Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Nicholas Long' _publ_contact_author_address ; Department of Chemistry Imperial College of Science, Techno South Kensington LONDON SW7 2AY UNITED KINGDOM ; _publ_contact_author_email N.LONG@IMPERIAL.AC.UK _publ_section_title ; Variable Coordination Behaviour of Pyrazole-Containing N,P and N,P(O) Ligands towards Palladium(II) ; _publ_requested_category FO loop_ _publ_author_name 'Nicholas Long' 'Peter B. Hitchcock' 'Antony Gee' 'Steven Kealey' 'Philip W. Miller' 'Andrew J. P. White' data_Compound_1c _database_code_depnum_ccdc_archive 'CCDC 640789' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '(C42 H34 N4 P2 Pd), (Cl 04)2' _chemical_formula_sum 'C42 H34 Cl2 N4 O8 P2 Pd' _chemical_formula_weight 961.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 13.8787(11) _cell_length_b 18.264(2) _cell_length_c 31.8160(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8064.7(13) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 49226 _cell_measurement_theta_min 3.6885 _cell_measurement_theta_max 31.9285 _exptl_crystal_description plates _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3904 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.94916 _exptl_absorpt_correction_T_max 1.06785 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.30.2 (release 11-05-2006 CrysAlis171 .NET) (compiled May 11 2006,17:41:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 102703 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0275 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 32.00 _reflns_number_total 13189 _reflns_number_gt 9927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0340P)^2^+9.5835P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13189 _refine_ls_number_parameters 540 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0613 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0915 _refine_ls_wR_factor_gt 0.0860 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.006 _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 Pd Pd 0.596410(11) 0.631501(8) 0.874586(5) 0.02134(4) Uani 1 1 d . . . N1 N 0.60435(13) 0.54150(10) 0.91418(6) 0.0272(4) Uani 1 1 d . . . N2 N 0.60320(15) 0.47338(10) 0.89713(7) 0.0340(4) Uani 1 1 d D . . H2 H 0.588(2) 0.4693(16) 0.8698(2) 0.040(8) Uiso 1 1 d D . . C3 C 0.6068(2) 0.42243(14) 0.92754(9) 0.0431(6) Uani 1 1 d . . . H3A H 0.6058 0.3709 0.9235 0.052 Uiso 1 1 calc R . . C4 C 0.61199(19) 0.45763(14) 0.96497(9) 0.0407(6) Uani 1 1 d . . . H4A H 0.6163 0.4359 0.9920 0.049 Uiso 1 1 calc R . . C5 C 0.60974(15) 0.53251(12) 0.95573(7) 0.0283(4) Uani 1 1 d . . . C6 C 0.60920(16) 0.59334(13) 0.98537(7) 0.0293(4) Uani 1 1 d . . . C7 C 0.64761(19) 0.58046(16) 1.02555(8) 0.0400(6) Uani 1 1 d . . . H7A H 0.6786 0.5351 1.0311 0.048 Uiso 1 1 calc R . . C8 C 0.6416(2) 0.63178(18) 1.05705(8) 0.0473(7) Uani 1 1 d . . . H8A H 0.6681 0.6216 1.0839 0.057 Uiso 1 1 calc R . . C9 C 0.5969(2) 0.69812(16) 1.04958(8) 0.0416(6) Uani 1 1 d . . . H9A H 0.5911 0.7332 1.0715 0.050 Uiso 1 1 calc R . . C10 C 0.56046(19) 0.71315(14) 1.00962(7) 0.0349(5) Uani 1 1 d . . . H10A H 0.5309 0.7592 1.0044 0.042 Uiso 1 1 calc R . . C11 C 0.56663(16) 0.66189(13) 0.97725(7) 0.0278(4) Uani 1 1 d . . . P12 P 0.51092(4) 0.68499(3) 0.926725(16) 0.02299(10) Uani 1 1 d . . . C13 C 0.51029(17) 0.78424(12) 0.92719(6) 0.0271(4) Uani 1 1 d . . . C14 C 0.59949(18) 0.81892(13) 0.92651(7) 0.0340(5) Uani 1 1 d . . . H14A H 0.6568 0.7908 0.9242 0.041 Uiso 1 1 calc R . . C15 C 0.6048(2) 0.89503(15) 0.92921(9) 0.0450(6) Uani 1 1 d . . . H15A H 0.6657 0.9188 0.9287 0.054 Uiso 1 1 calc R . . C16 C 0.5211(2) 0.93581(14) 0.93259(10) 0.0497(7) Uani 1 1 d . . . H16A H 0.5247 0.9876 0.9349 0.060 Uiso 1 1 calc R . . C17 C 0.4329(2) 0.90175(14) 0.93259(9) 0.0447(6) Uani 1 1 d . . . H17A H 0.3758 0.9302 0.9346 0.054 Uiso 1 1 calc R . . C18 C 0.42640(18) 0.82567(13) 0.92968(8) 0.0342(5) Uani 1 1 d . . . H18A H 0.3652 0.8024 0.9294 0.041 Uiso 1 1 calc R . . C19 C 0.38813(15) 0.65189(12) 0.93107(7) 0.0273(4) Uani 1 1 d . . . C20 C 0.32752(18) 0.67613(14) 0.96333(8) 0.0359(5) Uani 1 1 d . . . H20A H 0.3500 0.7110 0.9832 0.043 Uiso 1 1 calc R . . C21 C 0.2343(2) 0.64892(16) 0.96611(9) 0.0477(7) Uani 1 1 d . . . H21A H 0.1930 0.6655 0.9879 0.057 Uiso 1 1 calc R . . C22 C 0.2010(2) 0.59803(17) 0.93745(11) 0.0526(8) Uani 1 1 d . . . H22A H 0.1367 0.5804 0.9394 0.063 Uiso 1 1 calc R . . C23 C 0.26117(19) 0.57267(15) 0.90595(10) 0.0450(6) Uani 1 1 d . . . H23A H 0.2386 0.5371 0.8865 0.054 Uiso 1 1 calc R . . C24 C 0.35481(17) 0.59934(13) 0.90284(8) 0.0329(5) Uani 1 1 d . . . H24A H 0.3962 0.5816 0.8813 0.039 Uiso 1 1 calc R . . N31 N 0.69684(13) 0.58640(10) 0.83373(6) 0.0253(3) Uani 1 1 d . . . N32 N 0.77754(14) 0.55690(11) 0.85044(6) 0.0307(4) Uani 1 1 d D . . H32 H 0.786(2) 0.5602(16) 0.87839(16) 0.046(8) Uiso 1 1 d D . . C33 C 0.83984(18) 0.53840(15) 0.82024(9) 0.0423(6) Uani 1 1 d . . . H33A H 0.9016 0.5171 0.8243 0.051 Uiso 1 1 calc R . . C34 C 0.79890(18) 0.55552(15) 0.78246(8) 0.0405(6) Uani 1 1 d . . . H34A H 0.8258 0.5481 0.7553 0.049 Uiso 1 1 calc R . . C35 C 0.70927(16) 0.58611(12) 0.79195(7) 0.0271(4) Uani 1 1 d . . . C36 C 0.63762(16) 0.61513(12) 0.76231(7) 0.0274(4) Uani 1 1 d . . . C37 C 0.63920(19) 0.58823(14) 0.72123(8) 0.0373(5) Uani 1 1 d . . . H37A H 0.6838 0.5509 0.7139 0.045 Uiso 1 1 calc R . . C38 C 0.5771(2) 0.61501(16) 0.69107(8) 0.0438(6) Uani 1 1 d . . . H38A H 0.5798 0.5966 0.6632 0.053 Uiso 1 1 calc R . . C39 C 0.5111(2) 0.66849(16) 0.70144(8) 0.0427(6) Uani 1 1 d . . . H39A H 0.4677 0.6865 0.6808 0.051 Uiso 1 1 calc R . . C40 C 0.50816(19) 0.69598(14) 0.74207(7) 0.0353(5) Uani 1 1 d . . . H40A H 0.4627 0.7330 0.7490 0.042 Uiso 1 1 calc R . . C41 C 0.57091(16) 0.67014(12) 0.77282(6) 0.0265(4) Uani 1 1 d . . . P42 P 0.57613(4) 0.71626(3) 0.823837(16) 0.02267(10) Uani 1 1 d . . . C43 C 0.46534(17) 0.76784(14) 0.82595(7) 0.0323(5) Uani 1 1 d . . . C44 C 0.38013(19) 0.72799(19) 0.82719(8) 0.0457(7) Uani 1 1 d . . . H44A H 0.3822 0.6760 0.8260 0.055 Uiso 1 1 calc R . . C45 C 0.2924(2) 0.7634(3) 0.83008(10) 0.0689(11) Uani 1 1 d . . . H45A H 0.2345 0.7357 0.8310 0.083 Uiso 1 1 calc R . . C46 C 0.2888(3) 0.8381(3) 0.83161(10) 0.0800(14) Uani 1 1 d . . . H46A H 0.2284 0.8622 0.8337 0.096 Uiso 1 1 calc R . . C47 C 0.3717(3) 0.8781(2) 0.83009(10) 0.0696(12) Uani 1 1 d . . . H47A H 0.3681 0.9300 0.8309 0.084 Uiso 1 1 calc R . . C48 C 0.4627(2) 0.84394(16) 0.82729(8) 0.0452(7) Uani 1 1 d . . . H48A H 0.5203 0.8720 0.8263 0.054 Uiso 1 1 calc R . . C49 C 0.67763(16) 0.77693(12) 0.81686(7) 0.0276(4) Uani 1 1 d . . . C50 C 0.6773(2) 0.82603(14) 0.78316(8) 0.0393(6) Uani 1 1 d . . . H50A H 0.6219 0.8301 0.7657 0.047 Uiso 1 1 calc R . . C51 C 0.7575(2) 0.86856(16) 0.77529(9) 0.0513(7) Uani 1 1 d . . . H51A H 0.7567 0.9033 0.7530 0.062 Uiso 1 1 calc R . . C52 C 0.8384(2) 0.86063(17) 0.79964(10) 0.0537(8) Uani 1 1 d . . . H52A H 0.8942 0.8888 0.7935 0.064 Uiso 1 1 calc R . . C53 C 0.8398(2) 0.81233(16) 0.83288(10) 0.0476(7) Uani 1 1 d . . . H53A H 0.8961 0.8077 0.8496 0.057 Uiso 1 1 calc R . . C54 C 0.75890(17) 0.77028(13) 0.84204(8) 0.0340(5) Uani 1 1 d . . . H54A H 0.7592 0.7375 0.8652 0.041 Uiso 1 1 calc R . . Cl1 Cl 0.43003(4) 0.46476(3) 0.81130(2) 0.03815(13) Uani 1 1 d . . . O11 O 0.50186(16) 0.51665(12) 0.82248(7) 0.0558(6) Uani 1 1 d . . . O12 O 0.33637(15) 0.49552(14) 0.81641(7) 0.0604(6) Uani 1 1 d . . . O13 O 0.44339(18) 0.44401(15) 0.76848(8) 0.0695(7) Uani 1 1 d . . . O14 O 0.44123(18) 0.40204(13) 0.83830(9) 0.0736(8) Uani 1 1 d . . . Cl2 Cl 0.88711(5) 0.65105(4) 0.935707(19) 0.04202(15) Uani 1 1 d . . . O21 O 0.95662(19) 0.63233(13) 0.96664(8) 0.0672(7) Uani 1 1 d . . . O22 O 0.81596(17) 0.59326(16) 0.93366(7) 0.0695(7) Uani 1 1 d . . . O23 O 0.9332(2) 0.65519(18) 0.89620(8) 0.0848(9) Uani 1 1 d . . . O24 O 0.8440(3) 0.71861(18) 0.94555(11) 0.1071(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 Pd 0.02240(7) 0.02041(7) 0.02121(7) 0.00229(6) 0.00109(6) 0.00224(6) N1 0.0310(9) 0.0205(8) 0.0300(9) 0.0057(7) -0.0032(7) 0.0007(7) N2 0.0404(11) 0.0236(9) 0.0380(11) 0.0014(8) -0.0042(9) -0.0001(8) C3 0.0477(15) 0.0247(11) 0.0569(17) 0.0114(11) -0.0003(13) -0.0016(11) C4 0.0446(14) 0.0336(12) 0.0440(14) 0.0174(11) 0.0028(11) 0.0032(11) C5 0.0253(10) 0.0310(11) 0.0287(10) 0.0103(8) 0.0005(8) 0.0023(8) C6 0.0261(10) 0.0342(11) 0.0277(10) 0.0084(9) 0.0015(8) 0.0021(9) C7 0.0381(13) 0.0512(15) 0.0305(12) 0.0139(11) -0.0042(10) 0.0084(12) C8 0.0469(15) 0.0677(19) 