#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/06/7050611.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7050611
loop_
_publ_author_name
'Phadnis, Prasad P.'
'Jain, Vimal K.'
'Klein, Axel'
'Schurr, Thilo'
'Kaim, Wolfgang'
_publ_section_title
;
 Tri(allyl)- and tri(methylallyl)arsine complexes of palladium(ii) and
 platinum(ii): synthesis, spectroscopy, photochemistry and structures
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1584
_journal_paper_doi               10.1039/b303990k
_journal_volume                  27
_journal_year                    2003
_chemical_formula_sum            'C24 H42 As2 Cl4 Pd2'
_chemical_formula_weight         835.09
_chemical_name_common
;
trans-μ-Dichlorobis(chloro-tri(methylallyl)arsinepalladium(ii))
;
_chemical_name_systematic
;
trans-μ-Dichlorobis(chloro-tri(methylallyl)arsinepalladium(II))
;
_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                94.326(12)
_cell_angle_beta                 98.760(13)
_cell_angle_gamma                100.107(14)
_cell_formula_units_Z            2
_cell_length_a                   7.7802(15)
_cell_length_b                   10.0937(16)
_cell_length_c                   20.620(3)
_cell_measurement_temperature    173(2)
_cell_volume                     1566.9(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  Siemens-P4
_diffrn_measurement_method       '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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0533
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7514
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    3.596
_exptl_absorpt_correction_type   'empirical - psi scans'
_exptl_crystal_colour            'brown red'
_exptl_crystal_density_diffrn    1.770
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.158
_refine_diff_density_min         -1.361
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.189
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         7514
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.189
_refine_ls_R_factor_all          0.0747
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0580P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1162
_refine_ls_wR_factor_ref         0.1270
_reflns_number_gt                5602
_reflns_number_total             7514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303990k.txt
_cod_data_source_block           jain06
_cod_depositor_comments
;
 Replacing the "&#x00B5;" substring with the "\m" substring in the
 values of the _chemical_name_common and _chemical_name_systematic
 data items.

 Antanas Vaitkus,
 2017-03-30
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050611
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.48595(6) 0.59894(4) 0.329046(19) 0.02848(11) Uani 1 1 d . . .
Pd2 Pd 0.45849(6) 0.34760(4) 0.21116(2) 0.02954(11) Uani 1 1 d . . .
Cl1 Cl 0.7178(2) 0.76320(15) 0.37731(8) 0.0432(4) Uani 1 1 d . . .
Cl2 Cl 0.2388(2) 0.25196(16) 0.12554(7) 0.0429(3) Uani 1 1 d . . .
Cl3 Cl 0.2550(2) 0.42699(15) 0.27815(8) 0.0408(3) Uani 1 1 d . . .
Cl4 Cl 0.6842(2) 0.45557(15) 0.29520(7) 0.0404(3) Uani 1 1 d . . .
As1 As 0.28223(8) 0.72740(6) 0.35965(3) 0.03105(14) Uani 1 1 d . . .
As2 As 0.67447(8) 0.28401(5) 0.15478(3) 0.02982(14) Uani 1 1 d . . .
C11 C 0.3924(9) 0.9048(6) 0.4077(4) 0.0536(18) Uani 1 1 d . . .
H11A H 0.4285 0.8911 0.4545 0.064 Uiso 1 1 calc R . .
H11B H 0.5019 0.9378 0.3902 0.064 Uiso 1 1 calc R . .
C12 C 0.2860(10) 1.0144(7) 0.4061(4) 0.0526(18) Uani 1 1 d . . .
C13 C 0.3204(14) 1.1135(8) 0.3679(5) 0.086(3) Uani 1 1 d . . .
H13A H 0.2565 1.1855 0.3678 0.103 Uiso 1 1 calc R . .
H13B H 0.4088 1.1120 0.3409 0.103 Uiso 1 1 calc R . .
C14 C 0.1510(12) 1.0107(9) 0.4490(5) 0.071(2) Uani 1 1 d . . .
H14A H 0.1057 1.0954 0.4489 0.107 Uiso 1 1 calc R . .
H14B H 0.2038 0.9998 0.4941 0.107 Uiso 1 1 calc R . .
H14C H 0.0533 0.9345 0.4327 0.107 Uiso 1 1 calc R . .
C21 C 0.1050(8) 0.7551(7) 0.2858(3) 0.0423(14) Uani 1 1 d . . .
H21A H 0.0262 0.6667 0.2701 0.051 Uiso 1 1 calc R . .
H21B H 0.0314 0.8156 0.3030 0.051 Uiso 1 1 calc R . .
