Synthesis of hybrid nickel boron-oxo clusters for photocatalytic CO<sub>2</sub> reduction.
Zhang, Xiang-Ming; Fu, Jiang-Hong; Zhao, Pan-Pan; Chen, Shumei; Zhang, Hai-Xia; Zhang, Jian; Chemical communications (Cambridge, England) 62 (2026) 6904–6908; doi:10.1039/d5cc07399e

data_7135586
_publ_section_title
;
 Synthesis of hybrid nickel boron-oxo clusters for photocatalytic
 CO<sub>2</sub> reduction.
;
_journal_issue                   26
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              6904
_journal_page_last               6908
_journal_paper_doi               10.1039/d5cc07399e
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         'C9 H12 B9 N6 Ni1 O15, 1(H2 O)'
_chemical_formula_sum            'C9 H14 B9 N6 Ni O16'
_chemical_formula_weight         618.26
_space_group_crystal_system      trigonal
_space_group_IT_number           147
_space_group_name_Hall           '-P 3'
_space_group_name_H-M_alt        'P -3'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-12-09
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-12-11 deposited with the CCDC.	2026-03-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   17.9513(8)
_cell_length_b                   17.9513(8)
_cell_length_c                   7.5178(3)
_cell_measurement_reflns_used    2812
_cell_measurement_temperature    99.97(19)
_cell_measurement_theta_max      55.6650
_cell_measurement_theta_min      4.2660
_cell_volume                     2098.04(16)
_computing_cell_refinement       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_collection       'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_computing_data_reduction        'CrysAlisPro 1.171.43.131a (Rigaku OD, 2024)'
_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_environment      N~2~
_diffrn_ambient_temperature      99.97(19)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_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      0.00  56.00   0.50    1.00    --   67.10 -57.00  60.00  112
  2  \w      5.00  41.00   0.50    1.00    --   67.10 -38.00  60.00   72
  3  \w    -56.00  -7.00   0.50    1.00    --  -69.60  52.00 152.00   98
  4  \w    -18.00   7.00   0.50    1.00    --  -69.60  19.00   0.00   50
  5  \w   -143.00 -53.00   0.50    1.00    --  -69.60 -64.00-123.00  180
  6  \w   -138.00 -90.00   0.50    1.00    --  -69.60 -79.00  31.00   96
  7  \w     -7.00  20.00   0.50    0.25    --   -1.25 -99.00 -30.00   54
  8  \w     -4.00  33.00   0.50    0.25    --   -1.25 -98.00 141.00   74
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0156194000
_diffrn_orient_matrix_UB_12      0.0205383000
_diffrn_orient_matrix_UB_13      -0.1616614000
_diffrn_orient_matrix_UB_21      0.0821896000
_diffrn_orient_matrix_UB_22      0.0296414000
_diffrn_orient_matrix_UB_23      -0.0453350000
_diffrn_orient_matrix_UB_31      -0.0202789000
_diffrn_orient_matrix_UB_32      -0.0781831000
_diffrn_orient_matrix_UB_33      -0.0599098000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_av_unetI/netI     0.0712
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6952
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         55.968
_diffrn_reflns_theta_min         2.471
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    2.817
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.53948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.131a (Rigaku Oxford Diffraction, 2024)
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    0.979
_exptl_crystal_description       block
_exptl_crystal_F_000             622
_refine_diff_density_max         1.099
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.115
_refine_ls_extinction_coef       0.0027(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         2714
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0744
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1380P)^2^+0.8703P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2109
_refine_ls_wR_factor_ref         0.2228
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2018
_reflns_number_total             2714
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc07399e2.cif
_cod_data_source_block           22-13_auto
_cod_depositor_comments
'Adding full bibliography for 7135585--7135587.cif.'
_cod_original_cell_volume        2098.0(2)
_cod_database_code               7135586
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N B O Ni'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     53.78
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Others
 Fixed Sof: O1(0.33333) H1A(0.33333) H1B(0.33333)
3.a Riding coordinates:
 O1(H1A,H1B)
3.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C10(H10), C11(H11)
3.c Idealised tetrahedral OH refined as rotating group:
 O14(H14)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 263 electrons were 
found in a volume of 915\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
13[H2O] per Unit Cell 
which account for 260 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              9763
_shelx_hkl_checksum              14531
_shelx_fab_checksum              9829
_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 1.601
_oxdiff_exptl_absorpt_empirical_full_min 0.537