Ag-Assisted Fluorination of Unprotected 4,6-Disubstituted 2-Aminopyrimidines with Selectfluor.
Wang, Chenxi; Cai, Juewang; Zhang, Min; Zhao, Xiaoming; The Journal of organic chemistry 82 (2017) 1260–1265; doi:10.1021/acs.joc.6b02624

data_4032123
_publ_section_title
;
 Ag-Assisted Fluorination of Unprotected 4,6-Disubstituted
 2-Aminopyrimidines with Selectfluor.
;
_journal_issue                   2
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              1260
_journal_page_last               1265
_journal_paper_doi               10.1021/acs.joc.6b02624
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C12 H8 F N3 S2'
_chemical_formula_weight         277.33
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_hydrogens   mixed
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_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.3403(16)
_cell_length_b                   5.1091(6)
_cell_length_c                   18.453(2)
_cell_measurement_reflns_used    5177
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      3.25
_cell_volume                     1182.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
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_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-III CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       17
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_diffrn_reflns_limit_k_max       6
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_diffrn_reflns_limit_l_min       -23
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_diffrn_reflns_point_group_measured_fraction_full 0.999
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_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.558
_exptl_crystal_description       block
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.6788
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.323
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_refine_ls_extinction_coef       0.0015(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2733
_refine_ls_number_restraints     189
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0511
_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^)+(0.0536P)^2^+0.6090P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1242
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1879
_reflns_number_total             2733
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02624_si_002.cif
_cod_data_source_block           mo_160420c
_cod_depositor_comments
'Adding full bibliography for 4032123--4032124.cif.'
_cod_database_code               4032123
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.936
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              58165
_shelx_hkl_checksum              13867