#------------------------------------------------------------------------------
#$Date: 2020-10-06 10:38:37 +0300 (Tue, 06 Oct 2020) $
#$Revision: 257400 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558017.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1558017
loop_
_publ_author_name
'Müller, Matthias'
'Karttunen, Antti J.'
'Buchner, Magnus R.'
_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         '[Be4(NH2)6(NH3)4]2I6(NH3)'
_chemical_formula_sum            'Be4 H42 I2 N16'
_chemical_formula_weight         556.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                 112.2170(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0852(2)
_cell_length_b                   10.17190(10)
_cell_length_c                   18.4646(2)
_cell_measurement_reflns_used    39920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      152.92
_cell_measurement_theta_min      10.35
_cell_volume                     2449.08(5)
_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 0.998
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21462
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.696
_diffrn_reflns_theta_min         5.175
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    20.295
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             1104
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_transmission_factor_max   0.0089
_exptl_transmission_factor_min   0.0003
_refine_diff_density_max         1.605
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.00068(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         2547
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0343
_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/[σ²(Fo²)+(0.0689P)²+3.9091P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0886
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2518
_reflns_number_total             2547
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc01112f2.cif
_cod_data_source_block           6
_cod_depositor_comments
;Adding full bibliography for 1558013--1558021.cif.

 Adding full bibliography for 1558013--1558021.cif.
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               1558017
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Be1 Be 0.4021(2) 0.5935(3) 0.25341(18) 0.0152(6) Uani 1 1 d . . . . .
Be2 Be 0.5456(3) 0.7889(4) 0.3322(2) 0.0172(6) Uani 1 1 d . . . . .
I1 I 0.54487(2) 0.76760(2) 0.59443(2) 0.02094(13) Uani 1 1 d . . . . .
N1 N 0.35734(16) 0.6885(2) 0.17052(13) 0.0178(4) Uani 1 1 d . . . . .
H1A H 0.3036 0.7382 0.1705 0.021 Uiso 1 1 calc R U . . .
H1B H 0.3350 0.6360 0.1274 0.021 Uiso 1 1 calc R U . . .
N2 N 0.44771(16) 0.6917(2) 0.33529(12) 0.0165(4) Uani 1 1 d . . . . .
H2A H 0.3961 0.7432 0.3376 0.020 Uiso 1 1 calc R U . . .
H2B H 0.4708 0.6406 0.3790 0.020 Uiso 1 1 calc R U . . .
N3 N 0.5000 0.8865(3) 0.2500 0.0177(6) Uani 1 2 d S T P . .
H3A H 0.5512 0.9390 0.2479 0.021 Uiso 0.5 1 calc R U P . .
H3B H 0.4488 0.9390 0.2521 0.021 Uiso 0.5 1 calc R U P . .
N4 N 0.5000 0.4965(3) 0.2500 0.0157(6) Uani 1 2 d S T P . .
H4A H 0.4765 0.4441 0.2069 0.019 Uiso 0.5 1 calc R U P . .
H4B H 0.5235 0.4441 0.2931 0.019 Uiso 0.5 1 calc R U P . .
N5 N 0.30204(16) 0.4918(2) 0.25973(12) 0.0174(4) Uani 1 1 d . . . . .
H5A H 0.2610 0.5404 0.2774 0.026 Uiso 1 1 calc R U . . .
H5B H 0.3300 0.4243 0.2934 0.026 Uiso 1 1 calc R U . . .
H5C H 0.2642 0.4589 0.2116 0.026 Uiso 1 1 calc R U . . .
N6 N 0.40822(18) 0.8909(3) 0.08252(13) 0.0205(5) Uani 1 1 d . . . . .
H6A H 0.3428 0.9165 0.0735 0.031 Uiso 1 1 calc R U . . .
H6B H 0.4094 0.8450 0.0406 0.031 Uiso 1 1 calc R U . . .
H6C H 0.4490 0.9631 0.0902 0.031 Uiso 1 1 calc R U . . .
N7 N 0.18421(19) 0.4064(3) 0.08284(14) 0.0231(5) Uani 1 1 d . . . . .
N8 N 0.1618(2) 0.6722(3) 0.31711(16) 0.0243(5) Uani 1 1 d . . . . .
N9 N 0.8269(2) 1.0159(3) 0.47837(19) 0.0319(6) Uani 1 1 d . . . . .
H1 H 0.156(4) 0.476(5) 0.089(3) 0.042(12) Uiso 1 1 d . . . . .
H2 H 0.137(3) 0.351(5) 0.049(3) 0.036(11) Uiso 1 1 d . . . . .
