#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:43:26 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179986 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/80/7028012.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# 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_7028012
loop_
_publ_author_name
'Pelagatti, Paolo'
'Venturini, Andrea'
'Leporati, Andrea'
'Carcelli, Mauro'
'Costa, Mirco'
'Bacchi, Alessia'
'Pelizzi, Giancarlo'
'Pelizzi, Corrado'
_publ_section_title
;
 Chemoselective homogeneous hydrogenation of phenylacetylene using
 thiosemicarbazone and thiobenzoylhydrazone palladium(II) complexes as
 catalysts
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2715
_journal_paper_doi               10.1039/a804052d
_journal_year                    1998
_chemical_formula_sum            'C19 H14 Cl N3 Pd S'
_chemical_formula_weight         458.24
_chemical_name_systematic
; 

 ? 

;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   none
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 101.20(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.235(3)
_cell_length_b                   9.413(2)
_cell_length_c                   15.670(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_volume                     1770.3(7)
_computing_molecular_graphics    'ZORTEP (Zsolnai & Pritzkow, 1994)'
_computing_publication_material  'PARST95 (Nardelli, 1995)'
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1992)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Siemens AED diffractometer'
_diffrn_measurement_method       'θ/2θ scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0718
_diffrn_reflns_av_sigmaI/netI    0.1525
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3254
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         3.19
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 100
_diffrn_standards_number         1
_exptl_absorpt_coefficient_mu    1.323
_exptl_absorpt_correction_T_max  1.06
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   'Walker&Stuart (1983)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       prisms
_exptl_crystal_F_000             912
_refine_diff_density_max         1.333
_refine_diff_density_min         -1.150
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.012
_refine_ls_goodness_of_fit_obs   1.125
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3140
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_restrained_S_obs      1.125
_refine_ls_R_factor_all          0.2002
_refine_ls_R_factor_obs          0.0685
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s²(Fo²)+( 0.1117P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2534
_refine_ls_wR_factor_obs         0.1648
_reflns_number_observed          1227
_reflns_number_total             3140
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            d804052sup1.cif
_cod_data_source_block           2a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.1117P)^2^+0.0000P] 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^)+( 0.1117P)^2^+0.0000P] 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        1770(1)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7028012
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Pd Pd 0.57181(10) 0.22538(12) 0.03775(8) 0.0538(5) Uani 1 d .
Cl Cl 0.7571(3) 0.2735(4) 0.0476(3) 0.0691(12) Uani 1 d .
S S 0.5939(3) 0.0717(4) 0.1493(3) 0.0603(11) Uani 1 d .
N1 N 0.5126(10) 0.3535(12) -0.0677(7) 0.052(3) Uani 1 d .
N2 N 0.4148(10) 0.1847(13) 0.0283(7) 0.054(3) Uani 1 d .
N3 N 0.3731(9) 0.0978(13) 0.0846(7) 0.054(3) Uani 1 d .
C1 C 0.1536(13) 0.3537(17) -0.0522(9) 0.059(4) Uani 1 d .
H1 H 0.1840(13) 0.4445(17) -0.0477(9) 0.071 Uiso 1 calc R
C2 C 0.0420(14) 0.3367(19) -0.0637(10) 0.066(4) Uani 1 d .
H2 H -0.0031(14) 0.4163(19) -0.0642(10) 0.079 Uiso 1 calc R
C3 C -0.0052(12) 0.2076(19) -0.0744(10) 0.060(4) Uani 1 d .
H3 H -0.0824(12) 0.1996(19) -0.0841(10) 0.072 Uiso 1 calc R
C4 C 0.0586(12) 0.0873(17) -0.0712(9) 0.056(4) Uani 1 d .
H4 H 0.0255(12) -0.0019(17) -0.0789(9) 0.068 Uiso 1 calc R
C5 C 0.1727(12) 0.1012(15) -0.0564(10) 0.058(4) Uani 1 d .
H5 H 0.2161(12) 0.0196(15) -0.0526(10) 0.070 Uiso 1 calc R
C6 C 0.2253(10) 0.2321(15) -0.0471(8) 0.042(3) Uani 1 d .
C7 C 0.3422(11) 0.2538(15) -0.0335(8) 0.046(4) Uani 1 d .
C8 C 0.3963(12) 0.3414(15) -0.0889(10) 0.054(4) Uani 1 d .
C9 C 0.3404(13) 0.4113(17) -0.1633(10) 0.065(5) Uani 1 d .
H9 H 0.2640(13) 0.3986(17) -0.1814(10) 0.078 Uiso 1 calc R
C10 C 0.3974(16) 0.4995(16) -0.2108(12) 0.079(5) Uani 1 d .
