#------------------------------------------------------------------------------
#$Date: 2019-10-16 03:14:07 +0300 (Wed, 16 Oct 2019) $
#$Revision: 219370 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/43/7124316.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_7124316
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 Br2 H12 N4'
_chemical_formula_sum            'Be Br2 H12 N4'
_chemical_formula_weight         236.97
_chemical_name_systematic        Tetramminberylliumbromide
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.5332(2)
_cell_length_b                   6.93550(10)
_cell_length_c                   12.2289(3)
_cell_measurement_reflns_used    27341
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      160.05
_cell_measurement_theta_min      7.23
_cell_volume                     808.54(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (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 0.997
_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  0.0174
_diffrn_reflns_av_unetI/netI     0.0060
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13697
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.113
_diffrn_reflns_theta_min         5.885
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    12.030
_exptl_absorpt_correction_T_max  0.4613
_exptl_absorpt_correction_T_min  0.0387
_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    1.947
_exptl_crystal_description       plate
_exptl_crystal_F_000             456
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.360
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.00279(14)
_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   1.190
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     44
_refine_ls_number_reflns         948
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.190
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0175
_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)+(0.0202P)²+0.9261P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0451
_reflns_Friedel_coverage         0.000
_reflns_number_gt                946
_reflns_number_total             948
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc07712j2.cif
_cod_data_source_block           5_CCDC1
_cod_database_code               7124316
_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 4_a.res in Pnma
    5.res
    created by SHELXL-2018/3 at 15:10:08 on 10-Jan-2019
REM Old TITL 4 in Pnma
REM SHELXT solution in Pnma: R1 0.059, Rweak 0.003, Alpha 0.015
REM <I/s>   3.647 for  103 systematic absences,  Orientation as input
REM Formula found by SHELXT:  Be N4 Br2
CELL  1.54178   9.5332   6.9355  12.2289   90.000   90.000   90.000
ZERR    4.000   0.0002   0.0001   0.0003    0.000    0.000    0.000
LATT  1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, -Z
SYMM 1/2+X, 1/2-Y, 1/2-Z
SFAC BE H N BR
UNIT 4 48 16 8
L.S. 10
BOND
LIST 4
ACTA
TEMP -173.15
HTAB
EQIV $2 -x+1, -y+2, -z+1
HTAB N1 Br2_$2
EQIV $3 -x+1, -y+1, -z+1
HTAB N1 Br2_$3
HTAB N1 Br2
HTAB N2 Br1
EQIV $4 x, y+1, z
HTAB N2 Br1_$4
HTAB N2 Br2
EQIV $5 -x+2, -y+1, -z+1
HTAB N3 Br1_$5
EQIV $6 -x+3/2, -y+1, z+1/2
HTAB N3 Br1_$6
HTAB N3 Br1_$4
HTAB N3 Br2_$2
FMAP 2
PLAN 20
WGHT    0.020200    0.926100
EXTI    0.002794
FVAR       0.55035
BR1   4    0.844488    0.250000    0.398429    10.50000    0.02269    0.02387 =
         0.02457    0.00000    0.00235    0.00000
BR2   4    0.476245    0.750000    0.316873    10.50000    0.02317    0.01900 =
         0.01543    0.00000   -0.00141    0.00000
N1    3    0.564841    0.750000    0.593569    10.50000    0.02051    0.02288 =
         0.01584    0.00000   -0.00115    0.00000
AFIX 137
H1A   2    0.535372    0.864844    0.621272    10.50000   -1.50000
H1B   2    0.536882    0.652761    0.638526    10.50000   -1.50000
H1C   2    0.527033    0.732395    0.525975    10.50000   -1.50000
AFIX   0
N2    3    0.798564    0.750000    0.448975    10.50000    0.02939    0.04478 =
         0.02314    0.00000    0.00838    0.00000
AFIX 137
H2A   2    0.875742    0.674105    0.440921    10.50000   -1.50000
H2B   2    0.819375    0.872547    0.427909    10.50000   -1.50000
H2C   2    0.727676    0.703348    0.406742    10.50000   -1.50000
AFIX   0
N3    3    0.812457    0.950996    0.646812    11.00000    0.02272    0.03549 =
         0.05245   -0.02188   -0.00436    0.00008
AFIX 137
H3A   2    0.907802    0.945056    0.648035    11.00000   -1.50000
H3B   2    0.779329    0.957034    0.716517    11.00000   -1.50000
H3C   2    0.784916    1.057911    0.609399    11.00000   -1.50000
AFIX   0
BE1   1    0.747326    0.750000    0.583865    10.50000    0.01711    0.01729 =
         0.01666    0.00000    0.00159    0.00000
HKLF 4




REM  4_a.res in Pnma
REM wR2 = 0.0451, GooF = S = 1.190, Restrained GooF = 1.190 for all data
REM R1 = 0.0175 for 946 Fo > 4sig(Fo) and 0.0178 for all 948 data
REM 44 parameters refined using 0 restraints

END

WGHT      0.0202      0.9261

REM Instructions for potential hydrogen bonds
HTAB N1 Br2_$2
HTAB N1 Br2_$3
HTAB N1 Br2
HTAB N2 Br1
HTAB N2 Br1_$4
HTAB N2 Br2
HTAB N3 Br1_$5
HTAB N3 Br1_$6
HTAB N3 Br1_$4
HTAB N3 Br2_$2

