Ring expansion of an antiaromatic beryllole: synthesis of novel five-, seven- and nine-membered beryllacycles.
Tröster, Tobias; Saha, Koushik; Roy, Dipak Kumar; Dewhurst, Rian D.; Braunschweig, Holger; Chemical communications (Cambridge, England) 62 (2026) 5032–5036; doi:10.1039/d5cc05783c

data_7135343
_publ_section_title
;
 Ring expansion of an antiaromatic beryllole: synthesis of novel five-,
 seven- and nine-membered beryllacycles.
;
_journal_issue                   17
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5032
_journal_page_last               5036
_journal_paper_doi               10.1039/d5cc05783c
_journal_volume                  62
_journal_year                    2026
_chemical_formula_moiety         '2(C48 H51 Be N S2), C7 H8'
_chemical_formula_sum            'C103 H110 Be2 N2 S4'
_chemical_formula_weight         1522.18
_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     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-09-04
_audit_creation_method           'CIF-fill 1.4m (K.Radacki, 2005-23)'
_audit_update_record
;
2025-11-26 deposited with the CCDC.	2026-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                95.952(5)
_cell_angle_beta                 111.349(5)
_cell_angle_gamma                101.372(5)
_cell_formula_units_Z            1
_cell_length_a                   12.060(3)
_cell_length_b                   13.360(3)
_cell_length_c                   15.212(3)
_cell_measurement_reflns_used    4666
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.32
_cell_volume                     2196.3(9)
_computing_cell_refinement       'Saint+ ver. 8.38A (Bruker AXS)'
_computing_data_collection       'BIS 2011.8 / APEX4 ver. 2021.10 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.38A (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)''
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 4.166
_diffrn_detector_type            Apex2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Bruker X8-APEX II'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_orient_matrix_type
;
 Sparks R.A., Computational Crystallography p1-18 (Clarendon Press, 1982)
;
_diffrn_orient_matrix_UB_11      0.0886077
_diffrn_orient_matrix_UB_12      0.0125623
_diffrn_orient_matrix_UB_13      0.0435784
_diffrn_orient_matrix_UB_21      -0.0247475
_diffrn_orient_matrix_UB_22      -0.0355661
_diffrn_orient_matrix_UB_23      0.0471519
_diffrn_orient_matrix_UB_31      0.0026065
_diffrn_orient_matrix_UB_32      -0.0680448
_diffrn_orient_matrix_UB_33      -0.0324027
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.1087
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28426
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.802
_diffrn_reflns_theta_min         1.464
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Nonius FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.156
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_description       block
_exptl_crystal_F_000             814
_exptl_crystal_preparation
;
 Crystals were grown at -30 \%C from saturated solution in Toluene. For data 
 collection the crystal was immersed in a film of perfluoropolyether oil, 
 mounted on a polyimide loop and transferred to stream of cold nitrogen 
 (Oxford Cryostream 700).
;
_exptl_crystal_size_max          0.065
_exptl_crystal_size_mid          0.062
_exptl_crystal_size_min          0.053
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         10137
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0614
_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^)+(0.0561P)^2^+1.1504P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6422
_reflns_number_total             10137
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05783c2.cif
_cod_data_source_block           cop075_0m
_cod_depositor_comments
'Adding full bibliography for 7135342--7135346.cif.'
_cod_original_cell_volume        2196.3(8)
_cod_database_code               7135343
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
 Incident beam scaling, empirical absorption correction using spherical 
 harmonics, and outlier rejection was employed as implemented in SADABS. 
 Additional spherical absorption correction with mu*r value set to 0.2 was 
 applied.
;
_shelx_res_checksum              24797
_shelx_hkl_checksum              42269