#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/35/2003587.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_paper_doi               10.1107/S0108270194013119
_journal_volume                  51
_journal_year                    1995
_chemical_compound_source        synthetic
_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}-π-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                112.988(57)
_cell_angle_beta                 113.552(22)
_cell_angle_gamma                93.402(51)
_cell_formula_units_Z            1
_cell_length_a                   9.1706(41)
_cell_length_b                   9.3871(73)
_cell_length_c                   9.5577(27)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    250
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2
_cell_volume                     671.3(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       θ/2θ
_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   -0.003(30)
_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_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              -12
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_observed          3418
_reflns_number_total             3418
_reflns_observed_criterion       'F > 3.0\s(F)'
_cod_data_source_file            na1124.cif
_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_label
_atom_site_occupancy
_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
Pd1 1 .5001(3) .4958(3) .5007(3) .02460(3) Uani ? ?
N1 1 .5202(4) .5148(4) .7317(4) .0260(4) Uani ? ?
N2 1 .4122(4) .2476(4) .3987(4) .0265(4) Uani ? ?
O1 1 .5007(4) .4414(4) .9197(4) .0351(4) Uani ? ?
O2 1 .3937(4) .0108(4) .3985(4) .0374(4) Uani ? ?
C1 1 .5010(4) .4015(4) .7683(4) .0287(4) Uani ? ?
C2 1 .4911(4) .2279(4) .6739(4) .0289(7) Uani ? ?
C3 1 .3779(5) .1254(5) .7003(5) .0433(4) Uani ? ?
C4 1 .6675(5) .2081(5) .7491(5) .0447(4) Uani ? ?
C5 1 .4316(4) .1707(4) .4855(4) .0291(4) Uani ? ?
C6 1 .4975(5) .6085(4) .9846(4) .0360(6) Uani ? ?
C7 1 .5535(4) .6669(4) .8821(4) .0285(4) Uani ? ?
C8 1 .7356(4) .7520(4) .9783(4) .0329(4) Uani ? ?
C9 1 .7703(4) .9116(4) 1.1251(4) .0330(4) Uani ? ?
C10 1 .8406(5) .9341(5) 1.2921(4) .0455(5) Uani ? ?
C11 1 .8667(6) 1.0816(5) 1.4254(5) .0544(7) Uani ? ?
C12 1 .8255(6) 1.2064(5) 1.3906(5) .0520(7) Uani ? ?
C13 1 .7545(6) 1.1845(5) 1.2260(6) .0493(7) Uani ? ?
C14 1 .7281(5) 1.0392(4) 1.0940(5) .0414(4) Uani ? ?
C15 1 .3629(5) -.0240(4) .2258(4) .0405(6) Uani ? ?
C16 1 .3316(4) .1298(4) .2149(4) .0329(4) Uani ? ?
C17 1 .1491(4) .1242(4) .1302(4) .0377(4) Uani ? ?
C18 1 .1152(4) .2610(4) .0883(4) .0331(4) Uani ? ?
C19 1 .0829(4) .3924(5) .1921(4) .0388(4) Uani ? ?
C20 1 .0566(5) .5186(5) .1524(5) .0449(4) Uani ? ?
C21 1 .0639(5) .5156(5) .0097(5) .0442(5) Uani ? ?
C22 1 .0956(4) .3846(5) -.0950(4) .0410(5) Uani ? ?
C23 1 .1197(4) .2578(4) -.0566(4) .0371(4) Uani ? ?
C24 1 .5889(7) .7371(5) .5662(6) .0426(7) Uani ? ?
C25 .74(1) .4885(5) .6604(5) .3993(6) .0379(8) Uani ? ?
C26 1 .5098(6) .5210(6) .2937(6) .0412(8) Uani ? ?
C125 .26(1) .611(1) .641(1) .426(1) .036(2) Uani ? ?
P1 1 .0943(3) .7244(3) .6606(3) .0416(1) Uani ? ?
F1 1 .2439(5) .8409(5) .8425(4) .0717(8) Uani ? ?
F2 1 .2051(5) .7440(5) .5762(5) .0751(8) Uani ? ?
F3 1 .1580(5) .5739(5) .6691(6) .085(1) Uani ? ?
F4 1 -.0132(5) .7047(6) .7477(5) .091(1) Uani ? ?
F5 1 -.0538(4) .6106(4) .4773(4) .0697(4) Uani ? ?
F6 1 .0284(5) .8711(4) .6489(5) .0812(7) Uani ? ?
H241 .74(1) .573(3) .819(5) .652(4) .0486 Uiso ? ?
H242 .74(1) .707(4) .731(4) .599(2) .0486 Uiso ? ?
H251 .74(1) .374(5) .667(3) .366(2) .0663 Uiso ? ?
H261 .74(1) .431(3) .440(4) .181(4) .0500 Uiso ? ?
H262 .74(1) .625(4) .518(3) .325(4) .0500 Uiso ? ?
H121 .26(1) .673(4) .810(8) .681(6) .0500 Uiso ? ?
H1242 .26(1) .478(6) .753(8) .537(3) .0500 Uiso ? ?
H1251 .26(1) .724(5) .641(5) .453(4) .0500 Uiso ? ?
H1261 .26(1) .529(3) .44(1) .222(7) .0500 Uiso ? ?
H1262 .26(1) .391(6) .528(5) .251(6) .0500 Uiso ? ?
H31 1 .3720 .0099 .6369 .0490 Uiso calc C3
H32 1 .4226 .1564 .8250 .0490 Uiso calc C3
H33 1 .2652 .1431 .6560 .0490 Uiso calc C3
H41 1 .6668 .0935 .6896 .0424 Uiso calc C4
H42 1 .7096 .2417 .8742 .0424 Uiso calc C4
H43 1 .7405 .2764 .7323 .0424 Uiso calc C4
H61 1 .5748 .6692 1.1097 .0407 Uiso calc C6
H62 1 .3839 .6194 .9641 .0407 Uiso calc C6
H71 1 .4954 .7454 .8518 .0296 Uiso calc C7
H81 1 .7998 .6840 1.0237 .0329 Uiso calc C8
H82 1 .7701 .7687 .8977 .0329 Uiso calc C8
H101 1 .8730 .8438 1.3174 .0416 Uiso calc C10
H111 1 .9152 1.0966 1.5459 .0481 Uiso calc C11
H121b 1 .8476 1.3137 1.4863 .0504 Uiso calc C12
H131 1 .7214 1.2749 1.2011 .0493 Uiso calc C13
H141 1 .6778 1.0254 .9739 .0424 Uiso calc C14
H151 1 .4607 -.0481 .2081 .0396 Uiso calc C15
H152 1 .2646 -.1162 .1392 .0396 Uiso calc C15
H161 1 .3762 .1561 .1455 .0321 Uiso calc C16
H171 1 .1033 .1260 .2097 .0350 Uiso calc C17
H172 1 .0922 .0221 .0215 .0350 Uiso calc C18
H191 1 .0785 .3963 .2963 .0385 Uiso calc C19
H201 1 .0322 .6126 .2274 .0446 Uiso calc C20
H211 1 .0463 .6076 -.0178 .0438 Uiso calc C21
H221 1 .1011 .3817 -.1985 .0408 Uiso calc C22
H231 1 .1406 .1626 -.1340 .0358 Uiso calc C23
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
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) ?
