.0020(8) C12 0.0345(14) 0.0329(14) 0.0292(12) 0.0007(10) 0.0021(10) 0.0143(11) C13 0.0314(13) 0.0343(14) 0.0290(12) -0.0023(10) 0.0050(10) 0.0127(10) C14 0.0264(12) 0.0260(12) 0.0203(10) -0.0021(9) 0.0025(9) 0.0013(9) C15 0.0232(11) 0.0326(13) 0.0221(10) -0.0008(9) 0.0038(9) -0.0026(9) C16 0.0226(12) 0.0541(17) 0.0347(13) -0.0144(12) 0.0085(10) 0.0024(11) C17 0.0259(13) 0.0569(18) 0.0342(13) -0.0179(12) 0.0076(11) 0.0001(12) C18 0.0320(13) 0.0348(14) 0.0285(12) -0.0064(10) 0.0028(10) -0.0100(11) C21 0.0257(12) 0.0265(12) 0.0363(13) -0.0042(10) 0.0082(10) -0.0042(10) C22 0.0325(13) 0.0318(14) 0.0386(13) -0.0037(11) 0.0067(11) -0.0050(11) C23 0.0459(17) 0.0471(17) 0.0405(15) 0.0036(13) 0.0067(13) 0.0000(13) C24 0.0469(18) 0.0443(18) 0.0600(19) 0.0164(15) 0.0143(15) -0.0006(14) C25 0.0458(18) 0.0329(15) 0.068(2) 0.0057(14) 0.0062(15) -0.0117(13) C26 0.0367(15) 0.0336(15) 0.0492(16) -0.0064(12) 0.0034(12) -0.0114(12) C27 0.0217(12) 0.0391(15) 0.0386(13) -0.0099(11) -0.0009(10) -0.0080(10) C28 0.0480(16) 0.0332(14) 0.0356(13) -0.0142(11) 0.0116(12) -0.0077(12) C31 0.0228(11) 0.0249(12) 0.0361(12) -0.0025(10) 0.0081(10) 0.0062(9) C32 0.0273(13) 0.0432(15) 0.0370(14) -0.0053(11) 0.0028(11) 0.0051(11) C33 0.0483(18) 0.0531(19) 0.0345(14) -0.0014(13) 0.0127(13) 0.0059(14) C34 0.0467(18) 0.0465(17) 0.0533(18) 0.0008(14) 0.0250(15) 0.0001(14) C35 0.0260(13) 0.0395(16) 0.0609(18) -0.0043(13) 0.0090(13) -0.0025(11) C36 0.0277(13) 0.0309(13) 0.0382(13) -0.0027(10) 0.0035(10) 0.0043(10) C37 0.0415(17) 0.0260(14) 0.084(2) 0.0016(14) 0.0287(16) 0.0076(12) C38 0.0381(16) 0.062(2) 0.0359(14) 0.0149(13) 0.0067(12) 0.0162(14) N1S 0.102(3) 0.111(3) 0.060(2) -0.015(2) -0.002(2) -0.018(3) C1S 0.065(2) 0.070(3) 0.049(2) -0.0259(19) -0.0108(18) -0.001(2) C2S 0.072(3) 0.078(3) 0.055(2) -0.026(2) -0.0076(19) -0.007(2) N2S 0.103(8) 0.075(6) 0.173(10) 0.065(6) -0.026(7) -0.017(5) C3S 0.112(16) 0.040(8) 0.17(2) 0.033(10) -0.056(12) -0.002(8) C4S 0.070(8) 0.087(14) 0.101(10) 0.050(8) -0.023(9) -0.004(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 I1 Pd 2.6526(3) . ? Pd C11 2.052(2) . ? Pd P1 2.2778(6) . ? Pd P2 2.3236(7) . ? P1 C27 1.813(3) . ? P1 C28 1.814(2) . ? P1 C21 1.821(3) . ? P2 C38 1.811(3) . ? P2 C37 1.819(3) . ? P2 C31 1.819(2) . ? N11 C11 1.347(3) . ? N11 C12 1.394(3) . ? N11 C10 1.507(3) . ? N12 C11 1.360(3) . ? N12 C13 1.381(3) . ? N12 C14 1.451(3) . ? N13 C15 1.329(3) . ? N13 C16 1.384(3) . ? N13 C14 1.446(3) . ? N14 C15 1.322(3) . ? N14 C17 1.389(3) . ? N14 C18 1.500(3) . ? C1A C10 1.517(4) . ? C1B C10 1.522(4) . ? C1C C10 1.518(4) . ? C1D C18 1.524(4) . ? C1E C18 1.519(4) . ? C1F C18 1.516(4) . ? C12 C13 1.345(3) . ? C16 C17 1.341(4) . ? C21 C22 1.395(4) . ? C21 C26 1.395(4) . ? C22 C23 1.390(4) . ? C23 C24 1.385(5) . ? C24 C25 1.375(5) . ? C25 C26 1.384(4) . ? C31 C36 1.387(4) . ? C31 C32 1.394(4) . ? C32 C33 1.382(4) . ? C33 C34 1.387(5) . ? C34 C35 1.376(5) . ? C35 C36 1.392(4) . ? N1S C1S 1.128(5) . ? C1S C2S 1.460(6) . ? N2S C3S 1.135(11) . ? C3S C4S 1.468(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pd P1 91.23(6) . . ? C11 Pd P2 172.64(6) . . ? P1 Pd P2 96.12(3) . . ? C11 Pd I1 84.51(6) . . ? P1 Pd I1 173.519(17) . . ? P2 Pd I1 88.14(2) . . ? C27 P1 C28 102.18(13) . . ? C27 P1 C21 102.98(12) . . ? C28 P1 C21 106.39(12) . . ? C27 P1 Pd 114.49(9) . . ? C28 P1 Pd 115.47(9) . . ? C21 P1 Pd 113.90(8) . . ? C38 P2 C37 102.07(17) . . ? C38 P2 C31 107.02(13) . . ? C37 P2 C31 103.12(12) . . ? C38 P2 Pd 112.91(10) . . ? C37 P2 Pd 121.37(11) . . ? C31 P2 Pd 109.15(8) . . ? C11 N11 C12 110.48(18) . . ? C11 N11 C10 128.61(19) . . ? C12 N11 C10 120.71(19) . . ? C11 N12 C13 111.15(19) . . ? C11 N12 C14 124.21(19) . . ? C13 N12 C14 124.62(19) . . ? C15 N13 C16 108.5(2) . . ? C15 N13 C14 124.49(19) . . ? C16 N13 C14 126.7(2) . . ? C15 N14 C17 107.9(2) . . ? C15 N14 C18 126.4(2) . . ? C17 N14 C18 125.52(19) . . ? N11 C10 C1A 107.9(2) . . ? N11 C10 C1C 110.6(2) . . ? C1A C10 C1C 110.6(2) . . ? N11 C10 C1B 107.8(2) . . ? C1A C10 C1B 110.8(2) . . ? C1C C10 C1B 109.1(2) . . ? N11 C11 N12 104.84(19) . . ? N11 C11 Pd 133.24(15) . . ? N12 C11 Pd 121.50(16) . . ? C13 C12 N11 107.1(2) . . ? C12 C13 N12 106.4(2) . . ? N13 C14 N12 110.98(19) . . ? N14 C15 N13 109.2(2) . . ? C17 C16 N13 106.8(2) . . ? C16 C17 N14 107.6(2) . . ? N14 C18 C1F 107.3(2) . . ? N14 C18 C1E 107.9(2) . . ? C1F C18 C1E 111.8(3) . . ? N14 C18 C1D 107.2(2) . . ? C1F C18 C1D 111.4(2) . . ? C1E C18 C1D 111.0(3) . . ? C22 C21 C26 119.1(2) . . ? C22 C21 P1 120.21(19) . . ? C26 C21 P1 120.7(2) . . ? C23 C22 C21 120.2(3) . . ? C24 C23 C22 120.3(3) . . ? C25 C24 C23 119.4(3) . . ? C24 C25 C26 121.2(3) . . ? C25 C26 C21 119.8(3) . . ? C36 C31 C32 119.2(2) . . ? C36 C31 P2 122.8(2) . . ? C32 C31 P2 118.0(2) . . ? C33 C32 C31 120.2(3) . . ? C32 C33 C34 120.3(3) . . ? C35 C34 C33 119.8(3) . . ? C34 C35 C36 120.2(3) . . ? C31 C36 C35 120.3(3) . . ? N1S C1S C2S 179.6(5) . . ? N2S C3S C4S 165(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Pd P1 C27 -1.14(11) . . . . ? P2 Pd P1 C27 178.55(10) . . . . ? I1 Pd P1 C27 47.7(2) . . . . ? C11 Pd P1 C28 117.13(13) . . . . ? P2 Pd P1 C28 -63.18(12) . . . . ? I1 Pd P1 C28 165.96(18) . . . . ? C11 Pd P1 C21 -119.30(10) . . . . ? P2 Pd P1 C21 60.39(9) . . . . ? I1 Pd P1 C21 -70.5(2) . . . . ? C11 Pd P2 C38 59.9(5) . . . . ? P1 Pd P2 C38 -117.70(12) . . . . ? I1 Pd P2 C38 57.41(12) . . . . ? C11 Pd P2 C37 -179(11) . . . . ? P1 Pd P2 C37 3.87(13) . . . . ? I1 Pd P2 C37 178.97(13) . . . . ? C11 Pd P2 C31 -59.0(5) . . . . ? P1 Pd P2 C31 123.42(9) . . . . ? I1 Pd P2 C31 -61.48(9) . . . . ? C11 N11 C10 C1A -102.1(3) . . . . ? C12 N11 C10 C1A 72.3(3) . . . . ? C11 N11 C10 C1C 19.0(4) . . . . ? C12 N11 C10 C1C -166.7(3) . . . . ? C11 N11 C10 C1B 138.2(2) . . . . ? C12 N11 C10 C1B -47.4(3) . . . . ? C12 N11 C11 N12 1.9(3) . . . . ? C10 N11 C11 N12 176.7(2) . . . . ? C12 N11 C11 Pd -170.40(19) . . . . ? C10 N11 C11 Pd 4.4(4) . . . . ? C13 N12 C11 N11 -1.7(3) . . . . ? C14 N12 C11 N11 176.6(2) . . . . ? C13 N12 C11 Pd 171.72(17) . . . . ? C14 N12 C11 Pd -9.9(3) . . . . ? P1 Pd C11 N11 -98.8(2) . . . . ? P2 Pd C11 N11 83.6(5) . . . . ? I1 Pd C11 N11 86.1(2) . . . . ? P1 Pd C11 N12 89.93(17) . . . . ? P2 Pd C11 N12 -87.7(5) . . . . ? I1 Pd C11 N12 -85.18(17) . . . . ? C11 N11 C12 C13 -1.4(3) . . . . ? C10 N11 C12 C13 -176.7(2) . . . . ? N11 C12 C13 N12 0.3(3) . . . . ? C11 N12 C13 C12 0.9(3) . . . . ? C14 N12 C13 C12 -177.5(2) . . . . ? C15 N13 C14 N12 -75.6(3) . . . . ? C16 N13 C14 N12 111.8(3) . . . . ? C11 N12 C14 N13 132.5(2) . . . . ? C13 N12 C14 N13 -49.4(3) . . . . ? C17 N14 C15 N13 2.2(3) . . . . ? C18 N14 C15 N13 178.5(2) . . . . ? C16 N13 C15 N14 -1.8(3) . . . . ? C14 N13 C15 N14 -175.6(2) . . . . ? C15 N13 C16 C17 0.6(3) . . . . ? C14 N13 C16 C17 174.2(2) . . . . ? N13 C16 C17 N14 0.7(3) . . . . ? C15 N14 C17 C16 -1.8(3) . . . . ? C18 N14 C17 C16 -178.1(3) . . . . ? C15 N14 C18 C1F 119.9(3) . . . . ? C17 N14 C18 C1F -64.5(3) . . . . ? C15 N14 C18 C1E -0.7(4) . . . . ? C17 N14 C18 C1E 174.9(3) . . . . ? C15 N14 C18 C1D -120.3(3) . . . . ? C17 N14 C18 C1D 55.3(3) . . . . ? C27 P1 C21 C22 -107.6(2) . . . . ? C28 P1 C21 C22 145.4(2) . . . . ? Pd P1 C21 C22 17.0(2) . . . . ? C27 P1 C21 C26 70.1(2) . . . . ? C28 P1 C21 C26 -36.9(3) . . . . ? Pd P1 C21 C26 -165.28(19) . . . . ? C26 C21 C22 C23 -0.6(4) . . . . ? P1 C21 C22 C23 177.1(2) . . . . ? C21 C22 C23 C24 0.9(4) . . . . ? C22 C23 C24 C25 -0.7(5) . . . . ? C23 C24 C25 C26 0.3(5) . . . . ? C24 C25 C26 C21 0.0(5) . . . . ? C22 C21 C26 C25 0.2(4) . . . . ? P1 C21 C26 C25 -177.6(2) . . . . ? C38 P2 C31 C36 -2.0(2) . . . . ? C37 P2 C31 C36 -109.2(2) . . . . ? Pd P2 C31 C36 120.51(19) . . . . ? C38 P2 C31 C32 179.2(2) . . . . ? C37 P2 C31 C32 72.0(2) . . . . ? Pd P2 C31 C32 -58.3(2) . . . . ? C36 C31 C32 C33 0.0(4) . . . . ? P2 C31 C32 C33 178.9(2) . . . . ? C31 C32 C33 C34 0.5(4) . . . . ? C32 C33 C34 C35 -0.3(5) . . . . ? C33 C34 C35 C36 -0.4(5) . . . . ? C32 C31 C36 C35 -0.7(4) . . . . ? P2 C31 C36 C35 -179.5(2) . . . . ? C34 C35 C36 C31 0.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.093 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.094 #===END data_16b _database_code_depnum_ccdc_archive 'CCDC 726826' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H47 I N4 P2 Pd, 2(I), C3 H6 O' _chemical_formula_sum 'C27 H53 I3 N4 O P2 Pd' _chemical_formula_weight 998.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 14.2452(6) _cell_length_b 21.1101(8) _cell_length_c 12.9669(5) _cell_angle_alpha 90.00 _cell_angle_beta 94.9031(4) _cell_angle_gamma 90.00 _cell_volume 3885.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9878 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 2.968 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.3360 _exptl_absorpt_correction_T_max 0.5013 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 33796 _diffrn_reflns_av_R_equivalents 0.0162 _diffrn_reflns_av_sigmaI/netI 0.0132 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.73 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8906 _reflns_number_gt 8022 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-2008 (Beurskens et al., 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^)+(0.0380P)^2^+5.5389P] 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 8906 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0760 _refine_ls_wR_factor_gt 0.0734 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 I1 I 0.226301(17) 0.486600(12) 0.473032(16) 0.05051(7) Uani 1 1 d . . . Pd Pd 0.225538(15) 0.535123(10) 0.283222(16) 0.03221(6) Uani 1 1 d . . . P1 P 0.18992(5) 0.57113(4) 0.11910(6) 0.03720(16) Uani 1 1 d . . . P2 P 0.07332(6) 0.57043(4) 0.27176(7) 0.04008(17) Uani 1 1 d . . . N11 N 0.44569(18) 0.54570(11) 0.30609(19) 0.0357(5) Uani 1 1 d . . . N12 N 0.39672(16) 0.45948(11) 0.23211(19) 0.0328(5) Uani 1 1 d . . . N13 N 0.33119(16) 0.35650(11) 0.26208(18) 0.0320(5) Uani 1 1 d . . . N14 N 0.27826(17) 0.29129(12) 0.3709(2) 0.0375(5) Uani 1 1 d . . . C10 C 0.4569(2) 