Facile Synthesis of Halogenated Spiroketals via a Tandem Iodocyclization.
Wang, Jia; Zhu, Hai-Tao; Li, Ying-Xiu; Wang, Li-Jing; Qiu, Yi-Feng; Qiu, Zi-Hang; Zhong, Mei-Jin; Liu, Xue-Yuan; Liang, Yong-Min; Organic letters 16 (2014) 2236–2239; doi:10.1021/ol500741a

data_1514255
_publ_section_title
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 Facile Synthesis of Halogenated Spiroketals via a Tandem Iodocyclization.
;
_journal_issue                   8
_journal_name_full               'Organic letters'
_journal_page_first              2236
_journal_page_last               2239
_journal_paper_doi               10.1021/ol500741a
_journal_volume                  16
_journal_year                    2014
_chemical_formula_moiety         'C21 H17 I3 O3'
_chemical_formula_sum            'C21 H17 I3 O3'
_chemical_formula_weight         698.05
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_space_group_name_Hall           '-P 1'
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Olex2 1.2
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
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_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_diffrn_ambient_temperature      121.16(10)
_diffrn_detector_area_resol_mean 16.0733
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_diffrn_reflns_av_R_equivalents  0.0316
_diffrn_reflns_av_unetI/netI     0.0507
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_diffrn_source                   'SuperNova (Mo) X-ray Source'
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
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_exptl_crystal_colour            'clear light colourless'
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_refine_ls_extinction_coef       0.0163(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_structure_factor_coef Fsqd
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;
 w=1/[\s^2^(Fo^2^)+(0.0397P)^2^]
 where P=(Fo^2^+2Fc^2^)/3
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_refine_ls_weighting_scheme      calc
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_cod_depositor_comments
;Adding full bibliography for
 ./tmp-cod-update-bibliographies-8800/cifs/1514255.cif.
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_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C3(H3), C2(H2), C4(H4), C5(H5), C14(H14), C13(H13)
2.b Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C15(H15A,H15B,H15C)
;
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