#------------------------------------------------------------------------------
#$Date: 2024-07-05 19:46:42 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293120 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/61/7716168.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_7716168
loop_
_publ_author_name
'Tanwar, Deepika'
'Kaur, Tashmeen'
'Sudheendranath, Athul'
'Kumar, Umesh'
'Sharma, Deepika'
_publ_section_title
;
 Pd(II) complexes bearing NNS pincer ligands: unveiling potent
 cytotoxicity against breast and pancreatic cancer.
;
_journal_issue                   23
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9798
_journal_page_last               9811
_journal_paper_doi               10.1039/d4dt00282b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C17 H13 Cl N2 O Pd S'
_chemical_formula_sum            'C17 H13 Cl N2 O Pd S'
_chemical_formula_weight         435.20
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-12-21
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-17 deposited with the CCDC.	2024-05-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.0594(5)
_cell_length_b                   10.4533(3)
_cell_length_c                   16.3019(4)
_cell_measurement_reflns_used    12484
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      26.8040
_cell_measurement_theta_min      2.2170
_cell_volume                     3247.89(15)
_computing_cell_refinement       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.40.35a (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix3000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00  57.00   0.50   20.00    --  -14.97  73.00 -45.00  204
  2  ω    -62.00  -4.00   0.50   20.00    --  -14.97 117.00  29.00  116
  3  ω     40.00  85.00   0.50   20.00    --   16.22  49.00 160.00   90
  4  ω    -33.00  21.00   0.50   20.00    --  -14.97 -94.00  90.00  108
  5  ω    -32.00  -6.00   0.50   20.00    --  -14.97 -94.00  60.00   52
  6  ω    -37.00  22.00   0.50   20.00    --  -14.97 -94.00 -30.00  118
  7  ω      8.00  36.00   0.50   20.00    --   16.22-117.00 -58.00   56
  8  ω    -30.00  21.00   0.50   20.00    --  -14.97 -94.00-180.00  102
  9  ω      1.00  84.00   0.50   20.00    --   16.22  61.00-180.00  166
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix3000'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0008642000
_diffrn_orient_matrix_UB_12      0.0196783000
_diffrn_orient_matrix_UB_13      -0.0416367000
_diffrn_orient_matrix_UB_21      -0.0221503000
_diffrn_orient_matrix_UB_22      0.0518581000
_diffrn_orient_matrix_UB_23      0.0107556000
_diffrn_orient_matrix_UB_31      0.0298691000
_diffrn_orient_matrix_UB_32      0.0390837000
_diffrn_orient_matrix_UB_33      0.0067741000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            19837
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.929
_diffrn_reflns_theta_min         2.137
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.440
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31493
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.35a (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dull brown'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_description       block
_exptl_crystal_F_000             1728
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.473
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         3391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0610
_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)+(0.0868P)²+13.5905P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1759
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2843
_reflns_number_total             3391
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt00282b2.cif
_cod_data_source_block           exter76
_cod_depositor_comments
'Adding full bibliography for 7716168--7716170.cif.'
_cod_database_code               7716168
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C H N O S Pd'
_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.
;
_olex2_refinement_description
;
1. Uiso/Uaniso restraints and constraints
Uanis(N2) = Uanis(C10) = Uanis(Pd1)
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C7(H7), C8(H8), C13(H13), C14(H14), C15(H15),
 C16(H16), C17(H17)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.487
_oxdiff_exptl_absorpt_empirical_full_min 0.661
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'-x, y, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'x, -y, z-1/2'
'-x-1/2, y-1/2, 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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.4326(4) 0.4702(11) 0.5771(5) 0.086(3) Uani 1 1 d . . . . .
H1 H 0.408962 0.397091 0.559910 0.103 Uiso 1 1 calc R U . . .
C2 C 0.4057(6) 0.5918(15) 0.5570(7) 0.109(4) Uani 1 1 d . . . . .
H2 H 0.363475 0.597742 0.528760 0.131 Uiso 1 1 calc R U . . .
