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_7063976
_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         'C56 H44 Cu2 N8 O12'
_chemical_formula_sum            'C56 H44 Cu2 N8 O12'
_chemical_formula_weight         1148.07
_chemical_name_systematic
;
Bis{2-((Z)-(2-methyl-4-nitro-phenylimino)methyl)phenolato-\k^2^N,O}copper(II)
;
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-03-18
_audit_creation_method
;
Olex2 1.5
(compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188)
;
_audit_update_record
;
2025-06-12 deposited with the CCDC.	2025-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                106.1372(10)
_cell_angle_beta                 98.9681(11)
_cell_angle_gamma                102.7552(12)
_cell_formula_units_Z            4
_cell_length_a                   13.8495(2)
_cell_length_b                   19.6780(3)
_cell_length_c                   20.54938(19)
_cell_measurement_reflns_used    58908
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      79.0320
_cell_measurement_theta_min      2.4170
_cell_volume                     5103.90(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.90a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.959
_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   -119.00 -28.00   0.50    0.33    --  -48.47 -76.00 119.00  182
  2  \w   -119.00 -28.00   0.50    0.33    --  -48.47 -76.00 119.00  182
  3  \w     28.00 120.00   0.50    0.33    --   48.47  76.00-114.00  184
  4  \w    -22.00  69.00   0.50    0.33    --   48.47 -76.00 119.00  182
  5  \w   -161.00 -70.00   0.50    1.31    --  -90.00 -76.00 119.00  182
  6  \w   -106.00 -18.00   0.50    1.31    --  -90.00  76.00-114.00  176
  7  \w     41.00  96.00   0.50    1.31    --  111.50 -76.00 119.00  110
  8  \w     91.00 178.00   0.50    1.31    --  111.50  76.00-114.00  174
  9  \w   -119.00 -41.00   0.50    0.33    --  -48.47-178.00 -30.00  156
 10  \w    -31.00  25.00   0.50    0.33    --  -48.47  19.00-180.00  112
 11  \w    -69.00  24.00   0.50    0.33    --  -48.47  76.00-114.00  186
 12  \w    -31.00  25.00   0.50    0.33    --  -48.47  19.00-120.00  112
 13  \w     41.00 120.00   0.50    0.33    --   48.47  38.00  90.00  158
 14  \w    -24.00  21.00   0.50    0.33    --   48.47 -19.00-180.00   90
 15  \w    -56.00 -18.00   0.50    1.31    --  -90.00  45.00-120.00   76
 16  \w    -56.00 -18.00   0.50    1.31    --  -90.00  45.00  90.00   76
 17  \w    -76.00 -18.00   0.50    1.31    --  -90.00  61.00  90.00  116
 18  \w    -56.00 -18.00   0.50    1.31    --  -90.00  45.00  30.00   76
 19  \w    -76.00 -18.00   0.50    1.31    --  -90.00  61.00  60.00  116
 20  \w   -161.00 -83.00   0.50    1.31    --  -90.00 -95.00-180.00  156
 21  \w   -161.00 -83.00   0.50    1.31    --  -90.00 -95.00-150.00  156
 22  \w     42.00 103.00   0.50    1.31    --  111.50-102.00-157.34  122
 23  \w     42.00 103.00   0.50    1.31    --  111.50-102.00-157.34  122
 24  \w     43.00 104.00   0.50    1.31    --  111.50 -97.00  17.23  122
 25  \w    106.00 177.00   0.50    1.31    --  111.50  15.00  60.00  142
 26  \w    105.00 166.00   0.50    1.31    --  111.50  15.00 -30.00  122
 27  \w     78.00 108.00   0.50    1.31    --  111.50-108.00 110.29   60
 28  \w     49.00  74.00   0.50    1.31    --  111.50-108.00 110.29   50
 29  \w     82.00 108.00   0.50    1.31    --  111.50-125.00 -30.00   52
 30  \w     45.00 105.00   0.50    1.31    --  111.50 -95.00-120.00  120
 31  \w     43.00  79.00   0.50    1.31    --  111.50-125.00 -30.00   72
 32  \w    104.00 178.00   0.50    1.31    --  111.50  30.00-180.00  148
 33  \w    126.00 166.00   0.50    1.31    --  111.50  30.00-150.00   80
 34  \w     48.00 103.00   0.50    1.31    --  111.50 -95.00 150.00  110
 35  \w     81.00 107.00   0.50    1.31    --  111.50-102.00 -43.56   52
 36  \w    112.00 153.00   0.50    1.31    --  111.50  15.00 150.00   82
 37  \w     42.00  99.00   0.50    1.31    --  111.50 -95.00-150.00  114
 38  \w     93.00 175.00   0.50    1.31    --  111.50  77.00 150.00  164
 39  \w     80.00 105.00   0.50    1.31    --  111.50 -95.00 -30.00   50
