#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003588.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_2003588 _journal_name_full 'Acta Crystallographica' _journal_year 1995 _journal_volume C51 _journal_page_first 1109 _journal_page_last 1112 _publ_section_title ; (Allyl)palladium(II) Complexes with Chiral Ligands. I. (Allyl)palladium(II) Complexes with Methylenebis(oxazoline) Ligands ; _chemical_formula_moiety 'C38 H39 N2 O2 Pd ^+^, F6 P ^-^' _chemical_formula_sum 'C38 H39 F6 N2 O2 P Pd' _chemical_formula_weight 807.102 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' 'X+1/2,-Y+1/2,-Z' '-X,Y+1/2,-Z+1/2' '-X+1/2,-Y,Z+1/2' _symmetry_space_group_name_H-M 'P 21 21 21' _cell_length_a 12.6087(25) _cell_length_b 15.2262(192) _cell_length_c 18.5205(70) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3555.61(4.76) _cell_formula_units_Z 4 _exptl_crystal_density_diffrn 1.508 _exptl_crystal_density_meas 1.51 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 2 _cell_measurement_theta_max 28 _exptl_absorpt_coefficient_mu 0.6239 _cell_measurement_temperature 250 _exptl_crystal_description prism _exptl_crystal_size_max .4 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .3 _exptl_crystal_colour yellow _chemical_compound_source synthetic _diffrn_measurement_device ; Four Circle CAD-4 (Enraf-Nonius) diffractometer equipped with Oxford Cryostream Cooling Device ; _diffrn_measurement_method \q/2\q _exptl_absorpt_correction_type sphere _exptl_absorpt_correction_T_min 0.98 _exptl_absorpt_correction_T_max 1.00 _diffrn_reflns_number 4683 _reflns_number_total 4683 _reflns_number_observed 4183 _reflns_observed_criterion 'F>3.0\s(F)' _diffrn_reflns_theta_max 28 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _reflns_limit_h_min 0 _reflns_limit_h_max 16 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 24 _diffrn_standards_number 4 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.7 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs .0309 _refine_ls_wR_factor_obs .0183 _refine_ls_goodness_of_fit_obs 1.1326 _refine_ls_number_reflns 4183 _refine_ls_number_parameters 451 _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme 'Chebychev weighting (Carruthers & Watkin, 1979) _refine_ls_shift/esd_max 0.17 _refine_diff_density_max .64 _refine_diff_density_min -.46 _refine_ls_extinction_method 'Larson (1970)' _refine_ls_extinction_coef 58(2) loop_ _atom_type_symbol _atom_type_scat_source _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag C International_Tables_Vol_IV_Table_2.2B .017 .009 H International_Tables_Vol_IV_Table_2.2B 0 0 O International_Tables_Vol_IV_Table_2.2B .047 .032 N International_Tables_Vol_IV_Table_2.2B .029 .018 Pd International_Tables_Vol_IV_Table_2.2B -1.177 1.007 P International_Tables_Vol_IV_Table_2.2B .090 .095 F International_Tables_Vol_IV_Table_2.2B .014 .010 _refine_ls_abs_structure_details ; The absolute configuration was known by the chosen educts. Additionally it has been determined refining the enantiopole- parameter. ; _refine_ls_abs_structure_Flack -0.006 loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Pd1 .02848(2) .96547(2) .88343(1) .02770(3) N1 -.0989(2) 1.0493(2) .9144(1) .0284(3) C1 -.0825(3) 1.1310(2) .9216(2) .0303(3) C2 .0074(2) 1.1822(2) .8880(2) .0344(3) C3 .0103(3) 1.1676(2) .8056(2) .0411(3) C4 -.0027(3) 1.2806(2) .9031(2) .0467(4) C5 .1076(3) 1.1449(2) .9196(2) .0353(3) N2 .1253(2) 1.0635(2) .9291(2) .0354(3) O1 -.1469(2) 1.1747(2) .9661(1) .0367(3) C6 -.2114(3) 1.1076(3) 1.0018(2) .0390(3) C7 -.1985(2) 1.0280(2) .9532(2) .0318(3) C8 -.2910(3) 1.0146(2) .9001(2) .0359(3) C9 -.3254(2) 1.0970(2) .8634(2) .0373(3) C10 -.2753(3) 1.1271(3) .8014(2) .0453(3) C11 -.3048(4) 1.2063(3) .7709(3) .0607(4) C12 -.3836(4) 1.2557(3) .8020(3) .0717(4) C13 -.4355(4) 1.2253(3) .8622(3) .0655(4) C14 -.4077(3) 1.1465(3) .8922(2) .0507(3) O2 .1833(2) 1.2005(2) .9413(2) .0496(4) C15 .2731(4) 1.1459(3) .9601(3) .0640(4) C16 .2250(3) 1.0564(3) .9713(3) .0457(3) C17 .1951(4) 1.0349(4) 1.0503(2) .0538(3) C18 .1258(4) .9577(3) 1.0575(2) .0599(3) C19 .0220(4) .9673(4) 1.0786(3) .0964(3) C20 -.0424(5) .8936(4) 1.0826(4) .1145(4) C21 -.0006(5) .8131(4) 1.0626(4) .1011(4) C22 .1029(5) .8037(4) 1.0452(4) .1060(4) C23 .1666(4) .8758(3) 1.0428(3) .0825(4) C24 -.0388(3) .8478(2) .8359(2) .0367(3) C25 .0573(3) .8714(2) .8029(2) .0353(3) C26 .1477(3) .8785(2) .8464(2) .0379(3) C27 .2477(3) .9189(2) .8216(2) .0397(3) C28 .3416(3) .8967(3) .8565(2) .0535(3) C29 .4357(3) .9359(4) .8371(3) .0608(4) C30 .4364(3) .9986(4) .7834(3) .0678(4) C31 .3437(3) 1.0227(4) .7490(2) .0657(4) C32 .2495(3) .9827(3) .7678(2) .0493(3) C33 -.1413(3) .8488(2) .7987(2) .0362(3) C34 -.1608(3) .9069(3) .7426(2) .0449(3) C35 -.2582(3) .9082(3) .7085(2) .0551(4) C36 -.3359(3) .8494(4) .7287(3) .0655(4) C37 -.3163(3) .7898(3) .7830(3) .0634(4) C38 -.2197(3) .7906(3) .8189(3) .0533(4) P1 .5246(1) .93473(8) .08382(6) .0585(2) F1 .5871(4) .8874(3) .1444(2) .1458(4) F2 .4633(3) .9876(3) .1429(2) .1039(4) F3 .6113(3) 1.0072(3) .0811(2) .0928(4) F4 .5865(4) .8856(3) .0233(2) .1211(4) F5 .4625(3) .9848(3) .0236(2) .1302(4) F6 .4380(4) .8631(3) .0857(3) .1382(4) H31 .0703 1.2019 .7843 .0429 H32 -.0581 1.1877 .7839 .0429 H33 .0207 1.1037 .7952 .0429 H41 .0579 1.3124 .8802 .0473 H42 -.0017 1.2909 .9564 .0473 H43 -.0710 1.3028 .8826 .0473 H61 -.1843 1.0952 1.0515 .0399 H62 -.2873 1.1262 1.0045 .0399 H71 -.1948 .9718 .9809 .0325 H81 -.3527 .9902 .9275 .0364 H82 -.2683 .9716 .8624 .0364 H101 -.2177 1.0913 .7787 .0454 H111 -.2687 1.2277 .7261 .0655 H121 -.4032 1.3139 .7808 .0791 H131 -.4938 1.2609 .8842 .0700 H141 -.4471 1.1244 .9354 .0515 H151 .3077 1.1674 1.0053 .0692 H152 .3263 1.1448 .9201 .0692 H161 .2757 1.0097 .9555 .0509 H171 .1577 1.0868 1.0714 .0637 H172 .2619 1.0236 1.0780 .0637 H191 -.0067 1.0266 1.0909 .1017 H201 -.1175 .8986 1.0995 .1177 H211 -.0482 .7606 1.0611 .1085 H221 .1324 .7442 1.0343 .1077 H231 .2433 .8693 1.0302 .0830 H241 -.0373 .8293 .8877 .0379 H251 .0611 .8827 .7498 .0382 H261 .1444 .8550 .8968 .0392 H281 .3407 .8520 .8959 .0559 H291 .5031 .9190 .8618 .0649 H301 .5049 1.0269 .7692 .0771 H311 .3449 1.0689 .7106 .0699 H321 .1823 .9997 .7428 .0498 H341 -.1038 .9483 .7267 .0462 H351 -.2723 .9517 .6691 .0567 H361 -.4064 .8501 .7040 .0693 