Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Trans.' _publ_requested_coeditor_name ? _publ_contact_letter ; Oviedo 30/06/2006 Please receive the CIF for compounds 4,5b,7 and 9 submitted to be published in Dalton Trans. Thank you very much. J. Diez. ; _publ_contact_author_name 'Victorio Cadierno' _publ_contact_author_address ; Departamento de Qu\'imica Organica e Inorganica Universidad de Oviedo Facultad de Qu\'imica Julian Claveria s/n Oviedo 33071 SPAIN ; _publ_contact_author_email VCM@UNIOVI.ES _publ_section_title ; Synthesis and reactivity studies of palladium(II) complexes containing the N-phosphorylated iminophosphorane-phosphine ligands Ph2PCH2P{=NP(=O)(OR)2}Ph2 (R = Et, Ph): Application to the catalytic synthesis of 2,3-dimethylfuran. ; # The loop structure below should contain the names and addresses of all #authors, in the required order of publication. Repeat as necessary. loop_ _publ_author_name _publ_author_address 'Victorio Cadierno' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; 'Josefina Diez' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; 'Joaquin Garcia-Alvarez' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; 'Jose Gimeno' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; 'Noel Nebra' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; 'Javier Rubio-Garcia' ; Departamento de Quimica Organica e Inorganica Facultad de Quimica Universidad de Oviedo Avda. Julian Claveria, 8 33006 Oviedo Spain ; #=============================================================================== data_4 _database_code_depnum_ccdc_archive 'CCDC 613046' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H32 Cl2 N O3 P3 Pd' _chemical_formula_sum 'C37 H32 Cl2 N O3 P3 Pd' _chemical_formula_weight 808.85 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.6582(2) _cell_length_b 15.0716(4) _cell_length_c 21.1627(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3399.49(13) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5148 _cell_measurement_theta_min 3.597 _cell_measurement_theta_max 70.243 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_min 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_max 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.580 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1640 _exptl_absorpt_coefficient_mu 7.501 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.492462 _exptl_absorpt_correction_T_max 1 _exptl_absorpt_process_details 'SADABS (Sheldrick,G.M.,1997-2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14111 _diffrn_reflns_av_R_equivalents 0.0497 _diffrn_reflns_av_sigmaI/netI 0.0549 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 70.37 _reflns_number_total 5932 _reflns_number_gt 5438 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^)+(0.0572P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.022(8) _refine_ls_number_reflns 5932 _refine_ls_number_parameters 424 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0419 _refine_ls_R_factor_gt 0.0375 _refine_ls_wR_factor_ref 0.0936 _refine_ls_wR_factor_gt 0.0914 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.996 _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 Pd1 Pd 0.69683(3) 0.23057(2) 0.800637(15) 0.01793(9) Uani 1 1 d . . . Cl1 Cl 0.79776(12) 0.25417(8) 0.89465(5) 0.0270(2) Uani 1 1 d . . . Cl2 Cl 0.74846(12) 0.37405(8) 0.76290(5) 0.0271(3) Uani 1 1 d . . . N1 N 0.5992(4) 0.2019(3) 0.71516(16) 0.0188(8) Uani 1 1 d . . . O2 O 0.5048(3) 0.3368(2) 0.65410(16) 0.0268(8) Uani 1 1 d . . . O3 O 0.4317(3) 0.3137(2) 0.75682(16) 0.0253(8) Uani 1 1 d . . . O1 O 0.3684(4) 0.1988(2) 0.67212(17) 0.0290(8) Uani 1 1 d . . . P2 P 0.62563(10) 0.09857(8) 0.69843(6) 0.0174(2) Uani 1 1 d . . . P1 P 0.65757(11) 0.09222(8) 0.83330(5) 0.0175(2) Uani 1 1 d . . . P3 P 0.46928(10) 0.25473(8) 0.69802(6) 0.0216(2) Uani 1 1 d . . . C1 C 0.5749(5) 0.0374(3) 0.7672(2) 0.0206(10) Uani 1 1 d . . . H1A H 0.5991 -0.0258 0.7639 0.025 Uiso 1 1 calc R . . H1B H 0.4828 0.0415 0.7725 0.025 Uiso 1 1 calc R . . C2 C 0.5653(5) 0.3247(4) 0.5954(2) 0.0265(11) Uani 1 1 d . . . C3 C 0.6932(6) 0.3326(4) 0.5931(2) 0.0315(11) Uani 1 1 d . . . H3 H 0.7409 0.3402 0.6306 0.038 Uiso 1 1 calc R . . C4 C 0.7520(6) 0.3289(4) 0.5338(3) 0.0338(12) Uani 1 1 d . . . H4 H 0.8407 0.3342 0.5312 0.041 Uiso 1 1 calc R . . C5 C 0.6839(6) 0.3180(4) 0.4800(2) 0.0340(12) Uani 1 1 d . . . H5 H 0.7248 0.3170 0.4401 0.041 Uiso 1 1 calc R . . C6 C 0.5544(6) 0.3083(4) 0.4836(2) 0.0356(13) Uani 1 1 d . . . H6 H 0.5070 0.3000 0.4460 0.043 Uiso 1 1 calc R . . C7 C 0.4941(5) 0.3106(4) 0.5414(2) 0.0307(12) Uani 1 1 d . . . H7 H 0.4058 0.3028 0.5441 0.037 Uiso 1 1 calc R . . C8 C 0.3549(5) 0.2855(3) 0.8067(2) 0.0269(11) Uani 1 1 d . . . C9 C 0.4049(6) 0.2868(4) 0.8666(3) 0.0372(14) Uani 1 1 d . . . H9 H 0.4917 0.2986 0.8724 0.045 Uiso 1 1 calc R . . C10 C 0.3296(7) 0.2711(5) 0.9183(3) 0.0493(17) Uani 1 1 d . . . H10 H 0.3636 0.2748 0.9597 0.059 Uiso 1 1 calc R . . C11 C 0.2045(8) 0.2499(4) 0.9099(3) 0.058(2) Uani 1 1 d . . . H11 H 0.1524 0.2381 0.9453 0.070 Uiso 1 1 calc R . . C12 C 0.1557(7) 0.2459(5) 0.8491(4) 0.061(2) Uani 1 1 d . . . H12 H 0.0700 0.2306 0.8432 0.073 Uiso 1 1 calc R . . C13 C 0.2306(5) 0.2642(4) 0.7966(3) 0.0399(13) Uani 1 1 d . . . H13 H 0.1970 0.2620 0.7551 0.048 Uiso 1 1 calc R . . C14 C 0.5547(5) 0.0541(3) 0.6288(2) 0.0222(10) Uani 1 1 d . . . C15 C 0.6108(5) 0.0696(4) 0.5706(2) 0.0293(12) Uani 1 1 d . . . H15 H 0.6823 0.1070 0.5681 0.035 Uiso 1 1 calc R . . C16 C 0.5641(6) 0.0313(4) 0.5168(2) 0.0343(13) Uani 1 1 d . . . H16 H 0.6019 0.0438 0.4772 0.041 Uiso 1 1 calc R . . C17 C 0.4631(5) -0.0249(4) 0.5198(3) 0.0326(13) Uani 1 1 d . . . H17 H 0.4325 -0.0525 0.4825 0.039 Uiso 1 1 calc R . . C18 C 0.4059(5) -0.0415(4) 0.5773(3) 0.0323(12) Uani 1 1 d . . . H18 H 0.3358 -0.0803 0.5795 0.039 Uiso 1 1 calc R . . C19 C 0.4512(5) -0.0012(4) 0.6318(2) 0.0278(11) Uani 1 1 d . . . H19 H 0.4110 -0.0116 0.6712 0.033 Uiso 1 1 calc R . . C20 C 0.7911(5) 0.0825(3) 0.68937(18) 0.0200(9) Uani 1 1 d . . . C21 C 0.8370(5) -0.0043(3) 0.6842(2) 0.0220(10) Uani 1 1 d . . . H21 H 0.7801 -0.0529 0.6835 0.026 Uiso 1 1 calc R . . C22 C 0.9648(5) -0.0197(4) 0.6801(2) 0.0280(12) Uani 1 1 d . . . H22 H 0.9955 -0.0788 0.6776 0.034 Uiso 1 1 calc R . . C23 C 1.0477(5) 0.0507(4) 0.6795(2) 0.0320(13) Uani 1 1 d . . . H23 H 1.1353 0.0399 0.6766 0.038 Uiso 1 1 calc R . . C24 C 1.0037(5) 0.1367(4) 0.6832(2) 0.0276(11) Uani 1 1 d . . . H24 H 1.0611 0.1849 0.6824 0.033 Uiso 1 1 calc R . . C25 C 0.8754(5) 0.1532(3) 0.6882(2) 0.0208(10) Uani 1 1 d . . . H25 H 0.8454 0.2125 0.6909 0.025 Uiso 1 1 calc R . . C26 C 0.7937(5) 0.0217(3) 0.84495(19) 0.0208(9) Uani 1 1 d . . . C27 C 0.9165(5) 0.0523(4) 0.8376(2) 0.0228(10) Uani 1 1 d . . . H27 H 0.9323 0.1136 0.8308 0.027 Uiso 1 1 calc R . . C28 C 1.0154(5) -0.0079(4) 0.8405(2) 0.0326(13) Uani 1 1 d . . . H28 H 1.0992 0.0122 0.8353 0.039 Uiso 1 1 calc R . . C29 C 0.9914(5) -0.0972(4) 0.8509(2) 0.0326(13) Uani 1 1 d . . . H29 H 1.0591 -0.1382 0.8520 0.039 Uiso 1 1 calc R . . C30 C 0.8708(6) -0.1272(4) 0.8596(2) 0.0317(12) Uani 1 1 d . . . H30 H 0.8557 -0.1884 0.8673 0.038 Uiso 1 1 calc R . . C31 C 0.7714(5) -0.0680(3) 0.8570(2) 0.0234(11) Uani 1 1 d . . . H31 H 0.6881 -0.0885 0.8635 0.028 Uiso 1 1 calc R . . C32 C 0.5640(5) 0.0743(3) 0.9033(2) 0.0211(10) Uani 1 1 d . . . C33 C 0.6233(6) 0.0793(4) 0.9612(2) 0.0367(14) Uani 1 1 d . . . H33 H 0.7105 0.0920 0.9630 0.044 Uiso 1 1 calc R . . C34 C 0.5578(7) 0.0660(5) 1.0165(3) 0.0429(16) Uani 1 1 d . . . H34 H 0.6002 0.0680 1.0560 0.051 Uiso 1 1 calc R . . C35 C 0.4302(6) 0.0498(4) 1.0144(3) 0.0357(13) Uani 1 1 d . . . H35 H 0.3841 0.0415 1.0524 0.043 Uiso 1 1 calc R . . C36 C 0.3703(6) 0.0459(4) 0.9565(3) 0.0376(14) Uani 1 1 d . . . H36 H 0.2826 0.0349 0.9549 0.045 Uiso 1 1 calc R . . C37 C 0.4358(5) 0.0576(4) 0.9010(3) 0.0312(12) Uani 1 1 d . . . H37 H 0.3937 0.0542 0.8615 0.037 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 Pd1 0.02013(15) 0.01556(17) 0.01812(14) -0.00245(13) 0.00249(13) -0.00254(12) Cl1 0.0296(6) 0.0274(7) 0.0241(5) -0.0076(4) -0.0035(5) -0.0027(5) Cl2 0.0375(6) 0.0182(7) 0.0256(6) -0.0029(4) 0.0074(5) -0.0098(5) N1 0.023(2) 0.020(2) 0.0138(17) 0.0004(14) -0.0014(14) -0.0006(14) O2 0.029(2) 0.028(2) 0.0233(17) 0.0041(14) 0.0013(14) 0.0072(14) O3 0.0260(19) 0.022(2) 0.0279(18) -0.0013(14) 0.0046(14) 0.0007(14) O1 0.029(2) 0.024(2) 0.0344(18) -0.0074(15) -0.0023(15) 0.0032(14) P2 0.0210(6) 0.0152(6) 0.0161(5) -0.0002(5) 0.0009(5) -0.0012(4) P1 0.0197(6) 0.0162(7) 0.0165(5) -0.0011(4) 0.0010(4) -0.0013(4) P3 0.0215(6) 0.0178(7) 0.0255(5) -0.0013(5) 0.0016(5) 0.0031(4) C1 0.024(3) 0.016(3) 0.021(2) 0.0019(19) 0.0016(19) -0.0041(18) C2 0.031(3) 0.027(3) 0.021(2) 0.006(2) 0.000(2) 0.002(2) C3 0.028(3) 0.037(3) 0.029(3) 0.001(2) -0.005(2) 0.008(2) C4 0.036(3) 0.034(4) 0.032(3) 0.003(2) 0.006(2) 0.001(2) C5 0.047(4) 0.031(3) 0.025(2) 0.002(2) 0.007(2) -0.003(3) C6 0.051(4) 0.036(3) 0.020(2) 0.001(2) -0.007(2) 0.001(3) C7 0.034(3) 0.028(3) 0.030(3) 0.004(2) -0.001(2) 0.003(2) C8 0.029(2) 0.023(3) 0.029(2) -0.001(2) 0.006(2) 0.0014(18) C9 0.042(3) 0.038(4) 0.031(3) -0.002(2) 0.003(2) 0.011(3) C10 0.081(6) 0.038(4) 0.029(3) 0.000(3) 0.014(3) 0.011(4) C11 0.094(6) 0.022(4) 0.058(4) -0.002(3) 0.054(4) -0.003(3) C12 0.045(4) 0.049(5) 0.088(5) -0.023(4) 0.030(4) -0.026(3) C13 0.034(3) 0.036(3) 0.049(3) -0.013(3) 0.012(2) -0.008(2) C14 0.024(3) 0.016(3) 0.026(3) 0.0008(19) -0.001(2) 0.0027(18) C15 0.029(3) 0.035(3) 0.024(2) 0.004(2) -0.002(2) -0.006(2) C16 0.036(3) 0.046(4) 0.021(2) 0.003(2) 0.000(2) 0.001(3) C17 0.035(3) 0.036(4) 0.026(3) -0.007(2) -0.012(2) 0.006(2) C18 0.027(3) 0.032(3) 0.038(3) -0.003(2) -0.009(2) -0.009(2) C19 0.029(3) 0.027(3) 0.027(3) 0.001(2) -0.001(2) -0.003(2) C20 0.023(2) 0.026(3) 0.0112(19) 0.0018(16) -0.0022(17) -0.0002(18) C21 0.027(3) 0.022(3) 0.018(2) -0.0015(17) -0.0023(17) 0.0041(17) C22 0.034(3) 0.029(3) 0.021(2) -0.003(2) -0.004(2) 0.013(2) C23 0.026(3) 0.050(4) 0.019(2) 0.003(2) 0.0044(19) 0.015(2) C24 0.025(3) 0.036(3) 0.022(2) 0.003(2) 0.0007(18) -0.001(2) C25 0.026(3) 0.019(3) 0.018(2) 0.0039(17) 0.0037(17) 0.0013(17) C26 0.026(3) 0.022(3) 0.0141(19) -0.0025(17) -0.0006(19) 0.0033(19) C27 0.025(3) 0.027(3) 0.017(2) 0.0017(19) -0.0030(19) -0.0025(19) C28 0.024(3) 0.054(4) 0.020(2) 0.000(2) 0.003(2) 0.003(2) C29 0.032(3) 0.041(4) 0.025(2) -0.002(2) -0.004(2) 0.015(2) C30 0.042(3) 0.026(3) 