Synthesis and structures of molecular beryllium Grignard analogues featuring terminal and bridging pseudohalides.
Czernetzki, Corinna; Arrowsmith, Merle; Jürgensen, Malte; Hagspiel, Stephan; Braunschweig, Holger; Dalton transactions (Cambridge, England : 2003) 53 (2024) 18296–18303; doi:10.1039/d4dt02457e

data_7717298
_publ_section_title
;
 Synthesis and structures of molecular beryllium Grignard analogues
 featuring terminal and bridging pseudohalides.
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18296
_journal_page_last               18303
_journal_paper_doi               10.1039/d4dt02457e
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         '6(C21 H31 Be Br N2 O2), 3(C6 H6)'
_chemical_formula_sum            'C144 H204 Be6 Br6 N12 O6'
_chemical_formula_weight         2732.70
_chemical_name_systematic        '[(CAAC)BrBe(NCO)]6, 7'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CIF-fill 1.2n (K.Radacki 2005-21)'
_audit_update_record
;
2024-08-22 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.1780(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.35350(10)
_cell_length_b                   30.9252(2)
_cell_length_c                   25.8198(2)
_cell_measurement_reflns_used    31531
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.2420
_cell_measurement_theta_min      2.8720
_cell_volume                     14595.14(17)
_computing_cell_refinement       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.109a (Rigaku OD, 2021)'
_computing_molecular_graphics    'ShelXLe (Huebschle et all, 2011)'
_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(10)
_diffrn_detector                 'HPAD area detector (HyPix 6000)'
_diffrn_detector_area_resol_mean 10.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_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    -46.00  23.00   0.50    1.03    --  -47.71  43.00  42.00  138
   2  \w   -120.00 -50.00   0.50    1.03    --  -47.71 -43.00-108.00  140
   3  \w     53.00  78.00   0.50    1.03    --   47.71  43.00  42.00   50
   4  \w    -13.00  13.00   0.50    1.03    --   47.71 -43.00-108.00   52
   5  \w   -145.00-120.00   0.50    4.11    --  -91.75 -43.00-108.00   50
   6  \w    -48.00 -23.00   0.50    4.11    --  -91.75  43.00  42.00   50
   7  \w    110.00 165.00   0.50    4.11    --  113.25  43.00  42.00  110
   8  \w   -118.00 -73.00   0.50    1.03    --  -47.71-125.00-150.00   90
   9  \w   -118.00 -71.00   0.50    1.03    --  -47.71-125.00  30.00   94
  10  \w     31.00  93.00   0.50    1.03    --   47.71-125.00-120.00  124
  11  \w    -70.00 -43.00   0.50    4.11    --  -91.75  61.00 150.00   54
  12  \w    -46.00 -21.00   0.50    4.11    --  -91.75  45.00-150.00   50
  13  \w     42.00  68.00   0.50    4.11    --  113.25 -61.00-150.00   52
  14  \w     43.00  98.00   0.50    4.11    --  113.25 -77.00 -30.00  110
  15  \w     47.00 106.00   0.50    4.11    --  113.25 -77.00 -90.00  118
  16  \w    149.00 175.00   0.50    4.11    --  113.25  15.00 150.00   52
  17  \w    103.00 143.00   0.50    4.11    --  113.25  15.00 150.00   80
  18  \w     42.00  67.00   0.50    4.11    --  113.25 -61.00-120.00   50
  19  \w     42.00  82.00   0.50    4.11    --  113.25 -77.00   0.00   80
  20  \w     42.00  69.00   0.50    4.11    --  113.25 -61.00-180.00   54
  21  \w    148.00 174.00   0.50    4.11    --  113.25  15.00  60.00   52
  22  \w     43.00  71.00   0.50    4.11    --  113.25 -61.00 120.00   56
  23  \w    125.00 169.00   0.50    4.11    --  113.25  15.00-180.00   88
  24  \w     42.00  84.00   0.50    4.11    --  113.25 -94.00-180.00   84
  25  \w     45.00 112.00   0.50    4.11    --  113.25-125.00-150.00  134
  26  \w     55.00 101.00   0.50    4.11    --  113.25 -77.00  90.00   92
  27  \w    106.00 140.00   0.50    4.11    --  113.25  15.00 -60.00   68
  28  \w    153.00 178.00   0.50    4.11    --  113.25  15.00 -60.00   50
  29  \w     97.00 159.00   0.50    4.11    --  113.25  77.00 120.00  124
  30  \w    102.00 178.00   0.50    4.11    --  113.25  30.00  90.00  152
  31  \w     45.00  71.00   0.50    4.11    --  113.25 -61.00 150.00   52
  32  \w    122.00 177.00   0.50    4.11    --  113.25  45.00-180.00  110
  33  \w     42.00  68.00   0.50    4.11    --  113.25 -61.00  60.00   52
  34  \w     43.00  69.00   0.50    4.11    --  113.25 -61.00  90.00   52
  35  \w    103.00 128.00   0.50    4.11    --  113.25  15.00  60.00   50
  36  \w     46.00  73.00   0.50    4.11    --  113.25 -77.00 -60.00   54
  37  \w     42.00  70.00   0.50    4.11    --  113.25 -61.00 -90.00   56
  38  \w     44.00  71.00   0.50    4.11    --  113.25 -61.00  30.00   54
  39  \w     59.00 103.00   0.50    4.11    --  113.25 -94.00-150.00   88

;
_diffrn_measurement_device_type  'Rigaku OD XtaLAB Synergy-S'
_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  0.0456
_diffrn_reflns_av_unetI/netI     0.0295
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            67020
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.126
_diffrn_reflns_theta_min         2.858
_diffrn_source                   'microfocus sealed tube (PhotonJet)'
_exptl_absorpt_coefficient_mu    2.408
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.41.109a (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            colorless
_exptl_crystal_density_diffrn    1.244
_exptl_crystal_description       block
_exptl_crystal_F_000             5736
_exptl_crystal_size_max          0.253
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.067
_refine_diff_density_max         1.537
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         14343
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0923P)^2^+31.9424P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1497
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12047
_reflns_number_total             14343
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02457e2.cif
_cod_data_source_block           AnGa113_CoCz_a
_cod_depositor_comments
'Adding full bibliography for 7717294--7717301.cif.'
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_database_code               7717298
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.584
_shelx_estimated_absorpt_t_max   0.850
_shelx_res_checksum              28288
_shelx_hkl_checksum              58626