#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:52:31 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179351 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/48/4324865.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_4324865
loop_
_publ_author_name
'Shuanming Zhang'
'Roberto Pattacini'
'Pierre Braunstein'
_publ_contact_author_address
;Laboratoire de Chimie de Coordination
UMR 7177 CNRS
Université de Strasbourg
Institut Le Bel - 4 rue Blaise Pascal, 
CS 90032, F-67081 STRASBOURG cedex
France
;
_publ_contact_author_email       braunst@chimie.u-strasbg.fr
_publ_contact_author_fax         '+33 (0)3 68 85 13 22'
_publ_contact_author_name        'Dr. Pierre Braunstein'
_publ_contact_author_phone       '+33 (0)3 68 85 13 08'
_publ_section_title
;
 Unexpected Metal-Induced Isomerisms and Phosphoryl Migrations in Pt(II)
 and Pd(II) Complexes of the Functional Phosphine
 2-(Bis(diphenylphosphino)methyl)-oxazoline
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3511
_journal_page_last               3522
_journal_paper_doi               10.1021/ic1024422
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C56 H48 N2 O2 P4 Pd, 4(C H2 Cl2)'
_chemical_formula_sum            'C60 H56 Cl8 N2 O2 P4 Pd'
_chemical_formula_weight         1350.95
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                75.682(2)
_cell_angle_beta                 73.222(2)
_cell_angle_gamma                74.038(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8705(5)
_cell_length_b                   12.5788(5)
_cell_length_c                   13.3436(6)
_cell_measurement_reflns_used    4852
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      0.998
_cell_volume                     1499.46(12)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    ORTEP-3
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0727
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15842
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.62
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.817
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.496
_exptl_crystal_description       prism
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         6862
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0409P)²+0.9573P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1014
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                5287
_reflns_number_total             6862
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1024422_si_003_1.cif
_cod_data_source_block           compound3b
_cod_database_code               4324865
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Pd1 Pd 0.0000 1.0000 1.0000 0.01873(10) Uani 1 2 d S
P1 P 0.00159(8) 0.87929(6) 0.89132(6) 0.01980(17) Uani 1 1 d .
P2 P 0.06133(8) 1.08462(6) 0.82245(6) 0.02050(17) Uani 1 1 d .
N1 N 0.1098(3) 0.8599(2) 0.6341(2) 0.0322(6) Uani 1 1 d .
C1 C 0.1685(4) 0.8788(3) 0.5178(3) 0.0470(10) Uani 1 1 d .
H1A H 0.0977 0.8761 0.4815 0.056 Uiso 1 1 calc R
H1B H 0.2557 0.8221 0.4983 0.056 Uiso 1 1 calc R
C2 C 0.2022(4) 0.9951(3) 0.4892(3) 0.0465(10) Uani 1 1 d .
H2A H 0.3045 0.9911 0.4567 0.056 Uiso 1 1 calc R
H2B H 0.1462 1.0452 0.4404 0.056 Uiso 1 1 calc R
C3 C 0.1111(3) 0.9488(2) 0.6654(2) 0.0248(7) Uani 1 1 d .
C4 C 0.0714(3) 0.9651(2) 0.7735(2) 0.0227(6) Uani 1 1 d .
C5 C -0.1705(3) 0.8476(2) 0.8966(2) 0.0231(6) Uani 1 1 d .
C6 C -0.1785(4) 0.7828(3) 0.8284(3) 0.0312(7) Uani 1 1 d .
H6 H -0.0967 0.7579 0.7773 0.037 Uiso 1 1 calc R
C7 C -0.3090(4) 0.7557(3) 0.8372(3) 0.0364(8) Uani 1 1 d .
H7 H -0.3144 0.7122 0.7919 0.044 Uiso 1 1 calc R
C8 C -0.4311(4) 0.7930(3) 0.9129(3) 0.0350(8) Uani 1 1 d .
H8 H -0.5182 0.7742 0.9186 0.042 Uiso 1 1 calc R
C9 C -0.4243(4) 0.8576(3) 0.9797(3) 0.0348(8) Uani 1 1 d .
H9 H -0.5064 0.8827 1.0305 0.042 Uiso 1 1 calc R
C10 C -0.2942(3) 0.8853(3) 0.9711(3) 0.0282(7) Uani 1 1 d .
