#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2003587.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2003587
loop_
_publ_author_name
'Zehnder, M.'
'Neuburger, M.'
'von Matt, P.'
'Pfaltz, A.'
_publ_section_title
;
 (Allyl)palladium(II) Complexes with Chiral Ligands. I.
 (Allyl)palladium(II) Complexes with Methylenebis(oxazoline) Ligands
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1109
_journal_page_last               1112
_journal_volume                  51
_journal_year                    1995
_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
_chemical_melting_point          451.15
_chemical_name_systematic
;
(-)-{2,2-Bis-[(r)-4'-(benzyl)-oxazolin-2'-yl]propan}-\p-allyl-palladium(II)-
hexa-fluorophosphat
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_cell_angle_alpha                112.99(6)
_cell_angle_beta                 113.55(2)
_cell_angle_gamma                93.40(5)
_cell_formula_units_Z            1
_cell_length_a                   9.171(4)
_cell_length_b                   9.387(7)
_cell_length_c                   9.558(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    250
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     671.4(8)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'CRYSTALS (Watkin, 1990)'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      250
_diffrn_measurement_device
;Four Circle CAD-4 (Enraf-Nonius) diffractometer equipped with
Oxford Cryostream Cooling Device
;
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents
;0.0
(six independent reflections have been rejected by the data reduction
process)
;
_diffrn_reflns_av_sigmaI/netI    .0105
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3424
_diffrn_reflns_theta_max         28
_diffrn_reflns_theta_min         2
_diffrn_standards_decay_%        0.4
_diffrn_standards_interval_time  60
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    0.8063
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_type   'DIFABS (Walker & Stuart, 1983)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      1.62
_exptl_crystal_description       prism
_exptl_crystal_F_000             332
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         .68
_refine_diff_density_min         -.45
_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   -0.00(3)
_refine_ls_extinction_coef       30(3)
_refine_ls_extinction_method     'Larson (1970)'
_refine_ls_goodness_of_fit_obs   1.0996
_refine_ls_hydrogen_treatment
;Only coordinates of allyl H atoms refined, remaining H-atom parameters
not refined
;
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     385
_refine_ls_number_reflns         3418
_refine_ls_number_restraints     16
_refine_ls_R_factor_obs          .0176
_refine_ls_shift/esd_max         0.04
