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_7131772
_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         'C40 H59 Be Li2 N O2'
_chemical_formula_sum            'C40 H59 Be Li2 N O2'
_chemical_formula_weight         608.77
_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                 98.2680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.8193(2)
_cell_length_b                   15.1540(2)
_cell_length_c                   15.8904(2)
_cell_measurement_reflns_used    17097
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.2870
_cell_measurement_theta_min      2.8190
_cell_volume                     3769.74(8)
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (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 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     55.00  85.00   0.50    0.18    --   38.00  52.00  32.84   60
  2  \w     94.00 120.00   0.50    0.18    --   80.79  55.00  31.52   52
  3  \w     93.00 118.00   0.50    0.18    --   80.79  40.00 -27.63   50
  4  \w     36.00  98.00   0.50    0.18    --   84.66-120.00 115.00  124
  5  \w     22.00  97.00   0.50    0.18    --   71.30-120.00 115.00  150
  6  \w     37.00  97.00   0.50    0.18    --   84.66-112.00 150.00  120
  7  \w     28.00  98.00   0.50    0.18    --   76.93-120.00 115.00  140
  8  \w     34.00  83.00   0.50    0.18    --   76.93 -95.00 150.00   98
  9  \w     16.00  84.00   0.50    0.18    --   58.61-120.00 115.00  136
 10  \w     43.00  72.00   0.50    0.18    --   84.66 -95.00 -30.00   58
 11  \w     72.00  97.00   0.50    0.18    --   84.66-112.00-150.00   50
 12  \w     72.00  97.00   0.50    0.18    --   84.66-112.00-180.00   50
 13  \w     62.00  88.00   0.50    0.18    --   84.66 -95.00-180.00   52
 14  \w     50.00  92.00   0.50    0.18    --   84.66 -95.00-150.00   84
 15  \w    -85.00 -12.00   0.50    0.18    --  -60.19 120.00-160.00  146
 16  \w    -95.00 -21.00   0.50    0.18    --  -69.72 120.00-160.00  148
 17  \w    -98.00 -28.00   0.50    0.18    --  -76.37 120.00-160.00  140
 18  \w    -36.00 -11.00   0.50    0.18    --  -10.00 121.00 -21.57   50
 19  \w   -124.00 -92.00   0.50    0.18    --  -79.50 -63.00 -12.17   64
 20  \w   -122.00 -94.00   0.50    0.18    --  -79.50 -62.00 146.78   56
 21  \w   -117.00 -84.00   0.50    0.18    --  -70.00 -57.00 118.81   66
 22  \w   -113.00 -80.00   0.50    0.18    --  -66.00 -49.00 159.42   66
 23  \w   -128.00 -94.00   0.50    0.18    --  -79.50 -52.00  46.88   68
 24  \w   -106.00 -80.00   0.50    0.18    --  -62.00 -48.00  36.57   52
 25  \w   -117.00 -84.00   0.50    0.18    --  -70.00 -47.00 177.70   66
 26  \w   -124.00 -89.00   0.50    0.18    --  -74.00 -45.00 -94.73   70
 27  \w   -127.00 -93.00   0.50    0.18    --  -79.50 -50.00-117.52   68
 28  \w    -97.00 -64.00   0.50    0.18    --  -50.00 -52.00-179.02   66
 29  \w   -113.00 -87.00   0.50    0.18    --  -66.00 -48.00-161.67   52
;
_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      -0.0147764000
_diffrn_orient_matrix_UB_12      -0.0931938000
_diffrn_orient_matrix_UB_13      0.0336136000
_diffrn_orient_matrix_UB_21      -0.0609235000
_diffrn_orient_matrix_UB_22      0.0384658000
_diffrn_orient_matrix_UB_23      0.0580575000
_diffrn_orient_matrix_UB_31      -0.0758795000
_diffrn_orient_matrix_UB_32      -0.0127257000
_diffrn_orient_matrix_UB_33      -0.0713506000
_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  0.0272
_diffrn_reflns_av_unetI/netI     0.0204
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11142
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.065
_diffrn_reflns_theta_min         2.823
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021) Empirical 
 absorption correction using spherical harmonics, implemented in SCALE3 
 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.073
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_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          0.221
_exptl_crystal_size_mid          0.153
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.197
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         11142
_refine_ls_number_restraints     126
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0564P)^2^+1.0965P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1125
_refine_ls_wR_factor_ref         0.1176
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9357
_reflns_number_total             11142
_reflns_threshold_expression     'I > 2\s(I)'
_twin_dimensionality             triperiodic
_twin_formation_mechanism        gt
_twin_morphology                 polysynthetic
_twin_special_details
;
 Component 2 rotated by -179.6974\% 
 around [0.01 1.00 -0.00] (reciprocal) or [0.01 1.00 -0.00] (direct)
;
_cod_data_source_file            d3cc02736h2.cif
_cod_data_source_block           ToTr078_ToTr_twin1_hklf5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7131772
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.903
_shelx_estimated_absorpt_t_max   0.947
_shelx_res_checksum              62734
_shelx_hkl_checksum              4847