# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3
_database_code_depnum_ccdc_archive 'CCDC 1956201'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'N6, 4(H3 N), Be'
_chemical_formula_sum            'Be H12 N10'
_chemical_formula_weight         161.21

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'

_space_group_crystal_system      tetragonal
_space_group_IT_number           121
_space_group_name_H-M_alt        'I -4 2 m'
_space_group_name_Hall           'I -4 2'

_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.
;

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'

_cell_length_a                   8.0140(3)
_cell_length_b                   8.0140(3)
_cell_length_c                   6.4519(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     414.37(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1332
_cell_measurement_theta_min      17.65
_cell_measurement_theta_max      156.44

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_F_000             172
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    0.847
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2629
_exptl_absorpt_correction_T_max  0.9419
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            725
_diffrn_reflns_av_unetI/netI     0.0138
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         8.824
_diffrn_reflns_theta_max         78.225
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_point_group_measured_fraction_full 0.962
_reflns_number_total             234
_reflns_number_gt                232
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.550
_reflns_Friedel_fraction_max     0.874
_reflns_Friedel_fraction_full    0.924

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0759P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.049(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         234
_refine_ls_number_parameters     26
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0339
_refine_ls_R_factor_gt           0.0334
_refine_ls_wR_factor_ref         0.0946
_refine_ls_wR_factor_gt          0.0945
_refine_ls_goodness_of_fit_ref   1.188
_refine_ls_restrained_S_all      1.188
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 Be1 1.7242(18) . ?
N2 N3 1.1822(18) . ?

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
_geom_angle_publ_flag
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_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

_refine_diff_density_max         0.185
_refine_diff_density_min         -0.145
_refine_diff_density_rms         0.042

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 1956203'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            diamminberylliumbromide
_chemical_melting_point          ?
_chemical_formula_moiety         '2(Br), 2(H3 N), Be'
_chemical_formula_sum            'Be Br2 H6 N2'
_chemical_formula_weight         202.90

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   6.8278(2)
_cell_length_b                   12.2863(2)
_cell_length_c                   6.9291(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.446(2)
_cell_angle_gamma                90
_cell_volume                     569.71(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    23274
_cell_measurement_theta_min      7.19
_cell_measurement_theta_max      159.14

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.366
_exptl_crystal_F_000             376
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    16.827
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0982
_exptl_absorpt_correction_T_max  0.4248
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14114
_diffrn_reflns_av_unetI/netI     0.0094
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         7.209
_diffrn_reflns_theta_max         78.914
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1225
_reflns_number_gt                1151
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0358P)²+0.2563P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00117(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1225
_refine_ls_number_parameters     49
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0215
_refine_ls_R_factor_gt           0.0195
_refine_ls_wR_factor_ref         0.0507
_refine_ls_wR_factor_gt          0.0498
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Be1 2.183(3) . ?
Br2 Be1 2.219(3) . ?
N1 Be1 1.710(4) . ?
N2 Be1 1.717(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
_geom_angle_publ_flag
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_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

_refine_diff_density_max         0.394
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.097

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1956207'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Be H12 I2 N4'
_chemical_formula_weight         330.95

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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.
;

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'

_cell_length_a                   9.9007(2)
_cell_length_b                   7.3274(2)
_cell_length_c                   12.7965(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     928.34(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    15988
_cell_measurement_theta_min      6.91
_cell_measurement_theta_max      154.38

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.368
_exptl_crystal_F_000             600
_exptl_transmission_factor_min   0.0000
_exptl_transmission_factor_max   0.0001
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.065
_exptl_absorpt_coefficient_mu    52.617
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0000
_exptl_absorpt_correction_T_max  0.0001
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            8664
_diffrn_reflns_av_unetI/netI     0.0141
_diffrn_reflns_av_R_equivalents  0.0354
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         5.650
_diffrn_reflns_theta_max         76.386
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             1056
_reflns_number_gt                1034
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0821P)²+1.2286P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1056
_refine_ls_number_parameters     43
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0407
_refine_ls_wR_factor_ref         0.1123
_refine_ls_wR_factor_gt          0.1116
_refine_ls_goodness_of_fit_ref   1.186
_refine_ls_restrained_S_all      1.186
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
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 ?

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
_geom_angle_publ_flag
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) . . ?

_refine_diff_density_max         2.331
_refine_diff_density_min         -1.981
_refine_diff_density_rms         0.321

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4
_database_code_depnum_ccdc_archive 'CCDC 1956205'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Be Br2 H36 N12'
_chemical_formula_weight         373.24

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   10.4450(2)
_cell_length_b                   11.5311(2)
_cell_length_c                   16.3117(5)
_cell_angle_alpha                90
_cell_angle_beta                 101.353(2)
_cell_angle_gamma                90
_cell_volume                     1926.18(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12027
_cell_measurement_theta_min      5.53
_cell_measurement_theta_max      153.98

