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_7131775
_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         'C33 H34 Be N2, 0.198(C H2 Cl2)'
_chemical_formula_sum            'C33.2 H34.4 Be Cl0.4 N2'
_chemical_formula_weight         484.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2023-06-21
_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                 108.7170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.4121(2)
_cell_length_b                   16.0444(2)
_cell_length_c                   19.7334(3)
_cell_measurement_reflns_used    20212
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.9700
_cell_measurement_theta_min      3.6000
_cell_volume                     5521.17(13)
_computing_cell_refinement       'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.42.30a (Rigaku OD, 2021)'
_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    'SHELXT 2014/5 (Sheldrick, 2014)''
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_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 0.999
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     38.00 109.00   0.50    0.39    --   58.41  15.00 -30.00  142
  2  \w     68.00 129.00   0.50    0.39    --   82.37  15.00  90.00  122
  3  \w     53.00  91.00   0.50    0.39    --   82.37  15.00 -60.00   76
  4  \w     95.00 133.00   0.50    0.39    --   82.37  15.00 -60.00   76
  5  \w     64.00 131.00   0.50    0.39    --   82.37  15.00-180.00  134
  6  \w     40.00  65.00   0.50    0.39    --   82.37 -95.00-180.00   50
  7  \w     40.00  90.00   0.50    0.39    --   82.37 -95.00-120.00  100
  8  \w     20.00  87.00   0.50    0.39    --   58.41-126.00 -90.00  134
  9  \w     16.00  66.00   0.50    0.39    --   58.41 -95.00-150.00  100
 10  \w     40.00  90.00   0.50    0.39    --   82.37 -95.00 -90.00  100
 11  \w     40.00  86.00   0.50    0.39    --   82.37 -95.00 -30.00   92
 12  \w     40.00  90.00   0.50    0.39    --   82.37 -95.00   0.00  100
 13  \w     40.00  90.00   0.50    0.39    --   82.37 -95.00  30.00  100
 14  \w     16.00  66.00   0.50    0.39    --   58.41 -95.00  30.00  100
 15  \w     34.00 100.00   0.50    0.39    --   82.37-112.00 120.00  132
 16  \w   -110.00 -31.00   0.50    0.39    --  -60.26 -15.00  30.00  158
 17  \w   -127.00 -40.00   0.50    0.39    --  -76.33 -15.00 150.00  174
 18  \w    -96.00 -28.00   0.50    0.39    --  -76.33 112.00 120.00  136
 19  \w    -96.00 -28.00   0.50    0.39    --  -76.33 112.00  30.00  136
 20  \w    -98.00 -22.00   0.50    0.39    --  -69.77 126.00 -60.00  152
 21  \w   -127.00 -40.00   0.50    0.39    --  -76.33 -15.00-120.00  174
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-R'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
;
 CrysAlisPro convention (1999,Acta A55,543-557)
;
_diffrn_orient_matrix_UB_11      0.0729790000
_diffrn_orient_matrix_UB_12      0.0497783000
_diffrn_orient_matrix_UB_13      0.0046842000
_diffrn_orient_matrix_UB_21      -0.0013978000
_diffrn_orient_matrix_UB_22      0.0394921000
_diffrn_orient_matrix_UB_23      0.0707410000
_diffrn_orient_matrix_UB_31      0.0497569000
_diffrn_orient_matrix_UB_32      -0.0720514000
_diffrn_orient_matrix_UB_33      0.0419334000
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_xray_symbol    K-L~2,3~
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            55988
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.074
_diffrn_reflns_theta_min         3.631
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.846
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.648
_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    1.166
_exptl_crystal_description       plate
_exptl_crystal_F_000             2067
_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          0.222
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.188
_refine_diff_density_min         -0.230
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     718
_refine_ls_number_reflns         10464
_refine_ls_number_restraints     69
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0416
_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^)+(0.0595P)^2^+1.1938P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1057
_refine_ls_wR_factor_ref         0.1118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8571
_reflns_number_total             10464
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc02736h2.cif
_cod_data_source_block           ToTr072_ToTr_a
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C33.20 H34.40 Be Cl0.40 N2'
_cod_database_code               7131775
_shelx_shelxl_version_number     2019/1
_shelx_res_checksum              99758
_shelx_hkl_checksum              36127