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_7717294
_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_absolute_configuration unk
_chemical_formula_moiety         'C60 H92 Be N2 O4 P2, C5 H12'
_chemical_formula_sum            'C65 H104 Be N2 O4 P2'
_chemical_formula_weight         1048.45
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2024-10-09
_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                 93.364(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   30.9641(3)
_cell_length_b                   21.1528(4)
_cell_length_c                   9.8832(4)
_cell_measurement_reflns_used    9761
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.5600
_cell_measurement_theta_min      2.5610
_cell_volume                     6462.1(3)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
 List of Runs (angles in degrees, time in seconds):
 --------------------------------------------------------------------------
  1  \w     16.00  66.00   0.50    9.00    --   58.84 -95.00 120.00  100
  2  \w     38.00 109.00   0.50    9.00    --   58.84  15.00-120.00  142
  3  \w     20.00  87.00   0.50    9.00    --   58.84-126.00  60.00  134
  4  \w    -92.00 -31.00   0.50    9.00    --  -76.38 112.00 -90.00  122
  5  \w    -92.00 -31.00   0.50    9.00    --  -76.38 112.00 120.00  122
  6  \w   -127.00 -40.00   0.50    9.00    --  -76.38 -15.00 -30.00  174
  7  \w    -92.00 -31.00   0.50    9.00    --  -76.38 112.00 150.00  122
  8  \w   -127.00 -40.00   0.50    9.00    --  -76.38 -15.00 -90.00  174
  9  \w     40.00  90.00   0.50    9.00    --   82.25 -95.00 -90.00  100
 10  \w     40.00  90.00   0.50    9.00    --   82.25 -95.00  30.00  100
 11  \w     46.00 133.00   0.50    9.00    --   82.25  15.00 -60.00  174
 12  \w     37.00  93.00   0.50    9.00    --   82.25-112.00  30.00  112
 13  \w     37.00  93.00   0.50    9.00    --   82.25-112.00 -60.00  112
 14  \w     37.00  93.00   0.50    9.00    --   82.25-112.00-150.00  112
 15  \w     40.00  90.00   0.50    9.00    --   82.25 -95.00 120.00  100
 16  \w     40.00  90.00   0.50    9.00    --   82.25 -95.00  90.00  100
 17  \w     46.00 133.00   0.50    9.00    --   82.25  15.00-180.00  174
 18  \w     38.00 109.00   0.50    9.00    --   58.84  15.00 120.00  142
 19  \w    -97.00 -43.00   0.50    9.00    --  -69.79 126.00-180.00  108
;
_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      -0.0490632000
_diffrn_orient_matrix_UB_12      0.0062952000
_diffrn_orient_matrix_UB_13      0.0152006000
_diffrn_orient_matrix_UB_21      0.0001996000
_diffrn_orient_matrix_UB_22      -0.0626030000
_diffrn_orient_matrix_UB_23      0.0796621000
_diffrn_orient_matrix_UB_31      0.0088892000
_diffrn_orient_matrix_UB_32      0.0366732000
_diffrn_orient_matrix_UB_33      0.1334543000
_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  0.0419
_diffrn_reflns_av_unetI/netI     0.0378
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            32506
_diffrn_reflns_point_group_measured_fraction_full 0.880
_diffrn_reflns_point_group_measured_fraction_max 0.870
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.073
_diffrn_reflns_theta_min         2.531
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet-R X-ray Source'
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75377
_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            brown
_exptl_crystal_density_diffrn    1.078
_exptl_crystal_description       plate
_exptl_crystal_F_000             2296
_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          0.118
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.004(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         32506
_refine_ls_number_restraints     542
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0706
_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^)+(0.1515P)^2^] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.2047
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    0.761
_reflns_Friedel_fraction_max     0.743
_reflns_number_gt                25203
_reflns_number_total             32506
_reflns_threshold_expression     'I > 2\s(I)'
_twin_dimensionality             triperiodic
_twin_formation_mechanism        gt
_twin_morphology                 polysynthetic
_twin_special_details
;
 Component 2 rotated by 179.6553\% 
 around [-0.00 1.00 0.02] (reciprocal) or [0.00 1.00 0.10] (direct)
 Component 3 rotated by 1.7901\% 
 around [0.99 0.10 0.04] (reciprocal) or [0.85 0.18 0.50] (direct)
;
_cod_data_source_file            d4dt02457e2.cif
_cod_data_source_block           CoCz129_CoCz_twin1_hklf5
_cod_depositor_comments
'Adding full bibliography for 7717294--7717301.cif.'
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               7717294
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.897
_shelx_estimated_absorpt_t_max   0.953
_shelx_res_checksum              68054
_shelx_hkl_checksum              58745