Two-dimensional stable and ultrathin cluster-based metal‒organic layers for efficient electrocatalytic water oxidation
Yu, Bin-Bin; Hua, Yi-Wei; Huang, Qi; Ye, Si-Yuan; Zhang, Hao-Dong; Yan, Zheng; Li, Rui-Wen; Wu, Jun; Meng, Yan; Cao, Xuebo; CrystEngComm 23 (2021) 4700–4707; doi:10.1039/D1CE00350J

data_7242987
_publ_section_title
;
 Two-dimensional stable and ultrathin cluster-based metal--organic layers
 for efficient electrocatalytic water oxidation
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4700
_journal_page_last               4707
_journal_paper_doi               10.1039/D1CE00350J
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C16 H8 Co1.2 Ni1.8 O10'
_chemical_formula_sum            'C16 H8 Co1.2 Ni1.8 O10'
_chemical_formula_weight         536.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-11-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-03-04 deposited with the CCDC.	2021-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.170(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.7117(14)
_cell_length_b                   12.0990(13)
_cell_length_c                   11.7979(13)
_cell_measurement_reflns_used    1064
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.8860
_cell_measurement_theta_min      6.0530
_cell_volume                     1627.8(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0802
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.975
_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     78.00 105.00   1.00   10.00    --   36.77 178.00 -90.00   27
  2  \w     10.00  66.00   1.00   10.00    --   36.77  77.00 -90.00   56
  3  \w     27.00 103.00   1.00   10.00    --   36.77  57.00 150.00   76
  4  \w     28.00  56.00   1.00   10.00    --   36.77 -38.00 120.00   28
  5  \w    -29.00  49.00   1.00   10.00    --   36.77 -57.00  30.00   78
  6  \w     31.00  67.00   1.00   10.00    --   36.77 -99.00 -30.00   36
  7  \w     12.00  37.00   1.00   10.00    --   36.77  77.00 -30.00   25
  8  \w    110.00 177.00   1.00   30.00    --  108.00 111.00-150.00   67
  9  \w     70.00 108.00   1.00   30.00    --  108.00 -95.00 -60.00   38
 10  \w     59.00  88.00   1.00   30.00    --  108.00 -95.00 120.00   29
 11  \w     42.00 102.00   1.00   30.00    --  108.00 -95.00-120.00   60
 12  \w    103.00 177.00   1.00   30.00    --  108.00 111.00 150.00   74
 13  \w     41.00  66.00   1.00   30.00    --  108.00 -77.00-120.00   25
 14  \w     81.00 172.00   1.00   30.00    --  108.00  77.00 -30.00   91
 15  \w     50.00 144.00   1.00   30.00    --  108.00 -15.00 150.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1253116000
_diffrn_orient_matrix_UB_12      0.0417776000
_diffrn_orient_matrix_UB_13      -0.0512936000
_diffrn_orient_matrix_UB_21      -0.0385756000
_diffrn_orient_matrix_UB_22      -0.1185821000
_diffrn_orient_matrix_UB_23      -0.0387936000
_diffrn_orient_matrix_UB_31      -0.0320825000
_diffrn_orient_matrix_UB_32      -0.0208272000
_diffrn_orient_matrix_UB_33      0.1177193000
_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  0.0734
_diffrn_reflns_av_unetI/netI     0.1207
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            5749
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.194
_diffrn_reflns_theta_min         5.310
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.466
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.17213
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.190
_exptl_crystal_description       block
_exptl_crystal_F_000             1067
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.621
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.225
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3127
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1264
_refine_ls_R_factor_gt           0.0866
_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^)+(0.1296P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2141
_refine_ls_wR_factor_ref         0.2550
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1937
_reflns_number_total             3127
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce00350j2.cif
_cod_data_source_block           20180515a
_cod_depositor_comments          'Adding full bibliography for 7242987.cif.'
_cod_original_formula_sum        'C16 H8 Co1.20 Ni1.80 O10'
_cod_database_code               7242987
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Co Ni C H O'
_shelx_estimated_absorpt_t_max   0.189
_shelx_estimated_absorpt_t_min   0.189
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Co2, Ni2}
{Co1, Ni1}
{Ni8, Co4}
{Co3, Ni3}
3. Uiso/Uaniso restraints and constraints
Uanis(Co3) = Uanis(Ni3)
Uanis(Co1) = Uanis(Ni1)
Uanis(Co2) = Uanis(Ni2)
Uanis(Ni8) = Uanis(Co4)
4. Others
 Fixed Sof: Co1(0.2) Co2(0.4) Co3(0.2) Co4(0.4) Ni2(0.6) Ni1(0.3) Ni8(0.6)
 Ni3(0.3)
5.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14)
;
_shelx_res_checksum              25308
_shelx_hkl_checksum              95263
_olex2_date_sample_data_collection 2018-05-19
_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 3.654
_oxdiff_exptl_absorpt_empirical_full_min 0.465