AlCl3-promoted selective Michael addition with allenoate and methyleneindolinone: synthesis of spirocyclic oxindole by using allenoate as a four-carbon component building block.
Xu, Shibo; Li, Chunju; Jia, Xueshun; Li, Jian; The Journal of organic chemistry 79 (2014) 11161–11169; doi:10.1021/jo502209f

data_4030127
_publ_section_title
;
 AlCl3-promoted selective Michael addition with allenoate and
 methyleneindolinone: synthesis of spirocyclic oxindole by using allenoate
 as a four-carbon component building block.
;
_journal_issue                   22
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              11161
_journal_page_last               11169
_journal_paper_doi               10.1021/jo502209f
_journal_volume                  79
_journal_year                    2014
_chemical_formula_sum            'C24 H21 Cl N2 O6'
_chemical_formula_weight         468.88
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                91.515(12)
_cell_angle_beta                 100.990(11)
_cell_angle_gamma                115.566(12)
_cell_formula_units_Z            2
_cell_length_a                   9.554(10)
_cell_length_b                   11.029(12)
_cell_length_c                   12.179(13)
_cell_measurement_reflns_used    2775
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.32
_cell_measurement_theta_min      2.38
_cell_volume                     1128(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
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_diffrn_reflns_limit_l_min       -14
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_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.213
_exptl_absorpt_correction_T_max  0.9832
_exptl_absorpt_correction_T_min  0.9388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             488
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_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.185
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_refine_ls_extinction_method     none
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_refine_ls_number_reflns         3888
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_refine_ls_R_factor_all          0.0576
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_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^)+(0.0624P)^2^+0.2993P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1358
_reflns_number_gt                3092
_reflns_number_total             3888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502209f_si_003.cif
_cod_data_source_block           140614a_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4030127--4030129.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4030127