# Electronic Supplementary Material (ESI) for Metallomics # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Metallomics _journal_coden_cambridge 1400 _journal_year ? _journal_volume ? _journal_page_first ? _publ_requested_category FM _publ_contact_author_email rpnchemist@gmail.com _publ_contact_author_name 'R. Prabhakaran' loop_ _publ_author_name 'P. Kalaivani' 'R. Prabhakaran' 'F. Dallemer' K.Natarajan data_pp19-abs _database_code_depnum_ccdc_archive 'CCDC 842069' #TrackingRef '[Pd(DeaSal -mtsc)(PPh3)].doc' _audit_creation_date 2010-05-05T10:10:40-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H33 N4 O1 P1 Pd1 S1' _chemical_formula_sum 'C31 H33 N4 O P Pd S' _chemical_formula_weight 647.04 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.6590(2) _cell_length_b 11.2079(3) _cell_length_c 27.4126(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2967.61(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 18457 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 28.73 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.78 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.892 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'Omega + Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_reflns_av_R_equivalents 0.0769 _diffrn_reflns_av_unetI/netI 0.1803 _diffrn_reflns_number 18457 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.58 _diffrn_reflns_theta_max 28.73 _diffrn_reflns_theta_full 28.73 _diffrn_measured_fraction_theta_full 0.971 _diffrn_measured_fraction_theta_max 0.971 _reflns_number_total 7345 _reflns_number_gt 3915 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7345 _refine_ls_number_parameters 372 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1336 _refine_ls_R_factor_gt 0.0484 _refine_ls_wR_factor_ref 0.0842 _refine_ls_wR_factor_gt 0.0649 _refine_ls_goodness_of_fit_ref 0.859 _refine_ls_restrained_S_all 0.857 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(3) _refine_diff_density_max 0.493 _refine_diff_density_min -0.652 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.9564(5) 0.3597(4) 0.43233(15) 0.0331(12) Uani 1 1 d . . . C2 C 0.8967(5) 0.4664(4) 0.41840(17) 0.0415(13) Uani 1 1 d . . . H2 H 0.9056 0.4923 0.3863 0.05 Uiso 1 1 calc R . . C3 C 0.8231(5) 0.5359(5) 0.45169(19) 0.0513(15) Uani 1 1 d . . . H3 H 0.7841 0.6079 0.442 0.062 Uiso 1 1 calc R . . C4 C 0.8089(5) 0.4972(5) 0.4986(2) 0.0514(15) Uani 1 1 d . . . H4 H 0.757 0.5418 0.5206 0.062 Uiso 1 1 calc R . . C5 C 0.8700(6) 0.3940(5) 0.51355(18) 0.0510(15) Uani 1 1 d . . . H5 H 0.862 0.3699 0.5459 0.061 Uiso 1 1 calc R . . C6 C 0.9438(5) 0.3250(4) 0.48089(16) 0.0460(14) Uani 1 1 d . . . H6 H 0.9854 0.2548 0.4914 0.055 Uiso 1 1 calc R . . C7 C 1.2287(5) 0.3114(4) 0.39342(17) 0.0355(12) Uani 1 1 d . . . C8 C 1.2775(6) 0.3875(5) 0.42956(18) 0.0500(14) Uani 1 1 d . . . H8 H 1.2165 0.4181 0.4526 0.06 Uiso 1 1 calc R . . C9 C 1.4168(7) 0.4181(6) 0.4314(2) 0.0711(18) Uani 1 1 d . . . H9 H 1.4483 0.4706 0.4552 0.085 Uiso 1 1 calc R . . C10 C 1.5065(7) 0.3718(6) 0.3989(3) 0.0798(18) Uani 1 1 d . . . H10 H 1.6 0.391 0.4011 0.096 Uiso 1 1 calc R . . C11 C 1.4614(6) 0.2957(6) 0.3621(2) 0.0725(19) Uani 1 1 d . . . H11 H 1.5237 0.2654 0.3394 0.087 Uiso 1 1 calc R . . C12 C 1.3214(6) 0.2654(5) 0.35977(19) 0.0537(15) Uani 1 1 d . . . H12 H 1.2902 0.2141 0.3355 0.064 Uiso 1 1 calc R . . C13 C 0.9951(6) 0.3147(4) 0.33022(14) 0.0413(11) Uani 1 1 d . . . C14 C 1.0566(5) 0.4121(5) 0.30738(17) 0.0574(16) Uani 1 1 d . . . H14 H 1.1303 0.4506 0.3225 0.069 Uiso 1 1 calc R . . C15 C 1.0102(7) 0.4527(6) 0.26269(17) 0.0712(17) Uani 1 1 d . . . H15 H 1.0532 0.5171 0.2476 0.085 Uiso 1 1 calc R . . C16 C 0.9017(9) 0.3976(7) 0.2412(2) 0.091(3) Uani 1 1 d . . . H16 H 0.8706 0.4248 0.2111 0.109 Uiso 1 1 calc R . . C17 C 0.8365(9) 0.3029(7) 0.2627(3) 0.102(3) Uani 1 1 d . . . H17 H 0.7609 0.2672 0.2476 0.123 Uiso 1 1 calc R . . C18 C 0.8847(7) 0.2602(5) 0.3075(2) 0.0701(18) Uani 1 1 d . . . H18 H 0.842 0.1949 0.3221 0.084 Uiso 1 1 calc R . . C19 C 1.2593(5) -0.0760(5) 0.37366(14) 0.0353(11) Uani 1 1 d . . . C20 C 1.3928(5) -0.0801(5) 0.35441(16) 0.0442(13) Uani 1 1 d . . . H20 H 1.4377 -0.0083 0.3481 0.053 Uiso 1 1 calc R . . C21 C 1.4623(6) -0.1858(6) 0.34422(19) 0.0539(15) Uani 1 1 d . A . C22 C 1.3935(6) -0.2947(5) 0.3554(2) 0.0642(17) Uani 1 1 d . . . H22 H 1.436 -0.3676 0.3492 0.077 Uiso 1 1 calc R . . C23 C 1.2636(6) -0.2905(5) 0.37546(19) 0.0531(15) Uani 1 1 d . . . H23 H 1.2208 -0.3624 0.3832 0.064 Uiso 1 1 calc R . . C24 C 1.1906(5) -0.1839(5) 0.38513(16) 0.0360(13) Uani 1 1 d . . . C25 C 1.0560(5) -0.1932(4) 0.40441(18) 0.0425(13) Uani 1 1 d . . . H25 H 1.0249 -0.2702 0.4107 0.051 Uiso 1 1 calc R . . C26 C 0.7568(5) -0.0579(5) 0.44066(16) 0.0447(12) Uani 1 1 d . . . C27 C 0.5850(6) -0.2016(5) 0.4695(2) 0.0649(17) Uani 1 1 d . . . H27A H 0.5795 -0.2457 0.4396 0.097 Uiso 1 1 calc R . . H27B H 0.4953 -0.1989 0.4846 0.097 Uiso 1 1 calc R . . H27C H 0.6493 -0.2398 0.4912 0.097 Uiso 1 1 calc R . . C28 C 1.6627(6) -0.0757(6) 0.3126(2) 0.0672(17) Uani 1 1 d . A . H28A H 1.7616 -0.0901 0.3109 0.081 Uiso 1 1 calc R . . H28B H 1.6463 -0.0181 0.3383 0.081 Uiso 1 1 calc R . . C29 C 1.6157(7) -0.0234(7) 0.2650(2) 