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_7135587
_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         'C36 H36 B6 N14 Ni2 O10'
_chemical_formula_sum            'C36 H36 B6 N14 Ni2 O10'
_chemical_formula_weight         1007.07
_chemical_name_systematic        Ni(II)2[B3O3(OH)2Qi(Pz)2]2
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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                 95.728(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5281(7)
_cell_length_b                   16.6027(6)
_cell_length_c                   14.4927(5)
_cell_measurement_reflns_used    11834
_cell_measurement_temperature    99.97(12)
_cell_measurement_theta_max      32.4890
_cell_measurement_theta_min      2.0870
_cell_volume                     4435.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.101a 64-bit (release 13-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_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(12)
_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 0.962
_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     49.00 111.00   0.50    0.96    --   33.08-178.00   0.00  124
  2  \w     69.00 106.00   0.50    0.96    --   33.08-178.00  90.00   74
  3  \w   -116.00 -59.00   0.50    0.96    --  -32.30 -23.00  -2.00  114
  4  \w    -27.00  50.00   0.50    0.96    --  -32.30  23.00 162.00  154
  5  \w    -14.00  11.00   0.50    0.96    --   33.08 -99.00   0.00   50
  6  \w    -51.00  29.00   0.50    0.96    --   33.08 -23.00  -2.00  160
  7  \w     49.00  77.00   0.50    0.96    --   33.08 -99.00   0.00   56
  8  \w     47.00  74.00   0.50    0.96    --   33.08 -99.00-180.00   54
  9  \w    -14.00  11.00   0.50    0.96    --   33.08 -99.00-180.00   50
 10  \w   -117.00 -42.00   0.50    0.96    --  -32.30 178.00  30.00  150
 11  \w      7.00  88.00   0.50    0.96    --   33.08  77.00-120.00  162
 12  \w     67.00  93.00   0.50    0.96    --   33.08  57.00 -60.00   52
 13  \w     -5.00 115.00   0.50    0.96    --   33.08  23.00 162.00  240
 14  \w     80.00 115.00   0.50    0.96    --   33.08 178.00 120.00   70
 15  \w     82.00 111.00   0.50    0.96    --   33.08 178.00-150.00   58
 16  \w     50.00  76.00   0.50    0.96    --   33.08 178.00-150.00   52
 17  \w     49.00  78.00   0.50    0.96    --   33.08 178.00-180.00   58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0017951000
_diffrn_orient_matrix_UB_12      0.0258180000
_diffrn_orient_matrix_UB_13      0.0386917000
_diffrn_orient_matrix_UB_21      -0.0113568000
_diffrn_orient_matrix_UB_22      -0.0328672000
_diffrn_orient_matrix_UB_23      0.0263292000
_diffrn_orient_matrix_UB_31      0.0367067000
_diffrn_orient_matrix_UB_32      -0.0088771000
_diffrn_orient_matrix_UB_33      0.0151412000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1402
_diffrn_reflns_av_unetI/netI     0.1170
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            66028
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         37.790
_diffrn_reflns_theta_min         1.651
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.101a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             2064
_exptl_crystal_preparation
'All reagents were of analytical grade and were subjected to ultrasonic dissolution prior to the solvothermal reaction.'
_exptl_crystal_recrystallization_method
'It remains stable under a wide range of conditions and exhibits high purity.'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.455
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         11461
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.1232
_refine_ls_R_factor_gt           0.0591
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0557P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1415
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6376
_reflns_number_total             11461
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc07399e2.cif
_cod_data_source_block           boc-22-2_auto
_cod_depositor_comments
'Adding full bibliography for 7135585--7135587.cif.'
_cod_database_code               7135587
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N B O Ni'
_shelx_estimated_absorpt_t_max   0.882
_shelx_estimated_absorpt_t_min   0.852
_reflns_odcompleteness_completeness 99.99
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.23
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 O5-H5
 0.87 with sigma of 0.01
 Ni2-H5
 2.730089 with sigma of 0.02
 B3-H5
 1.942398 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C14(H14)
3.b Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 68 electrons were 
found in a volume of 460\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.75[CH3CN] per Unit Cell 
which account for 66 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              56875
_shelx_hkl_checksum              33787
_shelx_fab_checksum              57404
_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 1.393
_oxdiff_exptl_absorpt_empirical_full_min 0.910