C22 C 0.1709(9) 0.8127(7) 0.2275(3) 0.0454(15) Uani 1 1 d . . .
C23 C 0.1462(12) 0.9353(9) 0.2131(4) 0.071(2) Uani 1 1 d . . .
H23A H 0.0866 0.9861 0.2399 0.085 Uiso 1 1 calc R . .
H23B H 0.1882 0.9717 0.1760 0.085 Uiso 1 1 calc R . .
C24 C 0.2588(11) 0.7268(7) 0.1856(3) 0.0541(18) Uani 1 1 d . . .
H24A H 0.2960 0.7766 0.1495 0.081 Uiso 1 1 calc R . .
H24B H 0.1752 0.6433 0.1673 0.081 Uiso 1 1 calc R . .
H24C H 0.3627 0.7044 0.2126 0.081 Uiso 1 1 calc R . .
C31 C 0.1272(9) 0.6316(7) 0.4142(3) 0.0418(14) Uani 1 1 d . . .
H31A H 0.0474 0.6914 0.4272 0.050 Uiso 1 1 calc R . .
H31B H 0.0523 0.5510 0.3870 0.050 Uiso 1 1 calc R . .
C32 C 0.2192(10) 0.5865(8) 0.4752(3) 0.0525(17) Uani 1 1 d . . .
C33 C 0.2587(15) 0.6679(10) 0.5316(4) 0.093(3) Uani 1 1 d . . .
H33A H 0.2283 0.7551 0.5331 0.112 Uiso 1 1 calc R . .
H33B H 0.3173 0.6387 0.5702 0.112 Uiso 1 1 calc R . .
C34 C 0.2615(13) 0.4470(8) 0.4685(4) 0.075(3) Uani 1 1 d . . .
H34A H 0.2902 0.4177 0.5125 0.112 Uiso 1 1 calc R . .
H34B H 0.3631 0.4484 0.4456 0.112 Uiso 1 1 calc R . .
H34C H 0.1588 0.3840 0.4432 0.112 Uiso 1 1 calc R . .
C41 C 0.5864(8) 0.1700(7) 0.0717(3) 0.0436(15) Uani 1 1 d . . .
H41A H 0.4971 0.0931 0.0798 0.052 Uiso 1 1 calc R . .
H41B H 0.5248 0.2233 0.0406 0.052 Uiso 1 1 calc R . .
C42 C 0.7222(10) 0.1134(8) 0.0382(3) 0.0538(18) Uani 1 1 d . . .
C43 C 0.7974(14) 0.1828(11) -0.0079(4) 0.088(3) Uani 1 1 d . . .
H43A H 0.8822 0.1479 -0.0294 0.106 Uiso 1 1 calc R . .
H43B H 0.7650 0.2661 -0.0185 0.106 Uiso 1 1 calc R . .
C44 C 0.7705(13) -0.0151(9) 0.0551(4) 0.077(3) Uani 1 1 d . . .
H44A H 0.8151 -0.0568 0.0182 0.116 Uiso 1 1 calc R . .
H44B H 0.6660 -0.0760 0.0641 0.116 Uiso 1 1 calc R . .
H44C H 0.8628 0.0015 0.0944 0.116 Uiso 1 1 calc R . .
C51 C 0.8447(8) 0.2020(6) 0.2109(3) 0.0347(12) Uani 1 1 d . . .
H51A H 0.9098 0.1541 0.1820 0.042 Uiso 1 1 calc R . .
H51B H 0.9320 0.2758 0.2385 0.042 Uiso 1 1 calc R . .
C52 C 0.7707(8) 0.1048(6) 0.2555(3) 0.0384(13) Uani 1 1 d . . .
C53 C 0.8162(12) 0.1336(8) 0.3207(3) 0.061(2) Uani 1 1 d . . .
H53A H 0.7694 0.0725 0.3492 0.073 Uiso 1 1 calc R . .
H53B H 0.8954 0.2154 0.3385 0.073 Uiso 1 1 calc R . .
C54 C 0.6491(12) -0.0197(8) 0.2253(4) 0.072(3) Uani 1 1 d . . .
H54A H 0.5967 -0.0664 0.2596 0.109 Uiso 1 1 calc R . .
H54B H 0.7142 -0.0787 0.2030 0.109 Uiso 1 1 calc R . .
H54C H 0.5549 0.0028 0.1932 0.109 Uiso 1 1 calc R . .
C61 C 0.8329(9) 0.4414(6) 0.1326(3) 0.0427(14) Uani 1 1 d . . .
H61A H 0.8968 0.4952 0.1742 0.051 Uiso 1 1 calc R . .
H61B H 0.9222 0.4089 0.1093 0.051 Uiso 1 1 calc R . .
