#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/46/2234637.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_2234637
loop_
_publ_author_name
'Burgoyne, Andrew R.'
'Meijboom, Reinout'
'Chiririwa, Haleden'
'Kirsten, Leo'
_publ_section_title
;
 trans-Dichloridobis[diphenyl(thiophen-2-yl)phosphane-κP]palladium(II)
;
_journal_coeditor_code           HB6729
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m588
_journal_paper_doi               10.1107/S160053681201478X
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd Cl2 (C16 H13 P1 S1)2]'
_chemical_formula_moiety         'C32 H26 Cl2 P2 Pd S2'
_chemical_formula_sum            'C32 H26 Cl2 P2 Pd S2'
_chemical_formula_weight         713.91
_chemical_name_systematic
;
trans-Dichloridobis[diphenyl(thiophen-2-yl)phosphane-
κP]palladium(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000
_cell_angle_beta                 110.14(4)
_cell_angle_gamma                90.000
_cell_formula_units_Z            2
_cell_length_a                   9.019(2)
_cell_length_b                   18.427(4)
_cell_length_c                   9.658(2)
_cell_measurement_reflns_used    9973
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.51
_cell_volume                     1506.9(7)
_computing_cell_refinement       'SAINT-Plus (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT-Plus and XPREP (Bruker, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2005)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker X8 APEXII 4K KappaCCD'
_diffrn_measurement_method       'φ and ω 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  0.0194
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            20792
_diffrn_reflns_theta_full        28.38
_diffrn_reflns_theta_max         28.38
_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    1.060
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.812
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             720.0
_exptl_crystal_size_max          0.197
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.163
_refine_diff_density_max         1.539
_refine_diff_density_min         -1.488
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         3747
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0507
_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)+(0.0193P)²+7.7351P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                3591
_reflns_number_total             3747
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            hb6729.cif
_cod_data_source_block           I
_cod_original_cell_volume        1507.0(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2234637
_cod_database_fobs_code          2234637
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, 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
_atom_site_symmetry_multiplicity
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd1 0.5000 0.5000 0.5000 0.01794(11) Uani d S 1 2 . .
Cl Cl1 0.70661(12) 0.45351(6) 0.69206(10) 0.0280(2) Uani d . 1 1 . .
P P1 0.52138(11) 0.39844(5) 0.36286(10) 0.01804(18) Uani d . 1 1 . .
C C5 0.4185(5) 0.4000(2) 0.1640(4) 0.0225(7) Uani d . 1 1 A .
C C11 0.7266(4) 0.3790(2) 0.3872(4) 0.0205(7) Uani d . 1 1 A .
C C10 0.5040(6) 0.4028(2) 0.0598(5) 0.0310(9) Uani d . 1 1 . .
H H10 0.6137 0.4036 0.0907 0.037 Uiso calc R 1 1 A .
C C16 0.7978(5) 0.3108(2) 0.4353(4) 0.0231(7) Uani d . 1 1 . .
H H16 0.7386 0.2724 0.4507 0.028 Uiso calc R 1 1 A .
C C12 0.8193(6) 0.4352(2) 0.3639(5) 0.0325(9) Uani d . 1 1 . .
H H12 0.7745 0.4806 0.3342 0.039 Uiso calc R 1 1 A .
C C13 0.9756(5) 0.4240(3) 0.3845(5) 0.0362(10) Uani d . 1 1 A .
H H13 1.0357 0.4612 0.3655 0.043 Uiso calc R 1 1 . .
C C6 0.2505(5) 0.3988(2) 0.1073(5) 0.0309(9) Uani d . 1 1 . .
H H6 0.1941 0.3982 0.1717 0.037 Uiso calc R 1 1 A .
C C7 0.1722(7) 0.3984(3) -0.0409(5) 0.0442(12) Uani d . 1 1 A .
H H7 0.0624 0.3964 -0.0772 0.053 Uiso calc R 1 1 . .
C C8 0.2528(7) 0.4010(3) -0.1360(5) 0.0472(14) Uani d . 1 1 . .
