#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/94/2209484.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_2209484
loop_
_publ_author_name
'Meijboom, Reinout'
'Muller, Alfred'
'Roodt, Andreas'
_publ_section_title
;
 trans-Dichlorobis(tri-m-tolylphosphine)palladium(II)
;
_journal_coeditor_code           ER2006
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1603
_journal_page_last               m1605
_journal_paper_doi               10.1107/S1600536806022264
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Pd Cl2 (C21 H21 P)2]'
_chemical_formula_moiety         'C42 H42 Cl2 P2 Pd'
_chemical_formula_sum            'C42 H42 Cl2 P2 Pd'
_chemical_formula_weight         786
_chemical_name_systematic
;
trans-Dichlorobis(tri-m-tolylphosphine)palladium(II)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                108.102(2)
_cell_angle_beta                 114.206(2)
_cell_angle_gamma                102.811(2)
_cell_formula_units_Z            1
_cell_length_a                   10.1864(3)
_cell_length_b                   10.4434(3)
_cell_length_c                   11.1137(5)
_cell_measurement_reflns_used    7240
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.25
_cell_volume                     938.17(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker 2004)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al.,  1999)'
_diffrn_detector_area_resol_mean 8.2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX-II 4K KappaCCD area-detector'
_diffrn_measurement_method       'ω and φ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            44847
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         2.24
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.751
_exptl_absorpt_correction_T_max  0.9087
_exptl_absorpt_correction_T_min  0.8582
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 1998)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.329
_refine_diff_density_min         -0.499
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4673
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0319P)²+1.0272P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0693
_reflns_number_gt                4360
_reflns_number_total             4673
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            er2006.cif
_cod_data_source_block           I
_cod_database_code               2209484
_cod_database_fobs_code          2209484
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
C C1 0.8517(2) 0.49478(19) 0.71106(19) 0.0177(3) Uani d . 1
C C2 0.9068(2) 0.59641(19) 0.66733(19) 0.0187(3) Uani d . 1
H H2 0.8443 0.646 0.6311 0.022 Uiso calc R 1
C C3 1.0516(2) 0.6264(2) 0.6758(2) 0.0201(3) Uani d . 1
C C4 1.1112(2) 0.7389(2) 0.6323(2) 0.0258(4) Uani d . 1
H H4A 1.0238 0.7591 0.5729 0.039 Uiso calc R 1
H H4B 1.1568 0.7009 0.5741 0.039 Uiso calc R 1
H H4C 1.1917 0.8299 0.7214 0.039 Uiso calc R 1
C C5 1.1400(2) 0.5501(2) 0.7274(2) 0.0240(4) Uani d . 1
H H5 1.2385 0.5681 0.7332 0.029 Uiso calc R 1
C C6 1.0862(2) 0.4488(2) 0.7702(2) 0.0266(4) Uani d . 1
H H6 1.1479 0.3979 0.8048 0.032 Uiso calc R 1
C C7 0.9419(2) 0.4208(2) 0.7628(2) 0.0235(4) Uani d . 1
H H7 0.9057 0.3517 0.793 0.028 Uiso calc R 1
C C8 0.7177(2) 0.6107(2) 0.8804(2) 0.0195(3) Uani d . 1
C C9 0.8601(2) 0.7336(2) 0.9697(2) 0.0221(4) Uani d . 1
H H9 0.9372 0.7409 0.942 0.027 Uiso calc R 1
C C10 0.8923(3) 0.8465(2) 1.0992(2) 0.0270(4) Uani d . 1
C C11 1.0461(3) 0.9804(3) 1.1916(3) 0.0387(5) Uani d . 1
H H11A 1.0427 1.0453 1.1439 0.058 Uiso calc R 1
H H11B 1.1324 0.9495 1.2008 0.058 Uiso calc R 1
H H11C 1.063 1.0333 1.2901 0.058 Uiso calc R 1
C C12 0.7780(3) 0.8328(2) 1.1379(2) 0.0297(4) Uani d . 1
H H12 0.7976 0.9081 1.2256 0.036 Uiso calc R 1
C C13 0.6356(3) 0.7108(2) 1.0502(2) 0.0288(4) Uani d . 1
H H13 0.559 0.7033 1.0785 0.035 Uiso calc R 1
C C14 0.6046(2) 0.6001(2) 0.9220(2) 0.0248(4) Uani d . 1
H H14 0.5068 0.517 0.8622 0.03 Uiso calc R 1
C C15 0.5833(2) 0.2980(2) 0.6984(2) 0.0228(4) Uani d . 1
C C16 0.6561(2) 0.2717(2) 0.8199(2) 0.0262(4) Uani d . 1
H H16 0.7495 0.347 0.9073 0.031 Uiso calc R 1
C C17 0.5911(3) 0.1336(2) 0.8133(3) 0.0302(4) Uani d . 1
C C18 0.6666(3) 0.1041(3) 0.9433(3) 0.0356(5) Uani d . 1
H H18A 0.6123 0.1171 0.9985 0.053 Uiso calc R 1
H H18B 0.7773 0.1729 1.0079 0.053 Uiso calc R 1
H H18C 0.6595 0.0029 0.9086 0.053 Uiso calc R 1
C C19 0.4539(3) 0.0271(2) 0.6861(3) 0.0324(5) Uani d . 1
H H19 0.41 -0.0661 0.6811 0.039 Uiso calc R 1
C C20 0.3795(3) 0.0519(2) 0.5673(3) 0.0343(5) Uani d . 1
H H20 0.2842 -0.0229 0.4815 0.041 Uiso calc R 1
C C21 0.4441(2) 0.1878(2) 0.5722(3) 0.0287(4) Uani d . 1
H H21 0.3931 0.2051 0.4894 0.034 Uiso calc R 1
P P 0.66511(5) 0.47356(5) 0.70156(5) 0.01677(9) Uani d . 1
Cl Cl 0.53757(5) 0.31954(5) 0.35465(5) 0.02334(10) Uani d . 1
Pd Pd 0.5 0.5 0.5 0.01543(6) Uani d S 1
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 0 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C7 C1 C2 . . 119.62(16) ?
