Merging catalyst-free synthesis and iodine catalysis: one-pot synthesis of dihydrofuropyrimidines and spirodihydrofuropyrimidine pyrazolones
Zheng, Ya-Yun; Feng, Kai-Xiang; Xia, Ai-Bao; Liu, Jie; Tang, Cheng-Ke; Zhou, Zhan-Yu; Xu, Dan-Qian; RSC Advances 9 (2019) 9770–; doi:10.1039/C9RA01665A

data_7232547
_publ_section_title
;
 Merging catalyst-free synthesis and iodine catalysis: one-pot synthesis
 of dihydrofuropyrimidines and spirodihydrofuropyrimidine pyrazolones
;
_journal_issue                   17
_journal_name_full               'RSC Advances'
_journal_page_first              9770
_journal_paper_doi               10.1039/C9RA01665A
_journal_volume                  9
_journal_year                    2019
_chemical_formula_sum            'C15 H17 N5 O4'
_chemical_formula_weight         331.33
_chemical_name_systematic
; 
 ? 
;
_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_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc21kkry
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2019-01-26 deposited with the CCDC.    2019-03-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.350(12)
_cell_angle_gamma                90
_cell_formula_units_Z            8
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_cell_length_b                   7.7110(10)
_cell_length_c                   19.479(3)
_cell_measurement_reflns_used    3316
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      106.778
_cell_measurement_theta_min      6.763
_cell_volume                     3416.8(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.1568
_diffrn_reflns_av_unetI/netI     0.1773
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29886
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         54.988
_diffrn_reflns_theta_min         3.381
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_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4427
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
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_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1392
_exptl_crystal_size_max          0.100
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_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.775
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.109
_refine_ls_extinction_coef       0.0045(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         6485
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.2324
_refine_ls_R_factor_gt           0.1288
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3391
_refine_ls_wR_factor_ref         0.4207
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2598
_reflns_number_total             6485
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra01665a2.cif
_cod_data_source_block           wmj18081_0m
_cod_database_code               7232547
_shelx_estimated_absorpt_t_min   0.951
_shelx_estimated_absorpt_t_max   0.970
_shelxl_version_number           2013-4
_shelx_res_checksum              34413