#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/91/2209140.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_2209140
loop_
_publ_author_name
'Steyl, Gideon'
_publ_section_title
;
 trans-Dichlorobis(triphenylphosphine)palladium(II)
 dichloroethane solvate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1324
_journal_page_last               m1325
_journal_paper_doi               10.1107/S1600536806017521
_journal_volume                  62
_journal_year                    2006
_chemical_formula_moiety         'C36 H30 Cl2 P2 Pd, C2 H4 Cl2'
_chemical_formula_sum            'C38 H34 Cl4 P2 Pd'
_chemical_formula_weight         800.81
_chemical_name_systematic
;
trans-Dichlorobis(triphenylphosphine)palladium(II) dichloroethane solvate
;
_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                110.177(5)
_cell_angle_beta                 107.723(5)
_cell_angle_gamma                98.921(5)
_cell_formula_units_Z            1
_cell_length_a                   9.208(5)
_cell_length_b                   9.481(5)
_cell_length_c                   11.599(5)
_cell_measurement_reflns_used    5514
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.43
_cell_volume                     866.2(8)
_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, 2004)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 512
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_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  0.0337
_diffrn_reflns_av_sigmaI/netI    0.0222
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23018
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.41
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.9050
_exptl_absorpt_correction_T_min  0.8465
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 1998)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             406
_exptl_crystal_size_max          0.171
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.097
_refine_diff_density_max         2.992
_refine_diff_density_min         -1.406
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     199
_refine_ls_number_reflns         3774
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0422
_refine_ls_R_factor_gt           0.0390
_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)+(0.0356P)²+3.9311P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                3487
_reflns_number_total             3774
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2048.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (2
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_geom_torsion_publ_flag'
value 'Y' changed to 'y' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (3 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_bond_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (2
times).

'_geom_angle_publ_flag' value 'Y' changed to 'y' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_torsion_publ_flag' value 'Y' changed to 'y'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (3
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_database_code               2209140
_cod_database_fobs_code          2209140
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 0.5000 0.5000 0.5000 0.01059(10) Uani d S 1
P P 0.50557(9) 0.51019(9) 0.70576(8) 0.01194(17) Uani d . 1
Cl Cl 0.28594(8) 0.27371(8) 0.39862(7) 0.01059(10) Uani d . 1
Cl Cl41 0.94849(12) 0.21404(12) 0.59622(9) 0.0304(2) Uani d . 1
C C32 0.7823(4) 0.5724(4) 0.9282(3) 0.0180(7) Uani d . 1
H H32 0.7607 0.4641 0.8996 0.022 Uiso calc R 1
C C36 0.7166(4) 0.7976(4) 0.9004(3) 0.0194(7) Uani d . 1
H H36 0.6505 0.8408 0.8534 0.023 Uiso calc R 1
C C25 0.5670(5) 0.0835(4) 0.6662(4) 0.0251(8) Uani d . 1
H H25 0.6296 0.0248 0.6346 0.030 Uiso calc R 1
C C14 0.0974(4) 0.6867(4) 0.7977(3) 0.0188(7) Uani d . 1
H H14 0.0119 0.7170 0.8144 0.023 Uiso calc R 1
C C26 0.5739(4) 0.2284(4) 0.6612(3) 0.0209(7) Uani d . 1
H H26 0.6400 0.2658 0.6249 0.025 Uiso calc R 1
C C31 0.6822(4) 0.6344(4) 0.8555(3) 0.0143(6) Uani d . 1
C C21 0.4820(4) 0.3184(4) 0.7106(3) 0.0142(6) Uani d . 1
C C34 0.9488(4) 0.8328(4) 1.0866(3) 0.0221(7) Uani d . 1
H H34 1.0377 0.8988 1.1630 0.026 Uiso calc R 1
C C11 0.3476(4) 0.5844(4) 0.7444(3) 0.0139(6) Uani d . 1
C C35 0.8491(4) 0.8953(4) 1.0149(4) 0.0226(7) Uani d . 1
H H35 0.8714 1.0036 1.0439 0.027 Uiso calc R 1
C C23 0.3755(4) 0.1148(4) 0.7676(4) 0.0240(7) Uani d . 1
H H23 0.3090 0.0764 0.8031 0.029 Uiso calc R 1
C C24 0.4672(5) 0.0261(4) 0.7182(4) 0.0261(8) Uani d . 1
H H24 0.4614 -0.0718 0.7200 0.031 Uiso calc R 1
C C13 0.1007(4) 0.6467(4) 0.6720(3) 0.0190(7) Uani d . 1
H H13 0.0193 0.6541 0.6055 0.023 Uiso calc R 1
C C15 0.2225(4) 0.6815(4) 0.8989(3) 0.0207(7) Uani d . 1
H H15 0.2226 0.7123 0.9842 0.025 Uiso calc R 1
C C12 0.2250(4) 0.5954(4) 0.6447(3) 0.0160(6) Uani d . 1
H H12 0.2263 0.5684 0.5601 0.019 Uiso calc R 1
C C16 0.3470(4) 0.6303(4) 0.8722(3) 0.0186(7) Uani d . 1
H H16 0.4302 0.6266 0.9398 0.022 Uiso calc R 1
C C33 0.9148(4) 0.6718(4) 1.0436(3) 0.0211(7) Uani d . 1
H H33 0.9806 0.6295 1.0918 0.025 Uiso calc R 1
C C22 0.3828(4) 0.2616(4) 0.7641(3) 0.0187(7) Uani d . 1
H H22 0.3216 0.3210 0.7974 0.022 Uiso calc R 1
C C41 0.9615(7) 0.0049(9) 0.5432(5) 0.073(2) Uani d . 1
H H41A 1.0226 -0.0124 0.6188 0.087 Uiso calc R 1
H H41B 0.8564 -0.0705 0.4987 0.087 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 0.0000 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'
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
Cl Pd Cl 2_666 . 180.00(4) ?