0.0274(12) 0.0125(12) -0.0093(11) 0.0005(14) C9 0.0495(15) 0.0503(15) 0.0249(11) 0.0012(10) -0.0027(10) -0.0042(13) C10 0.0413(13) 0.0397(12) 0.0237(10) 0.0025(9) 0.0007(9) 0.0017(11) C11 0.0262(10) 0.0345(11) 0.0227(9) 0.0064(8) -0.0005(8) -0.0002(9) P12 0.0245(2) 0.0236(2) 0.0208(2) 0.00365(19) 0.00160(19) 0.0028(2) C13 0.0369(11) 0.0239(9) 0.0204(9) -0.0001(8) 0.0004(8) 0.0024(9) C14 0.0386(12) 0.0312(11) 0.0321(11) 0.0001(9) 0.0015(10) 0.0005(10) C15 0.0520(16) 0.0321(12) 0.0509(16) 0.0006(12) -0.0028(13) -0.0062(12) C16 0.069(2) 0.0251(11) 0.0552(17) -0.0028(11) -0.0042(15) 0.0014(13) C17 0.0548(16) 0.0309(12) 0.0482(15) -0.0004(11) -0.0011(13) 0.0118(12) C18 0.0368(12) 0.0321(11) 0.0337(12) 0.0003(9) -0.0003(10) 0.0052(10) C19 0.0254(10) 0.0287(10) 0.0279(10) 0.0098(8) 0.0037(8) 0.0047(8) C20 0.0372(12) 0.0372(12) 0.0335(12) 0.0091(10) 0.0090(10) 0.0091(10) C21 0.0368(13) 0.0525(16) 0.0539(16) 0.0203(13) 0.0214(12) 0.0167(12) C22 0.0273(12) 0.0516(17) 0.079(2) 0.0229(16) 0.0080(13) 0.0003(12) C23 0.0324(13) 0.0407(14) 0.0618(17) 0.0098(13) -0.0037(12) -0.0046(11) C24 0.0291(11) 0.0320(11) 0.0375(12) 0.0080(10) 0.0006(9) -0.0002(9) N31 0.0228(8) 0.0240(8) 0.0289(9) -0.0026(7) 0.0011(7) 0.0030(7) N32 0.0259(9) 0.0325(9) 0.0337(10) -0.0058(8) -0.0045(8) 0.0055(8) C33 0.0273(11) 0.0467(15) 0.0529(16) -0.0150(12) 0.0008(11) 0.0098(11) C34 0.0321(12) 0.0513(15) 0.0381(13) -0.0136(11) 0.0047(10) 0.0078(11) C35 0.0260(10) 0.0267(10) 0.0288(10) -0.0060(8) 0.0019(8) -0.0029(8) C36 0.0279(10) 0.0274(10) 0.0270(10) -0.0040(8) 0.0010(8) -0.0045(8) C37 0.0413(13) 0.0398(13) 0.0308(12) -0.0103(10) 0.0016(10) -0.0021(11) C38 0.0515(16) 0.0559(16) 0.0239(11) -0.0096(11) -0.0030(10) -0.0038(13) C39 0.0495(15) 0.0524(16) 0.0261(11) 0.0011(11) -0.0095(11) 0.0003(13) C40 0.0386(13) 0.0391(12) 0.0282(11) 0.0019(9) -0.0038(9) 0.0033(10) C41 0.0303(10) 0.0267(10) 0.0223(9) 0.0005(8) 0.0002(8) -0.0033(8) P42 0.0254(2) 0.0220(2) 0.0206(2) 0.00192(19) 0.00106(19) 0.00203(19) C43 0.0341(12) 0.0403(12) 0.0223(10) 0.0077(9) 0.0013(9) 0.0146(10) C44 0.0318(12) 0.0684(19) 0.0370(13) 0.0146(13) 0.0003(10) 0.0093(13) C45 0.0341(15) 0.125(3) 0.0474(18) 0.026(2) 0.0025(13) 0.0243(19) C46 0.058(2) 0.138(4) 0.0432(17) 0.020(2) 0.0077(15) 0.065(3) C47 0.095(3) 0.073(2) 0.0408(16) 0.0080(15) 0.0019(17) 0.060(2) C48 0.0600(17) 0.0426(14) 0.0330(12) 0.0049(11) 0.0002(12) 0.0252(13) C49 0.0329(11) 0.0242(10) 0.0258(10) -0.0030(8) 0.0051(8) -0.0031(8) C50 0.0528(15) 0.0338(12) 0.0313(12) 0.0032(10) 0.0030(11) -0.0096(11) C51 0.069(2) 0.0429(15) 0.0416(14) -0.0002(12) 0.0151(14) -0.0221(15) C52 0.0543(18) 0.0479(16) 0.0587(18) -0.0156(14) 0.0222(15) -0.0235(14) C53 0.0345(13) 0.0489(16) 0.0596(18) -0.0191(14) 0.0027(12) -0.0092(12) C54 0.0321(11) 0.0326(11) 0.0373(12) -0.0073(10) 0.0031(10) -0.0012(10) Cl1 0.0283(3) 0.0377(3) 0.0484(3) 0.0036(3) -0.0137(2) -0.0012(2) O11 0.0580(13) 0.0568(13) 0.0526(12) 0.0028(10) -0.0088(10) -0.0259(11) O12 0.0419(11) 0.0773(16) 0.0620(14) -0.0028(12) -0.0113(10) 0.0200(11) O13 0.0644(14) 0.0839(17) 0.0603(14) -0.0297(13) -0.0254(12) 0.0265(13) O14 0.0519(13) 0.0577(14) 0.111(2) 0.0410(15) -0.0092(14) -0.0034(11) Cl2 0.0430(3) 0.0534(4) 0.0296(3) -0.0079(3) -0.0056(2) -0.0038(3) O21 0.0783(17) 0.0636(14) 0.0598(14) 0.0031(11) -0.0340(13) -0.0128(13) O22 0.0552(13) 0.114(2) 0.0392(11) -0.0149(12) 0.0046(10) -0.0411(14) O23 0.0836(18) 0.124(2) 0.0464(13) -0.0064(15) 0.0160(13) -0.0481(18) O24 0.112(3) 0.094(2) 0.115(3) -0.044(2) -0.037(2) 0.048(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 Pd N1 2.0738(17) . ? Pd N31 2.0763(17) . ? Pd P42 2.2545(6) . ? Pd P12 2.2614(6) . ? N1 C5 1.334(3) . ? N1 N2 1.357(3) . ? N2 C3 1.343(3) . ? C3 C4 1.355(4) . ? C4 C5 1.399(3) . ? C5 C6 1.457(3) . ? C6 C7 1.405(3) . ? C6 C11 1.408(3) . ? C7 C8 1.375(4) . ? C8 C9 1.381(4) . ? C9 C10 1.395(3) . ? C10 C11 1.395(3) . ? C11 P12 1.833(2) . ? P12 C13 1.813(2) . ? P12 C19 1.813(2) . ? C13 C18 1.391(3) . ? C13 C14 1.391(3) . ? C14 C15 1.395(4) . ? C15 C16 1.384(4) . ? C16 C17 1.373(4) . ? C17 C18 1.395(4) . ? C19 C24 1.394(3) . ? C19 C20 1.399(3) . ? C20 C21 1.389(4) . ? C21 C22 1.382(5) . ? C22 C23 1.384(4) . ? C23 C24 1.391(3) . ? N31 C35 1.340(3) . ? N31 N32 1.352(2) . ? N32 C33 1.336(3) . ? C33 C34 1.366(4) . ? C34 C35 1.397(3) . ? C35 C36 1.469(3) . ? C36 C37 1.397(3) . ? C36 C41 1.406(3) . ? C37 C38 1.380(4) . ? C38 C39 1.379(4) . ? C39 C40 1.387(3) . ? C40 C41 1.392(3) . ? C41 P42 1.830(2) . ? P42 C43 1.804(2) . ? P42 C49 1.806(2) . ? C43 C44 1.389(4) . ? C43 C48 1.391(4) . ? C44 C45 1.382(4) . ? C45 C46 1.366(6) . ? C46 C47 1.364(6) . ? C47 C48 1.412(4) . ? C49 C54 1.389(3) . ? C49 C50 1.398(3) . ? C50 C51 1.381(4) . ? C51 C52 1.371(5) . ? C52 C53 1.377(5) . ? C53 C54 1.391(4) . ? Cl1 O11 1.421(2) . ? Cl1 O12 1.425(2) . ? Cl1 O13 1.426(2) . ? Cl1 O14 1.440(2) . ? Cl2 O24 1.407(3) . ? Cl2 O23 1.412(2) . ? Cl2 O21 1.420(2) . ? Cl2 O22 1.447(2) . ? 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 Pd N31 91.73(7) . . ? N1 Pd P42 170.37(5) . . ? N31 Pd P42 84.71(5) . . ? N1 Pd P12 85.68(5) . . ? N31 Pd P12 169.37(5) . . ? P42 Pd P12 99.39(2) . . ? C5 N1 N2 106.48(18) . . ? C5 N1 Pd 134.62(16) . . ? N2 N1 Pd 118.90(14) . . ? C3 N2 N1 110.3(2) . . ? N2 C3 C4 107.8(2) . . ? C3 C4 C5 106.1(2) . . ? N1 C5 C4 109.3(2) . . ? N1 C5 C6 123.16(19) . . ? C4 C5 C6 127.5(2) . . ? C7 C6 C11 118.4(2) . . ? C7 C6 C5 117.3(2) . . ? C11 C6 C5 124.1(2) . . ? C8 C7 C6 121.7(2) . . ? C7 C8 C9 120.0(2) . . ? C8 C9 C10 119.5(3) . . ? C11 C10 C9 121.2(2) . . ? C10 C11 C6 119.2(2) . . ? C10 C11 P12 117.85(17) . . ? C6 C11 P12 122.85(17) . . ? C13 P12 C19 109.16(11) . . ? C13 P12 C11 103.01(10) . . ? C19 P12 C11 104.64(10) . . ? C13 P12 Pd 116.14(7) . . ? C19 P12 Pd 113.88(8) . . ? C11 P12 Pd 108.82(8) . . ? C18 C13 C14 119.9(2) . . ? C18 C13 P12 123.27(18) . . ? C14 C13 P12 116.80(17) . . ? C13 C14 C15 120.0(2) . . ? C16 C15 C14 119.8(3) . . ? C17 C16 C15 120.3(2) . . ? C16 C17 C18 120.6(3) . . ? C13 C18 C17 119.4(2) . . ? C24 C19 C20 119.4(2) . . ? C24 C19 P12 119.50(17) . . ? C20 C19 P12 121.03(19) . . ? C21 C20 C19 119.6(3) . . ? C22 C21 C20 120.7(3) . . ? C21 C22 C23 120.1(3) . . ? C22 C23 C24 119.9(3) . . ? C23 C24 C19 120.3(2) . . ? C35 N31 N32 106.36(17) . . ? C35 N31 Pd 135.14(15) . . ? N32 N31 Pd 117.91(14) . . ? C33 N32 N31 110.7(2) . . ? N32 C33 C34 107.8(2) . . ? C33 C34 C35 105.8(2) . . ? N31 C35 C34 109.3(2) . . ? N31 C35 C36 123.22(19) . . ? C34 C35 C36 127.5(2) . . ? C37 C36 C41 118.9(2) . . ? C37 C36 C35 117.6(2) . . ? C41 C36 C35 123.42(19) . . ? C38 C37 C36 121.1(2) . . ? C39 C38 C37 120.0(2) . . ? C38 C39 C40 119.9(2) . . ? C39 C40 C41 120.9(2) . . ? C40 C41 C36 119.1(2) . . ? C40 C41 P42 119.46(17) . . ? C36 C41 P42 120.89(16) . . ? C43 P42 C49 110.42(11) . . ? C43 P42 C41 103.86(11) . . ? C49 P42 C41 101.78(10) . . ? C43 P42 Pd 115.99(8) . . ? C49 P42 Pd 114.33(8) . . ? C41 P42 Pd 108.91(7) . . ? C44 C43 C48 120.0(2) . . ? C44 C43 P42 116.9(2) . . ? C48 C43 P42 123.0(2) . . ? C45 C44 C43 120.5(3) . . ? C46 C45 C44 120.1(4) . . ? C47 C46 C45 120.2(3) . . ? C46 C47 C48 121.4(3) . . ? C43 C48 C47 117.8(3) . . ? C54 C49 C50 120.1(2) . . ? C54 C49 P42 120.59(17) . . ? C50 C49 P42 119.01(19) . . ? C51 C50 C49 119.8(3) . . ? C52 C51 C50 119.9(3) . . ? C51 C52 C53 120.9(3) . . ? C52 C53 C54 120.2(3) . . ? C49 C54 C53 119.1(2) . . ? O11 Cl1 O12 110.40(15) . . ? O11 Cl1 O13 108.98(15) . . ? O12 Cl1 O13 109.40(13) . . ? O11 Cl1 O14 107.79(14) . . ? O12 Cl1 O14 110.11(15) . . ? O13 Cl1 O14 110.14(17) . . ? O24 Cl2 O23 110.1(2) . . ? O24 Cl2 O21 110.25(17) . . ? O23 Cl2 O21 108.80(18) . . ? O24 Cl2 O22 111.1(2) . . ? O23 Cl2 O22 107.94(15) . . ? O21 Cl2 O22 108.62(15) . . ? _diffrn_measured_fraction_theta_max 0.941 _diffrn_reflns_theta_full 32.00 _diffrn_measured_fraction_theta_full 0.941 _refine_diff_density_max 0.664 _refine_diff_density_min -0.833 _refine_diff_density_rms 0.077 #===END # Attachment 'B704051B_compounds_pzphos,_1b,_2b,_2c.cif' data_(pzphos(O))-aug2206 _database_code_depnum_ccdc_archive 'CCDC 640790' _audit_creation_date 2006-09-01T14:28:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C21 H17 N2 O P, C H Cl3' _chemical_formula_sum 'C22 H18 Cl3 N2 O P' _chemical_formula_weight 463.7 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 9.9204(3) _cell_length_b 10.2022(3) _cell_length_c 11.5173(3) _cell_angle_alpha 71.592(2) _cell_angle_beta 78.246(2) _cell_angle_gamma 87.496(1) _cell_volume 1082.56(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8667 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.423 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 476 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.514 _exptl_absorpt_correction_type none #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.216742E-1 _diffrn_orient_matrix_ub_12 0.244206E-1 _diffrn_orient_matrix_ub_13 -0.852881E-1 _diffrn_orient_matrix_ub_21 -0.100679 _diffrn_orient_matrix_ub_22 -0.8089E-2 _diffrn_orient_matrix_ub_23 0.375329E-1 _diffrn_orient_matrix_ub_31 -0.4865E-3 _diffrn_orient_matrix_ub_32 0.100076 _diffrn_orient_matrix_ub_33 -0.64119E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0409 _diffrn_reflns_av_unetI/netI 0.0305 _diffrn_reflns_number 15085 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 4226 _reflns_number_gt 3615 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atom on N1 was refined; other H atoms were in riding mode. 