#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/06/7050609.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_7050609
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 Br2 Pd'
_chemical_formula_weight         746.64
_chemical_name_common
trans-Dibromobis(tri(methylallyl)arsine)palladium(ii)
_chemical_name_systematic
trans-Dibromobis(tri(methylallyl)arsine)palladium(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                108.471(13)
_cell_angle_beta                 103.331(14)
_cell_angle_gamma                96.937(12)
_cell_formula_units_Z            1
_cell_length_a                   8.8295(17)
_cell_length_b                   9.4059(14)
_cell_length_c                   9.5258(19)
_cell_measurement_temperature    173(2)
_cell_volume                     713.9(2)
_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 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0497
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3581
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.35
_exptl_absorpt_coefficient_mu    5.758
_exptl_absorpt_correction_type
;
empirical - XABS2 (S. Parkin, B. Moezzi,
H. Hope, J. Appl. Cryst. 1995, 28, 53.)
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             368
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.153
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         3366
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0520
_refine_ls_R_factor_gt           0.0360
_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)+(0.0444P)²+0.1565P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                2744
_reflns_number_total             3366
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b303990k.txt
_cod_data_source_block           jain07
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050609
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 0.5000 0.5000 0.0000 0.01694(11) Uani 1 2 d S . .
As1 As 0.69805(4) 0.60612(4) -0.09741(4) 0.01783(11) Uani 1 1 d . . .
Br1 Br 0.71076(5) 0.41935(6) 0.15294(6) 0.03245(13) Uani 1 1 d . . .
C1 C 0.8242(5) 0.4568(5) -0.1764(5) 0.0234(8) Uani 1 1 d . . .
H1A H 0.9270 0.5128 -0.1754 0.028 Uiso 1 1 calc R . .
H1B H 0.8474 0.3987 -0.1064 0.028 Uiso 1 1 calc R . .
C2 C 0.7415(5) 0.3454(5) -0.3378(5) 0.0314(10) Uani 1 1 d . . .
C3 C 0.8081(7) 0.3305(6) -0.4498(6) 0.0470(13) Uani 1 1 d . . .
H3A H 0.9105 0.3905 -0.4300 0.056 Uiso 1 1 calc R . .
H3B H 0.7540 0.2596 -0.5508 0.056 Uiso 1 1 calc R . .
C4 C 0.5804(6) 0.2514(6) -0.3607(7) 0.0440(12) Uani 1 1 d . . .
H4A H 0.5369 0.1836 -0.4691 0.066 Uiso 1 1 calc R . .
H4B H 0.5081 0.3200 -0.3333 0.066 Uiso 1 1 calc R . .
H4C H 0.5916 0.1897 -0.2946 0.066 Uiso 1 1 calc R . .
C11 C 0.8604(5) 0.7733(4) 0.0691(5) 0.0238(8) Uani 1 1 d . . .
H11A H 0.9426 0.7289 0.1205 0.029 Uiso 1 1 calc R . .
H11B H 0.9128 0.8393 0.0236 0.029 Uiso 1 1 calc R . .
C12 C 0.7924(5) 0.8704(5) 0.1881(5) 0.0273(9) Uani 1 1 d . . .
C13 C 0.8330(6) 0.8733(6) 0.3321(6) 0.0406(11) Uani 1 1 d . . .
H13A H 0.7885 0.9338 0.4060 0.049 Uiso 1 1 calc R . .
H13B H 0.9067 0.8148 0.3613 0.049 Uiso 1 1 calc R . .
C14 C 0.6773(7) 0.9598(6) 0.1352(6) 0.0453(13) Uani 1 1 d . . .
H14A H 0.6416 1.0182 0.2222 0.068 Uiso 1 1 calc R . .
H14B H 0.5853 0.8893 0.0530 0.068 Uiso 1 1 calc R . .
H14C H 0.7293 1.0306 0.0958 0.068 Uiso 1 1 calc R . .
C21 C 0.6311(5) 0.6870(5) -0.2644(5) 0.0270(9) Uani 1 1 d . . .
H21A H 0.5953 0.5998 -0.3641 0.032 Uiso 1 1 calc R . .
H21B H 0.5382 0.7333 -0.2503 0.032 Uiso 1 1 calc R . .
C22 C 0.7557(5) 0.8044(5) -0.2748(5) 0.0265(9) Uani 1 1 d . . .
