#------------------------------------------------------------------------------ #$Date: 2009-11-14 13:09:05 +0000 (Sat, 14 Nov 2009) $ #$Revision: 846 $ #$URL: svn://www.crystallography.net/cod/cif/2/2003587.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_2003587 _journal_name_full 'Acta Crystallographica C' _journal_volume 51 _journal_year 1995 _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 'C26 H31 N2 O2 Pd 1+, F6 P 1-' _chemical_formula_sum 'C26 H31 F6 N2 O2 P Pd' _chemical_formula_weight 654.91 loop_ _symmetry_equiv_pos_as_xyz '+x,+y,+z' _symmetry_space_group_name_H-M 'P 1' _cell_length_a 9.1706(41) _cell_length_b 9.3871(73) _cell_length_c 9.5577(27) _cell_angle_alpha 112.988(57) _cell_angle_beta 113.552(22) _cell_angle_gamma 93.402(51) _cell_volume 671.34(78) _cell_formula_units_Z 1 _exptl_crystal_density_diffrn 1.620 _exptl_crystal_density_meas 1.62 _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 0.8063 _cell_measurement_temperature 250 _exptl_crystal_description prism _exptl_crystal_size_max .4 _exptl_crystal_size_mid .2 _exptl_crystal_size_min .2 _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 'DIFABS (Walker & Stuart, 1983)' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 1.00 _diffrn_reflns_number 3424 _reflns_number_total 3418 _reflns_number_observed 3418 _reflns_observed_criterion 'F > 3.0\s(F)' _diffrn_reflns_av_R_equivalents ;0.0 (six independent reflections have been rejected by the data reduction process) ; _diffrn_reflns_theta_max 28 _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 0 _diffrn_reflns_limit_l_max 12 _reflns_limit_h_min -12 _reflns_limit_h_max 12 _reflns_limit_k_min -12 _reflns_limit_k_max 12 _reflns_limit_l_min 0 _reflns_limit_l_max 12 _diffrn_standards_number 4 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 0.4 _refine_ls_structure_factor_coef F _refine_ls_R_factor_obs .0176 _refine_ls_wR_factor_obs .0206 _refine_ls_goodness_of_fit_obs 1.0996 _refine_ls_number_reflns 3418 _refine_ls_number_parameters 385 _refine_ls_hydrogen_treatment ;Only coordinates of allyl H atoms refined, remaining H-atom parameters not refined ; _refine_ls_weighting_scheme 'Chebychev weighting (Carruthers & Watkin, 1979)' _refine_ls_shift/esd_max 0.04 _refine_diff_density_max .68 _refine_diff_density_min -.45 _refine_ls_extinction_method 'Larson (1970)' _refine_ls_extinction_coef 30(3) 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 -0.003(30) loop_ _atom_site_label _atom_site_occupancy _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv Pd1 1 .5001(3) .4958(3) .5007(3) .02460(3) N1 1 .5202(4) .5148(4) .7317(4) .0260(4) N2 1 .4122(4) .2476(4) .3987(4) .0265(4) O1 1 .5007(4) .4414(4) .9197(4) .0351(4) O2 1 .3937(4) .0108(4) .3985(4) .0374(4) C1 1 .5010(4) .4015(4) .7683(4) .0287(4) C2 1 .4911(4) .2279(4) .6739(4) .0289(7) C3 1 .3779(5) .1254(5) .7003(5) .0433(4) C4 1 .6675(5) .2081(5) .7491(5) .0447(4) C5 1 .4316(4) .1707(4) .4855(4) .0291(4) C6 1 .4975(5) .6085(4) .9846(4) .0360(6) C7 1 .5535(4) .6669(4) .8821(4) .0285(4) C8 1 .7356(4) .7520(4) .9783(4) .0329(4) C9 1 .7703(4) .9116(4) 1.1251(4) .0330(4) C10 1 .8406(5) .9341(5) 1.2921(4) .0455(5) C11 1 .8667(6) 1.0816(5) 1.4254(5) .0544(7) C12 1 .8255(6) 1.2064(5) 1.3906(5) .0520(7) C13 1 .7545(6) 1.1845(5) 1.2260(6) .0493(7) C14 1 .7281(5) 1.0392(4) 1.0940(5) .0414(4) C15 1 .3629(5) -.0240(4) .2258(4) .0405(6) C16 1 .3316(4) .1298(4) .2149(4) .0329(4) C17 1 .1491(4) .1242(4) .1302(4) .0377(4) C18 1 .1152(4) .2610(4) .0883(4) .0331(4) C19 1 .0829(4) .3924(5) .1921(4) .0388(4) C20 1 .0566(5) .5186(5) .1524(5) .0449(4) C21 1 .0639(5) .5156(5) .0097(5) .0442(5) C22 1 .0956(4) .3846(5) -.0950(4) .0410(5) C23 1 .1197(4) .2578(4) -.0566(4) .0371(4) C24 1 .5889(7) .7371(5) .5662(6) .0426(7) C25 .74(1) .4885(5) .6604(5) .3993(6) .0379(8) C26 1 .5098(6) .5210(6) .2937(6) .0412(8) C125 .26(1) .611(1) .641(1) .426(1) .036(2) P1 1 .0943(3) .7244(3) .6606(3) .0416(1) F1 1 .2439(5) .8409(5) .8425(4) .0717(8) F2 1 .2051(5) .7440(5) .5762(5) .0751(8) F3 1 .1580(5) .5739(5) .6691(6) .085(1) F4 1 -.0132(5) .7047(6) .7477(5) .091(1) F5 1 -.0538(4) .6106(4) .4773(4) .0697(4) F6 1 .0284(5) .8711(4) .6489(5) .0812(7) H241 .74(1) .573(3) .819(5) .652(4) .0486 H242 .74(1) .707(4) .731(4) .599(2) .0486 H251 .74(1) .374(5) .667(3) .366(2) .0663 H261 .74(1) .431(3) .440(4) .181(4) .0500 H262 .74(1) .625(4) .518(3) .325(4) .0500 H121 .26(1) .673(4) .810(8) .681(6) .0500 H1242 .26(1) .478(6) .753(8) .537(3) .0500 H1251 .26(1) .724(5) .641(5) .453(4) .0500 H1261 .26(1) .529(3) .44(1) .222(7) .0500 H1262 .26(1) .391(6) .528(5) .251(6) .0500 H31 1 .3720 .0099 .6369 .0490 H32 1 .4226 .1564 .8250 .0490 H33 1 .2652 .1431 .6560 .0490 H41 1 .6668 .0935 .6896 .0424 H42 1 .7096 .2417 .8742 .0424 H43 1 .7405 .2764 .7323 .0424 H61 1 .5748 .6692 1.1097 .0407 H62 1 .3839 .6194 .9641 .0407 H71 1 .4954 .7454 .8518 .0296 H81 1 .7998 .6840 1.0237 .0329 H82 1 .7701 .7687 .8977 .0329 H101 1 .8730 .8438 1.3174 .0416 H111 1 .9152 1.0966 1.5459 .0481 H121b 1 .8476 1.3137 1.4863 .0504 H131 1 .7214 1.2749 1.2011 .0493 H141 1 .6778 1.0254 .9739 .0424 H151 1 .4607 -.0481 .2081 .0396 H152 1 .2646 -.1162 .1392 .0396 H161 1 .3762 .1561 .1455 .0321 H171 1 .1033 .1260 .2097 .0350 H172 1 .0922 .0221 .0215 .0350 H191 1 .0785 .3963 .2963 .0385 H201 1 .0322 .6126 .2274 .0446 H211 1 .0463 .6076 -.0178 .0438 H221 1 .1011 .3817 -.1985 .0408 H231 1 .1406 .1626 -.1340 .0358 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 .03245(7) .01185(5) .01411(5) .02178(6) .00616(4) .02417(7) N1 .040(1) .0097(9) .0186(9) .020(1) .0080(9) .025(1) N2 .035(1) .0082(8) .0129(8) .021(1) .0065(8) .023(1) O1 .072(1) .0142(7) .0328(9) .0292(8) .0110(8) .0317(9) O2 .071(1) .0100(7) .0211(9) .0199(7) .0116(8) .0340(9) C1 .040(1) .0131(8) .0174(8) .027(1) .0078(8) .026(1) C2 .043(1) .0142(8) .0183(9) .0235(9) .0083(8) .029(1) C3 .065(2) .020(1) .036(1) .035(1) .003(1) .051(2) C4 .048(1) .016(1) .013(1) .039(1) .013(1) .042(1) C5 .037(1) .0092(8) .0156(9) .0205(9) .0076(8) .030(1) C6 .064(2) .011(1) .035(1) .029(1) .010(1) .037(1) C7 .042(1) .0091(8) .0204(9) .0223(9) .0087(8) .028(1) C8 .039(1) .0108(9) .0171(9) .030(1) .0119(9) .030(1) C9 .034(1) .0080(9) .0137(9) .028(1) .0053(8) .032(1) C10 .055(2) .012(1) .010(1) .041(1) .011(1) .032(1) C11 .068(2) .003(1) .012(1) .055(2) .010(2) .030(1) C12 .069(2) -.002(1) .033(2) .036(1) .001(1) .052(2) C13 .063(2) .017(1) .032(2) .031(1) .012(1) .062(2) C14 .055(1) .017(1) .025(1) .032(1) .012(1) .043(1) C15 .074(2) .0075(9) .023(1) .026(1) .016(1) .032(1) C16 .047(1) .0080(8) .0174(9) .026(1) .0100(9) .027(1) C17 .042(1) .0105(9) .012(1) .032(1) .0014(9) .031(1) C18 .031(1) .0109(9) .0107(8) .035(1) .0051(8) .027(1) C19 .039(1) .014(1) .018(1) .044(1) .012(1) .033(1) C20 .045(1) .015(1) .019(1) .045(1) .020(1) .043(1) C21 .039(1) .025(1) .012(1) .045(1) .011(1) .048(2) C22 .038(1) .021(1) .013(1) .053(2) .006(1) .034(1) C23 .039(1) .0109(9) .0154(9) .042(1) .0079(9) .028(1) C24 .078(2) .017(1) .033(2) .025(1) .008(1) .047(2) C25 .043(2) .028(2) .017(2) .039(2) .006(1) .044(2) C26 .068(2) .023(2) .028(2) .046(2) .006(2) .035(2) C125 .043(6) .033(5) .009(4) .052(7) -.016(5) .045(6) P1 .0474(4) .0169(3) .0206(3) .0443(4) .0154(3) .0357(3) F1 .067(1) .002(1) .011(1) .115(3) .039(2) .039(1) F2 .096(2) .012(2) .058(2) .086(2) -.016(2) .075(2) F3 .078(2) .062(2) .042(2) .074(2) .034(1) .140(3) F4 .090(2) .102(3) .074(2) .212(4) .060(2) .108(2) F5 .062(1) .007(1) .011(1) .061(1) -.001(1) .059(1) F6 .113(2) .023(1) .008(2) .054(1) .041(1) .084(2)