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   0.3743
_exptl_transmission_factor_max   0.7913
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.6
_exptl_crystal_size_min          0.6
_exptl_absorpt_coefficient_mu    5.340
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3743
_exptl_absorpt_correction_T_max  0.7913
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            9265
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_av_R_equivalents  0.0186
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         4.728
_diffrn_reflns_theta_max         76.386
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             3782
_reflns_number_gt                3487
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0421P)²+0.3056P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00092(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3782
_refine_ls_number_parameters     291
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0265
_refine_ls_R_factor_gt           0.0234
_refine_ls_wR_factor_ref         0.0600
_refine_ls_wR_factor_gt          0.0586
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.048
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.93010(2) 0.20190(2) 0.11211(2) 0.02058(7) Uani 1 1 d . . . . .
Br2 Br 0.39660(2) 0.25809(2) 0.42883(2) 0.02289(8) Uani 1 1 d . . . . .
N1 N 0.85237(14) 0.33799(14) 0.28691(9) 0.0180(3) Uani 1 1 d . . . . .
N2 N 0.80761(14) 0.14225(14) 0.37882(10) 0.0190(3) Uani 1 1 d . . . . .
N3 N 0.71515(14) 0.36072(14) 0.41784(9) 0.0182(3) Uani 1 1 d . . . . .
N4 N 0.59534(15) 0.24830(14) 0.27079(10) 0.0188(3) Uani 1 1 d . . . . .
N5 N 0.71663(16) 0.61793(16) 0.37763(12) 0.0282(4) Uani 1 1 d . . . . .
N7 N 0.84950(19) 0.57969(16) 0.20405(11) 0.0289(4) Uani 1 1 d . . . . .
N8 N 0.60367(16) 0.08314(17) 0.12302(11) 0.0256(3) Uani 1 1 d . . . . .
N9 N 0.8283(2) -0.07047(19) 0.26515(13) 0.0340(4) Uani 1 1 d . . . . .
N10 N 1.07182(15) 0.39575(16) 0.42741(11) 0.0242(3) Uani 1 1 d . . . . .
N11 N 1.09093(16) 0.11730(16) 0.48605(11) 0.0241(3) Uani 1 1 d . . . . .
N12 N 0.67106(18) 0.07388(19) 0.52165(12) 0.0330(4) Uani 1 1 d . . . . .
Be1 Be 0.7434(2) 0.2720(2) 0.33714(14) 0.0158(4) Uani 1 1 d . . . . .
H1A H 0.924(2) 0.354(2) 0.3270(16) 0.030(6) Uiso 1 1 d . . . . .
H1B H 0.831(2) 0.408(3) 0.2620(16) 0.038(7) Uiso 1 1 d . . . . .
H1C H 0.868(2) 0.298(2) 0.2470(16) 0.027(6) Uiso 1 1 d . . . . .
H2A H 0.803(2) 0.087(2) 0.3441(16) 0.032(6) Uiso 1 1 d . . . . .
H2B H 0.764(2) 0.119(2) 0.4164(16) 0.030(6) Uiso 1 1 d . . . . .
H2C H 0.890(2) 0.149(2) 0.4059(15) 0.024(6) Uiso 1 1 d . . . . .
H3A H 0.775(3) 0.349(2) 0.4625(16) 0.031(6) Uiso 1 1 d . . . . .
H3B H 0.639(3) 0.346(2) 0.4321(17) 0.041(7) Uiso 1 1 d . . . . .
H3C H 0.712(2) 0.442(3) 0.4011(17) 0.040(7) Uiso 1 1 d . . . . .
H4A H 0.571(2) 0.307(2) 0.2456(16) 0.030(7) Uiso 1 1 d . . . . .
H4B H 0.540(2) 0.2257(19) 0.3017(15) 0.019(5) Uiso 1 1 d . . . . .
H4C H 0.601(2) 0.197(2) 0.2359(17) 0.032(7) Uiso 1 1 d . . . . .
H5A H 0.666(3) 0.645(3) 0.329(2) 0.063(10) Uiso 1 1 d . . . . .
H5B H 0.685(3) 0.660(3) 0.414(2) 0.056(9) Uiso 1 1 d . . . . .
H5C H 0.794(3) 0.641(2) 0.3768(16) 0.033(7) Uiso 1 1 d . . . . .
H7A H 0.789(3) 0.629(3) 0.1850(18) 0.043(8) Uiso 1 1 d . . . . .
H7B H 0.897(3) 0.571(3) 0.1677(19) 0.049(9) Uiso 1 1 d . . . . .
H7C H 0.899(3) 0.611(3) 0.2478(19) 0.046(8) Uiso 1 1 d . . . . .
H8A H 0.680(3) 0.103(3) 0.1203(17) 0.041(7) Uiso 1 1 d . . . . .
H8B H 0.551(3) 0.115(3) 0.0800(18) 0.043(8) Uiso 1 1 d . . . . .
H8C H 0.595(3) 0.009(3) 0.1140(19) 0.047(8) Uiso 1 1 d . . . . .
H9A H 0.768(4) -0.111(3) 0.238(2) 0.070(11) Uiso 1 1 d . . . . .
H9B H 0.872(4) -0.037(4) 0.227(3) 0.105(15) Uiso 1 1 d . . . . .
H9C H 0.882(3) -0.120(3) 0.297(2) 0.054(9) Uiso 1 1 d . . . . .
H10A H 1.051(2) 0.372(2) 0.4736(17) 0.034(7) Uiso 1 1 d . . . . .
H10B H 1.152(3) 0.369(2) 0.4291(16) 0.035(7) Uiso 1 1 d . . . . .
H10C H 1.074(2) 0.475(3) 0.4277(17) 0.037(7) Uiso 1 1 d . . . . .
H11A H 1.154(3) 0.154(3) 0.4763(19) 0.050(8) Uiso 1 1 d . . . . .
H11B H 1.067(3) 0.150(3) 0.5231(18) 0.039(7) Uiso 1 1 d . . . . .
H11C H 1.123(3) 0.051(3) 0.5036(18) 0.049(8) Uiso 1 1 d . . . . .
H12A H 0.721(3) 0.110(3) 0.5624(19) 0.046(8) Uiso 1 1 d . . . . .
H12B H 0.602(3) 0.115(3) 0.5133(18) 0.042(7) Uiso 1 1 d . . . . .
H12C H 0.655(3) 0.004(3) 0.541(2) 0.062(10) Uiso 1 1 d . . . . .
N6A N 0.459(3) 0.443(3) 0.162(2) 0.053(6) Uani 0.30(4) 1 d . U P A 1
N6B N 0.4966(10) 0.4709(5) 0.1940(7) 0.036(2) Uani 0.70(4) 1 d . U P A 2
H6A H 0.448(4) 0.489(4) 0.219(3) 0.084(14) Uiso 1 1 d . . . B 2
H6B H 0.554(4) 0.510(4) 0.185(3) 0.106(18) Uiso 1 1 d . . . C 2
H6C H 0.438(6) 0.458(7) 0.139(4) 0.16(4) Uiso 1 1 d . . . D 2

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 0.01678(10) 0.02724(12) 0.01889(10) -0.00464(7) 0.00634(7) -0.00188(6)
Br2 0.01352(10) 0.02657(12) 0.03004(12) -0.00177(7) 0.00783(7) -0.00099(6)
N1 0.0203(7) 0.0181(8) 0.0169(7) -0.0016(6) 0.0069(6) -0.0010(5)
N2 0.0159(7) 0.0196(8) 0.0222(7) 0.0010(6) 0.0053(6) 0.0010(5)
N3 0.0141(6) 0.0235(8) 0.0175(7) -0.0031(6) 0.0048(5) -0.0003(5)
N4 0.0167(7) 0.0218(8) 0.0174(7) -0.0018(6) 0.0025(6) 0.0010(5)
N5 0.0191(7) 0.0316(10) 0.0334(9) -0.0025(7) 0.0037(7) -0.0014(6)
N7 0.0374(9) 0.0271(9) 0.0224(8) 0.0031(7) 0.0057(7) -0.0011(7)
N8 0.0200(8) 0.0320(10) 0.0256(8) -0.0029(7) 0.0063(6) -0.0004(6)
N9 0.0326(9) 0.0386(11) 0.0309(9) -0.0051(8) 0.0061(8) 0.0106(8)
N10 0.0209(7) 0.0271(9) 0.0244(8) 0.0037(7) 0.0041(6) 0.0031(6)
N11 0.0240(8) 0.0227(8) 0.0271(8) 0.0026(7) 0.0089(6) 0.0033(6)
N12 0.0307(9) 0.0354(11) 0.0367(10) 0.0118(9) 0.0159(8) 0.0100(8)
Be1 0.0137(9) 0.0183(10) 0.0162(10) 0.0008(8) 0.0051(8) 0.0004(7)
N6A 0.048(7) 0.060(9) 0.056(11) 0.020(9) 0.024(8) 0.020(7)
N6B 0.045(3) 0.027(2) 0.043(4) 0.0063(19) 0.023(3) 0.0134(18)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 Be1 1.707(3) . ?
N1 H1A 0.91(3) . ?
N1 H1B 0.92(3) . ?
N1 H1C 0.84(3) . ?
N2 Be1 1.724(3) . ?
N2 H2A 0.85(3) . ?
N2 H2B 0.88(3) . ?
N2 H2C 0.89(2) . ?
N3 Be1 1.737(3) . ?
N3 H3A 0.87(3) . ?
N3 H3B 0.89(3) . ?
N3 H3C 0.97(3) . ?
N4 Be1 1.726(3) . ?
N4 H4A 0.80(3) . ?
N4 H4B 0.88(2) . ?
N4 H4C 0.83(3) . ?
N5 H5A 0.91(4) . ?
N5 H5B 0.88(3) . ?
N5 H5C 0.86(3) . ?
N7 H7A 0.86(3) . ?
N7 H7B 0.85(3) . ?
N7 H7C 0.87(3) . ?
N8 H8A 0.84(3) . ?
N8 H8B 0.88(3) . ?
N8 H8C 0.87(3) . ?
N9 H9A 0.84(4) . ?
N9 H9B 0.93(4) . ?
N9 H9C 0.88(3) . ?
N10 H10A 0.87(3) . ?
N10 H10B 0.89(3) . ?
N10 H10C 0.91(3) . ?
N11 H11A 0.83(3) . ?
N11 H11B 0.79(3) . ?
N11 H11C 0.86(3) . ?
N12 H12A 0.86(3) . ?
N12 H12B 0.85(3) . ?
N12 H12C 0.89(4) . ?
N6B H6A 0.73(4) . ?
N6B H6B 0.78(5) . ?
N6B H6C 0.99(7) . ?

