Multinuclear beryllium amide and imide complexes: structure, properties and bonding.
Bekiş, Deniz F; Thomas-Hargreaves, Lewis R; Ivlev, Sergei I.; Buchner, Magnus R.; Dalton transactions (Cambridge, England : 2003) 53 (2024) 15551–15564; doi:10.1039/d4dt02269f

data_7716900
_publ_section_title
;
 Multinuclear beryllium amide and imide complexes: structure, properties
 and bonding.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15551
_journal_page_last               15564
_journal_paper_doi               10.1039/d4dt02269f
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C54 H72 Be3 N6, C6 H6'
_chemical_formula_sum            'C60 H78 Be3 N6'
_chemical_formula_weight         910.31
_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   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2019/1
_audit_update_record
;
2024-07-23 deposited with the CCDC.	2024-08-27 downloaded from the CCDC.
;
_cell_angle_alpha                63.743(8)
_cell_angle_beta                 71.969(9)
_cell_angle_gamma                72.777(8)
_cell_formula_units_Z            2
_cell_length_a                   14.2365(15)
_cell_length_b                   14.6407(15)
_cell_length_c                   15.7210(18)
_cell_measurement_reflns_used    20991
_cell_measurement_temperature    100
_cell_measurement_theta_max      75.93
_cell_measurement_theta_min      2.95
_cell_volume                     2745.2(6)
_computing_cell_refinement
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_data_reduction
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_publication_material
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image
processing, for the correction and scaling of reflection intensities and
for outlier rejection, version 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_diffrn_ambient_temperature      100
_diffrn_detector                 Pilatus300K
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_details      ' 5283 frames, detector distance = 60 mm'
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter'
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            67425
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        67.686
_diffrn_reflns_theta_max         76.230
_diffrn_reflns_theta_min         3.205
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.476
_exptl_absorpt_correction_T_max  0.9137
_exptl_absorpt_correction_T_min  0.2940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.201
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.00201(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     927
_refine_ls_number_reflns         11226
_refine_ls_number_restraints     2052
_refine_ls_restrained_S_all      0.838
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0733P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1377
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6113
_reflns_number_total             11226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02269f2.cif
_cod_data_source_block           LTH473
_cod_depositor_comments
'Adding full bibliography for 7716897--7716901.cif.'
_cod_database_code               7716900
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_min   0.911
_shelx_estimated_absorpt_t_max   0.954
_shelx_res_checksum              61671
_shelx_hkl_checksum              21815