#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/86/2208617.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_2208617
loop_
_publ_author_name
'Meijboom, Reinout'
'Muller, Alfred'
'Roodt, Andreas'
_publ_section_title
;
 Di-μ₂-chloro-bis[(benzyldiphenylphosphine)chloropalladium(II)]
;
_journal_coeditor_code           HG2025
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m897
_journal_page_last               m899
_journal_paper_doi               10.1107/S1600536806010580
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '[Pd Cl2 (C19 H17 P)]2'
_chemical_formula_moiety         'C38 H34 Cl4 P2 Pd2'
_chemical_formula_sum            'C38 H34 Cl4 P2 Pd2'
_chemical_formula_weight         907.19
_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                99.347(2)
_cell_angle_beta                 96.505(2)
_cell_angle_gamma                113.1430(10)
_cell_formula_units_Z            1
_cell_length_a                   9.2060(2)
_cell_length_b                   10.2804(2)
_cell_length_c                   10.8020(4)
_cell_measurement_reflns_used    6089
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.45
_cell_volume                     909.72(4)
_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_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
;
Bruker X8 APEXII
;
_diffrn_measurement_method       'ω and φ'
_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  0.032
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_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            15329
_diffrn_reflns_theta_full        28.33
_diffrn_reflns_theta_max         28.33
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.397
_exptl_absorpt_correction_T_max  0.9334
_exptl_absorpt_correction_T_min  0.8178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 1998)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.45
_refine_diff_density_min         -0.552
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.06
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         4530
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.06
_refine_ls_R_factor_gt           0.0254
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0292P)²+0.2322P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.064
_reflns_number_gt                3853
_reflns_number_total             4530
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hg2025.cif
_cod_data_source_block           I
_cod_database_code               2208617
_cod_database_fobs_code          2208617
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
Pd Pd 0.84148(2) 0.328676(17) 0.951948(14) 0.01312(6) Uani d . 1
P P 0.71935(7) 0.15169(6) 0.77710(5) 0.01475(12) Uani d . 1
Cl Cl1 1.01892(7) 0.48850(5) 0.85316(5) 0.01782(11) Uani d . 1
Cl Cl2 0.67930(7) 0.17734(6) 1.05986(5) 0.02234(13) Uani d . 1
C C1 0.4991(3) 0.0784(2) 0.7454(2) 0.0193(5) Uani d . 1
H H1A 0.4566 0.0049 0.6634 0.023 Uiso calc R 1
H H1B 0.4591 0.0282 0.8136 0.023 Uiso calc R 1
C C11 0.4325(3) 0.1899(2) 0.7384(2) 0.0202(5) Uani d . 1
C C12 0.3877(3) 0.2176(3) 0.6210(2) 0.0250(5) Uani d . 1
H H12 0.3999 0.1657 0.5446 0.03 Uiso calc R 1
C C13 0.3259(3) 0.3192(3) 0.6144(2) 0.0320(6) Uani d . 1
H H13 0.2965 0.3372 0.5339 0.038 Uiso calc R 1
C C14 0.3066(4) 0.3948(3) 0.7241(3) 0.0368(7) Uani d . 1
H H14 0.264 0.4648 0.7194 0.044 Uiso calc R 1
