#------------------------------------------------------------------------------
#$Date: 2016-03-25 11:27:31 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179791 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/87/7008788.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_7008788
loop_
_publ_author_name
'Chang, Xiaohong'
'Lee, Kyung-Eun'
'Il Jeon, Sang'
'Kim, Yong-Joo'
'Lee, H.-K.'
'Lee, Soon W.'
_publ_section_title
;
 Bis(isothiocyanato)bis(phosphine) complexes of group 10 metals:
 reactivity toward organic isocyanides
;
_journal_issue                   23
_journal_name_full               'Dalton Transactions'
_journal_page_first              3722
_journal_paper_doi               10.1039/b508134c
_journal_year                    2005
_chemical_formula_sum            'C20 H42 N2 P2 Pd S2'
_chemical_formula_weight         543.02
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.676(9)
_cell_angle_beta                 86.225(9)
_cell_angle_gamma                87.750(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7268(9)
_cell_length_b                   9.3401(12)
_cell_length_c                   17.114(2)
_cell_measurement_reflns_used    27
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.48
_cell_measurement_theta_min      4.94
_cell_volume                     1390.8(3)
_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      293(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω 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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            5192
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.18
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.940
_exptl_absorpt_correction_T_max  0.8930
_exptl_absorpt_correction_T_min  0.6359
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            'YELLOW '
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'BLOCK '
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         4843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0496
_refine_ls_R_factor_gt           0.0343
_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)+(0.0378P)²+0.6258P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0894
_reflns_number_gt                3783
_reflns_number_total             4843
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b508134c.txt
_cod_data_source_block           isomers
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        1390.9(3)
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7008788
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 0.05224(12) Uani 1 2 d S . .
S1 S 0.19903(17) 0.18558(14) -0.13450(9) 0.1028(4) Uani 1 1 d . . .
P1 P 0.33589(11) 0.69915(10) -0.01450(5) 0.0553(2) Uani 1 1 d . . .
N1 N 0.3700(4) 0.3741(4) -0.0583(2) 0.0719(9) Uani 1 1 d . . .
C1 C 0.2994(4) 0.2966(4) -0.0897(2) 0.0624(9) Uani 1 1 d . . .
C2 C 0.2868(5) 0.7880(4) 0.0783(2) 0.0667(10) Uani 1 1 d . . .
H2A H 0.3772 0.8333 0.0951 0.080 Uiso 1 1 calc R . .
H2B H 0.2091 0.8629 0.0707 0.080 Uiso 1 1 calc R . .
C3 C 0.2267(6) 0.6866(5) 0.1436(2) 0.0856(13) Uani 1 1 d . . .
H3A H 0.1321 0.6466 0.1285 0.103 Uiso 1 1 calc R . .
H3B H 0.3013 0.6080 0.1489 0.103 Uiso 1 1 calc R . .
C4 C 0.1971(7) 0.7589(6) 0.2208(3) 0.1157(18) Uani 1 1 d . . .
H4A H 0.1594 0.6909 0.2590 0.174 Uiso 1 1 calc R . .
H4B H 0.1219 0.8358 0.2163 0.174 Uiso 1 1 calc R . .
H4C H 0.2909 0.7964 0.2369 0.174 Uiso 1 1 calc R . .
C5 C 0.4272(4) 0.8326(4) -0.0770(2) 0.0610(9) Uani 1 1 d . . .
H5A H 0.3594 0.9174 -0.0780 0.073 Uiso 1 1 calc R . .
H5B H 0.5210 0.8596 -0.0545 0.073 Uiso 1 1 calc R . .
C6 C 0.4661(5) 0.7829(5) -0.1607(2) 0.0800(12) Uani 1 1 d . . .
H6A H 0.5350 0.6989 -0.1599 0.096 Uiso 1 1 calc R . .
H6B H 0.3727 0.7552 -0.1833 0.096 Uiso 1 1 calc R . .
C7 C 0.5404(6) 0.8959(5) -0.2117(3) 0.0944(14) Uani 1 1 d . . .
H7A H 0.5625 0.8588 -0.2636 0.142 Uiso 1 1 calc R . .
H7B H 0.6342 0.9224 -0.1903 0.142 Uiso 1 1 calc R . .