REM Highest difference peak  0.360,  deepest hole -0.558,  1-sigma level  0.100
Q1    1   0.7635  1.0305  0.6649  11.00000  0.05    0.36
Q2    1   0.8532  0.2500  0.4545  10.50000  0.05    0.35
Q3    1   0.8213  0.1634  0.3695  11.00000  0.05    0.31
Q4    1   0.7736  0.8668  0.6055  11.00000  0.05    0.31
Q5    1   0.5366  1.0556  0.6271  11.00000  0.05    0.29
Q6    1   0.7992  0.9007  0.6950  11.00000  0.05    0.27
Q7    1   0.8164  0.1241  0.4642  11.00000  0.05    0.27
Q8    1   0.5365  0.8463  0.3351  11.00000  0.05    0.26
Q9    1   0.8937  1.0372  0.4179  11.00000  0.05    0.26
Q10   1   0.8560  1.0251  0.7041  11.00000  0.05    0.26
Q11   1   0.8505  0.9460  0.6424  11.00000  0.05    0.25
Q12   1   0.5147  0.8724  0.2699  11.00000  0.05    0.24
Q13   1   0.7947  0.9950  0.4270  11.00000  0.05    0.21
Q14   1   0.6280  0.4884  0.4390  11.00000  0.05    0.19
Q15   1   0.8587  1.0588  0.5745  11.00000  0.05    0.19
Q16   1   0.9437  1.0212  0.5735  11.00000  0.05    0.19
Q17   1   0.8193  1.0294  0.3412  11.00000  0.05    0.19
Q18   1   0.5870  0.7500  0.2691  10.50000  0.05    0.19
Q19   1   0.6380  1.0061  0.5233  11.00000  0.05    0.17
Q20   1   0.5822  0.9923  0.5581  11.00000  0.05    0.17
;
_shelx_res_checksum              94765
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Br1 Br 0.84449(3) 0.250000 0.39843(2) 0.02371(11) Uani 1 2 d S T P
Br2 Br 0.47624(3) 0.750000 0.31687(2) 0.01920(11) Uani 1 2 d S T P
N1 N 0.5648(2) 0.750000 0.59357(17) 0.0197(5) Uani 1 2 d S T P
H1A H 0.535372 0.864844 0.621272 0.030 Uiso 0.5 1 calc R U P
H1B H 0.536882 0.652761 0.638526 0.030 Uiso 0.5 1 calc R U P
H1C H 0.527033 0.732395 0.525975 0.030 Uiso 0.5 1 calc R U P
N2 N 0.7986(3) 0.750000 0.4490(2) 0.0324(6) Uani 1 2 d S T P
H2A H 0.875742 0.674105 0.440921 0.049 Uiso 0.5 1 calc R U P
H2B H 0.819375 0.872547 0.427909 0.049 Uiso 0.5 1 calc R U P
H2C H 0.727676 0.703348 0.406742 0.049 Uiso 0.5 1 calc R U P
N3 N 0.81246(18) 0.9510(3) 0.64681(18) 0.0369(5) Uani 1 1 d . . .
H3A H 0.907802 0.945056 0.648035 0.055 Uiso 1 1 calc R U .
H3B H 0.779329 0.957034 0.716517 0.055 Uiso 1 1 calc R U .
H3C H 0.784916 1.057911 0.609399 0.055 Uiso 1 1 calc R U .
Be1 Be 0.7473(4) 0.750000 0.5839(3) 0.0170(6) Uani 1 2 d S T P
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 0.02269(17) 0.02387(18) 0.02457(17) 0.000 0.00235(10) 0.000
Br2 0.02317(16) 0.01900(16) 0.01543(15) 0.000 -0.00141(9) 0.000
N1 0.0205(11) 0.0229(12) 0.0158(10) 0.000 -0.0011(8) 0.000
N2 0.0294(13) 0.0448(17) 0.0231(12) 0.000 0.0084(10) 0.000
N3 0.0227(8) 0.0355(11) 0.0525(12) -0.0219(10) -0.0044(8) 0.0001(8)
Be1 0.0171(15) 0.0173(16) 0.0167(14) 0.000 0.0016(12) 0.000
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
_geom_angle_site_symmetry_1
N3 Be1 N3 109.3(2) 7_575
N3 Be1 N2 109.19(16) 7_575
N3 Be1 N2 109.19(16) .
N3 Be1 N1 109.38(15) 7_575
N3 Be1 N1 109.38(15) .
N2 Be1 N1 110.4(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 Be1 1.744(4)
N2 Be1 1.720(4)
N3 Be1 1.709(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 H1A Br2 0.91 2.78 3.6576(7) 162.8 5_676 yes
N1 H1B Br2 0.91 2.85 3.6576(7) 148.8 5_666 yes
N1 H1C Br2 0.91 2.61 3.488(2) 163.5 . yes
N2 H2A Br1 0.91 3.00 3.5495(5) 120.4 . yes
N2 H2B Br1 0.91 2.65 3.5495(5) 168.4 1_565 yes
N2 H2C Br2 0.91 2.66 3.472(3) 149.5 . yes
N3 H3A Br1 0.91 2.78 3.5979(18) 150.1 5_766 yes
N3 H3B Br1 0.91 2.90 3.695(2) 146.9 2_665 yes
N3 H3C Br1 0.91 2.96 3.690(2) 138.6 1_565 yes
N3 H3C Br2 0.91 2.96 3.4746(19) 117.1 5_676 yes
