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_7249645
_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(C0.703 H3.11 O), 0.593(O)'
_chemical_formula_sum            'C19.41 H30.22 Cu2 N8 O8.59'
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-11
_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                   12.08960(8)
_cell_length_b                   20.35323(15)
_cell_length_c                   13.73806(9)
_cell_measurement_reflns_used    18279
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      30.0060
_cell_measurement_theta_min      1.9390
_cell_volume                     3380.42(4)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      100(1)
_diffrn_detector                 'Dectris Pilatus'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -180.00 180.00   1.00    0.50   0.00   0.00   0.00    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dectris-CrysAlisPro-abstract goniometer imported dectris images'
_diffrn_measurement_method       '\f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0425063000
_diffrn_orient_matrix_UB_12      -0.0044604000
_diffrn_orient_matrix_UB_13      0.0339289000
_diffrn_orient_matrix_UB_21      0.0355078000
_diffrn_orient_matrix_UB_22      0.0101338000
_diffrn_orient_matrix_UB_23      0.0373749000
_diffrn_orient_matrix_UB_31      -0.0168851000
_diffrn_orient_matrix_UB_32      0.0325611000
_diffrn_orient_matrix_UB_33      -0.0069380000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.700
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 0.944
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            29910
_diffrn_reflns_point_group_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        24.835
_diffrn_reflns_theta_max         30.000
_diffrn_reflns_theta_min         1.930
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.255
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 2249 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(5)
_refine_ls_extinction_coef       0.0240(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         4990
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0522P)^2^+2.3407P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0805
_reflns_Friedel_coverage         0.829
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.976
_reflns_number_gt                4983
_reflns_number_total             4990
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce01070a2.cif
_cod_data_source_block           2_100k
_cod_depositor_comments
'Adding full bibliography for 7249643--7249648.cif.'
_cod_database_code               7249645
_shelx_shelxl_version_number     2018/3
_cell_oxdiff_angle_alpha         90.048(3)
_cell_oxdiff_angle_beta          90.041(4)
_cell_oxdiff_angle_gamma         89.992(3)
_cell_oxdiff_length_a            12.0888(6)
_cell_oxdiff_length_b            20.3534(4)
_cell_oxdiff_length_c            13.7389(7)
_cell_oxdiff_measurement_reflns_used 18284
_cell_oxdiff_volume              3380.4(2)
_reflns_odcompleteness_completeness 98.05
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.00
_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 C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-C10
 1.4 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O4 \\sim C10: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
within 2A
4. Rigid body (RIGU) restrains
 O4, C10
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=1-FVAR(1)
 Sof(O2W)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C5(H5)
6.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C1(H1C,H1D), C2(H2A,H2B), C6(H6A,H6B)
6.c Aromatic/amide H refined with riding coordinates:
 N4(H4), C8(H8), C9(H9)
6.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
6.e Idealised tetrahedral OH refined as rotating group:
 O4(H4A)
;
_shelx_res_checksum              94727
_shelx_hkl_checksum              85737
_shelx_fab_checksum              56244
_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 1.397
_oxdiff_exptl_absorpt_empirical_full_min 0.751