Diels–Alder Cycloaddition and Ring-Closing Metathesis: A Versatile, Stereoselective, and General Route to Embellished Bridged Bicyclic Systems, Carbocyclic Framework of Secoatisanes, and Homologues
Singh, Vishwakarma; Sahu, Pramod K.; Sahu, Bharat C.; Mobin, Shaikh M.; Journal of Organic Chemistry 74 (2009) 6092–6104; doi:10.1021/jo901279g

data_4024788
_publ_section_title
;
 Diels--Alder Cycloaddition and Ring-Closing Metathesis:
 A Versatile, Stereoselective, and General Route to Embellished Bridged
 Bicyclic Systems, Carbocyclic Framework of Secoatisanes, and Homologues
;
_journal_coden_ASTM              JOCEAH
_journal_issue                   16
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6092
_journal_page_last               6104
_journal_paper_doi               10.1021/jo901279g
_journal_volume                  74
_journal_year                    2009
_chemical_formula_sum            'C20 H20 O4'
_chemical_formula_weight         324.36
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.92(2)
_cell_angle_beta                 94.53(2)
_cell_angle_gamma                116.86(3)
_cell_formula_units_Z            2
_cell_length_a                   8.663(2)
_cell_length_b                   9.548(3)
_cell_length_c                   10.915(3)
_cell_measurement_reflns_used    3172
_cell_measurement_temperature    150(2)
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_cell_measurement_theta_min      3.0797
_cell_volume                     801.5(4)
_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    Ortep3
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'OXFORD DIFFRACTION XCALIBUR-S'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
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_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0144
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_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6636
_diffrn_reflns_theta_full        25.00
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_diffrn_reflns_theta_min         3.09
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.9789
_exptl_absorpt_correction_T_min  0.9700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.344
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             344
_exptl_crystal_size_max          0.33
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_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.215
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_refine_ls_number_parameters     217
_refine_ls_number_reflns         2818
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0319
_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^)+(0.0441P)^2^+0.1161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0823
_refine_ls_wR_factor_ref         0.0846
_reflns_number_gt                2305
_reflns_number_total             2818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo901279g_si_002.cif
_cod_data_source_block           vks020
_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 
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_cod_database_code               4024788