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_7717300
_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         'C29 H48 Be N O3 P'
_chemical_formula_sum            'C29 H48 Be N O3 P'
_chemical_formula_weight         498.66
_chemical_name_systematic        '[(THF)2(CAACH)Be(OCP)], 3'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-07-25
_audit_creation_method           'CIF-fill 1.5c (K.Radacki, 2005-23)'
_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            24
_cell_length_a                   61.1639(3)
_cell_length_b                   15.54960(10)
_cell_length_c                   18.65630(10)
_cell_measurement_reflns_used    83720
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.8180
_cell_measurement_theta_min      2.8660
_cell_volume                     17743.53(17)
_computing_cell_refinement       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.72a (Rigaku OD, 2022)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     16.00  65.02   0.38    0.50    --   58.57 -95.00 -81.00  129
  2  \w    -68.00 -17.84   0.38    0.50    --  -60.16  95.00  28.00  132
  3  \w    -77.00 -27.98   0.38    0.50    --  -69.76  95.00  28.00  129
  4  \w     29.00  78.02   0.38    0.50    --   71.34 -95.00 -81.00  129
  5  \w    -84.00 -33.84   0.38    0.50    --  -76.35  95.00  28.00  132
  6  \w     40.00  89.02   0.38    0.50    --   82.28 -95.00 -81.00  129
  7  \w     16.00  65.02   0.38    0.50    --   58.57 -95.00 150.00  129
  8  \w     16.00  65.02   0.38    0.50    --   58.57 -95.00-180.00  129
  9  \w   -110.00 -31.72   0.38    0.50    --  -60.16 -15.00-180.00  206
 10  \w     29.00  78.02   0.38    0.50    --   71.34 -95.00 -30.00  129
 11  \w     29.00  78.02   0.38    0.50    --   71.34 -95.00-150.00  129
 12  \w    -92.00 -31.96   0.38    0.50    --  -76.35 112.00  90.00  158
 13  \w   -127.00 -41.12   0.38    0.50    --  -76.35 -15.00 150.00  226
 14  \w     37.00  91.72   0.38    0.50    --   82.28-112.00  90.00  144
 15  \w     37.00  91.72   0.38    0.50    --   82.28-112.00 -30.00  144
 16  \w     37.00  91.72   0.38    0.50    --   82.28-112.00-180.00  144
 17  \w     37.00  91.72   0.38    0.50    --   82.28-112.00   0.00  144
 18  \w     43.00  69.22   0.38    0.50    --   82.28 -95.00  60.00   69
 19  \w     44.00  73.26   0.38    0.50    --   82.28 -95.00-180.00   77
 20  \w     52.00 122.30   0.38    0.50    --   82.28  15.00  90.00  185
 21  \w     40.00  85.22   0.38    0.50    --   82.28 -95.00-150.00  119
 22  \w     48.00  83.34   0.38    0.50    --   82.28 -95.00  90.00   93
;
_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      -0.0132246000
_diffrn_orient_matrix_UB_12      0.0824939000
_diffrn_orient_matrix_UB_13      -0.0145467000
_diffrn_orient_matrix_UB_21      -0.0096527000
_diffrn_orient_matrix_UB_22      -0.0411746000
_diffrn_orient_matrix_UB_23      -0.0680887000
_diffrn_orient_matrix_UB_31      -0.0191509000
_diffrn_orient_matrix_UB_32      -0.0362041000
_diffrn_orient_matrix_UB_33      0.0443798000
_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  0.0339
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       67
_diffrn_reflns_limit_h_min       -74
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            161661
_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         70.076
_diffrn_reflns_theta_min         2.890
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.72a (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 colourless'
_exptl_crystal_density_diffrn    1.120
_exptl_crystal_description       block
_exptl_crystal_F_000             6528
_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          0.440
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.692
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1239
_refine_ls_number_reflns         16840
_refine_ls_number_restraints     1339
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0463
_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^)+(0.0590P)^2^+10.6811P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1227
_refine_ls_wR_factor_ref         0.1252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15374
_reflns_number_total             16840
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02457e2.cif
_cod_data_source_block           CoCz134_CoCz_a
_cod_depositor_comments
'Adding full bibliography for 7717294--7717301.cif.'
_cod_database_code               7717300
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.660
_shelx_estimated_absorpt_t_max   0.922
_shelx_res_checksum              87538
_shelx_hkl_checksum              77094