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_7717297
_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
'0.93 [C41 H63 Be N2 O P], 0.07 [C40 H63 Be N2 Br]'
_chemical_formula_sum            'C40.93 H63 Be Br0.07 N2 O0.93 P0.93'
_chemical_formula_weight         641.30
_chemical_name_systematic        '[(CAAC)(CAACH)Be(OCP)], 4a'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-07-01
_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                73.555(2)
_cell_angle_beta                 83.483(2)
_cell_angle_gamma                78.427(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8175(2)
_cell_length_b                   11.1664(3)
_cell_length_c                   18.8250(4)
_cell_measurement_reflns_used    18483
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.7790
_cell_measurement_theta_min      4.1860
_cell_volume                     1935.52(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.63a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.63a (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 0.993
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w    -95.00 -60.00   0.50    2.11    --  -46.00 -47.00 163.48   70
  2  \w   -103.00 -68.00   0.50    2.11    --  -54.00 -48.00  78.55   70
  3  \w     16.00  66.00   0.50    2.11    --   58.60 -95.00   0.00  100
  4  \w   -110.00 -75.00   0.50    2.11    --  -62.00 -51.00 -15.65   70
  5  \w   -114.00 -79.00   0.50    2.11    --  -66.00 -52.00-102.46   70
  6  \w   -117.00 -84.00   0.50    2.11    --  -70.00 -57.00-112.38   66
  7  \w   -117.00 -83.00   0.50    2.11    --  -70.00 -55.00 -54.63   68
  8  \w   -118.00 -83.00   0.50    2.11    --  -70.00 -54.00  68.59   70
  9  \w    -92.00 -31.00   0.50    2.11    --  -76.30 112.00  90.00  122
 10  \w    -92.00 -31.00   0.50    2.11    --  -76.30 112.00 -90.00  122
 11  \w   -130.00 -92.00   0.50    2.11    --  -79.50 -43.00 -49.61   76
 12  \w   -128.00 -93.00   0.50    2.11    --  -79.50 -50.00 166.84   70
 13  \w   -104.00 -33.00   0.50    2.11    --  -79.50 133.00 -17.73  142
 14  \w   -126.00 -91.00   0.50    2.11    --  -79.50 -59.00-156.33   70
 15  \w    -98.00 -33.00   0.50    2.11    --  -79.50 119.00 158.39  130
 16  \w   -130.00 -91.00   0.50    2.11    --  -79.50 -40.00  44.47   78
 17  \w   -126.00 -93.00   0.50    2.11    --  -79.50-120.00 156.91   66
 18  \w     36.00  98.00   0.50    2.11    --   82.00-115.00 -52.78  124
 19  \w     40.00  90.00   0.50    2.11    --   82.35 -95.00-180.00  100
 20  \w     40.00  90.00   0.50    2.11    --   82.35 -95.00  60.00  100
 21  \w     37.00  93.00   0.50    2.11    --   82.35-112.00-150.00  112
 22  \w     40.00  90.00   0.50    2.11    --   82.35 -95.00   0.00  100
 23  \w     37.00  93.00   0.50    2.11    --   82.35-112.00-120.00  112
 24  \w     46.00 133.00   0.50    2.11    --   82.35  15.00 -30.00  174
 25  \w     40.00  90.00   0.50    2.11    --   82.35 -95.00 -60.00  100
 26  \w     37.00  93.00   0.50    2.11    --   82.35-112.00   0.00  112
 27  \w     37.00  93.00   0.50    2.11    --   82.35-112.00  60.00  112
 28  \w     46.00 133.00   0.50    2.11    --   82.35  15.00 150.00  174
 29  \w     37.00  93.00   0.50    2.11    --   82.35-112.00  90.00  112
 30  \w     37.00  93.00   0.50    2.11    --   82.35-112.00 -30.00  112
 31  \w     40.00  90.00   0.50    2.11    --   82.35 -95.00-150.00  100
 32  \w     97.00 132.00   0.50    2.11    --   85.25 125.00-101.30   70
 33  \w     44.00  90.00   0.50    2.11    --   85.25 -91.00 -47.75   92
 34  \w     96.00 138.00   0.50    2.11    --   85.25  31.00 -67.56   84
 35  \w     91.00 132.00   0.50    2.11    --   85.25 136.00-147.12   82
 36  \w     39.00  97.00   0.50    2.11    --   85.25-115.00 141.22  116
 37  \w     67.00 136.00   0.50    2.11    --   85.25  18.00 -92.44  138
 38  \w     99.00 130.00   0.50    2.11    --   85.25  63.00-166.24   62
 39  \w     73.00 137.00   0.50    2.11    --   85.25  21.00-155.12  128
 40  \w     39.00  98.00   0.50    2.11    --   85.25-117.00  -7.41  118
 41  \w     42.00  93.00   0.50    2.11    --   85.25 -98.00 150.68  102
 42  \w     40.00 109.00   0.50    2.11    --   85.25-140.00  60.04  138
 43  \w     44.00  91.00   0.50    2.11    --   85.25 -92.00  25.67   94
 44  \w     39.00 108.00   0.50    2.11    --   85.25-139.00-156.70  138
 45  \w     97.00 131.00   0.50    2.11    --   85.25  61.00 113.78   68
 46  \w     41.00  92.00   0.50    2.11    --   85.25-100.00   9.43  102
 47  \w     43.00  92.00   0.50    2.11    --   85.25 -94.00-124.40   98
