A captured room temperature stable Wheland intermediate as a key structure for the orthogonal decoration of 4-amino-pyrido[2,3-<i>d</i>]pyrimidin-7(8<i>H</i>)-ones.
Galve, Iñaki; Ondoño, Raül; de Rocafiguera, Claudi; Puig de la Bellacasa, Raimon; Batllori, Xavier; Puigjaner, Cristina; Font-Bardia, Mercè; Vallcorba, Oriol; Teixidó, Jordi; Borrell, José I; Organic & biomolecular chemistry 18 (2020) 9810–9815; doi:10.1039/d0ob01785j

data_7157715
_publ_section_title
;
 A captured room temperature stable Wheland intermediate as a key
 structure for the orthogonal decoration of
 4-amino-pyrido[2,3-<i>d</i>]pyrimidin-7(8<i>H</i>)-ones.
;
_journal_issue                   48
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              9810
_journal_page_last               9815
_journal_paper_doi               10.1039/d0ob01785j
_journal_volume                  18
_journal_year                    2020
_chemical_formula_moiety         'C13 H9 Br2 N5 O, C3 H6 O'
_chemical_formula_sum            'C16 H15 Br2 N5 O2'
_chemical_formula_weight         469.15
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-04-30 deposited with the CCDC.	2020-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.53
_cell_measurement_theta_min      2.94
_cell_volume                     1698.04(9)
_computing_cell_refinement       'Bruker SAINT'
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_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0429
_diffrn_reflns_av_unetI/netI     0.0256
_diffrn_reflns_Laue_measured_fraction_full 0.998
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_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
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_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            41290
_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_min         2.209
_diffrn_source                   microfocus
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_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5514
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_exptl_absorpt_process_details
'SADABS--2016/2 -- Bruker AXS area detector scaling and absorption correction'
_exptl_crystal_colour            yellow
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_exptl_crystal_description       prism
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_exptl_crystal_size_min          0.066
_refine_diff_density_max         1.780
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         5209
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0561
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+14.7200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1550
_refine_ls_wR_factor_ref         0.1626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4434
_reflns_number_total             5209
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ob01785j2.cif
_cod_data_source_block           mo_023VB5A_0m_a
_cod_depositor_comments          'Adding full bibliography for 7157715.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7157715
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              58748