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_4032124
_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            'C17 H14 F N3'
_chemical_formula_weight         279.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 121.277(5)
_cell_angle_gamma                90
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_cell_length_b                   18.450(8)
_cell_length_c                   12.193(5)
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_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.224
_cell_measurement_theta_min      2.949
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_computing_cell_refinement       'Bruker SMART'
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_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_unetI/netI     0.0699
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            6903
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.978
_diffrn_reflns_theta_min         1.937
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       sheet
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
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_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0019(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.860
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3080
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.1113
_refine_ls_R_factor_gt           0.0614
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0956P)^2^] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1549
_refine_ls_wR_factor_ref         0.1717
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1573
_reflns_number_total             3080
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b02624_si_001.cif
_cod_data_source_block           a50915a
_cod_depositor_comments
'Adding full bibliography for 4032123--4032124.cif.'
_cod_database_code               4032124
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.993
_shelxl_version_number           2013-2
_shelx_res_checksum              68421
_shelx_hkl_checksum              74844