0.027(3) -0.002(2) -0.003(2) 0.008(2) C31 0.024(3) 0.020(3) 0.026(2) 0.0020(19) -0.0020(19) 0.0003(17) C32 0.028(3) 0.011(3) 0.024(2) -0.0025(18) 0.0056(19) 0.0012(17) C33 0.041(3) 0.048(4) 0.021(2) 0.001(2) 0.004(2) -0.014(3) C34 0.056(4) 0.051(4) 0.021(3) -0.001(3) 0.004(3) -0.013(3) C35 0.050(4) 0.029(3) 0.028(3) 0.000(2) 0.017(3) 0.002(2) C36 0.031(3) 0.039(4) 0.043(3) 0.008(3) 0.011(3) 0.004(2) C37 0.031(3) 0.034(3) 0.028(3) 0.005(2) 0.003(2) 0.008(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 Pd1 N1 2.131(4) . ? Pd1 P1 2.2362(13) . ? Pd1 Cl1 2.2895(11) . ? Pd1 Cl2 2.3700(12) . ? N1 P2 1.621(4) . ? N1 P3 1.638(4) . ? O2 C2 1.412(6) . ? O2 P3 1.593(4) . ? O3 C8 1.402(6) . ? O3 P3 1.581(4) . ? O1 P3 1.473(4) . ? P2 C14 1.786(5) . ? P2 C20 1.790(5) . ? P2 C1 1.805(5) . ? P1 C32 1.805(5) . ? P1 C26 1.815(5) . ? P1 C1 1.848(5) . ? C2 C3 1.370(8) . ? C2 C7 1.388(8) . ? C3 C4 1.403(8) . ? C4 C5 1.361(8) . ? C5 C6 1.391(9) . ? C6 C7 1.382(8) . ? C8 C9 1.374(8) . ? C8 C13 1.380(7) . ? C9 C10 1.377(8) . ? C10 C11 1.382(11) . ? C11 C12 1.389(11) . ? C12 C13 1.396(9) . ? C14 C19 1.384(7) . ? C14 C15 1.389(7) . ? C15 C16 1.369(8) . ? C16 C17 1.371(8) . ? C17 C18 1.383(8) . ? C18 C19 1.390(7) . ? C20 C25 1.394(7) . ? C20 C21 1.401(7) . ? C21 C22 1.384(7) . ? C22 C23 1.381(9) . ? C23 C24 1.381(8) . ? C24 C25 1.394(7) . ? C26 C31 1.396(7) . ? C26 C27 1.397(7) . ? C27 C28 1.392(8) . ? C28 C29 1.389(9) . ? C29 C30 1.374(9) . ? C30 C31 1.387(7) . ? C32 C33 1.382(8) . ? C32 C37 1.390(8) . ? C33 C34 1.377(8) . ? C34 C35 1.383(9) . ? C35 C36 1.383(9) . ? C36 C37 1.377(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 N1 Pd1 P1 88.95(11) . . ? N1 Pd1 Cl1 176.85(11) . . ? P1 Pd1 Cl1 87.95(4) . . ? N1 Pd1 Cl2 90.72(11) . . ? P1 Pd1 Cl2 176.75(5) . . ? Cl1 Pd1 Cl2 92.41(4) . . ? P2 N1 P3 124.5(2) . . ? P2 N1 Pd1 107.2(2) . . ? P3 N1 Pd1 120.1(2) . . ? C2 O2 P3 121.5(3) . . ? C8 O3 P3 124.8(3) . . ? N1 P2 C14 117.8(2) . . ? N1 P2 C20 109.0(2) . . ? C14 P2 C20 106.1(2) . . ? N1 P2 C1 105.2(2) . . ? C14 P2 C1 110.3(2) . . ? C20 P2 C1 108.2(2) . . ? C32 P1 C26 104.0(2) . . ? C32 P1 C1 106.9(2) . . ? C26 P1 C1 102.8(2) . . ? C32 P1 Pd1 119.73(16) . . ? C26 P1 Pd1 116.03(17) . . ? C1 P1 Pd1 105.76(16) . . ? O1 P3 O3 115.4(2) . . ? O1 P3 O2 113.7(2) . . ? O3 P3 O2 94.77(19) . . ? O1 P3 N1 114.9(2) . . ? O3 P3 N1 108.27(19) . . ? O2 P3 N1 107.8(2) . . ? P2 C1 P1 103.9(2) . . ? C3 C2 C7 121.9(5) . . ? C3 C2 O2 118.3(5) . . ? C7 C2 O2 119.7(5) . . ? C2 C3 C4 118.2(5) . . ? C5 C4 C3 121.0(6) . . ? C4 C5 C6 119.7(5) . . ? C7 C6 C5 120.5(5) . . ? C6 C7 C2 118.6(5) . . ? C9 C8 C13 121.2(5) . . ? C9 C8 O3 117.7(5) . . ? C13 C8 O3 120.9(5) . . ? C8 C9 C10 120.3(6) . . ? C9 C10 C11 119.9(6) . . ? C10 C11 C12 119.4(5) . . ? C11 C12 C13 120.9(6) . . ? C8 C13 C12 118.2(6) . . ? C19 C14 C15 118.9(5) . . ? C19 C14 P2 121.7(4) . . ? C15 C14 P2 119.1(4) . . ? C16 C15 C14 120.7(5) . . ? C15 C16 C17 120.5(5) . . ? C16 C17 C18 119.9(5) . . ? C17 C18 C19 119.8(5) . . ? C14 C19 C18 120.2(5) . . ? C25 C20 C21 119.2(5) . . ? C25 C20 P2 122.2(4) . . ? C21 C20 P2 118.6(4) . . ? C22 C21 C20 120.3(5) . . ? C23 C22 C21 120.1(5) . . ? C24 C23 C22 120.2(5) . . ? C23 C24 C25 120.3(5) . . ? C20 C25 C24 119.8(5) . . ? C31 C26 C27 120.0(5) . . ? C31 C26 P1 117.1(4) . . ? C27 C26 P1 122.7(4) . . ? C28 C27 C26 119.3(5) . . ? C29 C28 C27 120.0(5) . . ? C30 C29 C28 120.8(5) . . ? C29 C30 C31 119.8(6) . . ? C30 C31 C26 120.0(5) . . ? C33 C32 C37 119.3(5) . . ? C33 C32 P1 117.9(4) . . ? C37 C32 P1 122.8(4) . . ? C34 C33 C32 121.0(6) . . ? C33 C34 C35 119.7(6) . . ? C34 C35 C36 119.4(5) . . ? C37 C36 C35 121.1(6) . . ? C36 C37 C32 119.5(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 P1 Pd1 N1 P2 -34.22(18) . . . . ? Cl1 Pd1 N1 P2 -44(2) . . . . ? Cl2 Pd1 N1 P2 142.55(18) . . . . ? P1 Pd1 N1 P3 115.6(2) . . . . ? Cl1 Pd1 N1 P3 105(2) . . . . ? Cl2 Pd1 N1 P3 -67.7(2) . . . . ? P3 N1 P2 C14 31.5(4) . . . . ? Pd1 N1 P2 C14 179.6(2) . . . . ? P3 N1 P2 C20 152.4(3) . . . . ? Pd1 N1 P2 C20 -59.5(2) . . . . ? P3 N1 P2 C1 -91.8(3) . . . . ? Pd1 N1 P2 C1 56.3(2) . . . . ? N1 Pd1 P1 C32 -117.8(2) . . . . ? Cl1 Pd1 P1 C32 61.6(2) . . . . ? Cl2 Pd1 P1 C32 158.0(8) . . . . ? N1 Pd1 P1 C26 116.05(19) . . . . ? Cl1 Pd1 P1 C26 -64.50(16) . . . . ? Cl2 Pd1 P1 C26 31.8(9) . . . . ? N1 Pd1 P1 C1 2.8(2) . . . . ? Cl1 Pd1 P1 C1 -177.72(17) . . . . ? Cl2 Pd1 P1 C1 -81.4(8) . . . . ? C8 O3 P3 O1 40.4(4) . . . . ? C8 O3 P3 O2 159.5(4) . . . . ? C8 O3 P3 N1 -90.0(4) . . . . ? C2 O2 P3 O1 -69.2(4) . . . . ? C2 O2 P3 O3 170.4(4) . . . . ? C2 O2 P3 N1 59.4(4) . . . . ? P2 N1 P3 O1 6.9(3) . . . . ? Pd1 N1 P3 O1 -137.4(2) . . . . ? P2 N1 P3 O3 137.6(3) . . . . ? Pd1 N1 P3 O3 -6.7(3) . . . . ? P2 N1 P3 O2 -121.0(3) . . . . ? Pd1 N1 P3 O2 94.7(2) . . . . ? N1 P2 C1 P1 -52.2(3) . . . . ? C14 P2 C1 P1 179.8(2) . . . . ? C20 P2 C1 P1 64.1(3) . . . . ? C32 P1 C1 P2 153.7(2) . . . . ? C26 P1 C1 P2 -97.0(3) . . . . ? Pd1 P1 C1 P2 25.1(3) . . . . ? P3 O2 C2 C3 -95.9(6) . . . . ? P3 O2 C2 C7 87.9(5) . . . . ? C7 C2 C3 C4 2.1(9) . . . . ? O2 C2 C3 C4 -174.1(5) . . . . ? C2 C3 C4 C5 0.0(9) . . . . ? C3 C4 C5 C6 -1.4(9) . . . . ? C4 C5 C6 C7 0.7(9) . . . . ? C5 C6 C7 C2 1.3(9) . . . . ? C3 C2 C7 C6 -2.8(9) . . . . ? O2 C2 C7 C6 173.3(5) . . . . ? P3 O3 C8 C9 120.6(5) . . . . ? P3 O3 C8 C13 -64.5(6) . . . . ? C13 C8 C9 C10 -3.3(9) . . . . ? O3 C8 C9 C10 171.5(5) . . . . ? C8 C9 C10 C11 3.0(10) . . . . ? C9 C10 C11 C12 -0.9(10) . . . . ? C10 C11 C12 C13 -0.9(11) . . . . ? C9 C8 C13 C12 1.5(9) . . . . ? O3 C8 C13 C12 -173.1(5) . . . . ? C11 C12 C13 C8 0.5(10) . . . . ? N1 P2 C14 C19 -104.2(5) . . . . ? C20 P2 C14 C19 133.5(4) . . . . ? C1 P2 C14 C19 16.5(5) . . . . ? N1 P2 C14 C15 81.1(5) . . . . ? C20 P2 C14 C15 -41.2(5) . . . . ? C1 P2 C14 C15 -158.2(4) . . . . ? C19 C14 C15 C16 0.5(9) . . . . ? P2 C14 C15 C16 175.3(5) . . . . ? C14 C15 C16 C17 -1.8(9) . . . . ? C15 C16 C17 C18 1.6(9) . . . . ? C16 C17 C18 C19 -0.1(9) . . . . ? C15 C14 C19 C18 1.0(8) . . . . ? P2 C14 C19 C18 -173.7(4) . . . . ? C17 C18 C19 C14 -1.2(9) . . . . ? N1 P2 C20 C25 -8.5(4) . . . . ? C14 P2 C20 C25 119.3(4) . . . . ? C1 P2 C20 C25 -122.4(4) . . . . ? N1 P2 C20 C21 170.5(3) . . . . ? C14 P2 C20 C21 -61.7(4) . . . . ? C1 P2 C20 C21 56.6(4) . . . . ? C25 C20 C21 C22 2.1(6) . . . . ? P2 C20 C21 C22 -177.0(3) . . . . ? C20 C21 C22 C23 -1.5(7) . . . . ? C21 C22 C23 C24 0.1(7) . . . . ? C22 C23 C24 C25 0.7(7) . . . . ? C21 C20 C25 C24 -1.2(6) . . . . ? P2 C20 C25 C24 177.8(3) . . . . ? C23 C24 C25 C20 -0.2(7) . . . . ? C32 P1 C26 C31 54.7(4) . . . . ? C1 P1 C26 C31 -56.7(4) . . . . ? Pd1 P1 C26 C31 -171.6(3) . . . . ? C32 P1 C26 C27 -130.2(4) . . . . ? C1 P1 C26 C27 118.4(4) . . . . ? Pd1 P1 C26 C27 3.5(4) . . . . ? C31 C26 C27 C28 2.1(7) . . . . ? P1 C26 C27 C28 -172.9(4) . . . . ? C26 C27 C28 C29 -0.4(7) . . . . ? C27 C28 C29 C30 -1.1(8) . . . . ? C28 C29 C30 C31 1.0(8) . . . . ? C29 C30 C31 C26 0.7(7) . . . . ? C27 C26 C31 C30 -2.3(7) . . . . ? P1 C26 C31 C30 173.0(4) . . . . ? C26 P1 C32 C33 48.5(5) . . . . ? C1 P1 C32 C33 156.9(4) . . . . ? Pd1 P1 C32 C33 -83.0(5) . . . . ? C26 P1 C32 C37 -132.6(5) . . . . ? C1 P1 C32 C37 -24.2(5) . . . . ? Pd1 P1 C32 C37 95.8(4) . . . . ? C37 C32 C33 C34 1.3(9) . . . . ? P1 C32 C33 C34 -179.8(5) . . . . ? C32 C33 C34 C35 -1.7(10) . . . . ? C33 C34 C35 C36 0.9(10) . . . . ? C34 C35 C36 C37 0.2(10) . . . . ? C35 C36 C37 C32 -0.5(9) . . . . ? C33 C32 C37 C36 -0.2(8) . . . . ? P1 C32 C37 C36 -179.1(4) . . . . ? _diffrn_measured_fraction_theta_max 0.950 _diffrn_reflns_theta_full 70.37 _diffrn_measured_fraction_theta_full 0.950 _refine_diff_density_max 1.186 _refine_diff_density_min -0.616 _refine_diff_density_rms 0.094 #===END #=============================================================================== data_5b _database_code_depnum_ccdc_archive 'CCDC 613047' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H41 Cl2 N2 O3 P3 Pd1' _chemical_formula_sum 'C38 H41 Cl2 N2 O3 P3 Pd' _chemical_formula_weight 843.94 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.64380(10) _cell_length_b 14.8151(2) _cell_length_c 23.1199(2) _cell_angle_alpha 90.00 _cell_angle_beta 122.635(5) _cell_angle_gamma 90.00 _cell_volume 3935.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7183 _cell_measurement_theta_min 2 _cell_measurement_theta_max 70 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1728 _exptl_absorpt_coefficient_mu 6.507 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.31 _exptl_absorpt_correction_T_max 0.6658 _exptl_absorpt_process_details ; 'XABS (Parkin, Hope,1995)' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33004 _diffrn_reflns_av_R_equivalents 0.099 _diffrn_reflns_av_sigmaI/netI 0.0475 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 68.46 _reflns_number_total 7224 _reflns_number_gt 6241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^)+(0.0936P)^2^+0.7660P] 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 7224 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0526 _refine_ls_R_factor_gt 0.0474 _refine_ls_wR_factor_ref 0.1348 _refine_ls_wR_factor_gt 0.1286 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0666(3) 0.6094(2) 0.71980(16) 0.0411(6) Uani 1 1 d . . . H1A H 0.0320 0.5797 0.6756 0.049 Uiso 1 1 calc R . . H1B H 0.0677 0.5663 0.7517 0.049 Uiso 1 1 calc R . . C2 C -0.2734(7) 0.9101(6) 0.5514(5) 0.188(5) Uani 1 1 d . . . H2A H -0.2661 0.9461 0.5885 0.226 Uiso 1 1 calc R . . H2B H -0.2715 0.9515 0.5195 0.226 Uiso 1 1 calc R . . C3 C -0.3782(7) 0.8717(9) 0.5188(5) 0.185(5) Uani 1 1 d . . . H3A H -0.3852 0.8309 0.4845 0.277 Uiso 1 1 calc R . . H3B H -0.4370 0.9175 0.4972 0.277 Uiso 1 1 calc R . . H3C H -0.3881 0.8390 0.5512 0.277 Uiso 1 1 calc R . . C4 C 0.0566(5) 0.8804(3) 0.5854(3) 0.0841(14) Uani 1 1 d . . . H4A H -0.0088 0.8738 0.5384 0.101 Uiso 1 1 calc R . . H4B H 0.0843 0.8207 0.6044 0.101 Uiso 1 1 calc R . . C5 C 0.1512(5) 0.9319(4) 0.5866(3) 0.1015(17) Uani 1 1 d . . . H5A H 0.2162 0.9376 0.6331 0.152 Uiso 1 1 calc R . . H5B H 0.1233 0.9909 0.5675 0.152 Uiso 1 1 calc R . . H5C H 0.1753 0.9005 0.5600 0.152 Uiso 1 1 calc R . . C6 C -0.1719(3) 0.6593(2) 0.65553(19) 0.0504(8) Uani 1 1 d . . . C7 C -0.2059(4) 0.6290(3) 0.5908(2) 0.0711(11) Uani 1 1 d . . . H7 H -0.1524 0.6280 0.5776 0.085 Uiso 1 1 calc R . . C8 C -0.3189(4) 0.6001(4) 0.5453(3) 0.0889(15) Uani 1 1 d . . . H8 H -0.3407 0.5797 0.5019 0.107 Uiso 1 1 calc R . . C9 