Free-Catalysed Synthesis of Thiazolidine-Thiourea Ligands for Metal Coordination (Au and Ag) and Preliminary Cytotoxic Studies
Salvador, Daniel; Herrera, Raquel; Gimeno, Maria Concepcion; Dalton Transactions  (2023) –; doi:10.1039/D3DT00079F

data_7712400
_publ_section_title
;
 Free-Catalysed Synthesis of Thiazolidine-Thiourea Ligands for Metal
 Coordination (Au and Ag) and Preliminary Cytotoxic Studies
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00079F
_journal_year                    2023
_chemical_formula_moiety         'C17 H13 F2 N3 S2'
_chemical_formula_sum            'C17 H13 F2 N3 S2'
_chemical_formula_weight         361.442
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2023-01-31
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2023.01.20 svn.r024a95a1 for OlexSys, GUI svn.r6444)
;
_audit_update_record
;
2023-02-17 deposited with the CCDC.	2023-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                66.050(3)
_cell_angle_beta                 75.680(3)
_cell_angle_gamma                86.964(2)
_cell_formula_units_Z            2
_cell_length_a                   7.2678(2)
_cell_length_b                   10.3032(3)
_cell_length_c                   11.8115(4)
_cell_measurement_reflns_used    9680
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.0250
_cell_measurement_theta_min      3.5110
_cell_volume                     782.07(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.9958
_diffrn_measured_fraction_theta_max 0.9312
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w rotations'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.9958
_diffrn_reflns_Laue_measured_fraction_max 0.9312
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21492
_diffrn_reflns_point_group_measured_fraction_full 0.9958
_diffrn_reflns_point_group_measured_fraction_max 0.9312
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         31.06
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    0.366
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84573
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_description       prism
_exptl_crystal_F_000             372.727
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.4661
_refine_diff_density_min         -0.2702
_refine_diff_density_rms         0.0662
_refine_ls_d_res_high            0.6888
_refine_ls_d_res_low             6.0512
_refine_ls_goodness_of_fit_ref   1.0443
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    27
_refine_ls_number_parameters     227
_refine_ls_number_reflns         4667
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.0418
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0323
_refine_ls_shift/su_max          0.0010
_refine_ls_shift/su_mean         0.0002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0428P)^2^+0.3772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0878
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -9
_reflns_limit_k_max              14
_reflns_limit_k_min              -13
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                4196
_reflns_number_total             4667
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt00079f2.cif
_cod_data_source_block           c547
_cod_original_cell_volume        782.08(5)
_cod_database_code               7712400
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Rigid body (RIGU) restrains
 C4, F3, C6, C5, F1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(F3)=Sof(H6)=1-FVAR(1)
 Sof(F1)=Sof(H4)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C8(H8a,H8b)
4.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C3(H3), C17(H17), C16(H16), C15(H15), C13(H13), C4(H4),
 C6(H6), N1(H1)
4.c X=CH2 refined with riding coordinates:
 C10(H10a,H10b)
;
_olex2_submission_special_instructions 'No special instructions were received'