0.60875(14) 0.3604(2) 0.0408(7) Uani 1 1 d . . . C11 C 0.3659(2) 0.51389(13) 0.2746(2) 0.0313(5) Uani 1 1 d . . . C12 C 0.5244(2) 0.51071(16) 0.2848(3) 0.0445(7) Uani 1 1 d . . . H12 H 0.5883 0.5227 0.3012 0.053 Uiso 1 1 calc R . . C13 C 0.4945(2) 0.45725(15) 0.2374(3) 0.0425(7) Uani 1 1 d . . . H13 H 0.5323 0.4245 0.2124 0.051 Uiso 1 1 calc R . . C14 C 0.3360(2) 0.40927(13) 0.1891(2) 0.0325(5) Uani 1 1 d . . . H14A H 0.3601 0.3936 0.1244 0.039 Uiso 1 1 calc R . . H14B H 0.2718 0.4263 0.1717 0.039 Uiso 1 1 calc R . . C15 C 0.2579(2) 0.34273(14) 0.3150(2) 0.0368(6) Uani 1 1 d . . . H15 H 0.2006 0.3659 0.3130 0.044 Uiso 1 1 calc R . . C16 C 0.4007(2) 0.31241(15) 0.2853(2) 0.0403(6) Uani 1 1 d . . . H16 H 0.4605 0.3109 0.2580 0.048 Uiso 1 1 calc R . . C17 C 0.3682(2) 0.27186(16) 0.3539(3) 0.0431(7) Uani 1 1 d . . . H17 H 0.4009 0.2365 0.3848 0.052 Uiso 1 1 calc R . . C18 C 0.2150(2) 0.25728(17) 0.4400(3) 0.0474(8) Uani 1 1 d . . . C1A C 0.3640(3) 0.64330(17) 0.3599(4) 0.0625(11) Uani 1 1 d . . . H1AA H 0.3195 0.6176 0.3956 0.075 Uiso 1 1 calc R . . H1AB H 0.3385 0.6506 0.2883 0.075 Uiso 1 1 calc R . . H1AC H 0.3737 0.6840 0.3954 0.075 Uiso 1 1 calc R . . C1B C 0.4953(3) 0.5961(2) 0.4712(3) 0.0647(11) Uani 1 1 d . . . H1BA H 0.4502 0.5702 0.5057 0.078 Uiso 1 1 calc R . . H1BB H 0.5052 0.6364 0.5080 0.078 Uiso 1 1 calc R . . H1BC H 0.5554 0.5734 0.4714 0.078 Uiso 1 1 calc R . . C1C C 0.5247(4) 0.6484(2) 0.3039(4) 0.0764(14) Uani 1 1 d . . . H1CA H 0.4977 0.6563 0.2331 0.092 Uiso 1 1 calc R . . H1CB H 0.5845 0.6256 0.3021 0.092 Uiso 1 1 calc R . . H1CC H 0.5358 0.6888 0.3401 0.092 Uiso 1 1 calc R . . C1D C 0.1173(3) 0.2850(3) 0.4237(5) 0.0920(19) Uani 1 1 d . . . H1DA H 0.1191 0.3298 0.4441 0.110 Uiso 1 1 calc R . . H1DB H 0.0748 0.2619 0.4659 0.110 Uiso 1 1 calc R . . H1DC H 0.0943 0.2815 0.3505 0.110 Uiso 1 1 calc R . . C1E C 0.2147(4) 0.1878(2) 0.4088(4) 0.0817(15) Uani 1 1 d . . . H1EA H 0.2789 0.1710 0.4187 0.098 Uiso 1 1 calc R . . H1EB H 0.1912 0.1838 0.3358 0.098 Uiso 1 1 calc R . . H1EC H 0.1736 0.1639 0.4516 0.098 Uiso 1 1 calc R . . C1F C 0.2558(3) 0.2650(2) 0.5504(3) 0.0635(10) Uani 1 1 d . . . H1FA H 0.3195 0.2472 0.5581 0.076 Uiso 1 1 calc R . . H1FB H 0.2160 0.2427 0.5967 0.076 Uiso 1 1 calc R . . H1FC H 0.2583 0.3101 0.5683 0.076 Uiso 1 1 calc R . . C20 C 0.0632(2) 0.5773(2) 0.1306(3) 0.0507(8) Uani 1 1 d . . . H20A H 0.0271 0.5420 0.0960 0.061 Uiso 1 1 calc R . . H20B H 0.0367 0.6185 0.1060 0.061 Uiso 1 1 calc R . . C21 C 0.2364(2) 0.64848(15) 0.0911(3) 0.0436(7) Uani 1 1 d . . . H21A H 0.2246 0.6775 0.1485 0.052 Uiso 1 1 calc R . . H21B H 0.3055 0.6450 0.0888 0.052 Uiso 1 1 calc R . . C22 C 0.1950(3) 0.6775(2) -0.0098(3) 0.0642(11) Uani 1 1 d . . . H22A H 0.2242 0.7188 -0.0196 0.077 Uiso 1 1 calc R . . H22B H 0.1269 0.6829 -0.0074 0.077 Uiso 1 1 calc R . . H22C H 0.2071 0.6494 -0.0674 0.077 Uiso 1 1 calc R . . C23 C 0.2036(3) 0.52147(17) 0.0068(3) 0.0487(8) Uani 1 1 d . . . H23A H 0.1806 0.4784 0.0212 0.058 Uiso 1 1 calc R . . H23B H 0.1632 0.5386 -0.0526 0.058 Uiso 1 1 calc R . . C24 C 0.3040(3) 0.51636(18) -0.0240(3) 0.0548(9) Uani 1 1 d . . . H24A H 0.3054 0.4880 -0.0837 0.066 Uiso 1 1 calc R . . H24B H 0.3448 0.4993 0.0342 0.066 Uiso 1 1 calc R . . H24C H 0.3265 0.5584 -0.0422 0.066 Uiso 1 1 calc R . . C25 C -0.0252(2) 0.52489(17) 0.3097(3) 0.0468(7) Uani 1 1 d . . . H25A H -0.0194 0.4808 0.2850 0.056 Uiso 1 1 calc R . . H25B H -0.0226 0.5237 0.3863 0.056 Uiso 1 1 calc R . . C26 C -0.1209(3) 0.5512(2) 0.2676(3) 0.0559(9) Uani 1 1 d . . . H26A H -0.1712 0.5240 0.2899 0.067 Uiso 1 1 calc R . . H26B H -0.1243 0.5523 0.1918 0.067 Uiso 1 1 calc R . . H26C H -0.1285 0.5942 0.2941 0.067 Uiso 1 1 calc R . . C27 C 0.0622(3) 0.65086(19) 0.3216(4) 0.0676(11) Uani 1 1 d . . . H27A H 0.1074 0.6787 0.2895 0.081 Uiso 1 1 calc R . . H27B H -0.0021 0.6667 0.3009 0.081 Uiso 1 1 calc R . . C28 C 0.0798(5) 0.6551(3) 0.4361(5) 0.109(2) Uani 1 1 d . . . H28A H 0.0750 0.6994 0.4578 0.131 Uiso 1 1 calc R . . H28B H 0.1431 0.6391 0.4574 0.131 Uiso 1 1 calc R . . H28C H 0.0330 0.6296 0.4686 0.131 Uiso 1 1 calc R . . I2 I 0.060765(15) 0.384083(13) 0.135392(18) 0.05092(7) Uani 1 1 d . . . I3 I 0.526485(16) 0.174285(11) 0.535537(18) 0.04948(7) Uani 1 1 d . . . O1S O 0.1801(4) 0.7723(2) 0.2124(5) 0.139(2) Uani 1 1 d . . . C1S C 0.3245(4) 0.8125(3) 0.1680(5) 0.0911(16) Uani 1 1 d . . . H1SA H 0.3683 0.8089 0.2303 0.109 Uiso 1 1 calc R . . H1SB H 0.3403 0.8502 0.1288 0.109 Uiso 1 1 calc R . . H1SC H 0.3295 0.7747 0.1250 0.109 Uiso 1 1 calc R . . C2S C 0.2271(4) 0.8183(2) 0.1984(4) 0.0775(14) Uani 1 1 d . . . C3S C 0.1952(7) 0.8822(3) 0.2148(5) 0.128(3) Uani 1 1 d . . . H3SA H 0.1476 0.8818 0.2650 0.153 Uiso 1 1 calc R . . H3SB H 0.1677 0.8998 0.1491 0.153 Uiso 1 1 calc R . . H3SC H 0.2487 0.9084 0.2414 0.153 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.06033(14) 0.06190(15) 0.03002(10) 0.00755(9) 0.00812(9) 0.00566(10) Pd 0.03529(11) 0.03407(11) 0.02728(10) 0.00156(8) 0.00277(8) 0.00317(8) P1 0.0378(4) 0.0415(4) 