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
_geom_angle_publ_flag
Be1 N1 H1A 106.0(15) . . ?
Be1 N1 H1B 118.9(16) . . ?
H1A N1 H1B 103(2) . . ?
Be1 N1 H1C 112.1(17) . . ?
H1A N1 H1C 114(2) . . ?
H1B N1 H1C 102(2) . . ?
Be1 N2 H2A 115.0(18) . . ?
Be1 N2 H2B 108.9(16) . . ?
H2A N2 H2B 106(2) . . ?
Be1 N2 H2C 112.6(16) . . ?
H2A N2 H2C 109(2) . . ?
H2B N2 H2C 105(2) . . ?
Be1 N3 H3A 109.7(16) . . ?
Be1 N3 H3B 112.5(18) . . ?
H3A N3 H3B 107(2) . . ?
Be1 N3 H3C 110.7(15) . . ?
H3A N3 H3C 111(2) . . ?
H3B N3 H3C 106(2) . . ?
Be1 N4 H4A 110.0(18) . . ?
Be1 N4 H4B 107.3(15) . . ?
H4A N4 H4B 111(2) . . ?
Be1 N4 H4C 111.3(18) . . ?
H4A N4 H4C 108(3) . . ?
H4B N4 H4C 109(2) . . ?
H5A N5 H5B 99(3) . . ?
H5A N5 H5C 106(3) . . ?
H5B N5 H5C 109(3) . . ?
H7A N7 H7B 108(3) . . ?
H7A N7 H7C 108(3) . . ?
H7B N7 H7C 106(3) . . ?
H8A N8 H8B 107(3) . . ?
H8A N8 H8C 109(3) . . ?
H8B N8 H8C 104(3) . . ?
H9A N9 H9B 107(3) . . ?
H9A N9 H9C 105(3) . . ?
H9B N9 H9C 109(3) . . ?
H10A N10 H10B 105(2) . . ?
H10A N10 H10C 109(2) . . ?
H10B N10 H10C 109(2) . . ?
H11A N11 H11B 107(3) . . ?
H11A N11 H11C 105(3) . . ?
H11B N11 H11C 109(3) . . ?
H12A N12 H12B 103(3) . . ?
H12A N12 H12C 106(3) . . ?
H12B N12 H12C 111(3) . . ?
N1 Be1 N2 109.36(13) . . ?
N1 Be1 N4 111.69(14) . . ?
N2 Be1 N4 109.92(14) . . ?
N1 Be1 N3 109.28(14) . . ?
N2 Be1 N3 108.85(14) . . ?
N4 Be1 N3 107.69(13) . . ?
H6A N6B H6B 125(5) . . ?
H6A N6B H6C 100(4) . . ?
H6B N6B H6C 106(5) . . ?

_refine_diff_density_max         0.684
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.065

_shelx_res_file                  
;

    4.res created by SHELXL-2014/7


TITL 1_a.res in P2(1)/c
REM Old TITL 1 in P2(1)/c

REM SHELXT solution in P2(1)/c
REM R1 0.090,  Rweak 0.004,  Alpha 0.023,  Orientation as input
REM Formula found by SHELXT:  Be N12 Br2