C62 C 0.7426(10) 0.5329(7) 0.0905(4) 0.0492(16) Uani 1 1 d . . .
C63 C 0.7760(14) 0.5478(10) 0.0301(4) 0.087(3) Uani 1 1 d . . .
H63A H 0.7254 0.6110 0.0051 0.105 Uiso 1 1 calc R . .
H63B H 0.8505 0.4954 0.0117 0.105 Uiso 1 1 calc R . .
C64 C 0.6263(14) 0.6132(8) 0.1211(5) 0.080(3) Uani 1 1 d . . .
H64A H 0.5814 0.6721 0.0896 0.121 Uiso 1 1 calc R . .
H64B H 0.6946 0.6686 0.1608 0.121 Uiso 1 1 calc R . .
H64C H 0.5265 0.5516 0.1330 0.121 Uiso 1 1 calc R . .
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'
As As 0.0499 2.0058 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl1 Pd1 Cl3 178.13(6) . . ?
Cl1 Pd1 As1 91.50(5) . . ?
Cl3 Pd1 As1 90.35(4) . . ?
Cl1 Pd1 Cl4 91.55(6) . . ?
Cl3 Pd1 Cl4 86.60(5) . . ?
As1 Pd1 Cl4 176.93(4) . . ?
Cl2 Pd2 Cl4 176.82(6) . . ?
Cl2 Pd2 As2 91.38(5) . . ?
Cl4 Pd2 As2 88.31(4) . . ?
Cl2 Pd2 Cl3 94.03(6) . . ?
Cl4 Pd2 Cl3 86.24(5) . . ?
As2 Pd2 Cl3 174.53(4) . . ?
Pd1 Cl3 Pd2 88.54(5) . . ?
Pd2 Cl4 Pd1 88.99(5) . . ?
C31 As1 C11 107.7(3) . . ?
C31 As1 C21 100.1(3) . . ?
C11 As1 C21 108.3(3) . . ?
C31 As1 Pd1 111.72(19) . . ?
C11 As1 Pd1 113.9(2) . . ?
C21 As1 Pd1 114.1(2) . . ?
C41 As2 C51 110.0(3) . . ?
C41 As2 C61 105.3(3) . . ?
C51 As2 C61 100.4(3) . . ?
C41 As2 Pd2 115.74(19) . . ?
C51 As2 Pd2 112.19(18) . . ?
C61 As2 Pd2 111.9(2) . . ?
C12 C11 As1 118.1(5) . . ?
C13 C12 C14 122.7(8) . . ?
C13 C12 C11 119.3(8) . . ?
C14 C12 C11 117.9(7) . . ?
C22 C21 As1 117.6(4) . . ?
C23 C22 C21 120.1(7) . . ?
C23 C22 C24 122.0(7) . . ?
C21 C22 C24 117.8(6) . . ?
C32 C31 As1 115.5(5) . . ?
C33 C32 C31 120.4(8) . . ?
C33 C32 C34 123.5(8) . . ?
C31 C32 C34 116.2(6) . . ?
C42 C41 As2 116.8(4) . . ?
C43 C42 C44 120.8(8) . . ?
C43 C42 C41 119.3(8) . . ?
C44 C42 C41 119.9(8) . . ?
C52 C51 As2 116.7(4) . . ?
C53 C52 C54 122.2(7) . . ?
C53 C52 C51 119.6(6) . . ?
C54 C52 C51 118.2(5) . . ?
C62 C61 As2 114.9(5) . . ?
C63 C62 C64 121.7(7) . . ?
C63 C62 C61 120.6(7) . . ?
C64 C62 C61 117.5(6) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 Cl1 2.2686(16) . ?
Pd1 Cl3 2.3236(15) . ?
Pd1 As1 2.3439(8) . ?
Pd1 Cl4 2.4329(16) . ?
Pd2 Cl2 2.2835(16) . ?
Pd2 Cl4 2.3218(15) . ?
Pd2 As2 2.3341(8) . ?
Pd2 Cl3 2.4498(16) . ?
As1 C31 1.955(6) . ?
As1 C11 1.964(6) . ?
As1 C21 1.965(6) . ?
As2 C41 1.949(6) . ?
As2 C51 1.959(6) . ?
As2 C61 1.961(6) . ?
C11 C12 1.493(10) . ?
C12 C13 1.334(12) . ?
C12 C14 1.472(11) . ?
C21 C22 1.494(9) . ?
C22 C23 1.333(10) . ?
C22 C24 1.497(10) . ?
C31 C32 1.492(9) . ?
C32 C33 1.334(10) . ?
C32 C34 1.502(11) . ?
