#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:57:32 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179163 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/24/4312426.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_4312426
loop_
_publ_author_name
'Zuzanna T. Cygan'
'Jeff W. Kampf'
'Mark M. Banaszak Holl'
_publ_section_title
;
 Reactions of Palladium Germylene Complexes: Formation of Sulfide Bridges
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7219
_journal_page_last               7226
_journal_paper_doi               10.1021/ic034613z
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C42 H108 Ge2 N4 P2 Pd2 S2 Si8'
_chemical_formula_weight         1378.08
_chemical_name_systematic
;
 ?
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.478(2)
_cell_angle_beta                 112.702(2)
_cell_angle_gamma                90.475(2)
_cell_formula_units_Z            1
_cell_length_a                   11.2870(13)
_cell_length_b                   12.7506(15)
_cell_length_c                   13.1569(15)
_cell_measurement_reflns_used    7856
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      3.42
_cell_volume                     1670.2(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      158(2)
_diffrn_detector_area_resol_mean 0.75
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0187
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            21115
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         3.42
_exptl_absorpt_coefficient_mu    1.705
_exptl_absorpt_correction_T_max  0.898
_exptl_absorpt_correction_T_min  0.726
_exptl_absorpt_correction_type   multi.scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             718
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     496
_refine_ls_number_reflns         8130
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0214
_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)+(0.0319P)²+0.6641P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0544
_refine_ls_wR_factor_ref         0.0566
_reflns_number_gt                7375
_reflns_number_total             8130
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034613zsi20030603_125230_4.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4312426
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 0.390192(11) -0.013640(9) -0.111266(9) 0.01533(4) Uani 1 1 d . . .
Ge1 Ge 0.628397(14) 0.190932(12) 0.232881(13) 0.01451(4) Uani 1 1 d . . .
S1 S 0.46722(4) 0.15350(3) 0.06023(3) 0.02289(8) Uani 1 1 d . . .
P1 P 0.25626(4) 0.08418(3) -0.21802(3) 0.01855(8) Uani 1 1 d . . .
Si1 Si 0.42086(5) 0.16487(4) 0.32690(4) 0.02700(10) Uani 1 1 d . . .
Si2 Si 0.69136(5) 0.27597(4) 0.50027(4) 0.02228(9) Uani 1 1 d . . .
Si3 Si 0.67882(4) 0.43397(4) 0.24213(4) 0.02000(9) Uani 1 1 d . . .
Si4 Si 0.87295(4) 0.27940(4) 0.21508(4) 0.02008(9) Uani 1 1 d . . .
N1 N 0.58127(13) 0.21437(11) 0.35734(11) 0.0204(3) Uani 1 1 d . . .
N2 N 0.74038(12) 0.30902(10) 0.25164(11) 0.0178(2) Uani 1 1 d . . .
C1 C 0.3942(3) 0.1761(3) 0.4614(2) 0.0585(8) Uani 1 1 d . . .
H1A H 0.436(3) 0.129(3) 0.502(3) 0.072(10) Uiso 1 1 d . . .
H1B H 0.306(4) 0.156(3) 0.436(3) 0.083(10) Uiso 1 1 d . . .
H1C H 0.416(3) 0.249(3) 0.515(3) 0.080(10) Uiso 1 1 d . . .
C2 C 0.3794(2) 0.01688(18) 0.2457(2) 0.0397(5) Uani 1 1 d . . .
H2A H 0.383(3) 0.003(2) 0.172(3) 0.067(9) Uiso 1 1 d . . .
H2B H 0.291(3) -0.009(2) 0.234(2) 0.062(8) Uiso 1 1 d . . .
H2C H 0.434(3) -0.021(2) 0.285(3) 0.061(9) Uiso 1 1 d . . .
C3 C 0.2983(2) 0.2439(2) 0.2479(2) 0.0408(5) Uani 1 1 d . . .
H3A H 0.308(3) 0.312(3) 0.292(3) 0.060(8) Uiso 1 1 d . . .
H3B H 0.209(3) 0.210(2) 0.227(2) 0.050(7) Uiso 1 1 d . . .
