#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/70/2237045.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_2237045
loop_
_publ_author_name
'Davis, Wade L.'
'Muller, Alfred'
_publ_section_title
;
 trans-Di-μ-chlorido-bis{chlorido[tris(3,5-dimethylphenyl)phosphane-κP]palladium(II)}
 dichloromethane monosolvate
;
_journal_coeditor_code           SU2534
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1563
_journal_page_last               m1564
_journal_paper_doi               10.1107/S1600536812048556
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd2 Cl4 (C24 H27 P1)2], C H2 Cl2'
_chemical_formula_moiety         'C48 H54 Cl4 P2 Pd2, C H2 Cl2'
_chemical_formula_sum            'C49 H56 Cl6 P2 Pd2'
_chemical_formula_weight         1132.38
_chemical_name_systematic
;
trans-Di-μ-chlorido-bis{chlorido[tris(3,5-dimethylphenyl)phosphane-
κP]palladium(II)} dichloromethane monosolvate
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 117.576(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.747(2)
_cell_length_b                   9.1038(13)
_cell_length_c                   21.376(3)
_cell_measurement_reflns_used    4452
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.24
_cell_volume                     2543.8(6)
_computing_cell_refinement       'SAINT (Bruker, 2008)'
_computing_data_collection       'APEX2 (Bruker, 2011)'
_computing_data_reduction        'SAINT and XPREP (Bruker, 2008)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material
'publCIF (Westrip, 2010) and WinGX (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.4
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX DUO 4K-CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30952
_diffrn_reflns_theta_full        28.36
_diffrn_reflns_theta_max         28.36
_diffrn_reflns_theta_min         1.56
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.8684
_exptl_absorpt_correction_T_min  0.8158
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2008)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             1148
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.901
_refine_diff_density_min         -1.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     273
_refine_ls_number_reflns         6349
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0402
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0419P)²+1.7351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0981
_reflns_number_gt                4776
_reflns_number_total             6349
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            su2534.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               2237045
_cod_database_fobs_code          2237045
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
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 Pd1 0.627522(18) 0.56103(3) 0.537254(13) 0.01368(8) Uani d . 1
Cl Cl1 0.49039(6) 0.53788(9) 0.42440(4) 0.01841(17) Uani d . 1