CELL  1.54178  10.4450  11.5311  16.3117   90.000  101.353   90.000
ZERR   4.000   0.0002   0.0002   0.0005    0.000    0.002    0.000
LATT  1
SYMM -X, 1/2+Y, 1/2-Z
SFAC BE H N BR
UNIT 4 144 48 8
L.S. 10
BOND $H
LIST 4
ACTA
ISOR 0.01 N6A N6B
SIMU 0.04 N6A N6B
DELU 0.01 N6A N6B
TEMP -173.15
REM DFIX 0.910 N5 H5A
REM DFIX 0.910 N5 H5B
REM DFIX 0.910 N5 H5C
REM DFIX 1.486 H5A H5B
REM DFIX 1.486 H5C H5B
REM DFIX 1.486 H5A H5C
REM DFIX 0.910 N10 H10A
REM DFIX 0.910 N10 H10B
REM DFIX 0.910 N10 H10C
REM DFIX 1.486 H10A H10B
REM DFIX 1.486 H10C H10B
REM DFIX 1.486 H10A H10C
REM DFIX 0.910 N7 H7A
REM DFIX 0.910 N7 H7B
REM DFIX 0.910 N7 H7C
REM DFIX 1.486 H7A H7B
REM DFIX 1.486 H7C H7B
REM DFIX 1.486 H7A H7C
REM DFIX 0.910 N12 H12A
REM DFIX 0.910 N12 H12B
REM DFIX 0.910 N12 H12C
REM DFIX 1.486 H12A H12B
REM DFIX 1.486 H12C H12B
REM DFIX 1.486 H12A H12C
REM DFIX 0.910 N11 H11A
REM DFIX 0.910 N11 H11B
REM DFIX 0.910 N11 H11C
REM DFIX 1.486 H11A H11B
REM DFIX 1.486 H11C H11B
REM DFIX 1.486 H11A H11C
REM DFIX 0.910 N9 H9A
REM DFIX 0.910 N9 H9B
REM DFIX 0.910 N9 H9C
REM DFIX 1.486 H9A H9B
REM DFIX 1.486 H9C H9B
REM DFIX 1.486 H9A H9C
REM DFIX 0.910 N8 H8A
REM DFIX 0.910 N8 H8B
REM DFIX 0.910 N8 H8C
REM DFIX 1.486 H8A H8B
REM DFIX 1.486 H8C H8B
REM DFIX 1.486 H8A H8C
REM DFIX 0.910 N6B H6A
REM DFIX 0.910 N6B H6B
REM DFIX 0.910 N6B H6C
REM DFIX 1.486 H6A H6B
REM DFIX 1.486 H6C H6B
REM DFIX 1.486 H6A H6C
FMAP 2
EQIV $1 1-x, 0.5+y, 1.5-z
EQIV $2 x, y, z
EQIV $3 1-x, 0.5+y, 0.5-z
EQIV $4 1-x, 1-y, 1-z
EQIV $5 x, 0.5-y, 0.5+z
EQIV $6 2-x, 0.5+y, 1.5-z
EQIV $7 1-x, -0.5+y, 0.5-z
EQIV $8 -1+x, 0.5-y, 0.5+z
EQIV $9 -1+x, 0.5-y, -0.5+z
EQIV $10 x, 1.5-y, 0.5+z
EQIV $11 x, 1+y, z
EQIV $12 2-x, 1-y, 1-z
EQIV $13 1-x, -y, 1-z
EQIV $14 -1+x, y, z
EQIV $15 2-x, 0.5+y, 0.5-z
EQIV $16 x, 0.5-y, -0.5+z
HTAB
PLAN 20
WGHT    0.042100    0.305600
EXTI    0.000921
FVAR       0.29965   0.30350
BR1   4    0.930098    0.201900    0.112107    11.00000    0.01678    0.02724 =
         0.01889   -0.00464    0.00634   -0.00188
BR2   4    0.396597    0.258088    0.428833    11.00000    0.01352    0.02657 =
         0.03004   -0.00177    0.00783   -0.00099
N1    3    0.852365    0.337987    0.286910    11.00000    0.02027    0.01809 =
         0.01690   -0.00156    0.00689   -0.00097
N2    3    0.807610    0.142254    0.378817    11.00000    0.01590    0.01962 =
         0.02220    0.00104    0.00534    0.00102
N3    3    0.715148    0.360720    0.417841    11.00000    0.01410    0.02352 =
         0.01753   -0.00310    0.00481   -0.00034
N4    3    0.595339    0.248298    0.270790    11.00000    0.01671    0.02178 =
         0.01743   -0.00184    0.00253    0.00097
N5    3    0.716635    0.617934    0.377629    11.00000    0.01914    0.03157 =
         0.03337   -0.00254    0.00375   -0.00140
N7    3    0.849496    0.579695    0.204050    11.00000    0.03736    0.02707 =
         0.02236    0.00310    0.00574   -0.00105
N8    3    0.603665    0.083144    0.123019    11.00000    0.01997    0.03199 =
         0.02555   -0.00293    0.00628   -0.00044
N9    3    0.828338   -0.070466    0.265153    11.00000    0.03257    0.03862 =
         0.03086   -0.00505    0.00606    0.01056
N10   3    1.071820    0.395755    0.427408    11.00000    0.02092    0.02708 =
         0.02442    0.00368    0.00411    0.00314
N11   3    1.090926    0.117298    0.486046    11.00000    0.02395    0.02269 =
         0.02712    0.00264    0.00892    0.00328
N12   3    0.671056    0.073882    0.521648    11.00000    0.03071    0.03536 =
         0.03665    0.01182    0.01585    0.01000
BE1   1    0.743366    0.272041    0.337137    11.00000    0.01369    0.01833 =
         0.01620    0.00084    0.00509    0.00040
H1A   2    0.923743    0.354189    0.327029    11.00000    0.02999
H1B   2    0.831267    0.408475    0.262021    11.00000    0.03800
H1C   2    0.868111    0.297757    0.247009    11.00000    0.02711
H2A   2    0.802743    0.086980    0.344113    11.00000    0.03217
H2B   2    0.763935    0.119160    0.416448    11.00000    0.02955
H2C   2    0.890020    0.148943    0.405946    11.00000    0.02432
H3A   2    0.775406    0.348911    0.462481    11.00000    0.03123
H3B   2    0.639112    0.346276    0.432098    11.00000    0.04109
H3C   2    0.712343    0.441823    0.401105    11.00000    0.04025
H4A   2    0.570891    0.306695    0.245613    11.00000    0.03023
H4B   2    0.539795    0.225674    0.301740    11.00000    0.01875
H4C   2    0.601324    0.197403    0.235909    11.00000    0.03162
H5A   2    0.665736    0.645087    0.329310    11.00000    0.06333
H5B   2    0.684634    0.660441    0.413988    11.00000    0.05615
H5C   2    0.794426    0.640744    0.376838    11.00000    0.03319
H7A   2    0.789474    0.628649    0.185010    11.00000    0.04346
H7B   2    0.896880    0.571371    0.167705    11.00000    0.04856
H7C   2    0.899316    0.610527    0.247850    11.00000    0.04588
H8A   2    0.679927    0.103191    0.120259    11.00000    0.04101
H8B   2    0.550529    0.114709    0.079971    11.00000    0.04299
H8C   2    0.594955    0.008900    0.113960    11.00000    0.04691
H9A   2    0.768112   -0.111409    0.238042    11.00000    0.07024
H9B   2    0.871953   -0.037102    0.226608    11.00000    0.10498
H9C   2    0.881545   -0.119686    0.296580    11.00000    0.05406
H10A  2    1.051261    0.372128    0.473637    11.00000    0.03368
H10B  2    1.152146    0.368553    0.429071    11.00000    0.03521
H10C  2    1.074322    0.474899    0.427721    11.00000    0.03654
H11A  2    1.154283    0.154466    0.476292    11.00000    0.05003
H11B  2    1.066843    0.149970    0.523070    11.00000    0.03945
H11C  2    1.122907    0.050900    0.503649    11.00000    0.04915
H12A  2    0.721036    0.109507    0.562391    11.00000    0.04600
H12B  2    0.602218    0.114938    0.513341    11.00000    0.04214
H12C  2    0.655473    0.004293    0.540905    11.00000    0.06227
PART 1
N6A   3    0.459026    0.442845    0.162224    21.00000    0.04832    0.05973 =
         0.05583    0.01976    0.02410    0.02038
PART 2
N6B   3    0.496642    0.470898    0.194039   -21.00000    0.04481    0.02652 =
         0.04257    0.00629    0.02254    0.01336
H6A   2    0.448049    0.488796    0.218547    11.00000    0.08446
H6B   2    0.553773    0.509841    0.185308    11.00000    0.10644
H6C   2    0.438288    0.457774    0.139317    11.00000    0.16000
PART 0
HKLF 4

REM  1_a.res in P2(1)/c
REM R1 =  0.0234 for    3487 Fo > 4sig(Fo)  and  0.0265 for all    3782 data
REM    291 parameters refined using     18 restraints

END

WGHT      0.0421      0.3056

REM Instructions for potential hydrogen bonds
HTAB N1 N10
HTAB N1 N7
HTAB N1 Br1
HTAB N2 N9
HTAB N2 N12
HTAB N2 N11
HTAB N3 Br1_$5
HTAB N3 Br2
HTAB N3 N5
HTAB N4 N6A
HTAB N4 N6B
HTAB N4 Br2
HTAB N4 N8
HTAB N5 Br2_$4
HTAB N5 Br1_$15
HTAB N7 Br2_$3
HTAB N7 N11_$15
HTAB N7 Br1_$15
HTAB N8 Br1
HTAB N8 Br2_$16
HTAB N8 Br2_$7
EQIV $17 -x+2, y-1/2, -z+1/2
HTAB N9 Br1_$17
HTAB N10 Br1_$5
EQIV $18 x+1, y, z
HTAB N10 Br2_$18
HTAB N10 Br1_$15
HTAB N11 Br2_$18
HTAB N11 Br1_$5
EQIV $19 -x+2, -y, -z+1
HTAB N11 N12_$19
HTAB N12 Br1_$5
HTAB N12 Br2
HTAB N12 Br2_$13

REM Highest difference peak  0.684,  deepest hole -0.573,  1-sigma level  0.065
Q1    1   0.8985  0.2042  0.1562  11.00000  0.05    0.68
Q2    1   0.4253  0.2535  0.3840  11.00000  0.05    0.65
Q3    1   0.3656  0.2631  0.4725  11.00000  0.05    0.63
Q4    1   0.9613  0.2045  0.0694  11.00000  0.05    0.61
Q5    1   0.8545  0.1929  0.0729  11.00000  0.05    0.49
Q6    1   1.0032  0.2075  0.1510  11.00000  0.05    0.44
Q7    1   0.4626  0.2456  0.4697  11.00000  0.05    0.38
Q8    1   0.5165  0.2465  0.3631  11.00000  0.05    0.35
Q9    1   0.3302  0.2509  0.3909  11.00000  0.05    0.32
Q10   1   0.7248  0.7423  0.4953  11.00000  0.05    0.31
Q11   1   0.8225  0.2002  0.1912  11.00000  0.05    0.31
Q12   1   1.0524  0.2834  0.5434  11.00000  0.05    0.30
Q13   1   0.7375  0.3428  0.3737  11.00000  0.05    0.28
Q14   1   0.7629  0.2001  0.3494  11.00000  0.05    0.27
Q15   1   0.9291  0.1078  0.1160  11.00000  0.05    0.26
Q16   1   0.7963  0.2973  0.3111  11.00000  0.05    0.24
Q17   1   0.8659  0.0688  0.1654  11.00000  0.05    0.22
Q18   1   0.3964  0.3305  0.4308  11.00000  0.05    0.22
Q19   1   0.8252  0.3401  0.3273  11.00000  0.05    0.22
Q20   1   0.4051  0.3582  0.3992  11.00000  0.05    0.21
;
_shelx_res_checksum              62310
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1956206'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Be H6 I2 N2'
_chemical_formula_sum            'Be H6 I2 N2'
_chemical_formula_weight         296.88