C7 C1 P . . 124.01(13) ?
C2 C1 P . . 116.33(13) ?
C3 C2 C1 . . 121.42(16) ?
C3 C2 H2 . . 119.3 ?
C1 C2 H2 . . 119.3 ?
C2 C3 C5 . . 118.01(17) ?
C2 C3 C4 . . 120.80(17) ?
C5 C3 C4 . . 121.18(16) ?
C3 C4 H4A . . 109.5 ?
C3 C4 H4B . . 109.5 ?
H4A C4 H4B . . 109.5 ?
C3 C4 H4C . . 109.5 ?
H4A C4 H4C . . 109.5 ?
H4B C4 H4C . . 109.5 ?
C6 C5 C3 . . 121.02(17) ?
C6 C5 H5 . . 119.5 ?
C3 C5 H5 . . 119.5 ?
C5 C6 C7 . . 120.51(17) ?
C5 C6 H6 . . 119.7 ?
C7 C6 H6 . . 119.7 ?
C1 C7 C6 . . 119.41(17) ?
C1 C7 H7 . . 120.3 ?
C6 C7 H7 . . 120.3 ?
C9 C8 C14 . . 119.07(17) ?
C9 C8 P . . 121.93(13) ?
C14 C8 P . . 118.65(15) ?
C8 C9 C10 . . 121.49(17) ?
C8 C9 H9 . . 119.3 ?
C10 C9 H9 . . 119.3 ?
C12 C10 C9 . . 118.17(19) ?
C12 C10 C11 . . 121.51(19) ?
C9 C10 C11 . . 120.30(19) ?
C10 C11 H11A . . 109.5 ?
C10 C11 H11B . . 109.5 ?
H11A C11 H11B . . 109.5 ?
C10 C11 H11C . . 109.5 ?
H11A C11 H11C . . 109.5 ?
H11B C11 H11C . . 109.5 ?
C13 C12 C10 . . 120.97(19) ?
C13 C12 H12 . . 119.5 ?
C10 C12 H12 . . 119.5 ?
C14 C13 C12 . . 120.40(18) ?
C14 C13 H13 . . 119.8 ?
C12 C13 H13 . . 119.8 ?
C13 C14 C8 . . 119.90(19) ?
C13 C14 H14 . . 120 ?
C8 C14 H14 . . 120 ?
C21 C15 C16 . . 119.33(18) ?
C21 C15 P . . 119.20(15) ?
C16 C15 P . . 121.47(16) ?
C15 C16 C17 . . 120.2(2) ?
C15 C16 H16 . . 119.9 ?
C17 C16 H16 . . 119.9 ?
C19 C17 C16 . . 118.8(2) ?
C19 C17 C18 . . 120.28(19) ?
C16 C17 C18 . . 120.9(2) ?
C17 C18 H18A . . 109.5 ?
C17 C18 H18B . . 109.5 ?
H18A C18 H18B . . 109.5 ?
C17 C18 H18C . . 109.5 ?
H18A C18 H18C . . 109.5 ?
H18B C18 H18C . . 109.5 ?
C20 C19 C17 . . 121.80(19) ?
C20 C19 H19 . . 119.1 ?
C17 C19 H19 . . 119.1 ?
C19 C20 C21 . . 119.7(2) ?
C19 C20 H20 . . 120.1 ?
C21 C20 H20 . . 120.1 ?
C15 C21 C20 . . 120.1(2) ?
C15 C21 H21 . . 119.9 ?
C20 C21 H21 . . 119.9 ?
C8 P C1 . . 104.74(8) ?
C8 P C15 . . 104.42(9) ?
C1 P C15 . . 108.57(8) ?
C8 P Pd . . 114.66(6) y
C1 P Pd . . 109.91(6) y
C15 P Pd . . 113.96(7) y
Cl Pd Cl 2_666 . 180 ?
Cl Pd P 2_666 2_666 87.772(16) ?
Cl Pd P . 2_666 92.228(16) ?