0.097(2) Uani 1 1 d . . . H29A H 1.6318 -0.0798 0.2393 0.145 Uiso 1 1 calc R . . H29B H 1.6664 0.0485 0.2586 0.145 Uiso 1 1 calc R . . H29C H 1.5186 -0.0056 0.2668 0.145 Uiso 1 1 calc R . . C30A C 1.6454(18) -0.2925(15) 0.2968(9) 0.068(4) Uani 0.5 1 d PU A 1 H30A H 1.5684 -0.3446 0.289 0.082 Uiso 0.5 1 calc PR A 1 H30B H 1.6879 -0.2668 0.2665 0.082 Uiso 0.5 1 calc PR A 1 C31A C 1.744(2) -0.3552(19) 0.3257(10) 0.124(9) Uani 0.5 1 d PU A 1 H31A H 1.8135 -0.3006 0.337 0.186 Uiso 0.5 1 calc PR A 1 H31B H 1.7867 -0.4164 0.3064 0.186 Uiso 0.5 1 calc PR A 1 H31C H 1.6982 -0.3908 0.3532 0.186 Uiso 0.5 1 calc PR A 1 C30B C 1.6900(19) -0.2956(15) 0.3333(9) 0.069(4) Uani 0.5 1 d PU A 2 H30C H 1.7778 -0.2725 0.3477 0.083 Uiso 0.5 1 calc PR A 2 H30D H 1.6459 -0.355 0.3538 0.083 Uiso 0.5 1 calc PR A 2 C31B C 1.708(4) -0.340(2) 0.2809(8) 0.169(12) Uani 0.5 1 d PU A 2 H31D H 1.6341 -0.3939 0.273 0.254 Uiso 0.5 1 calc PR A 2 H31E H 1.795 -0.3808 0.278 0.254 Uiso 0.5 1 calc PR A 2 H31F H 1.7061 -0.2734 0.259 0.254 Uiso 0.5 1 calc PR A 2 N1 N 0.9700(4) -0.1084(3) 0.41446(12) 0.0365(9) Uani 1 1 d . . . N2 N 0.8433(4) -0.1466(4) 0.43344(14) 0.0434(11) Uani 1 1 d . . . N3 N 0.6312(4) -0.0822(4) 0.45949(16) 0.0608(13) Uani 1 1 d . . . H3A H 0.5762 -0.0238 0.4658 0.073 Uiso 1 1 calc R . . N4 N 1.5939(5) -0.1853(5) 0.3248(2) 0.0776(17) Uani 1 1 d . . . O1 O 1.2067(3) 0.0303(3) 0.38027(11) 0.0416(9) Uani 1 1 d . . . P1 P 1.04894(13) 0.26455(11) 0.39022(4) 0.0339(3) Uani 1 1 d . . . S1 S 0.79301(14) 0.09292(12) 0.42905(5) 0.0498(4) Uani 1 1 d . . . Pd1 Pd 1.01170(4) 0.06543(3) 0.402810(11) 0.03508(11) 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 0.039(3) 0.029(3) 0.032(3) -0.003(2) 0.004(2) 0.003(2) C2 0.050(3) 0.037(3) 0.038(3) 0.002(2) 0.005(2) 0.007(3) C3 0.060(4) 0.041(4) 0.053(3) -0.011(3) 0.007(3) 0.012(3) C4 0.049(4) 0.050(4) 0.055(4) -0.023(3) 0.014(3) -0.001(3) C5 0.071(4) 0.045(4) 0.037(3) -0.008(3) 0.014(3) -0.015(3) C6 0.069(4) 0.029(3) 0.040(3) -0.002(2) 0.005(3) -0.003(3) C7 0.031(3) 0.039(3) 0.037(3) 0.011(2) 0.003(2) 0.004(2) C8 0.047(4) 0.047(4) 0.056(3) 0.008(3) -0.006(3) -0.005(3) C9 0.065(4) 0.067(5) 0.081(4) 0.008(4) -0.023(3) -0.026(4) C10 0.040(4) 0.081(5) 0.118(5) 0.033(4) -0.010(5) -0.013(4) C11 0.045(4) 0.079(5) 0.094(5) 0.026(4) 0.019(4) 0.012(4) C12 0.051(4) 0.053(4) 0.057(3) 0.017(3) -0.001(3) 0.000(3) C13 0.045(3) 0.041(3) 0.038(2) -0.003(2) -0.004(3) 0.012(3) C14 0.052(3) 0.074(5) 0.046(3) 0.014(3) 0.000(2) 0.010(3) C15 0.081(4) 0.088(5) 0.045(3) 0.020(3) 0.010(4) 0.021(5) C16 0.133(7) 0.099(7) 0.041(4) -0.002(4) -0.027(4) 0.030(5) C17 0.130(7) 0.091(7) 0.086(5) -0.013(5) -0.065(5) -0.001(6) C18 0.089(5) 0.059(5) 0.063(4) -0.004(3) -0.028(4) 0.002(4) C19 0.037(3) 0.033(3) 0.036(3) -0.007(2) -0.004(2) 0.008(3) C20 0.041(3) 0.034(3) 0.058(3) -0.003(3) 0.002(2) 0.004(3) C21 0.042(4) 0.051(4) 0.068(4) -0.003(3) 0.011(3) 0.009(3) C22 0.045(4) 0.049(4) 0.099(5) -0.007(4) 0.009(3) 0.017(3) C23 0.056(4) 0.033(4) 0.070(4) -0.003(3) -0.001(3) 0.008(3) C24 0.040(3) 0.029(3) 0.038(3) -0.006(2) -0.002(2) 0.002(3) C25 0.049(3) 0.036(3) 0.042(3) 0.001(3) -0.001(3) 0.010(2) C26 0.039(3) 0.045(3) 0.050(3) -0.006(3) 0.000(2) 0.005(3) C27 0.056(4) 0.053(4) 0.085(4) -0.002(3) 0.027(3) 0.002(3) C28 0.044(3) 0.067(5) 0.091(4) -0.008(4) 0.016(3) -0.004(4) C29 0.076(5) 0.127(7) 0.087(5) 0.010(5) 0.019(4) 0.006(5) C30A 0.063(10) 0.066(12) 0.076(12) -0.007(9) 0.011(10) 0.020(8) C31A 0.112(16) 0.14(2) 0.120(18) -0.015(13) -0.029(12) 0.090(14) C30B 0.044(10) 0.060(12) 0.102(16) 0.000(10) 0.018(10) 0.019(8) C31B 0.23(3) 0.15(2) 0.13(2) -0.056(16) -0.03(2) 0.10(2) N1 0.032(2) 0.034(2) 0.043(2) 0.0033(17) -0.0021(18) -0.0018(19) N2 0.034(3) 0.039(3) 0.057(3) 0.002(2) 0.009(2) -0.002(2) N3 0.039(3) 0.047(3) 0.097(3) 0.000(3) 0.023(2) 0.001(3) N4 0.054(3) 0.055(4) 0.124(5) -0.007(4) 0.039(3) 0.014(3) O1 0.037(2) 0.029(2) 0.059(2) -0.0035(16) 0.0064(16) 0.0036(16) P1 0.0374(8) 0.0286(7) 0.0356(7) 0.0015(5) 0.0000(5) 0.0035(6) S1 0.0410(8) 0.0384(9) 0.0700(9) -0.0051(7) 0.0116(6) 0.0050(7) Pd1 0.03590(19) 0.03062(18) 0.03872(18) -0.00275(17) 0.0004(2) 0.0033(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.382(6) . ? C1 C6 1.392(6) . ? C1 P1 1.808(4) . ? C2 C3 1.394(6) . ? C2 H2 0.93 . ? C3 C4 1.365(7) . ? C3 H3 0.93 . ? C4 C5 1.361(7) . ? C4 H4 0.93 . ? C5 C6 1.381(7) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C12 1.385(6) . ? C7 C8 1.389(6) . ? C7 P1 1.816(5) . ? C8 C9 1.390(7) . ? C8 H8 0.93 . ? C9 C10 1.347(8) . ? C9 H9 0.93 . ? C10 C11 1.391(8) . ? C10 H10 0.93 . ? C11 C12 1.396(8) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C18 1.377(7) . ? C13 C14 1.391(7) . ? C13 P1 1.814(4) . ? C14 C15 1.381(6) . ? C14 H14 0.93 . ? C15 C16 1.351(9) . ? C15 H15 0.93 . ? C16 C17 1.367(9) . ? C16 H16 0.93 . ? C17 C18 1.399(8) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 O1 1.309(5) . ? C19 C20 1.393(6) . ? C19 C24 1.415(7) . ? C20 C21 1.390(7) . ? C20 H20 0.93 . ? C21 N4 1.378(7) . ? C21 C22 1.423(8) . ? C22 C23 1.371(7) . ? C22 H22 0.93 . ? C23 C24 1.412(7) . ? C23 H23 0.93 . ? C24 C25 1.408(6) . ? C25 N1 1.291(5) . ? C25 H25 0.93 . ? C26 N2 1.313(6) . ? C26 N3 1.347(6) . ? C26 S1 