#------------------------------------------------------------------------------
#$Date: 2019-10-16 03:14:07 +0300 (Wed, 16 Oct 2019) $
#$Revision: 219370 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/43/7124312.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_7124312
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         '2(Br), 2(H3 N), Be'
_chemical_formula_sum            'Be Br2 H6 N2'
_chemical_formula_weight         202.90
_chemical_name_common            diamminberylliumbromide
_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                 101.446(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8278(2)
_cell_length_b                   12.2863(2)
_cell_length_c                   6.9291(2)
_cell_measurement_reflns_used    23274
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      159.14
_cell_measurement_theta_min      7.19
_cell_volume                     569.71(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0094
_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       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14114
_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         78.914
_diffrn_reflns_theta_min         7.209
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    16.827
_exptl_absorpt_correction_T_max  0.4248
_exptl_absorpt_correction_T_min  0.0982
_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    2.366
_exptl_crystal_description       block
_exptl_crystal_F_000             376
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.00117(15)
_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   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     49
_refine_ls_number_reflns         1225
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0195
_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)+(0.0358P)²+0.2563P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0498
_refine_ls_wR_factor_ref         0.0507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1151
_reflns_number_total             1225
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc07712j2.cif
_cod_data_source_block           5
_cod_database_code               7124312
_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
    5.res
    created by SHELXL-2018/3 at 12:06:08 on 11-Mar-2019
REM Old TITL 1 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.069, Rweak 0.004, Alpha 0.012
REM <I/s>   0.861 for   64 systematic absences,  Orientation as input
REM Formula found by SHELXT:  N3 I2
CELL  1.54178   6.8278  12.2863   6.9291   90.000  101.446   90.000
ZERR    4.000   0.0002   0.0002   0.0002    0.000    0.002    0.000
LATT  1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC BE H N Br
UNIT 4 24 8 8
L.S. 10
BOND
LIST 4
TEMP -173.15
ACTA
REM OMIT -1 1 1
FMAP 2
PLAN 20
HTAB
EQIV $1 -x+1, -y+1, -z+1
HTAB N1 Br2_$1
EQIV $2 x-1/2, -y+1/2, z+1/2
HTAB N1 Br1_$2
EQIV $3 x-1/2, -y+1/2, z-1/2
HTAB N1 Br1_$3
HTAB N1 Br2_$3
HTAB N2 Br1_$3
EQIV $4 -x+2, -y+1, -z+1
HTAB N2 Br2_$4
HTAB N2 Br2_$1
REM TWIN
REM BASF 0.51697
WGHT    0.035800    0.256300
EXTI    0.001167
FVAR       0.51659
BR1   4    0.945630    0.244324    0.425826    11.00000    0.02393    0.02621 =
         0.02065    0.00114    0.00630    0.00694
BR2   4    0.792498    0.459093    0.722250    11.00000    0.01879    0.02215 =
         0.02069   -0.00164    0.00472   -0.00111
N1    3    0.492925    0.302636    0.435466    11.00000    0.02255    0.02496 =
         0.01986   -0.00174    0.00541   -0.00179
AFIX 137
H1A   2    0.391792    0.351218    0.398745    11.00000   -1.50000
H1B   2    0.488393    0.275766    0.556884    11.00000   -1.50000
H1C   2    0.479333    0.247079    0.346954    11.00000   -1.50000
AFIX   0
N2    3    0.708867    0.455347    0.250297    11.00000    0.01853    0.02300 =
         0.02294    0.00107    0.00549    0.00007
AFIX 137
H2A   2    0.679463    0.418294    0.134435    11.00000   -1.50000
H2B   2    0.829696    0.488527    0.260938    11.00000   -1.50000
H2C   2    0.613096    0.506442    0.253579    11.00000   -1.50000
AFIX   0
BE1   1    0.717067    0.366250    0.442632    11.00000    0.01787    0.02462 =
         0.02156   -0.00058    0.00538   -0.00087
HKLF 4




REM  1_a.res in P2(1)/n
REM wR2 = 0.0507, GooF = S = 1.056, Restrained GooF = 1.056 for all data
REM R1 = 0.0195 for 1151 Fo > 4sig(Fo) and 0.0215 for all 1225 data
REM 49 parameters refined using 0 restraints

END

WGHT      0.0358      0.2563

REM Instructions for potential hydrogen bonds
HTAB N1 Br2_$1
HTAB N1 Br1_$2
HTAB N1 Br1_$3
HTAB N1 Br2_$3
HTAB N2 Br1_$3
HTAB N2 Br2_$4
HTAB N2 Br2_$1

