#------------------------------------------------------------------------------
#$Date: 2025-08-19 00:06:14 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301780 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/80/1558019.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_1558019
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_sum            'C8 H16 Be N6'
_chemical_formula_weight         205.28
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.9478(3)
_cell_length_b                   9.9478(3)
_cell_length_c                   5.4077(3)
_cell_measurement_reflns_used    4208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      151.23
_cell_measurement_theta_min      12.58
_cell_volume                     535.14(4)
_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 0.989
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_number            3136
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.716
_diffrn_reflns_theta_min         6.292
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_description       block
_exptl_crystal_F_000             220
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.148
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0651P)²+0.0470P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0954
_refine_ls_wR_factor_ref         0.0996
_reflns_Friedel_coverage         0.552
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                484
_reflns_number_total             555
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc01112f2.cif
_cod_data_source_block           4
_cod_depositor_comments
;Adding full bibliography for 1558013--1558021.cif.

 Adding full bibliography for 1558013--1558021.cif.
;
_cod_database_code               1558019
_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.
;
_shelx_res_file
;

    4.res created by SHELXL-2014/7


TITL 1_a.res in P4(2)2(1)2
REM Old TITL 1 in P4(2)2(1)2
REM SHELXT solution in P4(2)2(1)2
REM R1 0.101,  Rweak 0.011,  Alpha 0.002,  Orientation as input
REM Flack x =  0.406 ( 0.972 ) from Parsons' quotients
REM Formula found by SHELXT:  C8 Be N6
CELL  1.54178   9.9478   9.9478   5.4077   90.000   90.000   90.000
ZERR    2.000   0.0003   0.0003   0.0003    0.000    0.000    0.000
LATT -1
SYMM -X, -Y, Z
SYMM 1/2-Y, 1/2+X, 1/2+Z
SYMM 1/2+Y, 1/2-X, 1/2+Z
SYMM 1/2-X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, 1/2-Z
SYMM Y, X, -Z
SYMM -Y, -X, -Z
SFAC C H BE N
UNIT 16 32 2 12
L.S. 10
BOND $H
LIST 4
ACTA
TEMP -173.15
FMAP 2
PLAN 20
REM EXTI 0.000000
TWIN
HTAB
WGHT    0.065100    0.047000
BASF   0.19878
FVAR       2.03515
N1    4    0.358585    0.515315    0.329207    11.00000    0.02348    0.02299 =
         0.01927   -0.00119   -0.00030   -0.00149
H1    2    0.336494    0.454976    0.215490    11.00000    0.03079
BE1   3    0.500000    0.500000    0.500000    10.25000    0.02084    0.02084 =
         0.01971    0.00000    0.00000    0.00027
C1    1    0.272805    0.614127    0.341450    11.00000    0.02006    0.02270 =
         0.01915    0.00583    0.00422   -0.00383
N2    4    0.280014    0.719986    0.500000    10.50000    0.02157    0.02157 =
         0.02456    0.00320    0.00320    0.00111
C2    1    0.153524    0.615766    0.170325    11.00000    0.02146    0.02973 =
         0.02874    0.00389   -0.00051   -0.00039
AFIX 137
H2A   2    0.085784    0.678390    0.233904    11.00000   -1.50000
H2B   2    0.114879    0.525311    0.160312    11.00000   -1.50000
H2C   2    0.182230    0.644663    0.005317    11.00000   -1.50000
REM #####
AFIX   0
HKLF 4

REM  1_a.res in P4(2)2(1)2
REM R1 =  0.0369 for     484 Fo > 4sig(Fo)  and  0.0443 for all     555 data
REM     42 parameters refined using      0 restraints