H10 H 0.3600(16) 0.5528(16) -0.2574(12) 0.095 Uiso 1 calc R
C11 C 0.5085(16) 0.5044(19) -0.1866(13) 0.085(6) Uani 1 d .
H11 H 0.5487(16) 0.5604(19) -0.2186(13) 0.102 Uiso 1 calc R
C12 C 0.5655(13) 0.4297(16) -0.1162(11) 0.061(4) Uani 1 d .
H12 H 0.6429(13) 0.4337(16) -0.1030(11) 0.073 Uiso 1 calc R
C13 C 0.4526(10) 0.0383(14) 0.1416(8) 0.039(3) Uani 1 d .
C14 C 0.4175(11) -0.0589(14) 0.2024(9) 0.045(3) Uani 1 d .
C15 C 0.4906(13) -0.1162(16) 0.2745(10) 0.063(4) Uani 1 d .
H15 H 0.5656(13) -0.0921(16) 0.2827(10) 0.076 Uiso 1 calc R
C16 C 0.4570(15) -0.2057(18) 0.3335(10) 0.071(5) Uani 1 d .
H16 H 0.5071(15) -0.2325(18) 0.3834(10) 0.085 Uiso 1 calc R
C17 C 0.3519(14) -0.2548(17) 0.3196(10) 0.065(5) Uani 1 d .
H17 H 0.3298(14) -0.3194(17) 0.3578(10) 0.078 Uiso 1 calc R
C18 C 0.2778(14) -0.2076(17) 0.2479(10) 0.068(5) Uani 1 d .
H18 H 0.2050(14) -0.2414(17) 0.2379(10) 0.081 Uiso 1 calc R
C19 C 0.3074(12) -0.1141(18) 0.1916(10) 0.063(4) Uani 1 d .
H19 H 0.2542(12) -0.0846(18) 0.1442(10) 0.075 Uiso 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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_publ_flag
N2 Pd N1 82.3(5) y
N2 Pd S 84.3(4) y
N1 Pd S 166.5(3) y
N2 Pd Cl 179.5(3) y
N1 Pd Cl 97.3(4) y
S Pd Cl 96.1(2) y
C13 S Pd 95.4(5) y
C12 N1 C8 120.2(13) ?
C12 N1 Pd 130.7(11) ?
C8 N1 Pd 108.9(9) y
C7 N2 N3 118.4(12) ?
C7 N2 Pd 117.7(9) y
N3 N2 Pd 123.8(9) y
C13 N3 N2 111.9(11) y
C2 C1 C6 120.3(15) ?
C3 C2 C1 121.5(15) ?
C2 C3 C4 121.0(13) ?
C3 C4 C5 118.6(14) ?
C4 C5 C6 122.6(14) ?
C5 C6 C7 125.3(13) ?
C5 C6 C1 115.9(12) ?
C7 C6 C1 118.8(13) ?
N2 C7 C6 122.8(12) ?
N2 C7 C8 113.1(12) y
C6 C7 C8 123.9(12) ?
C9 C8 N1 118.0(14) ?
C9 C8 C7 124.2(13) ?
N1 C8 C7 117.8(13) y
C10 C9 C8 120.9(15) ?
C11 C10 C9 117.2(16) ?
C10 C11 C12 122.5(17) ?
N1 C12 C11 121.0(16) ?
N3 C13 C14 116.3(11) ?
N3 C13 S 124.5(11) y
C14 C13 S 119.2(9) ?
C15 C14 C19 113.3(13) ?
C15 C14 C13 123.3(12) ?
C19 C14 C13 123.3(12) ?
C16 C15 C14 123.4(15) ?
C17 C16 C15 120.3(15) ?
C16 C17 C18 118.7(15) ?
C19 C18 C17 122.0(16) ?
C18 C19 C14 122.0(15) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd N2 1.937(12) y
Pd N1 2.060(12) y
Pd S 2.245(4) y
Pd Cl 2.287(4) y
S C13 1.738(13) y
N1 C12 1.30(2) ?
N1 C8 1.40(2) y
N2 C7 1.35(2) y
N2 N3 1.372(15) y
N3 C13 1.312(15) y
C1 C2 1.35(2) ?
C1 C6 1.43(2) ?
C2 C3 1.34(2) ?
C3 C4 1.37(2) ?
C4 C5 1.38(2) ?
C5 C6 1.38(2) ?
C6 C7 1.42(2) ?
C7 C8 1.45(2) y
C8 C9 1.40(2) ?
C9 C10 1.39(2) ?
C10 C11 1.34(2) ?
C11 C12 1.38(2) ?
C13 C14 1.45(2) ?
C14 C15 1.40(2) ?
C14 C19 1.42(2) ?
C15 C16 1.37(2) ?
C16 C17 1.34(2) ?
C17 C18 1.37(2) ?
C18 C19 1.34(2) ?
