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_7135345
_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         'C36 H36 Be O2 S2'
_chemical_formula_sum            'C36 H36 Be O2 S2'
_chemical_formula_weight         573.78
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2x (K.Radacki, 2005-21)'
_audit_update_record
;
2025-10-09 deposited with the CCDC.	2026-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 111.967(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2072(8)
_cell_length_b                   10.3142(3)
_cell_length_c                   19.7310(9)
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_cell_measurement_temperature    100(2)
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_cell_volume                     3058.9(2)
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_computing_data_collection       'BIS 2011.8 / APEX2 ver. 2014.9 (Bruker AXS)'
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_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(11)
_diffrn_detector                 HPA
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'HyPix Arc150'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 
   # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
 --------------------------------------------------------------------------
   1  \w     16.00  66.00   0.50    0.50    --   58.41 -95.00 -60.00  100
   2  \w     16.00  66.00   0.50    0.50    --   58.41 -95.00   0.00  100
   3  \w     20.00  87.00   0.50    0.50    --   58.41-126.00-150.00  134
   4  \w     58.00 109.00   0.50    0.50    --   58.41  15.00 -30.00  102
   5  \w   -110.00 -50.00   0.50    0.50    --  -60.06 -15.00  30.00  120
   6  \w     28.00  79.00   0.50    0.50    --   71.12 -95.00  60.00  102
   7  \w    -96.00 -28.00   0.50    3.00    --  -76.33 112.00 120.00  136
   8  \w   -127.00 -50.00   0.50    3.00    --  -76.33 -15.00-150.00  154
   9  \w   -127.00 -50.00   0.50    3.00    --  -76.33 -15.00 -60.00  154
  10  \w     34.00 100.00   0.50    3.00    --   82.37-112.00-180.00  132
  11  \w     34.00 100.00   0.50    3.00    --   82.37-112.00 120.00  132
  12  \w     40.00  90.00   0.50    3.00    --   82.37 -95.00  30.00  100
  13  \w     34.00  94.00   0.50    3.00    --   82.37-112.00-150.00  120
  14  \w     44.00  74.00   0.50    3.00    --   82.37 -95.00 120.00   60
  15  \w     57.00 123.00   0.50    3.00    --   82.37  15.00 150.00  132
  16  \w     34.00  96.00   0.50    3.00    --   82.37-112.00 -90.00  124
  17  \w     61.00 133.00   0.50    3.00    --   82.37  15.00   0.00  144
  18  \w     47.00  88.00   0.50    3.00    --   82.37-112.00  90.00   82
  19  \w     34.00  84.00   0.50    3.00    --   82.37-112.00   0.00  100
  20  \w    101.00 127.00   0.50    3.00    --   82.37  15.00-180.00   52
  21  \w     57.00 127.00   0.50    3.00    --   82.37  15.00 -90.00  140
  22  \w     37.00  92.00   0.50    3.00    --   82.37-112.00  30.00  110
  23  \w     73.00 100.00   0.50    3.00    --   82.37-112.00 -30.00   54
  24  \w     46.00  72.00   0.50    3.00    --   82.37-112.00 -30.00   52

;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29971
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.729
_diffrn_reflns_theta_min         3.027
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R X-ray Source'
_exptl_absorpt_coefficient_mu    1.808
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.446
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.30a (Rigaku Oxford Diffraction, 2021) Numerical 
absorption correction based on gaussian integration over a multifaceted 
crystal model Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_description       plate
_exptl_crystal_F_000             1216
_exptl_crystal_size_max          0.368
_exptl_crystal_size_mid          0.248
_exptl_crystal_size_min          0.191
_refine_diff_density_max         0.409
_refine_diff_density_min         -0.521
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         6108
_refine_ls_number_restraints     432
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0940P)^2^+1.1755P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1576
_refine_ls_wR_factor_ref         0.1653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4895
_reflns_number_total             6108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc05783c2.cif
_cod_data_source_block           ToTr070b_ToTr_auto_a
_cod_depositor_comments
'Adding full bibliography for 7135342--7135346.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7135345
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              56757
_shelx_hkl_checksum              16847