1.755(6) . ? C27 N3 1.436(6) . ? C27 H27A 0.96 . ? C27 H27B 0.96 . ? C27 H27C 0.96 . ? C28 N4 1.437(8) . ? C28 C29 1.499(8) . ? C28 H28A 0.97 . ? C28 H28B 0.97 . ? C29 H29A 0.96 . ? C29 H29B 0.96 . ? C29 H29C 0.96 . ? C30A C31A 1.42(3) . ? C30A N4 1.509(19) . ? C30A H30A 0.97 . ? C30A H30B 0.97 . ? C31A H31A 0.96 . ? C31A H31B 0.96 . ? C31A H31C 0.96 . ? C30B C31B 1.53(3) . ? C30B N4 1.56(2) . ? C30B H30C 0.97 . ? C30B H30D 0.97 . ? C31B H31D 0.96 . ? C31B H31E 0.96 . ? C31B H31F 0.96 . ? N1 N2 1.398(5) . ? N1 Pd1 2.015(4) . ? N3 H3A 0.86 . ? O1 Pd1 2.021(3) . ? P1 Pd1 2.2867(13) . ? S1 Pd1 2.2526(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.0(4) . . ? C2 C1 P1 122.7(3) . . ? C6 C1 P1 119.3(3) . . ? C1 C2 C3 121.0(5) . . ? C1 C2 H2 119.5 . . ? C3 C2 H2 119.5 . . ? C4 C3 C2 119.4(5) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? C5 C4 C3 120.6(5) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.6(5) . . ? C5 C6 H6 119.7 . . ? C1 C6 H6 119.7 . . ? C12 C7 C8 119.0(5) . . ? C12 C7 P1 118.6(4) . . ? C8 C7 P1 122.4(4) . . ? C7 C8 C9 120.4(5) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 121.0(6) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C12 119.1(6) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C7 C12 C11 120.3(6) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C18 C13 C14 118.4(5) . . ? C18 C13 P1 119.6(4) . . ? C14 C13 P1 121.9(4) . . ? C15 C14 C13 121.3(5) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 119.2(6) . . ? C16 C15 H15 120.4 . . ? C14 C15 H15 120.4 . . ? C15 C16 C17 121.6(6) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C18 119.4(7) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C13 C18 C17 120.2(6) . . ? C13 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? O1 C19 C20 116.2(5) . . ? O1 C19 C24 124.4(4) . . ? C20 C19 C24 119.4(5) . . ? C21 C20 C19 123.4(5) . . ? C21 C20 H20 118.3 . . ? C19 C20 H20 118.3 . . ? N4 C21 C20 121.3(6) . . ? N4 C21 C22 121.1(6) . . ? C20 C21 C22 117.5(5) . . ? C23 C22 C21 119.0(5) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C22 C23 C24 124.1(5) . . ? C22 C23 H23 117.9 . . ? C24 C23 H23 117.9 . . ? C25 C24 C23 118.0(5) . . ? C25 C24 C19 125.5(5) . . ? C23 C24 C19 116.5(5) . . ? N1 C25 C24 128.3(5) . . ? N1 C25 H25 115.9 . . ? C24 C25 H25 115.9 . . ? N2 C26 N3 118.5(5) . . ? N2 C26 S1 125.1(4) . . ? N3 C26 S1 116.4(4) . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 C29 113.4(6) . . ? N4 C28 H28A 108.9 . . ? C29 C28 H28A 108.9 . . ? N4 C28 H28B 108.9 . . ? C29 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31A C30A N4 109(3) . . ? C31A C30A H30A 109.8 . . ? N4 C30A H30A 109.8 . . ? C31A C30A H30B 109.8 . . ? N4 C30A H30B 109.8 . . ? H30A C30A H30B 108.3 . . ? C30A C31A H31A 109.5 . . ? C30A C31A H31B 109.5 . . ? H31A C31A H31B 109.5 . . ? C30A C31A H31C 109.5 . . ? H31A C31A H31C 109.5 . . ? H31B C31A H31C 109.5 . . ? C31B C30B N4 101(2) . . ? C31B C30B H30C 111.6 . . ? N4 C30B H30C 111.6 . . ? C31B C30B H30D 111.6 . . ? N4 C30B H30D 111.6 . . ? H30C C30B H30D 109.4 . . ? C30B C31B H31D 109.5 . . ? C30B C31B H31E 109.5 . . ? H31D C31B H31E 109.5 . . ? C30B C31B H31F 109.5 . . ? H31D C31B H31F 109.5 . . ? H31E C31B H31F 109.5 . . ? C25 N1 N2 114.7(4) . . ? C25 N1 Pd1 123.3(3) . . ? N2 N1 Pd1 122.0(3) . . ? C26 N2 N1 112.4(4) . . ? C26 N3 C27 122.8(5) . . ? C26 N3 H3A 118.6 . . ? C27 N3 H3A 118.6 . . ? C21 N4 C28 121.3(6) . . ? C21 N4 C30A 119.8(8) . . ? C28 N4 C30A 114.2(7) . . ? C21 N4 C30B 119.2(8) . . ? C28 N4 C30B 115.9(7) . . ? C30A N4 C30B 41.5(7) . . ? C19 O1 Pd1 125.6(3) . . ? C1 P1 C13 104.7(2) . . ? C1 P1 C7 105.7(2) . . ? C13 P1 C7 103.2(2) . . ? C1 P1 Pd1 113.67(15) . . ? C13 P1 Pd1 113.22(16) . . ? C7 P1 Pd1 115.17(16) . . ? C26 S1 Pd1 96.49(17) . . ? N1 Pd1 O1 92.65(14) . . ? N1 Pd1 S1 83.93(12) . . ? O1 Pd1 S1 176.57(10) . . ? N1 Pd1 P1 177.48(12) . . ? O1 Pd1 P1 89.85(9) . . ? S1 Pd1 P1 93.57(5) . . ? # END of CIF # Attachment '[Pd(DeaSal -tsc)(PPh3)].doc' # CIF produced by WinGX routine CIF_UPDATE # Created on 2010-06-18 at 14:11:49 # Using CIFtbx version 2.6.2 16 Jun 1998 data_ppl15 _database_code_depnum_ccdc_archive 'CCDC 842070' #TrackingRef '[Pd(DeaSal -tsc)(PPh3)].doc' _audit_creation_date 2010-06-18T14:11:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C30 H33 N4 O1 P1 Pd1 S1' _chemical_formula_sum 'C30 H33 N4 O P Pd S' _chemical_formula_weight 635.03 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.6836(2) _cell_length_b 11.1912(2) _cell_length_c 27.4533(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2975.14(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22346 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 28.69 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.418 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.777 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.881 _exptl_absorpt_correction_T_max 0.884 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'Omega + Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_reflns_av_R_equivalents 0.0613 _diffrn_reflns_av_unetI/netI 0.1195 _diffrn_reflns_number 22346 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.69 _diffrn_reflns_theta_full 28.69 _diffrn_measured_fraction_theta_full 0.983 _diffrn_measured_fraction_theta_max 0.983 _reflns_number_total 7447 _reflns_number_gt 5470 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0086P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7447 _refine_ls_number_parameters 370 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.093 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.065 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(2) _refine_diff_density_max 0.807 _refine_diff_density_min -0.791 _refine_diff_density_rms 0.082 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.9584(3) 0.3673(3) 0.43250(12) 0.0328(9) Uani 1 1 d . . . C2 C 0.8948(4) 0.4723(3) 0.41895(14) 0.0414(10) Uani 1 1 d . . . H2 H 0.9022 0.4995 0.3871 0.05 Uiso 1 1 calc R . . C3 C 0.8201(4) 0.5372(4) 0.45269(16) 0.0516(11) Uani 1 1 d . . . H3 H 0.7783 0.6086 0.4435 0.062 Uiso 1 1 calc R . . C4 C 0.8073(5) 0.4975(4) 0.49916(17) 0.0554(13) Uani 1 1 d . . . H4 H 0.7552 0.5411 0.5214 0.066 Uiso 1 1 calc R . . C5 C 0.8696(5) 0.3952(4) 0.51344(15) 0.0510(12) Uani 1 1 d . . . H5 H 0.8619 0.3698 0.5456 0.061 Uiso 1 1 calc R . . C6 C 0.9442(4) 0.3287(3) 0.48078(13) 0.0442(11) Uani 1 1 d . . . H6 H 0.9855 0.2577 0.4907 0.053 Uiso 1 1 calc R . . C7 C 0.9936(4) 0.3234(3) 0.32981(11) 0.0385(8) Uani 1 1 d . . . C8 C 1.0557(4) 0.4205(4) 0.30735(13) 0.0524(11) Uani 1 1 d . . . H8 H 1.1297 0.4583 0.3225 0.063 Uiso 1 1 calc R . . C9 C 1.0096(6) 0.4615(4) 0.26307(15) 0.0719(14) Uani 1 1 d . . . H9 H 1.0519 0.527 0.2485 0.086 Uiso 1 1 calc R . . C10 C 0.9021(7) 0.4062(6) 0.24067(18) 0.0896(19) Uani 1 1 d . . . H10 H 0.8722 0.4331 0.2104 0.107 Uiso 1 1 calc R . . C11 C 0.8373(7) 0.3111(5) 0.2623(2) 0.096(2) Uani 1 1 d . . . H11 H 0.7617 0.2754 0.2473 0.115 Uiso 1 1 calc R . . C12 C 0.8855(5) 0.2684(4) 0.30678(17) 0.0657(14) Uani 1 1 d . . . H12 H 0.8439 0.2021 0.321 0.079 Uiso 1 1 calc R . . C13 C 1.2301(4) 0.3143(3) 0.39209(13) 0.0318(9) Uani 1 1 d . . . C14 C 1.2821(4) 0.3875(3) 0.42934(15) 0.0492(11) Uani 1 1 d . . . H14 H 1.2225 0.418 0.4528 0.059 Uiso 1 1 calc R . . C15 C 1.4201(5) 0.4142(4) 0.43143(19) 0.0659(13) Uani 1 1 d . . . H15 H 1.4541 0.4637 0.4559 0.079 Uiso 1 1 calc R . . C16 C 1.5077(5) 0.3674(4) 0.3971(2) 0.0751(13) Uani 1 1 d . . . H16 H 1.6016 0.384 0.3991 0.09 Uiso 1 1 calc R . . C17 C 1.4603(5) 0.2971(4) 0.36006(19) 0.0656(14) Uani 1 1 d . . . H17 H 1.5214 0.267 0.337 0.079 Uiso 1 1 calc R . . C18 C 1.3208(4) 0.2707(4) 0.35700(15) 0.0488(11) Uani 1 1 d . . . H18 H 1.2878 0.2239 0.3315 0.059 Uiso 1 1 calc R . . C19 C 1.2603(4) -0.0705(4) 0.37335(12) 0.0371(8) Uani 1 1 d . . . C20 C 1.3933(4) -0.0752(4) 0.35425(13) 0.0463(10) Uani 1 1 d . . . H20 H 1.4369 -0.0034 0.347 0.056 Uiso 1 1 calc R . . C21 C 1.4649(5) -0.1806(4) 0.34536(16) 0.0574(12) Uani 1 1 d . A . C22 C 1.3945(5) -0.2881(4) 0.35661(19) 0.0679(14) Uani 1 1 d . . . H22 H 1.4367 -0.3611 0.3504 0.082 Uiso 1 1 calc R . . C23 C 1.2669(5) -0.2854(4) 0.37630(16) 0.0575(12) Uani 1 1 d . . . H23 H 1.2254 -0.3578 0.3842 0.069 Uiso 1 1 calc R . . C24 C 1.1919(4) -0.1789(3) 0.38569(13) 0.0376(10) Uani 1 1 d . . . C25 C 1.0608(4) -0.1867(3) 0.40583(15) 0.0442(10) Uani 1 1 d . . . H25 H 1.0323 -0.2633 0.4141 0.053 Uiso 1 1 calc R . . C26 C 0.7623(4) -0.0502(4) 0.44228(14) 0.0458(10) Uani 1 1 d . . . C27 C 1.6622(5) -0.0711(5) 0.31313(19) 0.0738(14) Uani 1 1 d . A . H27A H 1.7612 -0.0841 0.3118 0.089 Uiso 1 1 calc R . . H27B H 1.6444 -0.0125 0.3384 0.089 Uiso 1 1 calc R . . C28 C 1.6161(6) -0.0215(5) 0.2657(2) 0.097(2) Uani 1 1 d . . . H28A H 1.6087 -0.085 0.2423 0.146 Uiso 1 1 calc R . . H28B H 1.682 0.0363 0.2545 0.146 Uiso 1 1 calc R . . H28C H 1.5277 0.0161 0.2697 0.146 Uiso 1 1 calc R . . C29 C 1.6885(13) -0.2841(10) 0.3341(4) 0.076(4) Uani 0.5 1 d PD A 1 H29A H 1.7768 -0.2565 0.3465 0.091 Uiso 0.5 1 calc PR A 1 H29B H 1.6491 -0.3393 0.3575 0.091 Uiso 0.5 1 calc PR A 1 C31 C 1.7063(18) -0.3423(14) 0.2873(4) 0.147(7) Uani 0.5 1 d PD A 1 H31A H 1.6201 -0.3765 0.2771 0.22 Uiso 0.5 1 calc PR A 1 H31B H 1.7744 -0.4043 0.2901 0.22 Uiso 0.5 1 calc PR A 1 H31C H 1.7362 -0.2847 0.2636 0.22 Uiso 0.5 1 calc PR A 1 C30 C 1.6446(11) -0.2869(8) 0.2990(4) 0.086(4) Uani 0.5 1 d PD A 2 H30A H 1.5687 -0.3386 0.2896 0.103 Uiso 0.5 1 calc PR A 2 H30B H 1.6952 -0.263 0.2701 0.103 Uiso 0.5 1 calc PR A 2 C32 C 1.7339(17) -0.3446(16) 0.3340(6) 0.142(7) Uani 0.5 1 d PD A 2 H32A H 1.8268 -0.3165 0.3298 0.213 Uiso 0.5 1 calc PR A 2 H32B H 1.7312 -0.4295 0.3292 0.213 Uiso 0.5 1 calc PR A 2 H32C H 1.7031 -0.3261 0.3664 0.213 Uiso 0.5 1 calc PR A 2 N1 N 0.9722(3) -0.1023(2) 0.41473(9) 0.0357(7) Uani 1 1 d . . . N2 N 0.8479(3) -0.1384(3) 0.43545(12) 0.0461(9) Uani 1 1 d . . . N3 N 0.6393(3) -0.0747(4) 0.46343(14) 0.0719(11) Uani 1 1 d . . . H3A H 0.6198 -0.1468 0.4719 0.086 Uiso 1 1 calc R . . H3B H 0.5807 -0.0183 0.4684 0.086 Uiso 1 1 calc R . . N4 N 1.5951(4) -0.1825(4) 0.32636(17) 0.0825(14) Uani 1 1 d D . . O1 O 1.2061(3) 0.0364(2) 0.37865(9) 0.0404(7) Uani 1 1 d . . . O2 O 0.4816(5) -0.2912(3) 0.47295(12) 0.1042(12) Uani 1 1 d . . . P1 P 1.04969(10) 0.27130(8) 0.38941(3) 0.0310(2) Uani 1 1 d . . . S1 S 0.79583(10) 0.09956(9) 0.42842(4) 0.0487(3) Uani 1 1 d . . . Pd1 Pd 1.01321(3) 0.07202(2) 