Decarboxylative Claisen rearrangement reactions: synthesis and reactivity of alkylidene-substituted indolines.
Camp, Jason E.; Craig, Donald; Funai, Kiyohiko; White, Andrew J. P.; Organic & biomolecular chemistry 9 (2011) 7904–7912; doi:10.1039/c1ob06212c

data_7152063
_publ_section_title
;
 Decarboxylative Claisen rearrangement reactions: synthesis and reactivity
 of alkylidene-substituted indolines.
;
_journal_issue                   22
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              7904
_journal_page_last               7912
_journal_paper_doi               10.1039/c1ob06212c
_journal_volume                  9
_journal_year                    2011
_chemical_formula_moiety         'C25 H25 N O4 S2, 0.10H2O'
_chemical_formula_sum            'C25 H25.2 N O4.1 S2'
_chemical_formula_weight         469.38
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
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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                79.253(3)
_cell_angle_beta                 76.645(3)
_cell_angle_gamma                86.290(3)
_cell_formula_units_Z            2
_cell_length_a                   9.1743(3)
_cell_length_b                   9.9834(4)
_cell_length_c                   13.0708(4)
_cell_measurement_reflns_used    4194
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.9598
_cell_measurement_theta_min      3.0451
_cell_volume                     1144.07(7)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd'
_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_detector_area_resol_mean 15.9832
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'OD Xcalibur 3'
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_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0462
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            8098
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         29.02
_diffrn_reflns_theta_min         3.05
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.266
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.925
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.41 (release 06-05-2009 CrysAlis171 .NET)
(compiled May 6 2009,17:20:42)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'Pale yellow'
_exptl_crystal_density_diffrn    1.363
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             494
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.477
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
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_refine_ls_number_parameters     295
_refine_ls_number_reflns         5098
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.988
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0392
_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^)+(0.0577P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1024
_reflns_number_gt                3652
_reflns_number_total             5098
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ob06212c.txt
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1144.06(7)
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C25 H25.20 N O4.10 S2'
_cod_database_code               7152063