C -0.3981(4) 0.6012(4) 0.5637(3) 0.0830(14) Uani 1 1 d . . . H9 H -0.4736 0.5810 0.5330 0.100 Uiso 1 1 calc R . . C10 C -0.3673(4) 0.6320(3) 0.6269(3) 0.0831(14) Uani 1 1 d . . . H10 H -0.4223 0.6339 0.6389 0.100 Uiso 1 1 calc R . . C11 C -0.2526(3) 0.6608(3) 0.6741(2) 0.0681(11) Uani 1 1 d . . . H11 H -0.2313 0.6807 0.7176 0.082 Uiso 1 1 calc R . . C12 C -0.0051(3) 0.7213(2) 0.79391(17) 0.0467(7) Uani 1 1 d . . . C13 C 0.0132(3) 0.8083(2) 0.8207(2) 0.0567(9) Uani 1 1 d . . . H13 H 0.0135 0.8573 0.7957 0.068 Uiso 1 1 calc R . . C14 C 0.0310(4) 0.8209(3) 0.8852(2) 0.0694(11) Uani 1 1 d . . . H14 H 0.0422 0.8790 0.9030 0.083 Uiso 1 1 calc R . . C15 C 0.0325(4) 0.7492(3) 0.9230(2) 0.0697(11) Uani 1 1 d . . . H15 H 0.0465 0.7586 0.9666 0.084 Uiso 1 1 calc R . . C16 C 0.0133(4) 0.6630(4) 0.8965(2) 0.0720(11) Uani 1 1 d . . . H16 H 0.0136 0.6145 0.9221 0.086 Uiso 1 1 calc R . . C17 C -0.0066(4) 0.6485(3) 0.8317(2) 0.0605(9) Uani 1 1 d . . . H17 H -0.0208 0.5905 0.8135 0.073 Uiso 1 1 calc R . . C18 C 0.2653(3) 0.7104(3) 0.82441(17) 0.0520(8) Uani 1 1 d . . . C19 C 0.2819(4) 0.6727(4) 0.8840(2) 0.0720(12) Uani 1 1 d . . . H19 H 0.2753 0.6106 0.8870 0.086 Uiso 1 1 calc R . . C20 C 0.3084(4) 0.7279(5) 0.9388(2) 0.0929(17) Uani 1 1 d . . . H20 H 0.3210 0.7025 0.9791 0.111 Uiso 1 1 calc R . . C21 C 0.3162(5) 0.8188(5) 0.9344(3) 0.107(2) Uani 1 1 d . . . H21 H 0.3327 0.8552 0.9714 0.128 Uiso 1 1 calc R . . C22 C 0.2999(5) 0.8571(4) 0.8759(3) 0.0948(18) Uani 1 1 d . . . H22 H 0.3057 0.9193 0.8734 0.114 Uiso 1 1 calc R . . C23 C 0.2744(4) 0.8026(3) 0.8199(2) 0.0659(11) Uani 1 1 d . . . H23 H 0.2637 0.8283 0.7801 0.079 Uiso 1 1 calc R . . C24 C 0.2955(3) 0.5336(2) 0.78053(17) 0.0482(7) Uani 1 1 d . . . C25 C 0.4100(3) 0.5317(3) 0.8351(2) 0.0680(10) Uani 1 1 d . . . H25 H 0.4461 0.5846 0.8587 0.082 Uiso 1 1 calc R . . C26 C 0.4712(4) 0.4512(4) 0.8548(3) 0.0892(15) Uani 1 1 d . . . H26 H 0.5482 0.4502 0.8917 0.107 Uiso 1 1 calc R . . C27 C 0.4181(5) 0.3723(4) 0.8199(3) 0.0866(16) Uani 1 1 d . . . H27 H 0.4590 0.3181 0.8333 0.104 Uiso 1 1 calc R . . C28 C 0.3053(5) 0.3745(3) 0.7655(3) 0.0778(13) Uani 1 1 d . . . H28 H 0.2697 0.3216 0.7417 0.093 Uiso 1 1 calc R . . C29 C 0.2442(4) 0.4538(3) 0.7457(2) 0.0603(9) Uani 1 1 d . . . H29 H 0.1674 0.4542 0.7085 0.072 Uiso 1 1 calc R . . C30 C 0.4003(3) 0.7410(2) 0.74356(18) 0.0497(7) Uani 1 1 d . . . C31 C 0.5860(3) 0.8207(3) 0.83410(19) 0.0554(9) Uani 1 1 d . . . C32 C 0.5814(4) 0.9137(3) 0.8380(2) 0.0618(9) Uani 1 1 d . . . C33 C 0.6844(5) 0.9561(4) 0.8879(3) 0.0818(14) Uani 1 1 d . . . H33 H 0.6854 1.0185 0.8927 0.098 Uiso 1 1 calc R . . C34 C 0.7828(5) 0.9085(5) 0.9294(3) 0.0926(17) Uani 1 1 d . . . H34 H 0.8502 0.9388 0.9617 0.111 Uiso 1 1 calc R . . C35 C 0.7846(4) 0.8178(5) 0.9246(3) 0.0914(18) Uani 1 1 d . . . H35 H 0.8530 0.7866 0.9542 0.110 Uiso 1 1 calc R . . C36 C 0.6862(3) 0.7701(3) 0.8762(2) 0.0717(11) Uani 1 1 d . . . C37 C 0.4736(4) 0.9661(3) 0.7903(3) 0.0837(13) Uani 1 1 d . . . H37A H 0.4458 0.9499 0.7437 0.126 Uiso 1 1 calc R . . H37B H 0.4908 1.0295 0.7966 0.126 Uiso 1 1 calc R . . H37C H 0.4149 0.9527 0.7999 0.126 Uiso 1 1 calc R . . C38 C 0.6887(5) 0.6700(4) 0.8667(4) 0.112(2) Uani 1 1 d . . . H38A H 0.6338 0.6410 0.8745 0.168 Uiso 1 1 calc R . . H38B H 0.7654 0.6474 0.8988 0.168 Uiso 1 1 calc R . . H38C H 0.6684 0.6577 0.8207 0.168 Uiso 1 1 calc R . . Cl1 Cl 0.08894(7) 0.61885(6) 0.58457(4) 0.0565(2) Uani 1 1 d . . . Cl2 Cl 0.32256(9) 0.71769(8) 0.59804(5) 0.0699(3) Uani 1 1 d . . . N1 N 0.0043(3) 0.78628(19) 0.68141(15) 0.0486(6) Uani 1 1 d . . . N2 N 0.4851(2) 0.7750(2) 0.78435(15) 0.0543(7) Uani 1 1 d . . . O1 O -0.0732(3) 0.94665(19) 0.68936(17) 0.0785(8) Uani 1 1 d . . . O2 O -0.1748(3) 0.8553(2) 0.57903(17) 0.0898(10) Uani 1 1 d . . . O3 O 0.0203(3) 0.92681(18) 0.62464(16) 0.0757(8) Uani 1 1 d . . . P1 P 0.21705(7) 0.63928(5) 0.74975(4) 0.04012(19) Uani 1 1 d . . . P2 P -0.02577(7) 0.70335(5) 0.71099(4) 0.04150(19) Uani 1 1 d . . . P3 P -0.05636(9) 0.88040(6) 0.64860(5) 0.0559(2) Uani 1 1 d . . . Pd1 Pd 0.257899(18) 0.685234(15) 0.671877(11) 0.04132(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0442(16) 0.0352(14) 0.0470(16) -0.0035(12) 0.0266(14) -0.0009(12) C2 0.106(6) 0.125(7) 0.184(8) -0.027(6) -0.020(6) 0.046(5) C3 0.104(6) 0.285(14) 0.140(7) 0.046(8) 0.049(5) 0.080(8) C4 0.127(4) 0.056(2) 0.104(3) 0.001(2) 0.085(3) -0.001(3) C5 0.111(4) 0.094(4) 0.126(4) 0.003(3) 0.081(4) -0.001(3) C6 0.0433(17) 0.0407(16) 0.064(2) 0.0019(15) 0.0272(16) 0.0025(14) C7 0.052(2) 0.091(3) 0.060(2) -0.004(2) 0.0240(18) -0.004(2) C8 0.061(3) 0.109(4) 0.070(3) -0.015(3) 0.018(2) -0.014(3) C9 0.044(2) 0.076(3) 0.097(3) -0.004(3) 0.018(2) -0.004(2) C10 0.053(2) 0.076(3) 0.122(4) 0.001(3) 0.048(3) -0.003(2) C11 0.057(2) 0.063(2) 0.090(3) -0.009(2) 0.044(2) -0.0033(18) C12 0.0483(17) 0.0470(17) 0.0504(17) -0.0024(14) 0.0304(15) 0.0035(14) C13 0.062(2) 0.051(2) 0.060(2) -0.0040(15) 0.0350(19) 0.0021(16) C14 0.073(3) 0.067(3) 0.069(3) -0.021(2) 0.039(2) 0.0011(19) C15 0.074(3) 0.089(3) 0.056(2) -0.007(2) 0.042(2) 0.004(2) C16 0.085(3) 0.079(3) 0.067(2) 0.005(2) 0.051(2) 0.005(2) C17 0.083(3) 0.049(2) 0.067(2) -0.0001(17) 0.053(2) 0.0008(18) C18 0.0437(17) 0.066(2) 0.0473(18) -0.0140(16) 0.0249(15) -0.0078(16) C19 0.068(3) 0.098(3) 0.047(2) -0.001(2) 0.030(2) 0.005(2) C20 0.067(3) 0.155(6) 0.050(2) -0.023(3) 0.028(2) -0.006(3) C21 0.082(3) 0.164(7) 0.085(4) -0.077(4) 0.052(3) -0.052(4) C22 0.091(3) 0.091(4) 0.126(4) -0.064(3) 0.074(3) -0.046(3) C23 0.068(2) 0.066(2) 0.078(3) -0.027(2) 0.049(2) -0.0249(19) C24 0.0476(18) 0.0506(18) 0.0540(18) 0.0119(15) 0.0324(15) 0.0084(14) C25 0.055(2) 0.073(3) 0.067(2) 0.010(2) 0.0263(19) 0.0124(19) C26 0.063(3) 0.106(4) 0.094(3) 0.036(3) 0.039(3) 0.033(3) C27 0.094(4) 0.077(3) 0.116(4) 0.046(3) 0.075(3) 0.047(3) C28 0.098(4) 0.049(2) 0.116(4) 0.012(2) 0.077(3) 0.016(2) C29 0.061(2) 0.0480(19) 0.080(2) 0.0050(18) 0.044(2) 0.0044(17) C30 0.0470(19) 0.0536(19) 0.0532(18) 0.0021(15) 0.0301(16) 0.0001(16) C31 0.0447(19) 0.067(2) 0.053(2) -0.0061(16) 0.0259(16) -0.0134(16) C32 0.068(2) 0.064(2) 0.061(2) -0.0061(18) 0.0400(19) -0.0159(19) C33 0.093(3) 0.081(3) 0.080(3) -0.021(2) 0.052(3) -0.037(3) C34 0.065(3) 0.125(5) 0.068(3) -0.012(3) 0.023(2) -0.039(3) C35 0.046(2) 0.132(6) 0.071(3) 0.013(3) 0.015(2) -0.011(3) C36 0.049(2) 0.086(3) 0.074(3) 0.008(2) 0.029(2) -0.004(2) C37 0.092(3) 0.066(3) 0.102(3) 0.004(2) 0.058(3) 0.005(2) C38 0.085(4) 0.086(4) 0.164(6) 0.024(4) 0.066(4) 0.019(3) Cl1 0.0490(4) 0.0689(5) 0.0447(4) -0.0082(4) 0.0207(3) -0.0097(4) Cl2 0.0716(6) 0.0915(7) 0.0582(5) -0.0002(5) 0.0425(5) -0.0182(5) N1 0.0555(16) 0.0375(13) 0.0548(16) -0.0009(12) 0.0310(14) -0.0014(12) N2 0.0417(16) 0.0650(19) 0.0545(16) -0.0046(14) 0.0248(14) -0.0094(14) O1 0.118(3) 0.0435(14) 0.102(2) -0.0008(14) 0.078(2) 0.0068(16) O2 0.075(2) 0.077(2) 0.083(2) 0.0045(17) 0.0196(17) 0.0179(17) O3 0.117(2) 0.0439(14) 0.097(2) 0.0059(14) 0.078(2) 0.0001(15) P1 0.0399(4) 0.0395(4) 0.0404(4) -0.0010(3) 0.0213(3) -0.0020(3) P2 0.0429(4) 0.0363(4) 0.0474(4) -0.0015(3) 0.0257(4) 0.0004(3) P3 0.0708(6) 0.0371(4) 0.0653(5) 0.0026(4) 0.0404(5) 0.0037(4) Pd1 0.04084(17) 0.04200(17) 0.04051(17) -0.00003(8) 0.02154(13) -0.00274(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 P2 1.813(3) . ? C1 P1 1.832(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.333(13) . ? C2 O2 1.396(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 O3 1.422(5) . ? C4 C5 1.486(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.382(6) . ? C6 C11 1.383(5) . ? C6 P2 1.813(4) . ? C7 C8 1.385(6) . ? C7 H7 0.9300 . ? C8 C9 1.359(7) . ? C8 H8 0.9300 . ? C9 C10 1.364(7) . ? C9 H9 0.9300 . ? C10 C11 1.407(6) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 C13 1.394(5) . ? C12 C17 1.394(5) . ? C12 P2 1.801(3) . ? C13 C14 1.387(6) . ? C13 H13 0.9300 . ? C14 C15 1.369(7) . ? C14 H14 0.9300 . ? C15 C16 1.379(7) . ? C15 H15 0.9300 . ? C16 C17 1.389(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C23 1.381(6) . ? C18 C19 1.387(6) . ? C18 P1 1.816(3) . ? C19 C20 1.383(7) . ? C19 H19 0.9300 . ? C20 C21 1.359(9) . ? C20 H20 0.9300 . ? C21 C22 1.371(9) . ? C21 H21 0.9300 . ? C22 C23 1.402(6) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C25 1.381(5) . ? C24 C29 1.389(5) . ? C24 P1 1.811(3) . ? C25 C26 1.385(7) . ? C25 H25 0.9300 . ? C26 C27 1.383(8) . ? C26 H26 0.9300 . ? C27 C28 1.365(8) . ? C27 H27 0.9300 . ? C28 C29 1.369(6) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 N2 1.143(4) . ? C30 Pd1 1.931(4) . ? C31 C32 1.385(6) . ? C31 C36 1.393(6) . ? C31 N2 1.403(5) . ? C32 C33 1.398(6) . ? C32 C37 1.494(6) . ? C33 C34 1.352(8) . ? C33 H33 0.9300 . ? C34 C35 1.351(8) . ? C34 H34 0.9300 . ? C35 C36 1.391(7) . ? C35 H35 0.9300 . ? C36 C38 1.502(8) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? Cl1 Pd1 2.3102(8) . ? Cl2 Pd1 2.3554(9) . ? N1 P2 1.564(3) . ? N1 P3 1.590(3) . ? O1 P3 1.462(3) . ? O2 P3 1.592(3) . ? O3 P3 1.581(3) . ? P1 Pd1 2.2579(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 P2 C1 P1 115.25(16) . . ? P2 C1 H1A 108.5 . . ? P1 C1 H1A 108.5 . . ? P2 C1 H1B 108.5 . . ? P1 C1 H1B 108.5 . . ? H1A C1 H1B 107.5 . . ? C3 C2 O2 119.1(8) . . ? C3 C2 H2A 107.5 . . ? O2 C2 H2A 107.5 . . ? C3 C2 H2B 107.5 . . ? O2 C2 H2B 107.5 . . ? H2A C2 H2B 107.0 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? O3 C4 C5 109.7(4) . . ? O3 C4 H4A 109.7 . . ? C5 C4 H4A 109.7 . . ? O3 C4 H4B 109.7 . . ? C5 C4 H4B 109.7 . . ? H4A C4 H4B 108.2 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 119.0(4) . . ? C7 C6 P2 118.8(3) . . ? C11 C6 P2 122.1(3) . . ? C6 C7 C8 120.6(4) . . ? C6 C7 H7 119.7 . . ? C8 C7 H7 119.7 . . ? C9 C8 C7 120.4(5) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.2(4) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 120.3(4) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C6 C11 C10 119.5(4) . . ? C6 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C17 119.8(3) . . ? C13 C12 P2 119.8(3) . . ? C17 C12 P2 120.4(3) . . ? C14 C13 C12 119.2(4) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C15 C14 C13 121.0(4) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 120.1(4) . . ? C14 C15 H15 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.2(4) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C12 119.7(4) . . ? C16 C17 H17 120.1 . . ? C12 C17 H17 120.1 . . ? C23 C18 C19 120.1(4) . . ? C23 C18 P1 120.2(3) . . ? C19 