_refine_ls_shift/esd_mean        0.0449
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme
'Chebychev weighting (Carruthers & Watkin, 1979)'
_refine_ls_wR_factor_obs         .0206
_reflns_number_observed          3418
_reflns_number_total             3418
_reflns_observed_criterion       'F > 3.0\s(F)'
_[local]_cod_data_source_file    na1124.cif
_[local]_cod_data_source_block   1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '178_C' was changed to '451.15' - it
was converted from degrees Celsius(C) to Kelvins(K).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        671.3(8)
_cod_database_code               2003587
loop_
_symmetry_equiv_pos_as_xyz
+x,+y,+z
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Pd1 .03245(7) .02178(6) .02417(7) .01185(5) .01411(5) .00616(4)
N1 .0400(10) .0200(10) .0250(10) .0097(9) .0186(9) .0080(9)
N2 .0350(10) .0210(10) .0230(10) .0082(8) .0129(8) .0065(8)
O1 .0720(10) .0292(8) .0317(9) .0142(7) .0328(9) .0110(8)
O2 .0710(10) .0199(7) .0340(9) .0100(7) .0211(9) .0116(8)
C1 .0400(10) .0270(10) .0260(10) .0131(8) .0174(8) .0078(8)
C2 .0430(10) .0235(9) .0290(10) .0142(8) .0183(9) .0083(8)
C3 .065(2) .0350(10) .051(2) .0200(10) .0360(10) .0030(10)
C4 .0480(10) .0390(10) .0420(10) .0160(10) .0130(10) .0130(10)
C5 .0370(10) .0205(9) .0300(10) .0092(8) .0156(9) .0076(8)
C6 .064(2) .0290(10) .0370(10) .0110(10) .0350(10) .0100(10)
C7 .0420(10) .0223(9) .0280(10) .0091(8) .0204(9) .0087(8)
C8 .0390(10) .0300(10) .0300(10) .0108(9) .0171(9) .0119(9)
C9 .0340(10) .0280(10) .0320(10) .0080(9) .0137(9) .0053(8)
C10 .055(2) .0410(10) .0320(10) .0120(10) .0100(10) .0110(10)
C11 .068(2) .055(2) .0300(10) .0030(10) .0120(10) .010(2)
C12 .069(2) .0360(10) .052(2) -.0020(10) .033(2) .0010(10)
C13 .063(2) .0310(10) .062(2) .0170(10) .032(2) .0120(10)
C14 .0550(10) .0320(10) .0430(10) .0170(10) .0250(10) .0120(10)
C15 .074(2) .0260(10) .0320(10) .0075(9) .0230(10) .0160(10)
C16 .0470(10) .0260(10) .0270(10) .0080(8) .0174(9) .0100(9)
C17 .0420(10) .0320(10) .0310(10) .0105(9) .0120(10) .0014(9)
C18 .0310(10) .0350(10) .0270(10) .0109(9) .0107(8) .0051(8)
C19 .0390(10) .0440(10) .0330(10) .0140(10) .0180(10) .0120(10)
C20 .0450(10) .0450(10) .0430(10) .0150(10) .0190(10) .0200(10)
C21 .0390(10) .0450(10) .048(2) .0250(10) .0120(10) .0110(10)
C22 .0380(10) .053(2) .0340(10) .0210(10) .0130(10) .0060(10)
C23 .0390(10) .0420(10) .0280(10) .0109(9) .0154(9) .0079(9)
C24 .078(2) .0250(10) .047(2) .0170(10) .033(2) .0080(10)
C25 .043(2) .039(2) .044(2) .028(2) .017(2) .0060(10)
C26 .068(2) .046(2) .035(2) .023(2) .028(2) .006(2)
C125 .043(6) .052(7) .045(6) .033(5) .009(4) -.016(5)
P1 .0474(4) .0443(4) .0357(3) .0169(3) .0206(3) .0154(3)
F1 .0670(10) .115(3) .0390(10) .0020(10) .0110(10) .039(2)
