Sequential five-component synthesis of spiropyrrolidinochromanones.
Marcaccini, Stefano; Neo, Ana G.; Marcos, Carlos F.; The Journal of organic chemistry 74 (2009) 6888–6890; doi:10.1021/jo900992w

data_4029503
_publ_section_title
;
 Sequential five-component synthesis of spiropyrrolidinochromanones.
;
_journal_issue                   17
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              6888
_journal_page_last               6890
_journal_paper_doi               10.1021/jo900992w
_journal_volume                  74
_journal_year                    2009
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C39 H39 N3 O5'
_chemical_formula_sum            'C39 H39 N3 O5'
_chemical_formula_weight         629.73
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2009-06-24T11:04:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5472(14)
_cell_length_b                   11.8178(15)
_cell_length_c                   23.6812(30)
_cell_measurement_reflns_used    5756
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.43
_cell_measurement_wavelength     0.71073
_cell_volume                     3231.6(7)
_computing_cell_refinement       'APEX2 v2009-3.0 (BRUKER AXS, Madison, 2009)'
_computing_data_collection       'APEX2 v2009-3.0 (BRUKER AXS, Madison, 2009)'
_computing_data_reduction        'APEX2 v2009-3.0 (BRUKER AXS, Madison, 2009)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1998)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART1000 CCD'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.042
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            38817
_diffrn_reflns_theta_full        27.21
_diffrn_reflns_theta_max         27.21
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.9862
_exptl_absorpt_correction_T_min  0.8307
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'BRUKER AXS - SADABS'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.294
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1336
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.245
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0032(4)
_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   1.14
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         4029
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.14
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0245P)^2^+2.4725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                2935
_reflns_number_total             4029
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            jo900992w_si_002.cif
_cod_data_source_block           ml01zl1n
_cod_database_code               4029503