Cl Pd P 2_666 2_666 88.03(3) ?
Cl Pd P . 2_666 91.97(3) ?
Cl Pd P 2_666 . 91.97(3) ?
Cl Pd P . . 88.03(3) y
P Pd P 2_666 . 180.0 ?
C11 P C21 . . 107.64(15) ?
C11 P C31 . . 102.66(15) ?
C21 P C31 . . 102.99(15) ?
C11 P Pd . . 111.14(11) ?
C21 P Pd . . 112.31(10) ?
C31 P Pd . . 119.08(11) ?
C31 C32 C33 . . 120.4(3) ?
C31 C32 H32 . . 119.8 ?
C33 C32 H32 . . 119.8 ?
C35 C36 C31 . . 120.2(3) ?
C35 C36 H36 . . 119.9 ?
C31 C36 H36 . . 119.9 ?
C24 C25 C26 . . 120.2(3) ?
C24 C25 H25 . . 119.9 ?
C26 C25 H25 . . 119.9 ?
C13 C14 C15 . . 119.8(3) ?
C13 C14 H14 . . 120.1 ?
C15 C14 H14 . . 120.1 ?
C25 C26 C21 . . 120.2(3) ?
C25 C26 H26 . . 119.9 ?
C21 C26 H26 . . 119.9 ?
C32 C31 C36 . . 118.9(3) ?
C32 C31 P . . 122.2(3) ?
C36 C31 P . . 118.8(2) ?
C22 C21 C26 . . 119.6(3) ?
C22 C21 P . . 123.4(3) ?
C26 C21 P . . 116.9(3) ?
C33 C34 C35 . . 119.5(3) ?
C33 C34 H34 . . 120.2 ?
C35 C34 H34 . . 120.2 ?
C16 C11 C12 . . 119.5(3) ?
C16 C11 P . . 121.0(2) ?
C12 C11 P . . 119.5(2) ?
C36 C35 C34 . . 120.6(3) ?
C36 C35 H35 . . 119.7 ?
C34 C35 H35 . . 119.7 ?
C24 C23 C22 . . 120.2(3) ?
C24 C23 H23 . . 119.9 ?
C22 C23 H23 . . 119.9 ?
C25 C24 C23 . . 120.0(3) ?
C25 C24 H24 . . 120.0 ?
C23 C24 H24 . . 120.0 ?
C14 C13 C12 . . 120.5(3) ?
C14 C13 H13 . . 119.8 ?
C12 C13 H13 . . 119.8 ?
C16 C15 C14 . . 119.9(3) ?
C16 C15 H15 . . 120.0 ?
C14 C15 H15 . . 120.0 ?
C13 C12 C11 . . 120.0(3) ?
C13 C12 H12 . . 120.0 ?
C11 C12 H12 . . 120.0 ?
C15 C16 C11 . . 120.3(3) ?
C15 C16 H16 . . 119.9 ?
C11 C16 H16 . . 119.9 ?
C34 C33 C32 . . 120.4(3) ?
C34 C33 H33 . . 119.8 ?
C32 C33 H33 . . 119.8 ?
C21 C22 C23 . . 119.7(3) ?
C21 C22 H22 . . 120.1 ?
C23 C22 H22 . . 120.1 ?
C41 C41 Cl41 2_756 . 102.5(6) ?
C41 C41 H41A 2_756 . 111.3 ?
Cl41 C41 H41A . . 111.3 ?
