#------------------------------------------------------------------------------
#$Date: 2025-08-22 10:56:18 +0200 (Fri 22 de Aug de 2025) $
#$Revision: 301860 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/43/7124315.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_7124315
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 H6 I2 N2'
_chemical_formula_sum            'Be H6 I2 N2'
_chemical_formula_weight         296.88
_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   geom
_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                 102.674(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.2739(4)
_cell_length_b                   13.1326(6)
_cell_length_c                   7.3586(4)
_cell_measurement_reflns_used    10557
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      158.44
_cell_measurement_theta_min      14.06
_cell_volume                     685.80(6)
_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 0.993
_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  0.0613
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            11337
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.205
_diffrn_reflns_theta_min         7.029
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    71.021
_exptl_absorpt_correction_T_max  0.6156
_exptl_absorpt_correction_T_min  0.0010
_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    2.875
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.522
_refine_diff_density_min         -2.272
_refine_diff_density_rms         0.302
_refine_ls_extinction_coef       0.00060(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   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1482
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0485
_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)+(0.0703P)²+10.2968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1285
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1219
_reflns_number_total             1482
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc07712j2.cif
_cod_data_source_block           4_CCDC1
_cod_database_code               7124315
_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 12:03:23 on 14-Jan-2019
REM Old TITL 1 in P2/n
REM SHELXT solution in P2(1)/n: R1 0.187, Rweak 0.004, Alpha 0.007
REM <I/s>   0.640 for   72 systematic absences,  Orientation as input
REM Formula found by SHELXT:  N I
CELL  1.54178   7.2739  13.1326   7.3586   90.000  102.674   90.000
ZERR    4.000   0.0004   0.0006   0.0004    0.000    0.005    0.000
LATT  1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC BE H N I
UNIT 4 24 8 8
L.S. 10
BOND
LIST 4
ACTA
FMAP 2
HTAB
EQIV $1 -x+1, -y+1, -z+1
HTAB N1 I1_$1
EQIV $2 x+1/2, -y+1/2, z-1/2
HTAB N1 I2_$2
EQIV $3 x+1/2, -y+1/2, z+1/2
HTAB N1 I1_$3
HTAB N1 I2_$3
HTAB N2 I2_$3
EQIV $4 -x, -y+1, -z+1
HTAB N2 I1_$4
HTAB N2 I1_$1
PLAN 20
TEMP -173.15
WGHT    0.070300   10.296800
EXTI    0.000601
FVAR       0.37674
I1    4    0.198509    0.460385    0.272244    11.00000    0.02898    0.02957 =
         0.03080    0.00326    0.00797    0.00218
N1    3    0.501371    0.308161    0.576353    11.00000    0.03663    0.02864 =
         0.02528    0.00403    0.00605    0.00713
AFIX 137
H1A   2    0.595284    0.355323    0.599179    11.00000   -1.50000
H1B   2    0.499945    0.276859    0.465725    11.00000   -1.50000
H1C   2    0.521554    0.261039    0.669283    11.00000   -1.50000
AFIX   0
BE1   1    0.289389    0.366983    0.566706    11.00000    0.03746    0.02714 =
         0.03689    0.01075    0.00977    0.01059
I2    4    0.058472    0.237968    0.589457    11.00000    0.03752    0.03499 =
         0.02881   -0.00099    0.00844   -0.01029
N2    3    0.297380    0.451002    0.743912    11.00000    0.03431    0.03524 =
         0.02731   -0.00041    0.00845    0.00064
AFIX 137
H2A   2    0.321701    0.416964    0.854318    11.00000   -1.50000
H2B   2    0.184615    0.483571    0.728815    11.00000   -1.50000
H2C   2    0.390104    0.497463    0.743493    11.00000   -1.50000
AFIX   0
HKLF 4




REM  1_a.res in P2(1)/n
REM wR2 = 0.1285, GooF = S = 1.053, Restrained GooF = 1.053 for all data
REM R1 = 0.0485 for 1219 Fo > 4sig(Fo) and 0.0640 for all 1482 data
REM 49 parameters refined using 0 restraints

END

WGHT      0.0704     10.4264

REM Instructions for potential hydrogen bonds
HTAB N1 I1_$1
HTAB N1 I2_$2
HTAB N1 I1_$3
HTAB N1 I2_$3
HTAB N2 I2_$3
HTAB N2 I1_$4
HTAB N2 I1_$1

