Preparation and characterization of colloidal Pd17Se15 nanoparticles from a novel Pd(II) pyridyl selenoether molecular precursor
Karmakar, Gourab; Tyagi, Adish; Kedarnath, G.; Naveen Kumar, N.; Phadnis, Prasad P.; Mishra, Ratikanta; Kumar, Mukesh; Inorganica Chimica Acta 529 (2022) 120668–; doi:10.1016/j.ica.2021.120668

data_1566024
_publ_section_title
;
 Preparation and characterization of colloidal Pd17Se15 nanoparticles from
 a novel Pd(II) pyridyl selenoether molecular precursor
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              120668
_journal_paper_doi               10.1016/j.ica.2021.120668
_journal_volume                  529
_journal_year                    2022
_chemical_formula_moiety         'C14 H12 Cl2 N2 O4 Pd Se2'
_chemical_formula_sum            'C14 H12 Cl2 N2 O4 Pd Se2'
_chemical_formula_weight         607.48
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   25.3661(9)
_cell_length_b                   25.3661(9)
_cell_length_c                   17.4250(11)
_cell_measurement_reflns_used    3053
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.2870
_cell_measurement_theta_min      5.4560
_cell_volume                     9709.8(8)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.1600
_diffrn_detector_type            Titan
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.956
_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    -66.00  33.00   1.00    5.00    --  -43.29  19.00-150.00   99
  2  \w     78.00 153.00   1.00   35.00    --  102.90  61.00 120.00   75
  3  \w    100.00 130.00   1.00   35.00    --  102.90 -61.00 -30.00   30
  4  \w     40.00  75.00   1.00   35.00    --  102.90 -61.00 -30.00   35
  5  \w     20.00  48.00   1.00   35.00    --  102.90 -95.00   0.00   28
  6  \w     25.00  91.00   1.00   35.00    --  102.90 -95.00 -30.00   66
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0323479000
_diffrn_orient_matrix_UB_12      -0.0369563000
_diffrn_orient_matrix_UB_13      0.0132076000
_diffrn_orient_matrix_UB_21      -0.0469954000
_diffrn_orient_matrix_UB_22      -0.0510244000
_diffrn_orient_matrix_UB_23      -0.0520094000
_diffrn_orient_matrix_UB_31      0.0407209000
_diffrn_orient_matrix_UB_32      0.0308059000
_diffrn_orient_matrix_UB_33      -0.0702903000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            6493
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.047
_diffrn_reflns_theta_min         3.485
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    13.256
_exptl_absorpt_correction_T_max  0.441
_exptl_absorpt_correction_T_min  0.095
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.870
_exptl_crystal_description       needle
_exptl_crystal_F_000             5220
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.105
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.427
_refine_diff_density_min         -1.201
_refine_diff_density_rms         0.176
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2076
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.1154
_refine_ls_R_factor_gt           0.0867
_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^)+(0.1102P)^2^+248.3120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2256
_refine_ls_wR_factor_ref         0.2493
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1511
_reflns_number_total             2076
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ICA-2022-529-120668.cif
_cod_data_source_block           prasad3_1
_cod_original_cell_volume        9709.9(9)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               1566024
_chemical_oxdiff_formula         'C14 H12 Cl2 N2 O4 Pd Se2'
_reflns_odcompleteness_completeness 97.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-08-25
_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 3.593
_oxdiff_exptl_absorpt_empirical_full_min 0.279