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   7.2739(4)
_cell_length_b                   13.1326(6)
_cell_length_c                   7.3586(4)
_cell_angle_alpha                90
_cell_angle_beta                 102.674(5)
_cell_angle_gamma                90
_cell_volume                     685.80(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    10557
_cell_measurement_theta_min      14.06
_cell_measurement_theta_max      158.44

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.875
_exptl_crystal_F_000             520
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    71.021
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0010
_exptl_absorpt_correction_T_max  0.6156
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            11337
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_av_R_equivalents  0.0613
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         7.029
_diffrn_reflns_theta_max         79.205
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1482
_reflns_number_gt                1219
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0703P)²+10.2968P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00060(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1482
_refine_ls_number_parameters     49
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0485
_refine_ls_wR_factor_ref         0.1285
_refine_ls_wR_factor_gt          0.1170
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Be1 2.451(14) . ?
N1 Be1 1.712(17) . ?
Be1 N2 1.699(19) . ?
Be1 I2 2.417(16) . ?

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
_geom_angle_publ_flag
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_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

_refine_diff_density_max         1.522
_refine_diff_density_min         -2.272
_refine_diff_density_rms         0.302

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1956209'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        Tetramminberylliumbromide
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Be Br2 H12 N4'
_chemical_formula_sum            'Be Br2 H12 N4'
_chemical_formula_weight         236.97

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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_H-M_alt        'P n m a'
_space_group_name_Hall           '-P 2ac 2n'

_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.
;

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'

_cell_length_a                   9.5332(2)
_cell_length_b                   6.93550(10)
_cell_length_c                   12.2289(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     808.54(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    27341
_cell_measurement_theta_min      7.23
_cell_measurement_theta_max      160.05

_exptl_crystal_description       plate
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.947
_exptl_crystal_F_000             456
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    12.030
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0387
_exptl_absorpt_correction_T_max  0.4613
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            13697
_diffrn_reflns_av_unetI/netI     0.0060
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         5.885
_diffrn_reflns_theta_max         79.113
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             948
_reflns_number_gt                946
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0202P)²+0.9261P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00279(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         948
_refine_ls_number_parameters     44
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0451
_refine_ls_wR_factor_gt          0.0450
_refine_ls_goodness_of_fit_ref   1.190
_refine_ls_restrained_S_all      1.190
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
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

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 Be1 1.744(4) . ?
N2 Be1 1.720(4) . ?
N3 Be1 1.709(3) . ?

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
_geom_angle_publ_flag
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_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

_refine_diff_density_max         0.360
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.100

_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
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1956204'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Be Cl2 H6 N2'
_chemical_formula_sum            'Be Cl2 H6 N2'
_chemical_formula_weight         113.98

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'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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'

_cell_length_a                   6.5519(2)
_cell_length_b                   11.8065(3)
_cell_length_c                   6.6589(2)
_cell_angle_alpha                90
_cell_angle_beta                 100.321(3)
_cell_angle_gamma                90
_cell_volume                     506.76(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14658
_cell_measurement_theta_min      15.00
_cell_measurement_theta_max      158.15

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_F_000             232
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_absorpt_coefficient_mu    10.140
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.0736
_exptl_absorpt_correction_T_max  0.5133
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            8180
_diffrn_reflns_av_unetI/netI     0.0142
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         7.504
_diffrn_reflns_theta_max         78.689
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1092
_reflns_number_gt                1005
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0672P)²+0.1590P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0045(13)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1092
_refine_ls_number_parameters     71
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0338
_refine_ls_wR_factor_ref         0.0957
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.78768(6) 0.54333(4) 0.71281(7) 0.0277(2) Uani 1 1 d . . . . .
Cl2 Cl 0.94067(7) 0.75300(4) 0.43330(7) 0.0302(2) Uani 1 1 d . . . . .
N1 N 0.7126(3) 0.54428(15) 0.2446(3) 0.0283(4) Uani 1 1 d . . . . .
N2 N 0.4864(3) 0.70013(15) 0.4421(3) 0.0285(4) Uani 1 1 d . . . . .
Be1 Be 0.7213(4) 0.6347(2) 0.4488(4) 0.0273(5) Uani 1 1 d . . . . .
H1 H 0.828(5) 0.512(3) 0.249(5) 0.041(7) Uiso 1 1 d . . . . .
H2 H 0.624(5) 0.495(3) 0.246(4) 0.041(7) Uiso 1 1 d . . . . .
H3 H 0.680(4) 0.576(2) 0.136(5) 0.030(6) Uiso 1 1 d . . . . .
H4 H 0.384(5) 0.657(3) 0.407(5) 0.050(8) Uiso 1 1 d . . . . .
H5 H 0.458(5) 0.763(3) 0.366(5) 0.040(7) Uiso 1 1 d . . . . .
H6 H 0.473(5) 0.724(3) 0.550(5) 0.042(8) Uiso 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
Cl1 0.0242(3) 0.0261(3) 0.0322(3) 0.00155(15) 0.00330(18) 0.00088(15)
Cl2 0.0280(3) 0.0292(3) 0.0331(3) -0.00103(16) 0.00463(19) -0.00613(16)
N1 0.0252(9) 0.0265(9) 0.0323(9) -0.0001(7) 0.0022(7) -0.0007(7)
N2 0.0261(8) 0.0282(9) 0.0308(8) 0.0009(7) 0.0040(6) 0.0013(7)
Be1 0.0226(11) 0.0261(11) 0.0328(12) -0.0011(9) 0.0038(9) -0.0003(9)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 Be1 2.042(3) . ?
Cl2 Be1 2.020(3) . ?
N1 Be1 1.722(3) . ?
N2 Be1 1.715(3) . ?

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
_geom_angle_publ_flag
N2 Be1 N1 110.86(16) . . ?
N2 Be1 Cl2 109.31(14) . . ?
N1 Be1 Cl2 108.17(14) . . ?
N2 Be1 Cl1 108.17(14) . . ?
N1 Be1 Cl1 108.91(14) . . ?
Cl2 Be1 Cl1 111.44(12) . . ?

