Disulfide/thiol switches in thiosemicarbazone ligands for redox-directed iron chelation.
Chang, Tsuhen M.; Tomat, Elisa; Dalton transactions (Cambridge, England : 2003) 42 (2013) 7846–7849; doi:10.1039/c3dt50824b

data_7021512
_publ_section_title
;
 Disulfide/thiol switches in thiosemicarbazone ligands for redox-directed
 iron chelation.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7846
_journal_page_last               7849
_journal_paper_doi               10.1039/c3dt50824b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C16 H16 Fe N6 S4, B F4, 2(C4 H8 O)'
_chemical_formula_sum            'C24 H32 B F4 Fe N6 O2 S4'
_chemical_formula_weight         707.46
_chemical_name_systematic
;
?
;
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-12-11
_audit_creation_method
;
Olex2 1.2
(compiled Oct 26 2012 17:09:49, GUI svn.r4371)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.284(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.8891(8)
_cell_length_b                   10.8996(7)
_cell_length_c                   25.8263(19)
_cell_measurement_reflns_used    4645
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.56
_cell_measurement_theta_min      2.45
_cell_volume                     3056.7(4)
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_av_unetI/netI     0.0545
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            25909
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.58
_diffrn_source                   'sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6583
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0642 before and 0.0545 after correction.
The Ratio of minimum to maximum transmission is 0.8833.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'dull black'
_exptl_crystal_colour_lustre     dull
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1460
_exptl_crystal_size_max          0.213
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.031
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         5387
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0668
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+2.7119P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0745
_refine_ls_wR_factor_ref         0.0850
_reflns_number_gt                3891
_reflns_number_total             5387
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt50824b.txt
_cod_data_source_block           mo_et205b_0mtest
_cod_database_code               7021512
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
{H12A,H12B} of C12, {H15C,H15D} of C15B, H3BC of C3B, {H14C,H14D} of C14B,
{H9AA,H9AB,H9BC,H9BD} of C9, {H14A,H14B} of C14, {H15A,H15B} of C15, H2A of
C2, H2BA of C2B, H4 of C4, {H13A,H13B,H13C,H13D} of C13, {H16A,H16B,H16C,
H16D} of C16, H4B of C4B, {H10A,H10B} of C10A, H3 of C3, H5 of C5, {H10C,
H10D} of C10B, H7B of C7B, H5B of C5B, H7 of C7, {H11A,H11B,H11C,H11D} of C11
2. Restrained distances
N2B-H2B = N3B-H3BB = N3B-H3BA = N3-H3B = N3-H3A = N2-H2
0.87 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C13 ~ C14 ~ C15 ~ C16: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C13) ~ Ueq, Uanis(C14) ~ Ueq, Uanis(C15) ~ Ueq, Uanis(C16) ~ Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Others
1-Sof(H9AB)=1-Sof(H9AB)=Sof(H9BC)=Sof(H9BD)=1-Sof(H9AB)=1-Sof(H9AB)=Sof(H11C)=
Sof(H11D)=1-Sof(H9AB)=1-Sof(H9AB)=1-Sof(H9AB)=Sof(C10B)=Sof(H10C)=Sof(H10D)
1-Sof(H16B)=1-Sof(H16B)=Sof(H16C)=Sof(H16D)=1-Sof(H16B)=1-Sof(H16B)=Sof(H13C)=
Sof(H13D)=1-Sof(H16B)=1-Sof(H16B)=1-Sof(H16B)=1-Sof(H16B)=1-Sof(H16B)=1-
Sof(H16B)=1-Sof(H16B)=Sof(O2B)=Sof(C15B)=Sof(H15C)=Sof(H15D)=Sof(C14B)=
Sof(H14C)=Sof(H14D)
5.a Secondary CH2 refined with riding coordinates:
C16(H16A,H16B), C16(H16C,H16D), C13(H13A,H13B), C13(H13C,H13D), C15(H15A,
H15B), C14(H14A,H14B), C15B(H15C,H15D), C14B(H14C,H14D), C9(H9AA,H9AB),
C9(H9BC,H9BD), C12(H12A,H12B), C11(H11A,H11B), C11(H11C,H11D), C10A(H10A,H10B),
C10B(H10C,H10D)
5.b Aromatic/amide H refined with riding coordinates:
C7(H7), C2B(H2BA), C2(H2A), C4(H4), C3B(H3BC), C5B(H5B), C7B(H7B), C5(H5),
C3(H3), C4B(H4B)
;