#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/11/7051164.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_7051164
loop_
_publ_author_name
'Marek Necas'
'Mark R. St J. Foreman'
'Jaromír Marek'
'J. Derek Woollins'
'Josef Novosad'
_publ_section_title
;
 New mixed-donor unsymmetrical P--N--P ligands and their palladium(II)
 complexes
;
_journal_issue                   10
_journal_name_full               'New J. Chem.'
_journal_page_first              1256
_journal_page_last               1263
_journal_paper_doi               10.1039/b103501k
_journal_volume                  25
_journal_year                    2001
_chemical_formula_moiety         '[Ph2P(S)-N-P(S)(OPh)2]2Pd'
_chemical_formula_sum            'C24 H20 N O2 P2 Pd0.5 S2'
_chemical_formula_weight         533.67
_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                108.78(3)
_cell_angle_beta                 105.07(3)
_cell_angle_gamma                95.40(3)
_cell_formula_units_Z            2
_cell_length_a                   10.698(2)
_cell_length_b                   10.890(2)
_cell_length_c                   11.220(2)
_cell_measurement_temperature    130(2)
_cell_volume                     1172.2(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.0291
_diffrn_reflns_av_sigmaI/netI    0.0471
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4349
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.80
_exptl_absorpt_coefficient_mu    0.757
_exptl_absorpt_correction_T_max  0.9631
_exptl_absorpt_correction_T_min  0.6193
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.777
_refine_diff_density_min         -1.286
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4110
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0621P)²+3.6876P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1255
_reflns_number_gt                3361
_reflns_number_total             4110
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b103501k.txt
_cod_data_source_block           13.cif
_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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+3.6876P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0621P)^2^+3.6876P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1172.2(4)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C24 H20 N O2 P2 Pd0.50 S2'
_cod_database_code               7051164
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.0000 0.0000 0.0000 0.01851(15) Uani 1 d S . .
S1 S -0.14514(11) -0.20372(10) -0.10290(11) 0.0244(3) Uani 1 d . . .
S2 S 0.18116(11) -0.10531(11) 0.02573(11) 0.0247(3) Uani 1 d . . .
P1 P -0.10049(11) -0.27891(11) -0.27151(11) 0.0224(3) Uani 1 d . . .
P2 P 0.18096(11) -0.18099(11) -0.16285(11) 0.0210(3) Uani 1 d . . .
O2 O -0.1706(3) -0.4314(3) -0.3363(3) 0.0261(7) Uani 1 d . . .
O1 O -0.1743(3) -0.2262(3) -0.3817(3) 0.0263(7) Uani 1 d . . .
C13 C 0.2962(4) -0.2910(4) -0.1644(4) 0.0232(9) Uani 1 d . . .
C2 C -0.3983(5) -0.3439(5) -0.5025(5) 0.0303(10) Uani 1 d . . .
C7 C -0.1084(4) -0.5281(4) -0.2996(5) 0.0270(10) Uani 1 d . . .
C1 C -0.3114(4) -0.2284(5) -0.4158(4) 0.0271(10) Uani 1 d . . .
N1 N 0.0452(4) -0.2650(4) -0.2719(4) 0.0261(8) Uani 1 d . . .
C3 C -0.5312(5) -0.3416(5) -0.5444(5) 0.0326(11) Uani 1 d . . .
C6 C -0.3530(5) -0.1122(5) -0.3699(5) 0.0321(11) Uani 1 d . . .
C4 C -0.5752(5) -0.2258(5) -0.5016(5) 0.0372(12) Uani 1 d . . .
C16 C 0.4652(5) -0.4677(5) -0.1599(5) 0.0343(11) Uani 1 d . . .
C5 C -0.4884(6) -0.1123(5) -0.4151(5) 0.0409(13) Uani 1 d . . .
C18 C 0.2641(5) -0.4025(4) -0.1337(5) 0.0287(10) Uani 1 d . . .
C15 C 0.4964(5) -0.3589(5) -0.1915(5) 0.0330(11) Uani 1 d . . .
