Synthesis, characterization and electrocatalytic activity of a novel binuclear polypyridine nickel complex
Dong, Jinfeng; Qi, Zhichao; Zhang, Lianghui; Li, Qianqian; Lin, Junqi; Qu, Yanbo; New Journal of Chemistry  (2025) –; doi:10.1039/D5NJ03685B

data_7064121
_publ_section_title
;
 Synthesis, characterization and electrocatalytic activity of a novel
 binuclear polypyridine nickel complex
;
_journal_name_full               'New Journal of Chemistry'
_journal_paper_doi               10.1039/D5NJ03685B
_journal_year                    2025
_chemical_formula_moiety         '2(C36 H42 N8 Ni2 O4), 8(Cl O4), 3(H2 O)'
_chemical_formula_sum            'C72 H90 Cl8 N16 Ni4 O43'
_chemical_formula_weight         2386.03
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2025-11-11
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-11-13 deposited with the CCDC.	2025-11-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.111(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.706(3)
_cell_length_b                   18.755(3)
_cell_length_c                   17.934(3)
_cell_measurement_reflns_used    4051
_cell_measurement_temperature    305(2)
_cell_measurement_theta_max      17.496
_cell_measurement_theta_min      2.305
_cell_volume                     4817.5(15)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker D8 Venture diffractometer'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2025/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      305(2)
_diffrn_detector                 'Bruker PHOTON-II area detector'
_diffrn_detector_area_resol_mean 7.4
_diffrn_detector_type            'CMOS-PHOTONII area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker PHOTON-II area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1765
_diffrn_reflns_av_unetI/netI     0.0535
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            99873
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.101
_diffrn_reflns_theta_max         25.101
_diffrn_reflns_theta_min         2.033
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.092
_exptl_absorpt_correction_T_max  0.7326
_exptl_absorpt_correction_T_min  0.5751
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1360 before and 0.1065 after correction.
The Ratio of minimum to maximum transmission is 0.7850.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear orangish orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2452
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.666
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     833
_refine_ls_number_reflns         8549
_refine_ls_number_restraints     630
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.1686
_refine_ls_R_factor_gt           0.1169
_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^)+(0.1293P)^2^+30.6688P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2799
_refine_ls_wR_factor_ref         0.3259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5325
_reflns_number_total             8549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj03685b2.cif
_cod_data_source_block           lin251101
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_diffrn_radiation_probe' value 'X-ray' was changed to
'x-ray' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 
;
_cod_original_cell_volume        4817.4(15)
_cod_database_code               7064121
_shelx_shelxl_version_number     2025/1
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.750
_exptl_crystal_mounting_method
;
 Crystals were removed from the crystallisation vial and immediately coated
 with PDMS (polydimethylsiloxane/Dimethicone, CAS: 9006-65-9 on a glass slide.
 A suitable single crystal was selected and mounted on a glass fiber using
 vacuum silicone grease as adhesive. The glass fiber with single crystal was
 mounted on copper pin with solid paraffin. Operator: DJ_Tokyo.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Ni2-H3A \\sim Ni2-H3B
 with sigma of 0.02
 Ni2-H4A \\sim Ni2-H4B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O7 \\sim Cl1 \\sim O5 \\sim O6 \\sim O8 \\sim O6A \\sim Cl1A \\sim O5A \\sim
O7A \\sim O8A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
Cl3 \\sim O13 \\sim O13A \\sim O16A \\sim O16 \\sim O14 \\sim O14A \\sim O15
\\sim O15A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O20A \\sim Cl4A \\sim O17A \\sim O18A \\sim O19A \\sim O18 \\sim Cl4 \\sim O17
\\sim O19 \\sim O20: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
Cl2A \\sim O9A \\sim O10A \\sim O11A \\sim O12A \\sim O9 \\sim Cl2 \\sim O10
\\sim O11 \\sim O12: within 2A with sigma of 0.01 and sigma for terminal atoms
of 0.02 within 2A
N7 \\sim C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(O22) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Same fragment restrains
{Cl3, O13A, O14A, O15A, O16A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{Cl3, O13, O14, O15, O16}
{Cl1A, O5A, O6A, O7A, O8A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{Cl1, O5, O6, O7, O8}
{Cl2A, O9A, O10A, O11A, O12A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{Cl2, O9, O10, O11, O12}
{Cl4A, O17A, O18A, O19A, O20A} sigma for 1-2: 0.01, 1-3: 0.01
as in
{Cl4, O17, O18, O19, O20}
5. Others
 Sof(Cl1A)=Sof(O5A)=Sof(O6A)=Sof(O7A)=Sof(O8A)=1-FVAR(1)
 Sof(Cl1)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=FVAR(1)
 Sof(Cl2A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=1-FVAR(2)
 Sof(Cl2)=Sof(O9)=Sof(O10)=Sof(O11)=Sof(O12)=FVAR(2)
 Sof(O13A)=Sof(O14A)=Sof(O15A)=Sof(O16A)=1-FVAR(3)
 Sof(O13)=Sof(O14)=Sof(O15)=Sof(O16)=FVAR(3)
 Sof(Cl4A)=Sof(O17A)=Sof(O18A)=Sof(O19A)=Sof(O20A)=1-FVAR(4)
 Sof(Cl4)=Sof(O17)=Sof(O18)=Sof(O19)=Sof(O20)=FVAR(4)
 Fixed Sof: O21(0.5) H21A(0.5) H21B(0.5) O22(0.75) H22A(0.75) H22B(0.75)
 O23(0.25) H23A(0.25) H23B(0.25)
6.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O3(H3A,H3B), O4(H4A,H4B), O21(H21A,H21B), O22(H22A,
 H22B), O23(H23A,H23B)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C24(H24A,H24B), C25(H25A,H25B),
 C31(H31A,H31B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C27(H27), C28(H28),
  C29(H29), C30(H30), C33(H33), C34(H34), C35(H35), C36(H36)
;
_shelx_res_checksum              2132
_olex2_submission_special_instructions 'No special instructions were received'