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_7717771
_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         'C44 H58 Cu4 N4 O14, N O3, Cl, 4(H2 O)'
_chemical_formula_sum            'C44 H66 Cl Cu4 N5 O21'
_chemical_formula_weight         1290.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-12-13
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-16 deposited with the CCDC.	2025-01-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.038(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.9803(8)
_cell_length_b                   25.4313(17)
_cell_length_c                   18.5445(13)
_cell_measurement_reflns_used    20494
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.81
_cell_volume                     5594.5(7)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'photon 100 CMOS'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0329
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59524
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.403
_diffrn_reflns_theta_min         1.948
_exptl_absorpt_coefficient_mu    1.625
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6316
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.248
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         11345
_refine_ls_number_restraints     63
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0693
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0792P)^2^+13.5249P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1344
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8737
_reflns_number_total             11345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03283g2.cif
_cod_data_source_block           complex-2
_cod_depositor_comments
'Adding full bibliography for 7717768--7717772.cif.'
_cod_database_code               7717771
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.608
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O13-H13A
 0.83 with sigma of 0.01
 N5-O16
 1.4 with sigma of 0.02
 O14-H14B
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(O18) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O21)
\\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(N5) \\sim Ueq, Uanis(O16) \\sim Ueq,
Uanis(O15) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O19) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: O19(0.75) H19D(0.75) H19E(0.75) O21(0.5) H21C(0.5) H21D(0.5)
 O18(0.5) H18D(0.5) H18E(0.5) O22(0.65) H22C(0.65) H22D(0.65) O23(0.6)
 H23A(0.6) H23B(0.6)
 Fixed X: H20B(0.155801)
 Fixed Y: H20B(0.4528)
 Fixed Z: H20B(0.239799)
5.a Free rotating group:
 O20(H20A,O19,H19D,H19E,O21,H21C,H21D,O18,H18D,H18E,O22,H22C,H22D,O23,H23A,H23B)
5.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,
 H32B), C33(H33A,H33B), C43(H43A,H43B), C44(H44A,H44B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C9(H9), C14(H14), C16(H16), C20(H20), C25(H25), C27(H27),
 C31(H31), C36(H36), C38(H38), C42(H42)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C18(H18A,H18B,H18C), C19(H19A,H19B,H19C),
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C)
;
_shelx_res_checksum              68765
_olex2_submission_special_instructions 'No special instructions were received'