#------------------------------------------------------------------------------
#$Date: 2019-11-05 11:22:48 +0100 (mar 05 de nov de 2019) $
#$Revision: 223327 $
#$URL: svn://www.crystallography.net/cod/cif/7/70/16/7701654.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_7701654
loop_
_publ_author_name
'Kalaiarasi, G.'
'Dharani, S.'
'Lynch, V. M.'
'Prabhakaran, R.'
_publ_section_title
;
 para metallation of 3-acetyl-chromen-2-one Schiff bases in tetranuclear
 palladacycles: focus on their biomolecular interaction and in vitro
 cytotoxicity.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12496
_journal_page_last               12511
_journal_paper_doi               10.1039/c9dt02663k
_journal_volume                  48
_journal_year                    2019
_chemical_formula_sum            'C52 H44 N12 O8 Pd4 S4'
_chemical_formula_weight         1518.83
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2019-07-19 deposited with the CCDC.	2019-07-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3910(17)
_cell_length_b                   14.3910(17)
_cell_length_c                   36.358(4)
_cell_measurement_reflns_used    4390
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.00
_cell_volume                     7529.8(15)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2015)'
_computing_structure_solution
;

SHELXT. G. M. Sheldrick (2015). Acta Cryst. A71, 3-8.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC-12 with a Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0747
_diffrn_reflns_av_unetI/netI     0.0559
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            29266
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.005
_diffrn_source                   'sealed fine focus tube'
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.769
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor.  T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.340
_exptl_crystal_description       prism
_exptl_crystal_F_000             3008
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.901
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         4310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0847
_refine_ls_R_factor_gt           0.0660
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0210P)²+67.6145P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1060
_refine_ls_wR_factor_ref         0.1120
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3416
_reflns_number_total             4310
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02663k2.cif
_cod_data_source_block           PDA3
_cod_original_cell_volume        7530(2)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               7701654
_shelx_shelxl_version_number     2016/6
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_platon_squeeze_void_probe_radius 1.20
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
C1 C 0.6283(3) 0.7856(4) 0.72086(12) 0.0307(11) Uani 1 1 d . .
C2 C 0.6597(3) 0.8770(4) 0.73267(13) 0.0350(13) Uani 1 1 d . .
C3 C 0.6732(4) 0.9538(4) 0.70958(15) 0.0407(13) Uani 1 1 d . .
H3 H 0.663828 0.946856 0.683864 0.049 Uiso 1 1 calc R U
C4 C 0.6999(4) 1.0393(4) 0.72327(16) 0.0459(15) Uani 1 1 d . .
H4 H 0.707490 1.090619 0.707103 0.055 Uiso 1 1 calc R U
C5 C 0.7155(4) 1.0502(5) 0.76083(17) 0.0493(16) Uani 1 1 d . .
H5 H 0.734832 1.108681 0.770204 0.059 Uiso 1 1 calc R U
C6 C 0.7033(4) 0.9770(5) 0.78419(16) 0.0489(16) Uani 1 1 d . .
H6 H 0.714553 0.984045 0.809785 0.059 Uiso 1 1 calc R U
C7 C 0.6743(4) 0.8930(4) 0.77022(14) 0.0387(13) Uani 1 1 d . .
C8 C 0.6330(4) 0.7368(4) 0.78655(14) 0.0397(14) Uani 1 1 d . .
C9 C 0.6146(3) 0.7184(4) 0.74766(12) 0.0326(12) Uani 1 1 d . .
C10 C 0.5836(4) 0.6256(4) 0.73651(13) 0.0346(13) Uani 1 1 d . .
C11 C 0.5561(4) 0.5261(4) 0.65076(13) 0.0334(12) Uani 1 1 d . .
C12 C 0.5570(4) 0.5490(4) 0.76189(13) 0.0398(13) Uani 1 1 d . .
