#------------------------------------------------------------------------------
#$Date: 2019-11-28 17:33:15 +0100 (jue 28 de nov de 2019) $
#$Revision: 244295 $
#$URL: svn://www.crystallography.net/cod/cif/7/23/86/7238691.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_7238691
loop_
_publ_author_name
'Dutta, Jayita'
'Datta, Sayanti'
'Kumar Seth, Dipravath'
'Bhattacharya, Samaresh'
_publ_section_title
;
 Mixed-ligand benzaldehyde thiosemicarbazone complexes of palladium
 containing N,O-donor ancillary ligands. Syntheses, structures, and
 catalytic application in C--C and C--N coupling reactions
;
_journal_issue                   31
_journal_name_full               'RSC Advances'
_journal_page_first              11751
_journal_paper_doi               10.1039/c2ra21078a
_journal_volume                  2
_journal_year                    2012
_chemical_formula_sum            'C18 H13 Cl N4 O Pd S'
_chemical_formula_weight         491.24
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.304(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5491(14)
_cell_length_b                   7.6562(7)
_cell_length_c                   15.7781(14)
_cell_measurement_temperature    273(2)
_cell_volume                     1811.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.1323
_diffrn_reflns_av_sigmaI/netI    0.0923
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            26837
_diffrn_reflns_theta_full        27.78
_diffrn_reflns_theta_max         27.78
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  0.732
_exptl_absorpt_correction_T_min  0.730
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.801
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             896
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.198
_refine_diff_density_min         -0.693
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.719
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4193
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.719
_refine_ls_R_factor_all          0.1101
_refine_ls_R_factor_gt           0.0597
_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)+(0.1865P)²+8.1677P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1765
_refine_ls_wR_factor_ref         0.2265
_reflns_number_gt                2550
_reflns_number_total             4193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra21078a.txt
_cod_data_source_block           jdp21c
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7238691
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Pd1 Pd 0.33839(4) 0.39045(8) 0.37949(4) 0.0449(2) Uani 1 1 d .
Cl1 Cl 0.85970(17) -0.0872(4) 0.64306(19) 0.0801(8) Uani 1 1 d .
S1 S 0.33537(15) 0.3386(3) 0.23896(13) 0.0567(5) Uani 1 1 d .
N2 N 0.4863(4) 0.1883(10) 0.3378(4) 0.0502(15) Uani 1 1 d .
N1 N 0.4575(4) 0.2656(8) 0.4043(3) 0.0406(13) Uani 1 1 d .
O2 O 0.1736(4) 0.5401(10) 0.2814(4) 0.0682(17) Uani 1 1 d .
O1 O 0.3348(4) 0.4389(7) 0.5073(3) 0.0503(13) Uani 1 1 d .
C1 C 0.4316(5) 0.2132(11) 0.2596(5) 0.0479(18) Uani 1 1 d .
C2 C 0.5071(5) 0.2444(10) 0.4834(5) 0.0483(17) Uani 1 1 d .
H2 H 0.4846 0.2951 0.5267 0.058 Uiso 1 1 calc R
C3 C 0.5921(5) 0.1548(10) 0.5165(5) 0.0484(18) Uani 1 1 d .
C4 C 0.6276(6) 0.1503(12) 0.6080(5) 0.055(2) Uani 1 1 d .
H4 H 0.5948 0.1992 0.6435 0.066 Uiso 1 1 calc R
C5 C 0.7089(6) 0.0766(11) 0.6471(6) 0.055(2) Uani 1 1 d .
H5 H 0.7311 0.0768 0.7079 0.066 Uiso 1 1 calc R
C6 C 0.7572(5) 0.0016(12) 0.5940(6) 0.059(2) Uani 1 1 d .
C7 C 0.7233(6) -0.0008(13) 0.5054(6) 0.064(2) Uani 1 1 d .
H7 H 0.7556 -0.0532 0.4704 0.077 Uiso 1 1 calc R
C8 C 0.6418(6) 0.0731(12) 0.4666(5) 0.057(2) Uani 1 1 d .
H8 H 0.6196 0.0684 0.4058 0.069 Uiso 1 1 calc R
N3 N 0.4537(5) 0.1374(11) 0.1911(4) 0.068(2) Uani 1 1 d .
H9A H 0.5016 0.0763 0.1998 0.081 Uiso 1 1 calc R
H9B H 0.4198 0.1501 0.1388 0.081 Uiso 1 1 calc R
N4 N 0.2200(5) 0.5077(9) 0.3563(4) 0.0542(16) Uani 1 1 d .
C9 C 0.1940(5) 0.5525(10) 0.4291(5) 0.0470(17) Uani 1 1 d .
C10 C 0.2612(6) 0.5129(11) 0.5088(5) 0.0533(19) Uani 1 1 d .
C11 C 0.2451(7) 0.5650(14) 0.5903(6) 0.072(3) Uani 1 1 d .
H13 H 0.2882 0.5465 0.6430 0.086 Uiso 1 1 calc R
C12 C 0.1681(8) 0.6401(15) 0.5899(7) 0.081(3) Uani 1 1 d .
H14 H 0.1592 0.6727 0.6437 0.097 Uiso 1 1 calc R
C13 C 0.0977(6) 0.6745(14) 0.5126(6) 0.068(2) Uani 1 1 d .
