#------------------------------------------------------------------------------
#$Date: 2019-10-16 02:14:07 +0200 (Wed 16 de Oct de 2019) $
#$Revision: 219370 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/43/7124313.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_7124313
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_sum            'Be H12 I2 N4'
_chemical_formula_weight         330.95
_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-2014/7
_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                   9.9007(2)
_cell_length_b                   7.3274(2)
_cell_length_c                   12.7965(3)
_cell_measurement_reflns_used    15988
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      154.38
_cell_measurement_theta_min      6.91
_cell_volume                     928.34(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0354
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8664
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.386
_diffrn_reflns_theta_min         5.650
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    52.617
_exptl_absorpt_correction_T_max  0.0001
_exptl_absorpt_correction_T_min  0.0000
_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    2.368
_exptl_crystal_description       block
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.065
_exptl_transmission_factor_max   0.0001
_exptl_transmission_factor_min   0.0000
_refine_diff_density_max         2.331
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.321
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         1056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.186
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0407
_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)+(0.0821P)²+1.2286P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1123
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1034
_reflns_number_total             1056
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9cc07712j2.cif
_cod_data_source_block           3_CCDC1
_cod_database_code               7124313
_shelx_shelxl_version_number     2014/7
_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
;

    3.res created by SHELXL-2014/7


TITL 1_a.res in Pnma
REM Old TITL 1 in Pnma

REM SHELXT solution in Pnma
REM R1 0.054,  Rweak 0.003,  Alpha 0.012,  Orientation as input
REM Formula found by SHELXT:  Be N4 I2

CELL  1.54178   9.9007   7.3274  12.7965   90.000   90.000   90.000
ZERR    4.000   0.0002   0.0002   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 I
UNIT 4 48 16 8
L.S. 10
BOND $H
LIST 4
ACTA
TEMP -173.15
FMAP 2
HTAB
PLAN 20
REM EXTI 0.000011
WGHT    0.082100    1.228600
FVAR       0.27377
I1    4    0.519781    0.250000    0.314359    10.50000    0.02311    0.02807 =
         0.02657    0.00000   -0.00056    0.00000
I2    4    0.164947    0.750000    0.404674    10.50000    0.02395    0.02773 =
         0.02730    0.00000   -0.00041    0.00000
N1    3    0.425348    0.250000    0.592706    10.50000    0.02157    0.03417 =
         0.02937    0.00000    0.00171    0.00000
AFIX 137
H1A   2    0.453243    0.175363    0.645287    10.50000   -1.50000
H1B   2    0.455372    0.365449    0.604844    10.50000   -1.50000
H1C   2    0.459264    0.209189    0.530881    10.50000   -1.50000
AFIX   0
N2    3    0.193550    0.250000    0.459288    10.50000    0.02493    0.03472 =
         0.03302    0.00000   -0.00059    0.00000
AFIX 137
H2A   2    0.198388    0.134825    0.432952    10.50000   -1.50000
H2B   2    0.246086    0.325846    0.420318    10.50000   -1.50000
H2C   2    0.106405    0.289330    0.457316    10.50000   -1.50000
AFIX   0
N3    3    0.188612    0.440644    0.648767    11.00000    0.02643    0.02774 =
         0.03340   -0.00697    0.00000   -0.00058
AFIX 137
H3A   2    0.096855    0.434922    0.651300    11.00000   -1.50000
H3B   2    0.214179    0.542019    0.612765    11.00000   -1.50000
H3C   2    0.222165    0.446108    0.714899    11.00000   -1.50000
AFIX   0
BE1   1    0.250143    0.250000    0.587186    10.50000    0.02182    0.02498 =
         0.02220    0.00000    0.00234    0.00000
HKLF 4

REM  1_a.res in Pnma
REM R1 =  0.0407 for    1034 Fo > 4sig(Fo)  and  0.0412 for all    1056 data
REM     43 parameters refined using      0 restraints

END

WGHT      0.0821      1.2286

REM Instructions for potential hydrogen bonds
EQIV $1 -x+1, -y, -z+1
HTAB N1 I1_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB N1 I1_$2
HTAB N1 I1
EQIV $3 x, y-1, z
HTAB N2 I2_$3
HTAB N2 I1
HTAB N2 I2
EQIV $4 -x, -y+1, -z+1
HTAB N2 I2_$4
HTAB N3 I2_$4
HTAB N3 I1_$2
HTAB N3 I2
EQIV $5 -x+1/2, -y+1, z+1/2
HTAB N3 I2_$5

