In-situ growth of Fe doped NiCo-MOF electrocatalyst from layered double hydroxide effectively enhances electrocatalytic oxygen evolution performance
Sun, Tingting; Lin, Shuang-Yan; Xu, Zhikun; Li, L.; CrystEngComm  (2021) –; doi:10.1039/D1CE01220G

data_7243558
_publ_section_title
;
 In-situ growth of Fe doped NiCo-MOF electrocatalyst from layered double
 hydroxide effectively enhances electrocatalytic oxygen evolution
 performance
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D1CE01220G
_journal_year                    2021
_chemical_formula_moiety         'C6 H18 Cl7 Cu7 S3'
_chemical_formula_sum            'C6 H18 Cl7 Cu7 S3'
_chemical_formula_weight         879.31
_space_group_crystal_system      hexagonal
_space_group_IT_number           186
_space_group_name_Hall           'P 6c -2c'
_space_group_name_H-M_alt        'P 63 m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-01-25
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2020.03.28 svn.rd84adfe8 for Rigaku Oxford Diffraction, GUI svn.r6032)
;
_audit_update_record
;
2021-05-25 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.9585(6)
_cell_length_b                   13.9585(6)
_cell_length_c                   6.4715(3)
_cell_measurement_reflns_used    2630
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.0320
_cell_measurement_theta_min      3.6000
_cell_volume                     1091.98(8)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-ac4 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.6426
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -62.00  31.00   1.00    1.00    --  -41.11  57.00 120.00   93
  2  \w     22.00  63.00   1.00    1.00    --   41.11  57.00 -60.00   41
  3  \w     39.00  98.00   1.00    1.00    --   41.11  57.00 -30.00   59
  4  \w     30.00 128.00   1.00    2.54    --  103.58 -77.00   0.00   98
  5  \w     93.00 176.00   1.00    2.54    --  103.58  45.00 -90.00   83
  6  \w     47.00  87.00   1.00    2.54    --  103.58 -77.00 -60.00   40
  7  \w    124.00 150.00   1.00    2.54    --  103.58  77.00 -30.00   26
  8  \w    103.00 164.00   1.00    2.54    --  103.58  77.00 120.00   61
  9  \w    144.00 177.00   1.00    2.54    --  103.58  77.00-180.00   33
 10  \w     79.00 125.00   1.00    2.54    --  103.58  45.00-120.00   46
 11  \w      2.00  42.00   1.00    1.00    --   41.23 -50.00-114.00   40
 12  \w    -20.00  48.00   1.00    1.00    --   41.23 -77.00-150.00   68
 13  \w     79.00 105.00   1.00    2.54    --  103.58  45.00 150.00   26
 14  \w    152.00 177.00   1.00    2.54    --  103.58  45.00 150.00   25
 15  \w     78.00 136.00   1.00    2.54    --  103.58  61.00 -30.00   58
 16  \w     70.00 128.00   1.00    2.54    --  103.58 -45.00 120.00   58
 17  \w     33.00  59.00   1.00    2.54    --  103.58 -45.00 -90.00   26
 18  \w    104.00 129.00   1.00    2.54    --  103.58 -45.00 -90.00   25
 19  \w     80.00 166.00   1.00    2.54    --  103.58  45.00  90.00   86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, 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      0.0585940000
_diffrn_orient_matrix_UB_12      0.1020951000
_diffrn_orient_matrix_UB_13      -0.1413886000
_diffrn_orient_matrix_UB_21      -0.0518522000
_diffrn_orient_matrix_UB_22      -0.0742510000
_diffrn_orient_matrix_UB_23      -0.1908626000
_diffrn_orient_matrix_UB_31      -0.1005616000
_diffrn_orient_matrix_UB_32      0.0171684000
_diffrn_orient_matrix_UB_33      0.0160904000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6520
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.000
_diffrn_reflns_theta_max         72.229
_diffrn_reflns_theta_min         3.656
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    17.845
_exptl_absorpt_correction_T_max  0.421
_exptl_absorpt_correction_T_min  0.016
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.674
_exptl_crystal_description       needle
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.658
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.072
_refine_diff_density_max         0.521
_refine_diff_density_min         -0.581
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 344 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.0014(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         806
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0276
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0437P)^2^+0.6349P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0671
_refine_ls_wR_factor_ref         0.0692
_reflns_Friedel_coverage         0.819
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                787
_reflns_number_total             806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01220g2.cif
_cod_data_source_block           7cucl_3dms_150
_cod_original_cell_volume        1091.98(11)
_cod_database_code               7243558
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Cu7 Cl7 S3 C6 H18'
_shelx_estimated_absorpt_t_max   0.360
_shelx_estimated_absorpt_t_min   0.030
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              76285
_shelx_hkl_checksum              6794
_olex2_date_sample_data_collection 2021-01-25
_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 1.525
_oxdiff_exptl_absorpt_empirical_full_min 0.697