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_7717453
_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_absolute_configuration ad
_chemical_formula_moiety         'C18 H22 N4 Ni O2, 2(C7 H4 N O3 S), 2(H2 O)'
_chemical_formula_sum            'C32 H34 N6 Ni O10 S2'
_chemical_formula_weight         785.48
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 94.258(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.1477(17)
_cell_length_b                   16.206(3)
_cell_length_c                   10.5149(17)
_cell_measurement_reflns_used    381
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      20.5980
_cell_measurement_theta_min      4.3390
_cell_volume                     1724.4(5)
_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    'SHELXT  (Sheldrick, 2015)'
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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    -27.00  29.00   1.00   11.19    --   14.36 -57.00 120.00   56
  2  \w    -39.00   8.00   1.00   11.19    --  -16.39 -77.00 -90.00   47
  3  \w    -70.00  -5.00   1.00   11.19    --  -16.39 -19.00-150.00   65
  4  \w     39.00  64.00   1.00   11.19    --   14.20 178.00  90.00   25
;
_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      -0.0242809000
_diffrn_orient_matrix_UB_12      -0.0409809000
_diffrn_orient_matrix_UB_13      -0.0066173000
_diffrn_orient_matrix_UB_21      -0.0389277000
_diffrn_orient_matrix_UB_22      0.0117039000
_diffrn_orient_matrix_UB_23      -0.0558531000
_diffrn_orient_matrix_UB_31      0.0530122000
_diffrn_orient_matrix_UB_32      -0.0101334000
_diffrn_orient_matrix_UB_33      -0.0374351000
_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  0.0425
_diffrn_reflns_av_unetI/netI     0.0990
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6532
_diffrn_reflns_point_group_measured_fraction_full 0.726
_diffrn_reflns_point_group_measured_fraction_max 0.726
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         2.971
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.947
_exptl_absorpt_correction_T_min  0.761
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_description       prism
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.073
_refine_ls_abs_structure_details
;
 Flack x determined using 760 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         4420
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      0.991
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0147P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0839
_reflns_Friedel_coverage         0.408
_reflns_Friedel_fraction_full    0.438
_reflns_Friedel_fraction_max     0.438
_reflns_number_gt                3335
_reflns_number_total             4420
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02258k2.cif
_cod_data_source_block           Compound_II
_cod_depositor_comments
'Adding full bibliography for 7717453--7717455.cif.'
_cod_original_cell_volume        1724.5(5)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7717453
_shelx_shelxl_version_number     2019/2
_chemical_oxdiff_formula         'C32 H34 N6 Ni O10 S2'
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.670
_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. Restrained distances
 Ni1-H1WA \\sim Ni1-H1WB
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C26, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C23, C24
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C2, C3
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C10, C11
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Free rotating group:
 O1W(H1WA,H1WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB)
4.b Rotating group:
 O2W(H2WA,H2WB)
4.c Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B)
4.d 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              56665
_shelx_hkl_checksum              67017
_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 1.170
_oxdiff_exptl_absorpt_empirical_full_min 0.918