#------------------------------------------------------------------------------
#$Date: 2026-04-05 13:37:45 +0200 (Sun 05 de Apr de 2026) $
#$Revision: 305291 $
#$URL: svn://www.crystallography.net/cod/cif/7/13/55/7135586.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7135586
loop_
_publ_author_name
'Zhang, Xiang-Ming'
'Fu, Jiang-Hong'
'Zhao, Pan-Pan'
'Chen, Shumei'
'Zhang, Hai-Xia'
'Zhang, Jian'
_publ_section_title
;
 Synthesis of hybrid nickel boron-oxo clusters for photocatalytic
 CO₂ 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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      0.00  56.00   0.50    1.00    --   67.10 -57.00  60.00  112
  2  ω      5.00  41.00   0.50    1.00    --   67.10 -38.00  60.00   72
  3  ω    -56.00  -7.00   0.50    1.00    --  -69.60  52.00 152.00   98
  4  ω    -18.00   7.00   0.50    1.00    --  -69.60  19.00   0.00   50
  5  ω   -143.00 -53.00   0.50    1.00    --  -69.60 -64.00-123.00  180
  6  ω   -138.00 -90.00   0.50    1.00    --  -69.60 -79.00  31.00   96
  7  ω     -7.00  20.00   0.50    0.25    --   -1.25 -99.00 -30.00   54
  8  ω     -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       'ω 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.1380P)²+0.8703P] where P=(Fo²+2Fc²)/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 > 2σ(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'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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 915Å³ 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
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.666667 0.333333 0.38430(12) 0.0246(4) Uani 1 3 d S T P . .
O7 O 0.58423(18) 0.24078(17) 0.2038(4) 0.0259(7) Uani 1 1 d . . . . .
O8 O 0.51297(18) 0.31320(18) 0.0987(3) 0.0279(7) Uani 1 1 d . . . . .
O5 O 0.53871(19) 0.09625(18) 0.1078(4) 0.0288(7) Uani 1 1 d . . . . .
O2 O 0.4688(2) 0.1723(2) 0.0019(4) 0.0361(8) Uani 1 1 d . . . . .
O14 O 0.4182(2) 0.0303(2) -0.0846(5) 0.0433(9) Uani 1 1 d . . . . .
H14 H 0.437043 -0.003630 -0.100781 0.065 Uiso 1 1 calc R U . . .
N13 N 0.5752(2) 0.3507(2) 0.5039(4) 0.0297(8) Uani 1 1 d . . . . .
N9 N 0.5382(2) 0.3831(2) 0.3924(4) 0.0289(8) Uani 1 1 d . . . . .
C12 C 0.5395(3) 0.3448(3) 0.6636(6) 0.0402(12) Uani 1 1 d . . . . .
H12 H 0.553195 0.324213 0.767933 0.048 Uiso 1 1 calc R U . . .
B6 B 0.5667(3) 0.3932(3) 0.1921(6) 0.0270(10) Uani 1 1 d . . . . .
B2 B 0.5223(3) 0.2436(3) 0.1026(6) 0.0271(11) Uani 1 1 d . . . . .
C10 C 0.4812(3) 0.3955(3) 0.4822(6) 0.0417(12) Uani 1 1 d . . . . .
H10 H 0.446608 0.416781 0.433720 0.050 Uiso 1 1 calc R U . . .
B1 B 0.4761(3) 0.0990(3) 0.0087(7) 0.0312(11) Uani 1 1 d . . . . .
C11 C 0.4809(3) 0.3723(3) 0.6570(6) 0.0423(12) Uani 1 1 d . . . . .
H11 H 0.447385 0.374794 0.752013 0.051 Uiso 1 1 calc R U . . .
O1 O 0.1466(6) -0.0609(6) 0.1883(12) 0.035(2) Uani 0.3333 1 d . . P . .
H1A H 0.132439 -0.089194 0.289973 0.052 Uiso 0.3333 1 d R U P . .
H1B H 0.194389 -0.013894 0.217744 0.052 Uiso 0.3333 1 d R U P . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0137 0.0067 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0070 0.0029 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0241 0.0134 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -1.3357 3.2904 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0389 0.0241 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Ni O7 82.09(12) . 3_665 ?
O7 Ni O7 82.09(12) 2_655 . ?
O7 Ni O7 82.09(12) 2_655 3_665 ?
N13 Ni O7 79.32(12) . 3_665 ?
N13 Ni O7 96.01(13) . . ?
N13 Ni O7 96.01(13) 2_655 2_655 ?
N13 Ni O7 161.39(13) . 2_655 ?
N13 Ni O7 79.32(12) 2_655 . ?
N13 Ni O7 161.39(13) 3_665 . ?
N13 Ni O7 96.01(13) 3_665 3_665 ?
N13 Ni O7 79.32(12) 3_665 2_655 ?
N13 Ni O7 161.39(13) 2_655 3_665 ?
N13 Ni N13 101.84(12) 3_665 . ?
N13 Ni N13 101.84(12) 2_655 . ?