H371 -.3718 .7459 .7967 .0700 H381 -.2068 .7487 .8595 .0552 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_22 _atom_site_aniso_U_23 _atom_site_aniso_U_33 Pd1 .02716(8) -.0043(1) -.0012(1) .02796(9) -.0004(1) .02870(9) N1 .0272(7) -.0008(7) .0023(7) .0281(8) -.0005(7) .0301(7) C1 .0321(8) .0001(7) .0021(8) .0335(8) .0004(8) .0259(8) C2 .0388(8) .0004(8) .0045(8) .0302(8) -.0047(7) .0358(8) C3 .0484(9) .0074(8) .0090(8) .0454(8) -.0076(8) .0359(8) C4 .0632(9) .0016(8) .0063(8) .0295(8) -.0083(8) .0574(9) C5 .0345(8) -.0070(8) .0000(8) .0364(8) -.0096(8) .0393(8) N2 .0325(8) -.0090(7) -.0038(7) .0380(8) -.0009(7) .0385(8) O1 .0431(8) -.0073(7) .0100(7) .0382(8) -.0006(7) .0338(7) C6 .0461(8) -.0029(8) .0086(8) .0468(8) -.0047(8) .0294(8) C7 .0331(8) .0036(8) .0071(7) .0324(8) .0009(8) .0318(8) C8 .0321(8) -.0018(8) .0063(8) .0379(8) -.0029(8) .0396(8) C9 .0294(8) .0003(8) -.0017(8) .0454(8) -.0009(8) .0390(8) C10 .0402(8) .0047(8) -.0009(8) .0561(9) -.0019(8) .0415(8) C11 .0546(9) .0319(9) -.0005(9) .0787(9) .0034(9) .0652(9) C12 .0718(9) .0335(9) -.0043(9) .0754(9) .0204(9) .0913(9) C13 .0559(9) .0087(9) .0050(9) .0773(9) .0270(9) .0793(9) C14 .0415(8) -.0001(9) .0044(9) .0588(9) .0097(8) .0559(9) O2 .0459(8) -.0150(8) -.0124(8) .0433(8) -.0172(8) .0858(9) C15 .0470(9) -.0233(9) -.0220(9) .0612(9) -.0079(9) .1158(9) C16 .0426(8) -.0199(8) -.0229(8) .0429(9) .0035(8) .0727(9) C17 .0731(9) -.0223(9) -.0351(8) .0642(9) .0144(9) .0554(9) C18 .0940(9) .0065(9) -.0301(9) .0754(9) .0013(9) .0407(8) C19 .0985(9) .0270(9) -.0278(9) .1107(9) .0040(9) .0974(9) C20 .1023(9) .0370(9) -.0113(9) .1412(9) -.0073(9) .1149(9) C21 .1164(9) .0354(9) -.0325(9) .1083(9) -.0249(9) .1032(9) C22 .1408(9) .0213(9) -.0061(9) .1000(9) -.0078(9) .0897(9) C23 .1132(9) -.0023(9) -.0129(9) .0799(9) -.0018(9) .0637(9) C24 .0397(8) -.0108(8) .0032(8) .0307(8) -.0003(8) .0445(8) C25 .0359(8) -.0178(8) .0021(8) .0349(8) .0021(8) .0446(8) C26 .0396(8) -.0109(8) .0041(8) .0357(8) .0024(8) .0426(8) C27 .0331(8) -.0165(8) -.0042(8) .0504(9) .0045(8) .0437(8) C28 .0421(8) -.0180(9) -.0056(8) .0711(9) .0124(9) .0588(9) C29 .0321(8) -.0342(9) -.0106(9) .1129(9) .0031(9) .0755(9) C30 .0468(9) -.0421(9) .0125(9) .1272(9) -.0308(9) .0764(9) C31 .0656(9) -.0163(9) .0163(9) .0922(9) -.0221(9) .0564(9) C32 .0438(8) -.0078(8) .0004(8) .0591(9) -.0049(8) .0478(8) C33 .0358(8) -.0176(8) .0020(8) .0374(8) -.0036(8) .0441(8) C34 .0404(8) -.0109(8) .0029(8) .0626(9) -.0093(8) .0390(8) C35 .0518(9) -.0117(9) -.0084(8) .0864(9) -.0039(9) .0407(8) C36 .0426(9) -.0281(9) -.0085(9) .1067(9) -.0101(9) .0737(9) C37 .0427(9) -.0218(9) .0124(9) .0796(9) -.0264(9) .1012(9) C38 .0480(9) -.0103(9) .0096(9) .0473(9) -.0113(8) .0740(9) P1 .0818(6) -.0002(4) .0124(5) .0614(5) -.0213(6) .0458(5) F1 .1844(9) .1122(9) .0262(9) .2324(9) .0646(9) .1345(9) F2 .1089(9) -.0285(9) .0443(9) .1449(9) -.0136(9) .0937(9) F3 .0984(9) -.0184(9) .0181(9) .1259(9) -.0551(9) .0895(9) F4 .2214(9) -.0363(9) .0866(9) .0896(9) -.0224(9) .1344(9) F5 .1263(9) .0475(9) -.0342(9) .2241(9) -.0027(9) .0970(9) F6 .2142(9) -.0170(9) .0438(9) .1494(9) -.1240(9) .1686(9)