REM Highest difference peak  1.522,  deepest hole -2.272,  1-sigma level  0.302
Q1    1   0.2794  0.5548  0.2366  11.00000  0.05    1.52
Q2    1  -0.0428  0.3127  0.4206  11.00000  0.05    1.29
Q3    1   0.1100  0.3379  0.5238  11.00000  0.05    1.20
Q4    1  -0.0037  0.3465  0.6329  11.00000  0.05    1.08
Q5    1   0.4437  0.3361  0.9435  11.00000  0.05    1.04
Q6    1   0.0419  0.2562  0.3800  11.00000  0.05    1.01
Q7    1   0.0454  0.3945  0.1735  11.00000  0.05    0.99
Q8    1   0.3259  0.4035  0.3786  11.00000  0.05    0.98
Q9    1   0.6002  0.5380  0.8220  11.00000  0.05    0.98
Q10   1  -0.0826  0.3159  0.5293  11.00000  0.05    0.98
Q11   1   0.3015  0.5395  0.4241  11.00000  0.05    0.97
Q12   1  -0.1578  0.2434  0.5265  11.00000  0.05    0.97
Q13   1  -0.1456  0.2342  0.5728  11.00000  0.05    0.94
Q14   1   0.3393  0.3779  0.1764  11.00000  0.05    0.90
Q15   1   0.3770  0.4426  0.3814  11.00000  0.05    0.90
Q16   1   0.7462  0.4388  0.6242  11.00000  0.05    0.89
Q17   1   0.2964  0.2261  0.6533  11.00000  0.05    0.88
Q18   1   0.1285  0.5571  0.1415  11.00000  0.05    0.87
Q19   1   0.1735  0.3565  0.3793  11.00000  0.05    0.85
Q20   1   0.5991  0.4731  0.8133  11.00000  0.05    0.84
;
_shelx_res_checksum              71635
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
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
I1 I 0.19851(9) 0.46039(5) 0.27224(9) 0.0296(2) Uani 1 1 d . .
N1 N 0.5014(13) 0.3082(7) 0.5764(12) 0.0303(19) Uani 1 1 d . .
H1A H 0.595284 0.355323 0.599179 0.045 Uiso 1 1 calc R U
H1B H 0.499945 0.276859 0.465725 0.045 Uiso 1 1 calc R U
H1C H 0.521554 0.261039 0.669283 0.045 Uiso 1 1 calc R U
Be1 Be 0.289(2) 0.3670(12) 0.567(2) 0.034(3) Uani 1 1 d . .
I2 I 0.05847(10) 0.23797(6) 0.58946(10) 0.0336(3) Uani 1 1 d . .
N2 N 0.2974(13) 0.4510(8) 0.7439(12) 0.032(2) Uani 1 1 d . .
H2A H 0.321701 0.416964 0.854318 0.048 Uiso 1 1 calc R U
H2B H 0.184615 0.483571 0.728815 0.048 Uiso 1 1 calc R U
H2C H 0.390104 0.497463 0.743493 0.048 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
I1 0.0290(4) 0.0296(4) 0.0308(4) 0.0033(3) 0.0080(3) 0.0022(3)
N1 0.037(5) 0.029(5) 0.025(4) 0.004(4) 0.006(4) 0.007(4)
Be1 0.037(8) 0.027(7) 0.037(8) 0.011(6) 0.010(6) 0.011(6)
I2 0.0375(4) 0.0350(4) 0.0288(4) -0.0010(3) 0.0084(3) -0.0103(3)
N2 0.034(5) 0.035(5) 0.027(5) 0.000(4) 0.008(4) 0.001(4)
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
N2 Be1 N1 112.5(10)
N2 Be1 I2 108.0(8)
N1 Be1 I2 108.3(8)
N2 Be1 I1 108.1(8)
N1 Be1 I1 109.2(8)
I2 Be1 I1 110.8(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
I1 Be1 2.451(14)
N1 Be1 1.712(17)
Be1 N2 1.699(19)
Be1 I2 2.417(16)
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 H1A I1 0.91 2.89 3.765(10) 160.6 3_666 yes
N1 H1B I2 0.91 2.90 3.746(9) 155.4 4_665 yes
N1 H1C I1 0.91 3.20 3.958(9) 141.8 4_666 yes
N1 H1C I2 0.91 3.04 3.756(9) 136.4 4_666 yes
N2 H2A I2 0.91 2.97 3.757(10) 146.3 4_666 yes
N2 H2B I1 0.91 2.88 3.767(9) 165.0 3_566 yes
N2 H2C I1 0.91 3.07 3.874(9) 148.2 3_666 yes
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168351033
