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_7151588
_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            'C11 H16 O2'
_chemical_formula_weight         180.27
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.000
_cell_angle_beta                 102.880(5)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   7.0166(3)
_cell_length_b                   10.5703(6)
_cell_length_c                   13.7222(13)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293
_cell_measurement_theta_max      45.08
_cell_measurement_theta_min      38.91
_cell_volume                     992.13(12)
_computing_cell_refinement       'local program'
_computing_data_collection       'Enraf-Nonius CAD-4 software'
_computing_data_reduction        'xtal ADDREF'
_computing_molecular_graphics    PLATON
_computing_publication_material  'xtal BONDLA CIFIO PLATON'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    CRUNCH
_diffrn_ambient_temperature      293
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_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       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2030
_diffrn_reflns_reduction_process 'perpendicular monochr Lp'
_diffrn_reflns_theta_max         74.86
_diffrn_reflns_theta_min         5.33
_diffrn_standards_decay_%        8
_diffrn_standards_interval_time  60
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    .648
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             392
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.20
_refine_diff_density_max         .321
_refine_diff_density_min         -.293
_refine_ls_extinction_coef       1931(183)
_refine_ls_extinction_expression 'Eq22 p292 "Cryst. Comp." Munksgaard 1970'
_refine_ls_extinction_method     Zachariasen
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_ref   1.09
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     183
_refine_ls_number_reflns         1743
_refine_ls_number_restraints     16
_refine_ls_R_factor_all          .078
_refine_ls_R_factor_gt           .071
_refine_ls_shift/su_max          .038
_refine_ls_shift/su_mean         .002
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     '1/[0.4 + 0.1(\s(Fobs))^2^ + 0.1/(\s(Fobs))]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .066
_refine_ls_wR_factor_ref         .064
_reflns_d_resolution_high        .799
_reflns_d_resolution_low         8.294
_reflns_limit_h_max              8
_reflns_limit_h_min              -8
_reflns_limit_k_max              13
_reflns_limit_k_min              0
_reflns_limit_l_max              17
_reflns_limit_l_min              0
_reflns_number_gt                1743
_reflns_number_total             2030
_reflns_threshold_expression     'Iobs > 2.50 sig(Iobs)'
_cod_data_source_file            b311415e.txt
_cod_data_source_block           Compound_17
_cod_depositor_comments
;
 Changing the _atom_site_occupancy data item value from '?' to '1'
 for all fully occupied atom sites.

 Antanas Vaitkus,
 2017-02-09
;
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_database_code               7151588