Speciation of Be2+ in acidic liquid ammonia and formation of tetra- and octanuclear beryllium amido clusters
Müller, Matthias; Karttunen, Antti J.; Buchner, Magnus R.; Chemical Science 11 (2020) 5415–5422; doi:10.1039/D0SC01112F

data_1558021
_publ_section_title
;
 Speciation of Be2+ in acidic liquid ammonia and formation of tetra- and
 octanuclear beryllium amido clusters
;
_journal_issue                   21
_journal_name_full               'Chemical Science'
_journal_page_first              5415
_journal_page_last               5422
_journal_paper_doi               10.1039/D0SC01112F
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C45 H69 Be8 I2 N21 O + 5(C5H5N)'
_chemical_formula_sum            'C20 H44 Be8 I2 N16 O'
_chemical_formula_weight         850.59
_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_Hall           '-C 2 2c'
_space_group_name_H-M_alt        'C c c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-06 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.1994(2)
_cell_length_b                   21.2118(2)
_cell_length_c                   23.3361(3)
_cell_measurement_reflns_used    73657
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      152.20
_cell_measurement_theta_min      6.04
_cell_volume                     9998.72(19)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            72530
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.241
_diffrn_reflns_theta_min         3.021
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    10.116
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   0.3520
_exptl_transmission_factor_min   0.0913
_refine_diff_density_max         0.530
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         5329
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0270
_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^)+(0.0371P)^2^+25.2398P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0732
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4864
_reflns_number_total             5329
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01112f2.cif
_cod_data_source_block           6_sq
_cod_depositor_comments
;Adding full bibliography for 1558013--1558021.cif.

 Adding full bibliography for 1558013--1558021.cif.
;
_cod_database_code               1558021
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              97262
_shelx_fab_checksum              38203