H10 H -0.2900 0.9298 1.0159 0.034 Uiso 1 1 calc R
C11 C 0.1181(3) 0.7389(2) 0.9102(2) 0.0226(6) Uani 1 1 d .
C12 C 0.2634(3) 0.7183(3) 0.8543(3) 0.0290(7) Uani 1 1 d .
H12 H 0.2993 0.7751 0.8029 0.035 Uiso 1 1 calc R
C13 C 0.3548(4) 0.6135(3) 0.8749(3) 0.0382(8) Uani 1 1 d .
H13 H 0.4513 0.6003 0.8373 0.046 Uiso 1 1 calc R
C14 C 0.3012(4) 0.5291(3) 0.9519(3) 0.0408(9) Uani 1 1 d .
H14 H 0.3624 0.4593 0.9666 0.049 Uiso 1 1 calc R
C15 C 0.1578(4) 0.5478(3) 1.0067(3) 0.0395(9) Uani 1 1 d .
H15 H 0.1222 0.4903 1.0575 0.047 Uiso 1 1 calc R
C16 C 0.0667(4) 0.6517(2) 0.9867(3) 0.0307(7) Uani 1 1 d .
H16 H -0.0298 0.6637 1.0244 0.037 Uiso 1 1 calc R
C17 C -0.0716(3) 1.2076(2) 0.7797(2) 0.0229(6) Uani 1 1 d .
C18 C -0.0520(4) 1.2661(3) 0.6751(3) 0.0322(7) Uani 1 1 d .
H18 H 0.0328 1.2440 0.6250 0.039 Uiso 1 1 calc R
C19 C -0.1581(4) 1.3568(3) 0.6456(3) 0.0388(9) Uani 1 1 d .
H19 H -0.1444 1.3951 0.5755 0.047 Uiso 1 1 calc R
C20 C -0.2840(4) 1.3911(3) 0.7190(3) 0.0395(9) Uani 1 1 d .
H20 H -0.3543 1.4528 0.6987 0.047 Uiso 1 1 calc R
C21 C -0.3053(4) 1.3332(3) 0.8227(3) 0.0376(8) Uani 1 1 d .
H21 H -0.3906 1.3553 0.8723 0.045 Uiso 1 1 calc R
C22 C -0.1992(3) 1.2419(3) 0.8528(3) 0.0301(7) Uani 1 1 d .
H22 H -0.2139 1.2033 0.9228 0.036 Uiso 1 1 calc R
C23 C 0.2345(3) 1.1272(2) 0.7779(2) 0.0232(6) Uani 1 1 d .
C24 C 0.2450(4) 1.2378(3) 0.7692(3) 0.0304(7) Uani 1 1 d .
H24 H 0.1616 1.2946 0.7781 0.037 Uiso 1 1 calc R
C25 C 0.3805(4) 1.2628(3) 0.7472(3) 0.0356(8) Uani 1 1 d .
H25 H 0.3871 1.3364 0.7416 0.043 Uiso 1 1 calc R
C26 C 0.5051(4) 1.1795(3) 0.7336(3) 0.0357(8) Uani 1 1 d .
H26 H 0.5953 1.1972 0.7182 0.043 Uiso 1 1 calc R
C27 C 0.4958(4) 1.0697(3) 0.7430(3) 0.0339(8) Uani 1 1 d .
H27 H 0.5796 1.0132 0.7345 0.041 Uiso 1 1 calc R
C28 C 0.3611(3) 1.0443(3) 0.7650(2) 0.0271(7) Uani 1 1 d .
H28 H 0.3554 0.9702 0.7713 0.033 Uiso 1 1 calc R
C29 C 0.3714(5) 1.2336(4) 0.4922(3) 0.0567(11) Uani 1 1 d .
H29A H 0.4179 1.2736 0.5214 0.068 Uiso 1 1 calc R
H29B H 0.3278 1.1805 0.5503 0.068 Uiso 1 1 calc R
C30 C 0.1908(5) 0.5873(4) 0.6875(4) 0.0607(12) Uani 1 1 d .
H30A H 0.2099 0.5578 0.7577 0.073 Uiso 1 1 calc R
H30B H 0.1552 0.6680 0.6813 0.073 Uiso 1 1 calc R
O1 O 0.1614(3) 1.03331(19) 0.59034(17) 0.0386(6) Uani 1 1 d .
