A bioinspired redox-modulating copper(II)-macrocyclic complex bearing non-steroidal anti-inflammatory drugs with anti-cancer stem cell activity
Johnson, Alice; Iffland, Linda; Northcote-Smith, Joshua; Singh, Kuldip; Ortu, Fabrizio; Apfel, Ulf-Peter; Suntharalingam, Kogularamanan; Dalton Transactions  (2022) –; doi:10.1039/D2DT00788F

data_7709770
_publ_section_title
;
 A bioinspired redox-modulating copper(II)-macrocyclic complex bearing
 non-steroidal anti-inflammatory drugs with anti-cancer stem cell activity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00788F
_journal_year                    2022
_chemical_formula_moiety         'C10 H24 Cu N4, 2(C14 H10 Cl2 N O2), 2(H2 O)'
_chemical_formula_sum            'C38 H48 Cl4 Cu N6 O6'
_chemical_formula_weight         890.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-12-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6403)
;
_audit_update_record
;
2021-12-22 deposited with the CCDC.	2022-03-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.713(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.109(15)
_cell_length_b                   7.269(7)
_cell_length_c                   15.999(14)
_cell_measurement_reflns_used    475
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.334
_cell_measurement_theta_min      2.297
_cell_volume                     2062(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex 2000 CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.3598
_diffrn_reflns_av_unetI/netI     0.3708
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15546
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         2.297
_exptl_absorpt_coefficient_mu    0.841
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_correction_T_min  0.191
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
absoprtion correction based on 1320 reflections(SADABS);Rint 0.2055 before
correction and 0.1147 after.
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       plate
_exptl_crystal_F_000             926
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.645
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.865
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4034
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.864
_refine_ls_R_factor_all          0.3005
_refine_ls_R_factor_gt           0.1013
_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^)+(0.0945P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2054
_refine_ls_wR_factor_ref         0.2788
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1171
_reflns_number_total             4034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt00788f2.cif
_cod_data_source_block           3
_cod_database_code               7709770
_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, All N(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O3-H3C = O3-H3D
 0.87 with sigma of 0.02
 H3C-H3D
 1.38 with sigma of 0.04
3.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2)
3.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C18(H18A,H18B)
3.c Aromatic/amide H refined with riding coordinates:
 N3(H3), C8(H8), C9(H9), C10(H10), C13(H13), C14(H14), C15(H15), C16(H16)
;
_shelx_res_checksum              52837
_olex2_submission_special_instructions 'No special instructions were received'