 40  \w     51.00  76.00   0.50    1.31    --  111.50 -95.00 -30.00   50
 41  \w     41.00 105.00   0.50    1.31    --  111.50 -95.00  90.00  128
 42  \w    104.00 162.00   0.50    1.31    --  111.50  30.00-120.00  116
 43  \w     82.00 110.00   0.50    1.31    --  111.50-125.00  90.00   56
 44  \w     79.00 104.00   0.50    1.31    --  111.50 -95.00 120.00   50
 45  \w     41.00  67.00   0.50    1.31    --  111.50 -95.00  60.00   52
 46  \w     80.00 105.00   0.50    1.31    --  111.50 -95.00  60.00   50
 47  \w     77.00 106.00   0.50    1.31    --  111.50-103.00  -3.62   58
 48  \w     43.00  85.00   0.50    1.31    --  111.50 -77.00-120.00   84
 49  \w     41.00  67.00   0.50    1.31    --  111.50 -95.00   0.00   52
 50  \w     42.00  68.00   0.50    1.31    --  111.50-103.00  -3.62   52
 51  \w     42.00  74.00   0.50    1.31    --  111.50-102.00 -43.56   64
;
_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      0.0666851000
_diffrn_orient_matrix_UB_12      0.0606990000
_diffrn_orient_matrix_UB_13      0.0668863000
_diffrn_orient_matrix_UB_21      -0.0847330000
_diffrn_orient_matrix_UB_22      0.0392429000
_diffrn_orient_matrix_UB_23      0.0028698000
_diffrn_orient_matrix_UB_31      -0.0460454000
_diffrn_orient_matrix_UB_32      -0.0444490000
_diffrn_orient_matrix_UB_33      0.0442147000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0471
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            101169
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         80.061
_diffrn_reflns_theta_min         2.434
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.633
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.369
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.90a (Rigaku Oxford Diffraction, 2020)
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 green'
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             2360
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1413
_refine_ls_number_reflns         21404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0387
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0487P)^2^+3.8803P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1079
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19160
_reflns_number_total             21404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj02584b2.cif
_cod_data_source_block           cul128
_cod_depositor_comments
'Adding full bibliography for 7063972--7063976.cif.'
_cod_original_cell_volume        5103.87(11)
_cod_database_code               7063976
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         CuC27H19N4O6
_cell_oxdiff_angle_alpha         106.1372(10)
_cell_oxdiff_angle_beta          98.9681(11)
_cell_oxdiff_angle_gamma         102.7552(12)
_cell_oxdiff_length_a            13.8495(2)
_cell_oxdiff_length_b            19.6780(3)
_cell_oxdiff_length_c            20.54938(19)
_cell_oxdiff_measurement_reflns_used 58908
_cell_oxdiff_volume              5103.87(11)
_shelx_estimated_absorpt_t_max   0.814
_shelx_estimated_absorpt_t_min   0.683
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C7A(H7A), C9A(H9A), C10A(H10A),
 C12A(H12A), C16A(H16A), C17A(H17A), C18A(H18A), C19A(H19A), C21A(H21A),
 C23A(H23A), C24A(H24A), C26A(H26A), C2B(H2B), C3B(H3B), C4B(H4B), C5B(H5B),
 C7B(H7B), C9B(H9B), C10B(H10B), C12B(H12B), C16B(H16B), C17B(H17B), C18B(H18B),
  C19B(H19B), C21B(H21B), C23B(H23B), C24B(H24B), C26B(H26B), C2C(H2C),
 C2D(H2D), C3C(H3C), C3D(H3D), C4C(H4C), C4D(H4D), C5C(H5C), C5D(H5D), C7C(H7C),
  C7D(H7D), C9C(H9C), C9D(H9D), C10C(H10C), C10D(H10D), C12C(H12C), C12D(H12D),
 C16C(H16C), C16D(H16D), C17C(H17C), C17D(H17D), C18C(H18C), C18D(H18D),
 C19C(H19C), C19D(H19D), C21C(H21C), C21D(H21D), C23C(H23C), C23D(H23D),
 C24C(H24C), C24D(H24D), C26C(H26C), C26D(H26D)
2.b Idealised Me refined as rotating group:
 C14A(H14A,H14B,H14C), C28A(H28A,H28B,H28C), C14B(H14D,H14E,H14F), C28B(H28D,
 H28E,H28F), C14C(H14G,H14H,H14I), C14D(H14J,H14K,H14L), C28C(H28G,H28H,H28I),
 C28D(H28J,H28K,H28L)
;
_shelx_res_checksum              98936
_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 2.137
_oxdiff_exptl_absorpt_empirical_full_min 0.668