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_7717772
_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         'C64 H56 Cu4 N8 O12, 1.5(H2 O)'
_chemical_formula_sum            'C64 H59 Cu4 N8 O13.5'
_chemical_formula_weight         1410.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_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            8
_cell_length_a                   36.4484(7)
_cell_length_b                   23.7380(4)
_cell_length_c                   14.0430(3)
_cell_measurement_reflns_used    35248
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      29.7140
_cell_measurement_theta_min      1.7960
_cell_volume                     12150.2(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.853
_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    -25.00  21.00   0.50    9.56    --    1.16  82.00  92.00   92
  2  \w    -65.00   5.00   0.50    9.56    --    1.16 -39.00 141.00  140
  3  \w    -15.00  37.00   0.50    9.56    --    1.16 -99.00 150.00  104
  4  \w    -15.00  37.00   0.50    9.56    --    1.16 -99.00 -90.00  104
  5  \w    -42.00  24.00   0.50    9.56    --    1.16 -77.00 -60.00  132
  6  \w    -22.00  19.00   0.50    9.56    --   -1.94  77.00-120.00   82
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Dual, Cu at home/near, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0440
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.853
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            61970
_diffrn_reflns_point_group_measured_fraction_full 0.979
_diffrn_reflns_point_group_measured_fraction_max 0.784
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.648
_diffrn_reflns_theta_min         2.022
_exptl_absorpt_coefficient_mu    1.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_description       block
_exptl_crystal_F_000             5784
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.667
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details
;
 Flack x determined using 4574 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.013(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     924
_refine_ls_number_reflns         13458
_refine_ls_number_restraints     934
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0478
_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^)+(0.0385P)^2^+58.4290P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1111
_reflns_Friedel_coverage         0.768
_reflns_Friedel_fraction_full    0.958
_reflns_Friedel_fraction_max     0.708
_reflns_number_gt                11616
_reflns_number_total             13458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03283g2.cif
_cod_data_source_block           complex-1
_cod_depositor_comments
'Adding full bibliography for 7717768--7717772.cif.'
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_original_formula_sum        'C64 H59 Cu4 N8 O13.50'
_cod_database_code               7717772
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.868
_shelx_estimated_absorpt_t_min   0.760
_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. Restrained distances
 C70-C69 \\sim C67-C72 \\sim C66-C71 \\sim C43-C49 \\sim C48-C53
 with sigma of 0.04
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
4. Others
 Fixed Sof: C71(0.65) H71(0.65) C67(0.35) H67(0.35) C48(0.5) H48(0.5) C47(0.5)
 H47(0.5) C73(0.65) H73(0.65) C46(0.5) H46(0.5) O14(0.75) H14A(0.75) H14B(0.75)
 O13(0.75) H13A(0.75) H13B(0.75) C75(0.65) H75(0.65) C44(0.5) H44(0.5)
 C74(0.65) H74(0.65) C69(0.35) H69(0.35) C70(0.35) H70(0.35) C66(0.35)
 H66(0.35) C72(0.65) H72(0.65) C45(0.5) H45(0.5) C43(0.5) C51(0.5) H51(0.5)
 C50(0.5) H50(0.5) C53(0.5) H53(0.5) C49(0.5) C54(0.5) H54(0.5) C52(0.5)
 H52(0.5) C68(0.35) H68(0.35)
5.a Free rotating group:
 O14(H14A,H14B), O13(H13A,H13B)
5.b Aromatic/amide H refined with riding coordinates:
 C71(H71), C39(H39), C36(H36), C28(H28), C16(H16), C20(H20), C7(H7), C30(H30),
 C58(H58), C23(H23), C41(H41), C29(H29), C15(H15), C4(H4), C61(H61), C67(H67),
 C32(H32), C12(H12), C9(H9), C25(H25), C48(H48), C63(H63), C47(H47), C73(H73),
 C31(H31), C13(H13), C14(H14), C46(H46), C75(H75), C44(H44), C74(H74), C69(H69),
  C70(H70), C66(H66), C72(H72), C45(H45), C51(H51), C50(H50), C53(H53),
 C54(H54), C52(H52), C68(H68)
5.c Idealised Me refined as rotating group:
 C22(H22A,H22B,H22C), C35(H35A,H35B,H35C), C60(H60A,H60B,H60C), C19(H19A,H19B,
 H19C), C38(H38A,H38B,H38C), C6(H6A,H6B,H6C), C3(H3A,H3B,H3C), C57(H57A,H57B,
 H57C)
;
_shelx_res_checksum              8309
_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
;