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_7717299
_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 N O P'
_chemical_formula_sum            'C31 H44 Be N O P'
_chemical_formula_weight         486.65
_chemical_name_systematic        '[(CAAC)(Dur)Be(OCP)], 4b'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-11-03
_audit_creation_method           'CIF-fill 1.3n (K.Radacki, 2005-22)'
_audit_update_record
;
2024-08-22 deposited with the CCDC.	2024-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   18.2979(2)
_cell_length_b                   16.8696(2)
_cell_length_c                   18.7109(2)
_cell_measurement_reflns_used    18876
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      74.9480
_cell_measurement_theta_min      4.2380
_cell_volume                     5775.65(11)
_computing_cell_refinement       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.68a (Rigaku OD, 2022)'
_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 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    -54.00 -15.00   0.50    1.08    --  -60.16 121.00 178.00   78
  2  \w     17.00  68.00   0.50    1.08    --   58.30-121.00  96.00  102
  3  \w     39.00  92.00   0.50    1.08    --   85.25-120.00-111.41  106
  4  \w     53.00  79.00   0.50    1.08    --   85.25 -96.00 -43.43   52
  5  \w     64.00  92.00   0.50    1.08    --   85.25 -94.00 152.63   56
  6  \w   -125.00 -93.00   0.50    1.08    --  -79.50 -54.00-164.34   64
  7  \w     52.00  78.00   0.50    1.08    --   85.25-106.00 143.06   52
  8  \w     46.00  95.00   0.50    1.08    --   85.25-115.00  29.38   98
  9  \w   -125.00 -99.00   0.50    1.08    --  -79.50-113.00  12.03   52
 10  \w    -93.00 -53.00   0.50    1.08    --  -69.71 121.00 178.00   80
 11  \w   -111.00 -78.00   0.50    1.08    --  -62.00 -47.00 -15.48   66
 12  \w    105.00 131.00   0.50    1.08    --   85.25 118.00 173.31   52
 13  \w    103.00 129.00   0.50    1.08    --   85.25 116.00-139.89   52
 14  \w    -97.00 -61.00   0.50    1.08    --  -46.00 -40.00  54.52   72
 15  \w     96.00 132.00   0.50    1.08    --   85.25 129.00 -67.85   72
 16  \w   -120.00 -94.00   0.50    1.08    --  -79.50 -64.00 136.72   52
 17  \w     42.00  76.00   0.50    1.08    --   85.25-100.00-117.71   68
 18  \w   -125.00-100.00   0.50    1.08    --  -78.00 -56.00   5.14   50
 19  \w    -88.00 -63.00   0.50    1.08    --  -76.30 121.00 178.00   50
 20  \w     -6.00  19.00   0.50    1.08    --  -10.00  78.00  39.20   50
 21  \w     46.00  71.00   0.50    1.08    --   85.25 -75.00  84.99   50
 22  \w     98.00 124.00   0.50    1.08    --   85.25  60.00 -57.09   52
 23  \w     99.00 125.00   0.50    1.08    --   85.25  59.00 -42.35   52
 24  \w     97.00 122.00   0.50    1.08    --   85.25  40.00  81.02   50
 25  \w     36.00  71.00   0.50    1.08    --   82.35-121.00  96.00   70
 26  \w     49.00  78.00   0.50    1.08    --   85.25 -77.00  27.08   58
 27  \w     50.00  78.00   0.50    1.08    --   85.25 -80.00 -98.90   56
 28  \w     48.00  73.00   0.50    1.08    --   85.25 -77.00 -86.78   50
 29  \w     35.00  60.00   0.50    1.08    --   71.06-121.00  96.00   50
 30  \w     45.00  71.00   0.50    1.08    --   85.25-126.00  83.98   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      -0.0494559000
_diffrn_orient_matrix_UB_12      -0.0312947000
_diffrn_orient_matrix_UB_13      0.0604474000
_diffrn_orient_matrix_UB_21      -0.0457250000
_diffrn_orient_matrix_UB_22      -0.0462293000
_diffrn_orient_matrix_UB_23      -0.0551896000
_diffrn_orient_matrix_UB_31      0.0505309000
_diffrn_orient_matrix_UB_32      -0.0722166000
_diffrn_orient_matrix_UB_33      0.0091786000
_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  0.0370
_diffrn_reflns_av_unetI/netI     0.0244
_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       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            39905
_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         70.071
_diffrn_reflns_theta_min         4.277
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.996
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.476
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.68a (Rigaku Oxford Diffraction, 2022) 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 light brown'
_exptl_crystal_density_diffrn    1.119
_exptl_crystal_description       plate
_exptl_crystal_F_000             2112
_exptl_crystal_preparation
;
 Crystalls were grown from saturated solution of Benzene. 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          0.440
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.160
_refine_diff_density_max         0.310
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         5478
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0509
_refine_ls_R_factor_gt           0.0443
_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^)+(0.0786P)^2^+1.5712P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1280
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4669
_reflns_number_total             5478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02457e2.cif
_cod_data_source_block           CoCz104_CoCz_a
_cod_depositor_comments
'Adding full bibliography for 7717294--7717301.cif.'
_cod_database_code               7717299
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.668
_shelx_estimated_absorpt_t_max   0.857
_shelx_res_checksum              59483
_shelx_hkl_checksum              86176