0.0320(4) 0.0071(3) 0.0012(3) -0.0028(3) P2 0.0386(4) 0.0404(4) 0.0418(4) 0.0040(3) 0.0066(3) 0.0057(3) N11 0.0394(13) 0.0303(12) 0.0368(12) -0.0036(10) -0.0009(10) -0.0025(10) N12 0.0334(12) 0.0293(11) 0.0356(12) -0.0019(9) 0.0022(9) -0.0014(9) N13 0.0341(11) 0.0294(11) 0.0323(11) -0.0012(9) 0.0018(9) -0.0011(9) N14 0.0373(12) 0.0379(13) 0.0374(13) 0.0025(10) 0.0026(10) -0.0050(10) C10 0.0498(17) 0.0332(15) 0.0384(16) -0.0068(12) -0.0032(13) -0.0054(13) C11 0.0367(14) 0.0301(13) 0.0270(12) 0.0011(10) 0.0022(10) -0.0003(11) C12 0.0342(15) 0.0419(16) 0.057(2) -0.0046(14) 0.0008(13) -0.0046(13) C13 0.0332(14) 0.0399(16) 0.0547(19) -0.0056(14) 0.0046(13) -0.0005(12) C14 0.0374(14) 0.0282(13) 0.0317(13) -0.0007(10) 0.0012(11) -0.0037(11) C15 0.0331(14) 0.0371(15) 0.0401(15) 0.0014(12) 0.0024(11) -0.0015(11) C16 0.0388(15) 0.0399(16) 0.0426(16) 0.0022(13) 0.0058(12) 0.0057(12) C17 0.0449(16) 0.0412(16) 0.0433(17) 0.0065(13) 0.0049(13) 0.0070(13) C18 0.0476(18) 0.0501(19) 0.0453(17) 0.0107(15) 0.0083(14) -0.0094(14) C1A 0.065(2) 0.0379(18) 0.081(3) -0.0204(18) -0.016(2) 0.0050(16) C1B 0.088(3) 0.058(2) 0.044(2) -0.0125(17) -0.0156(19) 0.014(2) C1C 0.108(4) 0.045(2) 0.081(3) -0.016(2) 0.033(3) -0.031(2) C1D 0.046(2) 0.124(5) 0.108(4) 0.058(4) 0.023(2) -0.002(3) C1E 0.114(4) 0.057(3) 0.079(3) -0.007(2) 0.033(3) -0.039(3) C1F 0.071(3) 0.080(3) 0.0405(19) 0.0042(18) 0.0137(17) -0.010(2) C20 0.0387(16) 0.068(2) 0.0450(18) 0.0188(16) 0.0011(14) -0.0002(15) C21 0.0472(17) 0.0402(16) 0.0433(17) 0.0085(13) 0.0032(13) -0.0037(13) C22 0.073(3) 0.058(2) 0.060(2) 0.0249(19) -0.007(2) -0.0115(19) C23 0.064(2) 0.0499(19) 0.0320(15) 0.0013(13) 0.0011(14) -0.0136(16) C24 0.074(2) 0.052(2) 0.0410(18) 0.0018(15) 0.0157(17) -0.0052(18) C25 0.0436(17) 0.0492(18) 0.0495(18) 0.0087(15) 0.0149(14) -0.0001(14) C26 0.0451(18) 0.068(2) 0.055(2) 0.0092(18) 0.0101(16) -0.0011(17) C27 0.061(2) 0.047(2) 0.097(3) -0.006(2) 0.021(2) 0.0074(18) C28 0.112(5) 0.093(4) 0.127(5) -0.055(4) 0.036(4) 0.001(4) I2 0.03870(11) 0.06843(16) 0.04513(12) 0.00206(10) 0.00061(9) -0.00098(9) I3 0.05259(13) 0.05127(13) 0.04666(12) 0.01134(9) 0.01630(10) 0.01271(10) O1S 0.151(4) 0.067(2) 0.214(6) -0.035(3) 0.099(4) -0.029(3) C1S 0.076(3) 0.098(4) 0.099(4) -0.007(3) 0.007(3) -0.015(3) C2S 0.118(4) 0.059(3) 0.058(3) -0.009(2) 0.018(3) -0.011(3) C3S 0.232(9) 0.076(4) 0.083(4) 0.018(3) 0.056(5) 0.031(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 I1 Pd 2.6651(3) . ? Pd C11 2.062(3) . ? Pd P1 2.2758(8) . ? Pd P2 2.2857(8) . ? P1 C21 1.811(3) . ? P1 C23 1.818(4) . ? P1 C20 1.829(3) . ? P2 C25 1.804(3) . ? P2 C27 1.829(4) . ? P2 C20 1.829(3) . ? N11 C11 1.353(4) . ? N11 C12 1.390(4) . ? N11 C10 1.508(4) . ? N12 C11 1.363(4) . ? N12 C13 1.390(4) . ? N12 C14 1.449(3) . ? N13 C15 1.329(4) . ? N13 C16 1.373(4) . ? N13 C14 1.467(4) . ? N14 C15 1.324(4) . ? N14 C17 1.381(4) . ? N14 C18 1.506(4) . ? C10 C1A 1.511(5) . ? C10 C1C 1.513(5) . ? C10 C1B 1.516(5) . ? C12 C13 1.338(5) . ? C16 C17 1.345(4) . ? C18 C1F 1.507(5) . ? C18 C1D 1.509(6) . ? C18 C1E 1.521(6) . ? C21 C22 1.517(5) . ? C23 C24 1.521(5) . ? C25 C26 1.529(5) . ? C27 C28 1.487(8) . ? O1S C2S 1.202(6) . ? C1S C2S 1.480(8) . ? C2S C3S 1.446(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Pd P1 99.29(8) . . ? C11 Pd P2 170.58(8) . . ? P1 Pd P2 72.29(3) . . ? C11 Pd I1 92.26(7) . . ? P1 Pd I1 167.14(2) . . ? P2 Pd I1 96.57(2) . . ? C21 P1 C23 107.05(16) . . ? C21 P1 C20 109.43(17) . . ? C23 P1 C20 106.29(18) . . ? C21 P1 Pd 115.65(11) . . ? C23 P1 Pd 121.71(12) . . ? C20 P1 Pd 95.17(11) . . ? C25 P2 C27 107.77(19) . . ? C25 P2 C20 108.58(17) . . ? C27 P2 C20 106.2(2) . . ? C25 P2 Pd 124.36(12) . . ? C27 P2 Pd 112.98(15) . . ? C20 P2 Pd 94.82(11) . . ? C11 N11 C12 110.3(2) . . ? C11 N11 C10 129.2(3) . . ? C12 N11 C10 120.4(3) . . ? C11 N12 C13 111.4(2) . . ? C11 N12 C14 124.7(2) . . ? C13 N12 C14 123.9(2) . . ? C15 N13 C16 108.8(2) . . ? C15 N13 C14 125.5(2) . . ? C16 N13 C14 125.7(2) . . ? C15 N14 C17 108.6(3) . . ? C15 N14 C18 127.1(3) . . ? C17 N14 C18 124.3(3) . . ? N11 C10 C1A 111.5(3) . . ? N11 C10 C1C 108.0(3) . . ? C1A C10 C1C 109.0(3) . . ? N11 C10 C1B 107.6(3) . . ? C1A C10 C1B 109.5(3) . . ? C1C C10 C1B 111.3(4) . . ? N11 C11 N12 104.4(2) . . ? N11 C11 Pd 132.0(2) . . ? N12 C11 Pd 123.6(2) . . ? C13 C12 N11 108.0(3) . . ? C12 C13 N12 105.8(3) . . ? N12 C14 N13 111.5(2) . . ? N14 C15 N13 108.5(3) . . ? C17 C16 N13 107.0(3) . . ? C16 C17 N14 107.1(3) . . ? N14 C18 C1F 108.2(3) . . ? N14 C18 C1D 108.9(3) . . ? C1F C18 C1D 111.6(4) . . ? N14 C18 C1E 106.8(3) . . ? C1F C18 C1E 110.5(4) . . ? C1D C18 C1E 110.8(4) . . ? P1 C20 P2 94.71(15) . . ? C22 C21 P1 114.5(3) . . ? C24 C23 P1 114.7(2) . . ? C26 C25 P2 113.5(2) . . ? C28 C27 P2 113.3(4) . . ? O1S C2S C3S 123.2(6) . . ? O1S C2S C1S 121.4(5) . . ? C3S C2S C1S 115.4(6) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Pd P1 C21 -73.17(15) . . . . ? P2 Pd P1 C21 102.48(13) . . . . ? I1 Pd P1 C21 133.23(15) . . . . ? C11 Pd P1 C23 59.61(16) . . . . ? P2 