#------------------------------------------------------------------------------
#$Date: 2019-10-16 02:14:07 +0200 (Wed 16 de Oct de 2019) $
#$Revision: 219370 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/43/7124311.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_7124311
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         'N6, 4(H3 N), Be'
_chemical_formula_sum            'Be H12 N10'
_chemical_formula_weight         161.21
_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_Hall           'I -4 2'
_space_group_name_H-M_alt        'I -4 2 m'
_symmetry_space_group_name_Hall  'I -4 2'
_symmetry_space_group_name_H-M   'I -4 2 m'
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.0140(3)
_cell_length_b                   8.0140(3)
_cell_length_c                   6.4519(3)
_cell_measurement_reflns_used    1332
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      156.44
_cell_measurement_theta_min      17.65
_cell_volume                     414.37(3)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            725
_diffrn_reflns_point_group_measured_fraction_full 0.962
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         78.225
_diffrn_reflns_theta_min         8.824
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.9419
_exptl_absorpt_correction_T_min  0.2629
_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    1.292
_exptl_crystal_description       rod
_exptl_crystal_F_000             172
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.042
_refine_ls_abs_structure_details
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_extinction_coef       0.049(12)
_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   1.188
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     26
_refine_ls_number_reflns         234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.188
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0334
_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)+(0.0759P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0946
_reflns_Friedel_coverage         0.550
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.874
_reflns_number_gt                232
_reflns_number_total             234
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc07712j2.cif
_cod_data_source_block           3
_cod_original_cell_volume        414.37(4)
_cod_database_code               7124311
_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 I-42m
    3.res
    created by SHELXL-2018/3 at 11:53:00 on 08-Jul-2019
REM Old TITL 1 in I-42m
REM SHELXT solution in I-42m: R1 0.066, Rweak 0.029, Alpha 0.001
REM <I/s>   0.000 for    0 systematic absences,  Orientation as input
REM Flack x =  0.332 ( 2.500 ) from    79 Parsons' quotients
REM Formula found by SHELXT:  Be N10
CELL  1.54178   8.0140   8.0140   6.4519   90.000   90.000   90.000
ZERR    2.000   0.0003   0.0003   0.0003    0.000    0.000    0.000
LATT -2
SYMM -X, -Y, Z
SYMM Y, -X, -Z
SYMM -Y, X, -Z
SYMM -X, Y, -Z
SYMM X, -Y, -Z
SYMM -Y, -X, Z
SYMM Y, X, Z
SFAC BE H N
UNIT 2 24 20
L.S. 10
BOND
HTAB
HTAB N1 N2
EQIV $5 -x+3/2, -y+3/2, z-1/2
HTAB N1 N2_$5
EQIV $6 y+1/2, -x+3/2, -z+3/2
HTAB N1 N2_$6
OMIT -3 9 2
LIST 4
ACTA
TEMP -173.15
FMAP 2
TWIN 0 1 0 1 0 0 0 0 1
PLAN 20
WGHT    0.075900
EXTI    0.048508
BASF   0.32012
FVAR       2.22118
N1    3    0.623904    0.623904    0.655057    10.50000    0.01873    0.01873 =
         0.02159   -0.00096   -0.00096   -0.00218
N2    3    0.852485    0.500000    1.000000    10.50000    0.01850    0.02492 =
         0.02462    0.00178    0.00000    0.00000
N3    3    1.000000    0.500000    1.000000    10.25000    0.02222    0.01438 =
         0.01874    0.00000    0.00000    0.00000
BE1   1    0.500000    0.500000    0.500000    10.12500    0.01710    0.01710 =
         0.01945    0.00000    0.00000    0.00000
H1    2    0.690194    0.568035    0.742184    11.00000    0.03418
H2    2    0.684847    0.684847    0.587498    10.50000    0.02960
HKLF 4




REM  1_a.res in I-42m
REM wR2 = 0.0946, GooF = S = 1.188, Restrained GooF = 1.188 for all data
REM R1 = 0.0334 for 232 Fo > 4sig(Fo) and 0.0339 for all 234 data
REM 26 parameters refined using 0 restraints