N13 Ni N13 101.84(12) 2_655 3_665 ?
B6 O7 Ni 108.6(2) 2_655 . ?
B2 O7 Ni 126.8(3) . . ?
B2 O7 B6 124.4(3) . 2_655 ?
B2 O8 B6 125.5(4) . . ?
B1 O5 B6 121.0(4) . 2_655 ?
B2 O2 B1 120.5(4) . . ?
B1 O14 H14 109.5 . . ?
N9 N13 Ni 113.3(2) . . ?
C12 N13 Ni 140.9(3) . . ?
C12 N13 N9 105.6(4) . . ?
N13 N9 B6 116.0(3) . . ?
C10 N9 N13 109.7(4) . . ?
C10 N9 B6 134.3(4) . . ?
N13 C12 H12 124.4 . . ?
N13 C12 C11 111.2(4) . . ?
C11 C12 H12 124.4 . . ?
O7 B6 O5 111.5(4) 3_665 3_665 ?
O7 B6 N9 103.1(3) 3_665 . ?
O8 B6 O7 113.7(3) . 3_665 ?
O8 B6 O5 108.8(4) . 3_665 ?
O8 B6 N9 109.5(3) . . ?
O5 B6 N9 110.3(3) 3_665 . ?
O7 B2 O2 118.2(4) . . ?
O8 B2 O7 121.9(4) . . ?
O8 B2 O2 119.9(4) . . ?
N9 C10 H10 125.7 . . ?
N9 C10 C11 108.6(5) . . ?
C11 C10 H10 125.7 . . ?
O5 B1 O2 121.6(4) . . ?
O14 B1 O5 121.4(4) . . ?
O14 B1 O2 117.0(4) . . ?
C12 C11 C10 104.9(4) . . ?
C12 C11 H11 127.6 . . ?
C10 C11 H11 127.6 . . ?
H1A O1 H1B 101.3 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni O7 2.082(3) . ?
Ni O7 2.082(3) 3_665 ?
Ni O7 2.082(3) 2_655 ?
Ni N13 2.029(4) . ?
Ni N13 2.029(4) 2_655 ?
Ni N13 2.029(4) 3_665 ?
O7 B6 1.455(6) 2_655 ?
O7 B2 1.369(5) . ?
O8 B6 1.449(6) . ?
O8 B2 1.342(6) . ?
O5 B6 1.458(6) 2_655 ?
O5 B1 1.370(6) . ?
O2 B2 1.380(6) . ?
O2 B1 1.386(6) . ?
O14 H14 0.8400 . ?
O14 B1 1.347(6) . ?
N13 N9 1.366(5) . ?
N13 C12 1.339(5) . ?
N9 B6 1.572(5) . ?
N9 C10 1.334(6) . ?
C12 H12 0.9500 . ?
C12 C11 1.368(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.377(7) . ?
C11 H11 0.9500 . ?
O1 H1A 0.8819 . ?
O1 H1B 0.8798 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni O7 B2 O8 6.0(6) . . . . ?
Ni O7 B2 O2 -174.4(3) . . . . ?
Ni N13 N9 B6 5.1(4) . . . . ?
Ni N13 N9 C10 -177.8(3) . . . . ?
Ni N13 C12 C11 176.0(4) . . . . ?
N13 N9 B6 O7 -34.3(4) . . . 3_665 ?
N13 N9 B6 O8 87.0(4) . . . . ?
N13 N9 B6 O5 -153.4(4) . . . 3_665 ?
N13 N9 C10 C11 0.9(5) . . . . ?
N13 C12 C11 C10 0.4(6) . . . . ?
N9 N13 C12 C11 0.1(5) . . . . ?
N9 C10 C11 C12 -0.8(6) . . . . ?
C12 N13 N9 B6 -177.7(4) . . . . ?
C12 N13 N9 C10 -0.6(5) . . . . ?
B6 O7 B2 O8 -169.5(4) 2_655 . . . ?
B6 O7 B2 O2 10.1(6) 2_655 . . . ?
B6 O8 B2 O7 2.2(6) . . . . ?
B6 O8 B2 O2 -177.4(4) . . . . ?
B6 O5 B1 O2 -7.8(6) 2_655 . . . ?
B6 O5 B1 O14 173.0(4) 2_655 . . . ?
B6 N9 C10 C11 177.3(4) . . . . ?
B2 O8 B6 O7 34.9(5) . . . 3_665 ?
B2 O8 B6 O5 159.7(4) . . . 3_665 ?
B2 O8 B6 N9 -79.8(5) . . . . ?
B2 O2 B1 O5 -3.3(7) . . . . ?
B2 O2 B1 O14 176.0(4) . . . . ?
C10 N9 B6 O7 149.4(5) . . . 3_665 ?
C10 N9 B6 O8 -89.3(6) . . . . ?
C10 N9 B6 O5 30.3(7) . . . 3_665 ?
B1 O2 B2 O7 2.3(6) . . . . ?
B1 O2 B2 O8 -178.1(4) . . . . ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 -0.606 915.0 262.8 '26 H2O'
