#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:09:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180005 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/99/7029968.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_7029968
loop_
_publ_author_name
'Castiñeiras, Alfonso'
'Fernández-Hermida, Nuria'
'García-Santos, Isabel'
'Gómez-Rodríguez, Lourdes'
_publ_section_title
;
 Neutral Ni(II), Pd(II) and Pt(II) ONS-pincer complexes of
 5-acetylbarbituric-4N-dimethylthiosemicarbazone: synthesis,
 characterization and properties.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13486
_journal_page_last               13495
_journal_paper_doi               10.1039/c2dt31753b
_journal_volume                  41
_journal_year                    2012
_chemical_formula_moiety         'C11 H17 N5 O4 Pd S2, C2 H6 O S'
_chemical_formula_sum            'C13 H23 N5 O5 Pd S3'
_chemical_formula_weight         531.94
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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                117.118(4)
_cell_angle_beta                 96.563(5)
_cell_angle_gamma                92.827(5)
_cell_formula_units_Z            2
_cell_length_a                   6.547(2)
_cell_length_b                   13.218(4)
_cell_length_c                   13.463(4)
_cell_measurement_reflns_used    909
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.02
_cell_measurement_theta_min      2.97
_cell_volume                     1023.4(5)
_computing_cell_refinement       'SMART-Software (Bruker, 1997)'
_computing_data_collection       'SMART-Software (Bruker, 1997)'
_computing_data_reduction        'SAINT-Software (Bruker, 1997)'
_computing_molecular_graphics    'PLATON (Spek, 2001)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'SMART CCD-1000 Bruker'
_diffrn_measurement_method       omega-scans
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11191
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    1.247
_exptl_absorpt_correction_T_max  0.9403
_exptl_absorpt_correction_T_min  0.4391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             540
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.732
_refine_diff_density_min         -1.054
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4154
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0706
_refine_ls_R_factor_gt           0.0402
_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)+(0.0496P)²+0.2366P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0888
_refine_ls_wR_factor_ref         0.1031
_reflns_number_gt                3034
_reflns_number_total             4154
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31753b.txt
_cod_data_source_block           02lg15
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        1023.4(6)
_cod_database_code               7029968
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
Pd1 Pd 0.17769(5) 0.84282(3) 0.15232(3) 0.03703(13) Uani 1 1 d .
S1 S 0.4250(2) 0.76646(12) 0.21590(11) 0.0548(3) Uani 1 1 d .
S2 S 0.09173(19) 0.94098(10) 0.32791(9) 0.0434(3) Uani 1 1 d .
O11 O -0.0354(5) 0.9116(3) 0.0906(2) 0.0458(8) Uani 1 1 d .
O13 O -0.5324(6) 0.9410(3) -0.1483(3) 0.0605(10) Uani 1 1 d .
O15 O -0.1149(6) 0.6705(3) -0.3060(3) 0.0676(11) Uani 1 1 d .
O21 O 0.0417(7) 0.8737(3) 0.3844(3) 0.0680(11) Uani 1 1 d .
N11 N -0.2735(6) 0.9215(3) -0.0328(3) 0.0409(9) Uani 1 1 d .
H11A H -0.3229 0.9739 0.0368 0.049 Uiso 1 1 d R
N12 N 0.2599(5) 0.7528(3) 0.0004(3) 0.0333(8) Uani 1 1 d .
N13 N 0.4382(6) 0.6959(3) -0.0055(3) 0.0462(10) Uani 1 1 d .
N14 N 0.6955(6) 0.6463(4) 0.0855(4) 0.0576(11) Uani 1 1 d .
N15 N -0.3039(6) 0.8139(3) -0.2243(3) 0.0434(9) Uani 1 1 d .
H15A H -0.3770 0.7929 -0.2930 0.052 Uiso 1 1 d R
C11 C -0.1024(7) 0.8725(4) -0.0144(3) 0.0360(10) Uani 1 1 d .
C13 C -0.3794(7) 0.8959(4) -0.1361(4) 0.0433(11) Uani 1 1 d .
C15 C -0.1413(7) 0.7533(4) -0.2178(4) 0.0430(11) Uani 1 1 d .