Cl Cl2 0.74975(6) 0.60182(10) 0.65077(4) 0.02141(19) Uani d . 1
P P1 0.72374(6) 0.67044(10) 0.49592(4) 0.01491(18) Uani d . 1
C C1 0.8616(2) 0.6459(4) 0.53793(17) 0.0175(7) Uani d . 1
C C2 0.9098(3) 0.5328(4) 0.58601(18) 0.0214(7) Uani d . 1
H H2 0.8715 0.472 0.6012 0.026 Uiso calc R 1
C C3 1.0148(3) 0.5092(4) 0.6118(2) 0.0258(8) Uani d . 1
C C4 1.0691(3) 0.3890(5) 0.6654(2) 0.0391(11) Uani d . 1
H H4A 1.0903 0.311 0.6434 0.059 Uiso calc R 1
H H4B 1.0226 0.3482 0.682 0.059 Uiso calc R 1
H H4C 1.1295 0.43 0.7055 0.059 Uiso calc R 1
C C5 1.0682(3) 0.6006(4) 0.5881(2) 0.0268(9) Uani d . 1
H H5 1.1393 0.5843 0.6051 0.032 Uiso calc R 1
C C6 1.0219(3) 0.7144(4) 0.54062(19) 0.0245(8) Uani d . 1
C C7 1.0833(3) 0.8123(5) 0.5172(2) 0.0371(10) Uani d . 1
H H7A 1.1272 0.7517 0.5045 0.056 Uiso calc R 1
H H7B 1.1258 0.8788 0.5558 0.056 Uiso calc R 1
H H7C 1.0367 0.87 0.4761 0.056 Uiso calc R 1
C C8 0.9174(2) 0.7360(4) 0.51530(18) 0.0202(7) Uani d . 1
H H8 0.8837 0.8125 0.4824 0.024 Uiso calc R 1
C C9 0.6976(2) 0.8629(4) 0.49952(18) 0.0174(7) Uani d . 1
C C10 0.7633(2) 0.9478(4) 0.55679(18) 0.0187(7) Uani d . 1
H H10 0.8275 0.909 0.5899 0.022 Uiso calc R 1
C C11 0.7352(3) 1.0906(4) 0.56585(19) 0.0224(8) Uani d . 1
C C12 0.8050(3) 1.1774(4) 0.6300(2) 0.0315(9) Uani d . 1
H H12A 0.8125 1.1266 0.6725 0.047 Uiso calc R 1
H H12B 0.7758 1.2752 0.6277 0.047 Uiso calc R 1
H H12C 0.8722 1.1871 0.6315 0.047 Uiso calc R 1
C C13 0.6423(3) 1.1449(4) 0.5154(2) 0.0234(8) Uani d . 1
H H13 0.6236 1.2422 0.5207 0.028 Uiso calc R 1
C C14 0.5749(3) 1.0627(4) 0.45713(19) 0.0228(8) Uani d . 1
C C15 0.4734(3) 1.1257(4) 0.4041(2) 0.0280(8) Uani d . 1
H H15A 0.4296 1.1409 0.4267 0.042 Uiso calc R 1
H H15B 0.4401 1.0573 0.3645 0.042 Uiso calc R 1
H H15C 0.4848 1.2198 0.3866 0.042 Uiso calc R 1
C C16 0.6032(3) 0.9208(4) 0.45022(19) 0.0199(7) Uani d . 1
H H16 0.5582 0.862 0.4116 0.024 Uiso calc R 1
C C17 0.6861(2) 0.6207(4) 0.40528(17) 0.0196(7) Uani d . 1
C C18 0.6758(3) 0.7236(4) 0.35443(18) 0.0244(8) Uani d . 1
H H18 0.6843 0.8251 0.3661 0.029 Uiso calc R 1
C C19 0.6527(3) 0.6785(5) 0.28588(19) 0.0305(9) Uani d . 1
C C20 0.6411(4) 0.7934(6) 0.2318(2) 0.0491(13) Uani d . 1
H H20A 0.5764 0.8459 0.217 0.074 Uiso calc R 1
H H20B 0.6413 0.7457 0.1907 0.074 Uiso calc R 1
H H20C 0.6981 0.863 0.2525 0.074 Uiso calc R 1
C C21 0.6429(3) 0.5291(5) 0.2705(2) 0.0338(10) Uani d . 1
H H21 0.6283 0.4982 0.2243 0.041 Uiso calc R 1
C C22 0.6539(3) 0.4227(5) 0.3208(2) 0.0286(9) Uani d . 1
C C23 0.6476(3) 0.2622(5) 0.3036(2) 0.0421(11) Uani d . 1
H H23A 0.6304 0.2069 0.336 0.063 Uiso calc R 1
H H23B 0.7137 0.2285 0.3085 0.063 Uiso calc R 1
H H23C 0.5946 0.2462 0.2549 0.063 Uiso calc R 1
C C24 0.6751(2) 0.4700(4) 0.38800(19) 0.0228(8) Uani d . 1
H H24 0.6822 0.3997 0.4229 0.027 Uiso calc R 1
Cl Cl3 0.94842(13) 0.9023(2) 0.79374(9) 0.0900(6) Uani d . 1
C C25 1 0.7942(9) 0.75 0.075(3) Uani d S 1
