Ultra-small palladium nano-particles synthesized using bulky S/Se and N donor ligands as a stabilizer: application as catalysts for Suzuki–Miyaura coupling
Oswal, Preeti; Arora, Aayushi; Kaushal, Jolly; Rao, Gyandshwar Kumar; Kumar, Sushil; Singh, Ajai K.; Kumar, Arun; RSC Advances 9 (2019) 22313–; doi:10.1039/C9RA03498F

data_7234985
_publ_section_title
;
 Ultra-small palladium nano-particles synthesized using bulky S/Se and N
 donor ligands as a stabilizer: application as catalysts for
 Suzuki--Miyaura coupling
;
_journal_issue                   39
_journal_name_full               'RSC Advances'
_journal_page_first              22313
_journal_paper_doi               10.1039/C9RA03498F
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C23 H21 N S'
_chemical_formula_sum            'C23 H21 N S'
_chemical_formula_weight         343.47
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-11-19
_audit_creation_method
;
Olex2 1.2-ac21
(compiled 2015.09.16 svn.r134, GUI svn.r4998)
;
_audit_update_record
;
2018-12-29 deposited with the CCDC.	2019-06-17 downloaded from the CCDC.
;
_cell_angle_alpha                89.910(8)
_cell_angle_beta                 84.752(10)
_cell_angle_gamma                89.905(9)
_cell_formula_units_Z            4
_cell_length_a                   5.3825(7)
_cell_length_b                   15.3166(13)
_cell_length_c                   21.472(3)
_cell_measurement_reflns_used    1902
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      67.0830
_cell_measurement_theta_min      3.5470
_cell_volume                     1762.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 66.00
_diffrn_measured_fraction_theta_max 67.00
_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    -35.00  61.00   1.00    1.00    --   25.51 -57.00-120.00   96
  2  \w     27.00  94.00   1.00    1.00    --   66.75 -77.00-120.00   67
  3  \w     86.00 113.00   1.00    1.00    --   66.75-111.00 -90.00   27
  4  \w     25.00 104.00   1.00    5.00    --  108.00-104.00  60.00   79
  5  \w     19.00  54.00   1.00    1.00    --   66.75-111.00 -90.00   35
  6  \w    -11.00  15.00   1.00    1.00    --   66.75 -77.00-120.00   26
  7  \w     39.00 141.00   1.00    1.00    --   66.75  61.00  60.00  102
  8  \w    144.00 170.00   1.00    5.00    --  108.00  77.00  60.00   26
  9  \w    117.00 178.00   1.00    5.00    --  108.00  54.00   0.00   61
 10  \w    102.00 162.00   1.00    5.00    --  108.00  54.00  60.00   60
 11  \w     86.00 166.00   1.00    5.00    --  108.00 138.00 120.00   80
 12  \w     75.00 105.00   1.00    5.00    --  108.00  54.00   0.00   30
 13  \w     72.00 177.00   1.00    5.00    --  108.00  65.00  30.00  105
 14  \w     72.00 120.00   1.00    5.00    --  108.00  77.00  60.00   48
 15  \w     71.00 166.00   1.00    5.00    --  108.00  77.00  90.00   95
 16  \w     30.00 132.00   1.00    1.00    --   66.75  61.00 120.00  102
 17  \w     11.00 100.00   1.00    1.00    --   25.51  77.00  60.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1399899000
_diffrn_orient_matrix_UB_12      -0.0684964000
_diffrn_orient_matrix_UB_13      0.0424756000
_diffrn_orient_matrix_UB_21      0.2364373000
_diffrn_orient_matrix_UB_22      -0.0572655000
_diffrn_orient_matrix_UB_23      -0.0036148000
_diffrn_orient_matrix_UB_31      0.0843545000
_diffrn_orient_matrix_UB_32      0.0463200000
_diffrn_orient_matrix_UB_33      0.0581110000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5306
_diffrn_reflns_theta_full        66.93
_diffrn_reflns_theta_max         66.93
_diffrn_reflns_theta_min         2.89
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.15000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.289
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.685
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     455
_refine_ls_number_reflns         3982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1042
_refine_ls_R_factor_gt           0.0821
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1828P)^2^+1.8414P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2427
_refine_ls_wR_factor_ref         0.2912
_reflns_number_gt                2938
_reflns_number_total             6305
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9ra03498f2.cif
_cod_data_source_block           rl2_lt_cu
_cod_database_code               7234985
_chemical_oxdiff_formula         'c h n s'
_reflns_odcompleteness_completeness 64.11
_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, All N(H) groups
2.a Riding coordinates:
 N3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B), C13(H13A,H13B), C18(H18A,H18B), C25(H25A,H25B), C33(H33A,H33B),
 C45(H45A,H45B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C12(H12), C16(H16), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24),
 C26(H26), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35),
  C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
 C43(H43), C44(H44), C46(H46), C47(H47), C48(H48)
;
_olex2_date_sample_data_collection 2018-07-24
_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 7.404
_oxdiff_exptl_absorpt_empirical_full_min 0.361