C16 C -0.0209(7) 0.7910(3) -0.1071(3) 0.0343(9) Uani 1 1 d .
C17 C 0.1688(7) 0.7414(4) -0.0953(4) 0.0359(10) Uani 1 1 d .
C18 C 0.5239(7) 0.6993(4) 0.0870(4) 0.0444(11) Uani 1 1 d .
C19 C 0.7673(8) 0.5809(5) -0.0217(5) 0.0618(15) Uani 1 1 d .
H19A H 0.6980 0.5044 -0.0578 0.093 Uiso 1 1 d R
H19B H 0.9139 0.5787 -0.0089 0.093 Uiso 1 1 d R
H19C H 0.7372 0.6163 -0.0693 0.093 Uiso 1 1 d R
C20 C 0.7840(9) 0.6263(5) 0.1775(5) 0.0671(16) Uani 1 1 d .
H20A H 0.7390 0.6793 0.2460 0.101 Uiso 1 1 d R
H20B H 0.9323 0.6370 0.1860 0.101 Uiso 1 1 d R
H20C H 0.7392 0.5495 0.1616 0.101 Uiso 1 1 d R
C21 C 0.2920(9) 1.0495(5) 0.4160(5) 0.0769(18) Uani 1 1 d .
H21A H 0.2582 1.0880 0.4910 0.115 Uiso 1 1 d R
H21B H 0.3088 1.1033 0.3873 0.115 Uiso 1 1 d R
H21C H 0.4185 1.0162 0.4178 0.115 Uiso 1 1 d R
C22 C -0.1146(9) 1.0248(5) 0.3270(5) 0.0723(17) Uani 1 1 d .
H22A H -0.2380 0.9749 0.2829 0.108 Uiso 1 1 d R
H22B H -0.0775 1.0733 0.2947 0.108 Uiso 1 1 d R
H22C H -0.1388 1.0712 0.4030 0.108 Uiso 1 1 d R
C170 C 0.2675(8) 0.6761(4) -0.1989(4) 0.0513(13) Uani 1 1 d .
H17A H 0.4140 0.6809 -0.1772 0.077 Uiso 1 1 d R
H17B H 0.2424 0.7083 -0.2497 0.077 Uiso 1 1 d R
H17C H 0.2092 0.5973 -0.2359 0.077 Uiso 1 1 d R
S3 S 0.6744(2) 0.37927(13) 0.49911(12) 0.0618(4) Uani 1 1 d .
O31 O 0.5786(7) 0.2594(3) 0.4269(3) 0.0804(12) Uani 1 1 d .
C31 C 0.9289(9) 0.3695(6) 0.5500(6) 0.087(2) Uani 1 1 d .
H31A H 0.9250 0.3245 0.5892 0.130 Uiso 1 1 d R
H31B H 0.9967 0.4448 0.6007 0.130 Uiso 1 1 d R
H31C H 1.0036 0.3338 0.4877 0.130 Uiso 1 1 d R
C32 C 0.5753(12) 0.4269(6) 0.6265(6) 0.097(2) Uani 1 1 d .
H32A H 0.4299 0.4323 0.6134 0.146 Uiso 1 1 d R
H32B H 0.6454 0.5008 0.6799 0.146 Uiso 1 1 d R
H32C H 0.5961 0.3738 0.6561 0.146 Uiso 1 1 d R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Pd Pd -0.9988 1.0072 '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'
O O 0.0106 0.0060 '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'
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'
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
N12 Pd1 O11 91.68(13) y
N12 Pd1 S1 86.26(10) y
O11 Pd1 S1 177.40(10) y
N12 Pd1 S2 177.65(10) y
O11 Pd1 S2 90.62(9) y
S1 Pd1 S2 91.46(5) ?
C18 S1 Pd1 95.33(16) ?
O21 S2 C21 108.4(3) ?
O21 S2 C22 109.4(3) ?
C21 S2 C22 100.6(3) ?
O21 S2 Pd1 116.35(15) ?
C21 S2 Pd1 109.9(2) ?
C22 S2 Pd1 111.07(18) ?
C11 O11 Pd1 123.8(3) ?
C13 N11 C11 125.3(4) ?