C18 C 0.1095(6) 0.6301(10) 0.4304(6) 0.056(2) Uani 1 1 d .
C17 C 0.0382(6) 0.6647(14) 0.3564(7) 0.073(3) Uani 1 1 d .
H17 H 0.0430 0.6350 0.3007 0.088 Uiso 1 1 calc R
C14 C 0.0208(7) 0.7510(17) 0.5208(7) 0.089(3) Uani 1 1 d .
H14A H 0.0149 0.7807 0.5762 0.106 Uiso 1 1 calc R
C16 C -0.0381(7) 0.7416(16) 0.3658(8) 0.088(3) Uani 1 1 d .
H16 H -0.0841 0.7654 0.3160 0.105 Uiso 1 1 calc R
C15 C -0.0483(8) 0.7843(17) 0.4468(8) 0.093(4) Uani 1 1 d .
H15 H -0.1010 0.8350 0.4521 0.112 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'
O O 0.0106 0.0060 '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
N4 Pd1 N1 178.5(2)
N4 Pd1 O1 80.6(2)
N1 Pd1 O1 98.9(2)
N4 Pd1 S1 96.93(19)
N1 Pd1 S1 83.52(16)
O1 Pd1 S1 177.34(16)
C1 S1 Pd1 96.9(2)
C1 N2 N1 113.0(6)
C2 N1 N2 116.8(6)
C2 N1 Pd1 121.8(5)
N2 N1 Pd1 121.3(4)
C10 O1 Pd1 110.6(5)
N2 C1 N3 116.8(7)
N2 C1 S1 124.7(6)
N3 C1 S1 118.5(6)
N1 C2 C3 131.1(7)
N1 C2 H2 114.4
C3 C2 H2 114.4
C8 C3 C4 116.4(8)
C8 C3 C2 126.6(7)
C4 C3 C2 116.9(7)
C5 C4 C3 122.5(9)
C5 C4 H4 118.7
C3 C4 H4 118.7
C4 C5 C6 118.7(8)
C4 C5 H5 120.7
C6 C5 H5 120.7
C7 C6 C5 120.1(8)
C7 C6 Cl1 121.4(8)
C5 C6 Cl1 118.5(7)
C6 C7 C8 121.0(9)
C6 C7 H7 119.5
C8 C7 H7 119.5
C7 C8 C3 121.3(8)
C7 C8 H8 119.4
C3 C8 H8 119.4
C1 N3 H9A 120.0
C1 N3 H9B 120.0
H9A N3 H9B 120.0
O2 N4 C9 121.9(7)
O2 N4 Pd1 123.0(5)
C9 N4 Pd1 115.1(5)
N4 C9 C10 112.1(7)
N4 C9 C18 126.1(7)
C10 C9 C18 121.8(7)
O1 C10 C11 120.6(7)
O1 C10 C9 121.5(7)
C11 C10 C9 117.9(8)
C12 C11 C10 119.2(9)
C12 C11 H13 120.4
C10 C11 H13 120.4
C11 C12 C13 124.7(9)
C11 C12 H14 117.6
C13 C12 H14 117.6
C14 C13 C18 121.6(10)
C14 C13 C12 119.2(9)
C18 C13 C12 119.2(8)
C13 C18 C17 117.1(8)
C13 C18 C9 117.1(8)
C17 C18 C9 125.8(8)
C16 C17 C18 120.5(10)
C16 C17 H17 119.8
C18 C17 H17 119.8
C13 C14 C15 120.0(10)
C13 C14 H14A 120.0
C15 C14 H14A 120.0
C17 C16 C15 121.4(10)
C17 C16 H16 119.3
C15 C16 H16 119.3
C16 C15 C14 119.3(10)
C16 C15 H15 120.4
C14 C15 H15 120.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Pd1 N4 1.993(7)
Pd1 N1 2.028(6)
Pd1 O1 2.065(5)
Pd1 S1 2.241(2)
Cl1 C6 1.718(8)
S1 C1 1.734(8)
N2 C1 1.314(9)
N2 N1 1.379(8)
N1 C2 1.293(9)
O2 N4 1.236(8)
O1 C10 1.283(9)
C1 N3 1.349(9)
C2 C3 1.458(11)
C2 H2 0.9300
C3 C8 1.390(12)
C3 C4 1.404(10)
C4 C5 1.373(13)
C4 H4 0.9300
C5 C6 1.388(13)
C5 H5 0.9300
C6 C7 1.359(12)
C7 C8 1.374(12)
C7 H7 0.9300
C8 H8 0.9300
N3 H9A 0.8600
N3 H9B 0.8600
N4 C9 1.360(10)
C9 C10 1.439(11)
C9 C18 1.447(11)
C10 C11 1.431(11)
C11 C12 1.327(14)
C11 H13 0.9300
C12 C13 1.432(14)
C12 H14 0.9300
C13 C14 1.369(13)
C13 C18 1.398(13)
C18 C17 1.407(13)
C17 C16 1.368(14)
C17 H17 0.9300
C14 C15 1.386(15)
C14 H14A 0.9300
C16 C15 1.368(14)
C16 H16 0.9300
C15 H15 0.9300
