Neutral self-assembly of dinuclear copper(ii) metallacycles derived from Schiff base ligands: synthesis, characterization and catalysis
Jain, Isha; Rohini,; Jain, Ravish Kumar; Devi, Sudha; Malik, Payal; New Journal of Chemistry 49 (2025) 951–958; doi:10.1039/D4NJ03994G

data_7063590
_publ_section_title
;
 Neutral self-assembly of dinuclear copper(ii) metallacycles derived from
 Schiff base ligands: synthesis, characterization and catalysis
;
_journal_issue                   3
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              951
_journal_page_last               958
_journal_paper_doi               10.1039/D4NJ03994G
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'C59.98 H84 Cu2 N4 O4'
_chemical_formula_sum            'C59.98 H84 Cu2 N4 O4'
_chemical_formula_weight         1052.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-11 deposited with the CCDC.	2024-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.948(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.1630(9)
_cell_length_b                   21.2607(11)
_cell_length_c                   18.3542(10)
_cell_measurement_reflns_used    9912
_cell_measurement_temperature    298
_cell_measurement_theta_max      24.93
_cell_measurement_theta_min      2.26
_cell_volume                     6212.0(6)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       Apex-4
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_av_unetI/netI     0.0398
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            43203
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.041
_diffrn_reflns_theta_max         25.041
_diffrn_reflns_theta_min         2.259
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5108
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1519 before and 0.0735 after correction.
The Ratio of minimum to maximum transmission is 0.6855.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic brownish brown'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             2248
_exptl_crystal_size_max          0.489
_exptl_crystal_size_mid          0.345
_exptl_crystal_size_min          0.256
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0773
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0645P)^2^+12.0976P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1526
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4086
_reflns_number_total             5457
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4nj03994g2.cif
_cod_data_source_block           i868_0m_a
_cod_depositor_comments
'Adding full bibliography for 7063589--7063590.cif.'
_cod_database_code               7063590
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.717
_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. Others
 Fixed Sof: C20(0.9899)
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C16(H16), C18(H18), C24(H24), C9(H9)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C28(H28A,H28B,H28C), C6(H6A,H6B,H6C), C29(H29A,H29B,H29C),
 C8(H8A,H8B,H8C), C13(H13A,H13B,H13C), C27(H27A,H27B,H27C), C22(H22A,H22B,H22C),
  C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C12(H12A,H12B,H12C), C21(H21A,H21B,
 H21C)
;
_shelx_res_checksum              40454
_olex2_submission_special_instructions 'No special instructions were received'