H7C H 0.4719 0.9786 -0.2138 0.142 Uiso 1 1 calc R . .
C8 C 0.1546(4) 0.6615(4) -0.0556(2) 0.0648(9) Uani 1 1 d . . .
H8A H 0.1775 0.6106 -0.1045 0.078 Uiso 1 1 calc R . .
H8B H 0.0996 0.5972 -0.0201 0.078 Uiso 1 1 calc R . .
C9 C 0.0480(5) 0.7884(5) -0.0714(3) 0.0825(12) Uani 1 1 d . . .
H9A H 0.0206 0.8384 -0.0226 0.099 Uiso 1 1 calc R . .
H9B H 0.1014 0.8542 -0.1066 0.099 Uiso 1 1 calc R . .
C10 C -0.0964(5) 0.7450(6) -0.1069(3) 0.1049(17) Uani 1 1 d . . .
H10A H -0.1600 0.8288 -0.1161 0.157 Uiso 1 1 calc R . .
H10B H -0.1512 0.6818 -0.0716 0.157 Uiso 1 1 calc R . .
H10C H -0.0700 0.6967 -0.1556 0.157 Uiso 1 1 calc R . .
Pd2 Pd 0.5000 0.0000 -0.5000 0.04984(12) Uani 1 2 d S . .
S2 S 0.67242(12) 0.08724(13) -0.41462(6) 0.0758(3) Uani 1 1 d . . .
P2 P 0.30263(11) 0.16428(10) -0.45602(5) 0.0557(2) Uani 1 1 d . . .
N2 N 0.7850(7) 0.3214(6) -0.4995(4) 0.148(2) Uani 1 1 d . . .
C11 C 0.7359(6) 0.2246(6) -0.4662(3) 0.0916(15) Uani 1 1 d . . .
C12 C 0.1425(4) 0.0688(4) -0.4101(2) 0.0633(9) Uani 1 1 d . . .
H12A H 0.0608 0.1375 -0.3933 0.076 Uiso 1 1 calc R . .
H12B H 0.1029 0.0061 -0.4483 0.076 Uiso 1 1 calc R . .
C13 C 0.1883(5) -0.0201(5) -0.3396(2) 0.0796(12) Uani 1 1 d . . .
H13A H 0.2767 -0.0819 -0.3554 0.095 Uiso 1 1 calc R . .
H13B H 0.2188 0.0438 -0.2995 0.095 Uiso 1 1 calc R . .
C14 C 0.0637(6) -0.1095(6) -0.3058(3) 0.1062(16) Uani 1 1 d . . .
H14A H 0.0994 -0.1626 -0.2619 0.159 Uiso 1 1 calc R . .
H14B H 0.0345 -0.1749 -0.3448 0.159 Uiso 1 1 calc R . .
H14C H -0.0234 -0.0490 -0.2888 0.159 Uiso 1 1 calc R . .
C15 C 0.3488(4) 0.2985(4) -0.3847(2) 0.0668(10) Uani 1 1 d . . .
H15A H 0.3955 0.2494 -0.3417 0.080 Uiso 1 1 calc R . .
H15B H 0.4252 0.3597 -0.4094 0.080 Uiso 1 1 calc R . .
C16 C 0.2154(6) 0.3929(5) -0.3513(3) 0.0915(14) Uani 1 1 d . . .
H16A H 0.1394 0.3329 -0.3251 0.110 Uiso 1 1 calc R . .
H16B H 0.1674 0.4423 -0.3938 0.110 Uiso 1 1 calc R . .
C17 C 0.2639(7) 0.5028(5) -0.2935(3) 0.1129(18) Uani 1 1 d . . .
H17A H 0.1756 0.5599 -0.2744 0.169 Uiso 1 1 calc R . .
H17B H 0.3379 0.5636 -0.3193 0.169 Uiso 1 1 calc R . .
H17C H 0.3089 0.4545 -0.2504 0.169 Uiso 1 1 calc R . .
C18 C 0.2218(5) 0.2663(4) -0.5356(2) 0.0692(10) Uani 1 1 d . . .
H18A H 0.1707 0.2012 -0.5684 0.083 Uiso 1 1 calc R . .
H18B H 0.1445 0.3347 -0.5135 0.083 Uiso 1 1 calc R . .