C18 P1 119.4(3) . . ? C20 C19 C18 119.6(5) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C21 C20 C19 120.7(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 120.4(5) . . ? C20 C21 H21 119.8 . . ? C22 C21 H21 119.8 . . ? C21 C22 C23 120.1(5) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C18 C23 C22 119.1(5) . . ? C18 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C29 118.7(4) . . ? C25 C24 P1 120.9(3) . . ? C29 C24 P1 120.1(3) . . ? C24 C25 C26 120.1(5) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C27 C26 C25 120.2(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C28 C27 C26 119.5(4) . . ? C28 C27 H27 120.2 . . ? C26 C27 H27 120.2 . . ? C27 C28 C29 120.7(5) . . ? C27 C28 H28 119.7 . . ? C29 C28 H28 119.7 . . ? C28 C29 C24 120.7(4) . . ? C28 C29 H29 119.6 . . ? C24 C29 H29 119.6 . . ? N2 C30 Pd1 177.7(3) . . ? C32 C31 C36 123.5(4) . . ? C32 C31 N2 118.3(4) . . ? C36 C31 N2 118.2(4) . . ? C31 C32 C33 116.1(4) . . ? C31 C32 C37 122.1(4) . . ? C33 C32 C37 121.8(4) . . ? C34 C33 C32 121.6(5) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C35 C34 C33 121.0(5) . . ? C35 C34 H34 119.5 . . ? C33 C34 H34 119.5 . . ? C34 C35 C36 121.3(5) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C35 C36 C31 116.5(5) . . ? C35 C36 C38 122.1(5) . . ? C31 C36 C38 121.3(4) . . ? C32 C37 H37A 109.5 . . ? C32 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C32 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P2 N1 P3 134.9(2) . . ? C30 N2 C31 177.1(4) . . ? C2 O2 P3 122.0(4) . . ? C4 O3 P3 122.5(3) . . ? C24 P1 C18 107.07(17) . . ? C24 P1 C1 104.15(15) . . ? C18 P1 C1 104.93(15) . . ? C24 P1 Pd1 103.06(10) . . ? C18 P1 Pd1 117.64(13) . . ? C1 P1 Pd1 118.65(10) . . ? N1 P2 C12 114.98(16) . . ? N1 P2 C6 114.90(16) . . ? C12 P2 C6 106.69(16) . . ? N1 P2 C1 108.75(15) . . ? C12 P2 C1 107.05(15) . . ? C6 P2 C1 103.63(15) . . ? O1 P3 O3 107.32(17) . . ? O1 P3 N1 120.23(17) . . ? O3 P3 N1 106.03(16) . . ? O1 P3 O2 112.4(2) . . ? O3 P3 O2 104.5(2) . . ? N1 P3 O2 105.14(17) . . ? C30 Pd1 P1 90.64(10) . . ? C30 Pd1 Cl1 178.80(10) . . ? P1 Pd1 Cl1 90.53(3) . . ? C30 Pd1 Cl2 86.45(10) . . ? P1 Pd1 Cl2 171.68(4) . . ? Cl1 Pd1 Cl2 92.35(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 C6 C7 C8 -0.4(7) . . . . ? P2 C6 C7 C8 -176.0(4) . . . . ? C6 C7 C8 C9 0.1(8) . . . . ? C7 C8 C9 C10 0.8(9) . . . . ? C8 C9 C10 C11 -1.4(8) . . . . ? C7 C6 C11 C10 -0.3(7) . . . . ? P2 C6 C11 C10 175.2(4) . . . . ? C9 C10 C11 C6 1.2(7) . . . . ? C17 C12 C13 C14 0.7(6) . . . . ? P2 C12 C13 C14 -178.9(3) . . . . ? C12 C13 C14 C15 0.9(7) . . . . ? C13 C14 C15 C16 -1.6(7) . . . . ? C14 C15 C16 C17 0.6(7) . . . . ? C15 C16 C17 C12 1.0(7) . . . . ? C13 C12 C17 C16 -1.7(6) . . . . ? P2 C12 C17 C16 177.9(3) . . . . ? C23 C18 C19 C20 -0.5(6) . . . . ? P1 C18 C19 C20 -174.2(4) . . . . ? C18 C19 C20 C21 1.2(8) . . . . ? C19 C20 C21 C22 -1.2(9) . . . . ? C20 C21 C22 C23 0.4(8) . . . . ? C19 C18 C23 C22 -0.3(6) . . . . ? P1 C18 C23 C22 173.3(3) . . . . ? C21 C22 C23 C18 0.4(7) . . . . ? C29 C24 C25 C26 -0.7(6) . . . . ? P1 C24 C25 C26 -175.4(3) . . . . ? C24 C25 C26 C27 0.1(7) . . . . ? C25 C26 C27 C28 0.5(8) . . . . ? C26 C27 C28 C29 -0.5(7) . . . . ? C27 C28 C29 C24 -0.1(7) . . . . ? C25 C24 C29 C28 0.7(6) . . . . ? P1 C24 C29 C28 175.4(3) . . . . ? C36 C31 C32 C33 -0.5(6) . . . . ? N2 C31 C32 C33 -179.4(3) . . . . ? C36 C31 C32 C37 177.7(4) . . . . ? N2 C31 C32 C37 -1.1(6) . . . . ? C31 C32 C33 C34 0.5(7) . . . . ? C37 C32 C33 C34 -177.7(4) . . . . ? C32 C33 C34 C35 -0.8(8) . . . . ? C33 C34 C35 C36 1.1(9) . . . . ? C34 C35 C36 C31 -1.1(8) . . . . ? C34 C35 C36 C38 175.6(6) . . . . ? C32 C31 C36 C35 0.8(6) . . . . ? N2 C31 C36 C35 179.6(4) . . . . ? C32 C31 C36 C38 -175.9(5) . . . . ? N2 C31 C36 C38 3.0(7) . . . . ? Pd1 C30 N2 C31 92(11) . . . . ? C32 C31 N2 C30 -17(7) . . . . ? C36 C31 N2 C30 164(7) . . . . ? C3 C2 O2 P3 -145.2(8) . . . . ? C5 C4 O3 P3 -165.1(4) . . . . ? C25 C24 P1 C18 -36.4(3) . . . . ? C29 C24 P1 C18 149.0(3) . . . . ? C25 C24 P1 C1 -147.2(3) . . . . ? C29 C24 P1 C1 38.2(3) . . . . ? C25 C24 P1 Pd1 88.3(3) . . . . ? C29 C24 P1 Pd1 -86.3(3) . . . . ? C23 C18 P1 C24 145.3(3) . . . . ? C19 C18 P1 C24 -41.1(4) . . . . ? C23 C18 P1 C1 -104.4(3) . . . . ? C19 C18 P1 C1 69.2(3) . . . . ? C23 C18 P1 Pd1 30.0(4) . . . . ? C19 C18 P1 Pd1 -156.4(3) . . . . ? P2 C1 P1 C24 161.27(17) . . . . ? P2 C1 P1 C18 48.9(2) . . . . ? P2 C1 P1 Pd1 -84.94(17) . . . . ? P3 N1 P2 C12 -74.0(3) . . . . ? P3 N1 P2 C6 50.4(3) . . . . ? P3 N1 P2 C1 166.0(2) . . . . ? C13 C12 P2 N1 12.2(4) . . . . ? C17 C12 P2 N1 -167.4(3) . . . . ? C13 C12 P2 C6 -116.4(3) . . . . ? C17 C12 P2 C6 64.0(3) . . . . ? C13 C12 P2 C1 133.1(3) . . . . ? C17 C12 P2 C1 -46.5(3) . . . . ? C7 C6 P2 N1 59.2(4) . . . . ? C11 C6 P2 N1 -116.3(4) . . . . ? C7 C6 P2 C12 -172.1(3) . . . . ? C11 C6 P2 C12 12.4(4) . . . . ? C7 C6 P2 C1 -59.3(4) . . . . ? C11 C6 P2 C1 125.2(3) . . . . ? P1 C1 P2 N1 39.0(2) . . . . ? P1 C1 P2 C12 -85.8(2) . . . . ? P1 C1 P2 C6 161.64(18) . . . . ? C4 O3 P3 O1 178.1(4) . . . . ? C4 O3 P3 N1 48.4(4) . . . . ? C4 O3 P3 O2 -62.4(4) . . . . ? P2 N1 P3 O1 62.9(3) . . . . ? P2 N1 P3 O3 -175.4(3) . . . . ? P2 N1 P3 O2 -65.1(3) . . . . ? C2 O2 P3 O1 18.3(7) . . . . ? C2 O2 P3 O3 -97.7(7) . . . . ? C2 O2 P3 N1 150.8(7) . . . . ? N2 C30 Pd1 P1 -177(100) . . . . ? N2 C30 Pd1 Cl1 16(13) . . . . ? N2 C30 Pd1 Cl2 11(9) . . . . ? C24 P1 Pd1 C30 -85.42(16) . . . . ? C18 P1 Pd1 C30 32.08(17) . . . . ? C1 P1 Pd1 C30 160.20(15) . . . . ? C24 P1 Pd1 Cl1 94.31(12) . . . . ? C18 P1 Pd1 Cl1 -148.20(14) . . . . ? C1 P1 Pd1 Cl1 -20.07(11) . . . . ? C24 P1 Pd1 Cl2 -15.9(3) . . . . ? C18 P1 Pd1 Cl2 101.5(3) . . . . ? C1 P1 Pd1 Cl2 -130.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 68.46 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.673 _refine_diff_density_min -0.894 _refine_diff_density_rms 0.097 #===END #=============================================================================== data_7 _database_code_depnum_ccdc_archive 'CCDC 613048' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H64 Cl2 N2 O6 P6 Pd1' _chemical_formula_sum 'C58 H64 Cl2 N2 O6 P6 Pd' _chemical_formula_weight 1248.23 _chemical_compound_source synthesis loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 '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' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5971(2) _cell_length_b 9.9089(2) _cell_length_c 17.5208(4) _cell_angle_alpha 102.3320(10) _cell_angle_beta 98.4270(10) _cell_angle_gamma 109.9560(10) _cell_volume 1485.66(5) _cell_formula_units_Z 1 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4586 _cell_measurement_theta_max 70 _cell_measurement_theta_min 2 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.395 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 644 _exptl_absorpt_coefficient_mu 5.276 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 1.080 _exptl_absorpt_process_details ; 'SORTAV (R.H. Blessing, Acta Cryst. (1995), A51, 33-38)' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'horizontally mounted graphite crystal' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_device '95 mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f and \w scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9981 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.66 _diffrn_reflns_theta_max 70.02 _reflns_number_total 5470 _reflns_number_gt 4989 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^)+(0.0899P)^2^+1.2057P] 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 5470 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0374 _refine_ls_wR_factor_ref 0.1376 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.105 _refine_ls_restrained_S_all 1.105 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0568(4) 0.8906(4) 0.17996(19) 0.0249(6) Uani 1 1 d . . . H1A H -0.0447 0.8139 0.1495 0.030 Uiso 1 1 calc R . . H1B H 0.1155 0.8371 0.2023 0.030 Uiso 1 1 calc R . . C2 C 0.4782(5) 1.1544(6) 0.4263(3) 0.0573(12) Uani 1 1 d . . . H2A H 0.5553 1.1129 0.4139 0.069 Uiso 1 1 calc R . . H2B H 0.4344 1.1751 0.3774 0.069 Uiso 1 1 calc R . . C3 C 0.5492(10) 1.2901(8) 0.4904(5) 0.123(3) Uani 1 1 d . . . H3A H 0.4805 1.3439 0.4935 0.185 Uiso 1 1 calc R . . H3B H 0.6447 1.3528 0.4805 0.185 Uiso 1 1 calc R . . H3C H 0.5712 1.2666 0.5413 0.185 Uiso 1 1 calc R . . C4 C 0.0129(10) 0.7327(8) 0.4293(6) 0.127(4) Uani 1 1 d . . . H4A H -0.0542 0.7028 0.3750 0.152 Uiso 1 1 calc R . . H4B H 0.0763 0.6720 0.4267 0.152 Uiso 1 1 calc R . . C5 C -0.0776(10) 0.6928(8) 0.4797(5) 0.117(3) Uani 1 1 d . . . H5A H -0.0156 0.6935 0.5296 0.175 Uiso 1 1 calc R . . H5B H -0.1558 0.5920 0.4540 0.175 Uiso 1 1 calc R . . H5C H -0.1269 0.7639 0.4920 0.175 Uiso 1 1 calc R . . C6 C 0.2139(4) 0.8208(4) 0.05878(19) 0.0268(7) Uani 1 1 d . . . C7 C 0.1599(4) 0.6771(4) 0.0669(2) 0.0315(7) Uani 1 1 d . . . H7 H 0.0860 0.6502 0.0973 0.038 Uiso 1 1 calc R . . C8 C 0.2143(5) 0.5714(4) 0.0301(2) 0.0395(8) Uani 1 1 d . . . H8 H 0.1778 0.4729 0.0358 0.047 Uiso 1 1 calc R . . C9 C 0.3212(4) 0.6114(5) -0.0141(2) 0.0420(9) Uani 1 1 d . . . H9 H 0.3587 0.5400 -0.0386 0.050 Uiso 1 1 calc R . . C10 C 0.3743(4) 0.7530(4) -0.0234(2) 0.0399(9) Uani 1 1 d . . . H10 H 0.4478 0.7791 -0.0543 0.048 Uiso 1 1 calc R . . C11 C 0.3202(4) 0.8573(4) 0.0123(2) 0.0332(7) Uani 1 1 d . . . H11 H 0.3558 0.9547 0.0053 0.040 Uiso 1 1 calc R . . C12 C 0.3324(4) 1.1165(4) 0.16616(18) 0.0266(7) Uani 1 1 d . . . C13 C 0.3557(4) 1.2659(4) 0.1804(2) 0.0320(7) Uani 1 1 d . . . H13 H 0.2760 1.2938 0.1593 0.038 Uiso 1 1 calc R . . C14 C 0.4956(5) 1.3760(4) 0.2257(2) 0.0442(9) Uani 1 1 d . . . H14 H 0.5112 1.4788 0.2358 0.053 Uiso 1 1 calc R . . C15 C 0.6130(5) 1.3344(5) 0.2562(3) 0.0492(10) Uani 1 1 d . . . H15 H 0.7090 1.4092 0.2865 0.059 Uiso 1 1 calc R . . C16 C 0.5901(4) 1.1864(5) 0.2425(2) 0.0439(9) Uani 1 1 d . . . H16 H 0.6700 1.1585 0.2632 0.053 Uiso 1 1 calc R . . C17 C 0.4509(4) 1.0780(4) 0.1987(2) 0.0345(8) Uani 1 1 d . . . H17 H 0.4349 0.9754 0.1903 0.041 Uiso 1 1 calc R . . C18 C -0.1700(4) 0.9148(4) 0.2696(2) 0.0283(7) Uani 1 1 d . . . C19 C -0.2888(4) 0.8338(4) 0.2020(2) 0.0349(8) Uani 1 1 d . . . H19 H -0.2691 0.8218 0.1499 0.042 Uiso 1 1 calc R . . C20 C -0.4376(4) 0.7699(5) 0.2107(2) 0.0404(8) Uani 1 1 d . . . H20 H -0.5185 0.7116 0.1644 0.049 Uiso 1 1 calc R . . C21 C -0.4680(5) 0.7908(5) 0.2859(3) 0.0442(9) Uani 1 1 d . . . H21 H -0.5696 