Configurations of Cycloadducts Formed in Asymmetric Intramolecular Diels–Alder Reactions
Breu, J.; Butz, T.; Range, K.-J.; Sauer, J.; Acta Crystallographica Section C 53 (1997) 515–517; doi:10.1107/S010827019601579X

data_2006041
_publ_section_title
;
 Configurations of Cycloadducts Formed in Asymmetric Intramolecular
 Diels--Alder Reactions
;
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              515
_journal_page_last               517
_journal_paper_doi               10.1107/S010827019601579X
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C14 H18 O5'
_chemical_formula_weight         266.29
_chemical_name_systematic
;
(3S,3aS,6R,7R,7aR)-Menthyl-1,6,7,7a-tetrahydro-3-(1,1-dimethylethyl)-1-oxo-
3H-3a,6-epoxyisobenzofuran-7-carboxylate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                79.235(8)
_cell_angle_beta                 88.902(10)
_cell_angle_gamma                75.125(9)
_cell_formula_units_Z            2
_cell_length_a                   7.7300(10)
_cell_length_b                   9.4267(10)
_cell_length_c                   9.9854(10)
_cell_measurement_reflns_used    '1736 with I/\s(I) > 12'
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.69
_cell_measurement_theta_min      2.28
_cell_volume                     690.54(14)
_computing_cell_refinement       'CELL (Stoe & Cie, 1996)'
_computing_data_collection       'EXPOSE (Stoe & Cie, 1996)'
_computing_data_reduction        'INTEGRATE (Stoe & Cie, 1996)'
_computing_molecular_graphics    'PLATON (Spek, 1990)'
_computing_publication_material  'PLATON, SHELXL93'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'STOE IPDS'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
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_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_sigmaI/netI    0.0283
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4199
_diffrn_reflns_reduction_process
;
 ?
;
_diffrn_reflns_theta_max         24.69
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.10
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_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.15
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_refine_diff_density_min         -0.13
_refine_ls_extinction_method     none
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_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_hydrogen_treatment    'H atoms riding'
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_refine_ls_number_reflns         2159
_refine_ls_number_restraints     0
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_refine_ls_restrained_S_obs      1.123
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_refine_ls_R_factor_obs          0.0402
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef F^2^
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.0961P]  where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1175
_refine_ls_wR_factor_obs         0.1130
_reflns_number_observed          1792
_reflns_number_total             2159
_reflns_observed_criterion       I>2\s(I)
_cod_data_source_file            bm1116.cif
_cod_data_source_block           V
_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_enum 1527 2010-12-29 10:47:43Z saulius 

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 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.0961P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0653P)^2^+0.0961P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        ' C14 H18 O5'
_cod_database_code               2006041