Ferromagnetically coupled tetranuclear Ni(ii)-2-oxy-aceto- or benzo-phenonate complexes
Haque, Imdadul; Enamullah, Mohammed; Jhumur, Nisat Taslum; Sidhu, Baldeep K.; Herbert, David E.; Haj Hassani Sohi, Takin; Havlíček, Lubomír; Nemec, Ivan; Janiak, Christoph; RSC Advances 15 (2025) 4250–4261; doi:10.1039/D4RA08700C

data_7249923
_publ_section_title
;
 Ferromagnetically coupled tetranuclear Ni(ii)-2-oxy-aceto- or
 benzo-phenonate complexes
;
_journal_issue                   6
_journal_name_full               'RSC Advances'
_journal_page_first              4250
_journal_page_last               4261
_journal_paper_doi               10.1039/D4RA08700C
_journal_volume                  15
_journal_year                    2025
_chemical_formula_moiety         'C56 H56 Ni4 O16, H2 O'
_chemical_formula_sum            'C56 H58 Ni4 O17'
_chemical_formula_weight         1237.86
_chemical_name_common
'tetrakis-[(\m~3~-methanolato-\k^3^O:O:O)(aqua-\kO)(2-oxybenzophenonato-\k^2^O,O')nickel(II)] monohydrate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-06-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-01-06 deposited with the CCDC.	2025-01-23 downloaded from the CCDC.
;
_cell_angle_alpha                76.144(9)
_cell_angle_beta                 74.388(10)
_cell_angle_gamma                82.908(7)
_cell_formula_units_Z            2
_cell_length_a                   11.6867(17)
_cell_length_b                   13.294(3)
_cell_length_c                   18.419(4)
_cell_measurement_reflns_used    9078
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      2.35
_cell_volume                     2670.5(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_collection       'APEX v4, Bruker AXS'
_computing_data_reduction        'SAINT V8.40B (?, 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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker D8 QUEST ECO PHOTON100'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'TRIUMPH curved--crystal'
_diffrn_radiation_source         'fine--focus tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            80855
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns.reduction_process narrow--frame
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.549
_diffrn_reflns_theta_min         2.329
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0688 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.7983.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_description       block
_exptl_crystal_F_000             1284
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/methanol'
_exptl_crystal_size_max          0.477
_exptl_crystal_size_mid          0.128
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.624
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     705
_refine_ls_number_reflns         12233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0436
_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^)+7.2589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0837
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10384
_reflns_number_total             12233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ra08700c2.cif
_cod_data_source_block           ena015
_cod_database_code               7249923
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.892
_shelx_estimated_absorpt_t_min   0.542
_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, All O(H,H) groups
2.a Free rotating group:
 O16(H16A,H16B)
2.b Rotating group:
 O14(H14A,H14B), O13(H13A,H13B), O15(H15A,H15B), O17(H17A,H17B)
2.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C9(H9), C4(H4), C5(H5), C39(H39), C2(H2), C41(H41), C31(H31),
 C44(H44), C15(H15), C35(H35), C12(H12), C48(H48), C43(H43), C36(H36), C42(H42),
  C3(H3), C28(H28), C30(H30), C22(H22), C37(H37), C11(H11), C29(H29), C16(H16),
 C38(H38), C52(H52), C26(H26), C10(H10), C51(H51), C49(H49), C18(H18), C25(H25),
  C17(H17), C50(H50), C24(H24), C23(H23)
2.d Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C54(H54A,H54B,
 H54C)
;
_shelx_res_checksum              28926
_shelx_hkl_checksum              63506
_olex2_submission_special_instructions 'No special instructions were received'