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_1558013
_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_sum            'Be4 H51 I2 N19'
_chemical_formula_weight         607.43
_space_group_crystal_system      trigonal
_space_group_IT_number           143
_space_group_name_Hall           'P 3'
_space_group_name_H-M_alt        'P 3'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_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                120
_cell_formula_units_Z            1
_cell_length_a                   9.77560(10)
_cell_length_b                   9.77560(10)
_cell_length_c                   8.7186(2)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      154.18
_cell_measurement_theta_min      10.15
_cell_volume                     721.55(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4283
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.826
_diffrn_reflns_theta_min         5.073
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    17.294
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             306
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   0.1060
_exptl_transmission_factor_min   0.0301
_refine_diff_density_max         0.972
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.182
_refine_ls_abs_structure_details
;
 Flack x determined using 751 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.413(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1779
_refine_ls_number_restraints     13
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0903P)^2^+2.1179P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1277
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_full    0.981
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                1767
_reflns_number_total             1779
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01112f2.cif
_cod_data_source_block           5
_cod_depositor_comments
;Adding full bibliography for 1558013--1558021.cif.

 Adding full bibliography for 1558013--1558021.cif.
;
_cod_database_code               1558013
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              29904