0.401799(9) 0.03110(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(2) 0.0280(18) 0.038(2) -0.0045(16) -0.0007(17) -0.0021(16) C2 0.048(3) 0.040(2) 0.036(2) 0.0022(17) 0.0082(19) 0.0085(19) C3 0.052(3) 0.051(3) 0.052(3) -0.011(2) 0.002(2) 0.013(2) C4 0.057(3) 0.050(3) 0.059(3) -0.025(2) 0.024(2) -0.003(2) C5 0.077(3) 0.041(3) 0.035(2) -0.0046(19) 0.016(2) -0.017(2) C6 0.070(3) 0.034(2) 0.028(2) -0.0034(17) 0.0074(19) -0.002(2) C7 0.043(2) 0.0402(19) 0.0320(18) -0.0025(16) -0.003(2) 0.011(2) C8 0.052(3) 0.068(3) 0.037(2) 0.011(2) -0.0007(18) 0.010(2) C9 0.075(4) 0.094(4) 0.046(3) 0.029(2) 0.007(3) 0.021(4) C10 0.124(5) 0.105(5) 0.040(3) 0.006(3) -0.020(3) 0.041(4) C11 0.128(6) 0.083(4) 0.076(4) -0.012(3) -0.062(4) 0.019(4) C12 0.088(4) 0.050(3) 0.058(3) -0.005(2) -0.032(3) 0.001(3) C13 0.039(2) 0.0283(19) 0.028(2) 0.0111(16) -0.0016(17) 0.0044(16) C14 0.049(3) 0.041(2) 0.058(3) 0.007(2) -0.009(2) 0.000(2) C15 0.062(3) 0.049(3) 0.087(4) 0.013(3) -0.025(3) -0.016(3) C16 0.038(3) 0.072(3) 0.115(4) 0.028(3) -0.006(4) -0.014(3) C17 0.039(3) 0.074(3) 0.084(3) 0.017(3) 0.016(3) 0.007(2) C18 0.045(3) 0.051(3) 0.050(3) 0.012(2) 0.006(2) -0.001(2) C19 0.042(2) 0.039(2) 0.030(2) -0.0077(19) -0.0029(16) 0.007(2) C20 0.042(2) 0.048(3) 0.049(2) -0.006(2) 0.0053(18) 0.003(2) C21 0.055(3) 0.052(3) 0.066(3) -0.009(2) 0.011(2) 0.016(2) C22 0.058(3) 0.053(3) 0.092(4) -0.008(3) 0.017(3) 0.022(3) C23 0.066(3) 0.032(2) 0.074(3) -0.004(2) 0.007(3) 0.009(2) C24 0.041(3) 0.030(2) 0.042(3) -0.0014(17) -0.0026(19) 0.0011(19) C25 0.049(3) 0.030(2) 0.054(3) -0.001(2) -0.004(2) -0.0081(17) C26 0.041(2) 0.045(3) 0.051(3) -0.010(2) 0.005(2) -0.005(2) C27 0.047(3) 0.088(4) 0.086(4) -0.020(4) 0.013(3) 0.009(3) C28 0.082(4) 0.125(5) 0.086(4) -0.001(4) 0.020(3) 0.011(4) C29 0.059(8) 0.091(10) 0.077(9) 0.000(8) -0.025(7) 0.052(7) C31 0.172(16) 0.161(14) 0.108(12) -0.074(11) -0.018(11) 0.104(12) C30 0.050(8) 0.100(10) 0.107(11) -0.019(9) 0.033(8) 0.028(7) C32 0.132(15) 0.153(18) 0.142(16) 0.023(13) -0.062(12) 0.072(12) N1 0.0361(18) 0.0322(16) 0.0389(17) -0.0024(12) 0.0015(14) -0.0006(14) N2 0.038(2) 0.039(2) 0.061(2) 0.0035(17) 0.0096(18) -0.0048(16) N3 0.049(2) 0.053(2) 0.114(3) -0.006(3) 0.031(2) -0.005(2) N4 0.062(3) 0.060(3) 0.126(4) -0.002(3) 0.040(3) 0.025(2) O1 0.0354(16) 0.0304(15) 0.0553(17) -0.0005(12) 0.0108(13) 0.0046(12) O2 0.121(3) 0.091(3) 0.101(3) 0.0037(19) -0.005(3) -0.030(3) P1 0.0365(6) 0.0289(5) 0.0276(5) -0.0003(4) 0.0002(4) 0.0034(4) S1 0.0389(6) 0.0365(6) 0.0707(7) -0.0057(5) 0.0110(5) 0.0030(5) Pd1 0.03135(14) 0.02849(12) 0.03345(14) -0.00326(12) -0.00007(14) 0.00208(14) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.378(5) . ? C1 C6 1.401(5) . ? C1 P1 1.826(3) . ? C2 C3 1.382(5) . ? C2 H2 0.93 . ? C3 C4 1.357(6) . ? C3 H3 0.93 . ? C4 C5 1.353(6) . ? C4 H4 0.93 . ? C5 C6 1.371(5) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C12 1.370(6) . ? C7 C8 1.386(5) . ? C7 P1 1.820(3) . ? C8 C9 1.374(5) . ? C8 H8 0.93 . ? C9 C10 1.359(7) . ? C9 H9 0.93 . ? C10 C11 1.370(8) . ? C10 H10 0.93 . ? C11 C12 1.392(7) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C18 1.392(5) . ? C13 C14 1.404(5) . ? C13 P1 1.813(4) . ? C14 C15 1.371(6) . ? C14 H14 0.93 . ? C15 C16 1.371(6) . ? C15 H15 0.93 . ? C16 C17 1.366(6) . ? C16 H16 0.93 . ? C17 C18 1.385(6) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 O1 1.315(4) . ? C19 C20 1.391(5) . ? C19 C24 1.422(5) . ? C20 C21 1.390(6) . ? C20 H20 0.93 . ? C21 N4 1.365(6) . ? C21 C22 1.416(6) . ? C22 C23 1.350(6) . ? C22 H22 0.93 . ? C23 C24 1.419(5) . ? C23 H23 0.93 . ? C24 C25 1.387(5) . ? C25 N1 1.299(4) . ? C25 H25 0.93 . ? C26 N2 1.303(5) . ? C26 N3 1.353(5) . ? C26 S1 1.749(4) . ? C27 N4 1.452(6) . ? C27 C28 1.483(7) . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 C31 1.453(5) . ? C29 N4 1.468(5) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C31 H31A 0.96 . ? C31 H31B 0.96 . ? C31 H31C 0.96 . ? C30 C32 1.446(5) . ? C30 N4 1.469(5) . ? C30 H30A 0.97 . ? C30 H30B 0.97 . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? N1 N2 1.391(4) . ? N1 Pd1 2.023(3) . ? N3 H3A 0.86 . ? N3 H3B 0.86 . ? O1 Pd1 2.013(2) . ? P1 Pd1 2.2835(9) . ? S1 Pd1 2.2495(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 118.3(3) . . ? C2 C1 P1 122.9(3) . . ? C6 C1 P1 118.6(3) . . ? C1 C2 C3 120.1(4) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 120.6(4) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 120.3(4) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.2(4) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C12 C7 C8 118.6(4) . . ? C12 C7 P1 119.9(3) . . ? C8 C7 P1 121.4(3) . . ? C9 C8 C7 121.0(4) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C10 C9 C8 119.8(5) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C11 120.6(5) . . ? C9 C10 H10 119.7 . . ? C11 C10 H10 119.7 . . ? C10 C11 C12 119.5(5) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C7 C12 C11 120.5(5) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C18 C13 C14 118.8(4) . . ? C18 C13 P1 119.1(3) . . ? C14 C13 P1 122.0(3) . . ? C15 C14 C13 120.5(4) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.4(4) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 