REM Highest difference peak  2.331,  deepest hole -1.981,  1-sigma level  0.321
Q1    1   0.1560  0.8660  0.4069  11.00000  0.05    2.33
Q2    1   0.5200  0.1324  0.3134  11.00000  0.05    2.31
Q3    1   0.5083  0.2500  0.3820  10.50000  0.05    1.73
Q4    1   0.1585  0.7500  0.4704  10.50000  0.05    1.38
Q5    1   0.1721  0.7500  0.3317  10.50000  0.05    1.34
Q6    1   0.5267  0.2500  0.2417  10.50000  0.05    1.22
Q7    1   0.0000  0.5000  0.5000  10.50000  0.05    0.60
Q8    1   0.1216 -0.0031  0.4219  11.00000  0.05    0.52
Q9    1   0.2058  0.5332  0.6536  11.00000  0.05    0.47
Q10   1   0.6237  0.1549  0.4224  11.00000  0.05    0.45
Q11   1   0.5404 -0.0022  0.6860  11.00000  0.05    0.45
Q12   1   0.2102 -0.0065  0.4297  11.00000  0.05    0.45
Q13   1   0.4427  0.5041  0.6545  11.00000  0.05    0.44
Q14   1  -0.0572  0.3554  0.4969  11.00000  0.05    0.43
Q15   1   0.1726  0.5124  0.7074  11.00000  0.05    0.41
Q16   1   0.4263 -0.0212  0.7128  11.00000  0.05    0.39
Q17   1   0.2772  0.6494  0.6128  11.00000  0.05    0.38
Q18   1   0.1764  0.5068  0.8004  11.00000  0.05    0.37
Q19   1   0.4013  0.3452  0.4115  11.00000  0.05    0.37
Q20   1   0.3073  0.6522  0.6564  11.00000  0.05    0.36
;
_shelx_res_checksum              72643
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
I1 I 0.51978(4) 0.2500 0.31436(3) 0.0259(2) Uani 1 2 d S T P
I2 I 0.16495(4) 0.7500 0.40467(3) 0.0263(2) Uani 1 2 d S T P
N1 N 0.4253(6) 0.2500 0.5927(5) 0.0284(13) Uani 1 2 d S T P
H1A H 0.4532 0.1754 0.6453 0.043 Uiso 0.5 1 calc R U P
H1B H 0.4554 0.3654 0.6048 0.043 Uiso 0.5 1 calc R U P
H1C H 0.4593 0.2092 0.5309 0.043 Uiso 0.5 1 calc R U P
N2 N 0.1935(7) 0.2500 0.4593(5) 0.0309(13) Uani 1 2 d S T P
H2A H 0.1984 0.1348 0.4330 0.046 Uiso 0.5 1 calc R U P
H2B H 0.2461 0.3258 0.4203 0.046 Uiso 0.5 1 calc R U P
H2C H 0.1064 0.2893 0.4573 0.046 Uiso 0.5 1 calc R U P
N3 N 0.1886(4) 0.4406(7) 0.6488(4) 0.0292(9) Uani 1 1 d . . .
H3A H 0.0969 0.4349 0.6513 0.044 Uiso 1 1 calc R U .
H3B H 0.2142 0.5420 0.6128 0.044 Uiso 1 1 calc R U .
H3C H 0.2222 0.4461 0.7149 0.044 Uiso 1 1 calc R U .
Be1 Be 0.2501(10) 0.2500 0.5872(7) 0.0230(16) 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
I1 0.0231(3) 0.0281(3) 0.0266(3) 0.000 -0.00056(14) 0.000
I2 0.0240(3) 0.0277(3) 0.0273(3) 0.000 -0.00041(14) 0.000
N1 0.022(3) 0.034(3) 0.029(3) 0.000 0.002(2) 0.000
N2 0.025(3) 0.035(3) 0.033(3) 0.000 -0.001(3) 0.000
N3 0.0264(19) 0.028(2) 0.033(2) -0.0070(18) 0.0000(17) -0.0006(17)
Be1 0.022(4) 0.025(4) 0.022(4) 0.000 0.002(3) 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'
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
_geom_angle_site_symmetry_1
Be1 N1 H1A 109.5 .
Be1 N1 H1B 109.5 .
H1A N1 H1B 109.5 .
Be1 N1 H1C 109.5 .
H1A N1 H1C 109.5 .
H1B N1 H1C 109.5 .
Be1 N2 H2A 109.5 .
Be1 N2 H2B 109.5 .
H2A N2 H2B 109.5 .
Be1 N2 H2C 109.5 .
H2A N2 H2C 109.5 .
H2B N2 H2C 109.5 .
Be1 N3 H3A 109.5 .
Be1 N3 H3B 109.5 .
H3A N3 H3B 109.5 .
Be1 N3 H3C 109.5 .
H3A N3 H3C 109.5 .
H3B N3 H3C 109.5 .
N3 Be1 N3 109.0(6) 7_565
N3 Be1 N2 108.6(4) 7_565
N3 Be1 N2 108.6(4) .
N3 Be1 N1 109.6(4) 7_565
N3 Be1 N1 109.6(4) .
N2 Be1 N1 111.2(5) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
N1 Be1 1.736(12) .
N1 H1A 0.9100 .
N1 H1B 0.9100 .
N1 H1C 0.9100 .
N2 Be1 1.730(11) .
N2 H2A 0.9100 .
N2 H2B 0.9100 .
N2 H2C 0.9100 .
N3 Be1 1.716(7) .
N3 H3A 0.9100 .
N3 H3B 0.9100 .
N3 H3C 0.9100 .
Be1 N3 1.716(7) 7_565