C19 C 0.3375(6) 0.3459(5) -0.5861(3) 0.0897(13) Uani 1 1 d . . .
H19A H 0.4189 0.2790 -0.6055 0.108 Uiso 1 1 calc R . .
H19B H 0.3830 0.4167 -0.5545 0.108 Uiso 1 1 calc R . .
C20 C 0.2684(7) 0.4199(6) -0.6547(3) 0.120(2) Uani 1 1 d . . .
H20A H 0.3470 0.4686 -0.6851 0.180 Uiso 1 1 calc R . .
H20B H 0.1895 0.4881 -0.6360 0.180 Uiso 1 1 calc R . .
H20C H 0.2248 0.3502 -0.6868 0.180 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'
N N 0.0061 0.0033 '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'
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
N1 Pd1 N1 180.00(17) . 2_665 ?
N1 Pd1 P1 87.16(10) . 2_665 ?
N1 Pd1 P1 92.84(10) 2_665 2_665 ?
N1 Pd1 P1 92.84(10) . . ?
N1 Pd1 P1 87.16(10) 2_665 . ?
P1 Pd1 P1 180.00(5) 2_665 . ?
C5 P1 C2 105.55(17) . . ?
C5 P1 C8 106.96(18) . . ?
C2 P1 C8 106.34(19) . . ?
C5 P1 Pd1 110.94(13) . . ?
C2 P1 Pd1 111.67(13) . . ?
C8 P1 Pd1 114.81(13) . . ?
C1 N1 Pd1 176.5(3) . . ?
N1 C1 S1 179.8(4) . . ?
C3 C2 P1 113.7(3) . . ?
C4 C3 C2 113.2(4) . . ?
C6 C5 P1 114.0(3) . . ?
C7 C6 C5 113.0(4) . . ?
C9 C8 P1 117.1(3) . . ?
C10 C9 C8 112.4(4) . . ?
S2 Pd2 S2 180.0 2_654 . ?
S2 Pd2 P2 92.93(4) 2_654 2_654 ?
S2 Pd2 P2 87.07(4) . 2_654 ?
S2 Pd2 P2 87.07(4) 2_654 . ?
S2 Pd2 P2 92.93(4) . . ?
P2 Pd2 P2 180.00(4) 2_654 . ?
C11 S2 Pd2 99.80(18) . . ?
C12 P2 C18 105.08(18) . . ?
C12 P2 C15 105.62(18) . . ?
C18 P2 C15 105.08(19) . . ?
C12 P2 Pd2 109.84(13) . . ?
C18 P2 Pd2 112.77(13) . . ?
C15 P2 Pd2 117.51(13) . . ?
N2 C11 S2 176.7(6) . . ?
C13 C12 P2 112.5(3) . . ?
C14 C13 C12 113.5(4) . . ?
C16 C15 P2 116.2(3) . . ?
C15 C16 C17 112.8(4) . . ?
C19 C18 P2 114.4(3) . . ?
C18 C19 C20 112.8(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 N1 1.983(3) . ?
Pd1 N1 1.983(3) 2_665 ?
Pd1 P1 2.3248(10) 2_665 ?
Pd1 P1 2.3248(10) . ?
S1 C1 1.612(4) . ?
P1 C5 1.812(4) . ?
P1 C2 1.815(4) . ?
P1 C8 1.821(4) . ?
N1 C1 1.130(5) . ?
C2 C3 1.540(6) . ?
C3 C4 1.490(6) . ?
C5 C6 1.520(5) . ?
C6 C7 1.506(6) . ?
C8 C9 1.512(5) . ?
C9 C10 1.504(6) . ?
Pd2 S2 2.3371(10) 2_654 ?
Pd2 S2 2.3371(10) . ?
Pd2 P2 2.3500(10) 2_654 ?
Pd2 P2 2.3500(10) . ?
S2 C11 1.646(6) . ?
P2 C12 1.820(4) . ?
P2 C18 1.823(4) . ?
P2 C15 1.829(4) . ?
N2 C11 1.148(6) . ?
C12 C13 1.526(5) . ?
C13 C14 1.482(6) . ?
C15 C16 1.516(5) . ?
C16 C17 1.521(6) . ?
C18 C19 1.502(6) . ?
C19 C20 1.507(6) . ?
