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_7717301
_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         'C100 H160 Be4 N8 O4, 2 (C5 H12) [squeezed]'
_chemical_formula_sum            'C110 H184 B E4 N8 O4'
_chemical_formula_weight         1718.78
_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_date             2024-10-10
_audit_creation_method           'CIF-fill 1.5g (K.Radacki, 2005-23)'
_audit_update_record
;
2024-10-11 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.089(10)
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   35.978(6)
_cell_length_b                   25.4382(16)
_cell_length_c                   36.315(3)
_cell_measurement_reflns_used    1461
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      61.7870
_cell_measurement_theta_min      3.1900
_cell_volume                     33214(7)
_computing_cell_refinement       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_collection
;
 CrysAlisPro system (CCD 42.67a 64-bit (release 29-08-2022))
;
_computing_data_reduction        'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_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 0.950
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -90.00 -24.00   0.50   41.00    --  -69.71 114.00  -0.00  132
  2  \w   -121.00 -58.00   0.50   41.00    --  -69.71 -21.00 101.00  126
  3  \w    -92.00 -31.00   0.50   41.00    --  -76.30 111.00  93.00  122
  4  \w     70.00 134.00   0.50   41.00    --   82.35  21.00 -91.00  128
  5  \w     37.00  97.00   0.50   41.00    --   82.35-114.00 -90.00  120
  6  \w   -106.00 -71.00   0.50   41.00    --  -58.00 -51.00 -83.10   70
  7  \w     47.00 110.00   0.50   41.00    --   58.60  21.00 -91.00  126
  8  \w     16.00  66.00   0.50   41.00    --   58.60 -95.00 -30.00  100
  9  \w   -129.00 -92.00   0.50   41.00    --  -79.50 -45.00  82.37   74
 10  \w   -125.00 -91.00   0.50   41.00    --  -79.50 -60.00  55.20   68
 11  \w   -128.00 -93.00   0.50   41.00    --  -79.50 -51.00 144.07   70
 12  \w   -121.00 -92.00   0.50   41.00    --  -79.50 -53.00  -1.32   58
 13  \w     64.00  90.00   0.50   41.00    --   82.35 -95.00  30.00   52
 14  \w     40.00  88.00   0.50   41.00    --   82.35 -95.00   0.00   96
;
_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      0.0282006000
_diffrn_orient_matrix_UB_12      -0.0418552000
_diffrn_orient_matrix_UB_13      -0.0117215000
_diffrn_orient_matrix_UB_21      0.0218883000
_diffrn_orient_matrix_UB_22      0.0425699000
_diffrn_orient_matrix_UB_23      -0.0202629000
_diffrn_orient_matrix_UB_31      0.0237222000
_diffrn_orient_matrix_UB_32      0.0104875000
_diffrn_orient_matrix_UB_33      0.0354376000
_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  0.1811
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 0.950
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            65532
_diffrn_reflns_point_group_measured_fraction_full 0.950
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        65.086
_diffrn_reflns_theta_max         65.086
_diffrn_reflns_theta_min         3.200
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.26107
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.43.111a (Rigaku Oxford Diffraction, 2024) Empirical 
 absorption correction using spherical harmonics, implemented in SCALE3 
 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_description       plate
_exptl_crystal_F_000             11376
_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          0.146
_exptl_crystal_size_mid          0.071
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.307
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2322
_refine_ls_number_reflns         65532
_refine_ls_number_restraints     3492
_refine_ls_restrained_S_all      1.296
_refine_ls_R_factor_all          0.2933
_refine_ls_R_factor_gt           0.1550
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4058
_refine_ls_wR_factor_ref         0.4805
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22716
_reflns_number_total             65532
_reflns_threshold_expression     'I > 2\s(I)'
_twin_dimensionality             triperiodic
_twin_formation_mechanism        gt
_twin_morphology                 polysynthetic
_twin_special_details
;
 Component 2 rotated by 1.6854\%
 around [0.07 0.58 0.81] (reciprocal) or [0.07 0.82 0.57] (direct)
;
_cod_data_source_file            d4dt02457e2.cif
_cod_data_source_block           CoCz089_CoCz_twin1_hklf5_sq
_cod_depositor_comments
'Adding full bibliography for 7717294--7717301.cif.'
_cod_original_cell_volume        33214(6)
_cod_original_sg_symbol_H-M      'I 2/a'
_cod_original_formula_sum        'C110 H184 BE4 N8 O4'
_cod_database_code               7717301
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.941
_shelx_estimated_absorpt_t_max   0.986
_shelx_res_checksum              34380
_shelx_hkl_checksum              32659
_shelx_fab_checksum              9743