Robustness and stability of the l-carnosine copper(ii) dimer: changes in the copper coordination sphere upon heating/solvent substitution
Mrvoš-Sermek, Draginja; Tašner, Marina; Vušak, Darko; Judaš, Nenad; Wzgarda-Raj, Kinga; Đilović, Ivica; Matković-Čalogović, Dubravka; CrystEngComm 27 (2025) 356–365; doi:10.1039/D4CE01070A

data_7249644
_publ_section_title
;
 Robustness and stability of the l-carnosine copper(ii) dimer: changes in
 the copper coordination sphere upon heating/solvent substitution
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              356
_journal_page_last               365
_journal_paper_doi               10.1039/D4CE01070A
_journal_volume                  27
_journal_year                    2025
_chemical_absolute_configuration syn
_chemical_formula_moiety         'C18 H28 Cu2 N8 O8, 2(H2 O)'
_chemical_formula_sum            'C18 H32 Cu2 N8 O10'
_chemical_formula_weight         647.60
_space_group_crystal_system      trigonal
_space_group_IT_number           152
_space_group_name_Hall           'P 31 2"'
_space_group_name_H-M_alt        'P 31 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-05
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-01-22 deposited with the CCDC.	2024-11-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   8.61755(19)
_cell_length_b                   8.61755(19)
_cell_length_c                   30.5882(6)
_cell_measurement_reflns_used    5065
_cell_measurement_temperature    270(1)
_cell_measurement_theta_max      76.1300
_cell_measurement_theta_min      5.9400
_cell_volume                     1967.22(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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      270.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0293
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            7754
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.126
_diffrn_reflns_theta_min         4.336
_exptl_absorpt_coefficient_mu    2.593
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92440
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.91a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.640
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.404
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 768 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     224
_refine_ls_number_reflns         2498
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0313
_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^)+(0.0493P)^2^+0.2151P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0849
_reflns_Friedel_coverage         0.554
_reflns_Friedel_fraction_full    0.888
_reflns_Friedel_fraction_max     0.801
_reflns_number_gt                2284
_reflns_number_total             2498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01070a2.cif
_cod_data_source_block           1_270
_cod_depositor_comments
'Adding full bibliography for 7249643--7249648.cif.'
_cod_original_cell_volume        1967.22(9)
_cod_database_code               7249644
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.950
_shelx_estimated_absorpt_t_min   0.729
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 Cu1-N1A \\sim Cu1-N1B
 with sigma of 0.005
 N1A-C1A \\sim N1B-C1B
 with sigma of 0.005
 C2A-C3A \\sim C2B-C3B
 with sigma of 0.005
 C3A-O3A \\sim C3B-O3B
 with sigma of 0.005
 C3A-N2 \\sim C3B-N2
 with sigma of 0.005
 Cu1-HW1A \\sim Cu1-HW1B
 with sigma of 0.02
3. Restrained planarity
 N2, C3A, O3A, C2A
 with sigma of 0.1
 N2, C3B, O3B, C2B
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
N1A \\sim N1B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C1A \\sim C1B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C2A \\sim C2B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
C3A \\sim C3B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
O3A \\sim O3B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04 within 2A
5. Others
 Sof(O3B)=Sof(N1B)=Sof(H1BA)=Sof(H1BB)=Sof(C1B)=Sof(H1BC)=Sof(H1BD)=Sof(C2B)=
 Sof(H2BA)=Sof(H2BB)=Sof(C3B)=1-FVAR(1)
 Sof(O3A)=Sof(N1A)=Sof(H1AA)=Sof(H1AB)=Sof(C1A)=Sof(H1AC)=Sof(H1AD)=Sof(C2A)=
 Sof(H2AA)=Sof(H2AB)=Sof(C3A)=FVAR(1)
6.a Free rotating group:
 OW1(HW1A,HW1B), OW2(HW2A,HW2B)
6.b Ternary CH refined with riding coordinates:
 C5(H5)
6.c Secondary CH2 refined with riding coordinates:
 N1A(H1AA,H1AB), N1B(H1BA,H1BB), C1A(H1AC,H1AD), C1B(H1BC,H1BD), C2A(H2AA,
 H2AB), C2B(H2BA,H2BB), C6(H6A,H6B)
6.d Aromatic/amide H refined with riding coordinates:
 N4(H4), C8(H8), C9(H9)
;
_shelx_res_checksum              40293
_shelx_hkl_checksum              58808
_olex2_submission_special_instructions 'No special instructions were received'