#------------------------------------------------------------------------------
#$Date: 2016-03-25 17:09:38 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180005 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/99/7029969.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_7029969
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 Pt S2, C2 H6 O S'
_chemical_formula_sum            'C13 H23 N5 O5 Pt S3'
_chemical_formula_weight         620.63
_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                116.863(3)
_cell_angle_beta                 96.683(4)
_cell_angle_gamma                92.316(4)
_cell_formula_units_Z            2
_cell_length_a                   6.6141(15)
_cell_length_b                   13.122(3)
_cell_length_c                   13.394(3)
_cell_measurement_reflns_used    965
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.1
_cell_measurement_theta_min      2.97
_cell_volume                     1024.3(4)
_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, 2000)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0465
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11334
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    7.189
_exptl_absorpt_correction_T_max  0.6330
_exptl_absorpt_correction_T_min  0.2470
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    2.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.704
_refine_diff_density_min         -1.463
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         4180
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0417P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0805
_reflns_number_gt                3429
_reflns_number_total             4180
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31753b.txt
_cod_data_source_block           02lg01
_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_database_code               7029969
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
Pt1 Pt 0.67787(4) 0.34434(2) 0.153523(18) 0.03643(9) Uani 1 1 d .
S1 S 0.9288(3) 0.26862(17) 0.21646(14) 0.0539(5) Uani 1 1 d .
O11 O 0.4598(7) 0.4107(4) 0.0906(3) 0.0455(11) Uani 1 1 d .
O13 O -0.0388(8) 0.4373(4) -0.1486(4) 0.0583(13) Uani 1 1 d .
O15 O 0.3857(8) 0.1705(5) -0.3071(4) 0.0701(16) Uani 1 1 d .
N11 N 0.2230(8) 0.4205(4) -0.0329(4) 0.0421(12) Uani 1 1 d .
H11 H 0.1903 0.4853 0.0293 0.051 Uiso 1 1 d R
N12 N 0.7553(7) 0.2548(4) 0.0002(4) 0.0323(10) Uani 1 1 d .
N13 N 0.9347(8) 0.1952(5) -0.0072(4) 0.0445(13) Uani 1 1 d .
N14 N 1.1899(9) 0.1425(5) 0.0830(5) 0.0560(15) Uani 1 1 d .
N15 N 0.1930(8) 0.3121(5) -0.2249(4) 0.0445(13) Uani 1 1 d .
H15 H 0.1040 0.3014 -0.2933 0.053 Uiso 1 1 d R
C11 C 0.3929(9) 0.3722(5) -0.0149(5) 0.0367(13) Uani 1 1 d .
C13 C 0.1154(10) 0.3934(6) -0.1372(5) 0.0448(15) Uani 1 1 d .
C15 C 0.3560(10) 0.2524(6) -0.2186(5) 0.0421(15) Uani 1 1 d .
C16 C 0.4770(9) 0.2906(5) -0.1067(5) 0.0357(13) Uani 1 1 d .
C17 C 0.6650(9) 0.2410(5) -0.0968(5) 0.0391(14) Uani 1 1 d .
C18 C 1.0213(10) 0.1992(6) 0.0866(5) 0.0448(15) Uani 1 1 d .
C19 C 1.2842(11) 0.1275(7) 0.1771(7) 0.064(2) Uani 1 1 d .
H19A H 1.4291 0.1483 0.1895 0.096 Uiso 1 1 calc R
H19B H 1.2585 0.0486 0.1609 0.096 Uiso 1 1 calc R
H19C H 1.2278 0.1755 0.2438 0.096 Uiso 1 1 calc R
C20 C 1.2633(12) 0.0779(7) -0.0239(6) 0.064(2) Uani 1 1 d .
H20A H 1.2033 -0.0003 -0.0583 0.095 Uiso 1 1 calc R
H20B H 1.4096 0.0802 -0.0108 0.095 Uiso 1 1 calc R
H20C H 1.2255 0.1112 -0.0733 0.095 Uiso 1 1 calc R
C170 C 0.7618(10) 0.1747(6) -0.2013(5) 0.0526(17) Uani 1 1 d .
H17A H 0.7415 0.2094 -0.2508 0.079 Uiso 1 1 calc R
H17B H 0.6997 0.0967 -0.2398 0.079 Uiso 1 1 calc R
H17C H 0.9058 0.1758 -0.1798 0.079 Uiso 1 1 calc R
S2 S 0.5914(3) 0.44121(14) 0.32663(12) 0.0422(4) Uani 1 1 d .
O21 O 0.5456(9) 0.3735(4) 0.3838(4) 0.0640(14) Uani 1 1 d .
C21 C 0.3860(12) 0.5227(7) 0.3249(6) 0.066(2) Uani 1 1 d .
