Synthesis of the cyclobutanone core of solanoeclepin A intramolecular allene butenolide photocycloaddition.
Hue, Bui T. B.; Dijkink, Jan; Kuiper, Sanne; Larson, Kimberly K.; Guziec, Jr, Frank S; Goubitz, Kees; Fraanje, Jan; Schenk, Henk; van Maarseveen, Jan H.; Hiemstra, Henk; Organic & biomolecular chemistry 1 (2003) 4364–4366; doi:10.1039/b311415e

data_7151587
_publ_section_title
;
 Synthesis of the cyclobutanone core of solanoeclepin A intramolecular
 allene butenolide photocycloaddition.
;
_journal_issue                   24
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              4364
_journal_page_last               4366
_journal_paper_doi               10.1039/b311415e
_journal_volume                  1
_journal_year                    2003
_chemical_formula_sum            'C12 H14 O2'
_chemical_formula_weight         190.24
_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                77.964(6)
_cell_angle_beta                 75.679(9)
_cell_angle_gamma                80.977(8)
_cell_formula_units_Z            2
_cell_length_a                   6.6969(4)
_cell_length_b                   7.0489(6)
_cell_length_c                   10.9328(7)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293
_cell_measurement_theta_max      42.88
_cell_measurement_theta_min      40.43
_cell_volume                     486.04(6)
_computing_cell_refinement       'local program'
_computing_data_collection       'Enraf-Nonius CAD4 software'
_computing_data_reduction        'xtal ADDREF'
_computing_molecular_graphics    PLATON
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    CRUNCH
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_reduction_process 'perpendicular monochr Lp'
_diffrn_reflns_theta_max         74.73
_diffrn_reflns_theta_min         4.24
_diffrn_standards_decay_%        13
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .698
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.3
_exptl_crystal_F_000             204
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .352
_refine_diff_density_min         -.345
_refine_ls_extinction_coef       1470(151)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   .989
_refine_ls_goodness_of_fit_ref   .996
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     184
_refine_ls_number_reflns         1806
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          .085
_refine_ls_R_factor_gt           .079
_refine_ls_shift/su_max          .135
_refine_ls_shift/su_mean         .01
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'1/[0.6 + 0.01*(\s(Fobs)^2^) + 0.01/(\s(Fobs))]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .104
_refine_ls_wR_factor_ref         .099
_reflns_d_resolution_high        .799
_reflns_d_resolution_low         10.425
_reflns_limit_h_max              8
_reflns_limit_h_min              -7
_reflns_limit_k_max              8
_reflns_limit_k_min              -8
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                1806
_reflns_number_total             1999
_reflns_threshold_expression     'Iobs > 2.50 sig(Iobs)'
_cod_data_source_file            b311415e.txt
_cod_data_source_block           Compound_12
_cod_original_sg_symbol_Hall     -p_1
_cod_original_sg_symbol_H-M      P_-1
_cod_database_code               7151587