0.7489 0.2914 0.053 Uiso 1 1 calc R . . C22 C -0.3496(5) 0.8731(5) 0.3532(2) 0.0464(10) Uani 1 1 d . . . H22 H -0.3701 0.8872 0.4051 0.056 Uiso 1 1 calc R . . C23 C -0.2011(4) 0.9351(4) 0.3455(2) 0.0378(8) Uani 1 1 d . . . H23 H -0.1204 0.9916 0.3920 0.045 Uiso 1 1 calc R . . C24 C 0.0411(4) 1.1879(4) 0.24913(19) 0.0268(7) Uani 1 1 d . . . C25 C -0.0453(4) 1.1968(4) 0.1811(2) 0.0311(7) Uani 1 1 d . . . H25 H -0.1157 1.1081 0.1418 0.037 Uiso 1 1 calc R . . C26 C -0.0285(5) 1.3359(4) 0.1706(2) 0.0395(8) Uani 1 1 d . . . H26 H -0.0852 1.3425 0.1233 0.047 Uiso 1 1 calc R . . C27 C 0.0708(5) 1.4651(4) 0.2290(2) 0.0416(9) Uani 1 1 d . . . H27 H 0.0811 1.5602 0.2220 0.050 Uiso 1 1 calc R . . C28 C 0.1549(4) 1.4562(4) 0.2974(2) 0.0377(8) Uani 1 1 d . . . H28 H 0.2220 1.5452 0.3376 0.045 Uiso 1 1 calc R . . C29 C 0.1418(4) 1.3177(4) 0.3077(2) 0.0352(8) Uani 1 1 d . . . H29 H 0.2010 1.3115 0.3543 0.042 Uiso 1 1 calc R . . Cl1 Cl 0.20744(9) 1.19216(9) -0.00997(5) 0.0326(2) Uani 1 1 d . . . N1 N 0.1421(3) 1.0449(3) 0.34681(16) 0.0303(6) Uani 1 1 d . . . O1 O 0.2231(3) 0.8149(3) 0.32683(16) 0.0402(6) Uani 1 1 d . . . O2 O 0.3593(3) 1.0472(3) 0.44894(16) 0.0430(6) Uani 1 1 d . . . O3 O 0.1104(3) 0.8814(3) 0.44533(16) 0.0456(7) Uani 1 1 d . . . P1 P 0.15232(9) 0.96731(9) 0.10636(4) 0.02242(19) Uani 1 1 d . . . P2 P 0.02588(9) 1.00997(9) 0.26550(5) 0.0246(2) Uani 1 1 d . . . P3 P 0.20726(10) 0.93832(10) 0.38440(5) 0.0289(2) Uani 1 1 d . . . Pd1 Pd 0.0000 1.0000 0.0000 0.02203(13) Uani 1 2 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0285(16) 0.0241(15) 0.0236(15) 0.0071(12) 0.0101(12) 0.0100(13) C2 0.039(2) 0.066(3) 0.050(3) 0.015(2) 0.0092(19) 0.001(2) C3 0.137(7) 0.064(4) 0.106(6) 0.007(4) 0.043(5) -0.033(4) C4 0.157(7) 0.064(4) 0.200(9) 0.064(5) 0.143(8) 0.035(4) C5 0.157(8) 0.056(4) 0.110(6) 0.016(4) 0.071(6) -0.004(4) C6 0.0266(16) 0.0274(16) 0.0238(15) 0.0026(13) 0.0023(12) 0.0118(13) C7 0.0350(19) 0.0257(17) 0.0319(17) 0.0061(14) 0.0068(14) 0.0112(14) C8 0.049(2) 0.0272(18) 0.042(2) 0.0044(16) 0.0047(17) 0.0208(16) C9 0.037(2) 0.044(2) 0.041(2) -0.0063(17) 0.0060(16) 0.0229(17) C10 0.036(2) 0.039(2) 0.039(2) -0.0005(16) 0.0146(16) 0.0133(16) C11 0.0329(18) 0.0295(18) 0.0342(18) 0.0040(14) 0.0137(14) 0.0091(14) C12 0.0316(17) 0.0238(16) 0.0211(15) 0.0029(12) 0.0067(13) 0.0087(13) C13 0.0338(18) 0.0343(18) 0.0276(16) 0.0093(14) 0.0123(14) 0.0102(15) C14 0.049(2) 0.0254(18) 0.043(2) 0.0006(16) 0.0082(18) 0.0032(16) C15 0.037(2) 0.049(2) 0.040(2) 0.0015(18) 0.0014(17) -0.0001(18) C16 0.034(2) 0.051(2) 0.038(2) 0.0067(18) 0.0022(16) 0.0125(18) C17 0.0365(19) 0.0354(19) 0.0316(18) 0.0087(15) 0.0047(15) 0.0158(15) C18 0.0361(18) 0.0265(16) 0.0293(16) 0.0114(13) 0.0143(14) 0.0156(14) C19 0.038(2) 0.0360(19) 0.0305(18) 0.0095(15) 0.0097(15) 0.0132(16) C20 0.0323(19) 0.041(2) 0.044(2) 0.0106(17) 0.0058(16) 0.0116(16) C21 0.038(2) 0.045(2) 0.061(3) 0.023(2) 0.0253(19) 0.0178(18) C22 0.055(3) 0.055(3) 0.038(2) 0.0163(19) 0.0253(19) 0.025(2) C23 0.038(2) 0.044(2) 0.0323(18) 0.0084(16) 0.0145(15) 0.0152(17) C24 0.0301(17) 0.0258(16) 0.0264(16) 0.0076(13) 0.0127(13) 0.0104(13) C25 0.0361(18) 0.0274(17) 0.0307(17) 0.0072(14) 0.0095(14) 0.0134(14) C26 0.051(2) 0.036(2) 0.0322(18) 0.0113(16) 0.0052(16) 0.0196(17) C27 0.062(3) 0.0273(18) 0.039(2) 0.0108(16) 0.0143(18) 0.0186(17) C28 0.048(2) 0.0247(17) 0.0322(18) 0.0019(14) 0.0089(16) 0.0080(15) C29 0.046(2) 0.0347(19) 0.0250(17) 0.0088(14) 0.0078(15) 0.0154(16) Cl1 0.0320(4) 0.0329(4) 0.0272(4) 0.0121(3) 0.0064(3) 0.0038(3) N1 0.0349(15) 0.0292(15) 0.0253(14) 0.0050(11) 0.0078(12) 0.0120(12) O1 0.0482(16) 0.0372(14) 0.0393(14) 0.0086(12) 0.0093(12) 0.0233(12) O2 0.0381(15) 0.0431(15) 0.0363(14) 0.0116(12) -0.0032(11) 0.0066(12) O3 0.0554(17) 0.0413(15) 0.0379(14) 0.0170(12) 0.0213(13) 0.0085(13) P1 0.0259(4) 0.0228(4) 0.0194(4) 0.0065(3) 0.0060(3) 0.0099(3) P2 0.0307(4) 0.0229(4) 0.0210(4) 0.0056(3) 0.0078(3) 0.0112(3) P3 0.0321(5) 0.0290(4) 0.0245(4) 0.0082(3) 0.0058(3) 0.0106(4) Pd1 0.0258(2) 0.0218(2) 0.01938(19) 0.00638(13) 0.00646(13) 0.00948(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 P2 1.829(3) . ? C1 P1 1.836(3) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 C3 1.428(8) . ? C2 O2 1.440(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.353(9) . ? C4 O3 1.390(7) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.385(5) . ? C6 C11 1.397(5) . ? C6 P1 1.834(3) . ? C7 C8 1.403(5) . ? C7 H7 0.9500 . ? C8 C9 1.377(6) . ? C8 H8 0.9500 . ? C9 C10 1.374(6) . ? C9 H9 0.9500 . ? C10 C11 1.384(5) . ? C10 H10 0.9500 . ? C11 H11 0.9500 . ? C12 C13 1.380(5) . ? C12 C17 1.401(5) . ? C12 P1 1.826(3) . ? C13 C14 1.393(5) . ? C13 H13 0.9500 . ? C14 C15 1.401(6) . ? C14 H14 0.9500 . ? C15 C16 1.367(6) . ? C15 H15 0.9500 . ? C16 C17 1.377(5) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C18 C19 1.386(5) . ? C18 C23 1.393(5) . ? C18 P2 1.813(3) . ? C19 C20 1.396(5) . ? C19 H19 0.9500 . ? C20 C21 1.379(6) . ? C20 H20 0.9500 . ? C21 C22 1.382(6) . ? C21 H21 0.9500 . ? C22 C23 1.386(6) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 C25 1.386(5) . ? C24 C29 1.392(5) . ? C24 P2 1.807(3) . ? C25 C26 1.388(5) . ? C25 H25 0.9500 . ? C26 C27 1.384(5) . ? C26 H26 0.9500 . ? C27 C28 1.381(6) . ? C27 H27 0.9500 . ? C28 C29 1.388(5) . ? C28 H28 0.9500 . ? C29 H29 0.9500 . ? Cl1 Pd1 2.2969(8) . ? N1 P2 1.567(3) . ? N1 P3 1.602(3) . ? O1 P3 1.477(3) . ? O2 P3 1.579(3) . ? O3 P3 1.585(3) . ? P1 Pd1 2.3446(8) . ? Pd1 Cl1 2.2969(8) 2_575 ? Pd1 P1 2.3446(8) 2_575 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 C1 P1 121.90(18) . . ? P2 C1 H1A 106.9 . . ? P1 C1 H1A 106.9 . . ? P2 C1 H1B 106.9 . . ? P1 C1 H1B 106.9 . . ? H1A C1 H1B 106.7 . . ? C3 C2 O2 109.9(4) . . ? C3 C2 H2A 109.7 . . ? O2 C2 H2A 109.7 . . ? C3 C2 H2B 109.7 . . ? O2 C2 H2B 109.7 . . ? H2A C2 H2B 108.2 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 O3 119.5(7) . . ? C5 C4 H4A 107.5 . . ? O3 C4 H4A 107.5 . . ? C5 C4 H4B 107.5 . . ? O3 C4 H4B 107.5 . . ? H4A C4 H4B 107.0 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 119.1(3) . . ? C7 C6 P1 123.1(3) . . ? C11 C6 P1 117.8(3) . . ? C6 C7 C8 120.1(3) . . ? C6 C7 H7 119.9 . . ? C8 C7 H7 119.9 . . ? C9 C8 C7 119.5(4) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C10 C9 C8 121.0(3) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 119.6(3) . . ? C9 C10 H10 120.2 . . ? C11 C10 H10 120.2 . . ? C10 C11 C6 120.7(3) . . ? C10 C11 H11 119.7 . . ? C6 C11 H11 119.7 . . ? C13 C12 C17 118.9(3) . . ? C13 C12 P1 122.2(3) . . ? C17 C12 P1 118.9(3) . . ? C12 C13 C14 120.2(4) . . ? C12 C13 H13 119.9 . . ? C14 C13 H13 119.9 . . ? C13 C14 C15 119.7(4) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 120.3(4) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 119.8(4) . . ? C15 C16 H16 120.1 . . ? C17 C16 H16 120.1 . . ? C16 C17 C12 121.1(4) . . ? C16 C17 H17 119.4 . . ? C12 C17 H17 119.4 . . ? C19 C18 C23 119.5(3) . . ? C19 C18 P2 123.7(3) . . ? C23 C18 P2 116.7(3) . . ? C18 C19 C20 119.8(3) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 119.6(4) . . ? C20 C21 H21 120.2 . . ? C22 C21 H21 120.2 . . ? C21 C22 C23 120.5(4) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C22 C23 C18 120.1(4) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? C25 C24 C29 120.4(3) . . ? C25 C24 P2 121.7(3) . . ? C29 C24 P2 117.9(3) . . ? C24 C25 C26 119.7(3) . . ? C24 C25 H25 120.2 . . ? C26 C25 H25 120.2 . . ? C27 C26 C25 120.1(3) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C28 C27 C26 120.2(3) . . ? C28 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C27 C28 C29 120.3(3) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C24 119.4(3) . . ? C28 C29 H29 120.3 . . ? C24 C29 H29 120.3 . . ? P2 N1 P3 130.61(19) . . ? C2 O2 P3 120.2(3) . . ? C4 O3 P3 121.9(4) . . ? C12 P1 C6 102.62(15) . . ? C12 P1 C1 105.01(15) . . ? C6 P1 C1 103.29(15) . . ? C12 P1 Pd1 121.57(11) . . ? C6 P1 Pd1 104.93(10) . . ? C1 P1 Pd1 116.98(11) . . ? N1 P2 C24 106.92(16) . . ? N1 P2 C18 112.29(15) . . ? C24 P2 C18 106.75(15) . . ? N1 P2 C1 113.54(15) . . ? C24 P2 C1 111.20(15) . . ? C18 P2 C1 106.00(15) . . ? O1 P3 O2 114.49(16) . . ? O1 P3 O3 112.37(16) . . ? O2 P3 O3 97.32(15) . . ? O1 P3 N1 116.63(15) . . ? O2 P3 N1 105.42(16) . . ? O3 P3 N1 108.71(16) . . ? Cl1 Pd1 Cl1 180.00(4) 2_575 . ? Cl1 Pd1 P1 90.41(3) 2_575 2_575 ? Cl1 Pd1 P1 89.59(3) . 2_575 ? Cl1 Pd1 P1 89.59(3) 2_575 . ? Cl1 Pd1 P1 90.41(3) . . ? P1 Pd1 P1 180.00(4) 2_575 . ? 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 C6 C7 C8 1.4(5) . . . . ? P1 C6 C7 C8 -178.7(3) . . . . ? C6 C7 C8 C9 -0.2(5) . . . . ? C7 C8 C9 C10 -0.5(6) . . . . ? C8 C9 C10 C11 0.2(6) . . . . ? C9 C10 C11 C6 1.0(6) . . . . ? C7 C6 C11 C10 -1.7(5) . . . . ? P1 C6 C11 C10 178.3(3) . . . . ? C17 C12 C13 C14 0.7(5) . . . . ? P1 C12 C13 C14 -179.3(3) . . . . ? C12 C13 C14 C15 0.5(6) . . . . ? C13 C14 C15 C16 -0.8(6) . . . . ? C14 C15 C16 C17 -0.1(6) . . . . ? C15 C16 C17 C12 1.3(6) . . . . ? C13 C12 C17 C16 -1.6(5) . . . . ? P1 C12 C17 C16 178.4(3) . . . . ? C23 C18 C19 C20 -1.8(5) . . . . ? P2 C18 C19 C20 -177.0(3) . . . . ? C18 C19 C20 C21 2.1(6) . . . . ? C19 C20 C21 C22 -1.3(6) . . . . ? C20 C21 C22 C23 0.3(6) . . . . ? C21 C22 C23 C18 -0.1(6) . . . . ? C19 C18 C23 C22 0.8(6) . . . . ? P2 C18 C23 C22 176.3(3) . . . . ? C29 C24 C25 C26 1.4(5) . . . . ? P2 C24 C25 C26 -179.2(3) . . . . ? C24 C25 C26 C27 -1.9(6) . . . . ? C25 C26 C27 C28 0.8(6) . . . . ? C26 C27 C28 C29 0.7(6) . . . . ? C27 C28 C29 C24 -1.1(6) . . . . ? C25 C24 C29 C28 0.1(5) . . . . ? P2 C24 C29 C28 -179.3(3) . . . . ? C3 C2 O2 P3 143.5(6) . . . . ? C5 C4 O3 P3 -173.9(7) . . . . ? C13 C12 P1 C6 148.0(3) . . . . ? C17 C12 P1 C6 -32.0(3) . . . . ? C13 C12 P1 C1 -104.3(3) . . . . ? C17 C12 P1 C1 75.7(3) . . . . ? C13 C12 P1 Pd1 31.4(3) . . . . ? C17 C12 P1 Pd1 -148.6(2) . . . . ? C7 C6 P1 C12 123.2(3) . . . . ? C11 C6 P1 C12 -56.9(3) . . . . ? C7 C6 P1 C1 14.2(3) . . . . ? C11 C6 P1 C1 -165.9(3) . . . . ? C7 C6 P1 Pd1 -108.9(3) . . . . ? C11 C6 P1 Pd1 71.1(3) . . . . ? P2 C1 P1 C12 53.1(2) . . . . ? P2 C1 P1 C6 160.32(19) . . . . ? P2 C1 P1 Pd1 -85.0(2) . . . . ? P3 N1 P2 C24 -165.5(2) . . . . ? P3 N1 P2 C18 77.8(3) . . . . ? P3 N1 P2 C1 -42.4(3) . . . . ? C25 C24 P2 N1 178.8(3) . . . . ? C29 C24 P2 N1 -1.8(3) . . . . ? C25 C24 P2 C18 -60.8(3) . . . . ? C29 C24 P2 C18 118.5(3) . . . . ? C25 C24 P2 C1 54.4(3) . . . . ? C29 C24 P2 C1 -126.3(3) . . . . ? C19 C18 P2 N1 -160.6(3) . . . . ? C23 C18 P2 N1 24.1(3) . . . . ? C19 C18 P2 C24 82.6(3) . . . . ? C23 C18 P2 C24 -92.7(3) . . . . ? C19 C18 P2 C1 -36.1(3) . . . . ? C23 C18 P2 C1 148.6(3) . . . . ? P1 C1 P2 N1 -101.8(2) . . . . ? P1 C1 P2 C24 18.8(3) . . . . ? P1 C1 P2 C18 134.4(2) . . . . ? C2 O2 P3 O1 74.7(4) . . . . ? C2 O2 P3 O3 -166.6(3) . . . . ? C2 O2 P3 N1 -54.9(4) . . . . ? C4 O3 P3 O1 -19.5(6) . . . . ? C4 O3 P3 O2 -139.8(6) . . . . ? C4 O3 P3 N1 111.2(6) . . . . ? P2 N1 P3 O1 31.6(3) . . . . ? P2 N1 P3 O2 159.9(2) . . . . ? P2 N1 P3 O3 -96.7(3) . . . . ? C12 P1 Pd1 Cl1 -158.65(12) . . . 