F2 .096(2) .086(2) .075(2) .012(2) .058(2) -.016(2)
F3 .078(2) .074(2) .140(3) .062(2) .042(2) .0340(10)
F4 .090(2) .212(4) .108(2) .102(3) .074(2) .060(2)
F5 .0620(10) .0610(10) .0590(10) .0070(10) .0110(10) -.0010(10)
F6 .113(2) .0540(10) .084(2) .0230(10) .008(2) .0410(10)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_calc_attached_atom
_atom_site_occupancy
Pd1 .5001(3) .4958(3) .5007(3) .02460(3) Uani ? ? 1
N1 .5202(4) .5148(4) .7317(4) .0260(4) Uani ? ? 1
N2 .4122(4) .2476(4) .3987(4) .0265(4) Uani ? ? 1
O1 .5007(4) .4414(4) .9197(4) .0351(4) Uani ? ? 1
O2 .3937(4) .0108(4) .3985(4) .0374(4) Uani ? ? 1
C1 .5010(4) .4015(4) .7683(4) .0287(4) Uani ? ? 1
C2 .4911(4) .2279(4) .6739(4) .0289(7) Uani ? ? 1
C3 .3779(5) .1254(5) .7003(5) .0433(4) Uani ? ? 1
C4 .6675(5) .2081(5) .7491(5) .0447(4) Uani ? ? 1
C5 .4316(4) .1707(4) .4855(4) .0291(4) Uani ? ? 1
C6 .4975(5) .6085(4) .9846(4) .0360(6) Uani ? ? 1
C7 .5535(4) .6669(4) .8821(4) .0285(4) Uani ? ? 1
C8 .7356(4) .7520(4) .9783(4) .0329(4) Uani ? ? 1
C9 .7703(4) .9116(4) 1.1251(4) .0330(4) Uani ? ? 1
C10 .8406(5) .9341(5) 1.2921(4) .0455(5) Uani ? ? 1
C11 .8667(6) 1.0816(5) 1.4254(5) .0544(7) Uani ? ? 1
C12 .8255(6) 1.2064(5) 1.3906(5) .0520(7) Uani ? ? 1
C13 .7545(6) 1.1845(5) 1.2260(6) .0493(7) Uani ? ? 1
C14 .7281(5) 1.0392(4) 1.0940(5) .0414(4) Uani ? ? 1
C15 .3629(5) -.0240(4) .2258(4) .0405(6) Uani ? ? 1
C16 .3316(4) .1298(4) .2149(4) .0329(4) Uani ? ? 1
C17 .1491(4) .1242(4) .1302(4) .0377(4) Uani ? ? 1
C18 .1152(4) .2610(4) .0883(4) .0331(4) Uani ? ? 1
C19 .0829(4) .3924(5) .1921(4) .0388(4) Uani ? ? 1
C20 .0566(5) .5186(5) .1524(5) .0449(4) Uani ? ? 1
C21 .0639(5) .5156(5) .0097(5) .0442(5) Uani ? ? 1
C22 .0956(4) .3846(5) -.0950(4) .0410(5) Uani ? ? 1
C23 .1197(4) .2578(4) -.0566(4) .0371(4) Uani ? ? 1
C24 .5889(7) .7371(5) .5662(6) .0426(7) Uani ? ? 1
C25 .4885(5) .6604(5) .3993(6) .0379(8) Uani ? ? .740(10)
C26 .5098(6) .5210(6) .2937(6) .0412(8) Uani ? ? 1
C125 .6110(10) .6410(10) .4260(10) .036(2) Uani ? ? .260(10)
P1 .0943(3) .7244(3) .6606(3) .04160(10) Uani ? ? 1
F1 .2439(5) .8409(5) .8425(4) .0717(8) Uani ? ? 1
F2 .2051(5) .7440(5) .5762(5) .0751(8) Uani ? ? 1
F3 .1580(5) .5739(5) .6691(6) .0850(10) Uani ? ? 1
F4 -.0132(5) .7047(6) .7477(5) .0910(10) Uani ? ? 1
F5 -.0538(4) .6106(4) .4773(4) .0697(4) Uani ? ? 1
F6 .0284(5) .8711(4) .6489(5) .0812(7) Uani ? ? 1
H241 .573(3) .819(5) .652(4) .0486 Uiso ? ? .740(10)
H242 .707(4) .731(4) .599(2) .0486 Uiso ? ? .740(10)
H251 .374(5) .667(3) .366(2) .0663 Uiso ? ? .740(10)
H261 .431(3) .440(4) .181(4) .0500 Uiso ? ? .740(10)
H262 .625(4) .518(3) .325(4) .0500 Uiso ? ? .740(10)
H121 .673(4) .810(8) .681(6) .0500 Uiso ? ? .260(10)
H1242 .478(6) .753(8) .537(3) .0500 Uiso ? ? .260(10)
H1251 .724(5) .641(5) .453(4) .0500 Uiso ? ? .260(10)
