#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/00/2230058.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_2230058
loop_
_publ_author_name
'Duong, Adam'
'Wuest, James D.'
'Maris, Thierry'
_publ_section_title
;
 trans-Dichloridobis[(pyridin-4-yl)boronic
 acid-κN]palladium(II) dimethyl sulfoxide disolvate
;
_journal_coeditor_code           KP2316
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m518
_journal_paper_doi               10.1107/S1600536811010713
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '[Pd Cl2 (C5 H6 B N O2)2], 2C2 H6 O S'
_chemical_formula_moiety         'C10 H12 B2 Cl2 N2 O4 Pd, 2(C2 H6 O S)'
_chemical_formula_sum            'C14 H24 B2 Cl2 N2 O6 Pd S2'
_chemical_formula_weight         579.39
_chemical_name_systematic
;
trans-Dichloridobis[(pyridin-4-yl)boronic acid-κN]palladium(II)
dimethyl sulfoxide disolvate
;
_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                80.687(3)
_cell_angle_beta                 82.248(3)
_cell_angle_gamma                77.456(3)
_cell_formula_units_Z            1
_cell_length_a                   6.2629(4)
_cell_length_b                   8.1515(5)
_cell_length_c                   11.7761(7)
_cell_measurement_reflns_used    4582
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.20
_cell_measurement_theta_min      3.82
_cell_volume                     576.00(6)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and Materials Studio (Accelrys, 2002)'
_computing_publication_material
'UdMX (Maris, 2004) and publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 5.5
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'Bruker SMART 6000'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  'Montel 200 optics'
_diffrn_radiation_source         'Rotating Anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_av_sigmaI/netI    0.0379
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6942
_diffrn_reflns_theta_full        72.19
_diffrn_reflns_theta_max         72.19
_diffrn_reflns_theta_min         3.82
_exptl_absorpt_coefficient_mu    10.616
_exptl_absorpt_correction_T_max  0.4277
_exptl_absorpt_correction_T_min  0.2524
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2004)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             292
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.868
_refine_ls_extinction_coef       0.0025(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2135
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0308
_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)+(0.0545P)²+0.0938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0819
_reflns_number_gt                2031
_reflns_number_total             2135
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            kp2316.cif
_cod_data_source_block           I
_cod_database_code               2230058
_cod_database_fobs_code          2230058
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd Pd1 0.0000 0.0000 1.0000 0.01847(14) Uani d S 1 . .
Cl Cl1 0.11789(13) -0.28133(9) 0.97775(6) 0.02895(19) Uani d . 1 . .
N N1 0.2223(4) 0.0656(3) 0.86854(18) 0.0200(5) Uani d . 1 . .
C C2 0.3867(5) 0.1387(4) 0.8834(2) 0.0236(6) Uani d . 1 . .
H H2 0.4017 0.1599 0.9586 0.028 Uiso calc R 1 . .
C C3 0.5340(5) 0.1837(4) 0.7926(2) 0.0233(6) Uani d . 1 . .
H H3 0.6538 0.2292 0.8067 0.028 Uiso calc R 1 . .
C C4 0.5097(5) 0.1633(4) 0.6795(2) 0.0203(6) Uani d . 1 . .
C C5 0.3368(5) 0.0875(4) 0.6668(2) 0.0217(6) Uani d . 1 . .
H H5 0.3141 0.0695 0.5920 0.026 Uiso calc R 1 . .
C C6 0.1981(5) 0.0384(4) 0.7615(2) 0.0223(6) Uani d . 1 . .
H H6 0.0835 -0.0156 0.7511 0.027 Uiso calc R 1 . .
B B7 0.6709(6) 0.2213(5) 0.5709(3) 0.0233(7) Uani d . 1 . .
O O8 0.8706(4) 0.2330(3) 0.59305(17) 0.0353(6) Uani d . 1 . .
H H8 0.9476 0.2547 0.5305 0.042 Uiso calc . 1 . .
O O9 0.6102(4) 0.2582(3) 0.46159(16) 0.0296(5) Uani d . 1 . .
H H9 0.4748 0.2611 0.4638 0.036 Uiso calc . 1 . .
O O10 0.1939(4) 0.2593(3) 0.41211(16) 0.0306(5) Uani d . 1 . .
S S10 0.13090(13) 0.28540(10) 0.28929(6) 0.02519(19) Uani d . 1 . .
C C11 0.3559(6) 0.3547(5) 0.1998(3) 0.0399(9) Uani d . 1 . .
H H11A 0.4844 0.2613 0.2002 0.060 Uiso calc R 1 . .
H H11B 0.3909 0.4503 0.2294 0.060 Uiso calc R 1 . .
H H11C 0.3164 0.3905 0.1205 0.060 Uiso calc R 1 . .
C C12 -0.0641(5) 0.4798(4) 0.2747(3) 0.0318(7) Uani d . 1 . .
H H12A -0.0058 0.5685 0.3002 0.048 Uiso calc R 1 . .
H H12B -0.2015 0.4657 0.3223 0.048 Uiso calc R 1 . .
H H12C -0.0925 0.5125 0.1935 0.048 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 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd 0.1215 3.9337 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 Pd1 N1 2_557 . . 180.0 ?
