Effect of chalcogen bonding interactions on molecular structures; theoretical and crystallographic studies on two palladium(ii) acetate complexes
Al-Noaimi, Mousa; Awwadi, Firas F.; Hendal, Abdellah; Aljammal, Azzam; Talib, Wamidh H.; Mahmod, Asma Ismail; New Journal of Chemistry 46 (2022) 18551–18562; doi:10.1039/D2NJ01995G

data_7061869
_publ_section_title
;
 Effect of chalcogen bonding interactions on molecular structures;
 theoretical and crystallographic studies on two palladium(ii) acetate
 complexes
;
_journal_issue                   38
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18551
_journal_page_last               18562
_journal_paper_doi               10.1039/D2NJ01995G
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C23 H20 N2 O3 Pd S2, H2 O'
_chemical_formula_sum            'C23 H22 N2 O4 Pd S2'
_chemical_formula_weight         560.94
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-09-05
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-09-05 deposited with the CCDC.	2022-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                82.933(7)
_cell_angle_beta                 86.757(6)
_cell_angle_gamma                70.139(6)
_cell_formula_units_Z            2
_cell_length_a                   9.4336(6)
_cell_length_b                   9.6103(7)
_cell_length_c                   13.3454(11)
_cell_measurement_reflns_used    3856
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8420
_cell_measurement_theta_min      3.7180
_cell_volume                     1129.14(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0534
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.844
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -24.00  44.00   1.00    2.00    --  -16.20  57.00  30.00   68
  2  \w      2.00  79.00   1.00    2.00    --   16.83  57.00   0.00   77
  3  \w      0.00  84.00   1.00    2.00    --   16.83  57.00 -90.00   84
  4  \w    -22.00  14.00   1.00    2.00    --  -16.20 -99.00  90.00   36
  5  \w    -63.00 -31.00   1.00    2.00    --  -16.20 -57.00  60.00   32
  6  \w     32.00  89.00   1.00    2.00    --   16.83-178.00-120.00   57
  7  \w    -13.00  17.00   1.00    2.00    --  -16.20 -99.00-180.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0408456000
_diffrn_orient_matrix_UB_12      0.0405431000
_diffrn_orient_matrix_UB_13      -0.0295842000
_diffrn_orient_matrix_UB_21      -0.0057285000
_diffrn_orient_matrix_UB_22      -0.0349320000
_diffrn_orient_matrix_UB_23      -0.0426926000
_diffrn_orient_matrix_UB_31      -0.0684935000
_diffrn_orient_matrix_UB_32      0.0580551000
_diffrn_orient_matrix_UB_33      -0.0130817000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.844
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9921
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.844
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.450
_diffrn_reflns_theta_min         3.077
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.040
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.650
_exptl_crystal_description       chunk
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5283
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0412
_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/[\s^2^(Fo^2^)+(0.0246P)^2^+0.1489P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4201
_reflns_number_total             5283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj01995g1.cif
_cod_data_source_block           exp_2554
_cod_depositor_comments
'Adding full bibliography for 7061868--7061870.cif.'
_cod_database_code               7061869
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'S Pd N O C H'
_chemical_oxdiff_usercomment     'firas mousa'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C2(H2), C3(H3), C4(H4), C17(H17), C21(H21), C15(H15), C20(H20),
 C18(H18), C11(H11), C14(H14), C19(H19), C13(H13), C12(H12)
2.c Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C00S(H00A,H00B,H00C)
;
_shelx_res_checksum              95066
_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 1.121
_oxdiff_exptl_absorpt_empirical_full_min 0.900