C C15 0.3495(3) 0.3682(3) 0.8411(2) 0.0335(6) Uani d . 1
H H15 0.3356 0.4196 0.9168 0.04 Uiso calc R 1
C C16 0.4127(3) 0.2670(3) 0.8486(2) 0.0259(5) Uani d . 1
H H16 0.4426 0.2501 0.9295 0.031 Uiso calc R 1
C C21 0.7808(3) 0.2041(2) 0.63209(19) 0.0178(5) Uani d . 1
C C22 0.7589(3) 0.3207(3) 0.5962(2) 0.0256(5) Uani d . 1
H H22 0.7153 0.3736 0.6487 0.031 Uiso calc R 1
C C23 0.8009(3) 0.3591(3) 0.4836(2) 0.0318(6) Uani d . 1
H H23 0.7845 0.4375 0.4585 0.038 Uiso calc R 1
C C24 0.8669(3) 0.2830(3) 0.4074(2) 0.0330(6) Uani d . 1
H H24 0.8948 0.3089 0.33 0.04 Uiso calc R 1
C C25 0.8915(3) 0.1707(3) 0.4440(2) 0.0315(6) Uani d . 1
H H25 0.9381 0.1199 0.3925 0.038 Uiso calc R 1
C C26 0.8488(3) 0.1303(3) 0.5561(2) 0.0236(5) Uani d . 1
H H26 0.8662 0.0521 0.5806 0.028 Uiso calc R 1
C C31 0.7707(3) 0.0017(2) 0.79246(19) 0.0190(5) Uani d . 1
C C32 0.9330(3) 0.0320(3) 0.8290(2) 0.0259(5) Uani d . 1
H H32 1.0123 0.1291 0.844 0.031 Uiso calc R 1
C C33 0.9791(4) -0.0782(3) 0.8437(2) 0.0342(7) Uani d . 1
H H33 1.0899 -0.057 0.868 0.041 Uiso calc R 1
C C34 0.8643(4) -0.2185(3) 0.8229(2) 0.0407(8) Uani d . 1
H H34 0.8962 -0.2941 0.8335 0.049 Uiso calc R 1
C C35 0.7035(4) -0.2503(3) 0.7869(3) 0.0415(8) Uani d . 1
H H35 0.6253 -0.3477 0.7727 0.05 Uiso calc R 1
C C36 0.6549(3) -0.1409(3) 0.7710(2) 0.0299(6) Uani d . 1
H H36 0.5439 -0.1631 0.7459 0.036 Uiso calc R 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_3
_geom_angle
_geom_angle_publ_flag
P Pd Cl2 . 87.18(2) y
P Pd Cl1 . 95.735(19) y
Cl2 Pd Cl1 . 176.50(2) y
P Pd Cl1 2_767 176.47(2) y
Cl2 Pd Cl1 2_767 91.437(19) y
Cl1 Pd Cl1 2_767 85.544(18) y
C31 P C21 . 106.16(10) ?
C31 P C1 . 106.71(11) ?
C21 P C1 . 106.02(10) ?
C31 P Pd . 109.12(7) ?
C21 P Pd . 113.50(7) ?
C1 P Pd . 114.78(7) ?
Pd Cl1 Pd 2_767 94.457(18) y
C11 C1 P . 114.65(15) ?
C11 C1 H1A . 108.6 ?
P C1 H1A . 108.6 ?
C11 C1 H1B . 108.6 ?
P C1 H1B . 108.6 ?
H1A C1 H1B . 107.6 ?
C16 C11 C12 . 118.3(2) ?
C16 C11 C1 . 120.8(2) ?
C12 C11 C1 . 120.8(2) ?
C13 C12 C11 . 120.9(2) ?
C13 C12 H12 . 119.6 ?
C11 C12 H12 . 119.6 ?
C14 C13 C12 . 120.3(2) ?
C14 C13 H13 . 119.8 ?
C12 C13 H13 . 119.8 ?
C13 C14 C15 . 119.6(2) ?
C13 C14 H14 . 120.2 ?
C15 C14 H14 . 120.2 ?
C14 C15 C16 . 120.5(2) ?
C14 C15 H15 . 119.8 ?
C16 C15 H15 . 119.8 ?
C15 C16 C11 . 120.4(2) ?
C15 C16 H16 . 119.8 ?
C11 C16 H16 . 119.8 ?
C26 C21 C22 . 119.3(2) ?
C26 C21 P . 121.30(17) ?
C22 C21 P . 119.36(17) ?
C23 C22 C21 . 119.9(2) ?
C23 C22 H22 . 120 ?
C21 C22 H22 . 120 ?
C22 C23 C24 . 120.1(2) ?
C22 C23 H23 . 119.9 ?
C24 C23 H23 . 119.9 ?
C25 C24 C23 . 119.9(2) ?
C25 C24 H24 . 120 ?
C23 C24 H24 . 120 ?
C24 C25 C26 . 120.6(2) ?
C24 C25 H25 . 119.7 ?
C26 C25 H25 . 119.7 ?
C21 C26 C25 . 120.1(2) ?
C21 C26 H26 . 120 ?
C25 C26 H26 . 120 ?
C32 C31 C36 . 119.5(2) ?
C32 C31 P . 117.91(18) ?
C36 C31 P . 122.58(19) ?
C33 C32 C31 . 120.4(3) ?
C33 C32 H32 . 119.8 ?
C31 C32 H32 . 119.8 ?
C34 C33 C32 . 119.9(3) ?
C34 C33 H33 . 120.1 ?
C32 C33 H33 . 120.1 ?
C33 C34 C35 . 120.5(3) ?
C33 C34 H34 . 119.8 ?
C35 C34 H34 . 119.8 ?
C34 C35 C36 . 120.5(3) ?
C34 C35 H35 . 119.8 ?
C36 C35 H35 . 119.8 ?
C35 C36 C31 . 119.3(3) ?
C35 C36 H36 . 120.4 ?
C31 C36 H36 . 120.4 ?
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
Pd P . 2.2218(6) y
Pd Cl2 . 2.2729(5) y
Pd Cl1 . 2.3155(5) y
Pd Cl1 2_767 2.4123(5) y
P C31 . 1.808(2) ?
