Amorphous conversion in pyrolytic symmetric trinuclear nickel clusters trigger trifunctional electrocatalysts.
Li, Li; Zhao, Hui-Feng; Gan, Mei-Xing; Zhang, Tao; Li, Jia-Ning; Tao, Shi; Peng, Jing; Yu, Hai-Bin; Peng, Xu; Chemical science 15 (2024) 7689–7697; doi:10.1039/d4sc01696c

data_1571446
_publ_section_title
;
 Amorphous conversion in pyrolytic symmetric trinuclear nickel clusters
 trigger trifunctional electrocatalysts.
;
_journal_issue                   20
_journal_name_full               'Chemical science'
_journal_page_first              7689
_journal_page_last               7697
_journal_paper_doi               10.1039/d4sc01696c
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '2(C21 H24 N3 Ni1.5 O6)'
_chemical_formula_sum            'C42 H50 N6 Ni3 O12'
_chemical_formula_weight         1007.01
_chemical_melting_point          293
_chemical_name_common            Ni3(H3sal-dahp)?DMF
_chemical_name_systematic        C42H50N6Ni3O12
_chemical_properties_physical    Heat-sensitive
_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             2021-12-29
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-06-15 deposited with the CCDC.	2024-04-16 downloaded from the CCDC.
;
_cell_angle_alpha                82.996(5)
_cell_angle_beta                 87.336(5)
_cell_angle_gamma                68.730(6)
_cell_formula_units_Z            2
_cell_length_a                   10.6889(7)
_cell_length_b                   14.1596(9)
_cell_length_c                   15.3942(9)
_cell_measurement_reflns_used    8094
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      74.1280
_cell_measurement_theta_min      2.8480
_cell_volume                     2155.0(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.34b (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.34b (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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 7.9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     32.00  92.00   0.50    2.13    --   37.97  57.00 -60.00  120
  2  \w     81.00 106.00   0.50    2.13    --   37.97  37.00 -60.00   50
  3  \w    121.00 178.00   0.50    2.13    --  112.45 111.00-180.00  114
  4  \w    109.00 148.00   0.50    2.13    --  112.45 178.00 -60.00   78
  5  \w    106.00 158.00   0.50    2.13    --  112.45 111.00  60.00  104
  6  \w    106.00 163.00   0.50    2.13    --  112.45 100.00 159.00  114
  7  \w     75.00 162.00   0.50    2.13    --  112.45  77.00  60.00  174
  8  \w     98.00 176.00   0.50    2.13    --  112.45  77.00 -60.00  156
  9  \w     80.00 155.00   0.50    2.13    --  112.45  61.00-150.00  150
 10  \w     62.00  98.00   0.50    2.13    --  112.45 178.00 -60.00   72
 11  \w     61.00 106.00   0.50    2.13    --   37.97 178.00  60.00   90
 12  \w     63.00 138.00   0.50    2.13    --  112.45 178.00  90.00  150
 13  \w      1.00  56.00   0.50    2.13    --   37.97  37.00 -60.00  110
 14  \w     29.00  92.00   0.50    2.13    --  112.45 -94.00-180.00  126
 15  \w     44.00 115.00   0.50    2.13    --  112.45-111.00 -90.00  142
 16  \w     55.00 105.00   0.50    2.13    --  112.45-111.00  30.00  100
 17  \w     58.00 111.00   0.50    2.13    --  112.45-100.00  54.00  106
 18  \w     80.00 105.00   0.50    2.13    --  112.45-111.00 150.00   50
 19  \w     30.00  76.00   0.50    2.13    --  112.45-111.00 150.00   92
 20  \w      0.00  87.00   0.50    2.13    --   37.97-100.00  54.00  174
 21  \w     29.00 105.00   0.50    2.13    --  112.45 -94.00 -90.00  152
 22  \w     34.00  86.00   0.50    2.13    --   37.97 -99.00-150.00  104
 23  \w     -1.00  24.00   0.50    0.53    --    0.00-100.00  54.00   50
 24  \w      1.00 116.00   0.50    2.13    --   37.97  77.00 150.00  230
 25  \w    -36.00 -11.00   0.50    0.53    --    0.00 100.00 159.00   50
 26  \w    -58.00  11.00   0.50    2.13    --  -37.97 100.00 159.00  138
 27  \w    -46.00 -21.00   0.50    2.13    --  -98.50 100.00 159.00   50
 28  \w    -77.00 -52.00   0.50    2.13    --  -98.50 100.00 159.00   50
 29  \w   -113.00 -10.00   0.50    2.13    --  -37.97 -57.00  30.00  206
 30  \w   -122.00 -82.00   0.50    2.13    --  -98.50-100.00  54.00   80
 31  \w   -131.00 -96.00   0.50    2.13    --  -98.50 -94.00 150.00   70
 32  \w   -164.00 -61.00   0.50    2.13    --  -98.50 -77.00  90.00  206
 33  \w   -169.00-144.00   0.50    2.13    --  -98.50 -94.00 150.00   50
 34  \w   -173.00 -78.00   0.50    2.13    --  -98.50-111.00   0.00  190
 35  \w    -67.00 -23.00   0.50    2.13    --  -98.50 111.00 -90.00   88
 36  \w    -70.00 -36.00   0.50    2.13    --  -98.50 178.00-120.00   68
 37  \w   -102.00 -47.00   0.50    2.13    --  -98.50 178.00 -90.00  110
 38  \w   -119.00 -94.00   0.50    2.13    --  -98.50 178.00-120.00   50
;
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0569712000
_diffrn_orient_matrix_UB_12      0.0851119000
_diffrn_orient_matrix_UB_13      -0.0256704000
_diffrn_orient_matrix_UB_21      0.0673712000
_diffrn_orient_matrix_UB_22      -0.0222603000
_diffrn_orient_matrix_UB_23      0.0903350000
_diffrn_orient_matrix_UB_31      0.1270278000
_diffrn_orient_matrix_UB_32      -0.0778943000
_diffrn_orient_matrix_UB_33      -0.0366968000
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18905
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.070
_diffrn_reflns_theta_max         67.070
_diffrn_reflns_theta_min         2.892
_exptl_absorpt_coefficient_mu    2.114
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.27937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.34b (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'brown gray'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_description       block
_exptl_crystal_F_000             1048
_exptl_crystal_recrystallization_method 'From the Melt'
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.563
_refine_diff_density_min         -0.640
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0683
_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^)+(0.1178P)^2^+2.2161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1949
_refine_ls_wR_factor_ref         0.2012
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6569
_reflns_number_total             7664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc01696c2.cif
_cod_data_source_block           exp_7069
_cod_depositor_comments          'Adding full bibliography for 1571446.cif.'
_cod_original_cell_volume        2155.0(2)
_cod_database_code               1571446
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Ni Cl'
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.816
_reflns_odcompleteness_completeness 99.65
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 O6(H6), O00I(H00I)
2.b Ternary CH refined with riding coordinates:
 C9(H9), C01J(H01J)
2.c Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C10(H10A,H10B), C01G(H01A,H01B), C01K(H01C,H01D)
2.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C11(H11), C14(H14), C17(H17),
 C18(H18), C19(H19), C20(H20), C21(H21), C00T(H00T), C00Z(H00Z), C01E(H01E),
 C01H(H01H), C01I(H01I), C01L(H01L), C01O(H01O), C01Q(H01Q), C010(H010),
 C013(H013), C016(H016), C019(H019)
2.e Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C01M(H01F,H01G,H01K), C01P(H01M,
 H01N,H01P)
;
_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 3.860
_oxdiff_exptl_absorpt_empirical_full_min 0.321