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 H3 Cl2 0.81(3) 2.76(3) 3.4461(19) 145(2) 4_575 yes
N1 H2 Cl1 0.82(3) 2.80(3) 3.4966(18) 144(3) 3_666 yes
N1 H1 Cl1 0.84(3) 2.57(3) 3.3969(18) 168(3) 3_766 yes
N2 H6 Cl2 0.79(3) 2.62(3) 3.3831(19) 165(3) 4_576 yes
N2 H5 Cl2 0.90(3) 2.87(3) 3.3929(19) 119(2) 4_575 yes
N2 H5 Cl1 0.90(3) 2.67(3) 3.5338(18) 163(3) 4_575 yes
N2 H4 Cl1 0.84(4) 2.68(4) 3.4478(19) 153(3) 3_666 yes

_refine_diff_density_max         0.316
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.080

_shelx_res_file                  
;
TITL 1_a.res in P2(1)/n
    4.res
    created by SHELXL-2018/3 at 11:15:04 on 04-Feb-2019
REM Old TITL 1 in P2(1)/n
REM SHELXT solution in P2(1)/n: R1 0.135, Rweak 0.003, Alpha 0.006
REM <I/s>   0.817 for   59 systematic absences,  Orientation as input
REM Formula found by SHELXT:  N3 Br2
CELL  1.54178   6.5519  11.8065   6.6589   90.000  100.321   90.000
ZERR    4.000   0.0002   0.0003   0.0002    0.000    0.003    0.000
LATT  1
SYMM 1/2-X, 1/2+Y, 1/2-Z
SFAC BE H N Cl
UNIT 4 24 8 8
L.S. 10
BOND
LIST 4
ACTA
HTAB
EQIV $1 x-1/2, -y+3/2, z-1/2
HTAB N1 Cl2_$1
EQIV $2 -x+1, -y+1, -z+1
HTAB N1 Cl1_$2
EQIV $3 -x+2, -y+1, -z+1
HTAB N1 Cl1_$3
EQIV $4 x-1/2, -y+3/2, z+1/2
HTAB N2 Cl2_$4
HTAB N2 Cl2_$1
HTAB N2 Cl1_$1
HTAB N2 Cl1_$2
TEMP -173.15
FMAP 2
PLAN 20
WGHT    0.067200    0.159000
EXTI    0.004531
FVAR       0.93458
CL1   4    0.787682    0.543335    0.712814    11.00000    0.02417    0.02613 =
         0.03218    0.00155    0.00330    0.00088
CL2   4    0.940673    0.752999    0.433300    11.00000    0.02798    0.02922 =
         0.03310   -0.00103    0.00463   -0.00613
N1    3    0.712569    0.544276    0.244589    11.00000    0.02515    0.02647 =
         0.03229   -0.00012    0.00218   -0.00069
N2    3    0.486397    0.700129    0.442110    11.00000    0.02605    0.02819 =
         0.03080    0.00090    0.00404    0.00126
BE1   1    0.721308    0.634711    0.448779    11.00000    0.02259    0.02614 =
         0.03276   -0.00112    0.00384   -0.00026
H1    2    0.828399    0.512034    0.249261    11.00000    0.04073
H2    2    0.624304    0.494934    0.246427    11.00000    0.04080
H3    2    0.680336    0.576258    0.136223    11.00000    0.03009
H4    2    0.383986    0.656993    0.407211    11.00000    0.04967
H5    2    0.457907    0.762892    0.366041    11.00000    0.03982
H6    2    0.473383    0.724301    0.549641    11.00000    0.04167
HKLF 4




REM  1_a.res in P2(1)/n
REM wR2 = 0.0957, GooF = S = 1.097, Restrained GooF = 1.097 for all data
REM R1 = 0.0338 for 1005 Fo > 4sig(Fo) and 0.0368 for all 1092 data
REM 71 parameters refined using 0 restraints

END

WGHT      0.0672      0.1590

REM Instructions for potential hydrogen bonds
HTAB N1 Cl1_$3
HTAB N1 Cl1_$2
HTAB N1 Cl2_$1
HTAB N2 Cl1_$2
HTAB N2 Cl1_$1
HTAB N2 Cl2_$1
HTAB N2 Cl2_$4

REM Highest difference peak  0.316,  deepest hole -0.376,  1-sigma level  0.080
Q1    1   0.7206  0.5835  0.3518  11.00000  0.05    0.32
Q2    1   0.7457  0.4453  0.7624  11.00000  0.05    0.28
Q3    1   0.5865  0.7619  0.5828  11.00000  0.05    0.27
Q4    1   1.0078  0.7281  0.6427  11.00000  0.05    0.26
Q5    1   0.7842  0.4511  0.2133  11.00000  0.05    0.26
Q6    1   0.3536  0.5652  0.3433  11.00000  0.05    0.26
Q7    1   0.5889  0.6872  0.4638  11.00000  0.05    0.26
Q8    1   0.9161  0.6807  0.4666  11.00000  0.05    0.25
Q9    1   0.8481  0.4450  0.3963  11.00000  0.05    0.24
Q10   1   0.4357  0.8158  0.4583  11.00000  0.05    0.24
Q11   1   0.7482  0.5030  0.4867  11.00000  0.05    0.22
Q12   1   0.9022  0.4654  0.8437  11.00000  0.05    0.21
Q13   1   0.4478  0.7964  0.6999  11.00000  0.05    0.21
Q14   1   0.4995  0.7193  0.7023  11.00000  0.05    0.21
Q15   1   1.0921  0.7663  0.2986  11.00000  0.05    0.21
Q16   1   0.7729  0.6146  0.9177  11.00000  0.05    0.21
Q17   1   0.7222  0.4686  0.9048  11.00000  0.05    0.20
Q18   1   0.5823  0.6223  0.6726  11.00000  0.05    0.20
Q19   1   0.4342  0.6466  0.7428  11.00000  0.05    0.19
Q20   1   0.6653  0.4939  0.8191  11.00000  0.05    0.19
;
_shelx_res_checksum              11658
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1956208'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H12 Be N6 S2'
_chemical_formula_sum            'C2 H12 Be N6 S2'
_chemical_formula_weight         193.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Be Be 0.0038 0.0014 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   11.9956(5)
_cell_length_b                   11.7990(4)
_cell_length_c                   13.2171(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1870.70(12)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13941
_cell_measurement_theta_min      14.77
_cell_measurement_theta_max      153.70

