Intramolecular Diels-Alder Reactions of Tethered Enoate Substituted Furans Induced by Dialkylaluminum Chloride.
Riedel, Sibylle; Maichle-Mössmer, Cäcilia; Maier, Martin E.; The Journal of organic chemistry 82 (2017) 12798–12805; doi:10.1021/acs.joc.7b02117

data_4033137
_publ_section_title
;
 Intramolecular Diels-Alder Reactions of Tethered Enoate Substituted
 Furans Induced by Dialkylaluminum Chloride.
;
_journal_issue                   23
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              12798
_journal_page_last               12805
_journal_paper_doi               10.1021/acs.joc.7b02117
_journal_volume                  82
_journal_year                    2017
_chemical_absolute_configuration unk
_chemical_formula_sum            'C13 H20 O3'
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_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
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_cell_angle_beta                 90
_cell_angle_gamma                90
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_cell_length_b                   8.975(2)
_cell_length_c                   25.944(6)
_cell_measurement_reflns_used    124
_cell_measurement_temperature    150(2)
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_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker COSMO'
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_diffrn_ambient_temperature      150(2)
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_diffrn_measurement_method       'omega scans'
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_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -34
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_diffrn_reflns_point_group_measured_fraction_full 0.998
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_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.401
_diffrn_source                   'ImuS-focus sealed tube'
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_exptl_absorpt_correction_T_min  0.6805
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   sadabs
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_exptl_crystal_description       column
_exptl_crystal_F_000             488
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_exptl_crystal_size_mid          0.154
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_refine_diff_density_max         0.244
_refine_diff_density_min         -0.152
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_refine_ls_abs_structure_details
;
 Flack x determined using 924 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.3(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0405
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0419P)^2^+0.2419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0952
_reflns_Friedel_coverage         0.677
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.979
_reflns_number_gt                2583
_reflns_number_total             2957
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b02117_si_002.cif
_cod_data_source_block           mo_sr112nl_0m_naphthalene_22_endo
_cod_depositor_comments
'Adding full bibliography for 4033135--4033140.cif.'
_cod_original_cell_volume        1208.2(5)
_cod_database_code               4033137
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.987
_shelx_estimated_absorpt_t_max   0.991
_shelx_res_checksum              50191
_shelx_hkl_checksum              74324