Cl Pd P 2_666 . 92.228(16) ?
Cl Pd P . . 87.772(16) y
P Pd P 2_666 . 180 y
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C7 . 1.389(2) ?
C1 C2 . 1.399(2) ?
C1 P . 1.8189(17) y
C2 C3 . 1.394(2) ?
C2 H2 . 0.95 ?
C3 C5 . 1.398(3) ?
C3 C4 . 1.503(3) ?
C4 H4A . 0.98 ?
C4 H4B . 0.98 ?
C4 H4C . 0.98 ?
C5 C6 . 1.383(3) ?
C5 H5 . 0.95 ?
C6 C7 . 1.396(3) ?
C6 H6 . 0.95 ?
C7 H7 . 0.95 ?
C8 C9 . 1.392(3) ?
C8 C14 . 1.401(2) ?
C8 P . 1.8188(19) y
C9 C10 . 1.399(3) ?
C9 H9 . 0.95 ?
C10 C12 . 1.392(3) ?
C10 C11 . 1.510(3) ?
C11 H11A . 0.98 ?
C11 H11B . 0.98 ?
C11 H11C . 0.98 ?
C12 C13 . 1.388(3) ?
C12 H12 . 0.95 ?
C13 C14 . 1.383(3) ?
C13 H13 . 0.95 ?
C14 H14 . 0.95 ?
C15 C21 . 1.394(3) ?
C15 C16 . 1.395(3) ?
C15 P . 1.8215(18) y
C16 C17 . 1.412(3) ?
C16 H16 . 0.95 ?
C17 C19 . 1.379(3) ?
C17 C18 . 1.498(3) ?
C18 H18A . 0.98 ?
C18 H18B . 0.98 ?
C18 H18C . 0.98 ?
C19 C20 . 1.366(3) ?
C19 H19 . 0.95 ?
C20 C21 . 1.400(3) ?
C20 H20 . 0.95 ?
C21 H21 . 0.95 ?
P Pd . 2.3289(4) y
Cl Pd . 2.2897(4) y
Pd Cl 2_666 2.2897(4) ?
Pd P 2_666 2.3289(4) ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C19 H19 Cl 2_656 0.95 2.76 3.531(2) 139.3
C21 H21 Cl . 0.95 2.82 3.467(2) 125.8
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_site_symmetry_4
_geom_torsion
C7 C1 C2 C3 . -0.6(3)
P C1 C2 C3 . 177.28(14)
C1 C2 C3 C5 . 1.0(3)
C1 C2 C3 C4 . -178.33(17)
C2 C3 C5 C6 . -0.6(3)
C4 C3 C5 C6 . 178.70(19)
C3 C5 C6 C7 . -0.1(3)
C2 C1 C7 C6 . -0.1(3)
P C1 C7 C6 . -177.85(15)
C5 C6 C7 C1 . 0.5(3)
C14 C8 C9 C10 . -0.3(3)
P C8 C9 C10 . 172.86(14)
C8 C9 C10 C12 . 0.4(3)
C8 C9 C10 C11 . -178.33(19)
C9 C10 C12 C13 . -0.2(3)
C11 C10 C12 C13 . 178.5(2)
C10 C12 C13 C14 . -0.1(3)
C12 C13 C14 C8 . 0.3(3)
C9 C8 C14 C13 . -0.1(3)
P C8 C14 C13 . -173.43(15)
C21 C15 C16 C17 . 1.5(3)
P C15 C16 C17 . -178.99(14)
C15 C16 C17 C19 . -1.1(3)
C15 C16 C17 C18 . -179.27(18)
C16 C17 C19 C20 . -0.2(3)
C18 C17 C19 C20 . 178.0(2)
C17 C19 C20 C21 . 1.0(3)
C16 C15 C21 C20 . -0.7(3)
P C15 C21 C20 . 179.78(16)
C19 C20 C21 C15 . -0.5(3)
C9 C8 P C1 . 21.84(17)
C14 C8 P C1 . -165.00(14)
C9 C8 P C15 . 135.89(15)
C14 C8 P C15 . -50.95(16)
C9 C8 P Pd . -98.70(15)
C14 C8 P Pd . 74.46(15)
C7 C1 P C8 . 89.03(17)
C2 C1 P C8 . -88.75(15)
C7 C1 P C15 . -22.07(19)
C2 C1 P C15 . 160.15(14)
C7 C1 P Pd . -147.33(15)
C2 C1 P Pd . 34.89(15)
C21 C15 P C8 . 134.50(15)
C16 C15 P C8 . -44.97(17)
C21 C15 P C1 . -114.19(16)
C16 C15 P C1 . 66.34(17)
C21 C15 P Pd . 8.65(17)
C16 C15 P Pd . -170.82(13)
C8 P Pd Cl 2_666 -7.92(7)
C1 P Pd Cl 2_666 -125.56(6)
C15 P Pd Cl 2_666 112.34(6)
C8 P Pd Cl . 172.08(7)
C1 P Pd Cl . 54.44(6)
C15 P Pd Cl . -67.66(6)
