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_1571511
_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         'C26 H26 O5 Si'
_chemical_formula_sum            'C26 H26 O5 Si'
_chemical_formula_weight         446.56
_chemical_melting_point          492.0(10)
_chemical_name_common            20094z
_chemical_properties_physical    Heat-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 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                90
_cell_angle_beta                 102.485(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4544(5)
_cell_length_b                   10.9663(7)
_cell_length_c                   21.7055(13)
_cell_measurement_reflns_used    2724
_cell_measurement_temperature    125(2)
_cell_measurement_theta_max      30.43
_cell_measurement_theta_min      2.67
_cell_volume                     2197.2(2)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      125(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.986
_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  0.0376
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24604
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.661
_diffrn_reflns_theta_min         2.206
_diffrn_source                   micro-focus
_exptl_absorpt_coefficient_mu    0.143
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/2, Sheldrick'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.080
_exptl_transmission_factor_max   0.7461
_exptl_transmission_factor_min   0.6783
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         6722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0422
_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^)+(0.0581P)^2^+0.8862P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5374
_reflns_number_total             6722
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00571f2.cif
_cod_data_source_block           20094z_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '491-493' was changed to
'492.0(10)' -- the average value was taken and precision was
estimated.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 1571511--1571514.cif.
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571511
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.972
_shelx_estimated_absorpt_t_max   0.989
_shelx_res_checksum              18110