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^)+(0.0486P)^2^+1.2788P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 4226 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0569 _refine_ls_R_factor_gt 0.0481 _refine_ls_wR_factor_ref 0.1297 _refine_ls_wR_factor_gt 0.1239 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.111 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.035 _refine_diff_density_min -0.651 _refine_diff_density_rms 0.101 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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 P P 0.23355(6) 0.35018(6) 0.26198(5) 0.02176(16) Uani 1 1 d . . . O O 0.13379(17) 0.26820(17) 0.37447(15) 0.0282(4) Uani 1 1 d . . . N1 N 0.0895(2) 0.6373(2) 0.4673(2) 0.0271(4) Uani 1 1 d . . . H1 H 0.008(3) 0.619(3) 0.511(3) 0.035(8) Uiso 1 1 d . . . N2 N 0.16395(19) 0.5346(2) 0.43597(18) 0.0253(4) Uani 1 1 d . . . C1 C 0.2837(2) 0.2486(2) 0.1565(2) 0.0228(5) Uani 1 1 d . . . C2 C 0.3573(2) 0.3039(3) 0.0346(2) 0.0290(5) Uani 1 1 d . . . H2 H 0.3859 0.3984 0.0041 0.035 Uiso 1 1 calc R . . C3 C 0.3888(3) 0.2219(3) -0.0423(2) 0.0341(6) Uani 1 1 d . . . H3 H 0.4409 0.2596 -0.1246 0.041 Uiso 1 1 calc R . . C4 C 0.3447(3) 0.0849(3) 0.0005(3) 0.0361(6) Uani 1 1 d . . . H4 H 0.3651 0.0293 -0.0531 0.043 Uiso 1 1 calc R . . C5 C 0.2711(3) 0.0291(3) 0.1206(3) 0.0401(7) Uani 1 1 d . . . H5 H 0.2404 -0.0647 0.1499 0.048 Uiso 1 1 calc R . . C6 C 0.2417(3) 0.1105(3) 0.1991(2) 0.0333(6) Uani 1 1 d . . . H6 H 0.1925 0.0714 0.2824 0.04 Uiso 1 1 calc R . . C7 C 0.1618(2) 0.5033(2) 0.1687(2) 0.0228(5) Uani 1 1 d . . . C8 C 0.0208(2) 0.5009(3) 0.1722(2) 0.0307(5) Uani 1 1 d . . . H8 H -0.0347 0.4242 0.2279 0.037 Uiso 1 1 calc R . . C9 C -0.0388(3) 0.6104(3) 0.0943(3) 0.0417(7) Uani 1 1 d . . . H9 H -0.1351 0.6085 0.0969 0.05 Uiso 1 1 calc R . . C10 C 0.0412(3) 0.7221(3) 0.0132(3) 0.0422(7) Uani 1 1 d . . . H10 H 0 0.7967 -0.0401 0.051 Uiso 1 1 calc R . . C11 C 0.1811(3) 0.7256(3) 0.0094(3) 0.0384(6) Uani 1 1 d . . . H11 H 0.236 0.8027 -0.0462 0.046 Uiso 1 1 calc R . . C12 C 0.2419(3) 0.6163(3) 0.0870(2) 0.0312(5) Uani 1 1 d . . . H12 H 0.3382 0.6189 0.0843 0.037 Uiso 1 1 calc R . . C13 C 0.3933(2) 0.4012(2) 0.2914(2) 0.0235(5) Uani 1 1 d . . . C14 C 0.5111(2) 0.3262(3) 0.2640(2) 0.0306(5) Uani 1 1 d . . . H14 H 0.5036 0.2515 0.2329 0.037 Uiso 1 1 calc R . . C15 C 0.6382(3) 0.3593(3) 0.2817(3) 0.0355(6) Uani 1 1 d . . . H15 H 0.7165 0.3065 0.2642 0.043 Uiso 1 1 calc R . . C16 C 0.6504(2) 0.4690(3) 0.3246(2) 0.0313(6) Uani 1 1 d . . . H16 H 0.7376 0.4937 0.3345 0.038 Uiso 1 1 calc R . . C17 C 0.5354(2) 0.5428(3) 0.3531(2) 0.0266(5) Uani 1 1 d . . . H17 H 0.545 0.6183 0.3826 0.032 Uiso 1 1 calc R . . C18 C 0.4053(2) 0.5100(2) 0.3398(2) 0.0229(5) Uani 1 1 d . . . C19 C 0.2890(2) 0.5913(2) 0.3807(2) 0.0230(5) Uani 1 1 d . . . C20 C 0.2928(3) 0.7299(3) 0.3779(2) 0.0317(6) Uani 1 1 d . . . H20 H 0.3691 0.793 0.3441 0.038 Uiso 1 1 calc R . . C21 C 0.1628(3) 0.7542(3) 0.4343(3) 0.0324(6) Uani 1 1 d . . . H21 H 0.1311 0.8386 0.4474 0.039 Uiso 1 1 calc R . . C22 C 0.2077(3) 0.1023(3) 0.6241(3) 0.0401(6) Uani 1 1 d . . . H22 H 0.1974 0.1692 0.5418 0.048 Uiso 1 1 calc R . . Cl1 Cl 0.14823(12) 0.17927(12) 0.74060(10) 0.0764(3) Uani 1 1 d . . . Cl2 Cl 0.10961(9) -0.04691(9) 0.65162(9) 0.0578(2) Uani 1 1 d . . . Cl3 Cl 0.38251(10) 0.06331(14) 0.61815(15) 0.0951(4) 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 P 0.0168(3) 0.0235(3) 0.0228(3) -0.0058(2) -0.0015(2) 0.0013(2) O 0.0255(9) 0.0275(9) 0.0270(9) -0.0068(7) 0.0029(7) -0.0013(7) N1 0.0198(10) 0.0312(11) 0.0289(11) -0.0120(9) 0.0018(8) 0.0033(8) N2 0.0201(10) 0.0296(11) 0.0266(10) -0.0118(9) -0.0011(8) 0.0022(8) C1 0.0176(11) 0.0249(12) 0.0253(12) -0.0078(9) -0.0042(9) 0.0039(9) C2 0.0266(12) 0.0270(12) 0.0288(13) -0.0048(10) -0.0016(10) -0.0005(10) C3 0.0348(14) 0.0384(15) 0.0252(12) -0.0079(11) -0.0015(10) 0.0047(11) C4 0.0434(15) 0.0348(14) 0.0342(14) -0.0167(12) -0.0097(12) 0.0099(12) C5 0.0524(17) 0.0256(13) 0.0413(16) -0.0104(12) -0.0067(13) -0.0025(12) C6 0.0378(14) 0.0276(13) 0.0293(13) -0.0060(10) 0.0005(11) -0.0022(11) C7 0.0216(11) 0.0257(12) 0.0234(11) -0.0109(9) -0.0057(9) 0.0047(9) C8 0.0216(12) 0.0415(15) 0.0307(13) -0.0140(11) -0.0057(10) 0.0048(10) C9 0.0299(14) 0.0598(19) 0.0416(16) -0.0218(14) -0.0154(12) 0.0193(13) C10 0.0542(18) 0.0439(17) 0.0342(15) -0.0169(13) -0.0195(13) 0.0270(14) C11 0.0548(18) 0.0272(13) 0.0309(14) -0.0049(11) -0.0113(12) 0.0046(12) C12 0.0292(13) 0.0311(13) 0.0326(13) -0.0078(11) -0.0085(10) 0.0009(10) C13 0.0184(11) 0.0285(12) 0.0203(11) -0.0031(9) -0.0042(9) 0.0018(9) C14 0.0239(12) 0.0367(14) 0.0328(13) -0.0127(11) -0.0078(10) 0.0078(10) C15 0.0217(12) 0.0496(16) 0.0358(14) -0.0145(12) -0.0074(10) 0.0113(11) C16 0.0185(11) 0.0491(16) 0.0246(12) -0.0089(11) -0.0048(9) 0.0010(10) C17 0.0214(11) 0.0362(13) 0.0203(11) -0.0068(10) -0.0028(9) -0.0020(10) C18 0.0190(11) 0.0294(12) 0.0163(10) -0.0031(9) -0.0010(8) 0.0003(9) C19 0.0192(11) 0.0292(12) 0.0189(11) -0.0058(9) -0.0029(9) 0.0003(9) C20 0.0251(12) 0.0288(13) 0.0387(14) -0.0080(11) -0.0040(10) -0.0025(10) C21 0.0318(13) 0.0263(13) 0.0389(14) -0.0113(11) -0.0056(11) 0.0029(10) C22 0.0421(16) 0.0415(16) 0.0381(15) -0.0138(12) -0.0096(12) 0.0036(12) Cl1 0.0987(8) 0.0867(7) 0.0689(6) -0.0528(6) -0.0321(6) 0.0236(6) Cl2 0.0558(5) 0.0423(4) 0.0762(6) -0.0195(4) -0.0137(4) -0.0006(4) Cl3 0.0395(5) 0.0959(9) 0.1540(12) -0.0486(8) -0.0150(6) 0.0084(5) #----------------------------------------------------------------------------# # 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 P O 1.4910(17) . ? P C7 1.804(2) . ? P C1 1.816(2) . ? P C13 1.816(2) . ? N1 C21 1.332(3) . ? N1 N2 1.355(3) . ? N1 H1 0.86(3) . ? N2 C19 1.337(3) . ? C1 C6 1.390(3) . ? C1 C2 1.393(3) . ? C2 C3 1.384(4) . ? C2 H2 0.95 . ? C3 C4 1.385(4) . ? C3 H3 0.95 . ? C4 C5 1.378(4) . ? C4 H4 0.95 . ? C5 C6 1.392(4) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C8 1.392(3) . ? C7 C12 1.392(3) . ? C8 C9 1.389(4) . ? C8 H8 0.95 . ? C9 C10 1.380(5) . ? C9 H9 0.95 . ? C10 C11 1.382(4) . ? C10 H10 0.95 . ? C11 C12 1.392(4) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C14 1.405(3) . ? C13 C18 1.410(3) . ? C14 C15 1.390(4) . ? C14 H14 0.95 . ? C15 C16 1.377(4) . ? C15 H15 0.95 . ? C16 C17 1.381(3) . ? C16 H16 0.95 . ? C17 C18 1.397(3) . ? C17 H17 0.95 . ? C18 C19 1.477(3) . ? C19 C20 1.406(3) . ? C20 C21 1.371(4) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 Cl2 1.750(3) . ? C22 Cl1 1.751(3) . ? C22 Cl3 1.755(3) . ? C22 H22 1 . ? 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 O P C7 113.74(10) . . ? O P C1 109.41(10) . . ? C7 P C1 103.81(10) . . ? O P C13 115.64(10) . . ? C7 P C13 107.64(11) . . ? C1 P C13 105.65(10) . . ? C21 N1 N2 112.6(2) . . ? C21 N1 H1 128(2) . . ? N2 N1 H1 119(2) . . ? C19 N2 N1 104.66(19) . . ? C6 C1 C2 119.0(2) . . ? C6 C1 P 117.80(18) . . ? C2 C1 P 123.16(18) . . ? C3 C2 C1 120.3(2) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 120.2(2) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.1(2) . