Progress toward the synthesis of the basiliolides and transtaganolides: an intramolecular pyrone Diels-Alder entry into a novel class of natural products.
Nelson, Hosea M.; Stoltz, Brian M.; Organic letters 10 (2008) 25–28; doi:10.1021/ol702501s

data_1504474
_publ_section_title
;
 Progress toward the synthesis of the basiliolides and transtaganolides:
 an intramolecular pyrone Diels-Alder entry into a novel class of natural
 products.
;
_journal_issue                   1
_journal_name_full               'Organic letters'
_journal_page_first              25
_journal_page_last               28
_journal_paper_doi               10.1021/ol702501s
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety         'C18 H21 Br O8'
_chemical_formula_sum            'C18 H21 Br O8'
_chemical_formula_weight         445.26
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.003(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.6117(3)
_cell_length_b                   19.4403(16)
_cell_length_c                   14.6195(13)
_cell_measurement_reflns_used    4422
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.90
_cell_measurement_theta_min      2.50
_cell_volume                     1844.6(2)
_computing_cell_refinement       'Bruker SAINT v6.45A'
_computing_data_collection       'Bruker SMART v5.630'
_computing_data_reduction        'Bruker SAINT v6.45A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF v6.12'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.891
_diffrn_measured_fraction_theta_max 0.891
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       '\w scans at 5 \f settings'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1081
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            11273
_diffrn_reflns_theta_full        33.90
_diffrn_reflns_theta_max         33.90
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    2.273
_exptl_absorpt_correction_T_max  0.7466
_exptl_absorpt_correction_T_min  0.5283
_exptl_absorpt_correction_type   TWINABS
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Fragment
_exptl_crystal_F_000             912
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.261
_refine_diff_density_min         -0.700
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_refine_ls_number_reflns         11273
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_refine_ls_restrained_S_all      1.437
_refine_ls_R_factor_all          0.1128
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/s^2^(Fo^2^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1245
_reflns_number_gt                7706
_reflns_number_total             11273
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol702501s-file002.cif
_cod_data_source_block           hmn01
_cod_depositor_comments
;
The following automatic conversions were performed:

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

'_refine_ls_weighting_scheme' value 'Sigma' changed to
'sigma' 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 

The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'Direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1504474