I2 or I2/PIFA one-pot induced system for rapid synthesis of chalcogenated enamides, uracils or 2-pyridones under mild conditions
Sanaa, Hamdi; Dondasse, Ismaël; Retailleau, Pascal; Nicolas, Cyril; Gillaizeau, Isabelle; New Journal of Chemistry 48 (2024) 12793–12799; doi:10.1039/D4NJ01989J

data_7063274
_publ_section_title
;
 I2 or I2/PIFA one-pot induced system for rapid synthesis of chalcogenated
 enamides, uracils or 2-pyridones under mild conditions
;
_journal_issue                   28
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              12793
_journal_page_last               12799
_journal_paper_doi               10.1039/D4NJ01989J
_journal_volume                  48
_journal_year                    2024
_chemical_formula_moiety         'C18 H15 Cl2 N O S'
_chemical_formula_sum            'C18 H15 Cl2 N O S'
_chemical_formula_weight         364.27
_chemical_name_systematic
;
'1-benzyl-5-((3,5-dichlorophenyl)thio)-3,4-dihydropyridin-2(1H)-one'
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2024-04-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-22 deposited with the CCDC.	2024-06-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.401(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1843(11)
_cell_length_b                   11.2815(3)
_cell_length_c                   10.2878(2)
_cell_measurement_reflns_used    9250
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      71.8
_cell_measurement_theta_min      3.0
_cell_volume                     1738.65(14)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Rapid 2 large curved IP'
_diffrn_measured_fraction_theta_full 0.9921
_diffrn_measured_fraction_theta_max 0.9827
_diffrn_measurement_device
;
Crystal Goniometer chi-partial 
;
_diffrn_measurement_device_type
;
Rigaku Spider Rapid2
;
_diffrn_measurement_specimen_support Fiber
_diffrn_radiation_monochromator  'Confocal CMF optics'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54187
_diffrn_reflns_av_R_equivalents  0.0774
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.9921
_diffrn_reflns_Laue_measured_fraction_max 0.9827
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16908
_diffrn_reflns_point_group_measured_fraction_full 0.9921
_diffrn_reflns_point_group_measured_fraction_max 0.9827
_diffrn_reflns_theta_full        67.6868
_diffrn_reflns_theta_max         72.10
_diffrn_reflns_theta_min         4.91
_diffrn_source                   'Rotating Anode mm007HF'
_diffrn_source_current           40.0
_diffrn_source_power             2.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    4.499
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Abscor (Higashi-Rigaku, 1995)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       tab
_exptl_crystal_F_000             752.0
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/pentane'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.4863
_refine_diff_density_min         -0.3072
_refine_diff_density_rms         0.0735
_refine_ls_d_res_high            0.8102
_refine_ls_d_res_low             9.0118
_refine_ls_goodness_of_fit_ref   1.0237
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     343
_refine_ls_number_reflns         3361
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0237
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0448
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0764P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1231
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              0
_reflns_number_gt                2634
_reflns_number_total             3361
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4nj01989j2.cif
_cod_data_source_block           HS443-P-HAR
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7063274.cif.
;
_cod_database_code               7063274
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
;
_olex2_submission_special_instructions 'No special instructions were received'