121.6(5) . . ? C17 C16 H16 119.2 . . ? C15 C16 H16 119.2 . . ? C16 C17 C18 119.7(5) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C17 C18 C13 119.9(4) . . ? C17 C18 H18 120 . . ? C13 C18 H18 120 . . ? O1 C19 C20 116.4(4) . . ? O1 C19 C24 124.3(3) . . ? C20 C19 C24 119.3(4) . . ? C21 C20 C19 124.1(4) . . ? C21 C20 H20 118 . . ? C19 C20 H20 118 . . ? N4 C21 C20 122.8(5) . . ? N4 C21 C22 121.0(4) . . ? C20 C21 C22 116.2(4) . . ? C23 C22 C21 120.6(4) . . ? C23 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C22 C23 C24 124.0(4) . . ? C22 C23 H23 118 . . ? C24 C23 H23 118 . . ? C25 C24 C23 119.2(4) . . ? C25 C24 C19 125.1(3) . . ? C23 C24 C19 115.8(4) . . ? N1 C25 C24 129.3(3) . . ? N1 C25 H25 115.3 . . ? C24 C25 H25 115.3 . . ? N2 C26 N3 117.9(4) . . ? N2 C26 S1 125.2(3) . . ? N3 C26 S1 116.8(3) . . ? N4 C27 C28 113.9(5) . . ? N4 C27 H27A 108.8 . . ? C28 C27 H27A 108.8 . . ? N4 C27 H27B 108.8 . . ? C28 C27 H27B 108.8 . . ? H27A C27 H27B 107.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 N4 107.0(9) . . ? C31 C29 H29A 110.3 . . ? N4 C29 H29A 110.3 . . ? C31 C29 H29B 110.3 . . ? N4 C29 H29B 110.3 . . ? H29A C29 H29B 108.6 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C32 C30 N4 102.1(9) . . ? C32 C30 H30A 111.3 . . ? N4 C30 H30A 111.3 . . ? C32 C30 H30B 111.3 . . ? N4 C30 H30B 111.3 . . ? H30A C30 H30B 109.2 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 N1 N2 116.0(3) . . ? C25 N1 Pd1 122.5(3) . . ? N2 N1 Pd1 121.5(2) . . ? C26 N2 N1 112.9(3) . . ? C26 N3 H3A 120 . . ? C26 N3 H3B 120 . . ? H3A N3 H3B 120 . . ? C21 N4 C27 119.7(4) . . ? C21 N4 C29 121.7(7) . . ? C27 N4 C29 115.2(7) . . ? C21 N4 C30 120.6(6) . . ? C27 N4 C30 114.2(6) . . ? C29 N4 C30 42.1(5) . . ? C19 O1 Pd1 125.8(2) . . ? C13 P1 C7 103.81(18) . . ? C13 P1 C1 106.48(16) . . ? C7 P1 C1 104.43(16) . . ? C13 P1 Pd1 113.72(11) . . ? C7 P1 Pd1 113.64(12) . . ? C1 P1 Pd1 113.79(11) . . ? C26 S1 Pd1 96.51(14) . . ? O1 Pd1 N1 92.68(11) . . ? O1 Pd1 S1 176.44(7) . . ? N1 Pd1 S1 83.76(9) . . ? O1 Pd1 P1 90.16(7) . . ? N1 Pd1 P1 177.08(9) . . ? S1 Pd1 P1 93.40(4) . . ? # END of CIF data_pp21 _database_code_depnum_ccdc_archive 'CCDC 842373' #TrackingRef '[Pd(DeaSal -etsc)(PPh3)].doc' _audit_creation_date 2010-05-10T15:57:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H35 N4 O1 P1 Pd1 S1' _chemical_formula_sum 'C32 H35 N4 O P Pd S' _chemical_formula_weight 661.07 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' _symmetry_Int_Tables_number 19 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.8285(2) _cell_length_b 11.3287(2) _cell_length_c 27.6805(7) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3082.06(11) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 27334 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 28.68 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.753 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; R.H. Blessing, Acta Cryst. (1995), A51, 33-38 ; _exptl_absorpt_correction_T_min 0.9 _exptl_absorpt_correction_T_max 0.903 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'Omega + Phi scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_unetI/netI 0.1449 _diffrn_reflns_number 27334 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 28.68 _diffrn_reflns_theta_full 28.68 _diffrn_measured_fraction_theta_full 0.955 _diffrn_measured_fraction_theta_max 0.955 _reflns_number_total 7503 _reflns_number_gt 4653 _reflns_threshold_expression >2sigma(I) _diffrn_reflns_reduction_process ; Scaled and merged with Sortav R.H. Blessing, (1987) Cryst. Rev. 1, 3-58 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397 ; #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0084P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7503 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1061 _refine_ls_R_factor_gt 0.043 _refine_ls_wR_factor_ref 0.0756 _refine_ls_wR_factor_gt 0.0647 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.38(2) _refine_diff_density_max 0.432 _refine_diff_density_min -0.961 _refine_diff_density_rms 0.094 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.4629(4) 0.3723(3) 0.43392(13) 0.0327(9) Uani 1 1 d . . . C2 C 0.3989(4) 0.4756(4) 0.42197(16) 0.0429(11) Uani 1 1 d . . . H2 H 0.4057 0.5049 0.3907 0.052 Uiso 1 1 calc R . . C3 C 0.3236(4) 0.5372(4) 0.45648(18) 0.0603(13) Uani 1 1 d . . . H3 H 0.2814 0.6079 0.4483 0.072 Uiso 1 1 calc R . . C4 C 0.3119(4) 0.4930(4) 0.50285(19) 0.0533(13) Uani 1 1 d . . . H4 H 0.2606 0.5332 0.5258 0.064 Uiso 1 1 calc R . . C5 C 0.3757(5) 0.3903(4) 0.51495(16) 0.0544(13) Uani 1 1 d . . . H5 H 0.3677 0.3609 0.5462 0.065 Uiso 1 1 calc R . . C6 C 0.4522(4) 0.3293(4) 0.48130(14) 0.0472(11) Uani 1 1 d . . . H6 H 0.4965 0.2599 0.49 0.057 Uiso 1 1 calc R . . C7 C 0.5052(4) 0.3441(3) 0.33191(12) 0.0362(9) Uani 1 1 d . . . C8 C 0.3975(5) 0.2927(4) 0.30721(17) 0.0620(14) Uani 1 1 d . . . H8 H 0.355 0.226 0.3197 0.074 Uiso 1 1 calc R . . C9 C 0.3534(6) 0.3408(5) 0.2638(2) 0.0806(18) Uani 1 1 d . . . H9 H 0.2807 0.3068 0.2474 0.097 Uiso 1 1 calc R . . C10 C 0.4172(6) 0.4385(5) 0.24516(18) 0.0725(16) Uani 1 1 d . . . H10 H 0.3877 0.4698 0.2159 0.087 Uiso 1 1 calc R . . C11 C 0.5228(5) 0.4902(4) 0.26875(16) 0.0623(13) Uani 1 