Hofmann-like metal‒organic-framework-derived PtxFe/C/N-GC composites as efficient electrocatalysts for methanol oxidation
Zhao, Jia; Huang, Hui; Liu, Ming; Wang, Jin-Hua; Liu, Kai; Li, Zhao-Yang; RSC Advances 9 (2019) 26450–; doi:10.1039/C9RA04652F

data_7233433
_publ_section_title
;
 Hofmann-like metal--organic-framework-derived PtxFe/C/N-GC composites as
 efficient electrocatalysts for methanol oxidation
;
_journal_issue                   45
_journal_name_full               'RSC Advances'
_journal_page_first              26450
_journal_paper_doi               10.1039/C9RA04652F
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C17 H12 Fe N6 O4 Pt'
_chemical_formula_sum            'C17 H12 Fe N6 O4 Pt'
_chemical_formula_weight         615.27
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_Hall           '-I 2b 2c'
_space_group_name_H-M_alt        'I b c a'
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-23 deposited with the CCDC.    2019-08-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   15.1120(4)
_cell_length_b                   21.1317(4)
_cell_length_c                   29.3846(8)
_cell_measurement_reflns_used    7002
_cell_measurement_temperature    296.14(10)
_cell_measurement_theta_max      73.9100
_cell_measurement_theta_min      5.1260
_cell_volume                     9383.7(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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      air
_diffrn_ambient_temperature      296.14(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.966
_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    -24.00  89.00   0.50    1.22    --    0.00  77.00 -30.00  226
  2  \w    -41.00 -14.00   0.50    1.22    --    0.00 -57.00  30.00   54
  3  \w      6.00 108.00   0.50    4.89    --   95.80 -61.00 120.00  204
  4  \w     58.00 107.00   0.50    4.89    --   95.80 -82.00  30.00   98
  5  \w     79.00 142.00   0.50    4.89    --   95.80  61.00-150.00  126
  6  \w     97.00 122.00   0.50    4.89    --   95.80 -77.00  30.00   50
  7  \w     17.00  98.00   0.50    4.89    --   95.80 -15.00-150.00  162
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0014754000
_diffrn_orient_matrix_UB_12      0.0529933000
_diffrn_orient_matrix_UB_13      0.0359609000
_diffrn_orient_matrix_UB_21      -0.0026854000
_diffrn_orient_matrix_UB_22      0.0500244000
_diffrn_orient_matrix_UB_23      -0.0381351000
_diffrn_orient_matrix_UB_31      -0.1019355000
_diffrn_orient_matrix_UB_32      -0.0021389000
_diffrn_orient_matrix_UB_33      0.0005542000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            14819
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.391
_diffrn_reflns_theta_min         4.690
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    16.231
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45792
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.742
_exptl_crystal_description       needlelike
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_platon_squeeze_details
;
TITL zj-3.4-7_a.res in Ibca
CELL   15.1120   21.1317   29.3846     90.00     90.00     90.00
SPGR Ibca
Q101 0.581 0.592 0.254 !       2.50 eA-3
C102 0.752 0.926 0.329 !       2.24 eA-3
C103 0.955 0.920 0.212 !       1.72 eA-3
Q104 0.216 0.359 0.123 !       1.26 eA-3
C105 0.095 0.513 0.189 !       1.12 eA-3
C106 0.313 0.500 0.250 !       0.94 eA-3
C107 0.270 0.468 0.230 !       0.86 eA-3
C108 0.158 0.496 0.197 !       0.80 eA-3
Q109 0.250 0.437 0.000 !       0.77 eA-3
C110 0.199 0.505 0.200 !       0.73 eA-3
Q111 1.001 0.240 0.415 !       0.72 eA-3
Q112 0.342 0.755 0.050 !       0.61 eA-3
C113 0.283 0.541 0.301 !       0.60 eA-3
Q114 0.327 0.642 0.128 !       0.51 eA-3
;
_refine_diff_density_max         1.197
_refine_diff_density_min         -1.562
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4640
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0324
_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^)+(0.0625P)^2^+18.6419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1084
_refine_ls_wR_factor_ref         0.1127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3740
_reflns_number_total             4640
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra04652f2.cif
_cod_data_source_block           zj-3-4-7_sq
_cod_database_code               7233433
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.855
_shelx_estimated_absorpt_t_min   0.497
_reflns_odcompleteness_completeness 99.56
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O3-H3
 0.85 with sigma of 0.01
 C18-H3
 1.8819 with sigma of 0.02
 Fe1-H3
 2.714386 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C18 \\sim O3: within 1.7A with sigma of 0.001 and sigma for terminal atoms of
0.002
4.a Rotating group:
 O1W(H1WA,H1WB)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C9(H9), C10(H10), C14(H14), C15(H15)
4.c Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_platon_squeeze_void_probe_radius 1.20
_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 2.142
_oxdiff_exptl_absorpt_empirical_full_min 0.683