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_7717455
_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
'C36 H36 Cl2 Fe2 N8 O, 2(C7 H4 N O3 S), 3(H2 O)'
_chemical_formula_sum            'C50 H50 Cl2 Fe2 N10 O10 S2'
_chemical_formula_weight         1197.72
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-30
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-30 deposited with the CCDC.	2024-11-01 downloaded from the CCDC.
;
_cell_angle_alpha                99.02(3)
_cell_angle_beta                 112.39(3)
_cell_angle_gamma                116.69(4)
_cell_formula_units_Z            4
_cell_length_a                   18.776(8)
_cell_length_b                   19.465(7)
_cell_length_c                   19.694(6)
_cell_measurement_reflns_used    499
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.3130
_cell_measurement_theta_min      3.5930
_cell_volume                     5458(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (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 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 8.0667
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.964
_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    -93.00   1.00   1.00   30.02    --  -22.18 -57.00  90.00   94
  2  \w    -37.00  10.00   1.00   30.02    --  -22.18 -77.00-111.00   47
  3  \w    -93.00   2.00   1.00   30.02    --  -22.18 -57.00 -30.00   95
  4  \w    -46.00  47.00   1.00   30.02    --  -22.18  57.00-120.00   93
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.3119
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            32405
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        25.105
_diffrn_reflns_theta_max         25.105
_diffrn_reflns_theta_min         3.061
_exptl_absorpt_coefficient_mu    0.772
_exptl_absorpt_correction_T_max  0.857
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (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            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       prism
_exptl_crystal_F_000             2472
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.302
_refine_diff_density_min         -0.783
_refine_diff_density_rms         0.181
_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     897
_refine_ls_number_reflns         32405
_refine_ls_number_restraints     1359
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.2389
_refine_ls_R_factor_gt           0.1241
_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^)+(0.1804P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3278
_refine_ls_wR_factor_ref         0.3835
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10907
_reflns_number_total             32405
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9730\% 
around [1.00 0.00 -0.00] (reciprocal) or [0.83 0.42 0.37] (direct)
Component 3 rotated by -179.8075\% 
around [-0.55 0.58 0.60] (reciprocal) or [0.00 0.71 0.71] (direct)
;
_cod_data_source_file            d4dt02258k2.cif
_cod_data_source_block           Compound_I
_cod_depositor_comments
'Adding full bibliography for 7717453--7717455.cif.'
_cod_original_cell_volume        5457(4)
_cod_database_code               7717455
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.825
_shelx_estimated_absorpt_t_min   0.743
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.471(2)
 0.3053(19) 0.2234(15)
2. 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
3. Restrained distances
 N2-C6
 1.5 with sigma of 0.02
 N15-C80
 1.4 with sigma of 0.02
 C80-C81
 1.5 with sigma of 0.02
 C79-C74 \\sim C79-C78 \\sim C78-C77 \\sim C77-C76 \\sim C76-C75 \\sim C75-C74
 with sigma of 0.02
 C93-C88 \\sim C93-C92 \\sim C92-C91 \\sim C91-C90 \\sim C90-C89 \\sim C89-C88
 with sigma of 0.02
 C86-C81 \\sim C86-C85 \\sim C85-C84 \\sim C84-C83 \\sim C83-C82 \\sim C82-C81
 with sigma of 0.02
 C95-C100 \\sim C96-C95 \\sim C97-C96 \\sim C98-C97 \\sim C99-C98 \\sim C99-C100
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(N20) = Uanis(N17) = Uanis(N18) = Uanis(N19)
Uanis(O8) = Uanis(O10) = Uanis(O9)
Uanis(N11) = Uanis(N12) = Uanis(N14) = Uanis(N13)
Uanis(N8) = Uanis(N9) = Uanis(N10) = Uanis(N7)
Uanis(N5) = Uanis(N16) = Uanis(N15) = Uanis(N6)
Uanis(N3) = Uanis(N2) = Uanis(N1) = Uanis(N4)
Uanis(O11) = Uanis(O12) = Uanis(O13)
Uanis(O2) = Uanis(O4) = Uanis(O3)
Uanis(O1) = Uanis(O14) = Uanis(O15) = Uanis(O16)
Uanis(C74) = Uanis(C79) = Uanis(C78) = Uanis(C77) = Uanis(C76) = Uanis(C75)
Uanis(C50) = Uanis(C51) = Uanis(C52) = Uanis(C53) = Uanis(C54)
Uanis(C68) = Uanis(C69) = Uanis(C70) = Uanis(C71) = Uanis(C72)
Uanis(C14) = Uanis(C15) = Uanis(C16) = Uanis(C17) = Uanis(C18)
Uanis(C32) = Uanis(C33) = Uanis(C34) = Uanis(C35) = Uanis(C36)
Uanis(C55) = Uanis(C56) = Uanis(C57) = Uanis(C58) = Uanis(C59) = Uanis(C60)
Uanis(C66) = Uanis(C65) = Uanis(C64) = Uanis(C63) = Uanis(C62) = Uanis(C61)
Uanis(C48) = Uanis(C47) = Uanis(C46) = Uanis(C45) = Uanis(C44) = Uanis(C43)
Uanis(C37) = Uanis(C38) = Uanis(C39) = Uanis(C40) = Uanis(C41) = Uanis(C42)
Uanis(C7) = Uanis(C6)
Uanis(C19) = Uanis(C20) = Uanis(C21) = Uanis(C22) = Uanis(C23) = Uanis(C24)
Uanis(C25) = Uanis(C26) = Uanis(C27) = Uanis(C28) = Uanis(C29) = Uanis(C30)
Uanis(O2W) = Uanis(O1W)
Uanis(O5W) = Uanis(O3W) = Uanis(O4W) = Uanis(O6W)
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Riding coordinates:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,
 H5WB), O6W(H6WA,H6WB)
6.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C13(H13A,H13B), C24(H24A,H24B), C25(H25A,H25B),
 C31(H31A,H31B), C42(H42A,H42B), C43(H43A,H43B), C49(H49A,H49B), C60(H60A,H60B),
  C61(H61A,H61B), C67(H67A,H67B)
6.c 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), C19(H19), C20(H20), C21(H21), C22(H22),
  C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37), C38(H38), C39(H39), C40(H40), C45(H45), C46(H46), C47(H47),
  C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56),
 C57(H57), C58(H58), C63(H63), C64(H64), C65(H65), C66(H66), C69(H69), C70(H70),
  C71(H71), C72(H72), C96(H96), C97(H97), C98(H98), C99(H99), C75(H75),
 C76(H76), C77(H77), C78(H78), C89(H89), C90(H90), C91(H91), C92(H92), C82(H82),
  C83(H83), C84(H84), C85(H85)
;
_shelx_res_checksum              58773
_shelx_hkl_checksum              82860
_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
;