#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:35:27 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179755 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/51/7005128.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_7005128
loop_
_publ_author_name
'Agostinho, Magno'
'Braunstein, Pierre'
'Welter, Richard'
_publ_section_title
;
 Phosphinito- and phosphonito-oxazoline Pd(II) complexes as CO/ethylene
 insertion intermediates: synthesis and structural characterization.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              759
_journal_page_last               770
_journal_paper_doi               10.1039/b616962g
_journal_year                    2007
_chemical_formula_moiety         'C19 H21 Cl N O3 P Pd'
_chemical_formula_sum            'C19 H21 Cl N O3 P Pd'
_chemical_formula_weight         484.19
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.79900(10)
_cell_length_b                   16.2160(2)
_cell_length_c                   21.6790(3)
_cell_measurement_reflns_used    14941
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.034
_cell_measurement_theta_min      0.998
_cell_volume                     3796.35(8)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'π scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.1135
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5540
_diffrn_reflns_theta_full        30.02
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    1.222
_exptl_absorpt_correction_T_max  0.887
_exptl_absorpt_correction_T_min  0.828
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements
Sortav (Blessing 1995)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.767
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         5539
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.767
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0300
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0978
_reflns_number_gt                3422
_reflns_number_total             5539
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b616962g.txt
_cod_data_source_block           welt46
_cod_database_code               7005128
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd 0.84787(2) 0.083440(14) 0.521098(11) 0.01912(8) Uani 1 1 d . . .
Cl Cl 0.89997(8) 0.13802(5) 0.42199(4) 0.02589(18) Uani 1 1 d . . .
P P 0.78109(8) 0.02481(5) 0.60431(4) 0.02049(18) Uani 1 1 d . . .
O1 O 1.1073(2) 0.18043(14) 0.65455(10) 0.0272(5) Uani 1 1 d . . .
O2 O 0.8602(2) 0.04817(14) 0.66523(10) 0.0243(5) Uani 1 1 d . . .
O3 O 0.7864(2) -0.07489(12) 0.60323(10) 0.0215(5) Uani 1 1 d . . .
N N 0.9833(2) 0.15563(15) 0.57322(12) 0.0196(6) Uani 1 1 d . . .
C1 C 1.1492(3) 0.2166(2) 0.51107(16) 0.0255(7) Uani 1 1 d . . .
H1A H 1.2060 0.1754 0.5282 0.038 Uiso 1 1 calc . . .
H1B H 1.1950 0.2672 0.5017 0.038 Uiso 1 1 calc . . .
H1C H 1.1116 0.1951 0.4732 0.038 Uiso 1 1 calc . . .
C2 C 0.9584(3) 0.2994(2) 0.53513(16) 0.0264(7) Uani 1 1 d . . .
H2A H 0.8940 0.3081 0.5663 0.040 Uiso 1 1 calc . . .
H2B H 0.9202 0.2806 0.4966 0.040 Uiso 1 1 calc . . .
H2C H 1.0025 0.3513 0.5278 0.040 Uiso 1 1 calc . . .
C3 C 1.0483(3) 0.23528(18) 0.55775(15) 0.0200(7) Uani 1 1 d . . .
C4 C 1.1040(3) 0.2583(2) 0.62080(16) 0.0278(7) Uani 1 1 d . . .
H4A H 1.1883 0.2814 0.6160 0.033 Uiso 1 1 calc . . .
H4B H 1.0513 0.2992 0.6423 0.033 Uiso 1 1 calc . . .
C5 C 1.0259(3) 0.1318(2) 0.62505(15) 0.0227(7) Uani 1 1 d . . .
C6 C 0.9928(3) 0.0532(2) 0.65768(16) 0.0280(8) Uani 1 1 d . . .
H6A H 1.0225 0.0054 0.6334 0.034 Uiso 1 1 calc . . .
H6B H 1.0335 0.0517 0.6986 0.034 Uiso 1 1 calc . . .
C7 C 0.7183(3) 0.0130(2) 0.47669(15) 0.0307(8) Uani 1 1 d . . .
H7A H 0.6675 -0.0160 0.5072 0.046 Uiso 1 1 calc . . .
H7B H 0.7601 -0.0273 0.4502 0.046 Uiso 1 1 calc . . .
H7C H 0.6654 0.0486 0.4514 0.046 Uiso 1 1 calc . . .
C8 C 0.7472(3) -0.1187(2) 0.65502(14) 0.0223(7) Uani 1 1 d . . .
C9 C 0.8118(3) -0.1900(2) 0.66863(15) 0.0280(8) Uani 1 1 d . . .
H9 H 0.8811 -0.2059 0.6444 0.034 Uiso 1 1 calc . . .
C10 C 0.7742(4) -0.2377(2) 0.71805(17) 0.0394(10) Uani 1 1 d . . .
H10 H 0.8166 -0.2875 0.7274 0.047 Uiso 1 1 calc . . .
C11 C 0.6751(4) -0.2131(2) 0.75371(18) 0.0393(10) Uani 1 1 d . . .
