#------------------------------------------------------------------------------
#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/43/7124317.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_7124317
loop_
_publ_author_name
'Müller, Matthias'
'Buchner, Magnus Richard'
_publ_section_title
;
 Preparation and Crystal Structures of the Beryllium Ammines [Be(NH3)4]X2
 (X = Br, I, CN, SCN, N3) and Be(NH3)2X’2 (X’ = Cl, Br, I).
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC07712J
_journal_year                    2019
_chemical_formula_moiety         'Be Cl2 H6 N2'
_chemical_formula_sum            'Be Cl2 H6 N2'
_chemical_formula_weight         113.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-09-26 deposited with the CCDC.    2019-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.321(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5519(2)
_cell_length_b                   11.8065(3)
_cell_length_c                   6.6589(2)
_cell_measurement_reflns_used    14658
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      158.15
_cell_measurement_theta_min      15.00
_cell_volume                     506.76(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_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  0.0323
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            8180
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.689
_diffrn_reflns_theta_min         7.504
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    10.140
_exptl_absorpt_correction_T_max  0.5133
_exptl_absorpt_correction_T_min  0.0736
_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(μ₂-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    1.494
_exptl_crystal_description       block
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.0045(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1092
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.097
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0338
_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/[σ²(Fo²)+(0.0672P)²+0.1590P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0957
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1005
_reflns_number_total             1092
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc07712j2.cif
_cod_data_source_block           4_CCDC2
_cod_database_code               7124317
_shelx_shelxl_version_number     2018/3
_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
;
TITL 1_a.res in P2(1)/n
    4.res
    created by SHELXL-2018/3 at 11:15:04 on 04-Feb-2019
REM Old TITL 1 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.135, Rweak 0.003, Alpha 0.006
REM <I/s>   0.817 for   59 systematic absences,  Orientation as input
REM Formula found by SHELXT:  N3 Br2
CELL  1.54178   6.5519  11.8065   6.6589   90.000  100.321   90.000
ZERR    4.000   0.0002   0.0003   0.0002    0.000    0.003    0.000
LATT  1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC BE H N Cl
UNIT 4 24 8 8
L.S. 10
BOND
LIST 4
ACTA
HTAB
EQIV $1 x-1/2, -y+3/2, z-1/2
HTAB N1 Cl2_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB N1 Cl1_$2
EQIV $3 -x+2, -y+1, -z+1
HTAB N1 Cl1_$3
EQIV $4 x-1/2, -y+3/2, z+1/2
HTAB N2 Cl2_$4
HTAB N2 Cl2_$1
HTAB N2 Cl1_$1
HTAB N2 Cl1_$2
TEMP -173.15
FMAP 2
PLAN 20
WGHT    0.067200    0.159000
EXTI    0.004531
FVAR       0.93458
CL1   4    0.787682    0.543335    0.712814    11.00000    0.02417    0.02613 =
         0.03218    0.00155    0.00330    0.00088
CL2   4    0.940673    0.752999    0.433300    11.00000    0.02798    0.02922 =
         0.03310   -0.00103    0.00463   -0.00613
N1    3    0.712569    0.544276    0.244589    11.00000    0.02515    0.02647 =
         0.03229   -0.00012    0.00218   -0.00069
N2    3    0.486397    0.700129    0.442110    11.00000    0.02605    0.02819 =
         0.03080    0.00090    0.00404    0.00126
BE1   1    0.721308    0.634711    0.448779    11.00000    0.02259    0.02614 =
         0.03276   -0.00112    0.00384   -0.00026
H1    2    0.828399    0.512034    0.249261    11.00000    0.04073
H2    2    0.624304    0.494934    0.246427    11.00000    0.04080
H3    2    0.680336    0.576258    0.136223    11.00000    0.03009
H4    2    0.383986    0.656993    0.407211    11.00000    0.04967
H5    2    0.457907    0.762892    0.366041    11.00000    0.03982
H6    2    0.473383    0.724301    0.549641    11.00000    0.04167
HKLF 4




REM  1_a.res in P2(1)/n
REM wR2 = 0.0957, GooF = S = 1.097, Restrained GooF = 1.097 for all data
REM R1 = 0.0338 for 1005 Fo > 4sig(Fo) and 0.0368 for all 1092 data
REM 71 parameters refined using 0 restraints

END

WGHT      0.0672      0.1590

REM Instructions for potential hydrogen bonds
HTAB N1 Cl1_$3
HTAB N1 Cl1_$2
HTAB N1 Cl2_$1
HTAB N2 Cl1_$2
HTAB N2 Cl1_$1
HTAB N2 Cl2_$1
HTAB N2 Cl2_$4

