#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/51/2235177.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_2235177
loop_
_publ_author_name
'Breunig, Jens'
'Lerner, Hans-Wolfram'
'Bolte, Michael'
_publ_section_title
;
 A triclinic polymorph of
 bis(μ-di-tert-butylphosphanido)bis[(di-tert-butylphosphane)palladium(I)]
;
_journal_coeditor_code           NG5274
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m836
_journal_paper_doi               10.1107/S1600536812023574
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Pd2 (C8 H18 P)2 (C8 H19 P)2]'
_chemical_formula_moiety         'C32 H74 P4 Pd2'
_chemical_formula_sum            'C32 H74 P4 Pd2'
_chemical_formula_weight         795.59
_chemical_name_systematic
;
bis(μ-di-tert-butylphosphanido)bis[(di-tert-
butylphosphane)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
_audit_creation_method           SHELXL97
_cell_angle_alpha                89.064(5)
_cell_angle_beta                 67.307(4)
_cell_angle_gamma                75.330(5)
_cell_formula_units_Z            1
_cell_length_a                   9.0721(5)
_cell_length_b                   10.5156(6)
_cell_length_c                   11.5351(6)
_cell_measurement_reflns_used    11232
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.0
_cell_measurement_theta_min      3.5
_cell_volume                     978.06(10)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2001)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2001)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Stoe IPDS II two-circle'
_diffrn_measurement_method       ω
_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  0.0658
_diffrn_reflns_av_sigmaI/netI    0.0451
_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       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13922
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         3.51
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.102
_exptl_absorpt_correction_T_max  0.9573
_exptl_absorpt_correction_T_min  0.7857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(MULABS; Spek, 2009; Blessing, 1995)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             418
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.310
_refine_diff_density_min         -1.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         4481
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0421
_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)+(0.0669P)²+1.1837P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1112
_reflns_number_gt                4083
_reflns_number_total             4481
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ng5274.cif
_cod_data_source_block           I
_cod_original_cell_volume        978.06(9)
