Cationic first-row transition metal saccharinate complexes with tris(2-pyridylmethyl)amine: synthesis, structures and anticancer studies.
Icsel, Ceyda; Aydinlik, Seyma; Aygun, Muhittin; Yilmaz, Veysel T.; Dalton transactions (Cambridge, England : 2003) 54 (2024) 247–258; doi:10.1039/d4dt02258k

data_7717454
_publ_section_title
;
 Cationic first-row transition metal saccharinate complexes with
 tris(2-pyridylmethyl)amine: synthesis, structures and anticancer studies.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              247
_journal_page_last               258
_journal_paper_doi               10.1039/d4dt02258k
_journal_volume                  54
_journal_year                    2024
_chemical_formula_moiety         'C25 H22 Cu N5 O3 S, C7 H4 N O3 S'
_chemical_formula_sum            'C32 H26 Cu N6 O6 S2'
_chemical_formula_weight         718.25
_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     dual
_audit_creation_date             2024-07-16
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2024-07-30 deposited with the CCDC.	2024-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                62.831(10)
_cell_angle_beta                 80.017(8)
_cell_angle_gamma                84.164(7)
_cell_formula_units_Z            2
_cell_length_a                   10.5153(9)
_cell_length_b                   12.5550(11)
_cell_length_c                   13.0375(14)
_cell_measurement_reflns_used    2151
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.1480
_cell_measurement_theta_min      3.6240
_cell_volume                     1507.6(3)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXD  (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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    -10.00  39.00   1.00   12.81    --   17.59  77.00 -30.00   49
  2  \w    -50.00  41.00   1.00   12.81    --   17.59 -37.00 -30.00   91
  3  \w     -8.00  88.00   1.00   12.81    --   17.59  37.00 150.00   96
  4  \w     -4.00  86.00   1.00   12.81    --   17.59  57.00-120.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0349720000
_diffrn_orient_matrix_UB_12      0.0532442000
_diffrn_orient_matrix_UB_13      -0.0053904000
_diffrn_orient_matrix_UB_21      -0.0529276000
_diffrn_orient_matrix_UB_22      -0.0345167000
_diffrn_orient_matrix_UB_23      0.0385119000
_diffrn_orient_matrix_UB_31      0.0258796000
_diffrn_orient_matrix_UB_32      -0.0029646000
_diffrn_orient_matrix_UB_33      0.0480193000
_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  0.0375
_diffrn_reflns_av_unetI/netI     0.0933
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8356
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         3.182
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.921
_exptl_absorpt_correction_T_max  0.888
_exptl_absorpt_correction_T_min  0.827
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       prism
_exptl_crystal_F_000             738
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5295
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0945
_refine_ls_R_factor_gt           0.0555
_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^)+(0.0297P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.1121
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3577
_reflns_number_total             5295
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02258k2.cif
_cod_data_source_block           Compound_III
_cod_depositor_comments
'Adding full bibliography for 7717453--7717455.cif.'
_cod_database_code               7717454
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C32 H26 Cu N6 O6 S2'
_shelx_estimated_absorpt_t_max   0.867
_shelx_estimated_absorpt_t_min   0.757
_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), C13(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24),
  C28(H28), C29(H29), C30(H30), C31(H31)
;
_shelx_res_checksum              94140
_shelx_hkl_checksum              27477
_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 1.131
_oxdiff_exptl_absorpt_empirical_full_min 0.865