H1261 .529(3) .440(10) .222(7) .0500 Uiso ? ? .260(10)
H1262 .391(6) .528(5) .251(6) .0500 Uiso ? ? .260(10)
H31 .3720 .0099 .6369 .0490 Uiso calc C3 1
H32 .4226 .1564 .8250 .0490 Uiso calc C3 1
H33 .2652 .1431 .6560 .0490 Uiso calc C3 1
H41 .6668 .0935 .6896 .0424 Uiso calc C4 1
H42 .7096 .2417 .8742 .0424 Uiso calc C4 1
H43 .7405 .2764 .7323 .0424 Uiso calc C4 1
H61 .5748 .6692 1.1097 .0407 Uiso calc C6 1
H62 .3839 .6194 .9641 .0407 Uiso calc C6 1
H71 .4954 .7454 .8518 .0296 Uiso calc C7 1
H81 .7998 .6840 1.0237 .0329 Uiso calc C8 1
H82 .7701 .7687 .8977 .0329 Uiso calc C8 1
H101 .8730 .8438 1.3174 .0416 Uiso calc C10 1
H111 .9152 1.0966 1.5459 .0481 Uiso calc C11 1
H121b .8476 1.3137 1.4863 .0504 Uiso calc C12 1
H131 .7214 1.2749 1.2011 .0493 Uiso calc C13 1
H141 .6778 1.0254 .9739 .0424 Uiso calc C14 1
H151 .4607 -.0481 .2081 .0396 Uiso calc C15 1
H152 .2646 -.1162 .1392 .0396 Uiso calc C15 1
H161 .3762 .1561 .1455 .0321 Uiso calc C16 1
H171 .1033 .1260 .2097 .0350 Uiso calc C17 1
H172 .0922 .0221 .0215 .0350 Uiso calc C18 1
H191 .0785 .3963 .2963 .0385 Uiso calc C19 1
H201 .0322 .6126 .2274 .0446 Uiso calc C20 1
H211 .0463 .6076 -.0178 .0438 Uiso calc C21 1
H221 .1011 .3817 -.1985 .0408 Uiso calc C22 1
H231 .1406 .1626 -.1340 .0358 Uiso calc C23 1
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C .017 .009 International_Tables_Vol_IV_Table_2.2B
H 0 0 International_Tables_Vol_IV_Table_2.2B
O .047 .032 International_Tables_Vol_IV_Table_2.2B
N .029 .018 International_Tables_Vol_IV_Table_2.2B
Pd -1.177 1.007 International_Tables_Vol_IV_Table_2.2B
P .090 .095 International_Tables_Vol_IV_Table_2.2B
F .014 .010 International_Tables_Vol_IV_Table_2.2B
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
8 2 6
12 2 5
24 -2 5
25 3 6
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
N2 Pd1 N1 87.60(10) yes
C24 Pd1 N1 101.30(10) yes
C24 Pd1 N2 171.00(10) ?
C25 Pd1 N1 133.30(10) ?
C25 Pd1 N2 135.60(10) ?
C25 Pd1 C24 36.7(2) ?
C26 Pd1 N1 169.10(10) ?
C26 Pd1 N2 102.80(10) yes
C26 Pd1 C24 68.2(2) yes
C26 Pd1 C25 38.3(2) ?
C125 Pd1 N1 135.1(3) ?
C125 Pd1 N2 133.0(4) ?
C125 Pd1 C24 38.3(4) ?
C125 Pd1 C25 29.8(4) ?
C125 Pd1 C26 34.1(3) ?
C1 N1 Pd1 127.1(2) ?
C7 N1 Pd1 124.9(2) ?
C7 N1 C1 107.9(2) ?
C5 N2 Pd1 125.3(2) ?
C16 N2 Pd1 126.6(2) ?
C16 N2 C5 107.9(2) ?
C6 O1 C1 105.7(2) ?
C15 O2 C5 105.8(2) ?
O1 C1 N1 116.6(2) ?
C2 C1 N1 129.6(2) ?
C2 C1 O1 113.7(2) ?
C3 C2 C1 110.0(2) ?
C4 C2 C1 106.7(2) ?
C4 C2 C3 110.2(2) ?
C5 C2 C1 113.5(2) ?
C5 C2 C3 109.0(2) ?
C5 C2 C4 107.4(2) ?
O2 C5 N2 116.6(2) ?
C2 C5 N2 130.9(2) ?
C2 C5 O2 112.5(2) ?
C7 C6 O1 103.6(2) ?
C6 C7 N1 101.8(2) ?
C8 C7 N1 110.4(2) ?
C8 C7 C6 112.6(2) ?
C9 C8 C7 111.2(2) ?
C10 C9 C8 121.5(2) ?
C14 C9 C8 120.0(2) ?
C14 C9 C10 118.5(2) ?
C11 C10 C9 120.5(3) ?
C12 C11 C10 119.6(3) ?