C3 C 0.4389(7) 0.6957(14) 0.5772(9) 0.119(5) Uani 1 1 d . . . . .
H3 H 0.421338 0.774636 0.560762 0.143 Uiso 1 1 calc R U . . .
C4 C 0.5027(6) 0.6899(9) 0.6250(7) 0.091(3) Uani 1 1 d . . . . .
C5 C 0.5260(4) 0.5646(8) 0.6438(5) 0.067(2) Uani 1 1 d . . . . .
C6 C 0.5421(8) 0.7947(10) 0.6530(10) 0.128(7) Uani 1 1 d . . . . .
H6 H 0.526783 0.877128 0.641057 0.154 Uiso 1 1 calc R U . . .
C7 C 0.6018(7) 0.7792(10) 0.6967(9) 0.103(4) Uani 1 1 d . . . . .
H7 H 0.627383 0.849733 0.714427 0.124 Uiso 1 1 calc R U . . .
C8 C 0.6239(5) 0.6562(9) 0.7147(6) 0.085(3) Uani 1 1 d . . . . .
H8 H 0.663937 0.646513 0.746822 0.102 Uiso 1 1 calc R U . . .
C9 C 0.5908(4) 0.5494(7) 0.6884(4) 0.0576(16) Uani 1 1 d . . . . .
C10 C 0.6668(3) 0.3830(6) 0.7403(4) 0.0508(2) Uani 1 1 d . . . . .
C11 C 0.6690(4) 0.2386(7) 0.7573(4) 0.0639(18) Uani 1 1 d . . . . .
H11A H 0.652903 0.223937 0.812929 0.077 Uiso 1 1 calc R U . . .
H11B H 0.717394 0.210345 0.754237 0.077 Uiso 1 1 calc R U . . .
C12 C 0.6702(3) 0.1358(6) 0.5982(4) 0.0507(14) Uani 1 1 d . . . . .
C13 C 0.7291(4) 0.2116(8) 0.5857(5) 0.072(2) Uani 1 1 d . . . . .
H13 H 0.743889 0.270198 0.625010 0.086 Uiso 1 1 calc R U . . .
C14 C 0.7649(5) 0.1967(9) 0.5126(6) 0.087(3) Uani 1 1 d . . . . .
H14 H 0.804700 0.246395 0.503808 0.104 Uiso 1 1 calc R U . . .
C15 C 0.7457(5) 0.1157(9) 0.4545(5) 0.075(2) Uani 1 1 d . . . . .
H15 H 0.771288 0.109557 0.406086 0.090 Uiso 1 1 calc R U . . .
C16 C 0.6866(4) 0.0398(8) 0.4670(5) 0.071(2) Uani 1 1 d . . . . .
H16 H 0.672054 -0.016936 0.426413 0.086 Uiso 1 1 calc R U . . .
C17 C 0.6493(4) 0.0488(7) 0.5400(4) 0.0616(17) Uani 1 1 d . . . . .
H17 H 0.610712 -0.003579 0.549343 0.074 Uiso 1 1 calc R U . . .
Cl1 Cl 0.46247(10) 0.1537(3) 0.59503(15) 0.0845(7) Uani 1 1 d . . . . .
N1 N 0.4906(3) 0.4590(6) 0.6197(4) 0.0602(14) Uani 1 1 d . . . . .
N2 N 0.6120(3) 0.4077(5) 0.6997(3) 0.0508(2) Uani 1 1 d . . . . .
O1 O 0.7172(3) 0.4485(5) 0.7608(3) 0.0745(15) Uani 1 1 d . . . . .
Pd1 Pd 0.54038(2) 0.29681(5) 0.65306(3) 0.0508(2) Uani 1 1 d . . . . .
S1 S 0.61785(9) 0.14208(17) 0.68966(11) 0.0567(4) 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'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
C2 C1 H1 119.7 . . ?
N1 C1 H1 119.7 . . ?
