Dinuclear vs. mononuclear copper(ii) complexes with nitrophenylimino-benzylal- vs. -naphthylal-based Schiff base ligands
Enamullah, Mohammed; Haque, Imdadul; Abdullah, Galib; Sourav, Fahad Hossain; Jhumur, Nisat Taslum; Islam, Mohammad Khairul; Haj Hassani Sohi, Takin; Ferber, Peter; Janiak, Christoph; New Journal of Chemistry 49 (2025) 17106–17123; doi:10.1039/D5NJ02584B

data_7063975
_publ_section_title
;
 Dinuclear vs. mononuclear copper(ii) complexes with
 nitrophenylimino-benzylal- vs. -naphthylal-based Schiff base ligands
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17106
_journal_page_last               17123
_journal_paper_doi               10.1039/D5NJ02584B
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C36 H26 Cu N4 O6'
_chemical_formula_sum            'C36 H26 Cu N4 O6'
_chemical_formula_weight         674.15
_chemical_name_systematic
bis{1-((Z)-(4-methyl-2-nitro-phenylimino)methyl))naphthalen-2-olato-\k^2^N,O}copper(II)
_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             2023-11-06
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2025-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.211(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.6103(2)
_cell_length_b                   11.1734(2)
_cell_length_c                   12.9695(3)
_cell_measurement_reflns_used    5516
_cell_measurement_temperature    299.17(10)
_cell_measurement_theta_max      76.2040
_cell_measurement_theta_min      4.7050
_cell_volume                     1460.56(6)
_computing_cell_refinement       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.94a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.17(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.931
_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   -103.00 -77.00   0.50    0.10    --  -84.25  77.00-150.00   52
  2  \w    -51.00 -26.00   0.50    0.10    --  -84.25  77.00-150.00   50
  3  \w    -48.00 -12.00   0.50    0.10    --  -84.25  38.00-120.00   72
  4  \w    -40.00 -15.00   0.50    0.10    --  -84.25  38.00-150.00   50
  5  \w    -46.00 -21.00   0.50    0.10    --  -84.25  38.00 -90.00   50
  6  \w    -48.00 -16.00   0.50    0.10    --  -84.25  38.00  90.00   64
  7  \w    -40.00 -15.00   0.50    0.10    --  -84.25  38.00 120.00   50
  8  \w    -39.00 -14.00   0.50    0.10    --  -84.25  29.00 119.00   50
  9  \w    -39.00  24.00   0.50    0.05    --  -48.16  29.00 119.00  126
 10  \w    -80.00 -54.00   0.50    0.05    --  -48.16 -29.00 -41.00   52
 11  \w   -132.00 -73.00   0.50    0.10    --  -84.25 -29.00 -41.00  118
 12  \w    -30.00  25.00   0.50    0.05    --  -48.16  19.00-120.00  110
 13  \w    -30.00  26.00   0.50    0.05    --  -48.16  19.00-180.00  112
 14  \w    -86.00 -27.00   0.50    0.10    --  -84.25 125.00-150.00  118
 15  \w     -4.00  22.00   0.50    0.05    --   48.16 -29.00 -41.00   52
 16  \w     34.00  81.00   0.50    0.10    --  105.75 -77.00-150.00   94
 17  \w     34.00  61.00   0.50    0.10    --  105.75 -57.00 -60.00   54
 18  \w     36.00  61.00   0.50    0.10    --  105.75 -57.00-120.00   50
 19  \w     34.00  59.00   0.50    0.10    --  105.75 -57.00 -30.00   50
 20  \w     35.00  60.00   0.50    0.10    --  105.75 -57.00 -90.00   50
 21  \w     35.00  75.00   0.50    0.10    --  105.75 -77.00   0.00   80
 22  \w     34.00  60.00   0.50    0.10    --  105.75 -57.00   0.00   52
 23  \w     34.00  59.00   0.50    0.10    --  105.75 -57.00  30.00   50
 24  \w     34.00  59.00   0.50    0.10    --  105.75 -57.00  90.00   50
 25  \w     34.00  59.00   0.50    0.10    --  105.75 -57.00 120.00   50
 26  \w     36.00  61.00   0.50    0.10    --  105.75 -57.00 150.00   50
 27  \w     94.00 159.00   0.50    0.10    --  105.75  29.00 119.00  130
 28  \w     56.00  81.00   0.50    0.05    --   48.16  29.00 119.00   50
 29  \w    140.00 166.00   0.50    0.10    --  105.75  38.00-150.00   52
 30  \w    107.00 132.00   0.50    0.10    --  105.75  38.00-150.00   50
 31  \w     39.00  65.00   0.50    0.10    --  105.75 -99.00-180.00   52
 32  \w     70.00  98.00   0.50    0.10    --  105.75 -99.00-180.00   56
 33  \w     95.00 120.00   0.50    0.05    --   48.16-178.00-150.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1446024000
_diffrn_orient_matrix_UB_12      0.0368555000
_diffrn_orient_matrix_UB_13      -0.0153502000
_diffrn_orient_matrix_UB_21      -0.0179560000
_diffrn_orient_matrix_UB_22      0.0329359000
_diffrn_orient_matrix_UB_23      -0.1191036000
_diffrn_orient_matrix_UB_31      -0.0460502000
_diffrn_orient_matrix_UB_32      -0.1287113000
_diffrn_orient_matrix_UB_33      -0.0349169000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.931
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11345
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.931
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.442
_diffrn_reflns_theta_min         4.721
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.539
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.722
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.94a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear red'
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             694
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CH2Cl2/methanol'
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         2858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0360
_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^)+(0.0518P)^2^+0.4689P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0982
_refine_ls_wR_factor_ref         0.1031
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2460
_reflns_number_total             2858
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj02584b2.cif
_cod_data_source_block           enam_cul118r1(1)
_cod_depositor_comments
'Adding full bibliography for 7063972--7063976.cif.'
_cod_database_code               7063975
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'C36 H26 Cu N4 O6'
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.791
_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:
 C1(H1), C4(H4), C16(H16), C10(H10), C13(H13), C9(H9), C14(H14), C5(H5),
 C6(H6), C7(H7)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C)
;
_shelx_res_checksum              97044
_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 1.385
_oxdiff_exptl_absorpt_empirical_full_min 0.839