H H25A 0.9457 0.7302 0.7153 0.09 Uiso calc PR 0.5
H H25B 1.0543 0.7302 0.7847 0.09 Uiso calc PR 0.5
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'
Cl Cl 0.1484 0.1585 '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'
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
P1 Pd1 Cl2 . . 90.82(3)
P1 Pd1 Cl1 . . 92.10(3)
Cl2 Pd1 Cl1 . . 173.20(3)
P1 Pd1 Cl1 . 3_666 173.90(3)
Cl2 Pd1 Cl1 . 3_666 92.18(3)
Cl1 Pd1 Cl1 . 3_666 84.35(3)
Pd1 Cl1 Pd1 . 3_666 95.65(3)
C9 P1 C17 . . 108.87(16)
C9 P1 C1 . . 108.11(16)
C17 P1 C1 . . 102.52(15)
C9 P1 Pd1 . . 103.29(11)
C17 P1 Pd1 . . 112.19(12)
C1 P1 Pd1 . . 121.50(12)
C2 C1 C8 . . 120.5(3)
C2 C1 P1 . . 121.8(3)
C8 C1 P1 . . 117.4(3)
C1 C2 C3 . . 119.8(3)
C1 C2 H2 . . 120.1
C3 C2 H2 . . 120.1
C5 C3 C2 . . 118.3(3)
C5 C3 C4 . . 121.1(3)
C2 C3 C4 . . 120.6(3)
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 . . 122.8(3)
C6 C5 H5 . . 118.6
C3 C5 H5 . . 118.6
C5 C6 C8 . . 118.1(3)
C5 C6 C7 . . 121.0(3)
C8 C6 C7 . . 120.9(3)
C6 C7 H7A . . 109.5
C6 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
C6 C7 H7C . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
C6 C8 C1 . . 120.4(3)
C6 C8 H8 . . 119.8
C1 C8 H8 . . 119.8
C10 C9 C16 . . 119.8(3)
C10 C9 P1 . . 120.1(3)
C16 C9 P1 . . 119.4(3)
C9 C10 C11 . . 120.4(3)
C9 C10 H10 . . 119.8
C11 C10 H10 . . 119.8
C13 C11 C10 . . 118.2(3)
C13 C11 C12 . . 122.4(3)
C10 C11 C12 . . 119.5(3)
C11 C12 H12A . . 109.5
C11 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
C11 C12 H12C . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
C11 C13 C14 . . 122.8(3)
C11 C13 H13 . . 118.6
C14 C13 H13 . . 118.6
C16 C14 C13 . . 117.9(3)
C16 C14 C15 . . 121.1(3)
C13 C14 C15 . . 121.0(3)
C14 C15 H15A . . 109.5
C14 C15 H15B . . 109.5
H15A C15 H15B . . 109.5
C14 C15 H15C . . 109.5
H15A C15 H15C . . 109.5
H15B C15 H15C . . 109.5
C14 C16 C9 . . 120.9(3)
C14 C16 H16 . . 119.5
C9 C16 H16 . . 119.5
C18 C17 C24 . . 119.6(3)
C18 C17 P1 . . 122.5(3)
C24 C17 P1 . . 117.7(3)
C17 C18 C19 . . 120.3(4)
C17 C18 H18 . . 119.8
C19 C18 H18 . . 119.8
C21 C19 C18 . . 118.8(4)
C21 C19 C20 . . 122.3(4)
C18 C19 C20 . . 118.9(4)
C19 C20 H20A . . 109.5
C19 C20 H20B . . 109.5
H20A C20 H20B . . 109.5
C19 C20 H20C . . 109.5
H20A C20 H20C . . 109.5
H20B C20 H20C . . 109.5
C19 C21 C22 . . 122.1(4)
C19 C21 H21 . . 118.9
C22 C21 H21 . . 118.9
C24 C22 C21 . . 118.1(4)
C24 C22 C23 . . 121.0(4)
C21 C22 C23 . . 120.8(4)
C22 C23 H23A . . 109.5
C22 C23 H23B . . 109.5
H23A C23 H23B . . 109.5
C22 C23 H23C . . 109.5
H23A C23 H23C . . 109.5
H23B C23 H23C . . 109.5
C22 C24 C17 . . 121.0(4)
C22 C24 H24 . . 119.5
C17 C24 H24 . . 119.5
Cl3 C25 Cl3 . 2_756 111.8(5)
Cl3 C25 H25A . . 109.3
Cl3 C25 H25A 2_756 . 109.3
Cl3 C25 H25B . . 109.3
Cl3 C25 H25B 2_756 . 109.3
H25A C25 H25B . . 107.9
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd1 P1 . 2.2241(9)
Pd1 Cl2 . 2.2859(9)
Pd1 Cl1 . 2.3317(9)
Pd1 Cl1 3_666 2.4138(8)
Cl1 Pd1 3_666 2.4138(8)
