Ultra-small Pd Nanoparticles Derived from Supramolecular Assembly for Enhanced Electrochemical Reduction of CO2 to CO
Chen, Ruru; Cao, Minna; Yang, Weiguang; Wang, Huimin; Zhang, Suyuan; Li, Hongfang; Cao, Rong; Chemical Communications  (2019) –; doi:10.1039/C9CC02393C

data_7123886
_publ_section_title
;
 Ultra-small Pd Nanoparticles Derived from Supramolecular Assembly for
 Enhanced Electrochemical Reduction of CO2 to CO
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC02393C
_journal_year                    2019
_chemical_formula_moiety         'Cl4 Pd, C40 H50 N20 O10, 4(H2 O), H4 O, O'
_chemical_formula_sum            'C40 H62 Cl4 N20 O16 Pd'
_chemical_formula_weight         1327.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-01-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-01 deposited with the CCDC.    2019-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.1030(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.1597(2)
_cell_length_b                   17.5930(2)
_cell_length_c                   22.3163(3)
_cell_measurement_reflns_used    6239
_cell_measurement_temperature    295.00(10)
_cell_measurement_theta_max      73.2200
_cell_measurement_theta_min      3.9450
_cell_volume                     5146.16(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5594
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
  1 omega   30.00   84.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -       40.1492   57.0000   30.0000 54

  2 omega   32.00  118.00   1.0000    6.3900
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -30.0000  -90.0000 86

  3 omega   76.00  178.00   1.0000    6.3900
omega____ theta____ kappa____ phi______ frames
    -      106.2872   30.0000 -150.0000 102

  4 omega  106.00  135.00   1.0000    6.3900
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -61.0000   30.0000 29

  5 omega   62.00   91.00   1.0000    6.3900
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -61.0000   30.0000 29

  6 omega   32.00   97.00   1.0000    6.3900
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -94.0000  -60.0000 65

  7 omega   22.00  108.00   1.0000    6.3900
omega____ theta____ kappa____ phi______ frames
    -      106.2872  -94.0000  120.0000 86

  8 omega  -70.00   27.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -      -40.1492   57.0000 -120.0000 97

  9 omega  -92.00  -12.00   1.0000    1.6000
omega____ theta____ kappa____ phi______ frames
    -      -40.1492  -57.0000   60.0000 80

 10 omega   71.00  157.00   1.0000    6.3900
omega____ theta____ kappa____ phi______ frames
    -      106.2872  165.0000   -8.0000 86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0254730000
_diffrn_orient_matrix_UB_12      -0.0819097000
_diffrn_orient_matrix_UB_13      -0.0178946000
_diffrn_orient_matrix_UB_21      0.1033077000
_diffrn_orient_matrix_UB_22      0.0273325000
_diffrn_orient_matrix_UB_23      -0.0195057000
_diffrn_orient_matrix_UB_31      0.0498860000
_diffrn_orient_matrix_UB_32      -0.0145627000
_diffrn_orient_matrix_UB_33      0.0640627000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0163
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10723
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.431
_diffrn_reflns_theta_min         3.978
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.606
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_F_000             2736
_refine_diff_density_max         1.109
_refine_diff_density_min         -1.019
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     378
_refine_ls_number_reflns         5032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0877P)^2^+12.9578P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4642
_reflns_number_total             5032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc02393c2.cif
_cod_data_source_block           PdCl4-Me10CB[5]
_cod_database_code               7123886
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C H O N Pd Cl'
_reflns_odcompleteness_completeness 99.77
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Riding coordinates:
 O9(H6D,H6E)
2.b Free rotating group:
 O8(H8C,H8D), O7(H7A,H7B)
2.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C4(H4A,H4B), C12(H12A,H12B), C16(H16A,H16B), C17(H17A,H17B)
2.d Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C1(H1A,H1B,H1C), C20(H20A,H20B,H20C), C11(H11A,H11B,H11C),
 C14(H14A,H14B,H14C)
;
_shelx_res_checksum              60773
_olex2_submission_special_instructions 'No special instructions were received'