#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:43:41 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179761 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/57/7005701.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_7005701
loop_
_publ_author_name
'Aguirre, Pedro A.'
'Lagos, Carolina A.'
'Moya, Sergio A.'
'Zúñiga, César'
'Vera-Oyarce, Cristian'
'Sola, Eduardo'
'Peris, Gabriel'
'Bayón, J Carles'
_publ_section_title
;
 Methoxycarbonylation of olefins catalyzed by palladium complexes
 bearing P,N-donor ligands.
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5419
_journal_page_last               5426
_journal_paper_doi               10.1039/b704615b
_journal_year                    2007
_chemical_formula_sum            'C37 H30 Cl6 N2 P2 Pd'
_chemical_formula_weight         883.67
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                94.061(2)
_cell_angle_beta                 95.855(2)
_cell_angle_gamma                99.201(2)
_cell_formula_units_Z            2
_cell_length_a                   9.6006(7)
_cell_length_b                   13.8728(10)
_cell_length_c                   15.8526(11)
_cell_measurement_temperature    293(2)
_cell_volume                     2065.1(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.49
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0725
_diffrn_reflns_av_sigmaI/netI    0.1703
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11899
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.942
_exptl_absorpt_correction_T_max  0.9456
_exptl_absorpt_correction_T_min  0.8555
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.421
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       prism
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.468
_refine_diff_density_min         -0.903
_refine_diff_density_rms         0.161
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         7270
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.1774
_refine_ls_R_factor_gt           0.0858
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1424P)²+5.2921P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2292
_refine_ls_wR_factor_ref         0.2871
_reflns_number_gt                3717
_reflns_number_total             7270
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b704615b.txt
_cod_data_source_block           str841m
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7005701
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
_atom_site_disorder_assembly
_atom_site_disorder_group
C31 C 0.8668(17) 0.8880(13) 0.9648(10) 0.072(5) Uani 1 1 d . . .
H31 H 0.9376 0.8620 0.9956 0.086 Uiso 1 1 calc R . .
Pd1 Pd 0.95107(10) 0.80983(7) 0.69077(6) 0.0322(3) Uani 1 1 d . . .
P2 P 0.7936(3) 0.6953(2) 0.61016(18) 0.0308(7) Uani 1 1 d . . .
P3 P 0.9070(3) 0.7647(2) 0.82275(18) 0.0338(8) Uani 1 1 d . . .
N1 N 1.0041(10) 0.8511(7) 0.5711(6) 0.036(2) Uani 1 1 d . . .
C24 C 1.1168(12) 0.9179(9) 0.5606(8) 0.040(3) Uani 1 1 d . . .
H24 H 1.1757 0.9483 0.6085 0.049 Uiso 1 1 calc R . .
C20 C 0.9215(12) 0.8078(9) 0.5022(7) 0.032(3) Uani 1 1 d . . .
C1 C 0.8163(12) 0.5701(9) 0.5974(7) 0.033(3) Uani 1 1 d . . .
C30 C 0.8311(14) 0.8593(9) 0.8776(8) 0.043(3) Uani 1 1 d . . .
C2 C 0.7072(14) 0.4960(9) 0.5657(8) 0.047(3) Uani 1 1 d . . .
H2 H 0.6166 0.5102 0.5520 0.057 Uiso 1 1 calc R . .
C21 C 0.9467(13) 0.8316(9) 0.4198(7) 0.037(3) Uani 1 1 d . . .
H21 H 0.8855 0.8024 0.3724 0.044 Uiso 1 1 calc R . .
C4 C 0.863(2) 0.3779(13) 0.5714(11) 0.081(5) Uani 1 1 d . . .
H4 H 0.8788 0.3137 0.5631 0.097 Uiso 1 1 calc R . .
C11 C 0.5662(15) 0.7901(11) 0.6082(10) 0.063(4) Uani 1 1 d . . .
H11 H 0.6258 0.8380 0.5847 0.076 Uiso 1 1 calc R . .
C22 C 1.0617(15) 0.8978(10) 0.4115(8) 0.048(4) Uani 1 1 d . . .
H22 H 1.0826 0.9129 0.3575 0.058 Uiso 1 1 calc R . .
C15 C 0.5217(12) 0.6349(10) 0.6623(8) 0.041(3) Uani 1 1 d . . .