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C4 C5 C6 119.9(2) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C1 C6 C5 120.5(2) . . ? C1 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C8 C7 C12 119.5(2) . . ? C8 C7 P 117.22(19) . . ? C12 C7 P 123.08(18) . . ? C9 C8 C7 120.1(3) . . ? C9 C8 H8 120 . . ? C7 C8 H8 120 . . ? C10 C9 C8 120.3(3) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H10 120 . . ? C11 C10 H10 120 . . ? C10 C11 C12 120.1(3) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C7 120.0(2) . . ? C11 C12 H12 120 . . ? C7 C12 H12 120 . . ? C14 C13 C18 118.8(2) . . ? C14 C13 P 117.19(19) . . ? C18 C13 P 124.03(17) . . ? C15 C14 C13 121.2(2) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 119.8(2) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 119.7(2) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? C16 C17 C18 122.0(2) . . ? C16 C17 H17 119 . . ? C18 C17 H17 119 . . ? C17 C18 C13 118.4(2) . . ? C17 C18 C19 116.8(2) . . ? C13 C18 C19 124.7(2) . . ? N2 C19 C20 110.6(2) . . ? N2 C19 C18 122.0(2) . . ? C20 C19 C18 127.2(2) . . ? C21 C20 C19 105.1(2) . . ? C21 C20 H20 127.4 . . ? C19 C20 H20 127.4 . . ? N1 C21 C20 107.1(2) . . ? N1 C21 H21 126.5 . . ? C20 C21 H21 126.5 . . ? Cl2 C22 Cl1 110.25(17) . . ? Cl2 C22 Cl3 110.65(17) . . ? Cl1 C22 Cl3 110.19(17) . . ? Cl2 C22 H22 108.6 . . ? Cl1 C22 H22 108.6 . . ? Cl3 C22 H22 108.6 . . ? #===END data_(1b)-aug2306 _database_code_depnum_ccdc_archive 'CCDC 640791' _audit_creation_date 2006-09-04T11:28:37-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H34 N4 P2 Pd, C H Cl3, 2(Cl), 2(H2 O)' _chemical_formula_sum 'C43 H39 Cl5 N4 O2 P2 Pd' _chemical_formula_weight 1021.37 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.5729(3) _cell_length_b 12.3105(1) _cell_length_c 24.1681(4) _cell_angle_alpha 90 _cell_angle_beta 98.680(1) _cell_angle_gamma 90 _cell_volume 4286.09(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 40264 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2072 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.868 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.8732 _exptl_absorpt_correction_T_max 0.9524 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.95265E-2 _diffrn_orient_matrix_ub_12 0.181881E-1 _diffrn_orient_matrix_ub_13 0.407914E-1 _diffrn_orient_matrix_ub_21 0.39879E-1 _diffrn_orient_matrix_ub_22 -0.659221E-1 _diffrn_orient_matrix_ub_23 0.80397E-2 _diffrn_orient_matrix_ub_31 0.560127E-1 _diffrn_orient_matrix_ub_32 0.438408E-1 _diffrn_orient_matrix_ub_33 -0.48339E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0795 _diffrn_reflns_av_unetI/netI 0.0487 _diffrn_reflns_number 64821 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.01 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 8415 _reflns_number_gt 6347 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The three peaks assumed to be O atoms of water molecules were initially refined with individual occupancies. This suggested that one O atom had full occupancy and the other two had partial occupancies summing to one atom. Final refinement therefore assumed that the occupancies of O2 and O3 exactly added to 1. The H atoms on the water molecules were not located and were omitted. The H atoms on N1 and N3 were refined; other H atoms were in riding mode. 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^)+(0.0699P)^2^+19.6937P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 8415 _refine_ls_number_parameters 532 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0839 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1593 _refine_ls_wR_factor_gt 0.1436 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.251 _refine_diff_density_min -1.051 _refine_diff_density_rms 0.114 #----------------------------------------------------------------------------# # 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 Pd Pd 0.28249(3) 0.24216(3) 0.066927(15) 0.02322(13) Uani 1 1 d . . . Cl1 Cl 0.13822(11) -0.00370(12) 0.07604(7) 0.0479(4) Uani 1 1 d . . . Cl2 Cl 0.35899(17) 0.39942(16) -0.03829(11) 0.0851(7) Uani 1 1 d . . . Cl3 Cl 0.65837(18) 0.7313(2) 0.20350(13) 0.0941(8) Uani 1 1 d . . . Cl4 Cl 0.74308(19) 0.5162(2) 0.21749(11) 0.0912(7) Uani 1 1 d . . . Cl5 Cl 0.82973(18) 0.6875(3) 0.16205(15) 0.1209(11) Uani 1 1 d . . . P1 P 0.23352(9) 0.38785(10) 0.11102(5) 0.0237(3) Uani 1 1 d . . . P2 P 0.39499(9) 0.17642(10) 0.13267(5) 0.0220(3) Uani 1 1 d . . . O1 O 0.0758(4) -0.0636(4) -0.0530(2) 0.0696(15) Uani 1 1 d . . . O2 O 0.4382(9) 0.5886(11) 0.0415(5) 0.058(5) Uani 0.374(13) 1 d P . . O3 O 0.1404(9) 0.0162(13) -0.1483(5) 0.142(6) Uani 0.626(13) 1 d P . . N1 N 0.1165(3) 0.1868(4) -0.01566(19) 0.0302(10) Uani 1 1 d . . . H1N H 0.130(4) 0.125(5) -0.005(2) 0.035(17) Uiso 1 1 d . . . N2 N 0.1660(3) 0.2726(3) 0.00849(17) 0.0266(9) Uani 1 1 d . . . N3 N 0.3358(3) 0.1567(4) -0.03778(18) 0.0335(11) Uani 1 1 d . . . H3N H 0.332(4) 0.224(5) -0.050(2) 0.034(16) Uiso 1 1 d . . . N4 N 0.3339(3) 0.1291(3) 0.01583(16) 0.0262(9) Uani 1 1 d . . . C1 C 0.1264(4) 0.3683(4) 0.1395(2) 0.0276(11) Uani 1 1 d . . . C2 C 0.0836(4) 0.4581(4) 0.1611(2) 0.0316(12) Uani 1 1 d . . . H2 H 0.1132 0.5271 0.1633 0.038 Uiso 1 1 calc R . . C3 C -0.0014(4) 0.4458(5) 0.1791(2) 0.0369(13) Uani 1 1 d . . . H3 H -0.0299 0.5062 0.1942 0.044 Uiso 1 1 calc R . . C4 C -0.0450(4) 0.3460(5) 0.1752(2) 0.0423(14) Uani 1 1 d . . . H4 H -0.1032 0.3377 0.1879 0.051 Uiso 1 1 calc R . . C5 C -0.0045(4) 0.2593(5) 0.1533(2) 0.0387(13) Uani 1 1 d . . . H5 H -0.0355 0.1912 0.15 0.046 Uiso 1 1 calc R . . C6 C 0.0816(4) 0.2693(4) 0.1356(2) 0.0315(12) Uani 1 1 d . . . H6 H 0.1094 0.2082 0.1208 0.038 Uiso 1 1 calc R . . C7 C 0.3191(4) 0.4505(4) 0.1632(2) 0.0331(13) Uani 1 1 d . . . C8 C 0.4027(4) 0.4799(4) 0.1446(3) 0.0436(15) Uani 1 1 d . . . H8 H 0.4097 0.4694 0.1066 0.052 Uiso 1 1 calc R . . C9 C 0.4745(5) 0.5239(5) 0.1816(4) 0.064(2) Uani 1 1 d . . . H9 H 0.5309 0.5434 0.1689 0.077 Uiso 1 1 calc R . . C10 C 0.4644(6) 0.5391(5) 0.2359(4) 0.071(3) Uani 1 1 d . . . H10 H 0.514 0.5697 0.2612 0.085 Uiso 1 1 calc R . . C11 C 0.3839(6) 0.5111(5) 0.2548(3) 0.062(2) Uani 1 1 d . . . H11 H 0.3784 0.5227 0.2931 0.075 Uiso 1 1 calc R . . C12 C 0.3088(5) 0.4654(4) 0.2187(2) 0.0433(16) Uani 1 1 d . . . H12 H 0.253 0.4455 0.232 0.052 Uiso 1 1 calc R . . C13 C 0.2027(3) 0.4944(4) 0.0584(2) 0.0224(10) Uani 1 1 d . . . C14 C 0.2247(4) 0.6025(4) 0.0729(2) 0.0281(11) Uani 1 1 d . . . H14 H 0.2601 0.6183 0.1083 0.034 Uiso 1 1 calc R . . C15 C 0.1956(4) 0.6869(4) 0.0362(2) 0.0285(11) Uani 1 1 d . . . H15 H 0.2106 0.76 0.0467 0.034 Uiso 1 1 calc R . . C16 C 0.1448(4) 0.6642(4) -0.0153(2) 0.0309(12) Uani 1 1 d . . . H16 H 0.1245 0.7216 -0.0404 0.037 Uiso 1 1 calc R . . C17 C 0.1233(4) 0.5582(4) -0.0303(2) 0.0300(12) Uani 1 1 d . . . H17 H 0.0891 0.5433 -0.0662 0.036 Uiso 1 1 calc R . . C18 C 0.1508(3) 0.4723(4) 0.0061(2) 0.0222(10) Uani 1 1 d . . . C19 C 0.1207(3) 0.3619(4) -0.0120(2) 0.0241(10) Uani 1 1 d . . . C20 C 0.0426(4) 0.3310(4) -0.0497(2) 0.0308(12) Uani 1 1 d . . . H20 H -0.0011 0.3779 -0.0709 0.037 Uiso 1 1 calc R . . C21 C 0.0417(4) 0.2197(4) -0.0498(2) 0.0330(12) Uani 1 1 d . . . H21 H -0.004 0.1745 -0.0704 0.04 Uiso 1 1 calc R . . C22 C 0.5131(4) 0.2076(4) 0.1227(2) 0.0275(11) Uani 1 1 d . . . C23 C 0.5871(4) 0.1538(5) 0.1546(2) 0.0364(13) Uani 1 1 d . . . H23 H 0.5755 0.1001 0.1809 0.044 Uiso 1 1 calc R . . C24 C 0.6774(4) 0.1785(7) 0.1479(3) 0.0544(19) Uani 1 1 d . . . H24 H 0.7276 0.1419 0.1698 0.065 Uiso 1 1 calc R . . C25 C 0.6951(5) 0.2559(7) 0.1094(3) 0.068(2) Uani 1 1 d . . . H25 H 0.7572 0.2729 0.105 0.081 Uiso 1 1 calc R . . C26 C 0.6230(6) 0.3074(6) 0.0779(3) 0.061(2) Uani 1 1 d . . . H26 H 0.6354 0.3605 0.0515 0.073 Uiso 1 1 calc R . . C27 C 0.5304(4) 0.2839(5) 0.0836(2) 0.0394(14) Uani 1 1 d . . . H27 H 0.4807 0.3199 0.0609 0.047 Uiso 1 1 calc R . . C28 C 0.3849(3) 0.2071(4) 0.2054(2) 0.0241(10) Uani 1 1 d . . . C29 C 0.4575(4) 0.2513(4) 0.2427(2) 0.0289(11) Uani 1 1 d . . . H29 H 0.516 0.2641 0.2312 0.035 Uiso 1 1 calc R . . C30 C 0.4437(4) 0.2764(5) 0.2969(2) 0.0372(13) Uani 1 1 d . . . H30 H 0.4932 0.306 0.3226 0.045 Uiso 1 1 calc R . . C31 C 0.3585(4) 0.2588(4) 0.3136(2) 0.0379(13) Uani 1 1 d . . . H31 H 0.3492 0.2771 0.3505 0.046 Uiso 1 1 calc R . . C32 C 0.2865(4) 0.2142(4) 0.2764(2) 0.0350(13) Uani 1 1 d . . . H32 H 0.2278 0.2016 0.2878 0.042 Uiso 1 1 calc R . . C33 C 0.3005(4) 0.1880(4) 0.2223(2) 0.0291(11) Uani 1 1 d . . . H33 H 0.2514 0.1568 0.197 0.035 Uiso 1 1 calc R . . C34 C 0.3903(3) 0.0271(4) 0.1285(2) 0.0237(10) Uani 1 1 d . . . C35 C 0.4066(4) -0.0326(4) 0.1781(2) 0.0317(12) Uani 1 1 d . . . H35 H 0.4111 0.004 0.213 0.038 Uiso 1 1 calc R . . C36 C 0.4161(4) -0.1439(4) 0.1770(2) 0.0374(13) Uani 1 1 d . . . H36 H 0.4277 -0.1835 0.2111 0.045 Uiso 1 1 calc R . . C37 C 0.4090(4) -0.1978(4) 0.1266(3) 0.0367(13) Uani 1 1 d . . . H37 H 0.4161 -0.2745 0.126 0.044 Uiso 1 1 calc R . . C38 C 0.3915(4) -0.1409(4) 0.0774(2) 0.0324(12) Uani 1 1 d . . . H38 H 0.3862 -0.1789 0.0428 0.039 Uiso 1 1 calc R . . C39 C 0.3814(3) -0.0274(4) 0.0771(2) 0.0264(11) Uani 1 1 d . . . C40 C 0.3669(4) 0.0278(4) 0.0225(2) 0.0264(11) Uani 1 1 d . . . C41 C 0.3874(4) -0.0093(5) -0.0289(2) 0.0390(14) Uani 1 1 d . . . H41 H 0.4102 -0.079 -0.0367 0.047 Uiso 1 1 calc R . . C42 C 0.3681(4) 0.0750(5) -0.0654(2) 0.0406(14) Uani 1 1 d . . . H42 H 0.3763 0.0754 -0.1037 0.049 Uiso 1 1 calc R . . C43 C 0.7255(6) 0.6308(8) 0.1727(4) 0.075(2) Uani 1 1 d . . . H43 H 0.6903 0.6077 0.1358 0.09 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 Pd 0.0295(2) 0.0183(2) 0.0199(2) -0.00085(14) -0.00279(14) 0.00486(15) Cl1 0.0473(9) 0.0339(8) 0.0592(10) 0.0107(7) -0.0027(7) -0.0005(6) Cl2 0.0922(16) 0.0428(10) 0.1137(19) -0.0042(11) -0.0065(14) -0.0002(10) Cl3 0.0773(16) 0.0911(17) 0.120(2) -0.0016(15) 0.0331(15) 0.0068(13) Cl4 0.0949(18) 0.0937(17) 0.0843(16) 0.0073(13) 0.0108(13) 0.0135(14) Cl5 0.0600(15) 0.152(3) 0.156(3) 0.023(2) 0.0325(17) -0.0155(16) P1 0.0307(7) 0.0172(6) 0.0209(6) -0.0011(5) -0.0030(5) 0.0033(5) P2 0.0254(7) 0.0190(6) 0.0206(6) 0.0015(5) 0.0003(5) 0.0029(5) O1 0.069(3) 0.059(3) 0.082(4) 0.000(3) 0.014(3) 0.013(3) O2 0.054(8) 0.078(10) 0.046(8) 0.015(6) 0.019(6) 0.000(7) O3 0.127(11) 0.195(15) 0.083(8) -0.039(9) -0.050(7) 0.048(10) N1 0.037(3) 0.020(2) 0.032(3) -0.0025(19) -0.001(2) -0.0011(19) N2 0.033(2) 0.022(2) 0.024(2) -0.0016(16) -0.0012(18) 0.0010(17) N3 0.046(3) 0.030(3) 0.024(2) 0.0017(19) 0.004(2) 0.005(2) N4 0.035(2) 0.025(2) 0.018(2) -0.0001(16) 0.0047(18) 0.0037(18) C1 0.037(3) 0.026(3) 0.018(2) 0.0039(19) -0.001(2) 0.002(2) C2 0.044(3) 0.030(3) 0.020(3) -0.002(2) 0.000(2) 0.002(2) C3 0.043(3) 0.041(3) 0.025(3) -0.001(2) 0.003(2) 0.013(3) C4 0.037(3) 0.060(4) 0.029(3) 0.005(3) 0.004(3) 0.000(3) C5 0.040(3) 0.042(3) 0.031(3) 0.001(3) -0.003(2) -0.011(3) C6 0.041(3) 0.027(3) 0.025(3) 0.002(2) -0.001(2) 0.002(2) C7 0.041(3) 0.017(2) 0.036(3) -0.001(2) -0.011(2) 0.008(2) C8 0.042(4) 0.022(3) 0.058(4) -0.001(3) -0.018(3) 0.003(2) C9 0.047(4) 0.030(3) 0.103(7) -0.003(4) -0.027(4) -0.002(3) C10 0.069(6) 0.033(4) 0.094(7) -0.023(4) -0.043(5) 0.008(3) C11 0.086(6) 0.040(4) 0.048(4) -0.020(3) -0.033(4) 0.032(4) C12 0.057(4) 0.028(3) 0.036(3) -0.007(2) -0.021(3) 0.016(3) C13 0.023(3) 0.022(2) 0.023(2) 0.0011(19) 0.003(2) 0.0034(19) C14 0.032(3) 0.021(2) 0.031(3) -0.003(2) 0.001(2) 0.001(2) C15 0.030(3) 0.018(2) 0.038(3) 0.001(2) 0.006(2) 0.001(2) C16 0.034(3) 0.027(3) 0.033(3) 0.010(2) 0.007(2) 0.004(2) C17 0.038(3) 0.028(3) 0.023(3) 0.004(2) 0.004(2) 0.003(2) C18 0.024(3) 0.022(2) 0.021(2) 0.0001(19) 0.005(2) 0.0022(19) C19 0.028(3) 0.025(3) 0.018(2) 0.0038(19) 0.002(2) 0.004(2) C20 0.029(3) 0.036(3) 0.023(3) 0.003(2) -0.006(2) -0.001(2) C21 0.033(3) 0.032(3) 0.031(3) 0.001(2) -0.006(2) -0.004(2) C22 0.033(3) 0.027(3) 0.022(3) -0.005(2) 0.005(2) -0.003(2) C23 0.030(3) 0.052(4) 0.027(3) -0.008(2) 0.003(2) 0.003(3) C24 0.027(3) 0.092(6) 0.042(4) -0.022(4) 0.000(3) 0.001(3) C25 0.041(4) 0.105(7) 0.060(5) -0.027(5) 0.016(4) -0.026(4) C26 0.081(6) 0.055(4) 0.054(4) -0.009(3) 0.032(4) -0.037(4) C27 0.052(4) 0.032(3) 0.035(3) -0.001(2) 0.011(3) -0.011(3) C28 0.029(3) 0.020(2) 0.022(3) 0.0036(19) -0.001(2) 0.005(2) C29 0.032(3) 0.028(3) 0.026(3) 0.000(2) 0.002(2) 0.004(2) C30 0.049(4) 0.035(3) 0.026(3) -0.003(2) -0.002(3) 0.002(3) C31 0.059(4) 0.029(3) 0.028(3) -0.003(2) 0.013(3) 0.001(3) C32 0.043(3) 0.029(3) 0.036(3) 0.003(2) 0.013(3) 0.004(2) C33 0.033(3) 0.024(3) 0.030(3) 0.003(2) 0.003(2) 0.004(2) C34 0.023(3) 0.018(2) 0.030(3) 0.0020(19) 0.002(2) -0.0004(19) C35 0.039(3) 0.023(3) 0.031(3) 0.007(2) -0.001(2) 0.000(2) C36 0.044(3) 0.025(3) 0.040(3) 0.014(2) -0.005(3) -0.002(2) C37 0.039(3) 0.017(3) 0.051(4) 0.003(2) -0.002(3) 0.002(2) C38 0.031(3) 0.023(3) 0.042(3) -0.005(2) 0.000(2) -0.001(2) C39 0.023(3) 0.022(2) 0.034(3) -0.001(2) 0.003(2) 0.000(2) C40 0.029(3) 0.022(2) 0.027(3) -0.004(2) 0.001(2) 0.003(2) C41 0.052(4) 0.034(3) 0.032(3) -0.004(2) 0.009(3) 0.011(3) C42 0.052(4) 0.045(3) 0.026(3) -0.003(2) 0.009(3) 0.005(3) C43 0.055(5) 0.096(7) 0.075(6) 0.013(5) 0.009(4) -0.004(4) #----------------------------------------------------------------------------# # 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 Pd N2 2.072(4) . ? Pd N4 2.074(4) . ? Pd P2 2.2541(13) . ? Pd P1 2.2565(13) . ? Cl3 C43 1.806(9) . ? Cl4 C43 1.773(9) . ? Cl5 C43 1.726(8) . ? P1 C7 1.807(5) . ? P1 C1 1.815(5) . ? P1 C13 1.834(5) . ? P2 C22 1.814(5) . ? P2 C28 1.824(5) . ? P2 C34 1.842(5) . ? N1 C21 1.327(7) . ? N1 N2 1.360(6) . ? N1 H1N 0.82(6) . ? N2 C19 1.337(6) . ? N3 C42 1.332(7) . ? N3 N4 1.344(6) . ? N3 H3N 0.87(6) . ? N4 C40 1.337(6) . ? C1 C6 1.379(7) . ? C1 C2 1.408(7) . ? C2 C3 1.382(8) . ? C2 H2 0.95 . ? C3 C4 1.380(9) . ? C3 H3 0.95 . ? C4 C5 1.366(9) . ? C4 H4 0.95 . ? C5 C6 1.390(8) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.384(8) . ? C7 C8 1.409(9) . ? C8 C9 1.379(9) . ? C8 H8 0.95 . ? C9 C10 1.358(12) . ? C9 H9 0.95 . ? C10 C11 1.366(12) . ? C10 H10 0.95 . ? C11 C12 1.411(9) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C18 1.399(7) . ? C13 C14 1.401(7) . ? C14 C15 1.390(7) . ? C14 H14 0.95 . ? C15 C16 1.378(7) . ? C15 H15 0.95 . ? C16 C17 1.378(7) . ? C16 H16 0.95 . ? C17 C18 1.394(7) . ? C17 H17 0.95 . ? C18 C19 1.475(7) . ? C19 C20 1.398(7) . ? C20 C21 1.371(8) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 C27 1.383(8) . ? C22 C23 1.395(8) . ? C23 C24 1.384(8) . ? C23 H23 0.95 . ? C24 C25 1.383(11) . ? C24 H24 0.95 . ? C25 C26 1.357(11) . ? C25 H25 0.95 . ? C26 C27 1.407(9) . ? C26 H26 0.95 . ? C27 H27 0.95 . ? C28 C33 1.374(7) . ? C28 C29 1.393(7) . ? C29 C30 1.389(8) . ? C29 H29 0.95 . ? C30 C31 1.379(9) . ? C30 H30 0.95 . ? C31 C32 1.389(8) . ? C31 H31 0.95 . ? C32 C33 1.390(7) . ? C32 H32 0.95 . ? C33 H33 0.95 . ? C34 C35 1.395(7) . ? C34 C39 1.402(7) . ? C35 C36 1.379(7) . ? C35 H35 0.95 . ? C36 C37 1.377(8) . ? C36 H36 0.95 . ? C37 C38 1.371(8) . ? C37 H37 0.95 . ? C38 C39 1.405(7) . ? C38 H38 0.95 . ? C39 C40 1.471(7) . ? C40 C41 1.396(7) . ? C41 C42 1.365(8) . ? C41 H41 0.95 . ? C42 H42 0.95 . ? C43 H43 1 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd N4 92.77(16) . . ? N2 Pd P2 168.33(12) . . ? N4 Pd P2 83.63(12) . . ? N2 Pd P1 83.86(12) . . ? N4 Pd P1 169.39(12) . . ? P2 Pd P1 101.57(5) . . ? C7 P1 C1 109.5(3) . . ? C7 P1 C13 104.5(2) . . ? C1 P1 C13 102.9(2) . . ? C7 P1 Pd 115.77(18) . . ? C1 P1 Pd 115.16(17) . . ? C13 P1 Pd 107.62(16) . . ? C22 P2 C28 107.4(2) . . ? C22 P2 C34 103.4(2) . . ? C28 P2 C34 104.6(2) . . ? C22 P2 Pd 115.72(17) . . ? C28 P2 Pd 116.65(16) . . ? C34 P2 Pd 107.62(16) . . ? C21 N1 N2 111.2(4) . . ? C21 N1 H1N 128(4) . . ? N2 N1 H1N 120(4) . . ? C19 N2 N1 106.2(4) . . ? C19 N2 Pd 135.1(3) . . ? N1 N2 Pd 118.6(3) . . ? C42 N3 N4 110.7(5) . . ? C42 N3 H3N 123(4) . . ? N4 N3 H3N 124(4) . . ? C40 N4 N3 107.0(4) . . ? C40 N4 Pd 135.2(3) . . ? N3 N4 Pd 117.8(3) . . ? C6 C1 C2 119.2(5) . . ? C6 C1 P1 121.1(4) . . ? C2 C1 P1 119.4(4) . . ? C3 C2 C1 119.9(5) . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3 120 . . ? C2 C3 H3 120 . . ? C5 C4 C3 120.1(6) . . ? C5 C4 H4 120 . . ? C3 C4 H4 120 . . ? C4 C5 C6 120.8(5) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C1 C6 C5 119.8(5) . . ? C1 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C12 C7 C8 120.0(5) . . ? C12 C7 P1 124.6(5) . . ? C8 C7 P1 115.3(4) . . ? C9 C8 C7 120.2(7) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 119.9(8) . . ? C10 C9 H9 120 . . ? C8 C9 H9 120 . . ? C9 C10 C11 120.8(7) . . ? C9 C10 H10 119.6 . . ? C11 C10 H10 119.6 . . ? C10 C11 C12 121.3(7) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C7 C12 C11 117.7(7) . . ? C7 C12 H12 121.1 . . ? C11 C12 H12 121.1 . . ? C18 C13 C14 118.8(4) . . ? C18 C13 P1 122.0(4) . . ? C14 C13 P1 118.9(4) . . ? C15 C14 C13 121.0(5) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C16 C15 C14 119.6(5) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.0(5) . . ? C15 C16 H16 120 . . ? C17 C16 H16 120 . . ? C16 C17 C18 121.3(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 119.2(4) . . ? C17 C18 C19 117.9(4) . . ? C13 C18 C19 122.8(4) . . ? N2 C19 C20 109.0(4) . . ? N2 C19 C18 122.7(4) . . ? C20 C19 C18 128.3(4) . . ? C21 C20 C19 106.2(5) . . ? C21 C20 H20 126.9 . . ? C19 C20 H20 126.9 . . ? N1 C21 C20 107.3(5) . . ? N1 C21 H21 126.3 . . ? C20 C21 H21 126.3 . . ? C27 C22 C23 119.6(5) . . ? C27 C22 P2 120.7(4) . . ? C23 C22 P2 119.7(4) . . ? C24 C23 C22 120.0(6) . . ? C24 C23 H23 120 . . ? C22 C23 H23 120 . . ? C25 C24 C23 120.5(7) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C26 C25 C24 119.5(6) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 121.5(7) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C22 C27 C26 118.9(6) . . ? C22 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C33 C28 C29 120.0(5) . . ? C33 C28 P2 117.3(4) . . ? C29 C28 P2 122.8(4) . . ? C30 C29 C28 119.6(5) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 120.4(5) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 119.9(5) . . ? C30 C31 H31 120 . . ? C32 C31 H31 120 . . ? C31 C32 C33 119.7(5) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C28 C33 C32 120.4(5) . . ? C28 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C39 119.4(5) . . ? C35 C34 P2 118.6(4) . . ? C39 C34 P2 121.6(4) . . ? C36 C35 C34 120.8(5) . . ? C36 C35 H35 119.6 . . ? C34 C35 H35 119.6 . . ? C37 C36 C35 120.1(5) . . ? C37 C36 H36 120 . . ? C35 C36 H36 120 . . ? C38 C37 C36 120.1(5) . . ? C38 C37 H37 120 . . ? C36 C37 H37 120 . . ? C37 C38 C39 121.2(5) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.4 . . ? C34 C39 C38 118.4(5) . . ? C34 C39 C40 123.7(4) . . ? C38 C39 C40 117.7(5) . . ? N4 C40 C41 108.6(5) . . ? N4 C40 C39 122.7(4) . . ? C41 C40 C39 128.6(5) . . ? C42 C41 C40 106.0(5) . . ? C42 C41 H41 127 . . ? C40 C41 H41 127 . . ? N3 C42 C41 107.6(5) . . ? N3 C42 H42 126.2 . . ? C41 C42 H42 126.2 . . ? Cl5 C43 Cl4 111.3(5) . . ? Cl5 C43 Cl3 109.1(5) . . ? Cl4 C43 Cl3 109.3(5) . . ? Cl5 C43 H43 109 . . ? Cl4 C43 H43 109 . . ? Cl3 C43 H43 109 . . ? #===END data_(2b)-sep106 _database_code_depnum_ccdc_archive 'CCDC 640792' _audit_creation_date 2006-09-01T14:07:24-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H34 Cl2 N4 O2 P2 Pd, 4(C H Cl3)' _chemical_formula_sum 'C46 H38 Cl14 N4 O2 P2 Pd' _chemical_formula_weight 1343.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 10.1514(3) _cell_length_b 11.8973(3) _cell_length_c 12.9736(3) _cell_angle_alpha 74.004(1) _cell_angle_beta 67.062(1) _cell_angle_gamma 77.013(2) _cell_volume 1374.87(6) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10505 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.623 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6864 _exptl_absorpt_correction_T_max 0.8305 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.121047E-1 _diffrn_orient_matrix_ub_12 0.372495E-1 _diffrn_orient_matrix_ub_13 -0.817414E-1 _diffrn_orient_matrix_ub_21 -0.828732E-1 _diffrn_orient_matrix_ub_22 0.620707E-1 _diffrn_orient_matrix_ub_23 0.253096E-1 _diffrn_orient_matrix_ub_31 0.680583E-1 _diffrn_orient_matrix_ub_32 0.504168E-1 _diffrn_orient_matrix_ub_33 -0.21418E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0421 _diffrn_reflns_av_unetI/netI 0.0315 _diffrn_reflns_number 18377 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 25.98 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 5368 _reflns_number_gt 4860 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atom on N1 was refined; other H atoms were in riding mode. 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^)+(0.0689P)^2^+3.3877P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5368 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0471 _refine_ls_R_factor_gt 0.042 _refine_ls_wR_factor_ref 0.1151 _refine_ls_wR_factor_gt 0.1105 _refine_ls_goodness_of_fit_ref 0.932 _refine_ls_restrained_S_all 0.932 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.262 _refine_diff_density_min -1.106 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 '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' 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 Pd Pd 0.5 0.5 0.5 0.01719(11) Uani 1 2 d S . . Cl1 Cl 0.47912(8) 0.33704(7) 0.64744(6) 0.02583(18) Uani 1 1 d . . . P1 P 0.73008(8) 0.31243(7) 0.11931(6) 0.02008(17) Uani 1 1 d . . . O1 O 0.7480(2) 0.41357(19) 0.15814(18) 0.0241(4) Uani 1 1 d . . . N1 N 0.4766(3) 0.4219(2) 0.3110(2) 0.0202(5) Uani 1 1 d . . . H1N H 0.560(4) 0.449(3) 0.269(3) 0.026(9) Uiso 1 1 d . . . N2 N 0.4220(3) 0.4186(2) 0.4244(2) 0.0214(5) Uani 1 1 d . . . C1 C 0.7088(3) 0.1795(3) 0.2296(3) 0.0246(6) Uani 1 1 d . . . C2 C 0.7624(5) 0.1682(4) 0.3165(3) 0.0448(9) Uani 1 1 d . . . H2 H 0.8109 0.2284 0.3152 0.054 Uiso 1 1 calc R . . C3 C 0.7449(6) 0.0694(4) 0.4044(4) 0.0608(13) Uani 1 1 d . . . H3 H 0.7816 0.062 0.4634 0.073 Uiso 1 1 calc R . . C4 C 0.6744(5) -0.0187(4) 0.4071(4) 0.0533(12) Uani 1 1 d . . . H4 H 0.6621 -0.0862 0.4679 0.064 Uiso 1 1 calc R . . C5 C 0.6223(4) -0.0083(3) 0.3215(3) 0.0426(9) Uani 1 1 d . . . H5 H 0.5746 -0.0691 0.3229 0.051 Uiso 1 1 calc R . . C6 C 0.6387(4) 0.0901(3) 0.2332(3) 0.0320(7) Uani 1 1 d . . . H6 H 0.6017 0.0966 0.1746 0.038 Uiso 1 1 calc R . . C7 C 0.8838(3) 0.2812(3) -0.0038(3) 0.0238(6) Uani 1 1 d . . . C8 C 0.9144(4) 0.1748(3) -0.0400(3) 0.0287(7) Uani 1 1 d . . . H8 H 0.852 0.116 0 0.034 Uiso 1 1 calc R . . C9 C 1.0357(4) 0.1554(3) -0.1340(3) 0.0319(7) Uani 1 1 d . . . H9 H 1.0559 0.0836 -0.1593 0.038 Uiso 1 1 calc R . . C10 C 1.1279(4) 0.2405(3) -0.1915(3) 0.0319(7) Uani 1 1 d . . . H10 H 1.2118 0.2263 -0.2554 0.038 Uiso 1 1 calc R . . C11 C 1.0982(4) 0.3462(3) -0.1563(3) 0.0312(7) Uani 1 1 d . . . H11 H 1.1615 0.4043 -0.1957 0.037 Uiso 1 1 calc R . . C12 C 0.9754(3) 0.3667(3) -0.0629(3) 0.0259(6) Uani 1 1 d . . . H12 H 0.954 0.4397 -0.0395 0.031 Uiso 1 1 calc R . . C13 C 0.5702(3) 0.3368(2) 0.0812(2) 0.0210(6) Uani 1 1 d . . . C14 C 0.5837(4) 0.3326(3) -0.0290(3) 0.0252(6) Uani 1 1 d . . . H14 H 0.6771 0.3216 -0.0848 0.03 Uiso 1 1 calc R . . C15 C 0.4624(4) 0.3443(3) -0.0586(3) 0.0292(7) Uani 1 1 d . . . H15 H 0.4735 0.3406 -0.1338 0.035 Uiso 1 1 calc R . . C16 C 0.3266(4) 0.3612(3) 0.0215(3) 0.0279(7) Uani 1 1 d . . . H16 H 0.2438 0.3681 0.0018 0.033 Uiso 1 1 calc R . . C17 C 0.3103(4) 0.3682(3) 0.1310(3) 0.0251(6) Uani 1 1 d . . . H17 H 0.2162 0.3812 0.1853 0.03 Uiso 1 1 calc R . . C18 C 0.4302(3) 0.3564(2) 0.1625(2) 0.0195(6) Uani 1 1 d . . . C19 C 0.4010(3) 0.3646(2) 0.2812(2) 0.0192(6) Uani 1 1 d . . . C20 C 0.2901(3) 0.3247(3) 0.3807(3) 0.0251(6) Uani 1 1 d . . . H20 H 0.2171 0.2821 0.3881 0.03 Uiso 1 1 calc R . . C21 C 0.3083(3) 0.3599(3) 0.4670(3) 0.0248(6) Uani 1 1 d . . . H21 H 0.2484 0.3444 0.5454 0.03 Uiso 1 1 calc R . . C22 C 0.8553(4) 0.2974(4) 0.5586(4) 0.0533(11) Uani 1 1 d . A 1 H22 H 0.7535 0.2802 0.5885 0.064 Uiso 1 1 calc R A 1 Cl2 Cl 0.89276(12) 0.38205(11) 0.41836(11) 0.0584(3) Uani 1 1 d . A 1 Cl3 Cl 0.87324(18) 0.37432(12) 0.64925(13) 0.0746(4) Uani 1 1 d . A 1 Cl4 Cl 0.97012(15) 0.16268(11) 0.56113(15) 0.0870(5) Uani 1 1 d . A 1 C23 C 0.3006(5) 0.0638(4) 0.1504(4) 0.0511(10) Uani 1 1 d . B 1 H23 H 0.377 0.1172 0.1103 0.061 Uiso 1 1 calc R B 1 Cl5 Cl 0.3855(2) -0.08144(13) 0.1619(2) 0.1091(7) Uani 1 1 d . B 1 Cl6 Cl 0.2076(3) 0.09096(16) 0.28665(14) 0.1264(9) Uani 1 1 d . B 1 Cl7 Cl 0.1916(3) 0.09160(14) 0.0717(2) 0.1221(9) Uani 1 1 d . B 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pd 0.01818(17) 0.02176(17) 0.01289(16) -0.00432(12) -0.00513(12) -0.00481(12) Cl1 0.0308(4) 0.0280(4) 0.0205(3) 0.0018(3) -0.0118(3) -0.0111(3) P1 0.0213(4) 0.0219(4) 0.0182(4) -0.0052(3) -0.0067(3) -0.0044(3) O1 0.0236(11) 0.0264(11) 0.0263(11) -0.0094(9) -0.0085(9) -0.0069(9) N1 0.0218(13) 0.0248(13) 0.0164(11) -0.0062(10) -0.0060(10) -0.0068(10) N2 0.0237(13) 0.0263(13) 0.0153(11) -0.0045(10) -0.0068(10) -0.0056(10) C1 0.0211(15) 0.0252(15) 0.0244(15) -0.0058(12) -0.0058(12) -0.0001(12) C2 0.061(3) 0.042(2) 0.039(2) 0.0002(17) -0.031(2) -0.0077(19) C3 0.084(4) 0.056(3) 0.042(2) 0.006(2) -0.038(2) 0.000(2) C4 0.058(3) 0.036(2) 0.039(2) 0.0100(17) -0.008(2) 0.0061(19) C5 0.034(2) 0.0247(17) 0.049(2) 0.0000(16) 0.0007(17) -0.0033(14) C6 0.0293(17) 0.0287(17) 0.0322(17) -0.0028(14) -0.0075(14) -0.0027(13) C7 0.0237(15) 0.0278(15) 0.0208(14) -0.0052(12) -0.0075(12) -0.0056(12) C8 0.0290(17) 0.0260(16) 0.0295(16) -0.0070(13) -0.0058(13) -0.0074(13) C9 0.0348(18) 0.0289(17) 0.0296(17) -0.0114(14) -0.0067(14) -0.0016(14) C10 0.0260(16) 0.0389(18) 0.0238(16) -0.0066(14) -0.0019(13) -0.0036(14) C11 0.0271(17) 0.0361(18) 0.0278(16) -0.0029(14) -0.0060(13) -0.0106(14) C12 0.0255(16) 0.0269(15) 0.0274(16) -0.0072(13) -0.0085(13) -0.0066(12) C13 0.0269(15) 0.0176(13) 0.0214(14) -0.0018(11) -0.0118(12) -0.0055(11) C14 0.0336(17) 0.0238(15) 0.0189(14) -0.0044(12) -0.0091(13) -0.0055(13) C15 0.049(2) 0.0254(15) 0.0213(15) -0.0029(12) -0.0220(15) -0.0063(14) C16 0.0389(18) 0.0223(15) 0.0324(17) -0.0025(13) -0.0242(15) -0.0058(13) C17 