DABCO-catalyzed unusual [4 + 2] cycloaddition reaction: non-substituted allenoate acts as a four-carbon synthon and facile synthesis of spirooxindoles.
Liu, Yufen; Du, Yanlong; Yu, Aimin; Mu, Haifeng; Meng, Xiangtai; Organic & biomolecular chemistry 14 (2016) 1226–1230; doi:10.1039/c5ob02383a

data_7154851
_publ_section_title
;
 DABCO-catalyzed unusual [4 + 2] cycloaddition reaction: non-substituted
 allenoate acts as a four-carbon synthon and facile synthesis of
 spirooxindoles.
;
_journal_issue                   4
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              1226
_journal_page_last               1230
_journal_paper_doi               10.1039/c5ob02383a
_journal_volume                  14
_journal_year                    2016
_chemical_formula_sum            'C21 H23 N O6'
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_symmetry_space_group_name_Hall  '-P 1'
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_atom_sites_solution_secondary   difmap
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_audit_update_record
;
2015-08-11 deposited with the CCDC.
2015-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                95.1770(10)
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_cell_angle_gamma                94.5590(10)
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_cell_length_c                   18.4533(11)
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_cell_measurement_temperature    173(2)
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_cell_volume                     1992.9(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  '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
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_diffrn_reflns_limit_l_min       -21
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_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.9860
_exptl_absorpt_correction_T_min  0.9832
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.285
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       BLOCK
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_reflns         7003
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0579
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0364P)^2^+0.8978P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0892
_refine_ls_wR_factor_ref         0.0982
_reflns_number_gt                5466
_reflns_number_total             7003
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ob02383a2.cif
_cod_data_source_block           n141127b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_exptl_crystal_density_meas' value 'NONE' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 

 Adding full bibliography for 7154849--7154851.cif.
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7154851