2_575 ? C6 P1 Pd1 Cl1 85.93(12) . . . 2_575 ? C1 P1 Pd1 Cl1 -27.81(12) . . . 2_575 ? C12 P1 Pd1 Cl1 21.35(12) . . . . ? C6 P1 Pd1 Cl1 -94.07(12) . . . . ? C1 P1 Pd1 Cl1 152.19(12) . . . . ? C12 P1 Pd1 P1 40(100) . . . 2_575 ? C6 P1 Pd1 P1 -76(100) . . . 2_575 ? C1 P1 Pd1 P1 171(100) . . . 2_575 ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 70.02 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.780 _refine_diff_density_min -0.834 _refine_diff_density_rms 0.121 #===END #=============================================================================== data_9 _database_code_depnum_ccdc_archive 'CCDC 613049' #=============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58 H64 N2 O6 P6 Pd, 2(F6 Sb), 2(C H2 Cl2)' _chemical_formula_sum 'C60 H68 Cl4 F12 N2 O6 P6 Pd Sb2' _chemical_formula_weight 1818.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.0562 5.8946 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5698(4) _cell_length_b 13.6979(4) _cell_length_c 21.3980(7) _cell_angle_alpha 82.941(2) _cell_angle_beta 86.073(2) _cell_angle_gamma 75.890(2) _cell_volume 3543.22(19) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 13845 _cell_measurement_theta_min 3.34 _cell_measurement_theta_max 69.996 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.705 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 11.403 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.0378 _exptl_absorpt_correction_T_max 0.0962 _exptl_absorpt_process_details ; 'XABS(Parkin S,Moezzi B & Hope H, 1995)' ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26848 _diffrn_reflns_av_R_equivalents 0.0426 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 70.03 _reflns_number_total 11585 _reflns_number_gt 9083 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'DIRDIF-99 (Beurskens, 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON (Spek, 2005)' _computing_publication_material 'SHELXL-97 (Sheldrick, 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^)+(0.1023P)^2^+16.5267P] 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 11585 _refine_ls_number_parameters 818 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1800 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3926(6) 0.2391(6) 0.8965(3) 0.0273(15) Uani 1 1 d . . . H1A H 0.3949 0.1668 0.9099 0.033 Uiso 1 1 calc R . . H1B H 0.4424 0.2607 0.9229 0.033 Uiso 1 1 calc R . . C1' C 0.2666(6) 0.1975(6) 0.6174(3) 0.0297(16) Uani 1 1 d . . . H1A' H 0.2223 0.2683 0.6131 0.036 Uiso 1 1 calc R . . H1B' H 0.3092 0.1865 0.5772 0.036 Uiso 1 1 calc R . . C2' C 0.1164(8) 0.0288(8) 0.8374(5) 0.0509(16) Uani 1 1 d . . . H2A' H 0.1355 0.0188 0.8822 0.061 Uiso 1 1 calc R . . H2B' H 0.1748 -0.0173 0.8144 0.061 Uiso 1 1 calc R . . C2 C 0.0686(8) 0.5310(8) 0.6985(4) 0.051(2) Uani 1 1 d . . . H2A H 0.0431 0.6026 0.7069 0.061 Uiso 1 1 calc R . . H2B H 0.0053 0.4993 0.7051 0.061 Uiso 1 1 calc R . . C3 C 0.1129(11) 0.5255(13) 0.6328(5) 0.090(5) Uani 1 1 d . . . H3A H 0.1390 0.4544 0.6250 0.135 Uiso 1 1 calc R . . H3B H 0.1739 0.5590 0.6261 0.135 Uiso 1 1 calc R . . H3C H 0.0549 0.5595 0.6037 0.135 Uiso 1 1 calc R . . C3' C 0.0136(8) 0.0005(8) 0.8330(5) 0.0509(16) Uani 1 1 d . . . H3A' H -0.0054 0.0087 0.7887 0.076 Uiso 1 1 calc R . . H3B' H -0.0444 0.0441 0.8568 0.076 Uiso 1 1 calc R . . H3C' H 0.0213 -0.0703 0.8505 0.076 Uiso 1 1 calc R . . C4 C 0.169(4) 0.633(2) 0.8435(12) 0.31(3) Uani 1 1 d . . . H4A H 0.2094 0.6280 0.8823 0.376 Uiso 1 1 calc R . . H4B H 0.0910 0.6590 0.8561 0.376 Uiso 1 1 calc R . . C4' C -0.1068(8) 0.2944(8) 0.7726(5) 0.0493(16) Uani 1 1 d . . . H4A' H -0.0570 0.3236 0.7945 0.059 Uiso 1 1 calc R . . H4B' H -0.1587 0.2709 0.8045 0.059 Uiso 1 1 calc R . . C5' C -0.1689(8) 0.3732(8) 0.7249(5) 0.0493(16) Uani 1 1 d . . . H5A' H -0.2132 0.4299 0.7461 0.074 Uiso 1 1 calc R . . H5B' H -0.2172 0.3436 0.7029 0.074 Uiso 1 1 calc R . . H5C' H -0.1170 0.3978 0.6943 0.074 Uiso 1 1 calc R . . C5 C 0.193(2) 0.7148(16) 0.8099(18) 0.25(2) Uani 1 1 d . . . H5A H 0.2534 0.7325 0.8291 0.379 Uiso 1 1 calc R . . H5B H 0.1282 0.7716 0.8096 0.379 Uiso 1 1 calc R . . H5C H 0.2149 0.7000 0.7666 0.379 Uiso 1 1 calc R . . C6' C 0.4258(6) 0.0522(6) 0.6936(3) 0.0292(16) Uani 1 1 d . . . C6 C 0.5611(6) 0.1544(6) 0.8079(3) 0.0264(15) Uani 1 1 d . . . C7 C 0.5627(6) 0.0566(6) 0.8368(4) 0.0332(17) Uani 1 1 d . . . H7 H 0.5000 0.0436 0.8605 0.040 Uiso 1 1 calc R . . C7' C 0.4019(6) -0.0026(6) 0.7500(4) 0.0321(16) Uani 1 1 d . . . H7' H 0.3562 0.0309 0.7818 0.039 Uiso 1 1 calc R . . C8 C 0.6556(7) -0.0213(6) 0.8309(4) 0.0381(18) Uani 1 1 d . . . H8 H 0.6564 -0.0876 0.8503 0.046 Uiso 1 1 calc R . . C8' C 0.4453(7) -0.1066(7) 0.7592(4) 0.0391(19) Uani 1 1 d . . . H8' H 0.4299 -0.1439 0.7978 0.047 Uiso 1 1 calc R . . C9 C 0.7469(7) -0.0021(7) 0.7968(4) 0.041(2) Uani 1 1 d . . . H9 H 0.8107 -0.0553 0.7930 0.050 Uiso 1 1 calc R . . C9' C 0.5111(8) -0.1562(6) 0.7126(4) 0.042(2) Uani 1 1 d . . . H9' H 0.5407 -0.2272 0.7195 0.050 Uiso 1 1 calc R . . C10' C 0.5339(7) -0.1032(6) 0.6562(4) 0.0381(18) Uani 1 1 d . . . H10' H 0.5791 -0.1377 0.6244 0.046 Uiso 1 1 calc R . . C10 C 0.7460(7) 0.0939(7) 0.7680(4) 0.042(2) Uani 1 1 d . . . H10 H 0.8087 0.1058 0.7438 0.050 Uiso 1 1 calc R . . C11 C 0.6549(6) 0.1730(6) 0.7741(4) 0.0332(17) Uani 1 1 d . . . H11 H 0.6558 0.2394 0.7554 0.040 Uiso 1 1 calc R . . C11' C 0.4906(7) 0.0009(6) 0.6458(4) 0.0318(16) Uani 1 1 d . . . H11' H 0.5047 0.0373 0.6067 0.038 Uiso 1 1 calc R . . C12 C 0.4826(6) 0.3717(6) 0.8003(4) 0.0303(16) Uani 1 1 d . . . C12' C 0.4647(6) 0.2476(6) 0.6386(3) 0.0292(16) Uani 1 1 d . . . C13' C 0.4267(8) 0.3457(7) 0.6102(4) 0.044(2) Uani 1 1 d . . . H13' H 0.3502 0.3760 0.6105 0.053 Uiso 1 1 calc R . . C13 C 0.4412(9) 0.4444(7) 0.7511(5) 0.055(3) Uani 1 1 d . . . H13 H 0.3871 0.4340 0.7254 0.067 Uiso 1 1 calc R . . C14 C 0.4791(14) 0.5318(9) 0.7399(8) 0.099(6) Uani 1 1 d . . . H14 H 0.4515 0.5807 0.7058 0.119 Uiso 1 1 calc R . . C14' C 0.5009(9) 0.4001(8) 0.5810(5) 0.051(2) Uani 1 1 d . . . H14' H 0.4746 0.4672 0.5616 0.062 Uiso 1 1 calc R . . C15' C 0.6123(8) 0.3565(8) 0.5803(4) 0.048(2) Uani 1 1 d . . . H15' H 0.6631 0.3934 0.5610 0.058 Uiso 1 1 calc R . . C15 C 0.5553(14) 0.5492(9) 0.7769(8) 0.099(6) Uani 1 1 d . . . H15 H 0.5809 0.6094 0.7682 0.119 Uiso 1 1 calc R . . C16' C 0.6481(7) 0.2601(8) 0.6075(4) 0.044(2) Uani 1 1 d . . . H16' H 0.7246 0.2297 0.6063 0.053 Uiso 1 1 calc R . . C16 C 0.5958(10) 0.4782(7) 0.8275(5) 0.053(3) Uani 1 1 d . . . H16 H 0.6469 0.4912 0.8543 0.063 Uiso 1 1 calc R . . C17 C 0.5608(7) 0.3886(6) 0.8385(4) 0.0339(17) Uani 1 1 d . . . H17 H 0.5901 0.3389 0.8718 0.041 Uiso 1 1 calc R . . C17' C 0.5765(7) 0.2047(7) 0.6369(4) 0.0369(18) Uani 1 1 d . . . H17' H 0.6040 0.1375 0.6559 0.044 Uiso 1 1 calc R . . C18 C 0.2534(7) 0.4101(6) 0.9572(4) 0.0317(16) Uani 1 1 d . . . C18' C 0.0652(6) 0.1723(6) 0.5726(4) 0.0302(16) Uani 1 1 d . . . C19' C 0.0107(8) 0.2725(8) 0.5740(5) 0.051(2) Uani 1 1 d . . . H19' H 0.0319 0.3110 0.6029 0.061 Uiso 1 1 calc R . . C19 C 0.3369(8) 0.4615(7) 0.9515(5) 0.046(2) Uani 1 1 d . . . H19 H 0.3976 0.4426 0.9229 0.055 Uiso 1 1 calc R . . C20 C 0.3318(8) 0.5406(7) 0.9876(5) 0.051(2) Uani 1 1 d . . . H20 H 0.3893 0.5752 0.9838 0.061 Uiso 1 1 calc R . . C20' C -0.0734(8) 0.3179(7) 0.5348(5) 0.049(2) Uani 1 1 d . . . H20' H -0.1072 0.3879 0.5351 0.059 Uiso 1 1 calc R . . C21 C 0.2428(8) 0.5690(7) 1.0293(4) 0.044(2) Uani 1 1 d . . . H21 H 0.2382 0.6240 1.0531 0.052 Uiso 1 1 calc R . . C21' C -0.1089(7) 0.2616(7) 0.4949(4) 0.0403(19) Uani 1 1 d . . . H21' H -0.1712 0.2915 0.4704 0.048 Uiso 1 1 calc R . . C22' C -0.0552(10) 0.1637(9) 0.4906(6) 0.066(3) Uani 1 1 d . . . H22' H -0.0772 0.1266 0.4611 0.079 Uiso 1 1 calc R . . C22 C 0.1619(8) 0.5171(7) 1.0355(5) 0.049(2) Uani 1 1 d . . . H22 H 0.1023 0.5353 1.0649 0.058 Uiso 1 1 calc R . . C23 C 0.1652(7) 0.4374(7) 0.9996(4) 0.0401(19) Uani 1 1 d . . . H23 H 0.1080 0.4025 1.0041 0.048 Uiso 1 1 calc R . . C23' C 0.0324(10) 0.1174(8) 0.5293(6) 0.062(3) Uani 1 1 d . . . H23' H 0.0697 0.0488 0.5263 0.074 Uiso 1 1 calc R . . C24' C 0.2429(6) -0.0051(6) 0.6013(4) 0.0302(16) Uani 1 1 d . . . C24 C 0.1703(6) 0.2347(6) 0.9459(3) 0.0278(15) Uani 1 1 d . . . C25' C 0.2973(7) -0.0113(6) 0.5429(4) 0.0353(17) Uani 1 1 d . . . H25' H 0.2965 0.0487 0.5153 0.042 Uiso 1 1 calc R . . C25 C 0.2106(7) 0.1610(7) 0.9949(4) 0.0385(19) Uani 1 1 d . . . H25 H 0.2846 0.1494 1.0065 0.046 Uiso 1 1 calc R . . C26' C 0.3529(7) -0.1041(7) 0.5246(4) 0.043(2) Uani 1 1 d . . . H26' H 0.3901 -0.1071 0.4845 0.052 Uiso 1 1 calc R . . C26 C 0.1426(7) 0.1054(7) 1.0264(4) 0.041(2) Uani 1 1 d . . . H26 H 0.1702 0.0545 1.0595 0.050 Uiso 1 1 calc R . . C27' C 0.3552(8) -0.1913(7) 0.5632(5) 0.046(2) Uani 1 1 d . . . H27' H 0.3934 -0.2548 0.5501 0.055 Uiso 1 1 calc R . . C27 C 0.0343(7) 0.1227(7) 1.0105(4) 0.0379(19) Uani 1 1 d . . . H27 H -0.0125 0.0846 1.0333 0.046 Uiso 1 1 calc R . . C28 C -0.0061(6) 0.1954(6) 0.9615(4) 0.0342(17) Uani 1 1 d . . . H28 H -0.0803 0.2066 0.9504 0.041 Uiso 1 1 calc R . . C28' C 0.3003(8) -0.1863(7) 0.6226(5) 0.046(2) Uani 1 1 d . . . H28' H 0.3013 -0.2467 0.6498 0.055 Uiso 1 1 calc R . . C29 C 0.0617(6) 0.2521(6) 0.9286(4) 0.0323(17) Uani 1 1 d . . . H29 H 0.0345 0.3020 0.8949 0.039 Uiso 1 1 calc R . . C29' C 0.2447(7) -0.0937(6) 0.6415(4) 0.0354(17) Uani 1 1 d . . . H29' H 0.2079 -0.0905 0.6818 0.042 Uiso 1 1 calc R . . C30 C 0.2011(11) 0.369(2) 0.1891(8) 0.146(11) Uani 1 1 d . . . H30A H 0.1547 0.4300 0.1662 0.175 Uiso 1 1 calc R . . H30B H 0.2309 0.3881 0.2262 0.175 Uiso 1 1 calc R . . C31 C 0.8581(15) 0.8646(14) 0.6479(9) 0.106(5) Uani 1 1 d . . . H31A H 0.8741 0.8189 0.6143 0.127 Uiso 1 1 calc R . . H31B H 0.7978 0.8461 0.6754 0.127 Uiso 1 1 calc R . . N1' N 0.1287(5) 0.0946(5) 0.6979(3) 0.0318(14) Uani 1 1 d . . . N1 N 0.2164(5) 0.3600(5) 