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_F_000             816
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    4.782
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2409
_exptl_absorpt_correction_T_max  0.7154
_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_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            12196
_diffrn_reflns_av_unetI/netI     0.0135
_diffrn_reflns_av_R_equivalents  0.0194
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         6.236
_diffrn_reflns_theta_max         76.296
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1955
_reflns_number_gt                1746
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0386P)²+0.2314P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00070(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1955
_refine_ls_number_parameters     149
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0204
_refine_ls_wR_factor_ref         0.0556
_refine_ls_wR_factor_gt          0.0541
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_restrained_S_all      0.992
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.43635(2) 0.64717(2) 0.35550(2) 0.01666(9) Uani 1 1 d . . . . .
S2 S 0.66930(2) 0.02843(2) 0.65892(2) 0.01685(9) Uani 1 1 d . . . . .
N1 N 0.29886(8) 0.24135(8) 0.49503(8) 0.01506(19) Uani 1 1 d . . . . .
N2 N 0.27874(8) 0.45547(8) 0.58723(8) 0.0164(2) Uani 1 1 d . . . . .
N3 N 0.09907(8) 0.30373(8) 0.59701(8) 0.01533(19) Uani 1 1 d . . . . .
N4 N 0.29473(8) 0.26050(9) 0.71000(8) 0.01616(19) Uani 1 1 d . . . . .
N5 N 0.45336(8) 0.41099(9) 0.38401(8) 0.0209(2) Uani 1 1 d . . . . .
N6 N 0.44595(8) 0.07486(8) 0.60927(8) 0.0199(2) Uani 1 1 d . . . . .
C1 C 0.44554(9) 0.50832(10) 0.37134(8) 0.0150(2) Uani 1 1 d . . . . .
C2 C 0.53785(9) 0.05564(9) 0.63178(8) 0.0143(2) Uani 1 1 d . . . . .
Be1 Be 0.24295(11) 0.31324(11) 0.59669(11) 0.0132(3) Uani 1 1 d . . . . .
H1A H 0.3396(13) 0.1889(14) 0.5132(12) 0.027(4) Uiso 1 1 d . . . . .
H1B H 0.3364(12) 0.2860(13) 0.4558(12) 0.023(4) Uiso 1 1 d . . . . .
H1C H 0.2510(13) 0.2141(12) 0.4552(12) 0.021(4) Uiso 1 1 d . . . . .
H2A H 0.330(2) 0.475(2) 0.6232(18) 0.071(8) Uiso 1 1 d . . . . .
H2B H 0.2893(19) 0.474(2) 0.5324(19) 0.069(8) Uiso 1 1 d . . . . .
H2C H 0.2196(19) 0.5002(18) 0.6027(16) 0.053(6) Uiso 1 1 d . . . . .
H3A H 0.0716(13) 0.3380(15) 0.5503(14) 0.034(5) Uiso 1 1 d . . . . .
H3B H 0.0742(13) 0.3333(15) 0.6513(12) 0.027(4) Uiso 1 1 d . . . . .
H3C H 0.0695(13) 0.2315(16) 0.5924(13) 0.035(4) Uiso 1 1 d . . . . .
H4A H 0.3560(17) 0.2309(16) 0.7010(15) 0.047(5) Uiso 1 1 d . . . . .
H4B H 0.2556(13) 0.2116(13) 0.7370(13) 0.029(4) Uiso 1 1 d . . . . .
H4C H 0.3019(14) 0.3154(16) 0.7552(15) 0.043(5) Uiso 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
S1 0.01590(15) 0.01739(15) 0.01670(15) 0.00158(10) 0.00070(10) 0.00046(9)
S2 0.01257(14) 0.02267(15) 0.01531(15) 0.00085(10) -0.00057(9) 0.00128(10)
N1 0.0150(4) 0.0168(4) 0.0134(4) 0.0004(4) 0.0008(4) 0.0005(4)
N2 0.0155(5) 0.0176(4) 0.0161(5) 0.0002(4) 0.0000(4) -0.0014(4)
N3 0.0139(4) 0.0172(4) 0.0149(5) 0.0002(4) -0.0004(4) -0.0008(3)
N4 0.0150(4) 0.0204(5) 0.0131(4) 0.0011(4) 0.0008(4) 0.0012(4)
N5 0.0201(5) 0.0219(5) 0.0207(5) 0.0037(4) 0.0025(4) 0.0013(4)
N6 0.0173(5) 0.0184(5) 0.0239(5) 0.0000(4) -0.0024(4) 0.0015(4)
C1 0.0102(5) 0.0228(6) 0.0121(5) 0.0011(4) 0.0010(4) -0.0002(4)
C2 0.0168(5) 0.0134(5) 0.0126(5) 0.0004(4) 0.0020(4) -0.0006(4)
Be1 0.0120(6) 0.0156(6) 0.0120(6) -0.0003(5) 0.0004(5) -0.0001(5)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.6552(12) . ?
S2 C2 1.6486(11) . ?
N1 Be1 1.7247(17) . ?
N1 H1A 0.824(17) . ?
N1 H1B 0.865(16) . ?
N1 H1C 0.843(16) . ?
N2 Be1 1.7367(16) . ?
N2 H2A 0.81(3) . ?
N2 H2B 0.77(3) . ?
N2 H2C 0.91(2) . ?
N3 Be1 1.7296(17) . ?
N3 H3A 0.808(19) . ?
N3 H3B 0.851(17) . ?
N3 H3C 0.925(18) . ?
N4 Be1 1.7366(17) . ?
N4 H4A 0.82(2) . ?
N4 H4B 0.825(17) . ?
N4 H4C 0.88(2) . ?
N5 C1 1.1644(16) . ?
N6 C2 1.1641(15) . ?

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
_geom_angle_publ_flag
Be1 N1 H1A 111.9(11) . . ?
Be1 N1 H1B 111.7(10) . . ?
H1A N1 H1B 108.8(14) . . ?
Be1 N1 H1C 114.1(10) . . ?
H1A N1 H1C 107.4(14) . . ?
H1B N1 H1C 102.3(14) . . ?
Be1 N2 H2A 114.9(17) . . ?
Be1 N2 H2B 112.9(18) . . ?
H2A N2 H2B 110(2) . . ?
Be1 N2 H2C 110.6(13) . . ?
H2A N2 H2C 107(2) . . ?
H2B N2 H2C 100(2) . . ?
Be1 N3 H3A 111.9(11) . . ?
Be1 N3 H3B 109.0(10) . . ?
H3A N3 H3B 107.2(15) . . ?
Be1 N3 H3C 116.2(10) . . ?
H3A N3 H3C 104.7(15) . . ?
H3B N3 H3C 107.4(14) . . ?
Be1 N4 H4A 110.4(14) . . ?
Be1 N4 H4B 114.8(11) . . ?
H4A N4 H4B 105.9(16) . . ?
Be1 N4 H4C 110.8(12) . . ?
H4A N4 H4C 108.7(16) . . ?
H4B N4 H4C 106.0(16) . . ?
N5 C1 S1 178.71(11) . . ?
N6 C2 S2 177.76(10) . . ?
N1 Be1 N3 110.98(9) . . ?
N1 Be1 N4 110.89(9) . . ?
N3 Be1 N4 109.36(9) . . ?
N1 Be1 N2 108.85(9) . . ?
N3 Be1 N2 108.03(9) . . ?
N4 Be1 N2 108.66(9) . . ?

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 N6 0.824(17) 2.247(17) 3.0418(14) 161.9(15) . yes
N1 H1C S1 0.843(16) 2.722(17) 3.5492(11) 167.3(13) 8_655 yes
N1 H1B N5 0.865(16) 2.246(16) 3.0974(14) 167.9(14) . yes
N2 H2A S2 0.81(3) 2.95(2) 3.5194(12) 129(2) 3_656 yes
N2 H2C N6 0.91(2) 2.17(2) 3.0551(14) 163.4(18) 8_665 yes
N2 H2B S2 0.77(3) 2.91(2) 3.5135(12) 137(2) 4_456 yes
N3 H3C N5 0.925(18) 2.206(18) 3.0881(14) 159.2(15) 4_456 yes
N3 H3B S1 0.851(17) 2.712(17) 3.4912(11) 152.8(14) 2_565 yes
N4 H4B S2 0.825(17) 2.763(17) 3.5725(11) 167.3(14) 6_557 yes
N4 H4A S1 0.82(2) 2.97(2) 3.5132(11) 125.4(16) 5_666 yes
N4 H4A N6 0.82(2) 2.45(2) 3.1402(14) 141.5(17) . yes
N4 H4C S2 0.88(2) 2.78(2) 3.6307(11) 161.7(16) 3_656 yes

_refine_diff_density_max         0.293
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.044

_shelx_res_file                  
;

TITL 1_a.res in Pbca
    3.res
    created by SHELXL-2018/3 at 13:33:49 on 12-Dec-2018
REM Old TITL 1 in Pbca

REM SHELXT solution in Pbca
REM R1 0.065,  Rweak 0.001,  Alpha 0.017,  Orientation as input
REM Formula found by SHELXT:  C2 Be N6 S2

