Regenerative γ-Lactone Annulations: A Modular, Iterative Approach to Oligo-tetrahydrofuran Molecular Stairs and Related Frameworks.
Rashid, Showkat; Bhat, Bilal A.; Mehta, Goverdhan; Organic letters 17 (2015) 3604–3607; doi:10.1021/acs.orglett.5b01707

data_1555106
_publ_section_title
;
 Regenerative \g-Lactone Annulations: A Modular, Iterative Approach to
 Oligo-tetrahydrofuran Molecular Stairs and Related Frameworks.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3604
_journal_page_last               3607
_journal_paper_doi               10.1021/acs.orglett.5b01707
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_compound_source        'see text'
_chemical_formula_iupac          'C12 H14 O6'
_chemical_formula_moiety         'C12 H14 O6'
_chemical_formula_structural     'C12 H14 O6'
_chemical_formula_sum            'C12 H14 O6'
_chemical_formula_weight         254.23
_chemical_name_systematic
;
(1S,2S,3R,7R,9S,11R,13S,17R)-6,8,10,12,14-
pentaoxapentacyclo[9.6.0.0^2,9^.0^3,7^.0^13,17^]heptadecan-5-one
;
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
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_symmetry_space_group_name_Hall  'F 2 -2d'
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_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   37.2102(15)
_cell_length_b                   18.0600(5)
_cell_length_c                   6.8155(3)
_cell_measurement_reflns_used    3364
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      71.4070
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_computing_cell_refinement
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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'PLATON (Spek, 2003) and CAMERON (Watkin et al., 1993)'
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_diffrn_ambient_temperature      291(2)
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;
  1 omega   31.00   57.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   57.0000 -120.0000 26

  2 omega  -83.00   12.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  111.0000  -60.0000 95

  3 omega  -32.00   30.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   25.0000 -120.0000 62

  4 omega  -50.00  -24.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   50.0000  -60.0000 26

  5 omega -109.00  -54.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  -77.0000  -60.0000 55

  6 omega  -12.00   29.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000   37.0000   90.0000 41

  7 omega  -89.00  -36.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -      -42.5000  125.0000  150.0000 53

  8 omega  -14.00   73.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       54.8467  -77.0000   30.0000 87

  9 omega   34.00  108.00   1.0000   12.0000
omega____ theta____ kappa____ phi______ frames
    -       54.8467   57.0000  150.0000 74

 10 omega   37.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -37.0000 -120.0000 30

 11 omega   45.00   93.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -25.0000   90.0000 48

 12 omega   51.00   87.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -25.0000  -30.0000 36

 13 omega   39.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -37.0000  -60.0000 53

 14 omega   44.00   92.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -37.0000  150.0000 48

 15 omega   48.00   75.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -37.0000   30.0000 27

 16 omega   86.00  113.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934 -111.0000 -120.0000 27

 17 omega   59.00  111.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934 -111.0000   30.0000 52

 18 omega  102.00  175.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  111.0000 -150.0000 73

 19 omega  102.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  111.0000    0.0000 25

 20 omega   78.00  171.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934   25.0000    0.0000 93

 21 omega   42.00  140.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -77.0000  150.0000 98

 22 omega   37.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934 -111.0000  150.0000 68

 23 omega   60.00   86.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -37.0000   60.0000 26

 24 omega   75.00  103.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -50.0000 -120.0000 28

 25 omega   88.00  177.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934   50.0000  -90.0000 89

 26 omega   41.00  143.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      109.6934  -91.0000  -60.0000 102

;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0364145000
_diffrn_orient_matrix_UB_12      -0.0129364000
_diffrn_orient_matrix_UB_13      -0.1019757000
_diffrn_orient_matrix_UB_21      -0.0182670000
_diffrn_orient_matrix_UB_22      0.0081725000
_diffrn_orient_matrix_UB_23      -0.2016780000
_diffrn_orient_matrix_UB_31      0.0073973000
_diffrn_orient_matrix_UB_32      0.0839134000
_diffrn_orient_matrix_UB_33      0.0039067000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0192
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            6740
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        66.57
_diffrn_reflns_theta_max         66.57
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_exptl_absorpt_coefficient_mu    1.017
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79589
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.168
_refine_diff_density_rms         0.032
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_coef       0.00037(4)
_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   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2005
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0414
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0468P)^2^+5.6093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1035
_reflns_number_gt                1897
_reflns_number_total             2005
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ol5b01707_si_002.cif
_cod_data_source_block           compound_20
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Orthorhombic' was changed
to 'orthorhombic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
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_cod_database_code               1555106