Tandem 1,5-migration/Michael reactions to prepare adducts of pyrazolone derivatives: protecting group-directed rearrangement
Lu, Zhijin; Xie, Chen; Han, Jianlin; Pan, Yi; RSC Advances 2 (2012) 8949–; doi:10.1039/c2ra21549g

data_7238718
_publ_section_title
;
 Tandem 1,5-migration/Michael reactions to prepare adducts of pyrazolone
 derivatives: protecting group-directed rearrangement
;
_journal_issue                   24
_journal_name_full               'RSC Advances'
_journal_page_first              8949
_journal_paper_doi               10.1039/c2ra21549g
_journal_volume                  2
_journal_year                    2012
_chemical_formula_moiety         'C23 H24 Cl N3 O5'
_chemical_formula_sum            'C23 H24 Cl N3 O5'
_chemical_formula_weight         457.90
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.254(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3812(14)
_cell_length_b                   19.472(3)
_cell_length_c                   13.1900(19)
_cell_measurement_temperature    273(2)
_cell_volume                     2313.1(6)
_computing_cell_refinement       'Bruker SHELXTL Program'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        Saint
_computing_molecular_graphics    'Bruker SHELXTL Program'
_computing_publication_material  'Bruker SHELXTL Program'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Apex II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0982
_diffrn_reflns_av_sigmaI/netI    0.0718
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15963
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.92
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_correction_T_min  0.943
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960.0
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     293
_refine_ls_number_reflns         5737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1102P)^2^+0.0189P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.1876
_reflns_number_gt                4202
_reflns_number_total             5737
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra21549g.txt
_cod_data_source_block           2011122m
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7238718