C17 C 0.3492(5) -0.4906(5) -0.1324(5) 0.0337(11) Uani 1 d . . .
C14 C 0.4123(4) -0.2705(4) -0.1940(4) 0.0254(9) Uani 1 d . . .
C19 C 0.2399(4) -0.0502(4) -0.2121(4) 0.0251(9) Uani 1 d . . .
C20 C 0.1805(5) -0.0516(5) -0.3384(5) 0.0295(10) Uani 1 d . . .
C24 C 0.3452(5) 0.0518(4) -0.1257(4) 0.0265(10) Uani 1 d . . .
C8 C -0.0413(5) -0.5982(5) -0.3803(5) 0.0316(11) Uani 1 d . . .
C22 C 0.3291(5) 0.1490(5) -0.2918(5) 0.0336(11) Uani 1 d . . .
C9 C 0.0189(6) -0.6948(5) -0.3444(5) 0.0405(12) Uani 1 d . . .
C23 C 0.3900(5) 0.1513(5) -0.1651(5) 0.0348(11) Uani 1 d . . .
C12 C -0.1201(5) -0.5513(5) -0.1900(5) 0.0341(11) Uani 1 d . . .
C21 C 0.2263(5) 0.0499(5) -0.3761(5) 0.0359(11) Uani 1 d . . .
C10 C 0.0096(6) -0.7200(5) -0.2350(5) 0.0419(13) Uani 1 d . . .
C11 C -0.0594(6) -0.6504(5) -0.1571(5) 0.0427(13) Uani 1 d . . .
H6 H -0.2812 -0.0296 -0.3113 0.050 Uiso 1 d . . .
H18 H 0.1731 -0.4204 -0.1122 0.050 Uiso 1 d . . .
H17 H 0.3208 -0.5741 -0.1168 0.050 Uiso 1 d . . .
H24 H 0.3868 0.0617 -0.0295 0.050 Uiso 1 d . . .
H22 H 0.3716 0.2180 -0.3148 0.050 Uiso 1 d . . .
H12 H -0.1750 -0.5058 -0.1391 0.050 Uiso 1 d . . .
H8 H -0.0367 -0.5780 -0.4695 0.050 Uiso 1 d . . .
H3 H -0.6044 -0.4294 -0.6020 0.050 Uiso 1 d . . .
H5 H -0.5029 -0.0199 -0.3851 0.050 Uiso 1 d . . .
H2 H -0.3707 -0.4369 -0.5416 0.050 Uiso 1 d . . .
H15 H 0.5863 -0.3403 -0.2052 0.050 Uiso 1 d . . .
H23 H 0.4692 0.2289 -0.1037 0.050 Uiso 1 d . . .
H14 H 0.4320 -0.1965 -0.2158 0.050 Uiso 1 d . . .
H20 H 0.0981 -0.1230 -0.3930 0.050 Uiso 1 d . . .
H21 H 0.1763 0.0426 -0.4729 0.050 Uiso 1 d . . .
H9 H 0.0806 -0.7392 -0.3984 0.050 Uiso 1 d . . .
H4 H -0.6796 -0.2246 -0.5257 0.050 Uiso 1 d . . .
H16 H 0.5218 -0.5300 -0.1788 0.050 Uiso 1 d . . .
H10 H 0.0545 -0.7949 -0.2161 0.050 Uiso 1 d . . .
H11 H -0.0645 -0.6459 -0.0618 0.050 Uiso 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'
O O 0.0106 0.0060 '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
S1 Pd1 S1 180.0 . 2 ?
S1 Pd1 S2 89.13(5) . 2 ?
S1 Pd1 S2 90.87(5) 2 2 ?
S1 Pd1 S2 90.87(5) . . ?
S1 Pd1 S2 89.13(5) 2 . ?
S2 Pd1 S2 180.0 2 . ?
P1 S1 Pd1 101.88(6) . . ?
P2 S2 Pd1 100.31(6) . . ?
