Exploring structural, magnetic, and catalytic diversity in tetranuclear {Cu<sub>4</sub>O<sub>4</sub>} cubane cores and a dinuclear complex derived from closely related ligand systems.
Jana, Narayan Ch; Escuer, Albert; Brandão, Paula; Panja, Anangamohan; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3000–3012; doi:10.1039/d4dt03283g

data_7717768
_publ_section_title
;
 Exploring structural, magnetic, and catalytic diversity in tetranuclear
 {Cu<sub>4</sub>O<sub>4</sub>} cubane cores and a dinuclear complex
 derived from closely related ligand systems.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3000
_journal_page_last               3012
_journal_paper_doi               10.1039/d4dt03283g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C16 H16 N2 O3, H2 O'
_chemical_formula_sum            'C16 H18 N2 O4'
_chemical_formula_weight         302.32
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-22
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-11-20 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.86772(10)
_cell_length_b                   13.6394(2)
_cell_length_c                   22.0354(4)
_cell_measurement_reflns_used    6625
_cell_measurement_temperature    149.98(16)
_cell_measurement_theta_max      77.4740
_cell_measurement_theta_min      3.8030
_cell_volume                     1462.99(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.89a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.98(16)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.970
_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    -72.00  17.00   0.50    0.12    --  -38.50  97.00 174.00  178
  2  \w      4.00  83.00   0.50    0.12    --   49.06 -97.00  65.00  158
  3  \w     40.00 107.00   0.50    0.69    --  106.83 -97.00  65.00  134
  4  \w    104.00 174.00   0.50    0.69    --  106.83  97.00 174.00  140
  5  \w    -42.00  28.00   0.50    0.12    --  -38.50  37.00 -90.00  140
  6  \w   -101.00 -27.00   0.50    0.12    --  -38.50 -57.00 -30.00  148
  7  \w    102.00 171.00   0.50    0.69    --  106.83  45.00 -60.00  138
  8  \w     42.00 111.00   0.50    0.69    --  106.83 -45.00  60.00  138
  9  \w    102.00 171.00   0.50    0.69    --  106.83  45.00 -30.00  138
 10  \w     44.00 112.00   0.50    0.69    --  106.83-125.00 -30.00  136
 11  \w    103.00 171.00   0.50    0.69    --  106.83  77.00-180.00  136
 12  \w     42.00 111.00   0.50    0.69    --  106.83 -45.00-180.00  138
 13  \w     38.00 112.00   0.50    0.12    --   49.06  57.00-180.00  148
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0310373000
_diffrn_orient_matrix_UB_12      0.0992685000
_diffrn_orient_matrix_UB_13      -0.0326667000
_diffrn_orient_matrix_UB_21      0.1055191000
_diffrn_orient_matrix_UB_22      0.0532268000
_diffrn_orient_matrix_UB_23      0.0570245000
_diffrn_orient_matrix_UB_31      0.2966991000
_diffrn_orient_matrix_UB_32      -0.0085350000
_diffrn_orient_matrix_UB_33      -0.0236919000
_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  0.0512
_diffrn_reflns_av_unetI/netI     0.0485
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -4
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            8671
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.941
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.795
_diffrn_reflns_theta_min         3.811
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.824
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.89a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'light yellow'
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_description       needle
_exptl_crystal_F_000             640
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.179
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 1017 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         2943
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0463P)^2^+0.2278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0953
_refine_ls_wR_factor_ref         0.0974
_reflns_Friedel_coverage         0.639
_reflns_Friedel_fraction_full    0.964
_reflns_Friedel_fraction_max     0.900
_reflns_number_gt                2765
_reflns_number_total             2943
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03283g2.cif
_cod_data_source_block           H2L1
_cod_depositor_comments
'Adding full bibliography for 7717768--7717772.cif.'
_cod_database_code               7717768
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N O'
_shelx_estimated_absorpt_t_max   0.922
_shelx_estimated_absorpt_t_min   0.853
_olex2_refinement_description
;
1. Restrained distances
 O4-H4A = O4-H4B
 0.87 with sigma of 0.02
 H4A-H4B
 1.38 with sigma of 0.04
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C7(H7), C9(H9), C12(H12), C16(H16), C15(H15), C13(H13), C14(H14)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C3(H3A,H3B,H3C)
2.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              95757
_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 1.669
_oxdiff_exptl_absorpt_empirical_full_min 0.438