Pd P1 C23 -124.75(15) . . . . ? I1 Pd P1 C23 -94.00(18) . . . . ? C11 Pd P1 C20 172.38(16) . . . . ? P2 Pd P1 C20 -11.98(14) . . . . ? I1 Pd P1 C20 18.77(19) . . . . ? C11 Pd P2 C25 155.6(5) . . . . ? P1 Pd P2 C25 128.39(16) . . . . ? I1 Pd P2 C25 -45.03(16) . . . . ? C11 Pd P2 C27 -70.6(5) . . . . ? P1 Pd P2 C27 -97.87(18) . . . . ? I1 Pd P2 C27 88.71(18) . . . . ? C11 Pd P2 C20 39.2(5) . . . . ? P1 Pd P2 C20 11.97(13) . . . . ? I1 Pd P2 C20 -161.45(13) . . . . ? C11 N11 C10 C1A -11.6(5) . . . . ? C12 N11 C10 C1A 170.6(3) . . . . ? C11 N11 C10 C1C -131.4(4) . . . . ? C12 N11 C10 C1C 50.9(4) . . . . ? C11 N11 C10 C1B 108.4(4) . . . . ? C12 N11 C10 C1B -69.3(4) . . . . ? C12 N11 C11 N12 -1.0(3) . . . . ? C10 N11 C11 N12 -178.9(3) . . . . ? C12 N11 C11 Pd 178.6(2) . . . . ? C10 N11 C11 Pd 0.7(5) . . . . ? C13 N12 C11 N11 0.2(3) . . . . ? C14 N12 C11 N11 178.7(2) . . . . ? C13 N12 C11 Pd -179.5(2) . . . . ? C14 N12 C11 Pd -0.9(4) . . . . ? P1 Pd C11 N11 99.7(3) . . . . ? P2 Pd C11 N11 73.4(6) . . . . ? I1 Pd C11 N11 -86.0(3) . . . . ? P1 Pd C11 N12 -80.8(2) . . . . ? P2 Pd C11 N12 -107.0(5) . . . . ? I1 Pd C11 N12 93.5(2) . . . . ? C11 N11 C12 C13 1.5(4) . . . . ? C10 N11 C12 C13 179.6(3) . . . . ? N11 C12 C13 N12 -1.3(4) . . . . ? C11 N12 C13 C12 0.7(4) . . . . ? C14 N12 C13 C12 -177.8(3) . . . . ? C11 N12 C14 N13 -100.3(3) . . . . ? C13 N12 C14 N13 78.0(3) . . . . ? C15 N13 C14 N12 106.7(3) . . . . ? C16 N13 C14 N12 -74.8(3) . . . . ? C17 N14 C15 N13 0.6(3) . . . . ? C18 N14 C15 N13 -177.8(3) . . . . ? C16 N13 C15 N14 -0.2(3) . . . . ? C14 N13 C15 N14 178.5(2) . . . . ? C15 N13 C16 C17 -0.4(4) . . . . ? C14 N13 C16 C17 -179.1(3) . . . . ? N13 C16 C17 N14 0.7(4) . . . . ? C15 N14 C17 C16 -0.8(4) . . . . ? C18 N14 C17 C16 177.6(3) . . . . ? C15 N14 C18 C1F -112.7(4) . . . . ? C17 N14 C18 C1F 69.2(4) . . . . ? C15 N14 C18 C1D 8.7(5) . . . . ? C17 N14 C18 C1D -169.5(4) . . . . ? C15 N14 C18 C1E 128.4(4) . . . . ? C17 N14 C18 C1E -49.8(5) . . . . ? C21 P1 C20 P2 -105.17(18) . . . . ? C23 P1 C20 P2 139.55(17) . . . . ? Pd P1 C20 P2 14.36(16) . . . . ? C25 P2 C20 P1 -143.03(16) . . . . ? C27 P2 C20 P1 101.3(2) . . . . ? Pd P2 C20 P1 -14.28(16) . . . . ? C23 P1 C21 C22 53.3(3) . . . . ? C20 P1 C21 C22 -61.4(3) . . . . ? Pd P1 C21 C22 -167.4(3) . . . . ? C21 P1 C23 C24 56.5(3) . . . . ? C20 P1 C23 C24 173.4(3) . . . . ? Pd P1 C23 C24 -79.7(3) . . . . ? C27 P2 C25 C26 60.1(3) . . . . ? C20 P2 C25 C26 -54.5(3) . . . . ? Pd P2 C25 C26 -164.2(2) . . . . ? C25 P2 C27 C28 70.5(4) . . . . ? C20 P2 C27 C28 -173.3(4) . . . . ? Pd P2 C27 C28 -70.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.290 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.096 #===END data_17b _database_code_depnum_ccdc_archive 'CCDC 726827' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H51 I3 N4 P Pd Rh' _chemical_formula_sum 'C29 H51 I3 N4 P Pd Rh' _chemical_formula_weight 1076.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 15.4844(14) _cell_length_b 11.9963(11) _cell_length_c 40.421(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7508.3(12) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9802 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 27.51 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.41 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.905 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4144 _exptl_absorpt_coefficient_mu 3.451 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.2403 _exptl_absorpt_correction_T_max 0.5786 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 59218 _diffrn_reflns_av_R_equivalents 0.0256 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -52 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.01 _diffrn_reflns_theta_max 27.52 _reflns_number_total 8629 _reflns_number_gt 8116 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR-97 (Altomare et al, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0143P)^2^+16.7787P] 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 8629 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0271 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0560 _refine_ls_wR_factor_gt 0.0550 _refine_ls_goodness_of_fit_ref 1.208 _refine_ls_restrained_S_all 1.208 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.583431(14) 0.053041(18) 0.554088(5) 0.03044(5) Uani 1 1 d . . . I2 I 0.434286(18) 0.39588(2) 0.607903(6) 0.04023(7) Uani 1 1 d . . . I3 I 0.584461(13) -0.161590(19) 0.699935(5) 0.02997(5) Uani 1 1 d . . . Pd Pd 0.511787(13) 0.235050(17) 0.576525(5) 0.01682(5) Uani 1 1 d . . . Rh Rh 0.427332(14) -0.156408(18) 0.671519(6) 0.01922(5) Uani 1 1 d . . . P P 0.42538(5) 0.24212(7) 0.529779(19) 0.02227(15) Uani 1 1 d . . . N11 N 0.66646(16) 0.2627(2) 0.62580(6) 0.0227(5) Uani 1 1 d . . . N12 N 0.56605(16) 0.1541(2) 0.64316(6) 0.0203(5) Uani 1 1 d . . . N13 N 0.44689(16) 0.0908(2) 0.67551(6) 0.0202(5) Uani 1 1 d . . . N14 N 0.38325(18) 0.0404(2) 0.72019(6) 0.0264(6) Uani 1 1 d . . . C1A C 0.7325(3) 0.4472(3) 