H H8 0.1975 0.4004 -0.2369 0.057 Uiso calc R 1 1 A .
C C9 0.4108(7) 0.4042(3) -0.0871(5) 0.0412(12) Uani d . 1 1 A .
H H9 0.4608 0.4076 -0.1566 0.049 Uiso calc R 1 1 . .
C C15 0.9557(5) 0.3024(3) 0.4588(5) 0.0340(10) Uani d . 1 1 A .
H H15 1.0043 0.2581 0.4929 0.041 Uiso calc R 1 1 . .
C C14 1.0427(5) 0.3582(3) 0.4327(5) 0.0347(10) Uani d . 1 1 . .
H H14 1.1493 0.3512 0.4482 0.042 Uiso calc R 1 1 A .
C C1A 0.4428(9) 0.3176(4) 0.4104(7) 0.01804(18) Uani d PDU 0.570(6) 1 A 1
C C2A 0.4540(9) 0.3048(5) 0.5578(9) 0.01804(18) Uani d PDU 0.570(6) 1 A 1
H H2A 0.4988 0.3356 0.6377 0.022 Uiso calc PR 0.570(6) 1 A 1
C C3A 0.3748(8) 0.2270(4) 0.5617(8) 0.0180(6) Uani d PDU 0.570(6) 1 A 1
H H3A 0.3626 0.2043 0.6432 0.022 Uiso calc PR 0.570(6) 1 A 1
C C4A 0.3287(19) 0.2006(7) 0.4190(13) 0.041(3) Uani d PDU 0.570(6) 1 A 1
H H4A 0.2832 0.1550 0.3943 0.049 Uiso calc PR 0.570(6) 1 A 1
S S1A 0.3563(4) 0.24996(17) 0.3057(3) 0.0386(7) Uani d PDU 0.570(6) 1 A 1
C C1B 0.4544(10) 0.3199(4) 0.4465(6) 0.0178(7) Uani d PGDU 0.430(6) 1 A 2
C C2B 0.3665(17) 0.2577(7) 0.3461(10) 0.071(6) Uani d PGDU 0.430(6) 1 A 2
H H2B 0.3453 0.2543 0.2451 0.085 Uiso calc PR 0.430(6) 1 A 2
C C3B 0.3197(19) 0.2020(6) 0.4418(12) 0.030(3) Uani d PGDU 0.430(6) 1 A 2
H H3B 0.2652 0.1589 0.4089 0.036 Uiso calc PR 0.430(6) 1 A 2
C C4B 0.3787(12) 0.2298(4) 0.6013(8) 0.043(2) Uani d PGDU 0.430(6) 1 A 2
H H4B 0.3662 0.2065 0.6820 0.052 Uiso calc PR 0.430(6) 1 A 2
S S1B 0.4619(3) 0.30264(15) 0.6042(3) 0.0244(7) Uani d PGD 0.430(6) 1 A 2
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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
Cl1 Pd1 Cl1 . 3_666 180.0000(10)
Cl1 Pd1 P1 . . 87.52(4)
Cl1 Pd1 P1 3_666 . 92.48(4)
Cl1 Pd1 P1 . 3_666 92.48(4)
Cl1 Pd1 P1 3_666 3_666 87.52(4)
P1 Pd1 P1 . 3_666 180.0
C1A P1 C11 . . 106.3(3)
C1A P1 C5 . . 100.5(2)
C11 P1 C5 . . 105.39(18)
C11 P1 C1B . . 105.0(3)
C5 P1 C1B . . 110.3(2)
C1A P1 Pd1 . . 114.0(2)
C11 P1 Pd1 . . 111.29(12)
C5 P1 Pd1 . . 118.21(13)
C1B P1 Pd1 . . 105.9(2)
C6 C5 C10 . . 118.6(4)
C6 C5 P1 . . 119.6(3)
C10 C5 P1 . . 121.8(3)
C12 C11 C16 . . 118.8(4)
C12 C11 P1 . . 118.1(3)
C16 C11 P1 . . 123.0(3)
