Stabilization of Nanoparticles Produced by Hydrogenation of Palladium-N-Heterocyclic Carbene Complexes on the Surface of Graphene and Implications in Catalysis.
Mollar-Cuni, Andrés; Ventura-Espinosa, David; Martín, Santiago; Mayoral, Álvaro; Borja, Pilar; Mata, Jose A.; ACS omega 3 (2018) 15217–15228; doi:10.1021/acsomega.8b02193

data_4516113
_publ_section_title
;
 Stabilization of Nanoparticles Produced by Hydrogenation of
 Palladium-N-Heterocyclic Carbene Complexes on the Surface of Graphene and
 Implications in Catalysis.
;
_journal_issue                   11
_journal_name_full               'ACS omega'
_journal_page_first              15217
_journal_page_last               15228
_journal_paper_doi               10.1021/acsomega.8b02193
_journal_volume                  3
_journal_year                    2018
_chemical_formula_moiety         'C34 H28 Br2 Cl N3 Pd'
_chemical_formula_sum            'C34 H28 Br2 Cl N3 Pd'
_chemical_formula_weight         780.26
_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
_audit_creation_date             2016-10-25
_audit_creation_method
;
Olex2 1.2-alpha
(compiled 2016.10.10 svn.r3347 for OlexSys, GUI svn.r5252)
;
_cell_angle_alpha                72.6495(16)
_cell_angle_beta                 81.6726(15)
_cell_angle_gamma                72.6336(16)
_cell_formula_units_Z            2
_cell_length_a                   9.14864(16)
_cell_length_b                   11.5032(2)
_cell_length_c                   15.6073(3)
_cell_measurement_reflns_used    19566
_cell_measurement_temperature    200.00(14)
_cell_measurement_theta_max      28.7950
_cell_measurement_theta_min      3.3800
_cell_volume                     1493.48(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      200.00(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4051
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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    -88.00 -40.00   0.60    3.00    --  -10.50 154.00 119.23   80
  2  \w    -85.00 -37.00   0.60    3.00    --  -10.50 151.00  23.44   80
  3  \w    -22.00  89.00   0.60    3.00    --   11.52  77.00-180.00  185
  4  \w    -20.00  52.00   0.60    3.00    --   11.52 -99.00  30.00  120
  5  \w    -62.00  40.00   0.60    3.00    --   11.52 -57.00 -90.00  170
  6  \w     35.00 101.00   0.60    3.00    --   11.52 178.00 -60.00  110
  7  \w    -35.00  92.20   0.60    3.00    --   11.52  19.00   0.00  212
  8  \w    -15.00  87.00   0.60    3.00    --   11.52  37.00  90.00  170
  9  \w     35.00  80.00   0.60    3.00    --  -10.50 178.00 -90.00   75
 10  \w    -73.00 -29.80   0.60    3.00    --  -10.50 133.00-149.38   72
 11  \w    -67.00 -22.00   0.60    3.00    --  -10.50 123.00   2.83   75
 12  \w    -73.00 -29.80   0.60    3.00    --  -10.50 133.00 -48.85   72
 13  \w    -74.00 -30.80   0.60    3.00    --  -10.50 136.00 167.50   72
 14  \w    -65.00  37.00   0.60    3.00    --   11.52 -37.00  60.00  170
 15  \w    -78.00 100.20   0.60    3.00    --   11.52   0.00-180.00  297
 16  \w    -78.00 100.20   0.60    3.00    --   11.52   0.00-150.00  297
 17  \w    -78.00  66.00   0.60    3.00    --   11.52   0.00-120.00  240
 18  \w    -67.00  44.00   0.60    3.00    --   11.52 -77.00   0.00  185
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0383255000
_diffrn_orient_matrix_UB_12      -0.0009369000
_diffrn_orient_matrix_UB_13      -0.0427816000
_diffrn_orient_matrix_UB_21      -0.0354406000
_diffrn_orient_matrix_UB_22      -0.0457778000
_diffrn_orient_matrix_UB_23      -0.0026727000
_diffrn_orient_matrix_UB_31      -0.0624411000
_diffrn_orient_matrix_UB_32      0.0490484000
_diffrn_orient_matrix_UB_33      -0.0209321000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0484
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60406
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.893
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.416
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (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            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.735
_exptl_crystal_description       trapezoid
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.313
_exptl_crystal_size_mid          0.164
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.604
_refine_diff_density_min         -0.453
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6105
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0268
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.5298P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0700
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5388
_reflns_number_total             6105
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao8b02193_si_002.cif
_cod_data_source_block           str1874
_cod_original_cell_volume        1493.47(5)
_cod_database_code               4516113
_chemical_oxdiff_formula         'C34 H28 N3 Br2 Pd Cl'
_reflns_odcompleteness_completeness 99.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C30(H30), C24(H24), C18(H18), C25(H25), C10(H10), C37(H37),
 C13(H13), C6(H6), C19(H19), C14(H14), C35(H35), C8(H8), C7(H7), C28(H28),
 C26(H26), C27(H27)
2.c Idealised Me refined as rotating group:
 C39(H39A,H39B,H39C), C41(H41A,H41B,H41C), C40(H40A,H40B,H40C)
;
_shelx_res_checksum              52263
_shelx_hkl_checksum              83028
_shelx_shelxl_version_number     2014/7
_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 1.291
_oxdiff_exptl_absorpt_empirical_full_min 0.794