H21A H 0.2650 0.4719 0.2814 0.099 Uiso 1 1 calc R
H21B H 0.4195 0.5711 0.2914 0.099 Uiso 1 1 calc R
H21C H 0.3618 0.5695 0.4010 0.099 Uiso 1 1 calc R
C22 C 0.7885(13) 0.5506(8) 0.4143(6) 0.079(3) Uani 1 1 d .
H22A H 0.7584 0.5868 0.4904 0.118 Uiso 1 1 calc R
H22B H 0.7983 0.6067 0.3871 0.118 Uiso 1 1 calc R
H22C H 0.9160 0.5180 0.4130 0.118 Uiso 1 1 calc R
S3 S 0.8263(3) 0.12048(18) 0.50050(16) 0.0631(5) Uani 1 1 d .
O31 O 0.9216(9) 0.2400(5) 0.5727(4) 0.0788(17) Uani 1 1 d .
C31 C 0.5743(13) 0.1319(9) 0.4499(8) 0.091(3) Uani 1 1 d .
H31A H 0.5031 0.1724 0.5128 0.136 Uiso 1 1 calc R
H31B H 0.5044 0.0565 0.4031 0.136 Uiso 1 1 calc R
H31C H 0.5782 0.1731 0.4063 0.136 Uiso 1 1 calc R
C32 C 0.9262(16) 0.0705(9) 0.3724(8) 0.098(3) Uani 1 1 d .
H32A H 0.9927 0.1342 0.3676 0.147 Uiso 1 1 calc R
H32B H 0.8169 0.0327 0.3100 0.147 Uiso 1 1 calc R
H32C H 1.0235 0.0173 0.3695 0.147 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
Pt Pt -1.7033 8.3905 '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 Pt1 O11 90.73(18) y
N12 Pt1 S1 86.70(14) y
O11 Pt1 S1 177.21(12) y
N12 Pt1 S2 178.59(14) y
O11 Pt1 S2 90.30(12) y
S1 Pt1 S2 92.29(6) y
C18 S1 Pt1 95.6(2) ?
C11 O11 Pt1 124.6(4) ?
C11 N11 C13 125.0(5) ?
C11 N11 H11 117.1 ?
C13 N11 H11 117.1 ?
C17 N12 N13 113.6(5) ?
C17 N12 Pt1 129.1(4) ?
N13 N12 Pt1 117.3(3) ?
C18 N13 N12 115.8(5) ?
C18 N14 C19 123.1(6) ?
C18 N14 C20 120.0(6) ?
C19 N14 C20 116.2(6) ?
C13 N15 C15 127.0(5) ?
C13 N15 H15 105.7 ?
C15 N15 H15 127.2 ?
O11 C11 N11 112.2(5) ?
O11 C11 C16 127.1(5) ?
N11 C11 C16 120.7(5) ?
O13 C13 N15 123.5(5) ?
O13 C13 N11 122.5(6) ?
N15 C13 N11 114.0(5) ?
O15 C15 N15 117.2(6) ?
O15 C15 C16 125.7(6) ?
N15 C15 C16 117.0(5) ?
C11 C16 C17 124.9(5) ?
C11 C16 C15 115.5(5) ?
C17 C16 C15 119.6(5) ?
N12 C17 C16 121.5(5) ?
N12 C17 C170 119.1(5) ?
C16 C17 C170 119.4(5) ?
N13 C18 N14 117.6(6) ?
N13 C18 S1 124.1(5) ?
N14 C18 S1 118.2(5) ?
N14 C19 H19A 109.5 ?
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 109.5 ?
N14 C20 H20B 109.5 ?
H20A C20 H20B 109.5 ?
N14 C20 H20C 109.5 ?
H20A C20 H20C 109.5 ?
H20B C20 H20C 109.5 ?
C17 C170 H17A 109.5 ?
C17 C170 H17B 109.5 ?
H17A C170 H17B 109.5 ?
C17 C170 H17C 109.5 ?
H17A C170 H17C 109.5 ?
H17B C170 H17C 109.5 ?
O21 S2 C22 108.4(4) ?
O21 S2 C21 109.4(4) ?
C22 S2 C21 101.2(5) ?
O21 S2 Pt1 116.2(2) ?
C22 S2 Pt1 109.4(3) ?
C21 S2 Pt1 111.3(2) ?
S2 C21 H21A 109.5 ?
S2 C21 H21B 109.5 ?
H21A C21 H21B 109.5 ?
S2 C21 H21C 109.5 ?
H21A C21 H21C 109.5 ?
H21B C21 H21C 109.5 ?
S2 C22 H22A 109.5 ?
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 ?
O31 S3 C32 106.5(4) ?
O31 S3 C31 105.9(4) ?
C32 S3 C31 98.4(5) ?
S3 C31 H31A 109.5 ?
S3 C31 H31B 109.5 ?
H31A C31 H31B 109.5 ?
S3 C31 H31C 109.5 ?
H31A C31 H31C 109.5 ?
H31B C31 H31C 109.5 ?
S3 C32 H32A 109.5 ?