0.0280(16) 0.0238(15) 0.0290(16) -0.0037(12) -0.0158(13) -0.0055(12) C18 0.0269(15) 0.0154(13) 0.0202(14) -0.0021(11) -0.0124(12) -0.0046(11) C19 0.0213(14) 0.0179(13) 0.0206(14) -0.0041(11) -0.0099(11) -0.0019(11) C20 0.0248(15) 0.0290(16) 0.0246(15) -0.0052(12) -0.0086(12) -0.0103(12) C21 0.0228(15) 0.0315(16) 0.0190(14) -0.0050(12) -0.0031(12) -0.0096(12) C22 0.030(2) 0.049(2) 0.078(3) -0.018(2) -0.011(2) -0.0062(17) Cl2 0.0452(6) 0.0637(7) 0.0667(7) -0.0242(6) -0.0167(5) -0.0005(5) Cl3 0.1007(11) 0.0588(7) 0.0839(9) -0.0107(7) -0.0609(9) -0.0016(7) Cl4 0.0564(7) 0.0371(6) 0.1213(13) -0.0047(7) 0.0090(8) -0.0050(5) C23 0.060(3) 0.036(2) 0.063(3) -0.0066(19) -0.030(2) -0.0079(19) Cl5 0.1053(13) 0.0405(7) 0.1634(19) -0.0062(9) -0.0497(13) 0.0113(7) Cl6 0.228(3) 0.0750(10) 0.0641(9) -0.0159(8) -0.0022(12) -0.0844(14) Cl7 0.186(2) 0.0598(8) 0.194(2) 0.0144(11) -0.1606(19) -0.0384(11) #----------------------------------------------------------------------------# # 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 Pd N2 1.999(2) . ? Pd N2 1.999(2) 2_666 ? Pd Cl1 2.2995(7) 2_666 ? Pd Cl1 2.2995(7) . ? P1 O1 1.496(2) . ? P1 C7 1.802(3) . ? P1 C1 1.806(3) . ? P1 C13 1.817(3) . ? N1 C19 1.348(4) . ? N1 N2 1.348(3) . ? N1 H1N 0.89(4) . ? N2 C21 1.334(4) . ? C1 C6 1.388(5) . ? C1 C2 1.394(5) . ? C2 C3 1.382(6) . ? C2 H2 0.95 . ? C3 C4 1.382(7) . ? C3 H3 0.95 . ? C4 C5 1.371(7) . ? C4 H4 0.95 . ? C5 C6 1.382(5) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.388(4) . ? C7 C8 1.398(4) . ? C8 C9 1.384(5) . ? C8 H8 0.95 . ? C9 C10 1.387(5) . ? C9 H9 0.95 . ? C10 C11 1.386(5) . ? C10 H10 0.95 . ? C11 C12 1.389(5) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C14 1.395(4) . ? C13 C18 1.416(4) . ? C14 C15 1.395(5) . ? C14 H14 0.95 . ? C15 C16 1.376(5) . ? C15 H15 0.95 . ? C16 C17 1.389(4) . ? C16 H16 0.95 . ? C17 C18 1.396(4) . ? C17 H17 0.95 . ? C18 C19 1.477(4) . ? C19 C20 1.389(4) . ? C20 C21 1.384(4) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 Cl4 1.758(5) . ? C22 Cl3 1.758(5) . ? C22 Cl2 1.758(5) . ? C22 H22 1 . ? C23 Cl7 1.704(5) . ? C23 Cl6 1.731(5) . ? C23 Cl5 1.744(4) . ? C23 H23 1 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd N2 180.00(11) . 2_666 ? N2 Pd Cl1 90.81(7) . 2_666 ? N2 Pd Cl1 89.19(7) 2_666 2_666 ? N2 Pd Cl1 89.19(7) . . ? N2 Pd Cl1 90.81(7) 2_666 . ? Cl1 Pd Cl1 180.00(3) 2_666 . ? O1 P1 C7 110.61(13) . . ? O1 P1 C1 112.41(14) . . ? C7 P1 C1 108.23(14) . . ? O1 P1 C13 113.88(13) . . ? C7 P1 C13 107.42(14) . . ? C1 P1 C13 103.90(14) . . ? C19 N1 N2 111.1(2) . . ? C19 N1 H1N 128(2) . . ? N2 N1 H1N 120(2) . . ? C21 N2 N1 106.4(2) . . ? C21 N2 Pd 130.6(2) . . ? N1 N2 Pd 122.87(19) . . ? C6 C1 C2 118.9(3) . . ? C6 C1 P1 123.0(3) . . ? C2 C1 P1 118.1(3) . . ? C3 C2 C1 120.1(4) . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C4 C3 C2 120.4(4) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 119.7(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C5 C6 C1 120.4(4) . . ? C5 C6 H6 119.8 . . ? C1 C6 H6 119.8 . . ? C12 C7 C8 119.6(3) . . ? C12 C7 P1 117.7(2) . . ? C8 C7 P1 122.7(2) . . ? C9 C8 C7 119.9(3) . . ? C9 C8 H8 120.1 . . ? C7 C8 H8 120.1 . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 120.3(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 119.7(3) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 120.4(3) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C18 118.8(3) . . ? C14 C13 P1 120.0(2) . . ? C18 C13 P1 121.2(2) . . ? C15 C14 C13 121.1(3) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C16 C15 C14 119.8(3) . . ? C16 C15 H15 120.1 . . ? C14 C15 H15 120.1 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C16 C17 C18 121.0(3) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C13 119.1(3) . . ? C17 C18 C19 116.7(3) . . ? C13 C18 C19 124.2(3) . . ? N1 C19 C20 106.6(3) . . ? N1 C19 C18 124.2(3) . . ? C20 C19 C18 129.0(3) . . ? C21 C20 C19 105.6(3) . . ? C21 C20 H20 127.2 . . ? C19 C20 H20 127.2 . . ? N2 C21 C20 110.3(3) . . ? N2 C21 H21 124.8 . . ? C20 C21 H21 124.8 . . ? Cl4 C22 Cl3 109.2(3) . . ? Cl4 C22 Cl2 111.1(3) . . ? Cl3 C22 Cl2 111.2(2) . . ? Cl4 C22 H22 108.4 . . ? Cl3 C22 H22 108.4 . . ? Cl2 C22 H22 108.4 . . ? Cl7 C23 Cl6 112.3(3) . . ? Cl7 C23 Cl5 111.5(3) . . ? Cl6 C23 Cl5 108.7(3) . . ? Cl7 C23 H23 108 . . ? Cl6 C23 H23 108 . . ? Cl5 C23 H23 108 . . ? #===END data_(2c)-sep206 _database_code_depnum_ccdc_archive 'CCDC 640793' _audit_creation_date 2006-09-04T09:33:38-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C42 H34 N4 O2 P2 Pd, 4(C H Cl3), 2(Cl O4)' _chemical_formula_sum 'C46 H38 Cl14 N4 O10 P2 Pd' _chemical_formula_weight 1471.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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 8.5748(3) _cell_length_b 19.1391(7) _cell_length_c 17.7847(6) _cell_angle_alpha 90 _cell_angle_beta 91.343(2) _cell_angle_gamma 90 _cell_volume 2917.92(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10936 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.675 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.071 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.9003 _exptl_absorpt_correction_T_max 0.9756 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.112973 _diffrn_orient_matrix_ub_12 0.64765E-2 _diffrn_orient_matrix_ub_13 0.134312E-1 _diffrn_orient_matrix_ub_21 -0.223792E-1 _diffrn_orient_matrix_ub_22 0.483047E-1 _diffrn_orient_matrix_ub_23 0.182666E-1 _diffrn_orient_matrix_ub_31 -0.185503E-1 _diffrn_orient_matrix_ub_32 -0.188329E-1 _diffrn_orient_matrix_ub_33 0.514711E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_unetI/netI 0.0611 _diffrn_reflns_number 17925 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 26.03 _diffrn_reflns_theta_full 26.03 _diffrn_measured_fraction_theta_full 0.99 _diffrn_measured_fraction_theta_max 0.99 _reflns_number_total 5693 _reflns_number_gt 3921 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _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 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The H atom on N1 was refined; other H atoms were in riding mode. One of the CHCl3 solvate molecules is disordered and SADI restraints were applied to the component parts. 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^)+(0.0649P)^2^+8.7488P] 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 mixed _refine_ls_extinction_method none _refine_ls_number_reflns 5693 _refine_ls_number_parameters 366 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0976 _refine_ls_R_factor_gt 0.0596 _refine_ls_wR_factor_ref 0.1576 _refine_ls_wR_factor_gt 0.1364 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.194 _refine_diff_density_min -0.718 _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' Cl Cl 0.1484 0.1585 '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' 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 Pd Pd 0 0.5 0.5 0.03290(18) Uani 1 2 d S . . Cl7 Cl -0.24102(17) 0.36890(9) 0.67944(8) 0.0485(4) Uani 1 1 d . . . P1 P -0.07260(15) 0.35499(7) 0.42143(8) 0.0318(3) Uani 1 1 d . . . O1 O 0.0343(4) 0.39966(18) 0.4716(2) 0.0378(9) Uani 1 1 d . . . O2 O -0.3586(8) 0.3207(4) 0.6709(4) 0.124(3) Uani 1 1 d . . . O3 O -0.2578(7) 0.4251(3) 0.6272(3) 0.0953(19) Uani 1 1 d . . . O4 O -0.2338(14) 0.3954(4) 0.7504(3) 0.177(5) Uani 1 1 d . . . O5 O -0.0998(7) 0.3396(3) 0.6640(6) 0.153(4) Uani 1 1 d . . . N1 N -0.1412(6) 0.5670(3) 0.3684(3) 0.0422(12) Uani 1 1 d . . . H1N H -0.073(6) 0.589(3) 0.371(3) 0.022(15) Uiso 1 1 d . . . N2 N -0.1601(5) 0.5146(2) 0.4173(2) 0.0346(10) Uani 1 1 d . . . C1 C -0.0080(6) 0.2664(3) 0.4321(3) 0.0342(12) Uani 1 1 d . . . C2 C 0.0582(7) 0.2453(3) 0.5006(3) 0.0474(14) Uani 1 1 d . . . H2 H 0.0677 0.2776 0.541 0.057 Uiso 1 1 calc R . . C3 C 0.1100(8) 0.1774(3) 0.5099(4) 0.0618(18) Uani 1 1 d . . . H3 H 0.1552 0.1632 0.5567 0.074 Uiso 1 1 calc R . . C4 C 0.0965(9) 0.1305(3) 0.4516(4) 0.0642(19) Uani 1 1 d . . . H4 H 0.1336 0.0841 0.4581 0.077 Uiso 1 1 calc R . . C5 C 0.0293(9) 0.1505(3) 0.3840(4) 0.0610(19) Uani 1 1 d . . . H5 H 0.0184 0.1175 0.3443 0.073 Uiso 1 1 calc R . . C6 C -0.0227(7) 0.2184(3) 0.3735(3) 0.0465(14) Uani 1 1 d . . . H6 H -0.0682 0.2322 0.3266 0.056 Uiso 1 1 calc R . . C7 C -0.0627(6) 0.3798(3) 0.3247(3) 0.0345(12) Uani 1 1 d . . . C8 C -0.1707(7) 0.3551(3) 0.2711(3) 0.0484(15) Uani 1 1 d . . . H8 H -0.2517 0.3244 0.2859 0.058 Uiso 1 1 calc R . . C9 C -0.1602(9) 0.3753(4) 0.1961(4) 0.065(2) Uani 1 1 d . . . H9 H -0.2318 0.3576 0.1592 0.078 Uiso 