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_7245587
_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         'C14 H16 Cl2 Cu2 N2 O2'
_chemical_formula_sum            'C14 H16 Cl2 Cu2 N2 O2'
_chemical_formula_weight         442.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2020-10-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2021-05-04 deposited with the CCDC.	2022-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                89.741(5)
_cell_angle_beta                 79.214(4)
_cell_angle_gamma                70.029(6)
_cell_formula_units_Z            1
_cell_length_a                   6.1899(3)
_cell_length_b                   8.0094(5)
_cell_length_c                   8.5356(4)
_cell_measurement_reflns_used    3388
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.9930
_cell_measurement_theta_min      4.0880
_cell_volume                     389.89(4)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.880
_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    -21.00  83.00   1.00    1.00    --    9.59  67.00-105.00  104
  2  \w    -63.00  40.00   1.00    1.00    --    9.59 -67.00 120.00  103
  3  \w    -23.00  39.00   1.00    1.00    --    9.59  77.00 -90.00   62
  4  \w    -45.00  39.00   1.00    1.00    --  -12.01  77.00   0.00   84
  5  \w   -100.00 -40.00   1.00    1.00    --  -12.01-179.00 150.00   60
  6  \w    -61.00 -35.00   1.00    1.00    --    9.51 -57.00 -30.00   26
  7  \w     -8.00  76.00   1.00    1.00    --    9.51  57.00 120.00   84
  8  \w    -81.00 -55.00   1.00    1.00    --  -11.93 145.00 -90.56   26
  9  \w    -84.00  -1.00   1.00    1.00    --  -11.93 -38.00 -30.00   83
 10  \w    -87.00 -62.00   1.00    1.00    --  -11.93 153.00 167.59   25
 11  \w    -88.00 -49.00   1.00    1.00    --  -11.93 154.00  68.32   39
;
_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      -0.0579148000
_diffrn_orient_matrix_UB_12      0.0263046000
_diffrn_orient_matrix_UB_13      -0.0650558000
_diffrn_orient_matrix_UB_21      0.0396443000
_diffrn_orient_matrix_UB_22      0.0734455000
_diffrn_orient_matrix_UB_23      -0.0085553000
_diffrn_orient_matrix_UB_31      0.1026761000
_diffrn_orient_matrix_UB_32      -0.0531870000
_diffrn_orient_matrix_UB_33      -0.0536683000
_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  0.0403
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.880
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7390
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.530
_diffrn_reflns_theta_min         3.526
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.076
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36007
_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            blue
_exptl_crystal_density_diffrn    1.884
_exptl_crystal_description       brick
_exptl_crystal_F_000             222
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.328
_refine_diff_density_min         -0.578
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     100
_refine_ls_number_reflns         1922
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0309
_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^)+(0.0311P)^2^+0.1058P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1611
_reflns_number_total             1922
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra05133h2.cif
_cod_data_source_block           cuk3
_cod_database_code               7245587
_shelx_shelxl_version_number     2018/3
_reflns_odcompleteness_completeness 99.75
_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
2.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4)
;
_shelx_res_checksum              37701
_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 2.203
_oxdiff_exptl_absorpt_empirical_full_min 0.698