_cod_database_code               2235177
_cod_database_fobs_code          2235177
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_symmetry_multiplicity
Pd Pd1 0.50058(3) 0.07733(2) 0.41089(2) 0.01892(10) Uani d . 1 1
P P1 0.46490(10) 0.14997(8) 0.61308(7) 0.02064(18) Uani d . 1 1
P P2 0.49486(11) 0.23437(8) 0.27214(8) 0.02250(18) Uani d . 1 1
H H2 0.479(6) 0.345(5) 0.312(4) 0.033(11) Uiso d . 1 1
C C1 0.2544(4) 0.2667(4) 0.7086(3) 0.0275(7) Uani d . 1 1
C C2 0.6381(4) 0.2167(3) 0.6181(3) 0.0256(7) Uani d . 1 1
C C3 0.3122(5) 0.2678(4) 0.2244(3) 0.0305(7) Uani d . 1 1
C C4 0.6950(5) 0.2228(4) 0.1328(3) 0.0290(7) Uani d . 1 1
C C11 0.2300(6) 0.4002(4) 0.6554(5) 0.0476(11) Uani d . 1 1
H H11A 0.3097 0.4445 0.6620 0.071 Uiso calc R 1 1
H H11B 0.1170 0.4546 0.7034 0.071 Uiso calc R 1 1
H H11C 0.2476 0.3874 0.5666 0.071 Uiso calc R 1 1
C C12 0.2212(6) 0.2872(5) 0.8483(4) 0.0439(10) Uani d . 1 1
H H12A 0.2370 0.2013 0.8827 0.066 Uiso calc R 1 1
H H12B 0.1070 0.3404 0.8943 0.066 Uiso calc R 1 1
H H12C 0.2983 0.3328 0.8574 0.066 Uiso calc R 1 1
C C13 0.1300(5) 0.1985(4) 0.6982(4) 0.0379(9) Uani d . 1 1
H H13A 0.1452 0.1125 0.7325 0.057 Uiso calc R 1 1
H H13B 0.1476 0.1859 0.6094 0.057 Uiso calc R 1 1
H H13C 0.0171 0.2533 0.7461 0.057 Uiso calc R 1 1
C C21 0.6472(6) 0.3438(4) 0.5533(5) 0.0418(10) Uani d . 1 1
H H21A 0.6534 0.3300 0.4676 0.063 Uiso calc R 1 1
H H21B 0.7460 0.3685 0.5496 0.063 Uiso calc R 1 1
H H21C 0.5480 0.4146 0.6013 0.063 Uiso calc R 1 1
C C22 0.6292(6) 0.2379(6) 0.7517(4) 0.0456(11) Uani d . 1 1
H H22A 0.6238 0.1561 0.7931 0.068 Uiso calc R 1 1
H H22B 0.5299 0.3085 0.8000 0.068 Uiso calc R 1 1
H H22C 0.7281 0.2626 0.7476 0.068 Uiso calc R 1 1
C C23 0.7975(5) 0.1095(4) 0.5433(4) 0.0360(8) Uani d . 1 1
H H23A 0.7947 0.0269 0.5837 0.054 Uiso calc R 1 1
H H23B 0.8935 0.1373 0.5416 0.054 Uiso calc R 1 1
H H23C 0.8063 0.0956 0.4568 0.054 Uiso calc R 1 1
C C31 0.1604(5) 0.2900(6) 0.3489(4) 0.0508(13) Uani d . 1 1
H H31A 0.1710 0.2125 0.3963 0.076 Uiso calc R 1 1
H H31B 0.0602 0.3038 0.3315 0.076 Uiso calc R 1 1
H H31C 0.1526 0.3679 0.3986 0.076 Uiso calc R 1 1
C C32 0.2917(7) 0.3882(6) 0.1519(5) 0.0564(14) Uani d . 1 1
H H32A 0.2869 0.4658 0.2005 0.085 Uiso calc R 1 1
H H32B 0.1889 0.4024 0.1382 0.085 Uiso calc R 1 1
H H32C 0.3862 0.3741 0.0703 0.085 Uiso calc R 1 1
C C33 0.3187(7) 0.1459(6) 0.1504(6) 0.0576(14) Uani d . 1 1
H H33A 0.3317 0.0689 0.1981 0.086 Uiso calc R 1 1
H H33B 0.4130 0.1307 0.0686 0.086 Uiso calc R 1 1
H H33C 0.2157 0.1599 0.1370 0.086 Uiso calc R 1 1
C C41 0.6962(6) 0.3430(5) 0.0581(5) 0.0507(12) Uani d . 1 1
H H41A 0.6656 0.4223 0.1148 0.076 Uiso calc R 1 1
H H41B 0.6163 0.3516 0.0186 0.076 Uiso calc R 1 1
H H41C 0.8074 0.3328 -0.0075 0.076 Uiso calc R 1 1
C C42 0.8260(6) 0.2088(6) 0.1887(4) 0.0475(11) Uani d . 1 1