C13 N11 H11A 121.0 ?
C11 N11 H11A 113.5 ?
C17 N12 N13 115.1(3) ?
C17 N12 Pd1 127.2(3) ?
N13 N12 Pd1 117.7(3) ?
C18 N13 N12 116.5(4) ?
C18 N14 C20 123.6(5) ?
C18 N14 C19 118.8(4) ?
C20 N14 C19 115.8(4) ?
C13 N15 C15 126.5(4) ?
C13 N15 H15A 115.3 ?
C15 N15 H15A 117.8 ?
O11 C11 N11 112.1(4) ?
O11 C11 C16 128.2(4) ?
N11 C11 C16 119.7(4) ?
O13 C13 N15 122.9(4) ?
O13 C13 N11 122.9(4) ?
N15 C13 N11 114.2(4) ?
O15 C15 N15 117.0(4) ?
O15 C15 C16 125.9(4) ?
N15 C15 C16 117.0(4) ?
C11 C16 C15 116.4(4) ?
C11 C16 C17 123.2(4) ?
C15 C16 C17 120.3(4) ?
N12 C17 C16 123.3(4) ?
N12 C17 C170 118.1(4) ?
C16 C17 C170 118.6(4) ?
N13 C18 N14 118.5(5) ?
N13 C18 S1 123.5(4) ?
N14 C18 S1 117.9(4) ?
N14 C19 H19A 109.4 ?
N14 C19 H19B 109.5 ?
H19A C19 H19B 109.5 ?
N14 C19 H19C 109.5 ?
H19A C19 H19C 109.5 ?
H19B C19 H19C 109.5 ?
N14 C20 H20A 109.3 ?
N14 C20 H20B 109.6 ?
H20A C20 H20B 109.5 ?
N14 C20 H20C 109.5 ?
H20A C20 H20C 109.5 ?
H20B C20 H20C 109.5 ?
S2 C21 H21A 109.5 ?
S2 C21 H21B 109.5 ?
H21A C21 H21B 109.5 ?
S2 C21 H21C 109.4 ?
H21A C21 H21C 109.5 ?
H21B C21 H21C 109.5 ?
S2 C22 H22A 109.4 ?
S2 C22 H22B 109.5 ?
H22A C22 H22B 109.5 ?
S2 C22 H22C 109.5 ?
H22A C22 H22C 109.5 ?
H22B C22 H22C 109.5 ?
C17 C170 H17A 109.4 ?
C17 C170 H17B 109.6 ?
H17A C170 H17B 109.5 ?
C17 C170 H17C 109.4 ?
H17A C170 H17C 109.5 ?
H17B C170 H17C 109.5 ?
O31 S3 C32 106.1(3) ?
O31 S3 C31 105.7(3) ?
C32 S3 C31 97.7(3) ?
S3 C31 H31A 109.5 ?
S3 C31 H31B 109.5 ?
H31A C31 H31B 109.5 ?
S3 C31 H31C 109.4 ?
H31A C31 H31C 109.5 ?
H31B C31 H31C 109.5 ?
S3 C32 H32A 109.4 ?
S3 C32 H32B 109.5 ?
H32A C32 H32B 109.5 ?
S3 C32 H32C 109.5 ?
H32A C32 H32C 109.5 ?
H32B C32 H32C 109.5 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Pd1 N12 1.997(3) y
Pd1 O11 2.003(3) y
Pd1 S1 2.2370(13) y
Pd1 S2 2.2734(13) y
S1 C18 1.769(5) ?
S2 O21 1.456(4) ?
S2 C21 1.758(5) ?
S2 C22 1.791(5) ?
O11 C11 1.276(5) ?
O13 C13 1.222(5) ?
O15 C15 1.232(5) ?
N11 C13 1.363(5) ?
N11 C11 1.375(5) ?
N11 H11A 0.9813 ?
N12 C17 1.294(5) ?
N12 N13 1.410(5) ?
N13 C18 1.287(6) ?
N14 C18 1.350(6) ?
N14 C20 1.445(6) ?
N14 C19 1.452(7) ?
N15 C13 1.358(6) ?
N15 C15 1.381(6) ?