0.8359(3) 0.0294(13) Uani 1 1 d . . . O1' O 0.1276(4) 0.2731(4) 0.7320(2) 0.0311(11) Uani 1 1 d . . . O1 O 0.0129(6) 0.4709(6) 0.8326(3) 0.060(2) Uani 1 1 d . . . O2' O 0.1151(4) 0.1313(4) 0.8127(2) 0.0340(12) Uani 1 1 d . . . O2 O 0.1536(5) 0.4787(4) 0.7408(3) 0.0379(13) Uani 1 1 d . . . O3 O 0.1719(10) 0.5509(5) 0.8401(4) 0.084(3) Uani 1 1 d . . . O3' O -0.0433(4) 0.2092(4) 0.7405(3) 0.0360(12) Uani 1 1 d . . . F1 F 0.2133(8) 0.4908(5) 0.3973(3) 0.100(3) Uani 1 1 d . . . F2 F 0.4045(7) 0.3842(8) 0.4345(5) 0.106(3) Uani 1 1 d . . . F3 F 0.3257(7) 0.2254(5) 0.4665(3) 0.088(3) Uani 1 1 d . . . F4 F 0.1331(7) 0.3277(9) 0.4275(4) 0.115(4) Uani 1 1 d . . . F5 F 0.3033(6) 0.3184(5) 0.3507(3) 0.0718(19) Uani 1 1 d . . . F6 F 0.2289(6) 0.3969(5) 0.5123(3) 0.0705(19) Uani 1 1 d . . . F7 F 0.6158(5) 0.0657(4) -0.0283(3) 0.0554(14) Uani 1 1 d . . . F8 F 0.5970(5) 0.2609(4) -0.0223(2) 0.0463(12) Uani 1 1 d . . . F9 F 0.4699(5) 0.1627(5) 0.0499(3) 0.0627(16) Uani 1 1 d . . . F10 F 0.6464(4) 0.0258(4) 0.0942(2) 0.0453(12) Uani 1 1 d . . . F11 F 0.7734(5) 0.1264(5) 0.0221(3) 0.0676(18) Uani 1 1 d . . . F12 F 0.6260(6) 0.2225(5) 0.1009(3) 0.0684(18) Uani 1 1 d . . . P1' P 0.36413(15) 0.18513(14) 0.67932(8) 0.0255(4) Uani 1 1 d . . . P1 P 0.43845(15) 0.25475(14) 0.81313(8) 0.0249(4) Uani 1 1 d . . . P2' P 0.17190(15) 0.11414(14) 0.62701(8) 0.0269(4) Uani 1 1 d . . . P2 P 0.25382(15) 0.31466(14) 0.90677(9) 0.0261(4) Uani 1 1 d . . . P3 P 0.12820(18) 0.46655(15) 0.81435(10) 0.0357(5) Uani 1 1 d . . . P3' P 0.08476(15) 0.17892(15) 0.74367(9) 0.0279(4) Uani 1 1 d . . . Cl1 Cl 0.9726(3) 0.8409(4) 0.6921(2) 0.1105(11) Uani 1 1 d . . . Cl2 Cl 0.8119(3) 0.9842(4) 0.6137(2) 0.1105(11) Uani 1 1 d . . . Cl3 Cl 0.3082(7) 0.3031(5) 0.1385(6) 0.244(4) Uani 1 1 d . . . Cl4 Cl 0.1246(7) 0.2660(5) 0.2114(6) 0.244(4) Uani 1 1 d . . . Pd1 Pd 0.28456(4) 0.26509(4) 0.76319(2) 0.02398(14) Uani 1 1 d . . . Sb1 Sb 0.26754(5) 0.35878(4) 0.43109(3) 0.04509(17) Uani 1 1 d . . . Sb2 Sb 0.62225(4) 0.14314(4) 0.03608(2) 0.03348(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.025(4) 0.027(4) 0.030(4) -0.003(3) -0.002(3) -0.006(3) C1' 0.030(4) 0.032(4) 0.030(4) -0.003(3) 0.002(3) -0.013(3) C2' 0.054(4) 0.051(4) 0.046(4) 0.011(3) -0.006(3) -0.017(3) C2 0.046(5) 0.056(6) 0.042(5) 0.000(4) -0.009(4) 0.002(5) C3 0.070(8) 0.127(13) 0.046(6) 0.016(7) -0.008(5) 0.018(8) C3' 0.054(4) 0.051(4) 0.046(4) 0.011(3) -0.006(3) -0.017(3) C4 0.71(9) 0.18(3) 0.15(2) 0.062(19) -0.22(4) -0.29(4) C4' 0.038(3) 0.048(4) 0.061(4) -0.008(3) 0.000(3) -0.008(3) C5' 0.038(3) 0.048(4) 0.061(4) -0.008(3) 0.000(3) -0.008(3) C5 0.17(2) 0.080(14) 0.51(6) 0.11(2) -0.20(3) -0.061(16) C6' 0.026(4) 0.033(4) 0.028(4) -0.004(3) -0.007(3) -0.004(3) C6 0.028(4) 0.030(4) 0.022(3) -0.007(3) -0.001(3) -0.007(3) C7 0.027(4) 0.030(4) 0.043(4) -0.007(3) -0.001(3) -0.006(3) C7' 0.030(4) 0.039(4) 0.029(4) -0.008(3) 0.001(3) -0.009(3) C8 0.033(4) 0.033(4) 0.047(5) -0.004(4) -0.006(4) -0.004(4) C8' 0.042(5) 0.037(4) 0.038(4) -0.002(4) -0.003(4) -0.008(4) C9 0.025(4) 0.047(5) 0.054(5) -0.019(4) -0.003(4) -0.004(4) C9' 0.051(5) 0.024(4) 0.047(5) -0.004(4) -0.008(4) -0.003(4) C10' 0.036(4) 0.036(4) 0.041(4) -0.010(4) -0.004(3) -0.004(4) C10 0.031(4) 0.054(5) 0.045(5) -0.015(4) 0.005(4) -0.014(4) C11 0.030(4) 0.040(4) 0.036(4) -0.013(4) 0.002(3) -0.017(3) C11' 0.034(4) 0.032(4) 0.029(4) -0.004(3) 0.000(3) -0.007(3) C12 0.027(4) 0.030(4) 0.035(4) -0.004(3) 0.002(3) -0.011(3) C12' 0.025(4) 0.034(4) 0.031(4) -0.006(3) -0.001(3) -0.011(3) C13' 0.036(5) 0.041(5) 0.054(5) 0.003(4) 0.002(4) -0.011(4) C13 0.061(6) 0.041(5) 0.070(7) 0.019(5) -0.037(5) -0.026(5) C14 0.120(12) 0.049(7) 0.139(13) 0.044(8) -0.091(11) -0.045(8) C14' 0.053(6) 0.048(5) 0.058(6) 0.003(5) -0.001(5) -0.025(5) C15' 0.047(5) 0.060(6) 0.047(5) -0.016(5) 0.012(4) -0.032(5) C15 0.130(13) 0.051(7) 0.134(12) 0.041(8) -0.086(11) -0.060(8) C16' 0.034(5) 0.060(6) 0.046(5) -0.021(5) 0.007(4) -0.018(4) C16 0.074(7) 0.040(5) 0.056(6) 0.004(4) -0.023(5) -0.035(5) C17 0.037(4) 0.032(4) 0.035(4) -0.002(3) -0.003(3) -0.013(3) C17' 0.029(4) 0.042(5) 0.043(4) -0.018(4) 0.003(3) -0.010(4) C18 0.033(4) 0.029(4) 0.034(4) -0.006(3) -0.005(3) -0.006(3) C18' 0.028(4) 0.031(4) 0.030(4) -0.003(3) -0.002(3) -0.005(3) C19' 0.044(5) 0.050(6) 0.060(6) -0.021(5) -0.020(4) -0.004(4) C19 0.047(5) 0.045(5) 0.054(5) -0.024(4) 0.013(4) -0.021(4) C20 0.049(6) 0.043(5) 0.069(6) -0.022(5) 0.001(5) -0.021(4) C20' 0.042(5) 0.038(5) 0.060(6) 0.000(4) -0.014(4) 0.005(4) C21 0.050(5) 0.038(5) 0.045(5) -0.018(4) -0.007(4) -0.006(4) C21' 0.027(4) 0.051(5) 0.041(4) -0.001(4) -0.013(3) -0.004(4) C22' 0.064(7) 0.058(7) 0.079(8) -0.019(6) -0.038(6) -0.005(6) C22 0.044(5) 0.049(5) 0.051(5) -0.021(5) 0.007(4) -0.002(4) C23 0.035(5) 0.047(5) 0.042(5) -0.018(4) 0.002(4) -0.010(4) C23' 0.063(7) 0.041(5) 0.082(8) -0.011(5) -0.040(6) -0.004(5) C24' 0.029(4) 0.029(4) 0.034(4) -0.003(3) -0.005(3) -0.008(3) C24 0.027(4) 0.029(4) 0.030(4) -0.006(3) -0.002(3) -0.011(3) C25' 0.038(4) 0.034(4) 0.035(4) -0.006(3) -0.001(3) -0.010(4) C25 0.033(4) 0.047(5) 0.038(4) -0.002(4) -0.005(3) -0.014(4) C26' 0.039(5) 0.052(5) 0.042(5) -0.019(4) 0.001(4) -0.013(4) C26 0.037(5) 0.046(5) 0.041(4) 0.003(4) -0.001(4) -0.014(4) C27' 0.041(5) 0.038(5) 0.058(6) -0.022(4) -0.002(4) -0.003(4) C27 0.039(5) 0.041(5) 0.040(4) -0.005(4) 0.002(4) -0.020(4) C28 0.025(4) 0.040(4) 0.037(4) -0.002(4) -0.002(3) -0.009(3) C28' 0.051(5) 0.034(4) 0.052(5) -0.007(4) -0.009(4) -0.007(4) C29 0.033(4) 0.028(4) 0.036(4) -0.003(3) -0.001(3) -0.005(3) C29' 0.036(4) 0.035(4) 0.037(4) -0.007(3) -0.007(3) -0.010(4) C30 0.038(7) 0.30(3) 0.091(10) 0.073(14) -0.028(7) -0.068(12) C31 0.092(12) 0.120(14) 0.112(12) -0.006(10) -0.044(10) -0.029(10) N1' 0.036(4) 0.031(3) 0.031(3) -0.006(3) -0.001(3) -0.011(3) N1 0.029(3) 0.029(3) 0.031(3) -0.009(3) 0.001(3) -0.007(3) O1' 0.026(3) 0.030(3) 0.038(3) -0.008(2) -0.002(2) -0.006(2) O1 0.045(4) 0.064(4) 0.046(4) 0.010(3) 0.013(3) 0.019(3) O2' 0.035(3) 0.040(3) 0.028(3) -0.006(2) -0.002(2) -0.011(2) O2 0.039(3) 0.036(3) 0.034(3) 0.000(2) -0.001(2) -0.002(3) O3 0.169(10) 0.033(4) 0.055(5) -0.006(3) -0.027(5) -0.027(5) O3' 0.029(3) 0.039(3) 0.041(3) -0.007(2) -0.001(2) -0.009(2) F1 0.161(8) 0.040(3) 0.071(4) 0.006(3) -0.021(5) 0.027(4) F2 0.082(6) 0.123(7) 0.118(7) 0.011(6) -0.005(5) -0.045(5) F3 0.146(7) 0.040(3) 0.055(4) -0.001(3) 0.030(4) 0.011(4) F4 0.072(5) 0.200(11) 0.096(6) -0.070(7) 0.020(4) -0.058(6) F5 0.099(5) 0.054(4) 0.044(3) -0.004(3) 0.019(3) 0.010(3) F6 0.094(5) 0.059(4) 0.046(3) -0.015(3) -0.013(3) 0.013(3) F7 0.076(4) 0.048(3) 0.045(3) -0.007(2) -0.014(3) -0.017(3) F8 0.056(3) 0.045(3) 0.043(3) 0.002(2) -0.014(2) -0.023(2) F9 0.038(3) 0.059(4) 0.086(4) 0.006(3) 0.005(3) -0.011(3) F10 0.045(3) 0.050(3) 0.041(3) 0.007(2) -0.005(2) -0.015(2) F11 0.039(3) 0.085(5) 0.077(4) 0.019(3) -0.002(3) -0.025(3) F12 0.113(6) 0.063(4) 0.039(3) -0.006(3) -0.010(3) -0.037(4) P1' 0.0243(9) 0.0266(9) 0.0260(8) -0.0056(7) 0.0008(7) -0.0062(7) P1 0.0241(9) 0.0254(9) 0.0269(9) -0.0049(7) -0.0006(7) -0.0080(7) P2' 0.0274(9) 0.0277(9) 0.0265(9) -0.0044(7) -0.0017(7) -0.0074(7) P2 0.0256(9) 0.0257(9) 0.0283(9) -0.0062(7) 0.0000(7) -0.0071(7) P3 0.0406(11) 0.0281(10) 0.0335(10) -0.0042(8) -0.0001(8) 0.0010(9) P3' 0.0248(9) 0.0311(10) 0.0287(9) -0.0049(8) -0.0007(7) -0.0073(8) Cl1 0.0847(17) 0.140(3) 0.0964(18) -0.0519(19) -0.0183(14) 0.0173(17) Cl2 0.0847(17) 0.140(3) 0.0964(18) -0.0519(19) -0.0183(14) 0.0173(17) Cl3 0.153(4) 0.101(3) 0.465(12) -0.029(5) 0.074(6) -0.030(3) Cl4 0.153(4) 0.101(3) 0.465(12) -0.029(5) 0.074(6) -0.030(3) Pd1 0.0222(3) 0.0247(3) 0.0258(3) -0.0055(2) -0.00070(19) -0.0057(2) Sb1 0.0524(4) 0.0316(3) 0.0447(3) -0.0044(2) 0.0041(3) 0.0010(3) Sb2 0.0309(3) 0.0416(3) 0.0310(3) 0.0015(2) -0.0052(2) -0.0161(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 C1 P2 1.813(7) . ? C1 P1 1.840(7) . ? C1' P2' 1.826(7) . ? C1' P1' 1.832(8) . ? C2' O2' 1.434(11) . ? C2' C3' 1.448(14) . ? C2 O2 1.439(11) . ? C2 C3 1.481(15) . ? C4 O3 1.12(2) . ? C4 C5 1.34(3) . ? C4' O3' 1.463(11) . ? C4' C5' 1.499(14) . ? C6' C7' 1.395(11) . ? C6' C11' 1.409(11) . ? C6' P1' 1.794(8) . ? C6 C11 1.401(10) . ? C6 C7 1.401(11) . ? C6 P1 1.806(7) . ? C7 C8 1.387(11) . ? C7' C8' 1.389(12) . ? C8 C9 1.380(12) . ? C8' C9' 1.387(13) . ? C9 C10 1.379(13) . ? C9' C10' 1.380(13) . ? C10' C11' 1.393(12) . ? C10 C11 1.383(12) . ? C12 C13 1.391(12) . ? C12 C17 1.398(12) . ? C12 P1 1.804(8) . ? C12' C17' 1.385(11) . ? C12' C13' 1.389(12) . ? C12' P1' 1.813(7) . ? C13' C14' 1.400(13) . ? C13 C14 1.382(14) . ? C14 C15 1.365(17) . ? C14' C15' 1.382(14) . ? C15' C16' 1.357(14) . ? C15 C16 1.398(15) . ? C16' C17' 1.386(12) . ? C16 C17 1.391(11) . ? C18 C23 1.391(11) . ? C18 C19 1.391(12) . ? C18 P2 1.794(8) . ? C18' C19' 1.379(13) . ? C18' C23' 1.403(13) . ? C18' P2' 1.804(8) . ? C19' C20' 1.372(13) . ? C19 C20 1.392(13) . ? C20 C21 1.391(14) . ? C20' C21' 1.379(14) . ? C21 C22 1.366(14) . ? C21' C22' 1.358(15) . ? C22' C23' 1.399(14) . ? C22 C23 1.402(13) . ? C24' C25' 1.384(11) . ? C24' C29' 1.395(11) . ? C24' P2' 1.791(8) . ? C24 C25 1.393(11) . ? C24 C29 1.395(11) . ? C24 P2 1.794(7) . ? C25' C26' 1.382(12) . ? C25 C26 1.369(12) . ? C26' C27' 1.361(14) . ? C26 C27 1.382(13) . ? C27' C28' 1.405(14) . ? C27 C28 1.385(12) . ? C28 C29 1.390(11) . ? C28' C29' 1.384(12) . ? C30 Cl3 1.80(2) . ? C30 Cl4 1.89(2) . ? C31 Cl2 1.690(18) . ? C31 Cl1 1.719(15) . ? N1' P3' 1.578(7) . ? N1' P2' 1.590(7) . ? N1 P2 1.622(7) . ? N1 P3 1.640(7) . ? N1 Pd1 2.148(6) . ? O1' P3' 1.502(5) . ? O1' Pd1 2.100(5) . ? O1 P3 1.464(7) . ? O2' P3' 1.573(5) . ? O2 P3 1.581(6) . ? O3 P3 1.565(8) . ? O3' P3' 1.566(6) . ? F1 Sb1 1.845(6) . ? F2 Sb1 1.846(8) . ? F3 Sb1 1.879(6) . ? F4 Sb1 1.849(8) . ? F5 Sb1 1.865(6) . ? F6 Sb1 1.874(6) . ? F7 Sb2 1.857(5) . ? F8 Sb2 1.891(5) . ? F9 Sb2 1.876(5) . ? F10 Sb2 1.884(5) . ? F11 Sb2 1.865(6) . ? F12 Sb2 1.874(6) . ? P1' Pd1 2.2637(18) . ? P1 Pd1 2.2397(19) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P2 C1 P1 109.6(4) . . ? P2' C1' P1' 117.9(4) . . ? O2' C2' C3' 114.4(8) . . ? O2 C2 C3 109.0(8) . . ? O3 C4 C5 142(4) . . ? O3' C4' C5' 109.0(8) . . ? C7' C6' C11' 119.5(7) . . ? C7' C6' P1' 120.1(6) . . ? C11' C6' P1' 120.1(6) . . ? C11 C6 C7 119.4(7) . . ? C11 C6 P1 120.5(6) . . ? C7 C6 P1 120.2(6) . . ? C8 C7 C6 120.2(7) . . ? C8' C7' C6' 119.7(7) . . ? C9 C8 C7 119.8(8) . . ? C9' C8' C7' 120.4(8) . . ? C10 C9 