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#$Date: 2019-11-24 00:41:46 +0200 (Sun, 24 Nov 2019) $
#$Revision: 235813 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/97/4349768.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_4349768
loop_
_publ_author_name
'Matesanz, Ana I.'
'Jimenez-Faraco, Eva'
'Ruiz, María C.'
'Balsa, Lucia M.'
'Navarro-Ranninger, Carmen'
'León, Ignacio E.'
'Quiroga, Adoracion G.'
_publ_section_title
;
 Mononuclear Pd(ii) and Pt(ii) complexes with an α-N-heterocyclic
 thiosemicarbazone: cytotoxicity, solution behaviour and interaction
 versus proven models from biological media
;
_journal_issue                   1
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              73
_journal_paper_doi               10.1039/C7QI00446J
_journal_volume                  5
_journal_year                    2018
_chemical_formula_sum            'C14 H16 Cl N4 O Pd0.5 S2'
_chemical_formula_weight         409.08
_chemical_name_common            Pd(LH)2
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_update_record
;
2016-11-10 deposited with the CCDC.
2017-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.995(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.627(4)
_cell_length_b                   5.7150(18)
_cell_length_c                   20.939(7)
_cell_measurement_reflns_used    5278
_cell_measurement_temperature    296.(2)
_cell_measurement_theta_max      21.9934
_cell_measurement_theta_min      2.4965
_cell_volume                     1743.7(9)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0538
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            26868
_diffrn_reflns_theta_full        25.37
_diffrn_reflns_theta_max         25.37
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.964
_exptl_absorpt_correction_T_max  0.95
_exptl_absorpt_correction_T_min  0.86
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             832
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.665
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0761P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1064
_refine_ls_wR_factor_ref         0.1297
_reflns_number_gt                2251
_reflns_number_total             3189
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7qi00446j2.cif
_cod_data_source_block           DocenciaInorganica01642
_cod_original_formula_sum        'C14 H16 Cl N4 O Pd0.50 S2'
_cod_database_code               4349768
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
C C1 0.4391(3) 1.1616(8) 0.3988(2) 0.0594(11) Uani d . . . 1
H H1 0.3834 1.2344 0.4044 0.071 Uiso calc U . R 1
C C2 0.4337(3) 0.9777(8) 0.3524(2) 0.0588(11) Uani d . . . 1
C C3 0.3567(3) 0.8951(11) 0.3168(2) 0.0762(13) Uani d . . . 1
H H3 0.2979 0.9574 0.3161 0.091 Uiso calc U . R 1
C C4 0.3822(4) 0.7046(10) 0.2825(2) 0.0803(15) Uani d . . . 1
H H4 0.3437 0.615 0.2545 0.096 Uiso calc U . R 1
C C5 0.4740(4) 0.6700(8) 0.2968(2) 0.0751(14) Uani d . . . 1
H H5 0.5092 0.5525 0.2804 0.09 Uiso calc U . R 1
C C6 0.6611(3) 1.2155(7) 0.46275(18) 0.0483(9) Uani d . . . 1