Cl1 Cl 0.50193(12) 1.16023(11) 0.39955(9) 0.0688(3) Uani 1 1 d .
Cl2 Cl 0.23561(15) 1.32959(10) 0.43623(10) 0.0799(4) Uani 1 1 d .
Cl3 Cl 0.35355(13) 0.55881(9) 0.59034(11) 0.0689(3) Uani 1 1 d .
Cl4 Cl 0.05724(13) 0.52760(9) 0.67456(10) 0.0623(3) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 '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'
Cl Cl 0.1484 0.1585 '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'
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
P2 Pd1 P2 180.000(1) . 2_577
P2 Pd1 P1 70.37(3) . .
P2 Pd1 P1 109.63(3) 2_577 .
P2 Pd1 P1 109.63(3) . 2_577
P2 Pd1 P1 70.37(3) 2_577 2_577
P1 Pd1 P1 180.00(2) . 2_577
C4 P1 C11 112.47(14) . .
C4 P1 C5 114.65(13) . .
C11 P1 C5 101.91(13) . .
C4 P1 Pd1 93.89(10) . .
C11 P1 Pd1 116.50(9) . .
C5 P1 Pd1 118.08(10) . .
C11 P1 P2 132.04(10) . .
C5 P1 P2 124.34(9) . .
Pd1 P1 P2 54.51(2) . .
C4 P2 C17 114.17(13) . .
C4 P2 C23 111.00(14) . .
C17 P2 C23 105.76(13) . .
C4 P2 Pd1 94.41(10) . .
C17 P2 Pd1 115.46(10) . .
C23 P2 Pd1 116.06(9) . .
C17 P2 P1 122.09(10) . .
C23 P2 P1 130.53(10) . .
Pd1 P2 P1 55.11(2) . .
C3 N1 C1 106.4(3) . .
N1 C1 C2 105.3(3) . .
N1 C1 H1A 110.7 . .
C2 C1 H1A 110.7 . .
N1 C1 H1B 110.7 . .
C2 C1 H1B 110.7 . .
H1A C1 H1B 108.8 . .
O1 C2 C1 104.5(3) . .
O1 C2 H2A 110.9 . .
C1 C2 H2A 110.9 . .
O1 C2 H2B 110.9 . .
C1 C2 H2B 110.9 . .
H2A C2 H2B 108.9 . .
N1 C3 O1 117.9(3) . .
N1 C3 C4 125.9(3) . .
O1 C3 C4 116.1(3) . .
C3 C4 P1 130.5(2) . .
C3 C4 P2 128.9(2) . .
P1 C4 P2 100.30(16) . .
C10 C5 C6 119.1(3) . .
C10 C5 P1 120.0(2) . .
C6 C5 P1 120.8(2) . .
C7 C6 C5 119.7(3) . .
C7 C6 H6 120.1 . .
C5 C6 H6 120.1 . .
C8 C7 C6 120.3(3) . .
C8 C7 H7 119.8 . .
C6 C7 H7 119.8 . .
C9 C8 C7 120.2(3) . .
C9 C8 H8 119.9 . .
C7 C8 H8 119.9 . .
C8 C9 C10 119.7(3) . .
C8 C9 H9 120.1 . .
C10 C9 H9 120.1 . .
C5 C10 C9 120.8(3) . .
C5 C10 H10 119.6 . .
C9 C10 H10 119.6 . .
C12 C11 C16 118.5(3) . .
C12 C11 P1 120.8(2) . .
C16 C11 P1 120.5(2) . .
C13 C12 C11 120.7(3) . .
C13 C12 H12 119.7 . .
C11 C12 H12 119.7 . .
C14 C13 C12 119.6(3) . .
C14 C13 H13 120.2 . .
C12 C13 H13 120.2 . .
C15 C14 C13 120.4(3) . .
C15 C14 H14 119.8 . .
C13 C14 H14 119.8 . .
C14 C15 C16 120.3(3) . .
C14 C15 H15 119.9 . .
C16 C15 H15 119.9 . .
C15 C16 C11 120.6(3) . .
C15 C16 H16 119.7 . .
C11 C16 H16 119.7 . .
C22 C17 C18 118.8(3) . .
C22 C17 P2 118.9(2) . .
C18 C17 P2 122.3(2) . .
C19 C18 C17 120.2(3) . .
