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_7714495
_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            'C36 H76 O10 Sn4'
_chemical_formula_weight         1143.72
_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     iterative
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-06-08 deposited with the CCDC.	2023-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.829(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.3594(3)
_cell_length_b                   10.2558(2)
_cell_length_c                   23.2596(5)
_cell_measurement_reflns_used    11052
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.9810
_cell_measurement_theta_min      3.8520
_cell_volume                     2458.41(10)
_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    'OLEX 1.2'
_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 0.998
_diffrn_measured_fraction_theta_max 0.963
_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      6.00  33.00   0.50    0.22    --   47.82 -49.00  25.00   54
  2  \w     35.00  65.00   0.50    0.89    --  107.74 -57.00 -90.00   60
  3  \w     37.00  64.00   0.50    0.89    --  107.74 -57.00 -60.00   54
  4  \w     61.00 105.00   0.50    0.89    --  107.74 -77.00 -30.00   88
  5  \w     79.00 105.00   0.50    0.89    --  107.74 -99.00  30.00   52
  6  \w     38.00 102.00   0.50    0.89    --  107.74 -77.00 120.00  128
  7  \w    137.00 178.00   0.50    0.89    --  107.74  19.00  90.00   82
  8  \w     95.00 177.00   0.50    0.89    --  107.74  49.00 173.00  164
  9  \w    148.00 178.00   0.50    0.89    --  107.74 125.00  60.00   60
 10  \w     96.00 121.00   0.50    0.89    --  107.74 125.00  60.00   50
 11  \w     40.00  93.00   0.50    0.22    --   47.82  49.00 173.00  106
 12  \w     95.00 120.00   0.50    0.89    --  107.74  19.00  90.00   50
 13  \w     37.00  94.00   0.50    0.89    --  107.74 -77.00  60.00  114
 14  \w     35.00  64.00   0.50    0.89    --  107.74 -99.00  30.00   58
 15  \w     36.00  66.00   0.50    0.89    --  107.74 -57.00-120.00   60
 16  \w     36.00  66.00   0.50    0.89    --  107.74 -57.00-180.00   60
 17  \w     46.00  96.00   0.50    0.89    --  107.74 -77.00-180.00  100
 18  \w     38.00  63.00   0.50    0.89    --  107.74 -57.00-150.00   50
 19  \w    -55.00  -7.00   0.50    0.22    --  -47.82  49.00 173.00   96
 20  \w     -4.00  25.00   0.50    0.22    --  -47.82  49.00 173.00   58
 21  \w    -42.00 -16.00   0.50    0.89    --  -86.25  49.00 173.00   52
 22  \w    -98.00 -73.00   0.50    0.89    --  -86.25 -49.00  25.00   50
 23  \w   -119.00 -48.00   0.50    0.22    --  -47.82 -49.00  25.00  142
 24  \w   -117.00 -73.00   0.50    0.22    --  -47.82-125.00 -30.00   88
 25  \w   -117.00 -73.00   0.50    0.22    --  -47.82-125.00-180.00   88
 26  \w    -42.00 -17.00   0.50    0.89    --  -86.25  37.00 -30.00   50
 27  \w    -86.00 -59.00   0.50    0.89    --  -86.25 125.00-150.00   54
 28  \w    -55.00 -14.00   0.50    0.89    --  -86.25 125.00-150.00   82
 29  \w    -39.00 -13.00   0.50    0.89    --  -86.25  37.00-150.00   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      -0.1241492000
_diffrn_orient_matrix_UB_12      -0.0154698000
_diffrn_orient_matrix_UB_13      -0.0418883000
_diffrn_orient_matrix_UB_21      0.0580054000
_diffrn_orient_matrix_UB_22      0.0900205000
_diffrn_orient_matrix_UB_23      -0.0437715000
_diffrn_orient_matrix_UB_31      0.0597908000
_diffrn_orient_matrix_UB_32      -0.1192285000
_diffrn_orient_matrix_UB_33      -0.0276015000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17696
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.240
_diffrn_reflns_theta_min         3.821
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.330
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06419
_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            colourless
_exptl_crystal_density_diffrn    1.545
_exptl_crystal_description       plate
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.365
_refine_diff_density_min         -1.596
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5020
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0532
_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^)+(0.1012P)^2^+0.9137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1506
_refine_ls_wR_factor_ref         0.1580
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4219
_reflns_number_total             5020
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02170j2.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7714495
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.139
_shelx_estimated_absorpt_t_max   0.292
_oxdiff_exptl_absorpt_empirical_full_min 0.370
_oxdiff_exptl_absorpt_empirical_full_max 11.989
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
01185fb185533b55f7e5b003430d8dcb7c00036345b
;
_diffrn_oxdiff_digest_hkl
;
01125ccddc47acd78975197b1c19d6257ad536
;
_shelx_res_checksum              74382