H3 H 0.228(3) 0.420(5) 0.061(3) 0.038(11) Uiso 1 1 d . . . . .
H4 H 0.126(4) 0.690(6) 0.265(3) 0.056(14) Uiso 1 1 d . . . . .
H5 H 0.114(3) 0.666(5) 0.338(2) 0.037(11) Uiso 1 1 d . . . . .
H6 H 0.200(3) 0.736(4) 0.333(3) 0.018(10) Uiso 1 1 d . . . . .
H7 H 0.802(5) 1.054(8) 0.442(4) 0.09(2) Uiso 1 1 d . . . . .
H8 H 0.852(3) 0.955(5) 0.470(2) 0.029(10) Uiso 1 1 d . . . . .
H9 H 0.873(3) 1.073(4) 0.510(3) 0.032(10) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Be Be 0.0038 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Be1 N4 108.67(19) . . ?
N1 Be1 N2 110.3(2) . . ?
N4 Be1 N2 109.12(19) . . ?
N1 Be1 N5 110.58(19) . . ?
N4 Be1 N5 109.5(2) . . ?
N2 Be1 N5 108.68(19) . . ?
N2 Be2 N3 109.0(2) . . ?
N2 Be2 N1 108.4(2) . 2_655 ?
N3 Be2 N1 110.6(2) . 2_655 ?
N2 Be2 N6 109.5(2) . 2_655 ?
N3 Be2 N6 109.3(2) . 2_655 ?
N1 Be2 N6 109.9(2) 2_655 2_655 ?
Be1 N1 Be2 109.4(2) . 2_655 ?
Be1 N1 H1A 109.8 . . ?
Be2 N1 H1A 109.8 2_655 . ?
Be1 N1 H1B 109.8 . . ?
Be2 N1 H1B 109.8 2_655 . ?
H1A N1 H1B 108.2 . . ?
Be2 N2 Be1 110.0(2) . . ?
Be2 N2 H2A 109.7 . . ?
Be1 N2 H2A 109.7 . . ?
Be2 N2 H2B 109.7 . . ?
Be1 N2 H2B 109.7 . . ?
H2A N2 H2B 108.2 . . ?
Be2 N3 Be2 109.5(3) . 2_655 ?
Be2 N3 H3A 109.8 . . ?
Be2 N3 H3A 109.8 2_655 . ?
Be2 N3 H3B 109.8 . . ?
Be2 N3 H3B 109.8 2_655 . ?
H3A N3 H3B 108.2 . . ?
Be1 N4 Be1 109.8(3) . 2_655 ?
Be1 N4 H4A 109.7 . . ?
Be1 N4 H4A 109.7 2_655 . ?
Be1 N4 H4B 109.7 . . ?
Be1 N4 H4B 109.7 2_655 . ?
H4A N4 H4B 108.2 . . ?
Be1 N5 H5A 109.5 . . ?
Be1 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
Be1 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
Be2 N6 H6A 109.5 2_655 . ?
Be2 N6 H6B 109.5 2_655 . ?
H6A N6 H6B 109.5 . . ?
Be2 N6 H6C 109.5 2_655 . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
H1 N7 H2 111(4) . . ?
H1 N7 H3 112(4) . . ?
H2 N7 H3 104(4) . . ?
H4 N8 H5 105(4) . . ?
H4 N8 H6 104(5) . . ?
H5 N8 H6 113(4) . . ?
H7 N9 H8 110(6) . . ?
H7 N9 H9 103(6) . . ?
H8 N9 H9 113(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Be1 N1 1.716(4) . ?
Be1 N4 1.716(4) . ?
Be1 N2 1.721(4) . ?
Be1 N5 1.787(4) . ?
Be2 N2 1.715(4) . ?
Be2 N3 1.722(4) . ?
Be2 N1 1.723(4) 2_655 ?
Be2 N6 1.791(4) 2_655 ?
N1 Be2 1.722(4) 2_655 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N3 Be2 1.722(4) 2_655 ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N4 Be1 1.716(4) 2_655 ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 H5C 0.9100 . ?
N6 Be2 1.791(4) 2_655 ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
N6 H6C 0.9100 . ?
N7 H1 0.84(5) . ?
N7 H2 0.91(5) . ?
N7 H3 0.87(5) . ?
N8 H4 0.93(6) . ?
N8 H5 0.89(4) . ?
N8 H6 0.83(4) . ?
N9 H7 0.74(8) . ?
N9 H8 0.76(5) . ?
N9 H9 0.90(5) . ?