N1 C1 C2 120.6(11) . . ?
C1 C2 H2 119.4 . . ?
C3 C2 C1 121.3(11) . . ?
C3 C2 H2 119.4 . . ?
C2 C3 H3 119.6 . . ?
C2 C3 C4 120.7(10) . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 114.8(11) . . ?
C6 C4 C3 126.4(11) . . ?
C6 C4 C5 118.8(11) . . ?
C4 C5 C9 118.7(9) . . ?
N1 C5 C4 122.3(9) . . ?
N1 C5 C9 119.0(7) . . ?
C4 C6 H6 119.1 . . ?
C7 C6 C4 121.9(10) . . ?
C7 C6 H6 119.1 . . ?
C6 C7 H7 120.7 . . ?
C6 C7 C8 118.7(11) . . ?
C8 C7 H7 120.7 . . ?
C7 C8 H8 118.1 . . ?
C9 C8 C7 123.8(11) . . ?
C9 C8 H8 118.1 . . ?
C5 C9 N2 112.9(6) . . ?
C8 C9 C5 118.0(8) . . ?
C8 C9 N2 129.1(7) . . ?
N2 C10 C11 108.5(6) . . ?
O1 C10 C11 118.6(6) . . ?
O1 C10 N2 132.6(7) . . ?
C10 C11 H11A 108.4 . . ?
C10 C11 H11B 108.4 . . ?
C10 C11 S1 115.5(5) . . ?
H11A C11 H11B 107.5 . . ?
S1 C11 H11A 108.4 . . ?
S1 C11 H11B 108.4 . . ?
C13 C12 S1 123.4(5) . . ?
C17 C12 C13 120.7(6) . . ?
C17 C12 S1 115.9(5) . . ?
C12 C13 H13 121.3 . . ?
C14 C13 C12 117.5(7) . . ?
C14 C13 H13 121.3 . . ?
C13 C14 H14 118.2 . . ?
C15 C14 C13 123.6(8) . . ?
C15 C14 H14 118.2 . . ?
C14 C15 H15 120.5 . . ?
C14 C15 C16 119.0(7) . . ?
C16 C15 H15 120.5 . . ?
C15 C16 H16 120.0 . . ?
C17 C16 C15 120.0(7) . . ?
C17 C16 H16 120.0 . . ?
C12 C17 C16 119.3(7) . . ?
C12 C17 H17 120.3 . . ?
C16 C17 H17 120.3 . . ?
C1 N1 C5 120.2(8) . . ?
C1 N1 Pd1 127.9(7) . . ?
C5 N1 Pd1 111.9(5) . . ?
C9 N2 Pd1 109.9(4) . . ?
C10 N2 C9 118.3(6) . . ?
C10 N2 Pd1 131.6(5) . . ?
N1 Pd1 Cl1 97.6(2) . . ?
N1 Pd1 S1 167.31(18) . . ?
N2 Pd1 Cl1 175.37(17) . . ?
N2 Pd1 N1 86.3(3) . . ?
N2 Pd1 S1 82.25(17) . . ?
S1 Pd1 Cl1 93.69(9) . . ?
C11 S1 C12 103.3(3) . . ?
C11 S1 Pd1 96.6(3) . . ?
C12 S1 Pd1 99.7(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 H1 0.9300 . ?
C1 C2 1.409(15) . ?
C1 N1 1.311(11) . ?
C2 H2 0.9300 . ?
C2 C3 1.299(19) . ?
C3 H3 0.9300 . ?
C3 C4 1.44(2) . ?
C4 C5 1.417(11) . ?
C4 C6 1.406(19) . ?
C5 C9 1.442(11) . ?
C5 N1 1.352(11) . ?
C6 H6 0.9300 . ?
C6 C7 1.352(18) . ?
C7 H7 0.9300 . ?
C7 C8 1.385(15) . ?
C8 H8 0.9300 . ?
C8 C9 1.353(11) . ?