C23 C 0.7459(6) 0.9497(6) -0.2375(6) 0.0408(11) Uani 1 1 d . . .
H23A H 0.8237 1.0211 -0.2487 0.049 Uiso 1 1 calc R . .
H23B H 0.6610 0.9831 -0.1993 0.049 Uiso 1 1 calc R . .
C24 C 0.8885(6) 0.7479(6) -0.3355(7) 0.0447(13) Uani 1 1 d . . .
H24A H 0.9616 0.8345 -0.3364 0.067 Uiso 1 1 calc R . .
H24B H 0.8441 0.6729 -0.4408 0.067 Uiso 1 1 calc R . .
H24C H 0.9462 0.6994 -0.2690 0.067 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'
Br Br -0.2901 2.4595 '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
As1 Pd1 As1 180.0 . 2_665 ?
As1 Pd1 Br1 92.02(2) . 2_665 ?
As1 Pd1 Br1 87.98(2) 2_665 2_665 ?
As1 Pd1 Br1 87.98(2) . . ?
As1 Pd1 Br1 92.02(2) 2_665 . ?
Br1 Pd1 Br1 180.00(2) 2_665 . ?
C11 As1 C1 102.71(16) . . ?
C11 As1 C21 105.55(17) . . ?
C1 As1 C21 104.20(18) . . ?
C11 As1 Pd1 111.32(12) . . ?
C1 As1 Pd1 111.91(12) . . ?
C21 As1 Pd1 119.58(12) . . ?
C2 C1 As1 113.2(3) . . ?
C3 C2 C1 121.3(5) . . ?
C3 C2 C4 122.7(5) . . ?
C1 C2 C4 116.0(4) . . ?
C12 C11 As1 112.9(3) . . ?
C13 C12 C14 122.5(4) . . ?
C13 C12 C11 120.6(4) . . ?
C14 C12 C11 116.9(4) . . ?
C22 C21 As1 115.9(3) . . ?
C23 C22 C24 121.3(4) . . ?
C23 C22 C21 121.5(4) . . ?
C24 C22 C21 117.1(4) . . ?
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 As1 2.4143(5) . ?
Pd1 As1 2.4143(5) 2_665 ?
Pd1 Br1 2.4397(6) 2_665 ?
Pd1 Br1 2.4397(6) . ?
As1 C11 1.967(4) . ?
As1 C1 1.968(4) . ?
As1 C21 1.975(4) . ?
C1 C2 1.507(6) . ?
C2 C3 1.311(7) . ?
C2 C4 1.511(7) . ?
C11 C12 1.507(6) . ?
C12 C13 1.326(7) . ?
C12 C14 1.494(6) . ?
C21 C22 1.505(5) . ?
C22 C23 1.318(6) . ?
C22 C24 1.504(6) . ?
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
As1 Pd1 As1 C11 -97(100) 2_665 . . . ?
Br1 Pd1 As1 C11 116.52(13) 2_665 . . . ?
Br1 Pd1 As1 C11 -63.48(13) . . . . ?
As1 Pd1 As1 C1 17(100) 2_665 . . . ?
Br1 Pd1 As1 C1 -129.18(13) 2_665 . . . ?
Br1 Pd1 As1 C1 50.82(13) . . . . ?
As1 Pd1 As1 C21 140(100) 2_665 . . . ?
Br1 Pd1 As1 C21 -7.02(15) 2_665 . . . ?
Br1 Pd1 As1 C21 172.98(15) . . . . ?
C11 As1 C1 C2 -159.4(3) . . . . ?
C21 As1 C1 C2 -49.4(3) . . . . ?
Pd1 As1 C1 C2 81.1(3) . . . . ?
As1 C1 C2 C3 123.4(4) . . . . ?
As1 C1 C2 C4 -57.7(5) . . . . ?
C1 As1 C11 C12 -156.7(3) . . . . ?
C21 As1 C11 C12 94.4(3) . . . . ?
Pd1 As1 C11 C12 -36.8(3) . . . . ?
As1 C11 C12 C13 114.6(4) . . . . ?
As1 C11 C12 C14 -64.5(4) . . . . ?
C11 As1 C21 C22 29.8(4) . . . . ?
C1 As1 C21 C22 -78.0(4) . . . . ?
Pd1 As1 C21 C22 156.1(3) . . . . ?
As1 C21 C22 C23 -109.2(4) . . . . ?
As1 C21 C22 C24 73.1(5) . . . . ?