P1 C9 . 1.803(4)
P1 C17 . 1.809(3)
P1 C1 . 1.816(3)
C1 C2 . 1.395(5)
C1 C8 . 1.397(5)
C2 C3 . 1.398(5)
C2 H2 . 0.95
C3 C5 . 1.392(5)
C3 C4 . 1.519(5)
C4 H4A . 0.98
C4 H4B . 0.98
C4 H4C . 0.98
C5 C6 . 1.388(5)
C5 H5 . 0.95
C6 C8 . 1.391(5)
C6 C7 . 1.512(5)
C7 H7A . 0.98
C7 H7B . 0.98
C7 H7C . 0.98
C8 H8 . 0.95
C9 C10 . 1.392(5)
C9 C16 . 1.402(5)
C10 C11 . 1.405(5)
C10 H10 . 0.95
C11 C13 . 1.384(5)
C11 C12 . 1.502(5)
C12 H12A . 0.98
C12 H12B . 0.98
C12 H12C . 0.98
C13 C14 . 1.399(5)
C13 H13 . 0.95
C14 C16 . 1.387(5)
C14 C15 . 1.511(5)
C15 H15A . 0.98
C15 H15B . 0.98
C15 H15C . 0.98
C16 H16 . 0.95
C17 C18 . 1.389(5)
C17 C24 . 1.410(5)
C18 C19 . 1.404(5)
C18 H18 . 0.95
C19 C21 . 1.391(6)
C19 C20 . 1.509(6)
C20 H20A . 0.98
C20 H20B . 0.98
C20 H20C . 0.98
C21 C22 . 1.401(6)
C21 H21 . 0.95
C22 C24 . 1.389(5)
C22 C23 . 1.500(6)
C23 H23A . 0.98
C23 H23B . 0.98
C23 H23C . 0.98
C24 H24 . 0.95
Cl3 C25 . 1.755(5)
C25 Cl3 2_756 1.755(5)
C25 H25A . 0.99
C25 H25B . 0.99
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
C25 H25A Cl2 . 0.99 2.82 3.733(4) 154
C21 H21 Cl1 2_655 0.95 2.85 3.693(4) 148
C5 H5 Cg1 3_766 0.95 2.95 3.847(5) 159
C15 H15A Cg2 3_676 0.99 2.79 3.620(5) 143
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
P1 Pd1 Cl1 Pd1 . 3_666 -175.03(3)
Cl1 Pd1 Cl1 Pd1 3_666 3_666 0
Cl2 Pd1 P1 C9 . . -82.49(12)
Cl1 Pd1 P1 C9 . . 91.38(12)
Cl2 Pd1 P1 C17 . . 160.43(13)
Cl1 Pd1 P1 C17 . . -25.71(13)
Cl2 Pd1 P1 C1 . . 38.80(13)
Cl1 Pd1 P1 C1 . . -147.34(13)
C9 P1 C1 C2 . . 134.7(3)
C17 P1 C1 C2 . . -110.4(3)
Pd1 P1 C1 C2 . . 15.8(3)
C9 P1 C1 C8 . . -51.4(3)
C17 P1 C1 C8 . . 63.6(3)
Pd1 P1 C1 C8 . . -170.3(2)
C8 C1 C2 C3 . . 0.0(5)
P1 C1 C2 C3 . . 173.7(3)
C1 C2 C3 C5 . . -0.1(5)
C1 C2 C3 C4 . . 178.6(4)
C2 C3 C5 C6 . . 0.6(6)
C4 C3 C5 C6 . . -178.1(4)
C3 C5 C6 C8 . . -0.8(6)
C3 C5 C6 C7 . . 179.0(4)
C5 C6 C8 C1 . . 0.6(5)
C7 C6 C8 C1 . . -179.2(3)
C2 C1 C8 C6 . . -0.2(5)
P1 C1 C8 C6 . . -174.2(3)
C17 P1 C9 C10 . . -144.0(3)
C1 P1 C9 C10 . . -33.4(3)
Pd1 P1 C9 C10 . . 96.6(3)
C17 P1 C9 C16 . . 45.8(3)
C1 P1 C9 C16 . . 156.4(3)
Pd1 P1 C9 C16 . . -73.6(3)
C16 C9 C10 C11 . . 0.6(5)
P1 C9 C10 C11 . . -169.5(3)
C9 C10 C11 C13 . . -1.7(5)
C9 C10 C11 C12 . . 177.0(3)
C10 C11 C13 C14 . . 1.4(5)
C12 C11 C13 C14 . . -177.2(3)
C11 C13 C14 C16 . . 0.0(5)
C11 C13 C14 C15 . . 179.0(3)
C13 C14 C16 C9 . . -1.2(5)
C15 C14 C16 C9 . . 179.8(3)
C10 C9 C16 C14 . . 0.9(5)
P1 C9 C16 C14 . . 171.1(3)
C9 P1 C17 C18 . . 21.2(3)
C1 P1 C17 C18 . . -93.2(3)
Pd1 P1 C17 C18 . . 134.9(3)
C9 P1 C17 C24 . . -163.9(3)
C1 P1 C17 C24 . . 81.8(3)
Pd1 P1 C17 C24 . . -50.2(3)
C24 C17 C18 C19 . . 1.1(5)
P1 C17 C18 C19 . . 176.0(3)
C17 C18 C19 C21 . . -1.6(5)
C17 C18 C19 C20 . . 179.5(3)
C18 C19 C21 C22 . . 1.0(5)
C20 C19 C21 C22 . . 179.9(4)
C19 C21 C22 C24 . . 0.1(5)
C19 C21 C22 C23 . . -177.2(3)
C21 C22 C24 C17 . . -0.5(5)
C23 C22 C24 C17 . . 176.7(3)
C18 C17 C24 C22 . . -0.1(5)
P1 C17 C24 C22 . . -175.2(3)