H11 H 0.6506 -0.2454 0.7881 0.047 Uiso 1 1 calc . . .
C12 C 0.6114(3) -0.1420(2) 0.73980(16) 0.0317(8) Uani 1 1 d . . .
H12 H 0.5439 -0.1258 0.7651 0.038 Uiso 1 1 calc . . .
C13 C 0.6441(3) -0.09287(19) 0.68895(14) 0.0215(7) Uani 1 1 d . . .
C14 C 0.5729(3) -0.0190(2) 0.67126(14) 0.0226(7) Uani 1 1 d . . .
C15 C 0.4505(3) -0.0065(2) 0.68997(15) 0.0298(8) Uani 1 1 d . . .
H15 H 0.4107 -0.0467 0.7150 0.036 Uiso 1 1 calc . . .
C16 C 0.3861(3) 0.0640(3) 0.67235(17) 0.0359(9) Uani 1 1 d . . .
H16 H 0.3035 0.0718 0.6861 0.043 Uiso 1 1 calc . . .
C17 C 0.4408(4) 0.1226(2) 0.63510(17) 0.0347(9) Uani 1 1 d . . .
H17 H 0.3963 0.1707 0.6235 0.042 Uiso 1 1 calc . . .
C18 C 0.5608(3) 0.1107(2) 0.61484(15) 0.0286(8) Uani 1 1 d . . .
H18 H 0.5982 0.1503 0.5885 0.034 Uiso 1 1 calc . . .
C19 C 0.6275(3) 0.04076(19) 0.63290(14) 0.0216(7) 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
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 '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'
P P 0.1023 0.0942 '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'
Pd Pd -0.9988 1.0072 '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
_geom_angle_publ_flag
C7 Pd P 85.36(10) . . ?
C7 Pd N 176.92(12) . . ?
P Pd N 91.56(7) . . ?
C7 Pd Cl 86.83(10) . . ?
P Pd Cl 172.18(3) . . ?
N Pd Cl 96.25(7) . . ?
O2 P O3 103.12(12) . . ?
O2 P C19 99.95(13) . . ?
O3 P C19 100.52(13) . . ?
O2 P Pd 113.69(9) . . ?
O3 P Pd 114.54(9) . . ?
C19 P Pd 122.30(11) . . ?
C5 O1 C4 104.6(2) . . ?
C6 O2 P 116.4(2) . . ?
C8 O3 P 119.1(2) . . ?
C5 N C3 106.7(3) . . ?
C5 N Pd 122.3(2) . . ?
C3 N Pd 130.90(19) . . ?
C3 C1 H1A 109.5 . . ?
C3 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C3 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C3 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C2 C3 N 111.3(2) . . ?
C2 C3 C1 112.6(3) . . ?
N C3 C1 108.2(2) . . ?
C2 C3 C4 111.9(3) . . ?
N C3 C4 101.1(2) . . ?
C1 C3 C4 111.1(3) . . ?
O1 C4 C3 104.2(2) . . ?
O1 C4 H4A 110.9 . . ?
C3 C4 H4A 110.9 . . ?
O1 C4 H4B 110.9 . . ?
C3 C4 H4B 110.9 . . ?
H4A C4 H4B 108.9 . . ?
N C5 O1 118.6(3) . . ?
N C5 C6 126.0(3) . . ?
O1 C5 C6 115.4(3) . . ?
O2 C6 C5 109.7(3) . . ?
O2 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
O2 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
Pd C7 H7A 109.5 . . ?
Pd C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Pd C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 O3 116.4(3) . . ?
C9 C8 C13 122.7(3) . . ?
O3 C8 C13 120.9(3) . . ?
C8 C9 C10 119.0(3) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C12 C11 C10 120.5(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 121.4(3) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C8 C13 C12 116.3(3) . . ?
C8 C13 C14 121.4(3) . . ?
C12 C13 C14 122.3(3) . . ?
C15 C14 C19 117.9(3) . . ?
C15 C14 C13 122.4(3) . . ?
C19 C14 C13 119.7(3) . . ?
C16 C15 C14 120.8(3) . . ?
C16 C15 H15 119.6 . . ?
C14 C15 H15 119.6 . . ?
C17 C16 C15 120.8(3) . . ?
C17 C16 H16 119.6 . . ?
C15 C16 H16 119.6 . . ?
C16 C17 C18 119.5(3) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C19 120.4(3) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C14 120.6(3) . . ?
C18 C19 P 119.8(3) . . ?
C14 C19 P 119.6(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd C7 2.047(3) . ?
Pd P 2.1629(8) . ?
Pd N 2.187(3) . ?
Pd Cl 2.3909(8) . ?
P O2 1.618(2) . ?
P O3 1.618(2) . ?
P C19 1.790(3) . ?
O1 C5 1.343(4) . ?
O1 C4 1.460(4) . ?
O2 C6 1.444(4) . ?
O3 C8 1.395(4) . ?
N C5 1.274(4) . ?
N C3 1.508(4) . ?