H12A H 0.519396 0.503251 0.748570 0.060 Uiso 1 1 calc R U
H12B H 0.520797 0.574356 0.782408 0.060 Uiso 1 1 calc R U
H12C H 0.613139 0.518965 0.771417 0.060 Uiso 1 1 calc R U
C13 C 0.4855(6) 0.3727(4) 0.65280(17) 0.0604(19) Uani 1 1 d . .
H13A H 0.534442 0.339977 0.666324 0.091 Uiso 1 1 calc R U
H13B H 0.456802 0.330275 0.635047 0.091 Uiso 1 1 calc R U
H13C H 0.438200 0.394860 0.670114 0.091 Uiso 1 1 calc R U
N1 N 0.5813(3) 0.6159(3) 0.70086(10) 0.0303(10) Uani 1 1 d . .
N2 N 0.5554(3) 0.5298(3) 0.68667(11) 0.0363(11) Uani 1 1 d . .
N3 N 0.5251(4) 0.4507(3) 0.63360(11) 0.0422(12) Uani 1 1 d . .
H3N H 0.529009 0.448299 0.609468 0.051 Uiso 1 1 calc R U
O1 O 0.6616(3) 0.8239(3) 0.79593(9) 0.0429(10) Uani 1 1 d . .
O2 O 0.6265(3) 0.6812(3) 0.81177(10) 0.0507(11) Uani 1 1 d . .
Pd1 Pd 0.60779(3) 0.72704(3) 0.66964(2) 0.02894(12) Uani 1 1 d . .
S1 S 0.59943(10) 0.61793(10) 0.62180(3) 0.0336(3) Uani 1 1 d . .
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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C9 C1 C2 117.8(4) . .
C9 C1 Pd1 109.2(4) . .
C2 C1 Pd1 132.8(4) . .
C7 C2 C3 115.7(5) . .
C7 C2 C1 118.9(5) . .
C3 C2 C1 125.4(5) . .
C4 C3 C2 121.7(5) . .
C4 C3 H3 119.2 . .
C2 C3 H3 119.2 . .
C3 C4 C5 119.8(6) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
C6 C5 C4 120.2(6) . .
C6 C5 H5 119.9 . .
C4 C5 H5 119.9 . .
C5 C6 C7 119.2(5) . .
C5 C6 H6 120.4 . .
C7 C6 H6 120.4 . .
C6 C7 O1 115.1(5) . .
C6 C7 C2 123.4(6) . .
O1 C7 C2 121.5(5) . .
O2 C8 O1 116.0(5) . .
O2 C8 C9 126.4(6) . .
O1 C8 C9 117.6(5) . .
C1 C9 C8 121.8(5) . .
C1 C9 C10 119.0(4) . .
C8 C9 C10 119.2(5) . .
N1 C10 C9 112.3(5) . .
N1 C10 C12 122.1(5) . .
C9 C10 C12 125.6(4) . .
N2 C11 N3 120.0(5) . .
N2 C11 S1 123.9(4) . .
N3 C11 S1 116.2(4) . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
N3 C13 H13A 109.5 . .
N3 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
N3 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C10 N1 N2 118.0(4) . .
C10 N1 Pd1 118.3(4) . .
N2 N1 Pd1 123.6(3) . .
C11 N2 N1 113.8(4) . .
C11 N3 C13 122.8(5) . .
C11 N3 H3N 118.6 . .
C13 N3 H3N 118.6 . .
C8 O1 C7 122.3(4) . .
N1 Pd1 C1 80.87(19) . .
N1 Pd1 S1 174.37(12) . 12_767
C1 Pd1 S1 104.58(16) . 12_767
N1 Pd1 S1 82.87(12) . .
C1 Pd1 S1 161.58(15) . .
S1 Pd1 S1 91.95(4) 12_767 .
N1 Pd1 Pd1 88.88(12) . 6_564
C1 Pd1 Pd1 93.14(13) . 6_564
S1 Pd1 Pd1 89.39(4) 12_767 6_564
S1 Pd1 Pd1 95.12(4) . 6_564
C11 S1 Pd1 102.99(18) . 15_566
C11 S1 Pd1 94.31(17) . .
