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_7712399
_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         '2(C10 H9 F N2 S)'
_chemical_formula_sum            'C20 H18 F2 N4 S2'
_chemical_formula_weight         416.522
_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                74.821(3)
_cell_angle_beta                 89.867(3)
_cell_angle_gamma                71.907(3)
_cell_formula_units_Z            2
_cell_length_a                   8.5021(3)
_cell_length_b                   10.7959(4)
_cell_length_c                   11.6276(4)
_cell_measurement_reflns_used    6188
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.3850
_cell_measurement_theta_min      3.6370
_cell_volume                     975.47(6)
_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 0.9963
_diffrn_measured_fraction_theta_max 0.9964
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.9963
_diffrn_reflns_Laue_measured_fraction_max 0.9964
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            19886
_diffrn_reflns_point_group_measured_fraction_full 0.9963
_diffrn_reflns_point_group_measured_fraction_max 0.9964
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54254
_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    1.418
_exptl_crystal_description       prism
_exptl_crystal_F_000             432.761
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.2757
_refine_diff_density_min         -0.3486
_refine_diff_density_rms         0.0638
_refine_ls_d_res_high            0.8255
_refine_ls_d_res_low             6.2822
_refine_ls_goodness_of_fit_ref   1.0815
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    35
_refine_ls_number_parameters     278
_refine_ls_number_reflns         3604
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0815
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0365
_refine_ls_shift/su_max          0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0365P)^2^+0.4597P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0846
_refine_ls_wR_factor_ref         0.0898
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              -12
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                3001
_reflns_number_total             3604
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt00079f2.cif
_cod_data_source_block           c537
_cod_original_cell_volume        975.46(6)
_cod_database_code               7712399
_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. Others
 Sof(F3)=Sof(F4)=Sof(Hi)=Sof(H17)=1-FVAR(1)
 Sof(F1)=Sof(Hg)=Sof(F2)=Sof(H19)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C3(Hc,Hd), C13(H13a,H13b)
3.b Aromatic/amide H refined with riding coordinates:
 C6(He), C8(Hf), C9(Hg), C10(Hh), C16(H16), C18(H18), C19(H19), C20(H20),
 C7(Hi), C17(H17)
3.c X=CH2 refined with riding coordinates:
 C2(Ha,Hb), C12(H12a,H12b)
;
_olex2_submission_special_instructions 'No special instructions were received'