#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/20/2202094.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_2202094
loop_
_publ_author_name
'Englert, Ulli'
'Matern, Eberhard'
'Olkowska-Oetzel, Jolanta'
'Pikies, Jerzy'
_publ_section_title
Bis(μ-di-tert-butylphosphido)bis[(triethylphosphine)palladium(I)](Pd---Pd)
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m376
_journal_page_last               m377
_journal_paper_doi               10.1107/S160053680301081X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Pd2 (C8 H18 P)2 (C6 H15 P)2]'
_chemical_formula_moiety         'C28 H66 P4 Pd2'
_chemical_formula_sum            'C28 H66 P4 Pd2'
_chemical_formula_weight         739.53
_chemical_name_common            ' ?'
_chemical_name_systematic
;
  [Bis(μ-di-tert-butylphosphido)bis(triethylphosphine)palladium(I)]
;
_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
_cell_angle_alpha                114.150(10)
_cell_angle_beta                 103.670(10)
_cell_angle_gamma                101.720(10)
_cell_formula_units_Z            1.00
_cell_length_a                   8.9820(9)
_cell_length_b                   10.935(2)
_cell_length_c                   11.296(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    233.0(10)
_cell_measurement_theta_max      14
_cell_measurement_theta_min      11
_cell_volume                     925.7(3)
_computing_cell_refinement       'CAD-4 Operations Manual'
_computing_data_collection
'CAD-4 Operations Manual (Enraf-Nonius, 1977)'
_computing_data_reduction        'PROCESS MolEN (Fair, 1990)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      233.0(10)
_diffrn_measured_fraction_theta_full .997
_diffrn_measured_fraction_theta_max .997
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       θ/2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4955
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         26.0
_diffrn_reflns_theta_min         3.3
_diffrn_standards_decay_%        0.47
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.158
_exptl_absorpt_correction_T_max  0.749
_exptl_absorpt_correction_T_min  0.695
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'cut fragment'
_exptl_crystal_F_000             386.00
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.295
_refine_diff_density_min         -.550
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0435
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.04P)²+8P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1341
_reflns_number_gt                3266
_reflns_number_total             3623
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            na6236.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        925.8(3)
_cod_database_code               2202094
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_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
_atom_site_type_symbol
Pd 0.53266(5) 0.93446(5) 0.56989(4) 0.02742(15) Uani d . 1 . . Pd
P1 0.35742(18) 0.82055(16) 0.33932(15) 0.0300(3) Uani d . 1 . . P
P2 0.5901(2) 0.81973(17) 0.69239(17) 0.0347(4) Uani d . 1 . . P
C1 0.4247(8) 0.7051(7) 0.2006(6) 0.0382(14) Uani d . 1 . . C