1 d . . . H11 H 0.5648 0.5568 0.256 0.075 Uiso 1 1 calc R . . C12 C 0.5667(4) 0.4423(4) 0.31194(15) 0.0489(12) Uani 1 1 d . . . H12 H 0.6395 0.477 0.328 0.059 Uiso 1 1 calc R . . C13 C 0.7345(3) 0.3301(3) 0.39524(17) 0.0384(9) Uani 1 1 d . . . C14 C 0.7793(4) 0.4012(4) 0.43329(16) 0.0566(12) Uani 1 1 d . . . H14 H 0.7177 0.4288 0.4561 0.068 Uiso 1 1 calc R . . C15 C 0.9156(5) 0.4302(5) 0.4369(2) 0.0811(17) Uani 1 1 d . . . H15 H 0.9454 0.4789 0.4618 0.097 Uiso 1 1 calc R . . C16 C 1.0061(5) 0.3880(6) 0.4041(2) 0.0914(19) Uani 1 1 d . . . H16 H 1.0979 0.4062 0.4072 0.11 Uiso 1 1 calc R . . C17 C 0.9634(5) 0.3191(5) 0.3667(2) 0.0785(16) Uani 1 1 d . . . H17 H 1.0261 0.2918 0.3441 0.094 Uiso 1 1 calc R . . C18 C 0.8273(4) 0.2893(4) 0.36206(18) 0.0540(13) Uani 1 1 d . . . H18 H 0.7988 0.2418 0.3366 0.065 Uiso 1 1 calc R . . C19 C 0.7611(4) -0.0524(4) 0.36586(14) 0.0354(10) Uani 1 1 d . . . C20 C 0.8915(4) -0.0576(4) 0.34713(15) 0.0434(11) Uani 1 1 d . . . H20 H 0.9379 0.013 0.3424 0.052 Uiso 1 1 calc R . . C21 C 0.9574(4) -0.1625(4) 0.33495(15) 0.0449(11) Uani 1 1 d . . . C22 C 0.8875(4) -0.2691(4) 0.34369(17) 0.0528(12) Uani 1 1 d . . . H22 H 0.9285 -0.341 0.3365 0.063 Uiso 1 1 calc R . . C23 C 0.7597(4) -0.2662(4) 0.36275(16) 0.0463(12) Uani 1 1 d . . . H23 H 0.7158 -0.3376 0.3685 0.056 Uiso 1 1 calc R . . C24 C 0.6906(4) -0.1614(4) 0.37420(14) 0.0361(10) Uani 1 1 d . . . C25 C 0.5555(3) -0.1707(3) 0.39138(14) 0.0380(9) Uani 1 1 d . . . H25 H 0.522 -0.247 0.3949 0.046 Uiso 1 1 calc R . . C26 C 0.2637(4) -0.0355(4) 0.42767(16) 0.0416(11) Uani 1 1 d . . . C27 C 0.0807(5) -0.1757(5) 0.45059(18) 0.0653(15) Uani 1 1 d . . . H27A H 0.1178 -0.2301 0.427 0.078 Uiso 1 1 calc R . . H27B H -0.0175 -0.1746 0.4469 0.078 Uiso 1 1 calc R . . C28 C 0.1159(6) -0.2161(5) 0.49970(19) 0.0854(18) Uani 1 1 d . . . H28A H 0.213 -0.2226 0.5026 0.128 Uiso 1 1 calc R . . H28B H 0.075 -0.2918 0.5055 0.128 Uiso 1 1 calc R . . H28C H 0.0827 -0.1603 0.523 0.128 Uiso 1 1 calc R . . C29 C 1.1594(4) -0.0524(5) 0.30769(18) 0.0620(14) Uani 1 1 d . . . H29A H 1.2564 -0.0683 0.3068 0.074 Uiso 1 1 calc R . . H29B H 1.1422 0.0004 0.3346 0.074 Uiso 1 1 calc R . . C30 C 1.1192(5) 0.0078(5) 0.2618(2) 0.090(2) Uani 1 1 d . . . H30A H 1.1334 -0.0447 0.235 0.135 Uiso 1 1 calc R . . H30B H 1.1735 0.0775 0.2575 0.135 Uiso 1 1 calc R . . H30C H 1.0248 0.0294 0.2633 0.135 Uiso 1 1 calc R . . C31 C 1.1503(6) -0.2701(6) 0.2940(3) 0.101(2) Uani 1 1 d . . . H31A H 1.0791 -0.3206 0.2813 0.121 Uiso 1 1 calc R . . H31B H 1.2085 -0.247 0.2673 0.121 Uiso 1 1 calc R . . C32 C 1.2279(8) -0.3337(7) 0.3283(3) 0.149(3) Uani 1 1 d . . . H32A H 1.303 -0.2861 0.3389 0.224 Uiso 1 1 calc R . . H32B H 1.2617 -0.4048 0.3138 0.224 Uiso 1 1 calc R . . H32C H 1.1716 -0.3533 0.3555 0.224 Uiso 1 1 calc R . . N1 N 0.4725(3) -0.0863(3) 0.40285(10) 0.0349(6) Uani 1 1 d . . . N2 N 0.3449(3) -0.1233(3) 0.41943(12) 0.0418(9) Uani 1 1 d . . . N3 N 0.1347(3) -0.0580(3) 0.44189(14) 0.0595(11) Uani 1 1 d . . . H3A H 0.0811 0.0012 0.4461 0.071 Uiso 1 1 calc R . . N4 N 1.0875(4) -0.1622(4) 0.31596(16) 0.0608(12) Uani 1 1 d . . . O1 O 0.7105(2) 0.0524(2) 0.37443(10) 0.0428(7) Uani 1 1 d . . . P1 P 0.55696(9) 0.28430(9) 0.39021(4) 0.0328(2) Uani 1 1 d . . . S1 S 0.30385(10) 0.11432(10) 0.42168(4) 0.0493(3) Uani 1 1 d . . . Pd1 Pd 0.51888(2) 0.08660(3) 0.396760(10) 0.03344(9) 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 0.036(2) 0.025(2) 0.037(2) -0.0016(17) -0.0009(18) -0.0010(17) C2 0.045(2) 0.044(3) 0.040(3) -0.005(2) 0.004(2) 0.011(2) C3 0.066(3) 0.055(3) 0.061(4) -0.010(3) -0.002(3) 0.020(3) C4 0.052(3) 0.054(4) 0.054(4) -0.018(3) 0.014(2) 0.000(2) C5 0.075(3) 0.053(4) 0.036(3) -0.002(3) 0.011(2) -0.028(3) C6 0.066(3) 0.035(3) 0.040(3) -0.006(2) 0.000(2) -0.005(2) C7 0.045(2) 0.032(2) 0.031(2) -0.0025(17) -0.002(2) 0.009(2) C8 0.081(3) 0.054(4) 0.051(3) 0.005(3) -0.022(3) -0.009(3) C9 0.103(4) 0.073(5) 0.066(4) -0.002(3) -0.047(3) -0.012(3) C10 0.106(4) 0.071(4) 0.041(3) -0.001(3) -0.016(3) 0.022(3) C11 0.076(3) 0.066(3) 0.045(3) 0.019(2) 0.005(3) 0.010(3) C12 0.052(2) 0.052(3) 0.043(3) 0.009(2) 0.000(2) 0.000(2) C13 0.041(2) 0.033(2) 0.041(2) 0.008(2) -0.007(2) 0.0010(17) C14 0.056(3) 0.054(3) 0.060(3) 0.007(3) -0.011(2) -0.003(3) C15 0.060(3) 0.079(5) 0.105(5) 0.004(4) -0.034(3) -0.028(3) C16 0.039(3) 0.101(5) 0.134(5) 0.030(4) -0.012(4) -0.019(3) C17 0.040(3) 0.084(4) 0.111(5) 0.020(4) 0.010(3) -0.002(3) C18 0.047(3) 0.053(3) 0.062(3) 0.010(3) 0.005(2) 0.000(2) C19 0.036(2) 0.034(3) 0.036(2) -0.003(2) -0.0065(18) 0.0050(19) C20 0.038(2) 0.044(3) 0.049(3) -0.002(2) -0.0023(19) 0.005(2) C21 0.040(3) 0.046(3) 0.049(3) -0.005(2) -0.002(2) 0.008(2) C22 0.049(3) 0.038(3) 0.071(3) -0.012(3) 0.000(2) 0.015(2) C23 0.048(3) 0.035(3) 0.057(3) -0.009(2) -0.001(2) 0.005(2) C24 0.032(2) 0.035(3) 0.041(3) -0.006(2) -0.0076(18) 0.0063(18) C25 0.042(2) 0.030(2) 0.041(2) -0.001(2) -0.003(2) 0.0003(17) C26 0.038(2) 0.039(3) 0.048(3) -0.002(2) 0.006(2) -0.004(2) C27 0.059(3) 0.071(4) 0.066(4) -0.002(3) 0.011(3) 0.004(3) C28 0.110(5) 0.083(5) 0.064(4) 0.000(4) 0.024(3) 0.020(3) C29 0.045(3) 0.069(4) 0.072(4) 0.010(3) 0.010(2) 0.009(3) C30 0.078(4) 0.106(5) 0.085(5) 0.028(4) 0.018(3) 