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_7238719
_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_sum            'C15 H17 Cl N2 O3'
_chemical_formula_weight         308.76
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.717(2)
_cell_angle_beta                 95.368(2)
_cell_angle_gamma                111.818(2)
_cell_formula_units_Z            4
_cell_length_a                   11.3854(12)
_cell_length_b                   12.1629(13)
_cell_length_c                   12.6647(13)
_cell_measurement_temperature    296(2)
_cell_volume                     1593.7(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0517
_diffrn_reflns_av_sigmaI/netI    0.0563
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11566
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.250
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             648
_refine_diff_density_max         0.186
_refine_diff_density_min         -0.272
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     387
_refine_ls_number_reflns         7825
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0404P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                4594
_reflns_number_total             7825
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ra21549g.txt
_cod_data_source_block           20120328d_0m
_cod_database_code               7238719