C2 0.3496(12) 0.6947(12) 0.0612(8) 0.072(3) Uani d . 1 . . C
H2A 0.3647 0.7906 0.0722 0.094 Uiso calc R 1 . . H
H2B 0.2330 0.6401 0.0225 0.094 Uiso calc R 1 . . H
H2C 0.4024 0.6468 -0.0018 0.094 Uiso calc R 1 . . H
C3 0.3926(17) 0.5565(10) 0.1821(11) 0.092(4) Uani d . 1 . . C
H3A 0.4215 0.4991 0.1040 0.119 Uiso calc R 1 . . H
H3B 0.2770 0.5133 0.1632 0.119 Uiso calc R 1 . . H
H3C 0.4586 0.5605 0.2670 0.119 Uiso calc R 1 . . H
C4 0.6061(11) 0.7793(12) 0.2528(11) 0.085(3) Uani d . 1 . . C
H4A 0.6567 0.7871 0.3438 0.111 Uiso calc R 1 . . H
H4B 0.6278 0.8747 0.2616 0.111 Uiso calc R 1 . . H
H4C 0.6518 0.7241 0.1871 0.111 Uiso calc R 1 . . H
C5 0.1329(8) 0.7433(7) 0.2995(6) 0.0398(14) Uani d . 1 . . C
C6 0.0284(9) 0.7211(11) 0.1605(9) 0.068(2) Uani d . 1 . . C
H6A -0.0865 0.6939 0.1509 0.089 Uiso calc R 1 . . H
H6B 0.0446 0.6454 0.0853 0.089 Uiso calc R 1 . . H
H6C 0.0595 0.8097 0.1556 0.089 Uiso calc R 1 . . H
C7 0.0965(10) 0.8548(10) 0.4130(9) 0.070(3) Uani d . 1 . . C
H7A 0.1354 0.9472 0.4166 0.091 Uiso calc R 1 . . H
H7B 0.1520 0.8623 0.5028 0.091 Uiso calc R 1 . . H
H7C -0.0212 0.8268 0.3928 0.091 Uiso calc R 1 . . H
C8 0.0852(12) 0.6046(10) 0.3040(13) 0.084(3) Uani d . 1 . . C
H8A -0.0311 0.5738 0.2891 0.109 Uiso calc R 1 . . H
H8B 0.1485 0.6187 0.3949 0.109 Uiso calc R 1 . . H
H8C 0.1074 0.5316 0.2311 0.109 Uiso calc R 1 . . H
C9 0.4145(9) 0.7102(9) 0.7022(9) 0.0521(18) Uani d . 1 . . C
H9A 0.3440 0.6349 0.6082 0.068 Uiso calc R 1 . . H
H9B 0.4527 0.6644 0.7561 0.068 Uiso calc R 1 . . H
C10 0.3165(12) 0.7967(13) 0.7688(11) 0.078(3) Uani d . 1 . . C
H10A 0.3856 0.8701 0.8639 0.102 Uiso calc R 1 . . H
H10B 0.2235 0.7337 0.7709 0.102 Uiso calc R 1 . . H
H10C 0.2771 0.8420 0.7147 0.102 Uiso calc R 1 . . H
C11 0.6868(10) 0.6887(8) 0.6243(8) 0.0520(18) Uani d . 1 . . C
H11A 0.7003 0.6421 0.6821 0.068 Uiso calc R 1 . . H
H11B 0.6139 0.6155 0.5303 0.068 Uiso calc R 1 . . H
C12 0.8496(13) 0.7484(13) 0.6190(13) 0.086(3) Uani d . 1 . . C
H12A 0.8398 0.8029 0.5687 0.111 Uiso calc R 1 . . H
H12B 0.8870 0.6702 0.5710 0.111 Uiso calc R 1 . . H
H12C 0.9282 0.8110 0.7137 0.111 Uiso calc R 1 . . H
C13 0.7248(10) 0.9301(8) 0.8759(7) 0.0543(19) Uani d . 1 . . C
H13A 0.8268 0.9866 0.8788 0.071 Uiso calc R 1 . . H
H13B 0.6739 0.9972 0.9226 0.071 Uiso calc R 1 . . H
C14 0.7681(12) 0.8562(10) 0.9613(9) 0.074(3) Uani d . 1 . . C
H14A 0.6680 0.7963 0.9577 0.097 Uiso calc R 1 . . H
H14B 0.8333 0.9280 1.0579 0.097 Uiso calc R 1 . . H
H14C 0.8310 0.7969 0.9232 0.097 Uiso calc R 1 . . H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P .1023 .0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H .0000 .0000 '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
P2 Pd P1 . 2_676 123.52(6) yes
P2 Pd P1 . . 123.77(6) yes
P1 Pd P1 2_676 . 112.71(5) yes
P2 Pd Pd . 2_676 179.95(6) yes
P1 Pd Pd 2_676 2_676 56.45(4) yes
P1 Pd Pd . 2_676 56.26(4) yes
C5 P1 C1 . . 111.7(3) no
C5 P1 Pd . 2_676 117.3(2) no
C1 P1 Pd . 2_676 117.2(2) no
C5 P1 Pd . . 118.3(2) no
C1 P1 Pd . . 118.5(2) no
Pd P1 Pd 2_676 . 67.29(5) yes
C11 P2 C9 . . 100.5(4) no
C11 P2 C13 . . 102.8(4) no
C9 P2 C13 . . 102.7(4) no
C11 P2 Pd . . 115.6(2) no
C9 P2 Pd . . 115.8(2) no
C13 P2 Pd . . 117.1(2) no