N1 Pd1 Cl1 2_557 . 2_557 90.64(7) ?
N1 Pd1 Cl1 . . 2_557 89.36(7) ?
N1 Pd1 Cl1 2_557 . . 89.36(7) ?
N1 Pd1 Cl1 . . . 90.64(7) ?
Cl1 Pd1 Cl1 2_557 . . 180.0 ?
C2 N1 C6 . . . 119.3(2) ?
C2 N1 Pd1 . . . 122.71(17) ?
C6 N1 Pd1 . . . 117.96(19) ?
N1 C2 C3 . . . 121.6(2) ?
N1 C2 H2 . . . 119.2 ?
C3 C2 H2 . . . 119.2 ?
C2 C3 C4 . . . 120.8(3) ?
C2 C3 H3 . . . 119.6 ?
C4 C3 H3 . . . 119.6 ?
C5 C4 C3 . . . 116.2(2) ?
C5 C4 B7 . . . 121.4(2) ?
C3 C4 B7 . . . 122.4(3) ?
C6 C5 C4 . . . 120.8(2) ?
C6 C5 H5 . . . 119.6 ?
C4 C5 H5 . . . 119.6 ?
N1 C6 C5 . . . 121.2(3) ?
N1 C6 H6 . . . 119.4 ?
C5 C6 H6 . . . 119.4 ?
O8 B7 O9 . . . 121.3(3) ?
O8 B7 C4 . . . 116.3(3) ?
O9 B7 C4 . . . 122.4(3) ?
B7 O8 H8 . . . 109.5 ?
B7 O9 H9 . . . 109.5 ?
O10 S10 C12 . . . 106.02(14) ?
O10 S10 C11 . . . 105.38(15) ?
C12 S10 C11 . . . 98.27(17) ?
S10 C11 H11A . . . 109.5 ?
S10 C11 H11B . . . 109.5 ?
H11A C11 H11B . . . 109.5 ?
S10 C11 H11C . . . 109.5 ?
H11A C11 H11C . . . 109.5 ?
H11B C11 H11C . . . 109.5 ?
S10 C12 H12A . . . 109.5 ?
S10 C12 H12B . . . 109.5 ?
H12A C12 H12B . . . 109.5 ?
S10 C12 H12C . . . 109.5 ?
H12A C12 H12C . . . 109.5 ?
H12B C12 H12C . . . 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N1 . 2_557 2.023(2) ?
Pd1 N1 . . 2.023(2) ?
Pd1 Cl1 . 2_557 2.2977(7) ?
Pd1 Cl1 . . 2.2977(7) ?
N1 C2 . . 1.340(4) ?
N1 C6 . . 1.348(3) ?
C2 C3 . . 1.372(4) ?
C2 H2 . . 0.9500 ?
C3 C4 . . 1.401(4) ?
C3 H3 . . 0.9500 ?
C4 C5 . . 1.393(4) ?
C4 B7 . . 1.594(4) ?
C5 C6 . . 1.380(4) ?
C5 H5 . . 0.9500 ?
C6 H6 . . 0.9500 ?
B7 O8 . . 1.338(4) ?
B7 O9 . . 1.360(4) ?
O8 H8 . . 0.8400 ?
O9 H9 . . 0.8400 ?
O10 S10 . . 1.5201(19) ?
S10 C12 . . 1.778(3) ?
S10 C11 . . 1.780(3) ?
C11 H11a . . 0.9800 ?
C11 H11b . . 0.9800 ?
C11 H11c . . 0.9800 ?
C12 H12a . . 0.9800 ?
C12 H12b . . 0.9800 ?
C12 H12c . . 0.9800 ?
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
O8 H8 O10 1_655 0.84 1.94 2.750(3) 163
O9 H9 O10 . 0.84 1.94 2.745(3) 160
C5 H5 O10 . 0.95 2.51 3.253(3) 135
C12 H12A O8 2_666 0.98 2.54 3.506(4) 169
C12 H12B O9 1_455 0.98 2.53 3.372(4) 144
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cl1 Pd1 N1 C2 2_557 . . . 63.4(2) ?
Cl1 Pd1 N1 C2 . . . . -116.6(2) ?
Cl1 Pd1 N1 C6 2_557 . . . -114.6(2) ?
Cl1 Pd1 N1 C6 . . . . 65.4(2) ?
C6 N1 C2 C3 . . . . -1.3(5) ?
Pd1 N1 C2 C3 . . . . -179.3(2) ?
N1 C2 C3 C4 . . . . 3.7(5) ?
C2 C3 C4 C5 . . . . -3.3(5) ?
C2 C3 C4 B7 . . . . 177.3(3) ?
C3 C4 C5 C6 . . . . 0.7(4) ?
B7 C4 C5 C6 . . . . -179.8(3) ?
C2 N1 C6 C5 . . . . -1.3(5) ?
Pd1 N1 C6 C5 . . . . 176.8(2) ?
C4 C5 C6 N1 . . . . 1.6(5) ?
C5 C4 B7 O8 . . . . -156.2(3) ?
C3 C4 B7 O8 . . . . 23.2(5) ?
C5 C4 B7 O9 . . . . 24.3(5) ?
C3 C4 B7 O9 . . . . -156.3(3) ?
