TiCl<sub>4</sub>-n-Bu<sub>3</sub>N-mediated cascade annulation of ketones with α-ketoesters: a facile synthesis of highly substituted fused γ-alkylidene-butenolides.
Palange, Megha N.; Gonnade, Rajesh G.; Kontham, Ravindar; Organic & biomolecular chemistry 17 (2019) 5749–5759; doi:10.1039/c9ob00649d

data_7156862
_publ_section_title
;
 TiCl<sub>4</sub>-n-Bu<sub>3</sub>N-mediated cascade annulation of ketones
 with \a-ketoesters: a facile synthesis of highly substituted fused
 \g-alkylidene-butenolides.
;
_journal_issue                   23
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              5749
_journal_page_last               5759
_journal_paper_doi               10.1039/c9ob00649d
_journal_volume                  17
_journal_year                    2019
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_chemical_formula_moiety         'C21 H22 O4 S'
_chemical_formula_sum            'C21 H22 O4 S'
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_audit_update_record
;
2018-12-13 deposited with the CCDC.    2019-05-16 downloaded from the CCDC.
;
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_computing_molecular_graphics    'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Photon II CPAD Area Detector'
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_diffrn_source                   'micro-focus sealed tube'
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_refine_diff_density_min         -0.237
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_refine_ls_abs_structure_details
;
 Flack x determined using 2148 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.00(2)
_refine_ls_extinction_method     none
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_refine_ls_R_factor_all          0.0357
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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
'w=1/[\s^2^(Fo^2^)+(0.0510P)^2^+0.1914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0818
_refine_ls_wR_factor_ref         0.0873
_reflns_Friedel_coverage         0.769
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_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5115
_reflns_number_total             5451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ob00649d2.cif
_cod_data_source_block           mo_MEGA1_0m_a_pl
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_absolute_configuration' value 'RMAD' changed to 'rmad'
according to
/home/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
/home/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.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7156862--7156864.cif.
;
_cod_database_code               7156862
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