Metal-free sequential decarbonylative annulation of N-cyanamides for the construction of 2,3-dihydropyrrolo[2,1-b]quinazolin-9(1H)-ones
Liu, Xueke; Qian, Ping; Wang, Yi; Pan, Yi; Organic Chemistry Frontiers 4 (2017) 2370–; doi:10.1039/C7QO00677B

data_1553868
_publ_section_title
;
 Metal-free sequential decarbonylative annulation of N-cyanamides for the
 construction of 2,3-dihydropyrrolo[2,1-b]quinazolin-9(1H)-ones
;
_journal_issue                   12
_journal_name_full               'Organic Chemistry Frontiers'
_journal_page_first              2370
_journal_paper_doi               10.1039/C7QO00677B
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C17 H22 N2 O2'
_chemical_formula_weight         286.36
_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-2014/7
_audit_update_record
;
2017-05-27 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.163(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.0777(7)
_cell_length_b                   22.245(3)
_cell_length_c                   11.8606(15)
_cell_measurement_reflns_used    1613
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.81
_cell_measurement_theta_min      2.52
_cell_volume                     1594.3(3)
_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-2014 (Sheldrick 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8866
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.006
_diffrn_reflns_theta_max         25.006
_diffrn_reflns_theta_min         1.831
_exptl_absorpt_coefficient_mu    0.079
_exptl_crystal_density_diffrn    1.193
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.831
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         2802
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0778
_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^)+(0.1525P)^2^+0.8837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2365
_refine_ls_wR_factor_ref         0.2740
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1766
_reflns_number_total             2802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7qo00677b2.cif
_cod_data_source_block           20170522PY_liuxueke_0m_a
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1553868
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.983
_shelx_res_checksum              12561
_shelx_hkl_checksum              97997