H3C H 0.305(3) 0.247(2) 0.179(2) 0.053(7) Uiso 1 1 d . . .
C4 C 0.7059(3) 0.1853(2) 0.5952(2) 0.0418(5) Uani 1 1 d . . .
H4A H 0.658(3) 0.196(3) 0.635(3) 0.078(10) Uiso 1 1 d . . .
H4B H 0.785(4) 0.197(3) 0.648(3) 0.094(12) Uiso 1 1 d . . .
H4C H 0.685(3) 0.115(3) 0.559(3) 0.085(11) Uiso 1 1 d . . .
C5 C 0.6437(2) 0.41006(19) 0.56230(19) 0.0390(5) Uani 1 1 d . . .
H5A H 0.651(3) 0.467(3) 0.525(3) 0.071(9) Uiso 1 1 d . . .
H5B H 0.701(3) 0.440(2) 0.632(3) 0.059(8) Uiso 1 1 d . . .
H5C H 0.557(3) 0.404(2) 0.556(3) 0.066(9) Uiso 1 1 d . . .
C6 C 0.86052(18) 0.30453(16) 0.51617(16) 0.0282(4) Uani 1 1 d . . .
H6A H 0.887(2) 0.238(2) 0.486(2) 0.036(6) Uiso 1 1 d . . .
H6B H 0.911(2) 0.336(2) 0.600(2) 0.042(6) Uiso 1 1 d . . .
H6C H 0.869(2) 0.355(2) 0.481(2) 0.039(6) Uiso 1 1 d . . .
C7 C 0.6637(2) 0.46052(17) 0.10472(17) 0.0310(4) Uani 1 1 d . . .
H7A H 0.741(3) 0.470(2) 0.099(2) 0.057(8) Uiso 1 1 d . . .
H7B H 0.623(2) 0.5268(19) 0.1020(19) 0.037(6) Uiso 1 1 d . . .
H7C H 0.613(3) 0.403(3) 0.048(3) 0.061(8) Uiso 1 1 d . . .
C8 C 0.51291(19) 0.43573(15) 0.24060(19) 0.0294(4) Uani 1 1 d . . .
H8A H 0.451(2) 0.390(2) 0.177(2) 0.041(6) Uiso 1 1 d . . .
H8B H 0.489(2) 0.511(2) 0.242(2) 0.042(6) Uiso 1 1 d . . .
H8C H 0.509(2) 0.4186(19) 0.307(2) 0.040(6) Uiso 1 1 d . . .
C9 C 0.7831(2) 0.55081(16) 0.36835(18) 0.0338(4) Uani 1 1 d . . .
H9A H 0.796(3) 0.545(2) 0.445(3) 0.062(8) Uiso 1 1 d . . .
H9B H 0.740(3) 0.608(3) 0.369(3) 0.073(10) Uiso 1 1 d . . .
H9C H 0.858(3) 0.570(3) 0.367(3) 0.072(9) Uiso 1 1 d . . .
C10 C 0.8207(2) 0.20733(18) 0.05847(17) 0.0328(4) Uani 1 1 d . . .
H10A H 0.767(3) 0.137(2) 0.039(2) 0.054(7) Uiso 1 1 d . . .
H10B H 0.892(3) 0.190(2) 0.041(2) 0.054(7) Uiso 1 1 d . . .
H10C H 0.777(3) 0.250(2) 0.010(2) 0.058(8) Uiso 1 1 d . . .
C11 C 0.97347(18) 0.19155(17) 0.29968(19) 0.0302(4) Uani 1 1 d . . .
H11A H 1.030(3) 0.235(2) 0.377(2) 0.053(7) Uiso 1 1 d . . .
H11B H 1.027(2) 0.158(2) 0.262(2) 0.041(6) Uiso 1 1 d . . .
H11C H 0.926(2) 0.134(2) 0.307(2) 0.039(6) Uiso 1 1 d . . .
C12 C 0.98564(19) 0.40572(17) 0.2545(2) 0.0317(4) Uani 1 1 d . . .
H12A H 0.946(2) 0.463(2) 0.217(2) 0.045(7) Uiso 1 1 d . . .
