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_7245589
_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         'C28 H36 Cl6 Cu4 N4 O'
_chemical_formula_sum            'C28 H36 Cl6 Cu4 N4 O'
_chemical_formula_weight         911.47
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-12-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-05-04 deposited with the CCDC.	2022-09-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.620(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7450(7)
_cell_length_b                   11.9340(6)
_cell_length_c                   18.8133(9)
_cell_measurement_reflns_used    7161
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      27.4930
_cell_measurement_theta_min      3.7230
_cell_volume                     3653.8(3)
_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_area_resol_mean 10.4015
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.871
_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      1.00  51.00   1.00   71.89    --    9.90 -99.00   0.00   50
  2  \w    -23.00  39.00   1.00   71.89    --    9.90  77.00 -90.00   62
  3  \w    -28.00  48.00   1.00   71.89    --  -11.54  38.00  60.00   76
  4  \w    -76.00   5.00   1.00   71.89    --  -11.54 -19.00-150.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0509
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.871
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            25795
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.871
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.523
_diffrn_reflns_theta_min         3.394
_exptl_absorpt_coefficient_mu    2.764
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64877
_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            green
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       prism
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.394
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         8883
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0793
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0299P)^2^+1.0482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0717
_refine_ls_wR_factor_ref         0.0857
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5788
_reflns_number_total             8883
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ra05133h2.cif
_cod_data_source_block           cuk1_2
_cod_database_code               7245589
_shelx_shelxl_version_number     2018/3
_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 C(H,H,H) groups
2. Others
 Fixed Sof: C20A(0.5) H20A(0.5) H20B(0.5) C21A(0.5) H21A(0.5) H21B(0.5)
 H21C(0.5) C20B(0.5) H20C(0.5) H20D(0.5) C21B(0.5) H21D(0.5) H21E(0.5) H21F(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C13(H13A,H13B), C27(H27A,H27B), C20A(H20A,H20B), C20B(H20C,H20D)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C8(H8), C9(H9), C10(H10), C11(H11), C15(H15),
 C16(H16), C17(H17), C18(H18), C22(H22), C23(H23), C24(H24), C25(H25)
3.c Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C14(H14A,H14B,H14C), C28(H28A,H28B,H28C), C21A(H21A,H21B,
 H21C), C21B(H21D,H21E,H21F)
;
_shelx_res_checksum              70265
_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
;