H15 H 0.5511 0.5766 0.6758 0.049 Uiso 1 1 calc R . .
C10 C 0.6128(12) 0.7024(9) 0.6264(7) 0.034(3) Uani 1 1 d . . .
C6 C 0.9508(14) 0.5490(11) 0.6160(8) 0.050(4) Uani 1 1 d . . .
H6 H 1.0253 0.5988 0.6377 0.060 Uiso 1 1 calc R . .
C40 C 1.0652(13) 0.7446(10) 0.8858(7) 0.041(3) Uani 1 1 d . . .
C23 C 1.1484(14) 0.9432(10) 0.4815(8) 0.043(3) Uani 1 1 d . . .
H23 H 1.2270 0.9901 0.4758 0.052 Uiso 1 1 calc R . .
C14 C 0.3899(15) 0.6498(12) 0.6792(9) 0.061(4) Uani 1 1 d . . .
H14 H 0.3307 0.6019 0.7030 0.074 Uiso 1 1 calc R . .
C3 C 0.7311(19) 0.3982(11) 0.5534(10) 0.068(4) Uani 1 1 d . . .
H3 H 0.6561 0.3482 0.5331 0.081 Uiso 1 1 calc R . .
C50 C 0.7865(13) 0.6519(9) 0.8291(7) 0.039(3) Uani 1 1 d . . .
C55 C 0.6547(13) 0.6496(11) 0.8624(8) 0.050(4) Uani 1 1 d . . .
H55 H 0.6252 0.7075 0.8806 0.061 Uiso 1 1 calc R . .
C51 C 0.8244(15) 0.5647(9) 0.8026(8) 0.047(3) Uani 1 1 d . . .
H51 H 0.9117 0.5654 0.7819 0.056 Uiso 1 1 calc R . .
C52 C 0.7392(17) 0.4772(11) 0.8055(9) 0.060(4) Uani 1 1 d . . .
H52 H 0.7675 0.4194 0.7858 0.071 Uiso 1 1 calc R . .
C35 C 0.726(2) 0.8965(13) 0.8327(12) 0.085(6) Uani 1 1 d . . .
H35 H 0.6986 0.8775 0.7752 0.101 Uiso 1 1 calc R . .
C5 C 0.9756(19) 0.4523(13) 0.6022(10) 0.068(5) Uani 1 1 d . . .
H5 H 1.0667 0.4382 0.6137 0.082 Uiso 1 1 calc R . .
C13 C 0.3448(17) 0.7362(14) 0.6608(11) 0.073(5) Uani 1 1 d . . .
H13 H 0.2554 0.7470 0.6728 0.088 Uiso 1 1 calc R . .
C12 C 0.4321(17) 0.8066(12) 0.6247(11) 0.072(5) Uani 1 1 d . . .
H12 H 0.4016 0.8647 0.6116 0.087 Uiso 1 1 calc R . .
C53 C 0.6111(18) 0.4743(13) 0.8376(10) 0.069(5) Uani 1 1 d . . .
H53 H 0.5517 0.4147 0.8389 0.083 Uiso 1 1 calc R . .
C33 C 0.690(2) 0.9914(15) 0.9592(16) 0.097(7) Uani 1 1 d . . .
H33 H 0.6402 1.0341 0.9869 0.117 Uiso 1 1 calc R . .
C41 C 1.2004(15) 0.7759(12) 0.8676(9) 0.060(4) Uani 1 1 d . . .
H41 H 1.2123 0.8104 0.8199 0.072 Uiso 1 1 calc R . .
C45 C 1.0551(17) 0.6953(14) 0.9593(8) 0.075(5) Uani 1 1 d . . .
H45 H 0.9656 0.6720 0.9744 0.090 Uiso 1 1 calc R . .
C44 C 1.1716(18) 0.6802(16) 1.0094(10) 0.087(6) Uani 1 1 d . . .
H44 H 1.1613 0.6496 1.0592 0.104 Uiso 1 1 calc R . .
C42 C 1.3192(16) 0.7592(14) 0.9161(11) 0.076(5) Uani 1 1 d . . .
H42 H 1.4097 0.7808 0.9017 0.091 Uiso 1 1 calc R . .