END

WGHT      0.0651      0.0470

REM No hydrogen bonds found for HTAB generation

REM Highest difference peak  0.148,  deepest hole -0.147,  1-sigma level  0.039
Q1    1   0.2974  0.5512  0.4156  11.00000  0.05    0.15
Q2    1   0.4245  0.4997  0.4252  11.00000  0.05    0.14
Q3    1   0.3084  0.7091  0.5561  11.00000  0.05    0.14
Q4    1   0.1012  0.7076  0.1303  11.00000  0.05    0.13
Q5    1   0.1745  0.6912  0.5734  11.00000  0.05    0.13
Q6    1   0.2085  0.7780  0.5548  11.00000  0.05    0.12
Q7    1   0.2055  0.6166  0.2545  11.00000  0.05    0.11
Q8    1   0.0773  0.6323  0.2524  11.00000  0.05    0.10
Q9    1   0.1380  0.5164  0.0424  11.00000  0.05    0.10
Q10   1   0.1581  0.7473 -0.0295  11.00000  0.05    0.10
Q11   1   0.4479  0.5521  0.0000  10.50000  0.05    0.10
Q12   1   0.2243  0.3599  0.1545  11.00000  0.05    0.09
Q13   1   0.3453  0.5841  0.2561  11.00000  0.05    0.09
Q14   1   0.0358  0.7317  0.3739  11.00000  0.05    0.09
Q15   1   0.2866  0.4184 -0.0067  11.00000  0.05    0.09
Q16   1   0.2030  0.5866  0.0260  11.00000  0.05    0.09
Q17   1   0.2976  0.3165  0.3070  11.00000  0.05    0.09
Q18   1   0.3527  0.3603  0.0935  11.00000  0.05    0.08
Q19   1   0.1310  0.7967  0.0816  11.00000  0.05    0.07
Q20   1   0.3576  0.7767  0.5115  11.00000  0.05    0.07
;
_shelx_res_checksum              5535
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y, x, -z'
'-y, -x, -z'
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
N1 N 0.35858(15) 0.51531(17) 0.3292(3) 0.0219(5) Uani 1 1 d . . . . .
H1 H 0.336(3) 0.455(3) 0.215(5) 0.031(7) Uiso 1 1 d . . . . .
Be1 Be 0.5000 0.5000 0.5000 0.0205(10) Uani 1 4 d S T P . .
C1 C 0.27281(19) 0.61413(18) 0.3414(4) 0.0206(5) Uani 1 1 d . . . . .
N2 N 0.28001(16) 0.71999(16) 0.5000 0.0226(6) Uani 1 2 d S T P . .
C2 C 0.1535(2) 0.6158(2) 0.1703(5) 0.0266(5) Uani 1 1 d . . . . .
H2A H 0.0858 0.6784 0.2339 0.040 Uiso 1 1 calc R U . . .
H2B H 0.1149 0.5253 0.1603 0.040 Uiso 1 1 calc R U . . .
H2C H 0.1822 0.6447 0.0053 0.040 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0235(9) 0.0230(9) 0.0193(9) -0.0012(8) -0.0003(8) -0.0015(6)
Be1 0.0208(14) 0.0208(14) 0.020(2) 0.000 0.000 0.0003(19)
C1 0.0201(9) 0.0227(9) 0.0191(9) 0.0058(8) 0.0042(9) -0.0038(7)
N2 0.0216(7) 0.0216(7) 0.0246(12) 0.0032(7) 0.0032(7) 0.0011(9)
C2 0.0215(10) 0.0297(10) 0.0287(11) 0.0039(11) -0.0005(11) -0.0004(8)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Be Be 0.0038 0.0014 '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'
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
C1 N1 Be1 125.82(15) . . ?
C1 N1 H1 112.5(17) . . ?
Be1 N1 H1 121.6(17) . . ?
N1 Be1 N1 98.55(12) . 8_666 ?
N1 Be1 N1 113.73(12) . 2_665 ?
N1 Be1 N1 116.67(11) 8_666 2_665 ?
N1 Be1 N1 116.67(11) . 7_556 ?
N1 Be1 N1 113.73(12) 8_666 7_556 ?
N1 Be1 N1 98.55(12) 2_665 7_556 ?
N1 C1 N2 125.56(19) . . ?
N1 C1 C2 119.55(19) . . ?
N2 C1 C2 114.89(18) . . ?
C1 N2 C1 118.6(2) 8_666 . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
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
N1 C1 1.303(2) . ?
N1 Be1 1.6897(17) . ?
N1 H1 0.89(3) . ?
Be1 N1 1.6898(17) 8_666 ?
Be1 N1 1.6898(17) 2_665 ?
Be1 N1 1.6898(17) 7_556 ?
C1 N2 1.360(2) . ?
C1 C2 1.505(3) . ?
N2 C1 1.360(2) 8_666 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168306374
