Well-Distributed Pt-Nanoparticles within Confined Coordination Interspaces of Self-Sensitized Porphyrin Metal-Organic Frameworks: Synergistic Effect Boosting Highly Efficient Photocatalytic Hydrogen Evolution Reaction
Li, Shuai; Mei, Hong-Min; Yao, Shi-Lin; Chen, Zhiyao; Lu, Yu-Lin; Zhang, Li; Su, Cheng-Yong; Chemical Science  (2019) –; doi:10.1039/C9SC01866B

data_1552365
_publ_section_title
;
 Well-Distributed Pt-Nanoparticles within Confined Coordination
 Interspaces of Self-Sensitized Porphyrin Metal-Organic Frameworks:
 Synergistic Effect Boosting Highly Efficient Photocatalytic Hydrogen
 Evolution Reaction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC01866B
_journal_year                    2019
_chemical_formula_moiety         'C52 H36 N4 O8 Pd'
_chemical_formula_sum            'C52 H36 N4 O8 Pd'
_chemical_formula_weight         951.25
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc22gvdt
_audit_creation_date             2019-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-05 deposited with the CCDC.    2019-09-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   33.5643(16)
_cell_length_b                   21.7048(9)
_cell_length_c                   6.9605(3)
_cell_measurement_reflns_used    2842
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.6240
_cell_measurement_theta_min      4.0600
_cell_volume                     5070.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6525
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.957
_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    -64.00 -18.00   1.00   14.00    --  -39.83  19.00  90.00   46
  2  \w   -112.00 -15.00   1.00   14.00    --  -39.83 -38.00 -90.00   97
  3  \w     52.00 174.00   1.00   60.00    --  104.53  15.00 -30.00  122
  4  \w    117.00 178.00   1.00   60.00    --  104.53 125.00-180.00   61
  5  \w     22.00  64.00   1.00   60.00    --  104.53 -94.00   0.00   42
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0431663000
_diffrn_orient_matrix_UB_12      0.0088420000
_diffrn_orient_matrix_UB_13      0.0703101000
_diffrn_orient_matrix_UB_21      -0.0063511000
_diffrn_orient_matrix_UB_22      0.0702718000
_diffrn_orient_matrix_UB_23      0.0045227000
_diffrn_orient_matrix_UB_31      -0.0143186000
_diffrn_orient_matrix_UB_32      -0.0044522000
_diffrn_orient_matrix_UB_33      0.2097660000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0462
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            9844
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.827
_diffrn_reflns_theta_min         4.074
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.394
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.49114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       needle
_exptl_crystal_F_000             1944
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.458
_refine_diff_density_min         -1.531
_refine_diff_density_rms         0.120
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         4842
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0932
_refine_ls_R_factor_gt           0.0720
_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^)+(0.0281P)^2^+37.9311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1524
_refine_ls_wR_factor_ref         0.1663
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3682
_reflns_number_total             4842
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc01866b2.cif
_cod_data_source_block           pd-tmcpp
_cod_database_code               1552365
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_usercomment     C4A-C5-MGCL2
_shelx_estimated_absorpt_t_max   0.429
_shelx_estimated_absorpt_t_min   0.429
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C14(H14), C15(H15), C7(H7), C6(H6), C21(H21), C1(H1),
 C20(H20), C2(H2), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C12(H12A,H12B,H12C)
;
_shelx_res_checksum              93893
_shelx_fab_checksum              18755
_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 4.949
_oxdiff_exptl_absorpt_empirical_full_min 0.411