N15 H15A 0.9020 ?
C11 C16 1.410(6) ?
C15 C16 1.452(6) ?
C16 C17 1.458(6) ?
C17 C170 1.508(6) ?
C19 H19A 0.9600 ?
C19 H19B 0.9599 ?
C19 H19C 0.9600 ?
C20 H20A 0.9600 ?
C20 H20B 0.9599 ?
C20 H20C 0.9600 ?
C21 H21A 0.9600 ?
C21 H21B 0.9600 ?
C21 H21C 0.9599 ?
C22 H22A 0.9600 ?
C22 H22B 0.9600 ?
C22 H22C 0.9600 ?
C170 H17A 0.9599 ?
C170 H17B 0.9600 ?
C170 H17C 0.9600 ?
S3 O31 1.486(4) ?
S3 C32 1.752(6) ?
S3 C31 1.761(6) ?
C31 H31A 0.9600 ?
C31 H31B 0.9600 ?
C31 H31C 0.9600 ?
C32 H32A 0.9599 ?
C32 H32B 0.9600 ?
C32 H32C 0.9600 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N11 H11A O13 0.98 1.82 2.786(5) 168.0 2_475
N15 H15A O31 0.90 1.92 2.813(5) 168.3 2_565
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
N12 Pd1 S1 C18 6.72(18)
O11 Pd1 S1 C18 -30(2)
S2 Pd1 S1 C18 -173.82(16)
N12 Pd1 S2 O21 -41(3)
O11 Pd1 S2 O21 127.1(2)
S1 Pd1 S2 O21 -54.4(2)
N12 Pd1 S2 C21 82(3)
O11 Pd1 S2 C21 -109.3(3)
S1 Pd1 S2 C21 69.2(3)
N12 Pd1 S2 C22 -167(3)
O11 Pd1 S2 C22 1.1(3)
S1 Pd1 S2 C22 179.6(2)
N12 Pd1 O11 C11 15.7(4)
S1 Pd1 O11 C11 53(2)
S2 Pd1 O11 C11 -163.8(3)
O11 Pd1 N12 C17 -8.5(4)
S1 Pd1 N12 C17 173.1(4)
S2 Pd1 N12 C17 160(2)
O11 Pd1 N12 N13 170.6(3)
S1 Pd1 N12 N13 -7.9(3)
S2 Pd1 N12 N13 -21(3)
C17 N12 N13 C18 -175.4(4)
Pd1 N12 N13 C18 5.4(5)
Pd1 O11 C11 N11 168.8(3)
Pd1 O11 C11 C16 -12.6(7)
C13 N11 C11 O11 -179.4(4)
C13 N11 C11 C16 1.8(7)
C15 N15 C13 O13 -175.3(5)
C15 N15 C13 N11 2.9(7)
C11 N11 C13 O13 179.1(4)
C11 N11 C13 N15 0.9(7)
C13 N15 C15 O15 169.4(5)
C13 N15 C15 C16 -8.8(7)
O11 C11 C16 C15 173.9(4)
N11 C11 C16 C15 -7.6(6)
O11 C11 C16 C17 -3.4(7)
N11 C11 C16 C17 175.1(4)
O15 C15 C16 C11 -167.4(5)
N15 C15 C16 C11 10.6(6)
O15 C15 C16 C17 10.0(7)
N15 C15 C16 C17 -172.0(4)
N13 N12 C17 C16 178.2(4)
Pd1 N12 C17 C16 -2.8(6)
N13 N12 C17 C170 -3.5(6)
Pd1 N12 C17 C170 175.5(3)
C11 C16 C17 N12 11.9(7)
C15 C16 C17 N12 -165.3(4)
C11 C16 C17 C170 -166.5(4)
C15 C16 C17 C170 16.4(6)
N12 N13 C18 N14 -179.7(4)
N12 N13 C18 S1 2.1(6)
C20 N14 C18 N13 -168.5(5)
C19 N14 C18 N13 -4.5(7)
C20 N14 C18 S1 9.8(7)
C19 N14 C18 S1 173.9(4)
Pd1 S1 C18 N13 -7.0(4)
Pd1 S1 C18 N14 174.8(4)