C8 120.4(8) . . ? C10' C9' C8' 120.5(8) . . ? C9' C10' C11' 119.9(8) . . ? C9 C10 C11 120.7(8) . . ? C10 C11 C6 119.5(8) . . ? C10' C11' C6' 119.9(7) . . ? C13 C12 C17 119.7(7) . . ? C13 C12 P1 120.0(6) . . ? C17 C12 P1 120.3(6) . . ? C17' C12' C13' 119.0(7) . . ? C17' C12' P1' 123.6(6) . . ? C13' C12' P1' 117.4(6) . . ? C12' C13' C14' 120.1(8) . . ? C14 C13 C12 119.7(9) . . ? C15 C14 C13 121.2(11) . . ? C15' C14' C13' 120.2(9) . . ? C16' C15' C14' 119.0(8) . . ? C14 C15 C16 120.0(10) . . ? C15' C16' C17' 122.1(8) . . ? C17 C16 C15 119.6(9) . . ? C16 C17 C12 119.9(8) . . ? C12' C17' C16' 119.7(9) . . ? C23 C18 C19 119.7(8) . . ? C23 C18 P2 119.6(6) . . ? C19 C18 P2 120.6(6) . . ? C19' C18' C23' 117.9(8) . . ? C19' C18' P2' 120.3(6) . . ? C23' C18' P2' 121.8(7) . . ? C20' C19' C18' 121.7(9) . . ? C18 C19 C20 120.2(8) . . ? C21 C20 C19 120.1(9) . . ? C19' C20' C21' 119.8(9) . . ? C22 C21 C20 119.4(8) . . ? C22' C21' C20' 120.3(8) . . ? C21' C22' C23' 120.2(10) . . ? C21 C22 C23 121.4(8) . . ? C18 C23 C22 119.1(8) . . ? C22' C23' C18' 120.0(10) . . ? C25' C24' C29' 119.2(7) . . ? C25' C24' P2' 121.6(6) . . ? C29' C24' P2' 119.1(6) . . ? C25 C24 C29 120.6(7) . . ? C25 C24 P2 121.0(6) . . ? C29 C24 P2 118.3(6) . . ? C26' C25' C24' 120.5(8) . . ? C26 C25 C24 119.5(8) . . ? C27' C26' C25' 121.1(8) . . ? C25 C26 C27 120.7(8) . . ? C26' C27' C28' 119.1(8) . . ? C26 C27 C28 120.1(8) . . ? C27 C28 C29 120.2(8) . . ? C29' C28' C27' 120.3(9) . . ? C28 C29 C24 118.9(7) . . ? C28' C29' C24' 119.8(8) . . ? Cl3 C30 Cl4 99.1(14) . . ? Cl2 C31 Cl1 117.3(11) . . ? P3' N1' P2' 125.3(4) . . ? P2 N1 P3 127.4(4) . . ? P2 N1 Pd1 115.7(3) . . ? P3 N1 Pd1 116.8(3) . . ? P3' O1' Pd1 117.6(3) . . ? C2' O2' P3' 124.8(6) . . ? C2 O2 P3 120.5(5) . . ? C4 O3 P3 151(2) . . ? C4' O3' P3' 119.8(5) . . ? C6' P1' C12' 108.6(4) . . ? C6' P1' C1' 105.5(4) . . ? C12' P1' C1' 101.4(3) . . ? C6' P1' Pd1 117.2(2) . . ? C12' P1' Pd1 111.1(3) . . ? C1' P1' Pd1 111.7(3) . . ? C12 P1 C6 106.2(4) . . ? C12 P1 C1 107.0(3) . . ? C6 P1 C1 103.7(3) . . ? C12 P1 Pd1 111.9(3) . . ? C6 P1 Pd1 124.2(2) . . ? C1 P1 Pd1 102.3(2) . . ? N1' P2' C24' 108.4(4) . . ? N1' P2' C18' 114.3(4) . . ? C24' P2' C18' 107.8(4) . . ? N1' P2' C1' 113.2(3) . . ? C24' P2' C1' 108.0(4) . . ? C18' P2' C1' 104.9(4) . . ? N1 P2 C24 113.1(3) . . ? N1 P2 C18 113.7(3) . . ? C24 P2 C18 107.1(4) . . ? N1 P2 C1 104.7(3) . . ? C24 P2 C1 108.7(3) . . ? C18 P2 C1 109.5(4) . . ? O1 P3 O3 113.0(6) . . ? O1 P3 O2 114.5(4) . . ? O3 P3 O2 105.1(4) . . ? O1 P3 N1 116.3(4) . . ? O3 P3 N1 105.4(4) . . ? O2 P3 N1 101.1(3) . . ? O1' P3' O3' 109.0(3) . . ? O1' P3' O2' 106.5(3) . . ? O3' P3' O2' 108.3(3) . . ? O1' P3' N1' 117.4(3) . . ? O3' P3' N1' 107.1(3) . . ? O2' P3' N1' 108.3(3) . . ? O1' Pd1 N1 91.4(2) . . ? O1' Pd1 P1 170.13(15) . . ? N1 Pd1 P1 81.02(18) . . ? O1' Pd1 P1' 90.95(15) . . ? N1 Pd1 P1' 171.61(18) . . ? P1 Pd1 P1' 97.44(7) . . ? F1 Sb1 F2 90.0(5) . . ? F1 Sb1 F4 92.1(5) . . ? F2 Sb1 F4 177.6(5) . . ? F1 Sb1 F5 90.8(3) . . ? F2 Sb1 F5 90.3(4) . . ? F4 Sb1 F5 88.6(4) . . ? F1 Sb1 F6 90.0(3) . . ? F2 Sb1 F6 91.2(4) . . ? F4 Sb1 F6 89.9(3) . . ? F5 Sb1 F6 178.4(3) . . ? F1 Sb1 F3 178.5(4) . . ? F2 Sb1 F3 88.7(4) . . ? F4 Sb1 F3 89.2(5) . . ? F5 Sb1 F3 89.8(3) . . ? F6 Sb1 F3 89.4(3) . . ? F7 Sb2 F11 91.4(3) . . ? F7 Sb2 F12 178.9(3) . . ? F11 Sb2 F12 89.6(3) . . ? F7 Sb2 F9 89.2(3) . . ? F11 Sb2 F9 178.9(3) . . ? F12 Sb2 F9 89.9(3) . . ? F7 Sb2 F10 90.1(2) . . ? F11 Sb2 F10 90.1(2) . . ? F12 Sb2 F10 90.3(2) . . ? F9 Sb2 F10 90.8(2) . . ? F7 Sb2 F8 89.8(2) . . ? F11 Sb2 F8 90.2(3) . . ? F12 Sb2 F8 89.8(2) . . ? F9 Sb2 F8 88.8(3) . . ? F10 Sb2 F8 179.6(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 C6 C7 C8 -1.3(12) . . . . ? P1 C6 C7 C8 177.7(6) . . . . ? C11' C6' C7' C8' 2.2(12) . . . . ? P1' C6' C7' C8' 176.5(6) . . . . ? C6 C7 C8 C9 0.4(13) . . . . ? C6' C7' C8' C9' -0.8(13) . . . . ? C7 C8 C9 C10 -0.5(14) . . . . ? C7' C8' C9' C10' -0.3(14) . . . . ? C8' C9' C10' C11' -0.1(14) . . . . ? C8 C9 C10 C11 1.5(14) . . . . ? C9 C10 C11 C6 -2.4(13) . . . . ? C7 C6 C11 C10 2.2(12) . . . . ? P1 C6 C11 C10 -176.8(6) . . . . ? C9' C10' C11' C6' 1.5(13) . . . . ? C7' C6' C11' C10' -2.6(12) . . . . ? P1' C6' C11' C10' -176.9(6) . . . . ? C17' C12' C13' C14' -0.7(13) . . . . ? P1' C12' C13' C14' 176.5(8) . . . . ? C17 C12 C13 C14 1.0(18) . . . . ? P1 C12 C13 C14 -177.1(12) . . . . ? C12 C13 C14 C15 -1(3) . . . . ? C12' C13' C14' C15' 0.1(15) . . . . ? C13' C14' C15' C16' 0.8(15) . . . . ? C13 C14 C15 C16 -1(3) . . . . ? C14' C15' C16' C17' -1.1(14) . . . . ? C14 C15 C16 C17 2(3) . . . . ? C15 C16 C17 C12 -2.4(17) . . . . ? C13 C12 C17 C16 0.8(13) . . . . ? P1 C12 C17 C16 178.8(8) . . . . ? C13' C12' C17' C16' 0.4(12) . . . . ? P1' C12' C17' C16' -176.5(6) . . . . ? C15' C16' C17' C12' 0.5(13) . . . . ? C23' C18' C19' C20' 0.3(15) . . . . ? P2' C18' C19' C20' -177.7(8) . . . . ? C23 C18 C19 C20 -0.7(15) . . . . ? P2 C18 C19 C20 175.3(8) . . . . ? C18 C19 C20 C21 -0.4(16) . . . . ? C18' C19' C20' C21' 3.3(16) . . . . ? C19 C20 C21 C22 1.6(16) . . . . ? C19' C20' C21' C22' -5.4(16) . . . . ? C20' C21' C22' C23' 3.9(18) . . . . ? C20 C21 C22 C23 -1.8(15) . . . . ? C19 C18 C23 C22 0.5(14) . . . . ? P2 C18 C23 C22 -175.5(7) . . . . ? C21 C22 C23 C18 0.8(15) . . . . ? C21' C22' C23' C18' 0(2) . . . . ? C19' C18' C23' C22' -1.8(17) . . . . ? P2' C18' C23' C22' 176.1(9) . . . . ? C29' C24' C25' C26' 0.0(12) . . . . ? P2' C24' C25' C26' 179.0(7) . . . . ? C29 C24 C25 C26 0.0(12) . . . . ? P2 C24 C25 C26 176.0(7) . . . . ? C24' C25' C26' C27' 0.2(13) . . . . ? C24 C25 C26 C27 -0.9(14) . . . . ? C25' C26' C27' C28' -0.2(14) . . . . ? C25 C26 C27 C28 1.3(14) . . . . ? C26 C27 C28 C29 -0.8(13) . . . . ? C26' C27' C28' C29' 0.0(14) . . . . ? C27 C28 C29 C24 -0.1(12) . . . . ? C25 C24 C29 C28 0.6(12) . . . . ? P2 C24 C29 C28 -175.6(6) . . . . ? C27' C28' C29' C24' 0.3(13) . . . . ? C25' C24' C29' C28' -0.3(12) . . . . ? P2' C24' C29' C28' -179.3(7) . . . . ? C3' C2' O2' P3' -56.4(11) . . . . ? C3 C2 O2 P3 -176.5(9) . . . . ? C5 C4 O3 P3 -73(10) . . . . ? C5' C4' O3' P3' 119.5(7) . . . . ? C7' C6' P1' C12' 142.0(6) . . . . ? C11' C6' P1' C12' -43.7(7) . . . . ? C7' C6' P1' C1' -110.0(7) . . . . ? C11' C6' P1' C1' 64.3(7) . . . . ? C7' C6' P1' Pd1 15.1(7) . . . . ? C11' C6' P1' Pd1 -170.6(5) . . . . ? C17' C12' P1' C6' -17.8(8) . . . . ? C13' C12' P1' C6' 165.2(7) . . . . ? C17' C12' P1' C1' -128.7(7) . . . . ? C13' C12' P1' C1' 54.3(7) . . . . ? C17' C12' P1' Pd1 112.5(6) . . . . ? C13' C12' P1' Pd1 -64.5(7) . . . . ? P2' C1' P1' C6' 48.7(5) . . . . ? P2' C1' P1' C12' 161.9(4) . . . . ? P2' C1' P1' Pd1 -79.8(4) . . . . ? C13 C12 P1 C6 121.6(8) . . . . ? C17 C12 P1 C6 -56.4(7) . . . . ? C13 C12 P1 C1 -128.1(8) . . . . ? C17 C12 P1 C1 53.9(7) . . . . ? C13 C12 P1 Pd1 -16.8(8) . . . . ? C17 C12 P1 Pd1 165.1(6) . . . . ? C11 C6 P1 C12 -23.9(7) . . . . ? C7 C6 P1 C12 157.1(6) . . . . ? C11 C6 P1 C1 -136.5(6) . . . . ? C7 C6 P1 C1 44.5(7) . . . . ? C11 C6 P1 Pd1 108.0(6) . . . . ? C7 C6 P1 Pd1 -71.0(7) . . . . ? P2 C1 P1 C12 81.0(5) . . . . ? P2 C1 P1 C6 -167.0(4) . . . . ? P2 C1 P1 Pd1 -36.8(4) . . . . ? P3' N1' P2' C24' 166.1(5) . . . . ? P3' N1' P2' C18' -73.7(6) . . . . ? P3' N1' P2' C1' 46.3(6) . . . . ? C25' C24' P2' N1' -174.8(7) . . . . ? C29' C24' P2' N1' 4.2(8) . . . . ? C25' C24' P2' C18' 61.1(7) . . . . ? C29' C24' P2' C18' -120.0(7) . . . . ? C25' C24' P2' C1' -51.8(8) . . . . ? C29' C24' P2' C1' 127.1(6) . . . . ? C19' C18' P2' N1' 71.4(8) . . . . ? C23' C18' P2' N1' -106.4(9) . . . . ? C19' C18' P2' C24' -168.0(7) . . . . ? C23' C18' P2' C24' 14.1(9) . . . . ? C19' C18' P2' C1' -53.1(8) . . . . ? C23' C18' P2' C1' 129.0(8) . . . . ? P1' C1' P2' N1' 37.7(6) . . . . ? P1' C1' P2' C24' -82.3(5) . . . . ? P1' C1' P2' C18' 162.9(4) . . . . ? P3 N1 P2 C24 90.4(5) . . . . ? Pd1 N1 P2 C24 -86.1(4) . . . . ? P3 N1 P2 C18 -31.9(6) . . . . ? Pd1 N1 P2 C18 151.6(4) . . . . ? P3 N1 P2 C1 -151.4(5) . . . . ? Pd1 N1 P2 C1 32.1(4) . . . . ? C25 C24 P2 N1 155.9(6) . . . . ? C29 C24 P2 N1 -28.0(7) . . . . ? C25 C24 P2 C18 -78.1(7) . . . . ? C29 C24 P2 C18 98.0(6) . . . . ? C25 C24 P2 C1 40.2(7) . . . . ? C29 C24 P2 C1 -143.7(6) . . . . ? C23 C18 P2 N1 99.6(7) . . . . ? C19 C18 P2 N1 -76.3(8) . . . . ? C23 C18 P2 C24 -26.0(8) . . . . ? C19 C18 P2 C24 158.1(7) . . . . ? C23 C18 P2 C1 -143.7(7) . . . . ? C19 C18 P2 C1 40.4(8) . . . . ? P1 C1 P2 N1 5.7(5) . . . . ? P1 C1 P2 C24 126.8(4) . . . . ? P1 C1 P2 C18 -116.5(4) . . . . ? C4 O3 P3 O1 -60(5) . . . . ? C4 O3 P3 O2 65(5) . . . . ? C4 O3 P3 N1 172(5) . . . . ? C2 O2 P3 O1 24.8(8) . . . . ? C2 O2 P3 O3 -99.8(8) . . . . ? C2 O2 P3 N1 150.7(7) . . . . ? P2 N1 P3 O1 -69.8(6) . . . . ? Pd1 N1 P3 O1 106.7(5) . . . . ? P2 N1 P3 O3 56.2(6) . . . . ? Pd1 N1 P3 O3 -127.3(5) . . . . ? P2 N1 P3 O2 165.5(5) . . . . ? Pd1 N1 P3 O2 -18.0(4) . . . . ? Pd1 O1' P3' O3' 159.3(3) . . . . ? Pd1 O1' P3' O2' 42.7(4) . . . . ? Pd1 O1' P3' N1' -78.7(4) . . . . ? C4' O3' P3' O1' -45.1(7) . . . . ? C4' O3' P3' O2' 70.3(7) . . . . ? C4' O3' P3' N1' -173.1(6) . . . . ? C2' O2' P3' O1' -162.6(7) . . . . ? C2' O2' P3' O3' 80.4(7) . . . . ? C2' O2' P3' N1' -35.5(7) . . . . ? P2' N1' P3' O1' -26.9(7) . . . . ? P2' N1' P3' O3' 96.0(5) . . . . ? P2' N1' P3' O2' -147.4(5) . . . . ? P3' O1' Pd1 N1 -109.8(3) . . . . ? P3' O1' Pd1 P1 -70.1(10) . . . . ? P3' O1' Pd1 P1' 78.2(3) . . . . ? P2 N1 Pd1 O1' 126.3(4) . . . . ? P3 N1 Pd1 O1' -50.6(4) . . . . ? P2 N1 Pd1 P1 -47.4(3) . . . . ? P3 N1 Pd1 P1 135.8(4) . . . . ? P2 N1 Pd1 P1' -127.3(11) . . . . ? P3 N1 Pd1 P1' 55.8(14) . . . . ? C12 P1 Pd1 O1' -111.7(9) . . . . ? C6 P1 Pd1 O1' 118.7(9) . . . . ? C1 P1 Pd1 O1' 2.5(9) . . . . ? C12 P1 Pd1 N1 -71.4(3) . . . . ? C6 P1 Pd1 N1 159.0(3) . . . . ? C1 P1 Pd1 N1 42.8(3) . . . . ? C12 P1 Pd1 P1' 100.3(3) . . . . ? C6 P1 Pd1 P1' -29.3(3) . . . . ? C1 P1 Pd1 P1' -145.5(2) . . . . ? C6' P1' Pd1 O1' -106.1(3) . . . . ? C12' P1' Pd1 O1' 128.2(3) . . . . ? C1' P1' Pd1 O1' 15.8(3) . . . . ? C6' P1' Pd1 N1 147.5(13) . . . . ? C12' P1' Pd1 N1 21.8(13) . . . . ? C1' P1' Pd1 N1 -90.6(13) . . . . ? C6' P1' Pd1 P1 68.7(3) . . . . ? C12' P1' Pd1 P1 -57.0(3) . . . . ? C1' P1' Pd1 P1 -169.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.861 _diffrn_reflns_theta_full 70.03 _diffrn_measured_fraction_theta_full 0.861 _refine_diff_density_max 3.170 _refine_diff_density_min -2.479 _refine_diff_density_rms 0.155 #===END