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_7249647
_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 H24 Cu2 N8 O6, 2(H2 O)'
_chemical_formula_sum            'C18 H28 Cu2 N8 O8'
_chemical_properties_physical    Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           23
_space_group_name_Hall           'I 2 2'
_space_group_name_H-M_alt        'I 2 2 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-18
_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                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                90.0
_cell_formula_units_Z            4
_cell_length_a                   12.09436(16)
_cell_length_b                   13.9509(2)
_cell_length_c                   20.3839(3)
_cell_measurement_reflns_used    8572
_cell_measurement_temperature    170(1)
_cell_measurement_theta_max      75.6690
_cell_measurement_theta_min      3.8620
_cell_volume                     3439.32(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.91a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.53a 64-bit (release 15-04-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.91a (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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      170(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.967
_diffrn_measured_fraction_theta_max 0.950
_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     35.00  65.00   0.50    0.80    --  106.90 -99.00 -60.00   60
  2  \w     72.00  98.00   0.50    0.80    --  106.90 -99.00 -60.00   52
  3  \w    -30.00  25.00   0.50    0.40    --  -47.16  35.00-167.00  110
  4  \w    -39.00 -14.00   0.50    0.80    --  -86.25  35.00-167.00   50
  5  \w    -61.00 -35.00   0.50    0.80    --  -86.25  57.00-120.00   52
  6  \w    -40.00 -13.00   0.50    0.80    --  -86.25  38.00   0.00   54
  7  \w    -25.00  28.00   0.50    0.40    --  -47.16  19.00 -30.00  106
  8  \w   -120.00 -35.00   0.50    0.40    --  -47.16 -35.00  35.00  170
  9  \w   -120.00 -95.00   0.50    0.80    --  -86.25-111.00-177.00   50
 10  \w   -119.00 -92.00   0.50    0.40    --  -47.16-125.00  90.00   54
 11  \w     39.00  65.00   0.50    0.80    --  106.90 -57.00 -60.00   52
 12  \w     38.00  66.00   0.50    0.80    --  106.90 -57.00   0.00   56
 13  \w     35.00  60.00   0.50    0.80    --  106.90 -57.00-150.00   50
 14  \w     38.00  66.00   0.50    0.80    --  106.90 -57.00 -90.00   56
 15  \w     35.00  60.00   0.50    0.80    --  106.90 -57.00 -30.00   50
 16  \w     38.00  63.00   0.50    0.80    --  106.90 -57.00  30.00   50
 17  \w     37.00  63.00   0.50    0.80    --  106.90 -57.00 150.00   52
 18  \w     41.00  66.00   0.50    0.80    --  106.90 -57.00-180.00   50
 19  \w     99.00 174.00   0.50    0.80    --  106.90  35.00-167.00  150
 20  \w    140.00 166.00   0.50    0.80    --  106.90  19.00-180.00   52
 21  \w     94.00 130.00   0.50    0.80    --  106.90  19.00-180.00   72
 22  \w     96.00 169.00   0.50    0.80    --  106.90  19.00 -30.00  146
 23  \w    138.00 177.00   0.50    0.80    --  106.90  92.00  20.00   78
 24  \w    142.00 176.00   0.50    0.80    --  106.90 125.00  30.00   68
 25  \w    100.00 130.00   0.50    0.80    --  106.90 125.00  30.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0819105000
_diffrn_orient_matrix_UB_12      -0.0820513000
_diffrn_orient_matrix_UB_13      0.0139773000
_diffrn_orient_matrix_UB_21      0.0941205000
_diffrn_orient_matrix_UB_22      0.0593775000
_diffrn_orient_matrix_UB_23      -0.0307188000
_diffrn_orient_matrix_UB_31      0.0257464000
_diffrn_orient_matrix_UB_32      0.0439237000
_diffrn_orient_matrix_UB_33      0.0676330000
_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  0.0150
_diffrn_reflns_av_unetI/netI     0.0128
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10171
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.934
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.368
_diffrn_reflns_theta_min         4.251
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68762
_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_colour_primary    blue
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.155
_exptl_crystal_size_mid          0.148
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.320
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 1452 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.026(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         3440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0299
_refine_ls_R_factor_gt           0.0298
_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^)+(0.0552P)^2^+2.0329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0818
_reflns_Friedel_coverage         0.757
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.913
_reflns_number_gt                3408
_reflns_number_total             3440
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01070a2.cif
_cod_data_source_block           2_170k
_cod_depositor_comments
'Adding full bibliography for 7249643--7249648.cif.'
_cod_original_cell_volume        3439.30(8)
_cod_database_code               7249647
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_angle_alpha         89.9988(11)
_cell_oxdiff_angle_beta          89.9698(11)
_cell_oxdiff_angle_gamma         89.9945(14)
_cell_oxdiff_length_a            12.0923(2)
_cell_oxdiff_length_b            13.9548(3)
_cell_oxdiff_length_c            20.38161(17)
_cell_oxdiff_measurement_reflns_used 8572
_cell_oxdiff_volume              3439.30(9)
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.757
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.a Free rotating group:
 OW1(HW1A,HW1B)
2.b Ternary CH refined with riding coordinates:
 C5(H5)
2.c Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B), C6(H6A,H6B)
2.d Aromatic/amide H refined with riding coordinates:
 N4(H4), C8(H8), C9(H9)
;
_shelx_res_checksum              84398
_shelx_hkl_checksum              13252
_shelx_fab_checksum              30442
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.502
_oxdiff_exptl_absorpt_empirical_full_min 0.739