P C21 . 1.816(2) ?
P C1 . 1.832(2) ?
Cl1 Pd 2_767 2.4123(5) ?
C1 C11 . 1.505(3) ?
C1 H1A . 0.99 ?
C1 H1B . 0.99 ?
C11 C16 . 1.391(3) ?
C11 C12 . 1.397(3) ?
C12 C13 . 1.379(4) ?
C12 H12 . 0.95 ?
C13 C14 . 1.377(4) ?
C13 H13 . 0.95 ?
C14 C15 . 1.383(4) ?
C14 H14 . 0.95 ?
C15 C16 . 1.385(3) ?
C15 H15 . 0.95 ?
C16 H16 . 0.95 ?
C21 C26 . 1.389(3) ?
C21 C22 . 1.397(3) ?
C22 C23 . 1.388(3) ?
C22 H22 . 0.95 ?
C23 C24 . 1.392(4) ?
C23 H23 . 0.95 ?
C24 C25 . 1.369(4) ?
C24 H24 . 0.95 ?
C25 C26 . 1.391(3) ?
C25 H25 . 0.95 ?
C26 H26 . 0.95 ?
C31 C32 . 1.394(3) ?
C31 C36 . 1.395(3) ?
C32 C33 . 1.382(3) ?
C32 H32 . 0.95 ?
C33 C34 . 1.375(4) ?
C33 H33 . 0.95 ?
C34 C35 . 1.378(5) ?
C34 H34 . 0.95 ?
C35 C36 . 1.392(4) ?
C35 H35 . 0.95 ?
C36 H36 . 0.95 ?
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
C1 H1B Cl2 2_657 0.99 2.68 3.636(2) 162.8
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_1
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cl2 Pd P C31 . . -67.18(8) ?
Cl1 Pd P C31 . . 110.86(8) ?
Cl2 Pd P C21 . . 174.66(9) y
Cl1 Pd P C21 . . -7.30(9) y
Cl2 Pd P C1 . . 52.50(8) y
Cl1 Pd P C1 . . -129.45(8) y
P Pd Cl1 Pd . 2_767 -176.69(2) y
Cl1 Pd Cl1 Pd 2_767 2_767 0 ?
C31 P C1 C11 . . 176.03(15) ?
C21 P C1 C11 . . -71.10(17) ?
Pd P C1 C11 . . 55.02(17) ?
P C1 C11 C16 . . -85.8(2) ?
P C1 C11 C12 . . 94.9(2) ?
C16 C11 C12 C13 . . 0.3(4) ?
C1 C11 C12 C13 . . 179.6(2) ?
C11 C12 C13 C14 . . -0.4(4) ?
C12 C13 C14 C15 . . 0.0(5) ?
C13 C14 C15 C16 . . 0.5(5) ?
C14 C15 C16 C11 . . -0.5(4) ?
C12 C11 C16 C15 . . 0.2(4) ?
C1 C11 C16 C15 . . -179.2(2) ?
C31 P C21 C26 . . 1.4(2) ?
C1 P C21 C26 . . -111.85(19) ?
Pd P C21 C26 . . 121.25(17) ?
C31 P C21 C22 . . -178.75(18) ?
C1 P C21 C22 . . 68.0(2) ?
Pd P C21 C22 . . -58.9(2) ?
C26 C21 C22 C23 . . 1.8(3) ?
P C21 C22 C23 . . -178.09(19) ?
C21 C22 C23 C24 . . -0.9(4) ?
C22 C23 C24 C25 . . -0.5(4) ?
C23 C24 C25 C26 . . 1.0(4) ?
C22 C21 C26 C25 . . -1.3(3) ?
P C21 C26 C25 . . 178.59(19) ?
C24 C25 C26 C21 . . -0.1(4) ?
C21 P C31 C32 . . 73.15(18) ?
C1 P C31 C32 . . -174.07(16) ?
Pd P C31 C32 . . -49.52(18) ?
C21 P C31 C36 . . -107.78(19) ?
C1 P C31 C36 . . 5.0(2) ?
Pd P C31 C36 . . 129.54(17) ?
C36 C31 C32 C33 . . 0.2(3) ?
P C31 C32 C33 . . 179.28(17) ?
C31 C32 C33 C34 . . -0.4(3) ?
C32 C33 C34 C35 . . 0.4(4) ?
C33 C34 C35 C36 . . -0.1(4) ?
C34 C35 C36 C31 . . -0.2(4) ?
C32 C31 C36 C35 . . 0.1(3) ?
P C31 C36 C35 . . -178.92(19) ?
