Hydrogen-bonded linear chain assemblies of palladium(II)-selenoether complexes: solid state aggregates as template for nano-structural Pd17Se15 leading to efficient electrocatalytic activity.
kumbhare, liladhar B.; Singla, Hardik; Prathap, Anu M. U.; Sawant, Shilpa; Wadawale, A. P.; Ruz, Priyanka; Bahadur, Jitendra; Dalton Transactions  (2023) –; doi:10.1039/D3DT02170J

data_7714497
_publ_section_title
;
 Hydrogen-bonded linear chain assemblies of palladium(II)-selenoether
 complexes: solid state aggregates as template for nano-structural
 Pd17Se15 leading to efficient electrocatalytic activity.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02170J
_journal_year                    2023
_chemical_formula_sum            'C13 H16 Cl2 N2 O Pd Se'
_chemical_formula_weight         472.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-06-02 deposited with the CCDC.	2023-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.022(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.6055(2)
_cell_length_b                   14.6919(4)
_cell_length_c                   14.4987(4)
_cell_measurement_reflns_used    42030
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      30.9110
_cell_measurement_theta_min      2.8120
_cell_volume                     1613.85(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.912
_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     16.00  42.00   0.50    0.69    --   -4.75-129.00   6.52   52
  2  \w     17.00  43.00   0.50    0.69    --   -4.75  33.00  82.46   52
  3  \w    -17.00   8.00   0.50    0.69    --   -4.75  19.00 -30.00   50
  4  \w     14.00  44.00   0.50    0.69    --   -4.75-127.00-178.06   60
  5  \w    -17.00   9.00   0.50    0.69    --   -4.75  37.00 -30.00   52
  6  \w    -15.00  46.00   0.50    0.69    --   -4.75  19.00-120.00  122
  7  \w     14.00  39.00   0.50    0.69    --   -4.75-117.00  77.60   50
  8  \w    -18.00  11.00   0.50    0.69    --   -4.75  33.00  82.46   58
  9  \w    -17.00   8.00   0.50    0.69    --   -4.75  37.00 150.00   50
 10  \w    -17.00  11.00   0.50    0.69    --   -4.75  37.00   0.00   56
 11  \w    -17.00   8.00   0.50    0.69    --   -4.75  26.00-149.41   50
 12  \w     17.00  44.00   0.50    0.69    --   -4.75-129.00  43.89   54
 13  \w    -17.00  13.00   0.50    0.69    --   -4.75  37.00  30.00   60
 14  \w    -17.00   9.00   0.50    0.69    --   -4.75  19.00-180.00   52
 15  \w    -59.00   3.00   0.50    0.69    --   -4.75 -19.00 -90.00  124
 16  \w    -16.00  33.00   0.50    0.69    --   -4.75  19.00  60.00   98
 17  \w      7.00  38.00   0.50    0.69    --   -4.75-117.00-117.32   62
 18  \w    -13.00  18.00   0.50    0.69    --    5.06 -37.00  30.00   62
 19  \w     -8.00  18.00   0.50    0.69    --    5.06 -37.00 -90.00   52
 20  \w    -10.00  18.00   0.50    0.69    --    5.06 -37.00 120.00   56
 21  \w    -26.00  18.00   0.50    0.69    --    5.06 -37.00  90.00   88
 22  \w    -65.00 -30.00   0.50    0.69    --    5.06 -37.00  90.00   70
 23  \w     -5.00  20.00   0.50    0.69    --    5.06  83.00 -60.52   50
 24  \w    -13.00  13.00   0.50    0.69    --    5.06  94.00  -7.86   52
 25  \w    -17.00  18.00   0.50    0.69    --    5.06 -37.00 150.00   70
 26  \w    -20.00  18.00   0.50    0.69    --    5.06 -37.00 -30.00   76
 27  \w     -7.00  20.00   0.50    0.69    --    5.06  37.00 -90.00   54
 28  \w    -56.00  18.00   0.50    0.69    --    5.06 -37.00-150.00  148
 29  \w    -50.00 -24.00   0.50    0.69    --    5.06 -37.00 150.00   52
 30  \w    -26.00  17.00   0.50    0.69    --    5.06 -37.00 -60.00   86
