Synthesis of Oxatricyclooctanes via Photoinduced Intramolecular Oxa-[4+2] Cycloaddition of Substituted o-Divinylbenzenes.
Liu, Qiang; Wang, Junlei; Li, Dazhi; Gao, Guo-Lin; Yang, Chao; Gao, Yuan; Xia, Wujiong; The Journal of organic chemistry 82 (2017) 7856–7868; doi:10.1021/acs.joc.7b01055

data_4032681
_publ_section_title
;
 Synthesis of Oxatricyclooctanes via Photoinduced Intramolecular Oxa-[4+2]
 Cycloaddition of Substituted o-Divinylbenzenes.
;
_journal_issue                   15
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              7856
_journal_page_last               7868
_journal_paper_doi               10.1021/acs.joc.7b01055
_journal_volume                  82
_journal_year                    2017
_chemical_formula_sum            'C15 H16 O3'
_chemical_formula_weight         244.28
_space_group_crystal_system      monoclinic
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_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
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_cell_angle_beta                 102.68(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.607(8)
_cell_length_b                   5.662(4)
_cell_length_c                   18.667(14)
_cell_measurement_reflns_used    654
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.62
_cell_measurement_theta_min      3.40
_cell_volume                     1300.0(16)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CCD
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0591
_diffrn_reflns_av_unetI/netI     0.0602
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7753
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.889
_diffrn_reflns_theta_max         24.889
_diffrn_reflns_theta_min         1.783
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.248
_exptl_crystal_description       Block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_transmission_factor_max   0.864
_exptl_transmission_factor_min   0.864
_refine_diff_density_max         0.203
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.940
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2252
_refine_ls_number_restraints     58
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.0961
_refine_ls_R_factor_gt           0.0608
_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^)+(0.0932P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1410
_refine_ls_wR_factor_ref         0.1672
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1369
_reflns_number_total             2252
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo7b01055_si_002.cif
_cod_data_source_block           1_a
_cod_original_cell_volume        1300.1(15)
_cod_database_code               4032681
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.985
_shelx_res_checksum              58542
_shelx_hkl_checksum              25560