N1 P1 O1 105.32(19) . . ?
N1 P1 O2 109.70(19) . . ?
O1 P1 O2 100.49(17) . . ?
N1 P1 S1 120.92(15) . . ?
O1 P1 S1 112.04(14) . . ?
O2 P1 S1 106.51(14) . . ?
N1 P2 C13 106.6(2) . . ?
N1 P2 C19 108.3(2) . . ?
C13 P2 C19 108.7(2) . . ?
N1 P2 S2 117.63(15) . . ?
C13 P2 S2 105.67(15) . . ?
C19 P2 S2 109.58(16) . . ?
C7 O2 P1 121.0(3) . . ?
C1 O1 P1 122.6(3) . . ?
C14 C13 C18 119.6(4) . . ?
C14 C13 P2 123.4(3) . . ?
C18 C13 P2 117.0(3) . . ?
C3 C2 C1 118.9(4) . . ?
C12 C7 C8 123.1(4) . . ?
C12 C7 O2 119.3(4) . . ?
C8 C7 O2 117.6(4) . . ?
C6 C1 C2 122.0(4) . . ?
C6 C1 O1 118.2(4) . . ?
C2 C1 O1 119.6(4) . . ?
P1 N1 P2 132.9(2) . . ?
C4 C3 C2 120.1(5) . . ?
C1 C6 C5 117.8(5) . . ?
C5 C4 C3 120.4(5) . . ?
C17 C16 C15 120.5(4) . . ?
C4 C5 C6 120.6(5) . . ?
C17 C18 C13 119.8(4) . . ?
C16 C15 C14 120.3(4) . . ?
C16 C17 C18 119.9(4) . . ?
C15 C14 C13 119.9(4) . . ?
C20 C19 C24 119.4(4) . . ?
C20 C19 P2 119.6(3) . . ?
C24 C19 P2 121.0(3) . . ?
C19 C20 C21 119.4(4) . . ?
C23 C24 C19 120.4(4) . . ?
C7 C8 C9 117.3(4) . . ?
C21 C22 C23 120.2(4) . . ?
C10 C9 C8 121.0(5) . . ?
C24 C23 C22 119.5(5) . . ?
C7 C12 C11 118.2(5) . . ?
C22 C21 C20 121.0(5) . . ?
C9 C10 C11 120.7(5) . . ?
C10 C11 C12 119.6(5) . . ?
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 S1 2.3315(15) . ?
Pd1 S1 2.3315(15) 2 ?
Pd1 S2 2.3442(13) 2 ?
Pd1 S2 2.3442(13) . ?
S1 P1 2.0059(17) . ?
S2 P2 2.0077(16) . ?
P1 N1 1.553(4) . ?
P1 O1 1.586(3) . ?
P1 O2 1.598(3) . ?
P2 N1 1.596(4) . ?
P2 C13 1.797(4) . ?
P2 C19 1.803(4) . ?
O2 C7 1.411(5) . ?
O1 C1 1.412(5) . ?
C13 C14 1.383(6) . ?
C13 C18 1.402(6) . ?
C2 C3 1.383(7) . ?
C2 C1 1.384(7) . ?
C7 C12 1.366(7) . ?
C7 C8 1.384(7) . ?
C1 C6 1.368(7) . ?
C3 C4 1.371(7) . ?
C6 C5 1.405(7) . ?
C4 C5 1.369(8) . ?
C16 C17 1.374(7) . ?
C16 C15 1.378(7) . ?
C18 C17 1.384(7) . ?
C15 C14 1.379(7) . ?
C19 C20 1.388(6) . ?
C19 C24 1.395(6) . ?
C20 C21 1.396(7) . ?
C24 C23 1.386(6) . ?
C8 C9 1.395(7) . ?
C22 C21 1.359(7) . ?
C22 C23 1.392(7) . ?
C9 C10 1.366(8) . ?
C12 C11 1.409(7) . ?
C10 C11 1.378(8) . ?
