Intramolecular [4 + 2] Trapping of a Hexadehydro-Diels-Alder (HDDA) Benzyne by Tethered Arenes.
Pogula, Vedamayee D.; Wang, Tao; Hoye, Thomas R.; Organic letters 17 (2015) 856–859; doi:10.1021/ol5037024

data_1518724
_publ_section_title
;
 Intramolecular [4 + 2] Trapping of a Hexadehydro-Diels-Alder (HDDA)
 Benzyne by Tethered Arenes.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              856
_journal_page_last               859
_journal_paper_doi               10.1021/ol5037024
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C31 H28 O4 Si'
_chemical_formula_sum            'C31 H28 O4 Si'
_chemical_formula_weight         492.62
_chemical_name_common            14239b
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_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-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 100.775(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0146(7)
_cell_length_b                   10.5314(5)
_cell_length_c                   16.6752(8)
_cell_measurement_temperature    123(2)
_cell_volume                     2417.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type  'Bruker-AXS D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0680
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20073
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.533
_diffrn_reflns_theta_min         3.788
_diffrn_source                   ImuS
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.7538
_exptl_absorpt_correction_T_min  0.6518
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2014/3 (Sheldrick, 2012)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   0.7538
_exptl_transmission_factor_min   0.6518
_refine_diff_density_max         0.282
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4767
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0523P)^2^+1.5470P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1273
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3756
_reflns_number_total             4767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol5037024_si_002.cif
_cod_data_source_block           14239b
_cod_depositor_comments
'Adding full bibliography for 1518723--1518724.cif.'
_cod_database_code               1518724
_shelxl_version_number           2014/6
_shelx_res_checksum              35222
_shelx_hkl_checksum              49051