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_7135585
_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         'C32 H32 B2 N12 Ni O2'
_chemical_formula_sum            'C32 H32 B2 N12 Ni O2'
_chemical_formula_weight         697.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_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                 109.013(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.6960(5)
_cell_length_b                   8.6183(3)
_cell_length_c                   16.3091(7)
_cell_measurement_reflns_used    9592
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      30.0530
_cell_measurement_theta_min      2.3450
_cell_volume                     1554.27(11)
_computing_cell_refinement       'CrysAlisPro 1.171.43.101a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.43.101a (Rigaku OD, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_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 0.823
_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    -18.00  37.00   0.50    1.29    --    5.25 -99.00  60.00  110
  2  \w    -16.00  28.00   0.50    1.29    --   -4.94 -99.00 -90.00   88
  3  \w    -15.00  26.00   0.50    1.29    --   -4.94 -99.00-180.00   82
  4  \w    -35.00  -8.00   0.50    1.29    --   -4.94 -48.00-109.00   54
  5  \w    -78.00   6.00   0.50    1.29    --   -4.94 -38.00  30.00  168
  6  \w     -6.00  22.00   0.50    1.29    --   -4.94  48.00  38.00   56
;
_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      0.0334747000
_diffrn_orient_matrix_UB_12      0.0395305000
_diffrn_orient_matrix_UB_13      -0.0228467000
_diffrn_orient_matrix_UB_21      0.0546144000
_diffrn_orient_matrix_UB_22      -0.0281610000
_diffrn_orient_matrix_UB_23      0.0300058000
_diffrn_orient_matrix_UB_31      -0.0032697000
_diffrn_orient_matrix_UB_32      -0.0664490000
_diffrn_orient_matrix_UB_33      -0.0263455000
_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  0.0766
_diffrn_reflns_av_unetI/netI     0.0646
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14773
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.722
_diffrn_reflns_theta_min         1.884
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Mova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89444
_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            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.838
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         3977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.1269
_refine_ls_R_factor_gt           0.1191
_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^)+(0.0001P)^2^+22.6951P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2796
_refine_ls_wR_factor_ref         0.2831
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3512
_reflns_number_total             3977
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc07399e2.cif
_cod_data_source_block           6-22-17-zipian_auto
_cod_depositor_comments
'Adding full bibliography for 7135585--7135587.cif.'
_cod_original_cell_volume        1554.26(11)
_cod_database_code               7135585
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N B O Ni'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C22(H22), C11(H11), C20(H20), C21(H21), C17(H17), C6(H6), C10(H10),
 C3(H3), C7(H7), C16(H16), C4(H4), C15(H15)
2.b Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C)
;
_shelx_res_checksum              90353
_shelx_hkl_checksum              36622
_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 1.233
_oxdiff_exptl_absorpt_empirical_full_min 0.732