C41 C41 H41B 2_756 . 111.3 ?
Cl41 C41 H41B . . 111.3 ?
H41A C41 H41B . . 109.2 ?
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 Cl 2_666 2.3255(12) ?
Pd Cl . 2.3255(12) y
Pd P 2_666 2.3394(13) ?
Pd P . 2.3394(13) y
P C11 . 1.819(3) ?
P C21 . 1.819(3) ?
P C31 . 1.824(3) ?
Cl41 C41 . 1.898(8) ?
C32 C31 . 1.394(5) ?
C32 C33 . 1.396(5) ?
C32 H32 . 0.9300 ?
C36 C35 . 1.387(5) ?
C36 C31 . 1.399(5) ?
C36 H36 . 0.9300 ?
C25 C24 . 1.382(6) ?
C25 C26 . 1.388(5) ?
C25 H25 . 0.9300 ?
C14 C13 . 1.385(5) ?
C14 C15 . 1.394(5) ?
C14 H14 . 0.9300 ?
C26 C21 . 1.399(5) ?
C26 H26 . 0.9300 ?
C21 C22 . 1.390(5) ?
C34 C33 . 1.381(5) ?
C34 C35 . 1.389(5) ?
C34 H34 . 0.9300 ?
C11 C16 . 1.395(5) ?
C11 C12 . 1.396(4) ?
C35 H35 . 0.9300 ?
C23 C24 . 1.389(6) ?
C23 C22 . 1.398(5) ?
C23 H23 . 0.9300 ?
C24 H24 . 0.9300 ?
C13 C12 . 1.390(5) ?
C13 H13 . 0.9300 ?
C15 C16 . 1.390(5) ?
C15 H15 . 0.9300 ?
C12 H12 . 0.9300 ?
C16 H16 . 0.9300 ?
C33 H33 . 0.9300 ?
C22 H22 . 0.9300 ?
C41 C41 2_756 1.380(12) ?
C41 H41A . 0.9700 ?
C41 H41B . 0.9700 ?
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
_geom_torsion_publ_flag
Cl Pd P C11 2_666 102.80(12) ?
Cl Pd P C11 . -77.20(12) y
Cl Pd P C21 2_666 -136.55(12) ?
Cl Pd P C21 . 43.45(12) y
Cl Pd P C31 2_666 -16.14(12) ?
Cl Pd P C31 . 163.86(12) y
C24 C25 C26 C21 . 1.0(5) ?
C33 C32 C31 C36 . -0.2(5) ?
C33 C32 C31 P . -178.9(3) ?
C35 C36 C31 C32 . 0.5(5) ?
C35 C36 C31 P . 179.3(3) ?
C11 P C31 C32 . 124.3(3) ?
C21 P C31 C32 . 12.6(3) ?
Pd P C31 C32 . -112.5(3) ?
C11 P C31 C36 . -54.4(3) ?
C21 P C31 C36 . -166.1(3) ?
Pd P C31 C36 . 68.8(3) ?
C25 C26 C21 C22 . -0.3(5) ?
C25 C26 C21 P . 177.5(3) ?
C11 P C21 C22 . -13.0(3) ?
C31 P C21 C22 . 95.0(3) ?
Pd P C21 C22 . -135.7(2) ?
C11 P C21 C26 . 169.2(3) ?
C31 P C21 C26 . -82.8(3) ?
Pd P C21 C26 . 46.5(3) ?
C21 P C11 C16 . 69.6(3) ?
C31 P C11 C16 . -38.6(3) ?
Pd P C11 C16 . -167.0(2) ?
C21 P C11 C12 . -110.2(3) ?
C31 P C11 C12 . 141.5(3) ?
Pd P C11 C12 . 13.1(3) ?
C31 C36 C35 C34 . -0.3(5) ?
C33 C34 C35 C36 . -0.3(5) ?
C26 C25 C24 C23 . -1.1(5) ?
C22 C23 C24 C25 . 0.5(5) ?
C15 C14 C13 C12 . 2.5(5) ?
C13 C14 C15 C16 . -2.5(5) ?
C14 C13 C12 C11 . -0.2(5) ?
C16 C11 C12 C13 . -2.2(5) ?
P C11 C12 C13 . 177.7(3) ?
C14 C15 C16 C11 . 0.2(5) ?
C12 C11 C16 C15 . 2.1(5) ?
P C11 C16 C15 . -177.7(3) ?
C35 C34 C33 C32 . 0.7(5) ?
C31 C32 C33 C34 . -0.4(5) ?
C26 C21 C22 C23 . -0.3(5) ?
P C21 C22 C23 . -178.0(3) ?
C24 C23 C22 C21 . 0.2(5) ?