Pd1 S1 Pd1 114.53(6) 15_566 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 C9 1.387(7) .
C1 C2 1.455(7) .
C1 Pd1 2.065(5) .
C2 C7 1.400(7) .
C2 C3 1.402(8) .
C3 C4 1.382(8) .
C3 H3 0.9500 .
C4 C5 1.393(8) .
C4 H4 0.9500 .
C5 C6 1.364(9) .
C5 H5 0.9500 .
C6 C7 1.377(8) .
C6 H6 0.9500 .
C7 O1 1.377(7) .
C8 O2 1.220(7) .
C8 O1 1.362(7) .
C8 C9 1.463(7) .
C9 C10 1.465(8) .
C10 N1 1.304(6) .
C10 C12 1.488(7) .
C11 N2 1.306(6) .
C11 N3 1.329(7) .
C11 S1 1.801(5) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 N3 1.439(7) .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
N1 N2 1.394(6) .
N1 Pd1 1.997(4) .
N3 H3N 0.8800 .
Pd1 S1 2.3439(14) 12_767
Pd1 S1 2.3463(13) .
Pd1 Pd1 3.1719(9) 6_564
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
N3 H3N O2 0.88 2.10 2.891(6) 149.4 7_544
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
_geom_torsion_site_symmetry_4
C9 C1 C2 C7 -0.2(7) .
Pd1 C1 C2 C7 -174.4(4) .
C9 C1 C2 C3 -177.2(5) .
Pd1 C1 C2 C3 8.6(8) .
C7 C2 C3 C4 0.4(8) .
C1 C2 C3 C4 177.5(5) .
C2 C3 C4 C5 1.2(9) .
C3 C4 C5 C6 -1.0(9) .
C4 C5 C6 C7 -0.7(9) .
C5 C6 C7 O1 -178.4(5) .
C5 C6 C7 C2 2.4(9) .
C3 C2 C7 C6 -2.2(8) .
C1 C2 C7 C6 -179.5(5) .
C3 C2 C7 O1 178.7(5) .
C1 C2 C7 O1 1.4(8) .
C2 C1 C9 C8 -1.5(7) .
Pd1 C1 C9 C8 174.0(4) .
C2 C1 C9 C10 -179.6(4) .
Pd1 C1 C9 C10 -4.1(6) .
O2 C8 C9 C1 -177.0(5) .
O1 C8 C9 C1 2.0(7) .
O2 C8 C9 C10 1.1(8) .
O1 C8 C9 C10 -179.9(4) .
C1 C9 C10 N1 6.3(7) .
C8 C9 C10 N1 -171.9(4) .
C1 C9 C10 C12 -173.6(5) .
C8 C9 C10 C12 8.2(8) .
C9 C10 N1 N2 178.3(4) .
C12 C10 N1 N2 -1.8(7) .
C9 C10 N1 Pd1 -5.3(6) .
C12 C10 N1 Pd1 174.6(4) .
N3 C11 N2 N1 -174.2(4) .
S1 C11 N2 N1 7.1(7) .
C10 N1 N2 C11 -179.3(5) .
Pd1 N1 N2 C11 4.5(6) .
N2 C11 N3 C13 3.4(9) .
S1 C11 N3 C13 -177.9(5) .
O2 C8 O1 C7 178.3(5) .
C9 C8 O1 C7 -0.8(7) .
C6 C7 O1 C8 179.9(5) .
C2 C7 O1 C8 -0.8(8) .
N2 C11 S1 Pd1 -128.6(4) 15_566
N3 C11 S1 Pd1 52.6(4) 15_566
N2 C11 S1 Pd1 -12.2(5) .
N3 C11 S1 Pd1 169.0(4) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.118 0.714 0.248 2883 991 ' '