C34 C 0.659(2) 0.9662(16) 0.8782(16) 0.108(7) Uani 1 1 d . . .
H34 H 0.5900 0.9946 0.8482 0.130 Uiso 1 1 calc R . .
C43 C 1.2994(19) 0.7092(15) 0.9872(12) 0.086(6) Uani 1 1 d . . .
H43 H 1.3782 0.6955 1.0205 0.103 Uiso 1 1 calc R . .
C32 C 0.799(2) 0.9528(15) 1.0041(13) 0.094(6) Uani 1 1 d . . .
H32 H 0.8247 0.9723 1.0617 0.113 Uiso 1 1 calc R . .
N2 N 0.8078(10) 0.7387(7) 0.5148(5) 0.037(2) Uani 1 1 d . . .
H70 H 0.7429 0.7175 0.4732 0.045 Uiso 1 1 calc R . .
Cl2 Cl 1.0837(4) 0.9540(3) 0.7617(2) 0.0611(11) Uani 1 1 d . . .
C54 C 0.5708(16) 0.5601(13) 0.8676(10) 0.069(5) Uani 1 1 d . . .
H54 H 0.4861 0.5576 0.8917 0.083 Uiso 1 1 calc R . .
Cl1 Cl 0.6416(4) 0.6263(3) 0.3510(2) 0.0508(9) Uani 1 1 d . . .
C61 C 0.8078(18) 0.6541(15) 0.1722(11) 0.088(6) Uani 1 1 d . . .
Cl20 Cl 0.8458(9) 0.5410(6) 0.1387(7) 0.119(3) Uani 0.67 1 d P . .
Cl21 Cl 0.7030(6) 0.6897(7) 0.0899(4) 0.107(3) Uani 0.67 1 d P . .
Cl22 Cl 0.9614(7) 0.7387(8) 0.1968(4) 0.125(4) Uani 0.67 1 d P . .
C60 C 0.4890(16) 0.8235(13) 0.3073(11) 0.074(5) Uani 1 1 d . . .
Cl12 Cl 0.4675(10) 0.8847(7) 0.4059(5) 0.119(3) Uani 0.67 1 d P . .
Cl10 Cl 0.6220(6) 0.8950(5) 0.2661(4) 0.0747(18) Uani 0.67 1 d P . .
Cl11 Cl 0.3292(7) 0.8047(5) 0.2454(6) 0.109(3) Uani 0.67 1 d P . .
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'
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
C32 C31 C30 120.3(17) . . ?
N1 Pd1 P2 82.4(3) . . ?
N1 Pd1 P3 176.7(3) . . ?
P2 Pd1 P3 99.59(11) . . ?
N1 Pd1 Cl2 92.4(3) . . ?
P2 Pd1 Cl2 166.89(13) . . ?
P3 Pd1 Cl2 86.19(12) . . ?
N2 P2 C1 106.2(5) . . ?
N2 P2 C10 102.9(5) . . ?
C1 P2 C10 110.0(6) . . ?
N2 P2 Pd1 99.5(4) . . ?
C1 P2 Pd1 122.4(4) . . ?
C10 P2 Pd1 113.1(4) . . ?
C40 P3 C50 102.0(6) . . ?
C40 P3 C30 109.5(6) . . ?
C50 P3 C30 105.4(6) . . ?
C40 P3 Pd1 112.2(4) . . ?
C50 P3 Pd1 118.1(4) . . ?
C30 P3 Pd1 109.1(4) . . ?
C20 N1 C24 118.1(10) . . ?
C20 N1 Pd1 118.0(8) . . ?
C24 N1 Pd1 123.8(8) . . ?
N1 C24 C23 122.4(12) . . ?
N1 C20 N2 116.9(10) . . ?
N1 C20 C21 122.2(11) . . ?
N2 C20 C21 120.9(10) . . ?
C2 C1 C6 119.5(12) . . ?
C2 C1 P2 122.5(9) . . ?
C6 C1 P2 117.9(10) . . ?
C35 C30 C31 119.8(14) . . ?
C35 C30 P3 117.4(11) . . ?
C31 C30 P3 122.5(12) . . ?
C1 C2 C3 120.7(13) . . ?
C22 C21 C20 118.0(11) . . ?
C3 C4 C5 120.4(16) . . ?