C C7 0.7776(3) 0.9927(7) 0.4088(2) 0.0500(10) Uani d . . . 1
C C8 0.7332(3) 0.7854(7) 0.39172(19) 0.0529(10) Uani d . . . 1
H H8 0.6807 0.7425 0.4109 0.063 Uiso calc U . R 1
C C9 0.7669(3) 0.6417(8) 0.3461(2) 0.0569(11) Uani d . . . 1
H H9 0.7368 0.5032 0.3339 0.068 Uiso calc U . R 1
C C10 0.8450(3) 0.7057(8) 0.31894(19) 0.0558(11) Uani d . . . 1
C C11 0.8903(3) 0.9076(9) 0.3361(2) 0.0633(11) Uani d . . . 1
H H11 0.9437 0.9471 0.3177 0.076 Uiso calc U . R 1
C C12 0.8563(3) 1.0529(8) 0.3811(2) 0.0621(12) Uani d . . . 1
H H12 0.8866 1.1916 0.3926 0.075 Uiso calc U . R 1
C C13 0.8922(4) 0.7590(10) 0.5501(3) 0.108(2) Uani d . . . 1
H H13A 0.925 0.8154 0.5154 0.162 Uiso calc U . R 1
H H13B 0.8966 0.8716 0.5843 0.162 Uiso calc U . R 1
H H13C 0.8289 0.7357 0.5353 0.162 Uiso calc U . R 1
C C14 0.8670(5) 0.4479(12) 0.6393(3) 0.108(2) Uani d . . . 1
H H14A 0.8041 0.4532 0.6219 0.162 Uiso calc U . R 1
H H14B 0.8774 0.5667 0.6716 0.162 Uiso calc U . R 1
H H14C 0.88 0.2971 0.6581 0.162 Uiso calc U . R 1
Cl Cl1 0.88964(11) 0.5218(2) 0.26268(7) 0.0850(4) Uani d . . . 1
N N1 0.5082(2) 1.2433(6) 0.43421(14) 0.0478(8) Uani d . . . 1
N N2 0.5938(2) 1.1415(6) 0.42365(15) 0.0508(8) Uani d . . . 1
N N3 0.5043(2) 0.8357(6) 0.33876(16) 0.0607(9) Uani d . . . 1
H H3N 0.5602 0.8503 0.3547 0.073 Uiso calc U . R 1
N N4 0.7481(2) 1.1417(6) 0.45659(16) 0.0583(9) Uani d . . . 1
H H4N 0.7897 1.1912 0.4849 0.07 Uiso calc U . R 1
O O1 0.9113(2) 0.3223(6) 0.52736(18) 0.0903(11) Uani d . . . 1
Pd Pd1 0.5 1.5 0.5 0.04589(19) Uani d . P S 1
S S1 0.65102(8) 1.4163(2) 0.52398(6) 0.0639(3) Uani d . . . 1
S S2 0.93938(9) 0.4971(2) 0.57771(7) 0.0699(4) Uani d . . . 1
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'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
N1 C1 C2 . . 130.7(4)
N3 C2 C3 . . 106.3(4)
N3 C2 C1 . . 125.6(4)
C3 C2 C1 . . 127.9(4)
C2 C3 C4 . . 108.0(5)
C5 C4 C3 . . 107.8(4)
N3 C5 C4 . . 107.8(4)
N2 C6 N4 . . 120.4(3)
N2 C6 S1 . . 125.0(3)
N4 C6 S1 . . 114.6(3)
C12 C7 C8 . . 119.7(4)
C12 C7 N4 . . 117.8(4)
C8 C7 N4 . . 122.4(4)
C7 C8 C9 . . 120.0(4)
C10 C9 C8 . . 119.2(4)
C11 C10 C9 . . 121.4(4)
C11 C10 Cl1 . . 119.1(3)
C9 C10 Cl1 . . 119.6(4)
C10 C11 C12 . . 119.6(4)
C7 C12 C11 . . 120.1(4)
C1 N1 N2 . . 115.0(3)
C1 N1 Pd1 . . 124.4(3)
N2 N1 Pd1 . . 120.7(2)
C6 N2 N1 . . 113.7(3)
C5 N3 C2 . . 110.1(4)
C6 N4 C7 . . 127.0(3)
N1 Pd1 N1 3_686 . 180.0
N1 Pd1 S1 3_686 . 96.67(9)
N1 Pd1 S1 . . 83.33(9)
N1 Pd1 S1 3_686 3_686 83.33(9)
N1 Pd1 S1 . 3_686 96.67(9)
S1 Pd1 S1 . 3_686 180.0
C6 S1 Pd1 . . 96.87(14)
O1 S2 C13 . . 105.5(3)
O1 S2 C14 . . 105.4(3)
C13 S2 C14 . . 97.8(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
C1 N1 . 1.288(5)
C1 C2 . 1.428(6)
C2 N3 . 1.364(5)
C2 C3 . 1.378(6)
C3 C4 . 1.374(7)
C4 C5 . 1.364(7)
C5 N3 . 1.340(5)
C6 N2 . 1.296(5)
C6 N4 . 1.357(5)
C6 S1 . 1.736(4)
C7 C12 . 1.378(6)
C7 C8 . 1.383(5)
C7 N4 . 1.410(5)
C8 C9 . 1.383(5)
C9 C10 . 1.369(6)
C10 C11 . 1.363(6)
C10 Cl1 . 1.747(4)
C11 C12 . 1.380(6)
C13 S2 . 1.727(6)
C14 S2 . 1.761(7)
N1 N2 . 1.415(4)
N1 Pd1 . 2.023(3)
O1 S2 . 1.484(3)
Pd1 N1 3_686 2.023(3)
Pd1 S1 . 2.2731(12)
Pd1 S1 3_686 2.2731(12)
