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_7714496
_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            'C24 H36 Cl12 O10 Sn4'
_chemical_formula_weight         1384.69
_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                 96.947(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1566(3)
_cell_length_b                   10.0994(3)
_cell_length_c                   23.0816(6)
_cell_measurement_reflns_used    11733
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      76.0860
_cell_measurement_theta_min      3.8800
_cell_volume                     2350.23(12)
_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 0.996
_diffrn_measured_fraction_theta_max 0.951
_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    -41.00  23.00   0.50    0.15    --  -47.70  40.00  66.00  128
  2  \w   -119.00 -76.00   0.50    0.15    --  -47.70 -40.00 -87.00   86
  3  \w    -72.00 -46.00   0.50    0.15    --  -47.70 -40.00 -87.00   52
  4  \w      8.00  34.00   0.50    0.15    --   47.70 -40.00 -87.00   52
  5  \w   -140.00-115.00   0.50    0.50    --  -86.25 -40.00 -87.00   50
  6  \w    -45.00 -20.00   0.50    0.50    --  -86.25  40.00  66.00   50
  7  \w     97.00 177.00   0.50    0.50    --  107.74  40.00  66.00  160
  8  \w   -119.00 -73.00   0.50    0.15    --  -47.70-125.00-150.00   92
  9  \w     -8.00  24.00   0.50    0.15    --  -47.70  19.00-150.00   64
 10  \w   -116.00 -77.00   0.50    0.15    --  -47.70-125.00  30.00   78
 11  \w     42.00  97.00   0.50    0.15    --   47.70  40.00  66.00  110
 12  \w    -42.00 -14.00   0.50    0.50    --  -86.25  37.00-180.00   56
 13  \w   -132.00 -87.00   0.50    0.50    --  -86.25 -57.00-180.00   90
 14  \w    -63.00 -15.00   0.50    0.50    --  -86.25  57.00-180.00   96
 15  \w    -63.00 -15.00   0.50    0.50    --  -86.25  57.00-120.00   96
 16  \w    -42.00 -14.00   0.50    0.50    --  -86.25  37.00 150.00   56
 17  \w    -41.00 -13.00   0.50    0.50    --  -86.25  37.00  30.00   56
 18  \w     37.00  62.00   0.50    0.50    --  107.74 -57.00   0.00   50
 19  \w    116.00 177.00   0.50    0.50    --  107.74  19.00-180.00  122
 20  \w     37.00  63.00   0.50    0.50    --  107.74 -57.00 -60.00   52
 21  \w     36.00  65.00   0.50    0.50    --  107.74 -57.00 -90.00   58
 22  \w     38.00 104.00   0.50    0.50    --  107.74 -77.00 150.00  132
 23  \w    145.00 170.00   0.50    0.50    --  107.74  57.00   0.00   50
 24  \w     98.00 124.00   0.50    0.50    --  107.74  57.00   0.00   52
 25  \w     67.00  95.00   0.50    0.50    --  107.74 -77.00-120.00   56
 26  \w     43.00 103.00   0.50    0.50    --  107.74 -77.00 -90.00  120
 27  \w     42.00 104.00   0.50    0.50    --  107.74-125.00 -90.00  124
 28  \w     37.00  62.00   0.50    0.50    --  107.74 -77.00-120.00   50
;
_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      -0.1304792000
_diffrn_orient_matrix_UB_12      -0.0768748000
_diffrn_orient_matrix_UB_13      0.0020477000
_diffrn_orient_matrix_UB_21      0.0160935000
_diffrn_orient_matrix_UB_22      0.0133734000
_diffrn_orient_matrix_UB_23      0.0669804000
_diffrn_orient_matrix_UB_31      -0.0779082000
_diffrn_orient_matrix_UB_32      0.1310445000
_diffrn_orient_matrix_UB_33      -0.0055775000
_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  0.0686
_diffrn_reflns_av_unetI/netI     0.0526
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            17484
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.155
_diffrn_reflns_theta_min         3.859
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    23.360
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03597
_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    1.957
_exptl_crystal_description       plate
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.761
_refine_diff_density_min         -1.868
_refine_diff_density_rms         0.204
_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     286
_refine_ls_number_reflns         4732
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1336P)^2^+0.1519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.1821
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4092
_reflns_number_total             4732
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02170j2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7714496
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.203
_shelx_estimated_absorpt_t_max   0.800
_oxdiff_exptl_absorpt_empirical_full_min 0.400
_oxdiff_exptl_absorpt_empirical_full_max 15.526
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_oxdiff_digest_frames
;
012481a7e2a1ff2627d6f7d1e9383c83fd0004704fd
;
_diffrn_oxdiff_digest_hkl
;
01f2eb6257976d2afed4f4d96c9d3a6f2b853a
;
_shelx_res_checksum              72389