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
Pt1 N12 1.994(4) y
Pt1 O11 2.008(4) y
Pt1 S1 2.2398(17) y
Pt1 S2 2.2412(15) y
S1 C18 1.758(7) ?
O11 C11 1.280(7) ?
O13 C13 1.219(7) ?
O15 C15 1.232(7) ?
N11 C11 1.362(7) ?
N11 C13 1.372(7) ?
N11 H11 0.9385 ?
N12 C17 1.294(7) ?
N12 N13 1.435(7) ?
N13 C18 1.297(8) ?
N14 C18 1.358(8) ?
N14 C19 1.439(9) ?
N14 C20 1.449(9) ?
N15 C13 1.355(8) ?
N15 C15 1.374(8) ?
N15 H15 0.9781 ?
C11 C16 1.409(8) ?
C15 C16 1.466(8) ?
C16 C17 1.446(8) ?
C17 C170 1.510(8) ?
C19 H19A 0.9600 ?
C19 H19B 0.9600 ?
C19 H19C 0.9600 ?
C20 H20A 0.9600 ?
C20 H20B 0.9600 ?
C20 H20C 0.9600 ?
C170 H17A 0.9600 ?
C170 H17B 0.9600 ?
C170 H17C 0.9600 ?
S2 O21 1.454(5) ?
S2 C22 1.763(7) ?
S2 C21 1.767(7) ?
C21 H21A 0.9600 ?
C21 H21B 0.9600 ?
C21 H21C 0.9600 ?
C22 H22A 0.9600 ?
C22 H22B 0.9600 ?
C22 H22C 0.9600 ?
S3 O31 1.484(6) ?
S3 C32 1.759(8) ?
S3 C31 1.763(9) ?
C31 H31A 0.9600 ?
C31 H31B 0.9600 ?
C31 H31C 0.9600 ?
C32 H32A 0.9600 ?
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 H11 O13 0.94 1.89 2.766(7) 154.0 2_565
N15 H15 O31 0.98 1.85 2.807(7) 164.0 1_454
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 Pt1 S1 C18 5.6(3)
O11 Pt1 S1 C18 -17(3)
S2 Pt1 S1 C18 -175.4(2)
N12 Pt1 O11 C11 14.3(5)
S1 Pt1 O11 C11 37(3)
S2 Pt1 O11 C11 -164.8(5)
O11 Pt1 N12 C17 -8.2(5)
S1 Pt1 N12 C17 172.9(5)
S2 Pt1 N12 C17 129(5)
O11 Pt1 N12 N13 172.4(4)
S1 Pt1 N12 N13 -6.5(4)
S2 Pt1 N12 N13 -51(6)
C17 N12 N13 C18 -174.9(6)
Pt1 N12 N13 C18 4.6(7)
Pt1 O11 C11 N11 169.7(4)
Pt1 O11 C11 C16 -10.8(9)
C13 N11 C11 O11 -178.2(6)
C13 N11 C11 C16 2.3(10)
C15 N15 C13 O13 -174.6(7)
C15 N15 C13 N11 3.8(10)
C11 N11 C13 O13 178.3(6)
C11 N11 C13 N15 -0.1(10)
C13 N15 C15 O15 170.0(7)
C13 N15 C15 C16 -9.0(10)
O11 C11 C16 C17 -4.3(10)
N11 C11 C16 C17 175.1(6)
O11 C11 C16 C15 173.4(6)
N11 C11 C16 C15 -7.2(9)
O15 C15 C16 C11 -168.8(7)
N15 C15 C16 C11 10.1(9)
O15 C15 C16 C17 9.0(11)
N15 C15 C16 C17 -172.1(6)
N13 N12 C17 C16 177.3(5)
Pt1 N12 C17 C16 -2.1(9)
N13 N12 C17 C170 -4.5(8)
Pt1 N12 C17 C170 176.1(4)
C11 C16 C17 N12 11.3(10)
C15 C16 C17 N12 -166.3(6)
C11 C16 C17 C170 -166.9(6)
C15 C16 C17 C170 15.5(9)
N12 N13 C18 N14 179.1(5)
N12 N13 C18 S1 1.5(9)
C19 N14 C18 N13 -171.6(7)
C20 N14 C18 N13 -1.7(10)
C19 N14 C18 S1 6.1(10)
C20 N14 C18 S1 176.0(6)
Pt1 S1 C18 N13 -5.7(6)
Pt1 S1 C18 N14 176.8(5)
N12 Pt1 S2 O21 -10(6)
O11 Pt1 S2 O21 126.5(3)
S1 Pt1 S2 O21 -54.5(3)
N12 Pt1 S2 C22 113(6)
O11 Pt1 S2 C22 -110.4(4)
S1 Pt1 S2 C22 68.6(4)
N12 Pt1 S2 C21 -136(6)
O11 Pt1 S2 C21 0.5(4)
S1 Pt1 S2 C21 179.5(3)
