Al12Co4: A Pioneering Heterometallic Aluminum-oxo Cluster with Surface-exposed Co Sites for Oxygen Evolution Reaction
Han, Er-Meng; Meng, Ru-Xin; Tian, Yi-Qi; Yan, Jun; Liu, Kaiyu; Liu, Chao; Chemical Communications  (2023) –; doi:10.1039/D3CC03672C

data_7132031
_publ_section_title
;
 Al12Co4: A Pioneering Heterometallic Aluminum-oxo Cluster with
 Surface-exposed Co Sites for Oxygen Evolution Reaction
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03672C
_journal_year                    2023
_chemical_formula_moiety         'C188 H246 Al6 N4 O28, 12[C3H7ON]'
_chemical_formula_sum            'C224 H330 Al6 N16 O40'
_chemical_formula_weight         4048.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-08-15
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2023-08-15 deposited with the CCDC.	2023-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                110.867(7)
_cell_angle_beta                 111.132(6)
_cell_angle_gamma                93.254(7)
_cell_formula_units_Z            1
_cell_length_a                   16.830(2)
_cell_length_b                   18.597(3)
_cell_length_c                   20.790(3)
_cell_measurement_reflns_used    3281
_cell_measurement_temperature    170.00
_cell_measurement_theta_max      40.764
_cell_measurement_theta_min      2.558
_cell_volume                     5541.8(14)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      170.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX2 microsource'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.2299
_diffrn_reflns_av_unetI/netI     0.4308
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            52096
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.906
_diffrn_reflns_theta_min         3.180
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           3.57
_diffrn_source_power             0.24954300000000001
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           69.9
_exptl_absorpt_coefficient_mu    0.562
_exptl_absorpt_correction_T_max  0.7506
_exptl_absorpt_correction_T_min  0.4078
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1435 before and 0.0852 after correction.
The Ratio of minimum to maximum transmission is 0.5433.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       plate
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.279
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1055
_refine_ls_number_reflns         20100
_refine_ls_number_restraints     117
_refine_ls_restrained_S_all      0.897
_refine_ls_R_factor_all          0.2899
_refine_ls_R_factor_gt           0.1081
_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^)+(0.1179P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2480
_refine_ls_wR_factor_ref         0.3349
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5164
_reflns_number_total             20100
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03672c2.cif
_cod_data_source_block           Al6
_cod_original_cell_volume        5542.1(13)
_cod_database_code               7132031
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.989
_shelx_estimated_absorpt_t_min   0.962
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O009-H009
 0.87 with sigma of 0.01
 Al03-H009
 2.58348 with sigma of 0.02
 Al02-H009
 2.239544 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C11 \\sim C12 \\sim C17 \\sim C5: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C14 \\sim C15 \\sim C16 \\sim C17: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C18 \\sim C21 \\sim C19 \\sim C20: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
C1 \\sim C2 \\sim C3 \\sim C4: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
Uanis(C12) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C10)
\\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C18) \\sim Ueq,
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C011(H01A,H01B), C012(H01C,H01D), C017(H01E,H01F), C01C(H01G,H01H), C01K(H01K,
 H01L), C01Z(H01R,H01T), C024(H02A,H02B), C02C(H02C,H02D)
4.b Aromatic/amide H refined with riding coordinates:
 C00P(H00P), C00R(H00R), C00V(H00V), C016(H016), C01E(H01I), C01I(H01J),
 C01M(H01P), C01N(H01Q), C01S(H01S), C01U(H01U), C01V(H01V), C01W(H01W),
 C01X(H01X), C01Y(H01Y), C021(H021), C023(H023), C026(H026), C02D(H02E)
4.c Idealised Me refined as rotating group:
 C01L(H01M,H01N,H01O), C02E(H02F,H02G,H02H), C02F(H02I,H02J,H02K), C02H(H02L,
 H02M,H02N), C02I(H02O,H02P,H02Q), C02J(H02R,H02S,H02T), C02K(H02U,H02V,H02W),
 C4(H4A,H4B,H4C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C13(H13A,H13B,H13C),
 C02P(H02X,H02Y,H), C6(H6A,H6B,H6C), C02S(H02Z,HA,HB), C21(H21A,H21B,H21C),
 C8(H8A,H8B,H8C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C02Z(H02,HC,HD), C030(H03A,
 H03B,H03C), C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C),
 C14(H14A,H14B,H14C), C7(H7A,H7B,H7C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C),
 C12(H12A,H12B,H12C)
4.d Idealised tetrahedral OH refined as rotating group:
 O007(H007), O008(H008), O00E(H00E), O00H(H00H)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              24316
_shelx_hkl_checksum              48717
_shelx_fab_checksum              28960
_olex2_submission_special_instructions 'No special instructions were received'