C2 C1 C3 . . 108.4(7) no
C2 C1 C4 . . 108.5(7) no
C3 C1 C4 . . 109.0(8) no
C2 C1 P1 . . 113.5(5) no
C3 C1 P1 . . 112.9(5) no
C4 C1 P1 . . 104.2(5) no
C1 C2 H2A . . 109.5 no
C1 C2 H2B . . 109.5 no
H2A C2 H2B . . 109.5 no
C1 C2 H2C . . 109.5 no
H2A C2 H2C . . 109.5 no
H2B C2 H2C . . 109.5 no
C1 C3 H3A . . 109.5 no
C1 C3 H3B . . 109.5 no
H3A C3 H3B . . 109.5 no
C1 C3 H3C . . 109.5 no
H3A C3 H3C . . 109.5 no
H3B C3 H3C . . 109.5 no
C1 C4 H4A . . 109.5 no
C1 C4 H4B . . 109.5 no
H4A C4 H4B . . 109.5 no
C1 C4 H4C . . 109.5 no
H4A C4 H4C . . 109.5 no
H4B C4 H4C . . 109.5 no
C8 C5 C6 . . 108.7(7) no
C8 C5 C7 . . 108.6(7) no
C6 C5 C7 . . 107.9(7) no
C8 C5 P1 . . 113.6(5) no
C6 C5 P1 . . 112.8(5) no
C7 C5 P1 . . 104.9(5) no
C5 C6 H6A . . 109.5 no
C5 C6 H6B . . 109.5 no
H6A C6 H6B . . 109.5 no
C5 C6 H6C . . 109.5 no
H6A C6 H6C . . 109.5 no
H6B C6 H6C . . 109.5 no
C5 C7 H7A . . 109.5 no
C5 C7 H7B . . 109.5 no
H7A C7 H7B . . 109.5 no
C5 C7 H7C . . 109.5 no
H7A C7 H7C . . 109.5 no
H7B C7 H7C . . 109.5 no
C5 C8 H8A . . 109.5 no
C5 C8 H8B . . 109.5 no
H8A C8 H8B . . 109.5 no
C5 C8 H8C . . 109.5 no
H8A C8 H8C . . 109.5 no
H8B C8 H8C . . 109.5 no
C10 C9 P2 . . 112.3(6) no
C10 C9 H9A . . 109.1 no
P2 C9 H9A . . 109.1 no
C10 C9 H9B . . 109.1 no
P2 C9 H9B . . 109.1 no
H9A C9 H9B . . 107.9 no
C9 C10 H10A . . 109.5 no
C9 C10 H10B . . 109.5 no
H10A C10 H10B . . 109.5 no
C9 C10 H10C . . 109.5 no
H10A C10 H10C . . 109.5 no
H10B C10 H10C . . 109.5 no
C12 C11 P2 . . 114.6(6) no
C12 C11 H11A . . 108.6 no
P2 C11 H11A . . 108.6 no
C12 C11 H11B . . 108.6 no
P2 C11 H11B . . 108.6 no
H11A C11 H11B . . 107.6 no
C11 C12 H12A . . 109.5 no
C11 C12 H12B . . 109.5 no
H12A C12 H12B . . 109.5 no
C11 C12 H12C . . 109.5 no
H12A C12 H12C . . 109.5 no
H12B C12 H12C . . 109.5 no
C14 C13 P2 . . 118.5(6) no
C14 C13 H13A . . 107.7 no
P2 C13 H13A . . 107.7 no
C14 C13 H13B . . 107.7 no
P2 C13 H13B . . 107.7 no
H13A C13 H13B . . 107.1 no
C13 C14 H14A . . 109.5 no
C13 C14 H14B . . 109.5 no
H14A C14 H14B . . 109.5 no
C13 C14 H14C . . 109.5 no
H14A C14 H14C . . 109.5 no
H14B C14 H14C . . 109.5 no
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 P2 . 2.2584(15) yes
Pd P1 2_676 2.3240(17) yes
Pd P1 . 2.3293(16) yes
Pd Pd 2_676 2.5782(9) yes
P1 C5 . 1.884(7) no
P1 C1 . 1.884(6) no
P2 C11 . 1.822(7) no
P2 C9 . 1.832(7) no
P2 C13 . 1.842(7) no
C1 C2 . 1.506(10) no
C1 C3 . 1.507(10) no
C1 C4 . 1.509(11) no
C2 H2A . 0.9801 no
C2 H2B . 0.9801 no
C2 H2C . 0.9801 no
C3 H3A . 0.9801 no
C3 H3B . 0.9801 no
C3 H3C . 0.9801 no
C4 H4A . 0.9801 no
C4 H4B . 0.9801 no
C4 H4C . 0.9801 no
C5 C8 . 1.515(11) no
C5 C6 . 1.518(9) no
C5 C7 . 1.523(10) no
C6 H6A . 0.9801 no
C6 H6B . 0.9801 no
C6 H6C . 0.9801 no
C7 H7A . 0.9801 no
C7 H7B . 0.9801 no
C7 H7C . 0.9801 no
C8 H8A . 0.9801 no
C8 H8B . 0.9801 no
C8 H8C . 0.9801 no
C9 C10 . 1.519(12) no
C9 H9A . 0.9800 no
C9 H9B . 0.9800 no
C10 H10A . 0.9801 no
C10 H10B . 0.9801 no
C10 H10C . 0.9801 no
C11 C12 . 1.500(12) no
C11 H11A . 0.9800 no
C11 H11B . 0.9800 no
C12 H12A . 0.9801 no
C12 H12B . 0.9801 no
C12 H12C . 0.9801 no
C13 C14 . 1.524(10) no
C13 H13A . 0.9800 no
C13 H13B . 0.9800 no
C14 H14A . 0.9801 no
C14 H14B . 0.9801 no
C14 H14C . 0.9801 no