H12B H 1.054(2) 0.382(2) 0.232(2) 0.045(7) Uiso 1 1 d . . .
H12C H 1.019(2) 0.436(2) 0.332(2) 0.046(7) Uiso 1 1 d . . .
C13 C 0.21710(17) 0.03313(14) -0.37270(14) 0.0228(3) Uani 1 1 d . . .
H13A H 0.300(2) 0.0278(19) -0.382(2) 0.042(6) Uiso 1 1 d . . .
H13B H 0.169(2) -0.0422(18) -0.3984(18) 0.027(5) Uiso 1 1 d . . .
C14 C 0.1371(2) 0.10150(17) -0.44703(16) 0.0296(4) Uani 1 1 d . . .
H14A H 0.055(3) 0.108(2) -0.440(2) 0.049(7) Uiso 1 1 d . . .
H14B H 0.118(2) 0.066(2) -0.527(2) 0.044(6) Uiso 1 1 d . . .
H14C H 0.183(2) 0.168(2) -0.431(2) 0.044(7) Uiso 1 1 d . . .
C15 C 0.32532(18) 0.22717(14) -0.18086(15) 0.0253(3) Uani 1 1 d . . .
H15A H 0.264(2) 0.2645(18) -0.224(2) 0.035(6) Uiso 1 1 d . . .
H15B H 0.338(2) 0.2606(17) -0.1024(19) 0.028(5) Uiso 1 1 d . . .
C16 C 0.4509(2) 0.23851(17) -0.19634(18) 0.0325(4) Uani 1 1 d . . .
H16A H 0.515(2) 0.204(2) -0.149(2) 0.040(6) Uiso 1 1 d . . .
H16B H 0.487(2) 0.314(2) -0.172(2) 0.044(7) Uiso 1 1 d . . .
H16C H 0.441(2) 0.208(2) -0.273(2) 0.048(7) Uiso 1 1 d . . .
C17 C 0.09783(18) 0.10160(16) -0.21043(16) 0.0274(4) Uani 1 1 d . . .
H17A H 0.074(2) 0.169(2) -0.226(2) 0.046(7) Uiso 1 1 d . . .
H17B H 0.036(2) 0.039(2) -0.270(2) 0.038(6) Uiso 1 1 d . . .
C18 C 0.0985(2) 0.1062(2) -0.0937(2) 0.0422(5) Uani 1 1 d . . .
H18A H 0.126(3) 0.041(3) -0.072(3) 0.064(9) Uiso 1 1 d . . .
H18B H 0.013(3) 0.109(2) -0.095(2) 0.058(8) Uiso 1 1 d . . .
H18C H 0.156(3) 0.167(2) -0.037(2) 0.052(7) Uiso 1 1 d . . .
C19 C 0.8751(4) 0.4586(3) -0.0765(3) 0.0746(9) Uani 1 1 d . . .
H19 H 0.790(3) 0.431(3) -0.126(3) 0.076(11) Uiso 1 1 d . . .
C20 C 0.9038(4) 0.5660(3) -0.0116(4) 0.0777(11) Uani 1 1 d . . .
H20 H 0.838(4) 0.615(3) -0.020(3) 0.096(12) Uiso 1 1 d . . .
C21 C 1.0281(5) 0.6072(3) 0.0639(4) 0.0760(10) Uani 1 1 d . . .
H21 H 1.055(4) 0.672(3) 0.106(3) 0.088(13) Uiso 1 1 d . . .
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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
P1 Pd1 Ge1 107.971(14) . 2_655 ?
P1 Pd1 S1 160.487(15) . 2_655 ?
Ge1 Pd1 S1 54.784(12) 2_655 2_655 ?
P1 Pd1 S1 89.719(16) . . ?
Ge1 Pd1 S1 162.086(11) 2_655 . ?
S1 Pd1 S1 107.304(14) 2_655 . ?
N2 Ge1 N1 111.00(6) . . ?
N2 Ge1 S1 108.76(4) . . ?
N1 Ge1 S1 116.15(4) . . ?
N2 Ge1 Pd1 124.06(4) . 2_655 ?
N1 Ge1 Pd1 121.33(4) . 2_655 ?