C9 C10 C5 . . 115.5(4)
C9 C10 H10 . . 122.3
C5 C10 H10 . . 122.3
C15 C16 C11 . . 118.9(4)
C15 C16 H16 . . 120.5
C11 C16 H16 . . 120.5
C13 C12 C11 . . 120.5(4)
C13 C12 H12 . . 119.7
C11 C12 H12 . . 119.7
C14 C13 C12 . . 119.8(4)
C14 C13 H13 . . 120.1
C12 C13 H13 . . 120.1
C7 C6 C5 . . 120.2(4)
C7 C6 H6 . . 119.9
C5 C6 H6 . . 119.9
C8 C7 C6 . . 120.5(5)
C8 C7 H7 . . 119.8
C6 C7 H7 . . 119.8
C9 C8 C7 . . 121.2(5)
C9 C8 H8 . . 119.4
C7 C8 H8 . . 119.4
C8 C9 C10 . . 124.0(5)
C8 C9 H9 . . 118.0
C10 C9 H9 . . 118.0
C14 C15 C16 . . 120.8(4)
C14 C15 H15 . . 119.6
C16 C15 H15 . . 119.6
C13 C14 C15 . . 121.1(4)
C13 C14 H14 . . 119.5
C15 C14 H14 . . 119.5
C2A C1A S1A . . 110.6(6)
C2A C1A P1 . . 120.3(5)
S1A C1A P1 . . 129.1(4)
C1A C2A C3A . . 107.1(6)
C1A C2A H2A . . 126.4
C3A C2A H2A . . 126.4
C4A C3A C2A . . 105.8(7)
C4A C3A H3A . . 127.1
C2A C3A H3A . . 127.1
C3A C4A S1A . . 116.4(7)
C3A C4A H4A . . 121.8
S1A C4A H4A . . 121.8
C4A S1A C1A . . 100.0(5)
S1B C1B C2B . . 108.0
S1B C1B P1 . . 133.1(4)
C2B C1B P1 . . 118.8(4)
C3B C2B C1B . . 108.0
C3B C2B H2B . . 126.0
C1B C2B H2B . . 126.0
C2B C3B C4B . . 108.0
C2B C3B H3B . . 126.0
C4B C3B H3B . . 126.0
S1B C4B C3B . . 108.0
S1B C4B H4B . . 126.0
C3B C4B H4B . . 126.0
C1B S1B C4B . . 108.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd1 Cl1 . 2.2950(12)
Pd1 Cl1 3_666 2.2950(12)
Pd1 P1 . 2.3387(11)
Pd1 P1 3_666 2.3387(11)
P1 C1A . 1.777(7)
P1 C11 . 1.820(4)
P1 C5 . 1.823(4)
P1 C1B . 1.857(6)
C5 C6 . 1.423(6)
C5 C10 . 1.465(6)
C11 C12 . 1.397(6)
C11 C16 . 1.414(5)
C10 C9 . 1.378(6)
C10 H10 . 0.9300
C16 C15 . 1.371(6)
C16 H16 . 0.9300
C12 C13 . 1.369(6)
C12 H12 . 0.9300
C13 C14 . 1.363(7)
C13 H13 . 0.9300
C6 C7 . 1.361(6)
C6 H6 . 0.9300
C7 C8 . 1.354(8)
C7 H7 . 0.9300
C8 C9 . 1.340(8)
C8 H8 . 0.9300
C9 H9 . 0.9300
C15 C14 . 1.370(7)
C15 H15 . 0.9300
C14 H14 . 0.9300
C1A C2A . 1.412(9)
C1A S1A . 1.625(7)
C2A C3A . 1.608(10)
C2A H2A . 0.9300
C3A C4A . 1.384(12)
C3A H3A . 0.9300
C4A S1A . 1.507(12)
C4A H4A . 0.9300
C1B S1B . 1.534(5)
C1B C2B . 1.534(5)
C2B C3B . 1.534(5)
C2B H2B . 0.9300
C3B C4B . 1.534(5)
C3B H3B . 0.9300
C4B S1B . 1.534(5)
C4B H4B . 0.9300