C13 C12 C11 120.1(3) ?
C14 C13 C12 120.5(3) ?
C13 C14 C9 120.8(3) ?
C16 C15 O2 103.5(2) ?
C15 C16 N2 101.3(2) ?
C17 C16 N2 110.8(2) ?
C17 C16 C15 113.4(2) ?
C18 C17 C16 114.0(2) ?
C19 C18 C17 121.8(2) ?
C23 C18 C17 119.4(2) ?
C23 C18 C19 118.8(2) ?
C20 C19 C18 120.4(2) ?
C21 C20 C19 120.4(2) ?
C22 C21 C20 119.6(2) ?
C23 C22 C21 119.9(2) ?
C22 C23 C18 120.8(2) ?
C25 C24 Pd1 71.6(2) ?
C125 C24 Pd1 71.8(4) ?
C125 C24 C25 47.1(5) ?
C24 C25 Pd1 71.7(2) ?
C26 C25 Pd1 71.2(2) ?
C26 C25 C24 121.6(4) ?
C125 C25 Pd1 76.5(5) ?
C125 C25 C24 69.6(7) ?
C125 C25 C26 58.9(7) ?
C25 C26 Pd1 70.5(2) ?
C125 C26 Pd1 73.7(5) ?
C125 C26 C25 48.5(7) ?
C24 C125 Pd1 69.9(4) ?
C25 C125 Pd1 73.8(5) ?
C25 C125 C24 63.2(8) ?
C26 C125 Pd1 72.2(4) ?
C26 C125 C24 127.7(9) ?
C26 C125 C25 72.6(7) ?
F2 P1 F1 88.5(2) ?
F3 P1 F1 91.1(2) ?
F3 P1 F2 88.9(2) ?
F4 P1 F1 90.7(2) ?
F4 P1 F2 178.9(2) ?
F4 P1 F3 90.4(2) ?
F5 P1 F1 178.7(2) ?
F5 P1 F2 90.5(2) ?
F5 P1 F3 89.6(2) ?
F5 P1 F4 90.4(2) ?
F6 P1 F1 89.9(2) ?
F6 P1 F2 91.3(2) ?
F6 P1 F3 178.9(2) ?
F6 P1 F4 89.5(2) ?
F6 P1 F5 89.30(10) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N1 2.075(3) yes
Pd1 N2 2.099(3) yes
Pd1 C24 2.110(4) yes
Pd1 C25 2.108(3) ?
Pd1 C26 2.117(4) yes
Pd1 C125 2.134(9) ?
N1 C1 1.266(3) ?
N1 C7 1.480(3) ?
N2 C5 1.267(4) ?
N2 C16 1.484(3) ?
O1 C1 1.347(3) ?
O1 C6 1.451(3) ?
O2 C5 1.341(3) ?
O2 C15 1.452(3) ?
C1 C2 1.499(3) ?
C2 C3 1.532(3) ?
C2 C4 1.542(4) ?
C2 C5 1.501(3) ?
C6 C7 1.520(3) ?
C7 C8 1.521(3) ?
C8 C9 1.503(3) ?
C9 C10 1.381(4) ?
C9 C14 1.383(3) ?
C10 C11 1.392(4) ?
C11 C12 1.372(5) ?
C12 C13 1.362(5) ?
C13 C14 1.372(4) ?
C15 C16 1.523(3) ?
C16 C17 1.528(4) ?
C17 C18 1.502(4) ?
C18 C19 1.384(3) ?
C18 C23 1.391(3) ?
C19 C20 1.385(4) ?
C20 C21 1.381(4) ?
C21 C22 1.383(4) ?
C22 C23 1.381(4) ?
C24 C25 1.327(6) ?
C24 C125 1.390(10) ?
C25 C26 1.387(6) ?
C25 C125 1.090(10) ?
C26 C125 1.240(10) ?
P1 F1 1.591(3) ?
P1 F2 1.570(3) ?
P1 F3 1.580(3) ?
P1 F4 1.566(3) ?
P1 F5 1.587(2) ?
P1 F6 1.561(2) ?