0.019(3) C31 0.070(4) 0.088(5) 0.144(6) 0.006(5) 0.008(4) 0.019(3) C32 0.141(7) 0.139(8) 0.168(8) -0.044(6) -0.038(6) 0.057(6) N1 0.0326(14) 0.0335(17) 0.0387(17) -0.0021(17) 0.0010(14) -0.0039(16) N2 0.0338(19) 0.037(2) 0.055(2) 0.0020(18) 0.0073(16) -0.0019(15) N3 0.047(2) 0.040(3) 0.092(3) 0.004(2) 0.024(2) -0.0021(18) N4 0.048(2) 0.055(3) 0.079(3) -0.004(3) 0.016(2) 0.019(2) O1 0.0408(15) 0.0287(18) 0.0591(19) -0.0011(14) 0.0061(13) 0.0043(13) P1 0.0356(6) 0.0297(6) 0.0331(6) -0.0008(5) 0.0002(5) 0.0021(4) S1 0.0403(6) 0.0366(7) 0.0711(8) -0.0072(6) 0.0116(5) 0.0032(5) Pd1 0.03508(15) 0.02928(16) 0.03597(15) -0.00302(15) 0.00045(13) 0.00257(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.369(5) . ? C1 C6 1.403(5) . ? C1 P1 1.820(4) . ? C2 C3 1.396(6) . ? C2 H2 0.93 . ? C3 C4 1.383(6) . ? C3 H3 0.93 . ? C4 C5 1.364(6) . ? C4 H4 0.93 . ? C5 C6 1.382(6) . ? C5 H5 0.93 . ? C6 H6 0.93 . ? C7 C12 1.381(5) . ? C7 C8 1.388(6) . ? C7 P1 1.823(4) . ? C8 C9 1.388(6) . ? C8 H8 0.93 . ? C9 C10 1.374(7) . ? C9 H9 0.93 . ? C10 C11 1.359(7) . ? C10 H10 0.93 . ? C11 C12 1.382(6) . ? C11 H11 0.93 . ? C12 H12 0.93 . ? C13 C18 1.375(6) . ? C13 C14 1.397(6) . ? C13 P1 1.826(4) . ? C14 C15 1.384(6) . ? C14 H14 0.93 . ? C15 C16 1.357(7) . ? C15 H15 0.93 . ? C16 C17 1.363(8) . ? C16 H16 0.93 . ? C17 C18 1.385(6) . ? C17 H17 0.93 . ? C18 H18 0.93 . ? C19 O1 1.309(4) . ? C19 C20 1.384(5) . ? C19 C24 1.435(5) . ? C20 C21 1.395(6) . ? C20 H20 0.93 . ? C21 N4 1.383(5) . ? C21 C22 1.410(6) . ? C22 C23 1.364(6) . ? C22 H22 0.93 . ? C23 C24 1.404(5) . ? C23 H23 0.93 . ? C24 C25 1.414(5) . ? C25 N1 1.296(4) . ? C25 H25 0.93 . ? C26 N2 1.296(5) . ? C26 N3 1.352(5) . ? C26 S1 1.750(4) . ? C27 N3 1.455(6) . ? C27 C28 1.476(7) . ? C27 H27A 0.97 . ? C27 H27B 0.97 . ? C28 H28A 0.96 . ? C28 H28B 0.96 . ? C28 H28C 0.96 . ? C29 N4 1.449(6) . ? C29 C30 1.496(7) . ? C29 H29A 0.97 . ? C29 H29B 0.97 . ? C30 H30A 0.96 . ? C30 H30B 0.96 . ? C30 H30C 0.96 . ? C31 C32 1.414(8) . ? C31 N4 1.498(7) . ? C31 H31A 0.97 . ? C31 H31B 0.97 . ? C32 H32A 0.96 . ? C32 H32B 0.96 . ? C32 H32C 0.96 . ? N1 N2 1.400(4) . ? N1 Pd1 2.018(3) . ? N3 H3A 0.86 . ? O1 Pd1 2.019(2) . ? P1 Pd1 2.2781(10) . ? S1 Pd1 2.2451(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 119.2(4) . . ? C2 C1 P1 122.7(3) . . ? C6 C1 P1 118.0(3) . . ? C1 C2 C3 120.4(4) . . ? C1 C2 H2 119.8 . . ? C3 C2 H2 119.8 . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C5 C4 C3 119.9(4) . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C4 C5 C6 120.7(4) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.8(4) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? C12 C7 C8 118.3(4) . . ? C12 C7 P1 122.1(3) . . ? C8 C7 P1 119.6(3) . . ? C9 C8 C7 120.0(5) . . ? C9 C8 H8 120 . . ? C7 C8 H8 120 . . ? C10 C9 C8 120.0(5) . . ? C10 C9 H9 120 . . ? C8 C9 H9 120 . . ? C11 C10 C9 121.0(5) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.0(5) . . ? C10 C11 H11 120.5 . . ? C12 C11 H11 120.5 . . ? C7 C12 C11 121.7(4) . . ? C7 C12 H12 119.1 . . ? C11 C12 H12 119.1 . . ? C18 C13 C14 119.3(4) . . ? C18 C13 P1 119.2(3) . . ? C14 C13 P1 121.5(3) . . ? C15 C14 C13 119.7(5) . . ? C15 C14 H14 120.1 . . ? C13 C14 H14 120.1 . . ? C16 C15 C14 120.2(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 120.5(5) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C18 120.5(5) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C13 C18 C17 119.8(5) . . ? C13 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? O1 C19 C20 117.3(4) . . ? O1 C19 C24 124.6(3) . . ? C20 C19 C24 118.1(4) . . ? C19 C20 C21 123.8(4) . . ? C19 C20 H20 118.1 . . ? C21 C20 H20 118.1 . . ? N4 C21 C20 121.3(4) . . ? N4 C21 C22 121.2(4) . . ? C20 C21 C22 117.5(4) . . ? C23 C22 C21 119.7(4) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 123.6(4) . . ? C22 C23 H23 118.2 . . ? C24 C23 H23 118.2 . . ? C23 C24 C25 117.9(4) . . ? C23 C24 C19 117.2(3) . . ? C25 C24 C19 124.9(3) . . ? N1 C25 C24 128.2(4) . . ? N1 C25 H25 115.9 . . ? C24 C25 H25 115.9 . . ? N2 C26 N3 119.0(4) . . ? N2 C26 S1 126.1(3) . . ? N3 C26 S1 114.9(3) . . ? N3 C27 C28 110.6(5) . . ? N3 C27 H27A 109.5 . . ? C28 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 C30 113.4(5) . . ? N4 C29 H29A 108.9 . . ? C30 C29 H29A 108.9 . . ? N4 C29 H29B 108.9 . . ? C30 C29 H29B 108.9 . . ? H29A C29 H29B 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C32 C31 N4 111.4(6) . . ? C32 C31 H31A 109.3 . . ? N4 C31 H31A 109.3 . . ? C32 C31 H31B 109.3 . . ? N4 C31 H31B 109.3 . . ? H31A C31 H31B 108 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C25 N1 N2 115.0(3) . . ? C25 N1 Pd1 123.6(2) . . ? N2 N1 Pd1 121.4(2) . . ? C26 N2 N1 112.3(3) . . ? C26 N3 C27 124.3(4) . . ? C26 N3 H3A 117.9 . . ? C27 N3 H3A 117.9 . . ? C21 N4 C29 120.9(4) . . ? C21 N4 C31 122.2(5) . . ? C29 N4 C31 115.8(4) . . ? C19 O1 Pd1 125.7(2) . . ? C1 P1 C7 104.09(17) . . ? C1 P1 C13 106.19(19) . . ? C7 P1 C13 103.2(2) . . ? C1 P1 Pd1 113.71(12) . . ? C7 P1 Pd1 112.95(13) . . ? C13 P1 Pd1 115.50(12) . . ? C26 S1 Pd1 96.07(14) . . ? N1 Pd1 O1 92.87(11) . . ? N1 Pd1 S1 84.11(8) . . ? O1 Pd1 S1 176.98(8) . . ? N1 Pd1 P1 176.39(8) . . ? O1 Pd1 P1 90.63(8) . . ? S1 Pd1 P1 92.38(4) . . ? # END of CIF