C12 C11 C10 121.0(14) . . ?
C21 C22 C23 120.8(11) . . ?
C14 C15 C10 122.8(13) . . ?
C15 C10 C11 117.1(12) . . ?
C15 C10 P2 126.4(10) . . ?
C11 C10 P2 116.1(9) . . ?
C1 C6 C5 120.1(14) . . ?
C41 C40 C45 115.3(12) . . ?
C41 C40 P3 124.3(10) . . ?
C45 C40 P3 120.3(10) . . ?
C22 C23 C24 118.4(12) . . ?
C15 C14 C13 119.7(15) . . ?
C4 C3 C2 119.7(16) . . ?
C51 C50 C55 118.2(12) . . ?
C51 C50 P3 119.2(10) . . ?
C55 C50 P3 122.6(10) . . ?
C54 C55 C50 119.0(14) . . ?
C52 C51 C50 122.4(13) . . ?
C51 C52 C53 119.8(15) . . ?
C30 C35 C34 117.1(18) . . ?
C4 C5 C6 119.6(14) . . ?
C12 C13 C14 120.0(15) . . ?
C13 C12 C11 119.4(15) . . ?
C52 C53 C54 119.8(16) . . ?
C34 C33 C32 118.7(19) . . ?
C40 C41 C42 123.3(15) . . ?
C44 C45 C40 122.2(15) . . ?
C43 C44 C45 119.9(16) . . ?
C41 C42 C43 117.5(16) . . ?
C33 C34 C35 123(2) . . ?
C44 C43 C42 121.7(17) . . ?
C31 C32 C33 120.8(18) . . ?
C20 N2 P2 121.0(8) . . ?
C53 C54 C55 120.8(14) . . ?
Cl21 C61 Cl22 110.0(11) . . ?
Cl21 C61 Cl20 107.0(11) . . ?
Cl22 C61 Cl20 110.8(11) . . ?
Cl10 C60 Cl11 114.4(11) . . ?
Cl10 C60 Cl12 106.8(10) . . ?
Cl11 C60 Cl12 107.8(10) . . ?
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
C31 C32 1.35(2) . ?
C31 C30 1.403(19) . ?
Pd1 N1 2.107(9) . ?
Pd1 P2 2.234(3) . ?
Pd1 P3 2.287(3) . ?
Pd1 Cl2 2.337(3) . ?
P2 N2 1.676(9) . ?
P2 C1 1.786(12) . ?
P2 C10 1.797(12) . ?
P3 C40 1.803(12) . ?
P3 C50 1.806(13) . ?
P3 C30 1.812(13) . ?
N1 C20 1.327(14) . ?
N1 C24 1.340(14) . ?
C24 C23 1.377(16) . ?
C20 N2 1.374(14) . ?
C20 C21 1.405(15) . ?
C1 C2 1.372(16) . ?
C1 C6 1.376(17) . ?
C30 C35 1.37(2) . ?
C2 C3 1.415(19) . ?
C21 C22 1.342(17) . ?
C4 C3 1.35(2) . ?
C4 C5 1.39(2) . ?
C11 C12 1.39(2) . ?
C11 C10 1.400(18) . ?
C22 C23 1.365(18) . ?
C15 C14 1.364(18) . ?
C15 C10 1.372(16) . ?
C6 C5 1.41(2) . ?
C40 C41 1.368(18) . ?
C40 C45 1.396(18) . ?
C14 C13 1.38(2) . ?
C50 C51 1.368(17) . ?
C50 C55 1.417(17) . ?
C55 C54 1.381(19) . ?
C51 C52 1.357(18) . ?
C52 C53 1.37(2) . ?
C35 C34 1.44(2) . ?
C13 C12 1.38(2) . ?
C53 C54 1.38(2) . ?
C33 C34 1.30(3) . ?
C33 C32 1.41(3) . ?
C41 C42 1.37(2) . ?
C45 C44 1.36(2) . ?
C44 C43 1.32(2) . ?
C42 C43 1.38(2) . ?
C61 Cl21 1.71(2) . ?
C61 Cl22 1.722(19) . ?
C61 Cl20 1.73(2) . ?
C60 Cl10 1.702(16) . ?
C60 Cl11 1.707(17) . ?
C60 Cl12 1.772(19) . ?