H H42A 0.7977 0.2872 0.2458 0.071 Uiso calc R 1 1
H H42B 0.9349 0.1998 0.1204 0.071 Uiso calc R 1 1
H H42C 0.8292 0.1303 0.2356 0.071 Uiso calc R 1 1
C C43 0.7432(7) 0.0998(5) 0.0447(4) 0.0513(12) Uani d . 1 1
H H43A 0.7428 0.0222 0.0928 0.077 Uiso calc R 1 1
H H43B 0.8544 0.0899 -0.0208 0.077 Uiso calc R 1 1
H H43C 0.6635 0.1081 0.0051 0.077 Uiso calc R 1 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'
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
P2 Pd1 P1 . 2_656 130.80(3)
P2 Pd1 P1 . . 116.70(3)
P1 Pd1 P1 2_656 . 112.50(2)
P2 Pd1 Pd1 . 2_656 172.88(3)
P1 Pd1 Pd1 2_656 2_656 56.31(2)
P1 Pd1 Pd1 . 2_656 56.19(2)
C2 P1 C1 . . 110.95(16)
C2 P1 Pd1 . 2_656 120.70(11)
C1 P1 Pd1 . 2_656 121.18(12)
C2 P1 Pd1 . . 114.53(11)
C1 P1 Pd1 . . 114.77(12)
Pd1 P1 Pd1 2_656 . 67.50(2)
C4 P2 C3 . . 111.79(16)
C4 P2 Pd1 . . 116.35(12)
C3 P2 Pd1 . . 115.50(12)
C4 P2 H2 . . 96(2)
C3 P2 H2 . . 99(2)
Pd1 P2 H2 . . 115(2)
C11 C1 C13 . . 109.2(3)
C11 C1 C12 . . 109.4(4)
C13 C1 C12 . . 108.0(3)
C11 C1 P1 . . 112.3(3)
C13 C1 P1 . . 104.7(3)
C12 C1 P1 . . 113.1(3)
C21 C2 C22 . . 109.5(3)
C21 C2 C23 . . 108.1(3)
C22 C2 C23 . . 108.3(3)
C21 C2 P1 . . 112.6(3)
C22 C2 P1 . . 113.2(3)
C23 C2 P1 . . 104.7(2)
C32 C3 C33 . . 110.2(4)
C32 C3 C31 . . 108.5(4)
C33 C3 C31 . . 107.5(4)
C32 C3 P2 . . 115.2(3)
C33 C3 P2 . . 110.3(3)
C31 C3 P2 . . 104.7(3)
C41 C4 C43 . . 109.4(4)
C41 C4 C42 . . 108.2(4)
C43 C4 C42 . . 108.0(4)
C41 C4 P2 . . 114.6(3)
C43 C4 P2 . . 111.1(3)
C42 C4 P2 . . 105.1(3)
C1 C11 H11A . . 109.5
C1 C11 H11B . . 109.5
H11A C11 H11B . . 109.5
C1 C11 H11C . . 109.5
H11A C11 H11C . . 109.5
H11B C11 H11C . . 109.5
C1 C12 H12A . . 109.5
C1 C12 H12B . . 109.5
H12A C12 H12B . . 109.5
C1 C12 H12C . . 109.5
H12A C12 H12C . . 109.5
H12B C12 H12C . . 109.5
C1 C13 H13A . . 109.5
C1 C13 H13B . . 109.5
H13A C13 H13B . . 109.5
C1 C13 H13C . . 109.5
H13A C13 H13C . . 109.5
H13B C13 H13C . . 109.5
C2 C21 H21A . . 109.5
C2 C21 H21B . . 109.5
H21A C21 H21B . . 109.5
C2 C21 H21C . . 109.5
H21A C21 H21C . . 109.5
H21B C21 H21C . . 109.5
C2 C22 H22A . . 109.5
C2 C22 H22B . . 109.5
H22A C22 H22B . . 109.5
C2 C22 H22C . . 109.5
H22A C22 H22C . . 109.5
H22B C22 H22C . . 109.5
C2 C23 H23A . . 109.5
C2 C23 H23B . . 109.5
H23A C23 H23B . . 109.5
C2 C23 H23C . . 109.5
H23A C23 H23C . . 109.5
H23B C23 H23C . . 109.5
C3 C31 H31A . . 109.5
C3 C31 H31B . . 109.5
H31A C31 H31B . . 109.5
C3 C31 H31C . . 109.5
H31A C31 H31C . . 109.5
H31B C31 H31C . . 109.5
C3 C32 H32A . . 109.5
C3 C32 H32B . . 109.5
H32A C32 H32B . . 109.5
C3 C32 H32C . . 109.5
H32A C32 H32C . . 109.5
H32B C32 H32C . . 109.5
C3 C33 H33A . . 109.5
C3 C33 H33B . . 109.5
H33A C33 H33B . . 109.5
C3 C33 H33C . . 109.5
H33A C33 H33C . . 109.5
H33B C33 H33C . . 109.5
