Ligand exchange at tetra-coordinated beryllium centres
Buchner, Magnus Richard; Cocic, Dusan; Ivlev, Sergei; Spang, Nils; Müller, Matthias; Puchta, Ralph; Dalton Transactions  (2023) –; doi:10.1039/D3DT00713H

data_7712665
_publ_section_title
;
 Ligand exchange at tetra-coordinated beryllium centres
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00713H
_journal_year                    2023
_chemical_formula_moiety         'C36 H66 Be2 Cl4 P2, 2(C6 D6)'
_chemical_formula_sum            'C48 H66 Be2 Cl4 D12 P2'
_chemical_formula_weight         889.0012
_chemical_melting_point          'non det.'
_chemical_name_common            'non det.'
_chemical_name_systematic        'Bis(tricyclohexyl)phosphine berylliumchloride'
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-03-22 deposited with the CCDC.	2023-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                69.384(3)
_cell_angle_beta                 82.093(4)
_cell_angle_gamma                71.718(4)
_cell_formula_units_Z            1
_cell_length_a                   8.3749(4)
_cell_length_b                   10.6551(5)
_cell_length_c                   15.0815(7)
_cell_measurement_reflns_used    15532
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      53.5
_cell_measurement_theta_min      2.9
_cell_volume                     1195.48(10)
_computing_cell_refinement       'X-Area v1.81 (Stoe, 2018)'
_computing_data_collection       'X-Area v1.81 (Stoe, 2018)'
_computing_data_reduction        'X-Area v1.81 (Stoe, 2018)'
_computing_molecular_graphics    'Diamond v4.5.2 (Brandenburg, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'image plate ( 34 cm diameter )'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_collimation    '0.5 mm, multiple pinhole'
_diffrn_radiation_monochromator  'planar graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0380
_diffrn_reflns_av_unetI/netI     0.0254
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15532
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.745
_diffrn_reflns_theta_min         1.443
_diffrn_source
'sealed X-ray tube, 12 x 0.4 mm long-fine focus'
_exptl_absorpt_coefficient_mu    0.346
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_meas      'non det.'
_exptl_crystal_description       column
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.421
_refine_diff_density_min         -0.154
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         5046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0273
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0411P)^2^+0.2876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0758
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4538
_reflns_number_total             5046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00713h2.cif
_cod_data_source_block           1_a
_cod_original_formula_sum        'C48 H66 Be2 Cl4 P2 D12'
_cod_database_code               7712665
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              92416
_shelx_hkl_checksum              53109