 48  \w     98.00 132.00   0.50    2.11    --   85.25 122.00 109.38   68
 49  \w     98.00 132.00   0.50    2.11    --   85.25 123.00 -15.84   68
 50  \w     97.00 136.00   0.50    2.11    --   85.25  39.00  22.95   78
 51  \w     39.00 100.00   0.50    2.11    --   85.25-123.00 -73.29  122
 52  \w     43.00  92.00   0.50    2.11    --   85.25 -94.00  93.09   98
 53  \w     25.00  54.00   0.50    2.11    --   14.00  61.00-126.70   58
 54  \w     30.00  56.00   0.50    2.11    --   18.00  60.00 -34.16   52
 55  \w     34.00  60.00   0.50    2.11    --   22.00  57.00  18.58   52
 56  \w     34.00  60.00   0.50    2.11    --   22.00  58.00  50.39   52
 57  \w    -79.00 -44.00   0.50    2.11    --  -30.00 -48.00  90.46   70
 58  \w   -121.00 -86.00   0.50    2.11    --  -74.00 -56.00  31.92   70
 59  \w   -121.00 -86.00   0.50    2.11    --  -74.00 -57.00 175.97   70
 60  \w   -121.00 -86.00   0.50    2.11    --  -74.00 -58.00-143.63   70
 61  \w   -122.00 -87.00   0.50    2.11    --  -74.00 -52.00 158.66   70
 62  \w   -121.00 -86.00   0.50    2.11    --  -74.00 -56.00 129.51   70
 63  \w   -121.00 -86.00   0.50    2.11    --  -74.00 -57.00 -66.78   70
 64  \w   -120.00 -86.00   0.50    2.11    --  -74.00 -59.00  22.19   68
 65  \w   -121.00 -86.00   0.50    2.11    --  -74.00 -56.00 139.10   70
 66  \w   -121.00 -86.00   0.50    2.11    --  -74.00 -55.00 117.17   70
 67  \w   -121.00 -86.00   0.50    2.11    --  -74.00 -58.00  58.61   70
 68  \w   -121.00 -86.00   0.50    2.11    --  -74.00 -58.00 -23.01   70
 69  \w   -129.00 -89.00   0.50    2.11    --  -78.00 -38.00  71.19   80
 70  \w   -125.00 -91.00   0.50    2.11    --  -79.50 -60.00  12.02   68
 71  \w   -130.00 -91.00   0.50    2.11    --  -79.50 -40.00  27.32   78
 72  \w   -102.00 -33.00   0.50    2.11    --  -79.50 132.00-161.86  138
 73  \w   -126.00 -91.00   0.50    2.11    --  -79.50-125.00-161.81   70
 74  \w   -125.00 -91.00   0.50    2.11    --  -79.50 -61.00 -63.94   68
 75  \w   -126.00 -92.00   0.50    2.11    --  -79.50-123.00  47.64   68
 76  \w   -125.00 -91.00   0.50    2.11    --  -79.50 -60.00-116.96   68
 77  \w   -125.00 -91.00   0.50    2.11    --  -79.50 -61.00 -85.25   68
 78  \w   -130.00 -91.00   0.50    2.11    --  -79.50 -41.00  64.08   78
 79  \w   -127.00 -90.00   0.50    2.11    --  -79.50-127.00 -48.16   74
 80  \w   -126.00 -88.00   0.50    2.11    --  -79.50-131.00  39.34   76
 81  \w   -124.00 -94.00   0.50    2.11    --  -79.50 -64.00 161.70   60
 82  \w   -125.00 -91.00   0.50    2.11    --  -79.50 -60.00-127.00   68
 83  \w   -125.00 -90.00   0.50    2.11    --  -79.50 -62.00 -32.75   70
 84  \w   -127.00 -89.00   0.50    2.11    --  -79.50-128.00-100.00   76
 85  \w   -124.00 -94.00   0.50    2.11    --  -79.50 -64.00 121.76   60
 86  \w     46.00 133.00   0.50    2.11    --   82.35  15.00  30.00  174
;
_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      -0.0453849000
_diffrn_orient_matrix_UB_12      -0.1306585000
_diffrn_orient_matrix_UB_13      0.0254838000
_diffrn_orient_matrix_UB_21      -0.1131882000
_diffrn_orient_matrix_UB_22      0.0492093000
_diffrn_orient_matrix_UB_23      0.0537039000
_diffrn_orient_matrix_UB_31      -0.1043020000
_diffrn_orient_matrix_UB_32      0.0432097000
_diffrn_orient_matrix_UB_33      -0.0614303000
_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  0.0645
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            62272
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.069
_diffrn_reflns_theta_min         4.194
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.42.63a (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 brown'
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       plate
_exptl_crystal_F_000             701
_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          0.120
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7274
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0474
_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^)+(0.0765P)^2^+0.5159P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1279
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5603
_reflns_number_total             7274
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02457e2.cif
_cod_data_source_block           CoCz087_CoCz_a
_cod_depositor_comments
'Adding full bibliography for 7717294--7717301.cif.'
_cod_database_code               7717297
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.899
_shelx_estimated_absorpt_t_max   0.982
_shelx_res_checksum              53990
_shelx_hkl_checksum              76478