C41 C42 1.514(9) . ?
C42 C43 1.366(12) . ?
C42 C44 1.465(11) . ?
C51 C52 1.497(8) . ?
C52 C53 1.333(9) . ?
C52 C54 1.465(9) . ?
C61 C62 1.504(9) . ?
C62 C63 1.325(10) . ?
C62 C64 1.493(11) . ?
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
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl1 Pd1 Cl3 Pd2 -13.9(19) . . . . ?
As1 Pd1 Cl3 Pd2 157.85(4) . . . . ?
Cl4 Pd1 Cl3 Pd2 -22.54(5) . . . . ?
Cl2 Pd2 Cl3 Pd1 -153.13(6) . . . . ?
Cl4 Pd2 Cl3 Pd1 23.69(6) . . . . ?
As2 Pd2 Cl3 Pd1 18.1(5) . . . . ?
Cl2 Pd2 Cl4 Pd1 72.4(11) . . . . ?
As2 Pd2 Cl4 Pd1 156.90(4) . . . . ?
Cl3 Pd2 Cl4 Pd1 -22.56(5) . . . . ?
Cl1 Pd1 Cl4 Pd2 -155.87(6) . . . . ?
Cl3 Pd1 Cl4 Pd2 23.85(6) . . . . ?
As1 Pd1 Cl4 Pd2 31.2(8) . . . . ?
Cl1 Pd1 As1 C31 -121.5(2) . . . . ?
Cl3 Pd1 As1 C31 58.7(2) . . . . ?
Cl4 Pd1 As1 C31 51.5(8) . . . . ?
Cl1 Pd1 As1 C11 0.9(3) . . . . ?
Cl3 Pd1 As1 C11 -178.9(3) . . . . ?
Cl4 Pd1 As1 C11 173.8(8) . . . . ?
Cl1 Pd1 As1 C21 125.9(2) . . . . ?
Cl3 Pd1 As1 C21 -53.9(2) . . . . ?
Cl4 Pd1 As1 C21 -61.2(8) . . . . ?
Cl2 Pd2 As2 C41 -6.2(2) . . . . ?
Cl4 Pd2 As2 C41 176.9(2) . . . . ?
Cl3 Pd2 As2 C41 -177.4(5) . . . . ?
Cl2 Pd2 As2 C51 -133.64(18) . . . . ?
Cl4 Pd2 As2 C51 49.53(18) . . . . ?
Cl3 Pd2 As2 C51 55.2(5) . . . . ?
Cl2 Pd2 As2 C61 114.4(2) . . . . ?
Cl4 Pd2 As2 C61 -62.4(2) . . . . ?
Cl3 Pd2 As2 C61 -56.8(5) . . . . ?
C31 As1 C11 C12 -79.6(7) . . . . ?
C21 As1 C11 C12 27.8(7) . . . . ?
Pd1 As1 C11 C12 155.8(5) . . . . ?
As1 C11 C12 C13 -104.2(8) . . . . ?
As1 C11 C12 C14 78.1(8) . . . . ?
C31 As1 C21 C22 -173.0(5) . . . . ?
C11 As1 C21 C22 74.4(6) . . . . ?
Pd1 As1 C21 C22 -53.6(6) . . . . ?
As1 C21 C22 C23 -113.6(7) . . . . ?
As1 C21 C22 C24 68.3(7) . . . . ?
C11 As1 C31 C32 -69.9(6) . . . . ?
C21 As1 C31 C32 177.1(5) . . . . ?
Pd1 As1 C31 C32 55.9(6) . . . . ?
As1 C31 C32 C33 89.4(9) . . . . ?
As1 C31 C32 C34 -91.0(8) . . . . ?
C51 As2 C41 C42 -44.4(6) . . . . ?
C61 As2 C41 C42 63.0(6) . . . . ?
Pd2 As2 C41 C42 -172.8(5) . . . . ?
As2 C41 C42 C43 -92.7(8) . . . . ?
As2 C41 C42 C44 87.7(8) . . . . ?
C41 As2 C51 C52 -88.6(5) . . . . ?
C61 As2 C51 C52 160.7(5) . . . . ?
Pd2 As2 C51 C52 41.8(5) . . . . ?
As2 C51 C52 C53 -116.7(6) . . . . ?
As2 C51 C52 C54 63.1(8) . . . . ?
C41 As2 C61 C62 67.7(6) . . . . ?
C51 As2 C61 C62 -178.0(5) . . . . ?
Pd2 As2 C61 C62 -58.9(5) . . . . ?
As2 C61 C62 C63 -115.5(8) . . . . ?
As2 C61 C62 C64 69.1(8) . . . . ?