END

WGHT      0.0759      0.0000

REM Instructions for potential hydrogen bonds
HTAB N1 N2
HTAB N1 N2_$5
HTAB N1 N2_$6

REM Highest difference peak  0.185,  deepest hole -0.145,  1-sigma level  0.042
Q1    1   0.8356  0.5005  0.8857  11.00000  0.05    0.19
Q2    1   0.5576  0.4424  0.9325  10.50000  0.05    0.13
Q3    1   0.5560  0.4440  0.7580  10.50000  0.05    0.12
Q4    1   0.6028  0.6028  0.8077  10.50000  0.05    0.12
Q5    1   1.0000  0.5000  0.8986  10.50000  0.05    0.11
Q6    1   0.5807  0.5808  0.5833  10.50000  0.05    0.10
Q7    1   0.8441  0.6387  0.6441  11.00000  0.05    0.10
Q8    1   0.6821  0.5073  0.8666  11.00000  0.05    0.10
Q9    1   0.4248  0.5752  0.5893  10.50000  0.05    0.10
Q10   1   0.5570  0.5570  0.8912  10.50000  0.05    0.09
Q11   1   0.5000  0.5000  0.8322  10.25000  0.05    0.09
Q12   1   0.7950  0.5730  0.7548  11.00000  0.05    0.09
Q13   1   1.0000  0.3054  1.0000  10.50000  0.05    0.08
Q14   1   0.5226  0.5226  0.6519  10.50000  0.05    0.08
Q15   1   0.8483  0.5969  1.1689  11.00000  0.05    0.07
Q16   1   0.9378  0.4262  1.2460  11.00000  0.05    0.07
Q17   1   0.6775  0.7802  0.4756  11.00000  0.05    0.06
Q18   1   1.0224  0.3408  0.9005  11.00000  0.05    0.05
Q19   1   0.7010  0.6293  0.8942  11.00000  0.05    0.05
Q20   1   0.6978  0.3776  0.8613  11.00000  0.05    0.05
;
_shelx_res_checksum              62644
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'-x, y, -z'
'x, -y, -z'
'-y, -x, z'
'y, x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'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+1/2, -x+1/2, z+1/2'
'y+1/2, x+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
N1 N 0.62390(18) 0.62390(18) 0.6551(3) 0.0197(7) Uani 1 2 d S T P
N2 N 0.8525(2) 0.500000 1.000000 0.0227(7) Uani 1 2 d S T P
N3 N 1.000000 0.500000 1.000000 0.0184(8) Uani 1 4 d S T P
Be1 Be 0.500000 0.500000 0.500000 0.0179(10) Uani 1 8 d S T P
H1 H 0.690(3) 0.568(3) 0.742(4) 0.034(8) Uiso 1 1 d . . .
H2 H 0.685(3) 0.685(3) 0.587(4) 0.030(11) Uiso 1 2 d S . 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
N1 0.0187(8) 0.0187(8) 0.0216(9) -0.0010(6) -0.0010(6) -0.0022(8)
N2 0.0185(10) 0.0249(10) 0.0246(10) 0.0018(11) 0.000 0.000
N3 0.0222(13) 0.0144(11) 0.0187(12) 0.000 0.000 0.000
Be1 0.0171(14) 0.0171(14) 0.019(2) 0.000 0.000 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'
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
N2 N3 N2 180.0 2_765 .
N1 Be1 N1 109.07(13) 4_656 3_566
N1 Be1 N1 109.67(7) 4_656 2_665
N1 Be1 N1 109.67(7) 3_566 2_665
N1 Be1 N1 109.67(7) 4_656 .
N1 Be1 N1 109.67(7) 3_566 .
N1 Be1 N1 109.07(13) 2_665 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 Be1 1.7242(18)
N2 N3 1.1822(18)
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 H1 N2 0.89(3) 2.18(2) 3.0487(17) 164(2) . yes
N1 H2 N2 0.82(3) 2.61(2) 3.1814(16) 128.8(7) 10_664 yes
N1 H2 N2 0.82(3) 2.61(2) 3.1814(16) 128.8(7) 11_566 yes