0.62721(10) 0.0440(9) Uani 1 1 d . . . H1AA H 0.6762 0.4843 0.6290 0.053 Uiso 1 1 calc R . . H1AB H 0.7737 0.4974 0.6164 0.053 Uiso 1 1 calc R . . H1AC H 0.7535 0.4282 0.6494 0.053 Uiso 1 1 calc R . . C1B C 0.6851(3) 0.3686(4) 0.57333(9) 0.0467(11) Uani 1 1 d . . . H1BA H 0.6803 0.3002 0.5602 0.056 Uiso 1 1 calc R . . H1BB H 0.7227 0.4217 0.5618 0.056 Uiso 1 1 calc R . . H1BC H 0.6277 0.4015 0.5762 0.056 Uiso 1 1 calc R . . C1C C 0.8099(2) 0.2839(4) 0.60200(11) 0.0466(10) Uani 1 1 d . . . H1CA H 0.8022 0.2176 0.5881 0.056 Uiso 1 1 calc R . . H1CB H 0.8331 0.2617 0.6236 0.056 Uiso 1 1 calc R . . H1CC H 0.8502 0.3353 0.5912 0.056 Uiso 1 1 calc R . . C1D C 0.2766(3) 0.0396(4) 0.76507(12) 0.0579(12) Uani 1 1 d . . . H1DA H 0.2288 0.0429 0.7492 0.070 Uiso 1 1 calc R . . H1DB H 0.2952 0.1155 0.7705 0.070 Uiso 1 1 calc R . . H1DC H 0.2574 0.0016 0.7852 0.070 Uiso 1 1 calc R . . C1E C 0.3225(4) -0.1396(4) 0.74049(11) 0.0643(15) Uani 1 1 d . . . H1EA H 0.2749 -0.1346 0.7246 0.077 Uiso 1 1 calc R . . H1EB H 0.3029 -0.1793 0.7603 0.077 Uiso 1 1 calc R . . H1EC H 0.3708 -0.1802 0.7304 0.077 Uiso 1 1 calc R . . C1F C 0.4259(3) -0.0296(5) 0.77460(11) 0.0634(13) Uani 1 1 d . . . H1FA H 0.4740 -0.0714 0.7649 0.076 Uiso 1 1 calc R . . H1FB H 0.4063 -0.0670 0.7948 0.076 Uiso 1 1 calc R . . H1FC H 0.4450 0.0461 0.7800 0.076 Uiso 1 1 calc R . . C10 C 0.7230(2) 0.3414(3) 0.60680(8) 0.0273(7) Uani 1 1 d . . . C11 C 0.58849(18) 0.2208(2) 0.61748(7) 0.0196(5) Uani 1 1 d . . . C12 C 0.6916(2) 0.2223(3) 0.65679(8) 0.0265(6) Uani 1 1 d . . . H12 H 0.7435 0.2402 0.6682 0.032 Uiso 1 1 calc R . . C13 C 0.6295(2) 0.1541(3) 0.66752(7) 0.0252(6) Uani 1 1 d . . . H13 H 0.6288 0.1137 0.6877 0.030 Uiso 1 1 calc R . . C14 C 0.4884(2) 0.0867(3) 0.64333(7) 0.0231(6) Uani 1 1 d . . . H14A H 0.5032 0.0086 0.6379 0.028 Uiso 1 1 calc R . . H14B H 0.4479 0.1145 0.6262 0.028 Uiso 1 1 calc R . . C15 C 0.41569(18) -0.0011(3) 0.69134(7) 0.0220(6) Uani 1 1 d . . . C16 C 0.4354(2) 0.1870(3) 0.69396(8) 0.0273(6) Uani 1 1 d . . . H16 H 0.4518 0.2605 0.6880 0.033 Uiso 1 1 calc R . . C17 C 0.3962(2) 0.1550(3) 0.72199(9) 0.0320(7) Uani 1 1 d . . . H17 H 0.3803 0.2021 0.7399 0.038 Uiso 1 1 calc R . . C18 C 0.3516(3) -0.0240(3) 0.74989(8) 0.0357(8) Uani 1 1 d . . . C21 C 0.2969(2) -0.1685(3) 0.65460(9) 0.0304(7) Uani 1 1 d . . . H21 H 0.2554 -0.1211 0.6673 0.036 Uiso 1 1 calc R . . C22 C 0.3449(2) -0.1104(3) 0.63136(8) 0.0292(7) Uani 1 1 d . . . H22 H 0.3315 -0.0290 0.6301 0.035 Uiso 1 1 calc R . . C23 C 0.3808(3) -0.1597(3) 0.59957(9) 0.0397(9) Uani 1 1 d . . . H23A H 0.4248 -0.1080 0.5906 0.048 Uiso 1 1 calc R . . H23B H 0.3335 -0.1646 0.5832 0.048 Uiso 1 1 calc R . . C24 C 0.4216(3) -0.2746(3) 0.60316(9) 0.0419(9) Uani 1 1 d . . . H24A H 0.3769 -0.3322 0.5995 0.050 Uiso 1 1 calc R . . H24B H 0.4665 -0.2840 0.5859 0.050 Uiso 1 1 calc R . . C25 C 0.4622(2) -0.2922(3) 0.63703(9) 0.0320(7) Uani 1 1 d . . . H25 H 0.5256 -0.3082 0.6362 0.038 Uiso 1 1 calc R . . C26 C 0.4215(2) -0.3373(3) 0.66387(9) 0.0306(7) Uani 1 1 d . . . H26 H 0.4606 -0.3807 0.6788 0.037 Uiso 1 1 calc R . . C27 C 0.3276(3) -0.3726(3) 0.66564(10) 0.0402(9) Uani 1 1 d . . . H27A H 0.3209 -0.4454 0.6544 0.048 Uiso 1 1 calc R . . H27B H 0.3112 -0.3828 0.6891 0.048 Uiso 1 1 calc R . . C28 C 0.2670(2) -0.2891(3) 0.64991(11) 0.0403(9) Uani 1 1 d . . . H28A H 0.2088 -0.2978 0.6597 0.048 Uiso 1 1 calc R . . H28B H 0.2625 -0.3051 0.6259 0.048 Uiso 1 1 calc R . . C31 C 0.3529(2) 0.1230(3) 0.52634(8) 0.0304(7) Uani 1 1 d . . . H31A H 0.3172 0.1314 0.5062 0.037 Uiso 1 1 calc R . . H31B H 0.3876 0.0542 0.5239 0.037 Uiso 1 1 calc R . . C32 C 0.2940(3) 0.1114(3) 0.55610(10) 0.0432(9) Uani 1 1 d . . . H32A H 0.2552 0.0478 0.5528 0.052 Uiso 1 1 calc R . . H32B H 0.2598 0.1796 0.5587 0.052 Uiso 1 1 calc R . . H32C H 0.3289 0.0993 0.5760 0.052 Uiso 1 1 calc R . . C33 C 0.4868(2) 0.2398(3) 0.49107(8) 0.0330(7) Uani 1 1 d . . . H33A H 0.5176 0.1678 0.4893 0.040 Uiso 1 1 calc R . . H33B H 0.4462 0.2452 0.4722 0.040 Uiso 1 1 calc R . . C34 C 0.5521(3) 0.3348(4) 0.48886(10) 0.0570(12) Uani 1 1 d . . . H34A H 0.5825 0.3307 0.4676 0.068 Uiso 1 1 calc R . . H34B H 0.5938 0.3282 0.5070 0.068 Uiso 1 1 calc R . . H34C H 0.5218 0.4063 0.4905 0.068 Uiso 1 1 calc R . . C35 C 0.3544(2) 0.3634(3) 0.52591(9) 0.0364(8) Uani 1 1 d . . . H35A H 0.3138 0.3631 0.5448 0.044 Uiso 1 1 calc R . . H35B H 0.3902 0.4314 0.5278 0.044 Uiso 1 1 calc R . . C36 C 0.3017(4) 0.3714(5) 0.49411(13) 0.0792(19) Uani 1 1 d . . . H36A H 0.2647 0.4376 0.4950 0.095 Uiso 1 1 calc R . . H36B H 0.2657 0.3047 0.4918 0.095 Uiso 1 1 calc R . . H36C H 0.3408 0.3770 0.4751 0.095 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I1 0.03508(11) 0.02701(10) 0.02922(11) -0.00420(8) 0.00090(9) 0.01247(8) I2 0.05486(15) 0.03249(12) 0.03333(12) -0.01135(9) -0.00228(10) 0.01882(11) I3 0.02452(10) 0.03465(11) 0.03075(11) 0.00719(9) -0.00514(8) -0.00039(8) Pd 0.01810(10) 0.01657(10) 0.01580(10) -0.00032(8) -0.00077(8) 0.00044(8) Rh 0.01971(11) 0.01859(10) 0.01937(11) -0.00051(8) 