C1 C3 1.517(4) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.505(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 C4 1.539(4) . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.501(5) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.382(5) . ?
C8 C13 1.398(4) . ?
C9 C10 1.383(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.380(5) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(5) . ?
C11 H11 0.9500 . ?
C12 C13 1.406(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.474(4) . ?
C14 C15 1.398(4) . ?
C14 C19 1.406(4) . ?
C15 C16 1.391(5) . ?
C15 H15 0.9500 . ?
C16 C17 1.380(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.381(5) . ?
C17 H17 0.9500 . ?
C18 C19 1.400(5) . ?
C18 H18 0.9500 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C7 Pd P O2 174.25(15) . . . . ?
N Pd P O2 -5.67(12) . . . . ?
Cl Pd P O2 177.7(2) . . . . ?
C7 Pd P O3 56.04(14) . . . . ?
N Pd P O3 -123.89(12) . . . . ?
Cl Pd P O3 59.4(3) . . . . ?
C7 Pd P C19 -65.70(16) . . . . ?
N Pd P C19 114.38(14) . . . . ?
Cl Pd P C19 -62.3(3) . . . . ?
O3 P O2 C6 84.6(2) . . . . ?
C19 P O2 C6 -172.0(2) . . . . ?
Pd P O2 C6 -40.0(3) . . . . ?
O2 P O3 C8 55.0(2) . . . . ?
C19 P O3 C8 -47.9(3) . . . . ?
Pd P O3 C8 179.1(2) . . . . ?
C7 Pd N C5 24(2) . . . . ?
P Pd N C5 25.4(3) . . . . ?
Cl Pd N C5 -155.0(2) . . . . ?
C7 Pd N C3 -159(2) . . . . ?
P Pd N C3 -157.8(2) . . . . ?
Cl Pd N C3 21.7(2) . . . . ?
C5 N C3 C2 -134.5(3) . . . . ?
Pd N C3 C2 48.3(3) . . . . ?
C5 N C3 C1 101.3(3) . . . . ?
Pd N C3 C1 -75.8(3) . . . . ?
C5 N C3 C4 -15.5(3) . . . . ?
Pd N C3 C4 167.4(2) . . . . ?
C5 O1 C4 C3 -19.8(3) . . . . ?
C2 C3 C4 O1 139.7(3) . . . . ?
N C3 C4 O1 21.1(3) . . . . ?
C1 C3 C4 O1 -93.5(3) . . . . ?
C3 N C5 O1 3.6(4) . . . . ?
Pd N C5 O1 -179.0(2) . . . . ?
C3 N C5 C6 -176.9(3) . . . . ?
Pd N C5 C6 0.5(5) . . . . ?
C4 O1 C5 N 11.0(4) . . . . ?
C4 O1 C5 C6 -168.6(3) . . . . ?
P O2 C6 C5 75.6(3) . . . . ?
N C5 C6 O2 -54.8(4) . . . . ?
O1 C5 C6 O2 124.7(3) . . . . ?
P O3 C8 C9 -144.1(3) . . . . ?
P O3 C8 C13 38.7(4) . . . . ?
O3 C8 C9 C10 -177.5(3) . . . . ?
C13 C8 C9 C10 -0.5(5) . . . . ?
C8 C9 C10 C11 -1.4(6) . . . . ?
C9 C10 C11 C12 1.3(6) . . . . ?
C10 C11 C12 C13 0.6(6) . . . . ?
C9 C8 C13 C12 2.2(5) . . . . ?
O3 C8 C13 C12 179.2(3) . . . . ?
C9 C8 C13 C14 -176.6(3) . . . . ?
O3 C8 C13 C14 0.3(5) . . . . ?
C11 C12 C13 C8 -2.3(5) . . . . ?
C11 C12 C13 C14 176.6(3) . . . . ?
C8 C13 C14 C15 158.3(3) . . . . ?
C12 C13 C14 C15 -20.5(5) . . . . ?
C8 C13 C14 C19 -20.0(5) . . . . ?
C12 C13 C14 C19 161.2(3) . . . . ?
C19 C14 C15 C16 -1.7(5) . . . . ?
C13 C14 C15 C16 -180.0(3) . . . . ?
C14 C15 C16 C17 1.2(5) . . . . ?
C15 C16 C17 C18 0.4(6) . . . . ?
C16 C17 C18 C19 -1.3(5) . . . . ?
C17 C18 C19 C14 0.8(5) . . . . ?
C17 C18 C19 P 178.1(3) . . . . ?
C15 C14 C19 C18 0.7(5) . . . . ?
C13 C14 C19 C18 179.0(3) . . . . ?
C15 C14 C19 P -176.6(2) . . . . ?
C13 C14 C19 P 1.8(4) . . . . ?
O2 P C19 C18 105.2(3) . . . . ?
O3 P C19 C18 -149.3(3) . . . . ?
Pd P C19 C18 -21.2(3) . . . . ?
O2 P C19 C14 -77.5(3) . . . . ?
O3 P C19 C14 28.0(3) . . . . ?
Pd P C19 C14 156.1(2) . . . . ?
