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_7131774
_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 H39 Be N'
_chemical_formula_sum            'C32 H39 Be N'
_chemical_formula_weight         446.65
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-06-23
_audit_creation_method           'CIF-fill 1.4j (K.Radacki, 2005-23)'
_audit_update_record
;
2023-06-23 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                   17.0285(17)
_cell_length_b                   10.2006(11)
_cell_length_c                   30.307(3)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.80
_cell_measurement_theta_min      2.42
_cell_volume                     5264.4(9)
_computing_cell_refinement       'Saint+ ver. 8.40B (Bruker AXS)'
_computing_data_collection       'BIS 6.2.14 / 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                 CPA
_diffrn_detector_area_resol_mean 7.5
_diffrn_detector_type            'Photon II'
_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 D8-Quest'
_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      0,0258017
_diffrn_orient_matrix_UB_12      0,0058797
_diffrn_orient_matrix_UB_13      -0,0316605
_diffrn_orient_matrix_UB_21      0,0944747
_diffrn_orient_matrix_UB_22      0,0011126
_diffrn_orient_matrix_UB_23      0,0087872
_diffrn_orient_matrix_UB_31      0,0043961
_diffrn_orient_matrix_UB_32      -0,0584194
_diffrn_orient_matrix_UB_33      -0,0030192
_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  0.1595
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            48426
_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         25.679
_diffrn_reflns_theta_min         2.423
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Incoatec ImS 2.0'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.5592
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2016/2 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.127
_exptl_crystal_description       plate
_exptl_crystal_F_000             1936
_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 800).
;
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       0.0174(11)
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4996
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1075
_refine_ls_R_factor_gt           0.0620
_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^)+(0.0480P)^2^+2.9422P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3306
_reflns_number_total             4996
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02736h2.cif
_cod_data_source_block           3runs_a
_cod_original_cell_volume        5264.3(9)
_cod_database_code               7131774
_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   0.993
_shelx_estimated_absorpt_t_max   0.998
_shelx_res_checksum              12069
_shelx_hkl_checksum              26148