REM Highest difference peak  0.394,  deepest hole -0.450,  1-sigma level  0.097
Q1    1   0.7732  0.5200  0.8559  11.00000  0.05    0.39
Q2    1   0.7593  0.5391  0.8143  11.00000  0.05    0.38
Q3    1   0.5883  0.3394  0.4456  11.00000  0.05    0.37
Q4    1   0.9369  0.1807  0.5804  11.00000  0.05    0.34
Q5    1   1.1349  0.2384  0.5770  11.00000  0.05    0.33
Q6    1   0.6164  0.4514  0.5807  11.00000  0.05    0.32
Q7    1   0.9998  0.3219  0.3181  11.00000  0.05    0.32
Q8    1   0.9074  0.3220  0.5305  11.00000  0.05    0.31
Q9    1   0.9552  0.2090  0.6185  11.00000  0.05    0.31
Q10   1   0.7173  0.4199  0.3391  11.00000  0.05    0.28
Q11   1   0.9079  0.1637  0.5271  11.00000  0.05    0.28
Q12   1   0.8677  0.2404  0.4317  11.00000  0.05    0.28
Q13   1   0.7566  0.3964  0.8607  11.00000  0.05    0.27
Q14   1   0.4292  0.2584  0.7171  11.00000  0.05    0.27
Q15   1   0.8376  0.3831  0.6174  11.00000  0.05    0.27
Q16   1   0.6470  0.5322  0.8437  11.00000  0.05    0.27
Q17   1   0.8415  0.5387  0.6243  11.00000  0.05    0.26
Q18   1   0.7624  0.2303  0.2792  11.00000  0.05    0.26
Q19   1   0.6858  0.4099  0.5404  11.00000  0.05    0.26
Q20   1   0.8519  0.6247  0.2777  11.00000  0.05    0.25
;
_shelx_res_checksum              26250
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
Br1 Br 0.94563(4) 0.24432(2) 0.42583(3) 0.02334(10) Uani 1 1 d . .
Br2 Br 0.79250(3) 0.45909(2) 0.72225(3) 0.02044(10) Uani 1 1 d . .
N1 N 0.4929(3) 0.30264(17) 0.4355(3) 0.0223(4) Uani 1 1 d . .
H1A H 0.391792 0.351218 0.398745 0.033 Uiso 1 1 calc R U
H1B H 0.488393 0.275766 0.556884 0.033 Uiso 1 1 calc R U
H1C H 0.479333 0.247079 0.346954 0.033 Uiso 1 1 calc R U
N2 N 0.7089(3) 0.45535(17) 0.2503(3) 0.0213(4) Uani 1 1 d . .
H2A H 0.679463 0.418294 0.134435 0.032 Uiso 1 1 calc R U
H2B H 0.829696 0.488527 0.260938 0.032 Uiso 1 1 calc R U
H2C H 0.613096 0.506442 0.253579 0.032 Uiso 1 1 calc R U
Be1 Be 0.7171(4) 0.3663(3) 0.4426(4) 0.0211(6) Uani 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
Br1 0.02393(15) 0.02621(15) 0.02065(15) 0.00114(8) 0.00630(10) 0.00694(9)
Br2 0.01879(14) 0.02215(15) 0.02069(14) -0.00164(8) 0.00472(9) -0.00111(8)
N1 0.0225(9) 0.0250(10) 0.0199(9) -0.0017(7) 0.0054(8) -0.0018(8)
N2 0.0185(10) 0.0230(10) 0.0229(10) 0.0011(7) 0.0055(7) 0.0001(7)
Be1 0.0179(13) 0.0246(14) 0.0216(14) -0.0006(11) 0.0054(10) -0.0009(11)
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'
Br Br -0.6763 1.2805 '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
N1 Be1 N2 112.19(19)
N1 Be1 Br1 109.26(17)
N2 Be1 Br1 108.04(16)
N1 Be1 Br2 108.15(16)
N2 Be1 Br2 108.43(17)
Br1 Be1 Br2 110.78(13)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Br1 Be1 2.183(3)
Br2 Be1 2.219(3)
N1 Be1 1.710(4)
N2 Be1 1.717(4)
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 Br2 0.91 2.70 3.566(2) 159.0 3_666 yes
N1 H1B Br1 0.91 2.64 3.5238(19) 163.6 4_566 yes
N1 H1C Br1 0.91 2.88 3.529(2) 129.2 4_565 yes
N1 H1C Br2 0.91 2.89 3.687(2) 147.0 4_565 yes
N2 H2A Br1 0.91 2.78 3.564(2) 145.3 4_565 yes
N2 H2B Br2 0.91 2.64 3.532(2) 167.3 3_766 yes
N2 H2C Br2 0.91 2.84 3.622(2) 144.9 3_666 yes