C9 N2 1.547(9) . ?
C10 C11 1.535(10) . ?
C10 N2 1.263(8) . ?
C10 O1 1.225(8) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 S1 1.784(8) . ?
C12 C13 1.390(10) . ?
C12 C17 1.374(10) . ?
C12 S1 1.795(6) . ?
C13 H13 0.9300 . ?
C13 C14 1.382(11) . ?
C14 H14 0.9300 . ?
C14 C15 1.322(12) . ?
C15 H15 0.9300 . ?
C15 C16 1.394(12) . ?
C16 H16 0.9300 . ?
C16 C17 1.389(10) . ?
C17 H17 0.9300 . ?
Cl1 Pd1 2.310(2) . ?
N1 Pd1 2.018(6) . ?
N2 Pd1 1.945(5) . ?
Pd1 S1 2.2699(18) . ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -3.4(18) . . . . ?
C2 C1 N1 C5 -1.1(12) . . . . ?
C2 C1 N1 Pd1 -178.2(6) . . . . ?
C2 C3 C4 C5 2.4(15) . . . . ?
C2 C3 C4 C6 -177.8(11) . . . . ?
C3 C4 C5 C9 177.5(7) . . . . ?
C3 C4 C5 N1 -0.8(11) . . . . ?
C3 C4 C6 C7 -179.3(11) . . . . ?
C4 C5 C9 C8 4.3(10) . . . . ?
C4 C5 C9 N2 -176.3(6) . . . . ?
C4 C5 N1 C1 0.2(10) . . . . ?
C4 C5 N1 Pd1 177.8(6) . . . . ?
C4 C6 C7 C8 -0.5(18) . . . . ?
C5 C4 C6 C7 0.5(16) . . . . ?
C5 C9 N2 C10 -177.7(5) . . . . ?
C5 C9 N2 Pd1 -2.5(6) . . . . ?
C6 C4 C5 C9 -2.4(12) . . . . ?
C6 C4 C5 N1 179.4(8) . . . . ?
C6 C7 C8 C9 2.6(17) . . . . ?
C7 C8 C9 C5 -4.5(13) . . . . ?
C7 C8 C9 N2 176.2(8) . . . . ?
C8 C9 N2 C10 1.6(10) . . . . ?
C8 C9 N2 Pd1 176.8(7) . . . . ?
C9 C5 N1 C1 -178.0(6) . . . . ?
C9 C5 N1 Pd1 -0.5(7) . . . . ?
C10 C11 S1 C12 77.0(6) . . . . ?
C10 C11 S1 Pd1 -24.7(5) . . . . ?
C11 C10 N2 C9 169.1(5) . . . . ?
C11 C10 N2 Pd1 -4.9(8) . . . . ?
C12 C13 C14 C15 0.6(15) . . . . ?
C13 C12 C17 C16 -1.9(11) . . . . ?
C13 C12 S1 C11 -10.1(7) . . . . ?
C13 C12 S1 Pd1 89.1(6) . . . . ?
C13 C14 C15 C16 -0.5(16) . . . . ?
C14 C15 C16 C17 -0.8(14) . . . . ?
C15 C16 C17 C12 2.0(12) . . . . ?
C17 C12 C13 C14 0.7(12) . . . . ?
C17 C12 S1 C11 169.0(5) . . . . ?
C17 C12 S1 Pd1 -91.8(5) . . . . ?
N1 C1 C2 C3 2.8(16) . . . . ?
N1 C5 C9 C8 -177.4(7) . . . . ?
N1 C5 C9 N2 2.0(8) . . . . ?
N2 C10 C11 S1 21.5(7) . . . . ?
O1 C10 C11 S1 -153.1(6) . . . . ?
O1 C10 N2 C9 -17.4(10) . . . . ?
O1 C10 N2 Pd1 168.7(6) . . . . ?
S1 C12 C13 C14 179.7(7) . . . . ?
S1 C12 C17 C16 179.0(6) . . . . ?
