Ruthenium-Catalyzed Synthesis of Fused Tricyclic 1H-2,3-Dihydropyrimido[1,2-a]quinolines in One Step.
Wang, Xingyong; Liu, Chulong; Zeng, Xiaobao; Wang, Xuesong; Wang, Xinyan; Hu, Yuefei; Organic letters 19 (2017) 3378–3381; doi:10.1021/acs.orglett.7b01330

data_1556054
_publ_section_title
;
 Ruthenium-Catalyzed Synthesis of Fused Tricyclic
 1H-2,3-Dihydropyrimido[1,2-a]quinolines in One Step.
;
_journal_issue                   13
_journal_name_full               'Organic letters'
_journal_page_first              3378
_journal_page_last               3381
_journal_paper_doi               10.1021/acs.orglett.7b01330
_journal_volume                  19
_journal_year                    2017
_chemical_formula_sum            'C19 H18 N2 O2 S'
_chemical_formula_weight         338.41
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 93.229(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.8427(8)
_cell_length_b                   22.614(2)
_cell_length_c                   18.528(2)
_cell_measurement_reflns_used    2998
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      46.703
_cell_measurement_theta_min      4.758
_cell_volume                     3280.8(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0439
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            18744
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_min         1.801
_exptl_absorpt_coefficient_mu    0.211
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.365
_refine_diff_density_min         -0.199
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         6107
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0507
_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^)+(0.0744P)^2^+0.0659P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1264
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4059
_reflns_number_total             6107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol7b01330_si_002.cif
_cod_data_source_block           cd16011
_cod_depositor_comments
;

2022-11-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C38 H36 N4 O4 S2'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     676.83
_cod_database_code               1556054
_shelx_estimated_absorpt_t_min   0.957
_shelx_estimated_absorpt_t_max   0.973
_shelxl_version_number           2013-4
_shelx_res_checksum              10950
_shelx_hkl_checksum              29585