C19 C18 H18 119.9 . .
C17 C18 H18 119.9 . .
C20 C19 C18 120.7(3) . .
C20 C19 H19 119.6 . .
C18 C19 H19 119.6 . .
C19 C20 C21 119.6(3) . .
C19 C20 H20 120.2 . .
C21 C20 H20 120.2 . .
C20 C21 C22 119.9(3) . .
C20 C21 H21 120.0 . .
C22 C21 H21 120.0 . .
C17 C22 C21 120.7(3) . .
C17 C22 H22 119.6 . .
C21 C22 H22 119.6 . .
C28 C23 C24 118.7(3) . .
C28 C23 P2 118.4(2) . .
C24 C23 P2 122.4(2) . .
C25 C24 C23 119.8(3) . .
C25 C24 H24 120.1 . .
C23 C24 H24 120.1 . .
C26 C25 C24 120.7(3) . .
C26 C25 H25 119.6 . .
C24 C25 H25 119.6 . .
C25 C26 C27 119.8(3) . .
C25 C26 H26 120.1 . .
C27 C26 H26 120.1 . .
C26 C27 C28 119.7(3) . .
C26 C27 H27 120.1 . .
C28 C27 H27 120.1 . .
C27 C28 C23 121.2(3) . .
C27 C28 H28 119.4 . .
C23 C28 H28 119.4 . .
Cl1 C29 Cl2 112.1(2) . .
Cl1 C29 H29A 109.2 . .
Cl2 C29 H29A 109.2 . .
Cl1 C29 H29B 109.2 . .
Cl2 C29 H29B 109.2 . .
H29A C29 H29B 107.9 . .
Cl4 C30 Cl3 112.0(2) . .
Cl4 C30 H30A 109.2 . .
Cl3 C30 H30A 109.2 . .
Cl4 C30 H30B 109.2 . .
Cl3 C30 H30B 109.2 . .
H30A C30 H30B 107.9 . .
C3 O1 C2 106.0(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Pd1 P2 2.3219(7) .
Pd1 P2 2.3219(7) 2_577
Pd1 P1 2.3391(7) .
Pd1 P1 2.3391(7) 2_577
P1 C4 1.748(3) .
P1 C11 1.826(3) .
P1 C5 1.827(3) .
P1 P2 2.6859(10) .
P2 C4 1.751(3) .
P2 C17 1.822(3) .
P2 C23 1.823(3) .
N1 C3 1.291(4) .
N1 C1 1.475(4) .
C1 C2 1.522(6) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 O1 1.455(4) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 O1 1.362(4) .
C3 C4 1.432(4) .
C5 C10 1.385(4) .
C5 C6 1.393(4) .
C6 C7 1.387(4) .
C6 H6 0.9300 .
C7 C8 1.384(5) .
C7 H7 0.9300 .
C8 C9 1.371(5) .
C8 H8 0.9300 .
C9 C10 1.387(4) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 C12 1.397(4) .
C11 C16 1.399(4) .
C12 C13 1.391(4) .
C12 H12 0.9300 .
C13 C14 1.385(5) .
C13 H13 0.9300 .
C14 C15 1.378(5) .
C14 H14 0.9300 .
C15 C16 1.380(4) .
C15 H15 0.9300 .
C16 H16 0.9300 .
C17 C22 1.387(4) .
C17 C18 1.393(4) .
C18 C19 1.383(4) .
C18 H18 0.9300 .
C19 C20 1.379(5) .
C19 H19 0.9300 .
C20 C21 1.381(5) .
C20 H20 0.9300 .
C21 C22 1.389(4) .
C21 H21 0.9300 .
C22 H22 0.9300 .
C23 C28 1.388(4) .
C23 C24 1.398(4) .
C24 C25 1.389(4) .
C24 H24 0.9300 .
C25 C26 1.378(5) .
C25 H25 0.9300 .
C26 C27 1.382(5) .
C26 H26 0.9300 .
C27 C28 1.385(4) .
C27 H27 0.9300 .
C28 H28 0.9300 .
C29 Cl1 1.741(4) .
C29 Cl2 1.748(4) .
C29 H29A 0.9700 .
C29 H29B 0.9700 .
C30 Cl4 1.753(4) .
C30 Cl3 1.761(5) .
C30 H30A 0.9700 .
C30 H30B 0.9700 .