0.00116(8) -0.00181(8) P 0.0245(4) 0.0224(4) 0.0199(4) -0.0002(3) -0.0045(3) 0.0015(3) N11 0.0217(12) 0.0263(12) 0.0201(12) 0.0036(10) -0.0026(10) -0.0054(10) N12 0.0214(12) 0.0225(12) 0.0172(11) 0.0008(9) -0.0015(9) -0.0034(10) N13 0.0214(12) 0.0191(11) 0.0201(12) -0.0023(9) -0.0003(10) -0.0031(9) N14 0.0310(14) 0.0267(13) 0.0216(13) -0.0045(10) 0.0065(11) -0.0078(11) C1A 0.058(3) 0.0313(18) 0.043(2) 0.0004(16) 0.0023(19) -0.0155(18) C1B 0.044(2) 0.063(3) 0.0326(19) 0.0218(18) -0.0101(16) -0.030(2) C1C 0.034(2) 0.050(2) 0.055(2) 0.016(2) 0.0137(18) -0.0028(17) C1D 0.058(3) 0.065(3) 0.052(3) 0.000(2) 0.033(2) -0.005(2) C1E 0.108(4) 0.045(2) 0.040(2) -0.0083(19) 0.035(3) -0.036(3) C1F 0.071(3) 0.079(4) 0.040(2) 0.018(2) 0.003(2) -0.010(3) C10 0.0255(15) 0.0311(16) 0.0251(15) 0.0064(13) -0.0010(12) -0.0109(13) C11 0.0201(13) 0.0190(13) 0.0197(13) -0.0006(11) -0.0002(11) -0.0018(11) C12 0.0251(15) 0.0319(16) 0.0227(15) 0.0045(13) -0.0074(12) -0.0038(13) C13 0.0262(15) 0.0304(16) 0.0190(14) 0.0042(12) -0.0053(12) -0.0019(13) C14 0.0257(15) 0.0255(14) 0.0182(13) 0.0004(11) 0.0012(11) -0.0081(12) C15 0.0186(13) 0.0242(14) 0.0232(14) -0.0018(12) -0.0011(11) -0.0034(11) C16 0.0322(16) 0.0200(14) 0.0297(16) -0.0033(12) 0.0015(13) -0.0036(12) C17 0.0379(18) 0.0266(16) 0.0316(17) -0.0110(13) 0.0053(14) -0.0054(14) C18 0.049(2) 0.0356(18) 0.0223(15) -0.0012(14) 0.0138(15) -0.0127(16) C21 0.0193(14) 0.0303(16) 0.0415(19) -0.0075(14) -0.0029(13) -0.0012(12) C22 0.0389(18) 0.0248(15) 0.0238(15) -0.0015(12) -0.0112(13) -0.0103(13) C23 0.053(2) 0.041(2) 0.0253(17) 0.0000(15) -0.0050(16) -0.0152(18) C24 0.048(2) 0.047(2) 0.0309(18) -0.0123(16) 0.0067(16) -0.0075(18) C25 0.0309(17) 0.0302(17) 0.0349(18) -0.0136(14) 0.0035(14) 0.0011(14) C26 0.0404(19) 0.0188(14) 0.0324(17) -0.0065(13) -0.0021(14) 0.0028(13) C27 0.046(2) 0.0253(16) 0.049(2) -0.0043(15) 0.0105(18) -0.0115(15) C28 0.0288(18) 0.0376(19) 0.054(2) -0.0070(17) 0.0051(16) -0.0123(15) C31 0.0303(16) 0.0294(16) 0.0316(17) -0.0089(13) -0.0047(14) -0.0039(13) C32 0.039(2) 0.043(2) 0.048(2) -0.0051(18) 0.0051(17) -0.0139(17) C33 0.0395(19) 0.0413(19) 0.0181(14) 0.0003(13) -0.0019(13) -0.0037(15) C34 0.067(3) 0.072(3) 0.031(2) 0.004(2) 0.009(2) -0.031(3) C35 0.0395(19) 0.0323(18) 0.0374(19) 0.0005(15) -0.0143(16) 0.0132(15) C36 0.099(4) 0.076(3) 0.063(3) -0.011(3) -0.049(3) 0.044(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Pd 2.6116(3) . ? I2 Pd 2.6022(3) . ? I3 Rh 2.6913(4) . ? Pd C11 2.045(3) . ? Pd P 2.3168(8) . ? Rh C15 2.037(3) . ? Rh C21 2.137(3) . ? Rh C22 2.137(3) . ? Rh C26 2.194(3) . ? Rh C25 2.211(3) . ? P C31 1.822(3) . ? P C35 1.830(3) . ? P C33 1.831(3) . ? N11 C11 1.350(4) . ? N11 C12 1.398(4) . ? N11 C10 1.500(4) . ? N12 C11 1.356(4) . ? N12 C13 1.391(4) . ? N12 C14 1.450(4) . ? N13 C15 1.363(4) . ? N13 C16 1.386(4) . ? N13 C14 1.452(4) . ? N14 C15 1.364(4) . ? N14 C17 1.391(4) . ? N14 C18 1.509(4) . ? C1A C10 1.521(5) . ? C1B C10 1.511(5) . ? C1C C10 1.524(5) . ? C1D C18 1.520(6) . ? C1E C18 1.507(5) . ? C1F C18 1.524(6) . ? C12 C13 1.336(4) . ? C16 C17 1.341(5) . ? C21 C22 1.386(5) . ? C21 C28 1.530(5) . ? C22 C23 1.520(5) . ? C23 C24 1.523(6) . ? C24 C25 1.521(5) . ? C25 C26 1.367(5) . ? C26 C27 1.516(5) . ? C27 C28 1.513(6) . ? C31 C32 1.516(5) . ? C33 C34 1.526(5) . ? C35 C36 1.525(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 C11 Pd P 177.28(8) . . ? C11 Pd I2 86.29(8) . . ? P Pd I2 95.97(2) . . ? C11 Pd I1 87.97(8) . . ? P Pd I1 89.58(2) . . ? I2 Pd I1 170.078(12) . . ? C15 Rh C21 96.00(12) . . ? C15 Rh C22 90.55(12) . . ? C21 Rh C22 37.85(13) . . ? C15 Rh C26 163.14(13) . . ? C21 Rh C26 81.30(13) . . ? C22 Rh C26 97.12(13) . . ? C15 Rh C25 160.70(13) . . ? C21 Rh C25 88.80(13) . . ? C22 Rh C25 81.80(13) . . ? C26 Rh C25 36.15(13) . . ? C15 Rh I3 86.17(8) . . ? C21 Rh I3 171.62(10) . . ? C22 Rh I3 150.44(9) . . ? C26 Rh I3 94.27(9) . . ? C25 Rh I3 91.78(9) . . ? C31 P C35 104.27(17) . . ? C31 P C33 104.05(16) . . ? C35 P C33 104.53(18) . . ? C31 P Pd 112.91(12) . . ? C35 P Pd 116.48(12) . . ? C33 P Pd 113.36(12) . . ? C11 N11 C12 110.1(2) . . ? C11 N11 C10 129.0(2) . . ? C12 N11 C10 120.9(2) . . ? C11 N12 C13 111.2(2) . . ? C11 N12 C14 123.0(2) . . ? C13 N12 C14 125.6(2) . . ? C15 N13 C16 112.0(2) . . ? C15 N13 C14 123.4(2) . . ? C16 N13 C14 124.6(3) . . ? C15 N14 C17 110.6(3) . . ? C15 N14 C18 127.8(3) . . ? C17 N14 C18 120.7(3) . . ? N11 C10 C1B 111.6(3) . . ? N11 C10 C1A 107.7(3) . . ? C1B C10 C1A 110.1(3) . . ? N11 C10 C1C 107.2(3) . . ? C1B C10 C1C 109.1(3) . . ? C1A C10 C1C 111.2(3) . . ? N11 C11 N12 105.0(2) . . ? N11 C11 Pd 133.6(2) . . ? N12 C11 Pd 121.4(2) . . ? C13 C12 N11 107.6(3) . . ? C12 C13 N12 106.2(3) . . ? N12 C14 N13 110.6(2) . . ? N13 C15 N14 103.7(3) . . ? N13 C15 Rh 121.6(2) . . ? N14 C15 Rh 134.6(2) . . ? C17 C16 N13 105.9(3) . . ? C16 C17 N14 107.7(3) . . ? C1E C18 N14 111.6(3) . . ? C1E C18 C1D 109.6(4) . . ? N14 C18 C1D 108.2(3) . . ? C1E C18 C1F 110.5(4) . . ? N14 C18 C1F 107.4(3) . . ? C1D