Dibenzoberylloles: antiaromatic s-block fluorene analogues
Tröster, Tobias; Endres, Franziska; Arrowsmith, Merle; Endres, Lukas; Fantuzzi, Felipe; Braunschweig, Holger; Chemical Communications  (2023) –; doi:10.1039/D3CC02736H

data_7131768
_publ_section_title
;
 Dibenzoberylloles: antiaromatic s-block fluorene analogues
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC02736H
_journal_year                    2023
_chemical_formula_moiety         'C32 H36 Be2 O2 [0.25 (C4 H10 O)]'
_chemical_formula_sum            'C33 H38.5 Be2 O2.25'
_chemical_formula_weight         489.19
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-06-22
_audit_creation_method           'CIF-fill 1.4j (K.Radacki, 2005-23)'
_audit_update_record
;
2023-06-27 deposited with the CCDC.	2023-06-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.323(3)
_cell_length_b                   17.323(3)
_cell_length_c                   18.354(4)
_cell_measurement_reflns_used    3989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.75
_cell_measurement_theta_min      2.77
_cell_volume                     5507.8(18)
_computing_cell_refinement       'Saint+ ver. 8.40B (Bruker AXS)'
_computing_data_collection       'BIS 2011.8 / APEX4 ver. 2021.10 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 8.40B (Bruker AXS)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_computing_publication_material  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXS 2013/1 (Sheldrick, 2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.998
_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      0,0036309
_diffrn_orient_matrix_UB_12      0,0002576
_diffrn_orient_matrix_UB_13      0,0543744
_diffrn_orient_matrix_UB_21      0,0409652
_diffrn_orient_matrix_UB_22      0,0406351
_diffrn_orient_matrix_UB_23      -0,0026045
_diffrn_orient_matrix_UB_31      -0,0405667
_diffrn_orient_matrix_UB_32      0,0410573
_diffrn_orient_matrix_UB_33      0,0022366
_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  0.0740
_diffrn_reflns_av_unetI/netI     0.0533
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16085
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.636
_diffrn_reflns_theta_min         1.616
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'Nonius FR-591'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6351
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.180
_exptl_crystal_description       block
_exptl_crystal_F_000             2016
_exptl_crystal_preparation
;
 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          0.286
_exptl_crystal_size_mid          0.282
_exptl_crystal_size_min          0.282
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.165
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         2612
_refine_ls_number_restraints     144
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0484
_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^)+(0.0357P)^2^+2.8575P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1006
_refine_ls_wR_factor_ref         0.1092
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2012
_reflns_number_total             2612
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02736h2.cif
_cod_data_source_block           1run_a_sq
_cod_original_cell_volume        5508(2)
_cod_original_sg_symbol_H-M      'P 4/n n c'
_cod_database_code               7131768
_shelx_shelxl_version_number     2019/1
_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_estimated_absorpt_t_min   0.981
_shelx_estimated_absorpt_t_max   0.981
_shelx_res_checksum              56168
_shelx_hkl_checksum              68951
_shelx_fab_checksum              30965