REM Highest difference peak  0.316,  deepest hole -0.376,  1-sigma level  0.080
Q1    1   0.7206  0.5835  0.3518  11.00000  0.05    0.32
Q2    1   0.7457  0.4453  0.7624  11.00000  0.05    0.28
Q3    1   0.5865  0.7619  0.5828  11.00000  0.05    0.27
Q4    1   1.0078  0.7281  0.6427  11.00000  0.05    0.26
Q5    1   0.7842  0.4511  0.2133  11.00000  0.05    0.26
Q6    1   0.3536  0.5652  0.3433  11.00000  0.05    0.26
Q7    1   0.5889  0.6872  0.4638  11.00000  0.05    0.26
Q8    1   0.9161  0.6807  0.4666  11.00000  0.05    0.25
Q9    1   0.8481  0.4450  0.3963  11.00000  0.05    0.24
Q10   1   0.4357  0.8158  0.4583  11.00000  0.05    0.24
Q11   1   0.7482  0.5030  0.4867  11.00000  0.05    0.22
Q12   1   0.9022  0.4654  0.8437  11.00000  0.05    0.21
Q13   1   0.4478  0.7964  0.6999  11.00000  0.05    0.21
Q14   1   0.4995  0.7193  0.7023  11.00000  0.05    0.21
Q15   1   1.0921  0.7663  0.2986  11.00000  0.05    0.21
Q16   1   0.7729  0.6146  0.9177  11.00000  0.05    0.21
Q17   1   0.7222  0.4686  0.9048  11.00000  0.05    0.20
Q18   1   0.5823  0.6223  0.6726  11.00000  0.05    0.20
Q19   1   0.4342  0.6466  0.7428  11.00000  0.05    0.19
Q20   1   0.6653  0.4939  0.8191  11.00000  0.05    0.19
;
_shelx_res_checksum              11658
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Cl1 Cl 0.78768(6) 0.54333(4) 0.71281(7) 0.0277(2) Uani 1 1 d
Cl2 Cl 0.94067(7) 0.75300(4) 0.43330(7) 0.0302(2) Uani 1 1 d
N1 N 0.7126(3) 0.54428(15) 0.2446(3) 0.0283(4) Uani 1 1 d
N2 N 0.4864(3) 0.70013(15) 0.4421(3) 0.0285(4) Uani 1 1 d
Be1 Be 0.7213(4) 0.6347(2) 0.4488(4) 0.0273(5) Uani 1 1 d
H1 H 0.828(5) 0.512(3) 0.249(5) 0.041(7) Uiso 1 1 d
H2 H 0.624(5) 0.495(3) 0.246(4) 0.041(7) Uiso 1 1 d
H3 H 0.680(4) 0.576(2) 0.136(5) 0.030(6) Uiso 1 1 d
H4 H 0.384(5) 0.657(3) 0.407(5) 0.050(8) Uiso 1 1 d
H5 H 0.458(5) 0.763(3) 0.366(5) 0.040(7) Uiso 1 1 d
H6 H 0.473(5) 0.724(3) 0.550(5) 0.042(8) Uiso 1 1 d
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
Cl1 0.0242(3) 0.0261(3) 0.0322(3) 0.00155(15) 0.00330(18) 0.00088(15)
Cl2 0.0280(3) 0.0292(3) 0.0331(3) -0.00103(16) 0.00463(19) -0.00613(16)
N1 0.0252(9) 0.0265(9) 0.0323(9) -0.0001(7) 0.0022(7) -0.0007(7)
N2 0.0261(8) 0.0282(9) 0.0308(8) 0.0009(7) 0.0040(6) 0.0013(7)
Be1 0.0226(11) 0.0261(11) 0.0328(12) -0.0011(9) 0.0038(9) -0.0003(9)
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'
Cl Cl 0.3639 0.7018 '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
N2 Be1 N1 110.86(16)
N2 Be1 Cl2 109.31(14)
N1 Be1 Cl2 108.17(14)
N2 Be1 Cl1 108.17(14)
N1 Be1 Cl1 108.91(14)
Cl2 Be1 Cl1 111.44(12)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cl1 Be1 2.042(3)
Cl2 Be1 2.020(3)
N1 Be1 1.722(3)
N2 Be1 1.715(3)
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H3 Cl2 0.81(3) 2.76(3) 3.4461(19) 145(2) 4_575 yes
N1 H2 Cl1 0.82(3) 2.80(3) 3.4966(18) 144(3) 3_666 yes
N1 H1 Cl1 0.84(3) 2.57(3) 3.3969(18) 168(3) 3_766 yes
N2 H6 Cl2 0.79(3) 2.62(3) 3.3831(19) 165(3) 4_576 yes
N2 H5 Cl2 0.90(3) 2.87(3) 3.3929(19) 119(2) 4_575 yes
N2 H5 Cl1 0.90(3) 2.67(3) 3.5338(18) 163(3) 4_575 yes
N2 H4 Cl1 0.84(4) 2.68(4) 3.4478(19) 153(3) 3_666 yes
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168351034