C18 C1F 109.5(4) . . ? C22 C21 C28 123.6(3) . . ? C22 C21 Rh 71.10(18) . . ? C28 C21 Rh 113.0(2) . . ? C21 C22 C23 125.0(3) . . ? C21 C22 Rh 71.05(19) . . ? C23 C22 Rh 108.9(2) . . ? C22 C23 C24 115.0(3) . . ? C25 C24 C23 112.5(3) . . ? C26 C25 C24 125.4(3) . . ? C26 C25 Rh 71.23(19) . . ? C24 C25 Rh 111.4(2) . . ? C25 C26 C27 126.2(3) . . ? C25 C26 Rh 72.62(19) . . ? C27 C26 Rh 108.0(2) . . ? C28 C27 C26 112.9(3) . . ? C27 C28 C21 112.7(3) . . ? C32 C31 P 112.5(2) . . ? C34 C33 P 112.5(3) . . ? C36 C35 P 116.3(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Pd P C31 37.2(18) . . . . ? I2 Pd P C31 -108.72(12) . . . . ? I1 Pd P C31 63.05(12) . . . . ? C11 Pd P C35 157.8(17) . . . . ? I2 Pd P C35 11.91(15) . . . . ? I1 Pd P C35 -176.33(15) . . . . ? C11 Pd P C33 -80.8(17) . . . . ? I2 Pd P C33 133.28(13) . . . . ? I1 Pd P C33 -54.96(13) . . . . ? C11 N11 C10 C1B -3.5(5) . . . . ? C12 N11 C10 C1B 176.8(3) . . . . ? C11 N11 C10 C1A 117.3(3) . . . . ? C12 N11 C10 C1A -62.3(4) . . . . ? C11 N11 C10 C1C -122.9(3) . . . . ? C12 N11 C10 C1C 57.5(4) . . . . ? C12 N11 C11 N12 -0.5(3) . . . . ? C10 N11 C11 N12 179.8(3) . . . . ? C12 N11 C11 Pd -177.5(2) . . . . ? C10 N11 C11 Pd 2.8(5) . . . . ? C13 N12 C11 N11 0.1(3) . . . . ? C14 N12 C11 N11 -176.0(3) . . . . ? C13 N12 C11 Pd 177.5(2) . . . . ? C14 N12 C11 Pd 1.5(4) . . . . ? P Pd C11 N11 119.2(16) . . . . ? I2 Pd C11 N11 -94.8(3) . . . . ? I1 Pd C11 N11 93.3(3) . . . . ? P Pd C11 N12 -57.4(19) . . . . ? I2 Pd C11 N12 88.7(2) . . . . ? I1 Pd C11 N12 -83.3(2) . . . . ? C11 N11 C12 C13 0.8(4) . . . . ? C10 N11 C12 C13 -179.5(3) . . . . ? N11 C12 C13 N12 -0.7(4) . . . . ? C11 N12 C13 C12 0.4(4) . . . . ? C14 N12 C13 C12 176.3(3) . . . . ? C11 N12 C14 N13 -138.5(3) . . . . ? C13 N12 C14 N13 46.1(4) . . . . ? C15 N13 C14 N12 -135.1(3) . . . . ? C16 N13 C14 N12 43.9(4) . . . . ? C16 N13 C15 N14 0.7(3) . . . . ? C14 N13 C15 N14 179.8(3) . . . . ? C16 N13 C15 Rh -177.4(2) . . . . ? C14 N13 C15 Rh 1.7(4) . . . . ? C17 N14 C15 N13 -1.2(3) . . . . ? C18 N14 C15 N13 -170.5(3) . . . . ? C17 N14 C15 Rh 176.6(3) . . . . ? C18 N14 C15 Rh 7.2(5) . . . . ? C21 Rh C15 N13 -102.6(2) . . . . ? C22 Rh C15 N13 -65.1(2) . . . . ? C26 Rh C15 N13 177.6(4) . . . . ? C25 Rh C15 N13 1.1(5) . . . . ? I3 Rh C15 N13 85.5(2) . . . . ? C21 Rh C15 N14 80.0(3) . . . . ? C22 Rh C15 N14 117.5(3) . . . . ? C26 Rh C15 N14 0.2(6) . . . . ? C25 Rh C15 N14 -176.3(3) . . . . ? I3 Rh C15 N14 -91.9(3) . . . . ? C15 N13 C16 C17 0.1(4) . . . . ? C14 N13 C16 C17 -179.0(3) . . . . ? N13 C16 C17 N14 -0.8(4) . . . . ? C15 N14 C17 C16 1.3(4) . . . . ? C18 N14 C17 C16 171.5(3) . . . . ? C15 N14 C18 C1E -24.9(5) . . . . ? C17 N14 C18 C1E 166.7(4) . . . . ? C15 N14 C18 C1D -145.5(4) . . . . ? C17 N14 C18 C1D 46.1(4) . . . . ? C15 N14 C18 C1F 96.4(4) . . . . ? C17 N14 C18 C1F -72.0(4) . . . . ? C15 Rh C21 C22 83.1(2) . . . . ? C26 Rh C21 C22 -113.7(2) . . . . ? C25 Rh C21 C22 -78.1(2) . . . . ? I3 Rh C21 C22 -172.2(5) . . . . ? C15 Rh C21 C28 -157.5(3) . . . . ? C22 Rh C21 C28 119.4(3) . . . . ? C26 Rh C21 C28 5.7(3) . . . . ? C25 Rh C21 C28 41.3(3) . . . . ? I3 Rh C21 C28 -52.8(8) . . . . ? C28 C21 C22 C23 -5.3(5) . . . . ? Rh C21 C22 C23 100.2(3) . . . . ? C28 C21 C22 Rh -105.5(3) . . . . ? C15 Rh C22 C21 -99.1(2) . . . . ? C26 Rh C22 C21 65.8(2) . . . . ? C25 Rh C22 C21 98.7(2) . . . . ? I3 Rh C22 C21 177.70(15) . . . . ? C15 Rh C22 C23 139.4(2) . . . . ? C21 Rh C22 C23 -121.5(3) . . . . ? C26 Rh C22 C23 -55.7(2) . . . . ? C25 Rh C22 C23 -22.9(2) . . . . ? I3 Rh C22 C23 56.2(3) . . . . ? C21 C22 C23 C24 -43.3(5) . . . . ? Rh C22 C23 C24 36.3(4) . . . . ? C22 C23 C24 C25 -31.0(5) . . . . ? C23 C24 C25 C26 91.6(4) . . . . ? C23 C24 C25 Rh 10.0(4) . . . . ? C15 Rh C25 C26 178.3(3) . . . . ? C21 Rh C25 C26 -76.8(2) . . . . ? C22 Rh C25 C26 -114.2(2) . . . . ? I3 Rh C25 C26 94.8(2) . . . . ? C15 Rh C25 C24 -60.1(5) . . . . ? C21 Rh C25 C24 44.7(3) . . . . ? C22 Rh C25 C24 7.4(2) . . . . ? C26 Rh C25 C24 121.6(3) . . . . ? I3 Rh C25 C24 -143.7(2) . . . . ? C24 C25 C26 C27 -3.4(5) . . . . ? Rh C25 C26 C27 99.9(3) . . . . ? C24 C25 C26 Rh -103.3(3) . . . . ? C15 Rh C26 C25 -178.1(4) . . . . ? C21 Rh C26 C25 100.0(2) . . . . ? C22 Rh C26 C25 65.5(2) . . . . ? I3 Rh C26 C25 -87.2(2) . . . . ? C15 Rh C26 C27 58.6(5) . . . . ? C21 Rh C26 C27 -23.3(3) . . . . ? C22 Rh C26 C27 -57.8(3) . . . . ? C25 Rh C26 C27 -123.3(3) . . . . ? I3 Rh C26 C27 149.5(2) . . . . ? C25 C26 C27 C28 -43.4(5) . . . . ? Rh C26 C27 C28 37.9(4) . . . . ? C26 C27 C28 C21 -34.6(5) . . . . ? C22 C21 C28 C27 95.4(4) . . . . ? Rh C21 C28 C27 13.4(4) . . . . ? C35 P C31 C32 -69.4(3) . . . . ? C33 P C31 C32 -178.7(3) . . . . ? Pd P C31 C32 57.9(3) . . . . ? C31 P C33 C34 179.8(3) . . . . ? C35 P C33 C34 70.7(3) . . . . ? Pd P C33 C34 -57.2(3) . . . . ? C31 P C35 C36 -58.5(4) . . . . ? C33 P C35 C36 50.4(4) . . . . ? Pd P C35 C36 176.3(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.924 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.096 #===END