Copper(ii) complexes with 2-ethylpyridine and related hydroxyl pyridine derivatives: structural, spectroscopic, magnetic and anticancer in vitro studies
Malik, Magdalena; Świtlicka, Anna; Bieńko, Alina; Komarnicka, Urszula K.; Bieńko, Dariusz C.; Kozieł, Sandra; Kyzioł, Agnieszka; Mazur, Tomasz; Machura, Barbara; RSC Advances 12 (2022) 27648–27665; doi:10.1039/D2RA05133H

data_7245588
_publ_section_title
;
 Copper(ii) complexes with 2-ethylpyridine and related hydroxyl pyridine
 derivatives: structural, spectroscopic, magnetic and anticancer in vitro
 studies
;
_journal_issue                   42
_journal_name_full               'RSC Advances'
_journal_page_first              27648
_journal_page_last               27665
_journal_paper_doi               10.1039/D2RA05133H
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C12 H12 Cu N2 O2, 4(H2 O)'
_chemical_formula_sum            'C12 H20 Cu N2 O6'
_chemical_formula_weight         351.84
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-01-30
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-12-01 deposited with the CCDC.	2022-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 110.398(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.5721(14)
_cell_length_b                   7.1790(5)
_cell_length_c                   8.2686(6)
_cell_measurement_reflns_used    2151
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6690
_cell_measurement_theta_min      4.5200
_cell_volume                     755.13(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -22.00  39.00   1.00    1.13    --   10.37  77.00  60.00   61
  2  \w    -86.00   4.00   1.00    1.13    --  -11.39 -38.00  30.00   90
  3  \w    -51.00  27.00   1.00    1.13    --  -11.39  19.00 -90.00   78
  4  \w     -4.00  67.00   1.00    1.13    --   10.22  38.00 -90.00   71
  5  \w     14.00  39.00   1.00    1.13    --  -11.23  77.00 150.00   25
  6  \w    -44.00  17.00   1.00    1.13    --  -11.23 -57.00  90.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0280914000
_diffrn_orient_matrix_UB_12      -0.0937570000
_diffrn_orient_matrix_UB_13      -0.0039438000
_diffrn_orient_matrix_UB_21      -0.0749463000
_diffrn_orient_matrix_UB_22      0.0269741000
_diffrn_orient_matrix_UB_23      -0.0375484000
_diffrn_orient_matrix_UB_31      0.0389253000
_diffrn_orient_matrix_UB_32      -0.0156905000
_diffrn_orient_matrix_UB_33      -0.0410422000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0189
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3292
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.049
_diffrn_reflns_theta_max         25.049
_diffrn_reflns_theta_min         3.362
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.474
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.07772
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       brick
_exptl_crystal_F_000             366
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.275
_refine_diff_density_rms         0.069
_refine_ls_extinction_coef       0.040(3)
_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   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         728
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0291
_refine_ls_R_factor_gt           0.0283
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0354P)^2^+1.0586P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                712
_reflns_number_total             728
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra05133h2.cif
_cod_data_source_block           cuk2
_cod_original_cell_volume        755.12(11)
_cod_database_code               7245588
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C20 H15 N3 O2 Cl2 Cu1'
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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 O(H,H) groups
2. Others
 Fixed Sof: H6A(0.5) H6B(0.5)
3.a Free rotating group:
 O2(H2A,H2B)
3.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
;
_shelx_res_checksum              29711
_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 7.661
_oxdiff_exptl_absorpt_empirical_full_min 0.584