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_1571514
_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         '8(C29 H30 O6 Si), 3(C5 H12)'
_chemical_formula_sum            'C247 H276 O48 Si8'
_chemical_formula_weight         4237.5566
_chemical_melting_point          392.0(10)
_chemical_name_common            'the cyclopropane'
_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
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2023-10-21 deposited with the CCDC.	2024-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                71.929(2)
_cell_angle_beta                 86.176(2)
_cell_angle_gamma                73.612(2)
_cell_formula_units_Z            1
_cell_length_a                   12.6362(7)
_cell_length_b                   18.9096(13)
_cell_length_c                   25.0480(17)
_cell_measurement_reflns_used    9635
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.66
_cell_measurement_theta_min      2.25
_cell_volume                     5457.3(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX4'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
'SHELXLE, Hubschle, C. B. et al. J.Appl. Cryst. 44, (2011), 1281-1284.'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/2 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0563
_diffrn_reflns_av_unetI/netI     0.0499
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            98015
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.903
_diffrn_source                   micro-focus
_exptl_absorpt_coefficient_mu    0.129
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.7000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS, Krause, L. et al. J. Appl. Cryst.(2015), 48, 3-10.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2254
_exptl_crystal_recrystallization_method 'vapor diffusion from DCM and pentane'
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_transmission_factor_max   0.7453
_exptl_transmission_factor_min   0.7000
_refine_diff_density_max         1.786
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1415
_refine_ls_number_reflns         19978
_refine_ls_number_restraints     133
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+4.2149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1033
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14318
_reflns_number_total             19978
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc00571f2.cif
_cod_data_source_block           23151c_a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_chemical_melting_point' value '391-393' was changed to
'392.0(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_database_code               1571514
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.988
_shelx_estimated_absorpt_t_max   0.997
_shelx_res_checksum              3239