 31  \w    -61.00 -34.00   0.50    0.69    --    5.06 -37.00 -30.00   54
 32  \w     -8.00  18.00   0.50    0.69    --    5.06 -37.00-120.00   52
 33  \w    -68.00 -39.00   0.50    0.69    --    5.06 -37.00 -60.00   58
 34  \w    -14.00  18.00   0.50    0.69    --    5.06 -37.00   0.00   64
 35  \w    -49.00 -23.00   0.50    0.69    --    5.06 -37.00-120.00   52
 36  \w    -17.00  11.00   0.50    0.69    --   -4.75  37.00 120.00   56
 37  \w     12.00  38.00   0.50    0.69    --   -4.75-118.00-113.65   52
 38  \w    -38.00  -5.00   0.50    0.69    --   -4.75 -19.00   0.00   66
 39  \w    -16.00   9.00   0.50    0.69    --   -4.75  28.00-137.83   50
 40  \w     -8.00  18.00   0.50    0.69    --    5.06 -37.00  60.00   52
 41  \w     -7.00  18.00   0.50    0.69    --    5.06 -37.00 -60.00   50
 42  \w    -52.00 -26.00   0.50    0.69    --    5.06 -37.00 -60.00   52
 43  \w    -16.00   9.00   0.50    0.69    --   -4.75  19.00  30.00   50
 44  \w     45.00  70.00   0.50    0.69    --   -4.75  28.00 -77.62   50
 45  \w    -16.00   9.00   0.50    0.69    --   -4.75  28.00 -77.62   50
 46  \w    -51.00 -23.00   0.50    0.69    --   -4.75   6.00  61.26   56
 47  \w     32.00  58.00   0.50    0.69    --   -4.75  30.00 135.89   52
 48  \w     20.00  45.00   0.50    0.69    --   -4.75-138.00 -49.09   50
 49  \w      5.00  30.00   0.50    0.69    --   -4.75-114.00  -6.41   50
 50  \w    -16.00   9.00   0.50    0.69    --   -4.75  26.00-156.83   50
 51  \w    -17.00   9.00   0.50    0.69    --   -4.75  30.00 135.89   52
 52  \w     -8.00  18.00   0.50    0.69    --    5.06 -37.00-180.00   52
 53  \w    -60.00 -34.00   0.50    0.69    --    5.06 -37.00-180.00   52
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0503313000
_diffrn_orient_matrix_UB_12      0.0331078000
_diffrn_orient_matrix_UB_13      -0.0217116000
_diffrn_orient_matrix_UB_21      -0.0605308000
_diffrn_orient_matrix_UB_22      0.0342255000
_diffrn_orient_matrix_UB_23      0.0110115000
_diffrn_orient_matrix_UB_31      0.0506515000
_diffrn_orient_matrix_UB_32      0.0079994000
_diffrn_orient_matrix_UB_33      0.0426479000
_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  0.0992
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.912
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            87798
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.912
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.961
_diffrn_reflns_theta_min         2.773
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.732
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.945
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.395
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         4664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0677
_refine_ls_R_factor_gt           0.0451
_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/[\s^2^(Fo^2^)+(0.1056P)^2^+4.7987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3809
_reflns_number_total             4664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02170j2.cif
_cod_data_source_block           LBK-6d
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7714497
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.522
_shelx_estimated_absorpt_t_max   0.835
_oxdiff_exptl_absorpt_empirical_full_min 0.575
_oxdiff_exptl_absorpt_empirical_full_max 3.748
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01a963ea59fe6731e72b42baf37aa34c53000290d6c
;
_diffrn_oxdiff_digest_hkl
;
014cf9d87199bf45a17f3108ee3b7dd77b3cc1
;
_shelx_res_checksum              38550