Enantiomeric pairs of copper(ii) complexes with tridentate Schiff bases derived from R- and S-methionine: the role of decorating organic groups of the ligand in crystal packing and biological activity
Maxim, Catalin; Ene, Cristian D.; Nicolau, Ioana; Ruta, Lavinia L.; Farcasanu, Ileana C.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02620A

data_7711497
_publ_section_title
;
 Enantiomeric pairs of copper(ii) complexes with tridentate Schiff bases
 derived from R- and S-methionine: the role of decorating organic groups
 of the ligand in crystal packing and biological activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02620A
_journal_year                    2022
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C24 H28 Cu2 N2 O7 S2'
_chemical_formula_sum            'C24 H28 Cu2 N2 O7 S2'
_chemical_formula_weight         647.68
_chemical_name_common            1?[Cu2(R-salmet)2(H2O)]
_chemical_name_systematic        1?[Cu2(R-salmet)2(H2O)]
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-01-30
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-06-05 deposited with the CCDC.	2022-10-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.06810(12)
_cell_length_b                   13.2698(4)
_cell_length_c                   37.6991(10)
_cell_measurement_reflns_used    10691
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.3120
_cell_measurement_theta_min      2.147
_cell_volume                     2535.37(12)
_computing_cell_refinement       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.74a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.74a (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      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -32.00  53.00   0.50   14.00    --  -10.08  49.00   5.00  170
  2  \w    -55.00 -18.00   0.50   14.00    --  -10.08 135.00  53.00   74
  3  \w    -23.00   8.00   0.50   14.00    --  -10.08 -99.00 -30.00   62
  4  \w    -18.00  21.00   0.50   14.00    --  -10.08 -99.00-120.00   78
  5  \w    -24.00  14.00   0.50   14.00    --  -10.08 -99.00-180.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at offset/far, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0307139000
_diffrn_orient_matrix_UB_12      0.0499913000
_diffrn_orient_matrix_UB_13      0.0052185000
_diffrn_orient_matrix_UB_21      -0.0808633000
_diffrn_orient_matrix_UB_22      0.0189302000
_diffrn_orient_matrix_UB_23      -0.0138427000
_diffrn_orient_matrix_UB_31      -0.1100189000
_diffrn_orient_matrix_UB_32      0.0000699000
_diffrn_orient_matrix_UB_33      0.0116224000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0325
_diffrn_reflns_av_unetI/netI     0.0327
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            14444
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.161
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.891
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78001
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.74a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'greenish black'
_exptl_crystal_density_diffrn    1.697
_exptl_crystal_description       prism
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details
;
 Flack x determined using 1617 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.009(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4429
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0289
_refine_ls_R_factor_gt           0.0261
_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^)+(0.0277P)^2^+0.8160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0593
_refine_ls_wR_factor_ref         0.0609
_reflns_Friedel_coverage         0.693
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                4174
_reflns_number_total             4429
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02620a2.cif
_cod_data_source_block           1Rw
_cod_original_cell_volume        2535.36(12)
_cod_database_code               7711497
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H10 Cu1 N2 O10'
_olex2_refinement_description
;
1.a Rotating group:
 O1W(H1WA,H1WB)
1.b Ternary CH refined with riding coordinates:
 C8(H8), C19(H19)
1.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C21(H21A,H21B), C22(H22A,H22B), C10(H10A,H10B)
1.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C7(H7), C2(H2), C3(H3), C1(H1), C16(H16), C6(H6), C13(H13),
 C17(H17), C12(H12)
1.e Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              81688
_shelx_hkl_checksum              55236
_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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.538