Cascade reactions of HDDA-benzynes with tethered cyclohexadienones: strain-driven events originating from <i>ortho</i>-annulated benzocyclobutenes.
Chinta, Bhavani Shankar; Sneddon, Dorian S.; Hoye, Thomas R.; Chemical science 15 (2024) 8181–8189; doi:10.1039/d4sc00571f

data_1571512
_publ_section_title
;
 Cascade reactions of HDDA-benzynes with tethered cyclohexadienones:
 strain-driven events originating from <i>ortho</i>-annulated
 benzocyclobutenes.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              8181
_journal_page_last               8189
_journal_paper_doi               10.1039/d4sc00571f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C32 H32 O9 Si, 0.5(C H Cl3)'
_chemical_formula_sum            'C32.5 H32.5 Cl1.5 O9 Si'
_chemical_formula_weight         648.35
_chemical_name_common            21152z
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-10-21 deposited with the CCDC.	2024-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                76.320(12)
_cell_angle_beta                 77.845(8)
_cell_angle_gamma                79.645(9)
_cell_formula_units_Z            2
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_cell_length_b                   12.361(3)
_cell_length_c                   13.998(4)
_cell_measurement_reflns_used    2982
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.40
_cell_measurement_theta_min      2.45
_cell_volume                     1548.9(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0677
_diffrn_reflns_av_unetI/netI     0.0920
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            14235
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         2.042
_diffrn_source                   micro-focus
_exptl_absorpt_coefficient_mu    0.260
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5085
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/1, Sheldrick'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.390
_exptl_crystal_description       Needle
_exptl_crystal_F_000             678
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.7454
_exptl_transmission_factor_min   0.5085
_refine_diff_density_max         1.974
_refine_diff_density_min         -1.752
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5638
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.1567
_refine_ls_R_factor_gt           0.1068
_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^)+(0.1720P)^2^+5.7019P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2893
_refine_ls_wR_factor_ref         0.3364
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3519
_reflns_number_total             5638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00571f2.cif
_cod_data_source_block           21152z
_cod_depositor_comments
'Adding full bibliography for 1571511--1571514.cif.'
_cod_original_formula_sum        'C32.50 H32.50 Cl1.50 O9 Si'
_cod_database_code               1571512
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              98539