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_7717295
_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         'C31 H44 Be N2 S'
_chemical_formula_sum            'C31 H44 Be N2 S'
_chemical_formula_weight         485.75
_chemical_name_common            (CAAC)BDur(NCS)
_chemical_name_systematic        2b
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-09-25
_audit_creation_method           'CIF-fill 1.5g (K.Radacki, 2005-23)'
_audit_update_record
;
2024-09-25 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.294(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.4324(5)
_cell_length_b                   18.541(5)
_cell_length_c                   15.2352(7)
_cell_measurement_reflns_used    3176
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.1620
_cell_measurement_theta_min      4.7820
_cell_volume                     2942.0(8)
_computing_cell_refinement       'CrysAlisPro 1.171.43.111a (Rigaku OD, 2024)'
_computing_data_collection
;
 CrysAlisPro system (CCD 42.72a 64-bit (release 07-10-2022))
;
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     40.00  69.00   0.50    0.05    --   82.35 -95.00   0.00   58
  2  \w     45.00  86.00   0.50    0.05    --   85.25-104.00-152.60   82
  3  \w   -106.00 -71.00   0.50    0.05    --  -58.00 -52.00 -73.90   70
  4  \w     65.00  90.00   0.50    0.05    --   82.35 -95.00 150.00   50
  5  \w   -126.00 -93.00   0.50    0.05    --  -79.50-120.00 -42.55   66
  6  \w     81.00 129.00   0.50    0.05    --   85.25  11.00  63.33   96
  7  \w   -124.00 -97.00   0.50    0.05    --  -79.50 -63.00 141.05   54
  8  \w     29.00  79.00   0.50    0.05    --   71.26 -95.00 150.00  100
  9  \w     45.00  71.00   0.50    0.05    --   82.35-112.00 150.00   52
 10  \w     16.00  66.00   0.50    0.05    --   58.60 -95.00-120.00  100
 11  \w   -126.00 -88.00   0.50    0.05    --  -79.50-130.00-113.69   76
 12  \w   -123.00 -95.00   0.50    0.05    --  -79.50 -50.00  42.84   56
 13  \w   -115.00 -80.00   0.50    0.05    --  -66.00 -47.00 -36.88   70
 14  \w     43.00  92.00   0.50    0.05    --   85.25-101.00 124.67   98
 15  \w     52.00  89.00   0.50    0.05    --   85.25-107.00 -54.60   74
 16  \w     16.00  66.00   0.50    0.05    --   58.60 -95.00 120.00  100
 17  \w    -99.00 -64.00   0.50    0.05    --  -50.00 -50.00  43.91   70
 18  \w   -122.00 -96.00   0.50    0.05    --  -79.50-120.00 106.54   52
 19  \w     39.00  65.00   0.50    0.05    --   85.25-134.00 129.82   52
 20  \w    101.00 126.00   0.50    0.05    --   85.25 118.00   0.91   50
 21  \w     40.00  78.00   0.50    0.05    --   85.25-104.00 110.51   76
 22  \w     42.00  73.00   0.50    0.05    --   82.35-112.00   0.00   62
 23  \w   -118.00 -83.00   0.50    0.05    --  -70.00 -53.00 -98.11   70
 24  \w     76.00 116.00   0.50    0.05    --   64.93  39.00-165.06   80
 25  \w     49.00  75.00   0.50    0.05    --   85.25 -91.00 165.36   52
 26  \w     42.00  73.00   0.50    0.05    --   85.25 -99.00  72.78   62
 27  \w     37.00  62.00   0.50    0.05    --   82.35-112.00 -60.00   50
 28  \w     98.00 126.00   0.50    0.05    --   85.25  37.00 -47.44   56
 29  \w     52.00  79.00   0.50    0.05    --   85.25-124.00 177.64   54
 30  \w     78.00 104.00   0.50    0.05    --   85.25  11.00 165.39   52
 31  \w     96.00 121.00   0.50    0.05    --   85.25  62.00 -50.80   50
 32  \w     96.00 132.00   0.50    0.05    --   85.25 138.00 -40.81   72
 33  \w    103.00 129.00   0.50    0.05    --   85.25  48.00 127.41   52
 34  \w     40.00 105.00   0.50    0.05    --   85.25-139.00 -52.19  130
 35  \w     51.00 100.00   0.50    0.05    --   85.25-127.00 -93.49   98
 36  \w     46.00  71.00   0.50    0.05    --   85.25 -87.00 -99.55   50
 37  \w     44.00  69.00   0.50    0.05    --   85.25 -73.00  20.11   50
 38  \w     45.00  71.00   0.50    0.05    --   85.25 -73.00-149.06   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      0.1304012000
_diffrn_orient_matrix_UB_12      0.0330792000
_diffrn_orient_matrix_UB_13      0.0309838000
_diffrn_orient_matrix_UB_21      0.0698136000
_diffrn_orient_matrix_UB_22      -0.0649943000
_diffrn_orient_matrix_UB_23      -0.0384827000
_diffrn_orient_matrix_UB_31      0.0055539000
_diffrn_orient_matrix_UB_32      0.0398865000
_diffrn_orient_matrix_UB_33      -0.0882827000
_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  0.0302
_diffrn_reflns_av_unetI/netI     0.0090
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11874
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.073
_diffrn_reflns_theta_min         3.759
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58354
_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            colourless
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       block
_exptl_crystal_F_000             1056
_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_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.472
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_min          0.159
_refine_diff_density_max         0.274
_refine_diff_density_min         -0.309
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         11874
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0719P)^2^+0.4095P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10723
_reflns_number_total             11874
_reflns_threshold_expression     'I > 2\s(I)'
_twin_dimensionality             triperiodic
_twin_formation_mechanism        gt
_twin_morphology                 polysynthetic
_twin_special_details
;
 Component 2 rotated by 179.9521\% 
 around [-0.00 1.00 0.01] (reciprocal) or [-0.01 1.00 0.02] (direct)
;
_cod_data_source_file            d4dt02457e2.cif
_cod_data_source_block           CoCz111_CoCz_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7717294--7717301.cif.'
_cod_original_cell_volume        2942.1(9)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7717295
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.623
_shelx_estimated_absorpt_t_max   0.844
_shelx_res_checksum              73840
_shelx_hkl_checksum              21299