C4 C41 H41A . . 109.5
C4 C41 H41B . . 109.5
H41A C41 H41B . . 109.5
C4 C41 H41C . . 109.5
H41A C41 H41C . . 109.5
H41B C41 H41C . . 109.5
C4 C42 H42A . . 109.5
C4 C42 H42B . . 109.5
H42A C42 H42B . . 109.5
C4 C42 H42C . . 109.5
H42A C42 H42C . . 109.5
H42B C42 H42C . . 109.5
C4 C43 H43A . . 109.5
C4 C43 H43B . . 109.5
H43A C43 H43B . . 109.5
C4 C43 H43C . . 109.5
H43A C43 H43C . . 109.5
H43B C43 H43C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Pd1 P2 . 2.2860(8)
Pd1 P1 2_656 2.3374(9)
Pd1 P1 . 2.3405(8)
Pd1 Pd1 2_656 2.5988(5)
P1 C2 . 1.896(4)
P1 C1 . 1.898(4)
P1 Pd1 2_656 2.3373(9)
P2 C4 . 1.881(4)
P2 C3 . 1.891(4)
P2 H2 . 1.21(5)
C1 C11 . 1.521(6)
C1 C13 . 1.523(5)
C1 C12 . 1.529(5)
C2 C21 . 1.526(5)
C2 C22 . 1.529(5)
C2 C23 . 1.533(5)
C3 C32 . 1.517(6)
C3 C33 . 1.528(6)
C3 C31 . 1.528(6)
C4 C41 . 1.519(6)
C4 C43 . 1.520(6)
C4 C42 . 1.532(6)
C11 H11A . 0.9800
C11 H11B . 0.9800
C11 H11C . 0.9800
C12 H12A . 0.9800
C12 H12B . 0.9800
C12 H12C . 0.9800
C13 H13A . 0.9800
C13 H13B . 0.9800
C13 H13C . 0.9800
C21 H21A . 0.9800
C21 H21B . 0.9800
C21 H21C . 0.9800
C22 H22A . 0.9800
C22 H22B . 0.9800
C22 H22C . 0.9800
C23 H23A . 0.9800
C23 H23B . 0.9800
C23 H23C . 0.9800
C31 H31A . 0.9800
C31 H31B . 0.9800
C31 H31C . 0.9800
C32 H32A . 0.9800
C32 H32B . 0.9800
C32 H32C . 0.9800
C33 H33A . 0.9800
C33 H33B . 0.9800
C33 H33C . 0.9800
C41 H41A . 0.9800
C41 H41B . 0.9800
C41 H41C . 0.9800
C42 H42A . 0.9800
C42 H42B . 0.9800
C42 H42C . 0.9800
C43 H43A . 0.9800
C43 H43B . 0.9800
C43 H43C . 0.9800
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_4
_geom_torsion
P2 Pd1 P1 C2 . . -65.64(13)
P1 Pd1 P1 C2 2_656 . 114.74(13)
Pd1 Pd1 P1 C2 2_656 . 114.74(13)
P2 Pd1 P1 C1 . . 64.42(13)
P1 Pd1 P1 C1 2_656 . -115.21(13)
Pd1 Pd1 P1 C1 2_656 . -115.21(13)
P2 Pd1 P1 Pd1 . 2_656 179.63(3)
P1 Pd1 P1 Pd1 2_656 2_656 0.0
P1 Pd1 P2 C4 2_656 . -67.41(14)
P1 Pd1 P2 C4 . . 113.05(14)
P1 Pd1 P2 C3 2_656 . 66.64(15)
P1 Pd1 P2 C3 . . -112.90(14)
C2 P1 C1 C11 . . 63.1(3)
Pd1 P1 C1 C11 2_656 . -146.4(3)
Pd1 P1 C1 C11 . . -68.7(3)
C2 P1 C1 C13 . . -178.6(2)
Pd1 P1 C1 C13 2_656 . -28.1(3)
Pd1 P1 C1 C13 . . 49.6(3)
C2 P1 C1 C12 . . -61.3(3)
Pd1 P1 C1 C12 2_656 . 89.3(3)
Pd1 P1 C1 C12 . . 167.0(3)
C1 P1 C2 C21 . . -65.6(3)
Pd1 P1 C2 C21 2_656 . 143.7(3)
Pd1 P1 C2 C21 . . 66.4(3)
C1 P1 C2 C22 . . 59.4(3)
Pd1 P1 C2 C22 2_656 . -91.3(3)
Pd1 P1 C2 C22 . . -168.7(3)
C1 P1 C2 C23 . . 177.2(2)
Pd1 P1 C2 C23 2_656 . 26.5(3)
Pd1 P1 C2 C23 . . -50.9(3)
C4 P2 C3 C32 . . -54.6(4)
Pd1 P2 C3 C32 . . 169.3(3)
C4 P2 C3 C33 . . 71.0(4)
Pd1 P2 C3 C33 . . -65.1(4)
C4 P2 C3 C31 . . -173.6(3)
Pd1 P2 C3 C31 . . 50.3(3)
C3 P2 C4 C41 . . 56.2(4)
Pd1 P2 C4 C41 . . -168.2(3)
C3 P2 C4 C43 . . -68.6(4)
Pd1 P2 C4 C43 . . 67.1(3)
C3 P2 C4 C42 . . 174.9(3)
Pd1 P2 C4 C42 . . -49.5(3)
