One-pot, multicomponent route to pyrazoloquinolizinones.
Chebanov, Valentin A.; Saraev, Vyacheslav E.; Desenko, Sergey M.; Chernenko, Vitaliy N.; Shishkina, Svetlana V.; Shishkin, Oleg V.; Kobzar, Kiril M.; Kappe, C. Oliver; Organic letters 9 (2007) 1691–1694; doi:10.1021/ol070411l

data_1505363
_publ_section_title
;
 One-pot, multicomponent route to pyrazoloquinolizinones.
;
_journal_issue                   9
_journal_name_full               'Organic letters'
_journal_page_first              1691
_journal_page_last               1694
_journal_paper_doi               10.1021/ol070411l
_journal_volume                  9
_journal_year                    2007
_chemical_formula_moiety         'C24 H24 Br N3 O2, 0.25(C4 H10 O)'
_chemical_formula_sum            'C25 H26.5 Br N3 O2.25'
_chemical_formula_weight         484.90
_chemical_name_systematic
; 
 4-(4-Bromo-phenyl)-5a-hydroxy-7,7-dimethyl-3-phenyl-4,5,5a,6,7,8-hexahydro-
1H-1,2,9a-triaza-cyclopenta[a]naphthalen-9-one
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 132.682(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            16
_cell_length_a                   36.322(5)
_cell_length_b                   13.144(5)
_cell_length_c                   25.296(5)
_cell_measurement_reflns_used    15683
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      8
_cell_volume                     8878(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.27p5 beta (release 01-04-2005 CrysAlis171 .NET)
(compiled Apr  1 2005,17:53:34)
;
_computing_molecular_graphics    'XP (Siemens, 1998)'
_computing_publication_material  'SHELXTL (Sheldrick, 1998)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 1998)'
_computing_structure_solution    'SHELXTL (Sheldrick, 1998)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Xcalibur"3
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_sigmaI/netI    0.0778
_diffrn_reflns_limit_h_max       51
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            32926
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         3.17
_diffrn_standards_interval_count 50
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.881
_exptl_absorpt_correction_T_max  0.8342
_exptl_absorpt_correction_T_min  0.7048
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.451
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4008
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.578
_refine_diff_density_min         -1.313
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     571
_refine_ls_number_reflns         12864
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.1065
_refine_ls_R_factor_gt           0.0656
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1066P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1924
_reflns_number_gt                7385
_reflns_number_total             12864
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol070411lsi20070219_052209.cif
_cod_data_source_block           experimental
_cod_depositor_comments
;

2019-05-05
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_moiety     '4(C24 H24 Br N3 O2), C4 H10 O'
_cod_original_formula_sum        'C100 H106 Br4 N12 O9'
_cod_original_formula_units_Z    4
_cod_original_formula_weight     1939.61
_cod_database_code               1505363