1 1 calc R . . C10 C -0.0437(10) 0.4215(4) 0.1761(4) 0.068(2) Uani 1 1 d . . . H10 H -0.0369 0.4361 0.1252 0.081 Uiso 1 1 calc R . . C11 C 0.0610(9) 0.4461(3) 0.2283(4) 0.063(2) Uani 1 1 d . . . H11 H 0.1395 0.478 0.2137 0.076 Uiso 1 1 calc R . . C12 C 0.0538(7) 0.4249(3) 0.3025(4) 0.0481(15) Uani 1 1 d . . . H12 H 0.129 0.4414 0.3384 0.058 Uiso 1 1 calc R . . C13 C -0.2729(6) 0.3604(3) 0.4488(3) 0.0327(12) Uani 1 1 d . . . C14 C -0.3425(6) 0.3043(3) 0.4837(3) 0.0372(12) Uani 1 1 d . . . H14 H -0.2833 0.2632 0.4938 0.045 Uiso 1 1 calc R . . C15 C -0.4976(7) 0.3071(3) 0.5041(3) 0.0444(14) Uani 1 1 d . . . H15 H -0.5439 0.2685 0.5288 0.053 Uiso 1 1 calc R . . C16 C -0.5846(6) 0.3666(3) 0.4882(3) 0.0433(14) Uani 1 1 d . . . H16 H -0.6913 0.3684 0.5013 0.052 Uiso 1 1 calc R . . C17 C -0.5174(6) 0.4232(3) 0.4537(3) 0.0401(13) Uani 1 1 d . . . H17 H -0.5784 0.4636 0.4431 0.048 Uiso 1 1 calc R . . C18 C -0.3603(6) 0.4218(3) 0.4341(3) 0.0342(12) Uani 1 1 d . . . C19 C -0.2962(6) 0.4833(3) 0.3971(3) 0.0361(13) Uani 1 1 d . . . C20 C -0.3614(7) 0.5185(3) 0.3348(3) 0.0461(15) Uani 1 1 d . . . H20 H -0.4572 0.5085 0.3091 0.055 Uiso 1 1 calc R . . C21 C -0.2580(7) 0.5704(3) 0.3187(3) 0.0485(15) Uani 1 1 d . . . H21 H -0.2682 0.6032 0.2788 0.058 Uiso 1 1 calc R . . C22 C 0.3912(9) 0.5773(4) 0.0958(4) 0.081(2) Uani 0.733(4) 1 d PD A 1 H22 H 0.3387 0.6069 0.1341 0.098 Uiso 0.733(4) 1 calc PR A 1 Cl1 Cl 0.5588(4) 0.53134(18) 0.13676(16) 0.0860(10) Uani 0.733(4) 1 d PD A 1 Cl2 Cl 0.2656(4) 0.51015(15) 0.06152(17) 0.0870(10) Uani 0.733(4) 1 d PD A 1 Cl3 Cl 0.4473(5) 0.62653(16) 0.0191(2) 0.1108(15) Uani 0.733(4) 1 d PD A 1 C23 C 0.3761(8) 0.2245(4) 0.7225(3) 0.0574(17) Uani 1 1 d . B 1 H23 H 0.4449 0.2628 0.7042 0.069 Uiso 1 1 calc R B 1 Cl4 Cl 0.4229(3) 0.14827(13) 0.67504(17) 0.1056(9) Uani 1 1 d . B 1 Cl5 Cl 0.18171(19) 0.24798(9) 0.70254(9) 0.0559(4) Uani 1 1 d . B 1 Cl6 Cl 0.4054(3) 0.2166(3) 0.81814(13) 0.1656(18) Uani 1 1 d . B 1 C22A C 0.3912(9) 0.5773(4) 0.0958(4) 0.081(2) Uani 0.267(4) 1 d P A 2 H22A H 0.2997 0.5853 0.1286 0.098 Uiso 0.267(4) 1 calc PR A 2 Cl1A Cl 0.445(2) 0.5004(6) 0.1214(10) 0.202(8) Uiso 0.267(4) 1 d PD A 2 Cl2A Cl 0.3093(15) 0.5917(6) 0.0073(6) 0.134(5) Uiso 0.267(4) 1 d PD A 2 Cl3A Cl 0.5089(14) 0.6503(6) 0.1184(7) 0.137(5) Uiso 0.267(4) 1 d PD A 2 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 Pd 0.0184(3) 0.0362(3) 0.0442(3) -0.0102(3) 0.0018(2) -0.0014(2) Cl7 0.0360(8) 0.0700(10) 0.0395(7) 0.0001(7) 0.0036(6) -0.0069(7) P1 0.0194(6) 0.0347(7) 0.0414(7) -0.0065(6) 0.0027(5) -0.0003(5) O1 0.0247(18) 0.035(2) 0.054(2) -0.0128(17) -0.0009(16) 0.0031(16) O2 0.098(5) 0.161(7) 0.113(5) 0.033(5) -0.013(4) -0.088(5) O3 0.101(5) 0.102(4) 0.081(4) 0.037(3) -0.024(3) -0.023(4) O4 0.338(14) 0.150(7) 0.046(4) -0.016(4) 0.024(5) -0.073(8) O5 0.050(4) 0.074(4) 0.338(12) 0.028(6) 0.049(5) 0.009(3) N1 0.031(3) 0.042(3) 0.054(3) -0.004(2) 0.004(2) -0.006(2) N2 0.025(2) 0.035(3) 0.044(2) -0.006(2) 0.0027(19) -0.0007(18) C1 0.023(3) 0.035(3) 0.045(3) 0.003(2) 0.010(2) 0.004(2) C2 0.044(3) 0.046(4) 0.052(4) 0.001(3) -0.002(3) 0.001(3) C3 0.066(5) 0.053(4) 0.067(4) 0.008(4) -0.007(4) 0.010(4) C4 0.072(5) 0.040(4) 0.082(5) 0.001(4) 0.015(4) 0.010(3) C5 0.083(5) 0.038(4) 0.062(4) -0.010(3) 0.009(4) 0.006(3) C6 0.054(4) 0.040(3) 0.046(3) -0.006(3) 0.005(3) 0.004(3) C7 0.027(3) 0.035(3) 0.042(3) -0.003(2) 0.007(2) 0.005(2) C8 0.031(3) 0.067(4) 0.047(3) -0.001(3) 0.004(3) 0.004(3) C9 0.055(4) 0.093(6) 0.047(4) 0.000(4) 0.005(3) 0.018(4) C10 0.081(6) 0.072(5) 0.051(4) 0.018(4) 0.021(4) 0.025(4) C11 0.073(5) 0.048(4) 0.069(5) 0.008(3) 0.032(4) 0.005(4) C12 0.047(4) 0.040(3) 0.058(4) -0.009(3) 0.014(3) 0.001(3) C13 0.021(2) 0.040(3) 0.037(3) -0.009(2) 0.001(2) -0.002(2) C14 0.030(3) 0.045(3) 0.037(3) -0.008(2) 0.004(2) -0.002(2) C15 0.031(3) 0.056(4) 0.047(3) -0.011(3) 0.010(2) -0.006(3) C16 0.021(3) 0.052(4) 0.057(4) -0.021(3) 0.007(2) -0.004(3) C17 0.023(3) 0.050(3) 0.047(3) -0.014(3) -0.005(2) 0.006(3) C18 0.021(2) 0.041(3) 0.040(3) -0.014(2) 0.000(2) -0.001(2) C19 0.021(3) 0.040(3) 0.047(3) -0.012(2) 0.001(2) 0.002(2) C20 0.036(3) 0.046(4) 0.055(4) -0.006(3) -0.009(3) 0.007(3) C21 0.050(4) 0.042(3) 0.053(4) -0.001(3) -0.006(3) 0.005(3) C22 0.099(7) 0.061(5) 0.085(6) 0.004(4) 0.028(5) -0.004(5) Cl1 0.096(2) 0.098(2) 0.0641(17) 0.0003(15) -0.0083(15) -0.0052(18) Cl2 0.098(2) 0.078(2) 0.0847(19) -0.0111(15) 0.0083(17) -0.0251(16) Cl3 0.132(3) 0.068(2) 0.134(3) 0.0376(19) 0.042(2) -0.0014(19) C23 0.049(4) 0.074(5) 0.049(4) 0.007(3) 0.000(3) -0.005(3) Cl4 0.0564(13) 0.0860(15) 0.174(3) -0.0229(16) 0.0013(14) 0.0202(11) Cl5 0.0514(9) 0.0555(9) 0.0605(10) 0.0086(8) -0.0024(7) 0.0076(8) Cl6 0.0840(18) 0.358(5) 0.0540(13) 0.037(2) -0.0070(12) 0.069(3) C22A 0.099(7) 0.061(5) 0.085(6) 0.004(4) 0.028(5) -0.004(5) #----------------------------------------------------------------------------# # 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 Pd N2 2.008(4) 3_566 ? Pd N2 2.008(4) . ? Pd O1 2.009(3) . ? Pd O1 2.009(3) 3_566 ? Cl7 O4 1.361(6) . ? Cl7 O5 1.369(6) . ? Cl7 O2 1.373(6) . ? Cl7 O3 1.426(5) . ? P1 O1 1.526(4) . ? P1 C7 1.789(5) . ? P1 C1 1.793(5) . ? P1 C13 1.800(5) . ? N1 C21 1.322(8) . ? N1 N2 1.339(7) . ? N1 H1N 0.73(5) . ? N2 C19 1.353(7) . ? C1 C6 1.392(8) . ? C1 C2 1.392(8) . ? C2 C3 1.381(9) . ? C2 H2 0.95 . ? C3 C4 1.375(10) . ? C3 H3 0.95 . ? C4 C5 1.376(10) . ? C4 H4 0.95 . ? C5 C6 1.386(8) . ? C5 H5 0.95 . ? C6 H6 0.95 . ? C7 C12 1.385(8) . ? C7 C8 1.396(8) . ? C8 C9 1.395(9) . ? C8 H8 0.95 . ? C9 C10 1.386(10) . ? C9 H9 0.95 . ? C10 C11 1.361(10) . ? C10 H10 0.95 . ? C11 C12 1.383(9) . ? C11 H11 0.95 . ? C12 H12 0.95 . ? C13 C14 1.383(7) . ? C13 C18 1.415(7) . ? C14 C15 1.388(7) . ? C14 H14 0.95 . ? C15 C16 1.387(8) . ? C15 H15 0.95 . ? C16 C17 1.377(8) . ? C16 H16 0.95 . ? C17 C18 1.400(7) . ? C17 H17 0.95 . ? C18 C19 1.462(8) . ? C19 C20 1.403(8) . ? C20 C21 1.366(8) . ? C20 H20 0.95 . ? C21 H21 0.95 . ? C22 Cl3 1.735(7) . ? C22 Cl2 1.775(7) . ? C22 Cl1 1.823(8) . ? C22 H22 1 . ? C23 Cl6 1.721(7) . ? C23 Cl4 1.738(7) . ? C23 Cl5 1.754(7) . ? C23 H23 1 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pd N2 180.0000(10) 3_566 . ? N2 Pd O1 87.11(16) 3_566 . ? N2 Pd O1 92.89(16) . . ? N2 Pd O1 92.89(16) 3_566 3_566 ? N2 Pd O1 87.11(16) . 3_566 ? O1 Pd O1 180.0(2) . 3_566 ? O4 Cl7 O5 108.5(7) . . ? O4 Cl7 O2 111.8(5) . . ? O5 Cl7 O2 110.7(5) . . ? O4 Cl7 O3 108.9(5) . . ? O5 Cl7 O3 104.8(5) . . ? O2 Cl7 O3 111.9(4) . . ? O1 P1 C7 111.8(2) . . ? O1 P1 C1 106.7(2) . . ? C7 P1 C1 109.3(2) . . ? O1 P1 C13 111.9(2) . . ? C7 P1 C13 108.2(2) . . ? C1 P1 C13 108.7(2) . . ? P1 O1 Pd 126.4(2) . . ? C21 N1 N2 111.8(5) . . ? C21 N1 H1N 127(4) . . ? N2 N1 H1N 121(4) . . ? N1 N2 C19 106.0(5) . . ? N1 N2 Pd 119.3(3) . . ? C19 N2 Pd 134.7(4) . . ? C6 C1 C2 119.5(5) . . ? C6 C1 P1 121.5(4) . . ? C2 C1 P1 119.0(4) . . ? C3 C2 C1 120.0(6) . . ? C3 C2 H2 120 . . ? C1 C2 H2 120 . . ? C4 C3 C2 120.2(7) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.4(6) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 119.6(6) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? C12 C7 C8 119.2(5) . . ? C12 C7 P1 119.4(4) . . ? C8 C7 P1 121.4(4) . . ? C9 C8 C7 120.1(6) . . ? C9 C8 H8 119.9 . . ? C7 C8 H8 119.9 . . ? C10 C9 C8 119.1(7) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C11 C10 C9 120.9(7) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 120.4(7) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 120.2(6) . . ? C11 C12 H12 119.9 . . ? C7 C12 H12 119.9 . . ? C14 C13 C18 119.8(5) . . ? C14 C13 P1 120.1(4) . . ? C18 C13 P1 120.2(4) . . ? C13 C14 C15 120.9(5) . . ? C13 C14 H14 119.6 . . ? C15 C14 H14 119.6 . . ? C16 C15 C14 119.5(5) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C17 C16 C15 120.5(5) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.7(5) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 118.6(5) . . ? C17 C18 C19 118.2(5) . . ? C13 C18 C19 123.3(4) . . ? N2 C19 C20 108.7(5) . . ? N2 C19 C18 124.7(5) . . ? C20 C19 C18 126.6(5) . . ? C21 C20 C19 105.5(5) . . ? C21 C20 H20 127.3 . . ? C19 C20 H20 127.3 . . ? N1 C21 C20 108.0(6) . . ? N1 C21 H21 126 . . ? C20 C21 H21 126 . . ? Cl3 C22 Cl2 107.5(4) . . ? Cl3 C22 Cl1 110.2(4) . . ? Cl2 C22 Cl1 104.7(4) . . ? Cl3 C22 H22 111.4 . . ? Cl2 C22 H22 111.4 . . ? Cl1 C22 H22 111.4 . . ? Cl6 C23 Cl4 112.1(4) . . ? Cl6 C23 Cl5 109.8(4) . . ? Cl4 C23 Cl5 110.2(4) . . ? Cl6 C23 H23 108.2 . . ? Cl4 C23 H23 108.2 . . ? Cl5 C23 H23 108.2 . . ? #===END