S1 Ge1 Pd1 65.265(12) . 2_655 ?
Ge1 S1 Pd1 59.951(11) . 2_655 ?
Ge1 S1 Pd1 132.646(18) . . ?
Pd1 S1 Pd1 72.695(13) 2_655 . ?
C13 P1 C15 102.78(8) . . ?
C13 P1 C17 104.00(8) . . ?
C15 P1 C17 101.67(9) . . ?
C13 P1 Pd1 114.43(6) . . ?
C15 P1 Pd1 113.36(6) . . ?
C17 P1 Pd1 118.63(6) . . ?
N1 Si1 C2 112.13(9) . . ?
N1 Si1 C3 112.95(9) . . ?
C2 Si1 C3 109.49(12) . . ?
N1 Si1 C1 112.14(10) . . ?
C2 Si1 C1 104.91(14) . . ?
C3 Si1 C1 104.66(14) . . ?
N1 Si2 C6 113.87(7) . . ?
N1 Si2 C5 110.78(9) . . ?
C6 Si2 C5 106.60(10) . . ?
N1 Si2 C4 112.33(10) . . ?
C6 Si2 C4 103.53(11) . . ?
C5 Si2 C4 109.33(12) . . ?
N2 Si3 C8 112.91(7) . . ?
N2 Si3 C7 110.91(8) . . ?
C8 Si3 C7 105.40(10) . . ?
N2 Si3 C9 111.13(8) . . ?
C8 Si3 C9 106.19(10) . . ?
C7 Si3 C9 110.05(10) . . ?
N2 Si4 C10 111.89(8) . . ?
N2 Si4 C12 111.93(8) . . ?
C10 Si4 C12 109.07(10) . . ?
N2 Si4 C11 110.32(7) . . ?
C10 Si4 C11 108.69(10) . . ?
C12 Si4 C11 104.65(9) . . ?
Si2 N1 Si1 120.44(7) . . ?
Si2 N1 Ge1 122.55(8) . . ?
Si1 N1 Ge1 116.92(7) . . ?
Si4 N2 Si3 118.38(7) . . ?
Si4 N2 Ge1 117.36(7) . . ?
Si3 N2 Ge1 118.39(7) . . ?
C14 C13 P1 116.58(13) . . ?
C16 C15 P1 113.67(13) . . ?
C18 C17 P1 113.64(14) . . ?
C20 C19 C21 119.3(4) . 2_765 ?
C19 C20 C21 120.1(3) . . ?
C20 C21 C19 120.6(4) . 2_765 ?
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 P1 2.2674(4) . ?
Pd1 Ge1 2.3488(3) 2_655 ?
Pd1 S1 2.4645(4) 2_655 ?
Pd1 S1 2.5055(5) . ?
Ge1 N2 1.8587(13) . ?
Ge1 N1 1.8621(13) . ?
Ge1 S1 2.2169(5) . ?
Ge1 Pd1 2.3488(3) 2_655 ?
S1 Pd1 2.4645(4) 2_655 ?
P1 C13 1.8316(17) . ?
P1 C15 1.8378(18) . ?
P1 C17 1.8411(18) . ?
Si1 N1 1.7672(14) . ?
Si1 C2 1.856(2) . ?
Si1 C3 1.866(2) . ?
Si1 C1 1.876(2) . ?
Si2 N1 1.7576(14) . ?
Si2 C6 1.860(2) . ?
Si2 C5 1.868(2) . ?
Si2 C4 1.880(2) . ?
Si3 N2 1.7591(14) . ?
Si3 C8 1.8654(19) . ?
Si3 C7 1.8713(19) . ?
Si3 C9 1.872(2) . ?
Si4 N2 1.7553(13) . ?
Si4 C10 1.866(2) . ?
Si4 C12 1.8687(19) . ?
Si4 C11 1.8689(19) . ?
C13 C14 1.523(2) . ?
C15 C16 1.519(3) . ?
C17 C18 1.518(3) . ?
C19 C20 1.365(5) . ?
C19 C21 1.369(5) 2_765 ?
C20 C21 1.366(6) . ?
C21 C19 1.369(5) 2_765 ?