CELL  1.54178  11.9956  11.7990  13.2171   90.000   90.000   90.000
ZERR    8.000   0.0005   0.0004   0.0005    0.000    0.000    0.000
LATT  1
SYMM 1/2-X, -Y, 1/2+Z
SYMM -X, 1/2+Y, 1/2-Z
SYMM 1/2+X, 1/2-Y, -Z
SFAC C H BE N S
UNIT 16 96 8 48 16
L.S. 10
BOND $H
LIST 4
TEMP -173.15
ACTA
OMIT 2 6 14
HTAB
HTAB N1 N6
EQIV $1 -x+1/2, y-1/2, z
HTAB N1 S1_$1
HTAB N1 N5
EQIV $2 -x+1, y+1/2, -z+3/2
HTAB N2 S2_$2
EQIV $3 -x+1/2, y+1/2, z
HTAB N2 N6_$3
EQIV $4 x-1/2, -y+1/2, -z+1
HTAB N2 S2_$4
HTAB N3 N5_$4
EQIV $5 -x+1/2, -y+1, z+1/2
HTAB N3 S1_$5
EQIV $6 x-1/2, y, -z+3/2
HTAB N4 S2_$6
EQIV $7 -x+1, -y+1, -z+1
HTAB N4 S1_$7
HTAB N4 N6
HTAB N4 S2_$2
FMAP 2
PLAN 20
WGHT    0.038600    0.231400
EXTI    0.000701
FVAR       0.12043
S1    5    0.436352    0.647168    0.355501    11.00000    0.01590    0.01739 =
         0.01670    0.00158    0.00070    0.00046
S2    5    0.669295    0.028429    0.658922    11.00000    0.01257    0.02267 =
         0.01531    0.00085   -0.00057    0.00128
N1    4    0.298860    0.241351    0.495030    11.00000    0.01496    0.01680 =
         0.01341    0.00041    0.00077    0.00051
N2    4    0.278744    0.455467    0.587232    11.00000    0.01548    0.01758 =
         0.01612    0.00025   -0.00003   -0.00136
N3    4    0.099072    0.303728    0.597012    11.00000    0.01390    0.01719 =
         0.01491    0.00017   -0.00044   -0.00075
N4    4    0.294728    0.260496    0.709996    11.00000    0.01501    0.02036 =
         0.01312    0.00110    0.00079    0.00121
N5    4    0.453357    0.410989    0.384008    11.00000    0.02014    0.02189 =
         0.02066    0.00366    0.00246    0.00133
N6    4    0.445948    0.074855    0.609271    11.00000    0.01726    0.01843 =
         0.02390   -0.00002   -0.00240    0.00152
C1    1    0.445543    0.508322    0.371341    11.00000    0.01019    0.02282 =
         0.01210    0.00108    0.00104   -0.00018
C2    1    0.537849    0.055636    0.631780    11.00000    0.01684    0.01344 =
         0.01265    0.00040    0.00200   -0.00055
BE1   3    0.242953    0.313240    0.596690    11.00000    0.01201    0.01555 =
         0.01197   -0.00032    0.00036   -0.00009
H1A   2    0.339602    0.188925    0.513204    11.00000    0.02665
H1B   2    0.336399    0.285954    0.455804    11.00000    0.02330
H1C   2    0.250967    0.214099    0.455209    11.00000    0.02131
H2A   2    0.330042    0.475052    0.623235    11.00000    0.07101
H2B   2    0.289292    0.474383    0.532408    11.00000    0.06949
H2C   2    0.219604    0.500223    0.602741    11.00000    0.05272
H3A   2    0.071615    0.337980    0.550305    11.00000    0.03365
H3B   2    0.074174    0.333291    0.651255    11.00000    0.02717
H3C   2    0.069535    0.231524    0.592416    11.00000    0.03476
H4A   2    0.355982    0.230879    0.701049    11.00000    0.04665
H4B   2    0.255558    0.211581    0.736991    11.00000    0.02854
H4C   2    0.301908    0.315373    0.755163    11.00000    0.04269
HKLF 4




REM  1_a.res in Pbca
REM wR2 = 0.0556, GooF = S = 0.992, Restrained GooF = 0.992 for all data
REM R1 = 0.0204 for 1746 Fo > 4sig(Fo) and 0.0244 for all 1955 data
REM 149 parameters refined using 0 restraints

END

WGHT      0.0398      0.0000

REM Instructions for potential hydrogen bonds
HTAB N1 N6
HTAB N1 N5
HTAB N1 S1_$1
HTAB N2 S2_$2
HTAB N2 S2_$4
HTAB N2 N6_$3
HTAB N3 S1_$5
HTAB N3 N5_$4
HTAB N4 S1_$7
HTAB N4 N6
HTAB N4 S2_$6
HTAB N4 S2_$2

REM Highest difference peak  0.293,  deepest hole -0.151,  1-sigma level  0.044
Q1    1   0.2655  0.2759  0.5446  11.00000  0.05    0.29
Q2    1   0.6686  0.0571  0.7199  11.00000  0.05    0.27
Q3    1   0.6643  0.0063  0.7191  11.00000  0.05    0.24
Q4    1   0.2729  0.2857  0.6538  11.00000  0.05    0.23
Q5    1   0.4418  0.6515  0.2879  11.00000  0.05    0.21
Q6    1   0.6850  0.0551  0.5976  11.00000  0.05    0.21
Q7    1   0.3428  0.4668  0.5424  11.00000  0.05    0.19
Q8    1   0.1744  0.2946  0.5941  11.00000  0.05    0.19
Q9    1   0.6781  0.0058  0.5904  11.00000  0.05    0.18
Q10   1   0.4475  0.4660  0.4153  11.00000  0.05    0.16
Q11   1   0.4986  0.0775  0.6524  11.00000  0.05    0.16
Q12   1   0.4579  0.4656  0.3468  11.00000  0.05    0.16
Q13   1   0.4293  0.5998  0.4008  11.00000  0.05    0.15
Q14   1   0.5986  0.0394  0.6444  11.00000  0.05    0.15
Q15   1   0.5160  0.0801  0.5884  11.00000  0.05    0.15
Q16   1   0.2945  0.4737  0.6512  11.00000  0.05    0.15
Q17   1   0.4331  0.6760  0.4199  11.00000  0.05    0.15
Q18   1   0.2490  0.4834  0.5235  11.00000  0.05    0.14
Q19   1   0.2618  0.3949  0.5994  11.00000  0.05    0.13
Q20   1   0.4235  0.0982  0.6115  11.00000  0.05    0.13
;
_shelx_res_checksum              62114
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_FVAR2
_database_code_depnum_ccdc_archive 'CCDC 1956202'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2019-09-26 deposited with the CCDC.	2019-10-15 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT315_FVAR2               
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).        C1B Check
RESPONSE: in CN Anions C is singly bonded
;
# Added during the CSD deposition process: Thursday 26 September 2019 04:39 PM
# end Validation Reply Form


_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C2 H12 Be1 N6'
_chemical_formula_sum            'C2 H12 Be N6'
_chemical_formula_weight         129.19

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Be Be 0.0038 0.0014 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_H-M_alt        'P n a 21'
_space_group_name_Hall           'P 2c -2n'

_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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   9.1188(3)
_cell_length_b                   12.6103(6)
_cell_length_c                   6.9022(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     793.69(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6773
_cell_measurement_theta_min      11.98
_cell_measurement_theta_max      158.34

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_F_000             280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    0.626
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_detector_area_resol_mean 5.81
_diffrn_reflns_number            8066
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         5.988
_diffrn_reflns_theta_max         78.681
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_point_group_measured_fraction_full 0.836
_reflns_number_total             1390
_reflns_number_gt                1129
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.508
_reflns_Friedel_fraction_max     0.596
_reflns_Friedel_fraction_full    0.643

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0505P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.4(9)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1390
_refine_ls_number_parameters     133
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0457
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0866
_refine_ls_wR_factor_gt          0.0813
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_restrained_S_all      0.998
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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
_atom_site_disorder_assembly
_atom_site_disorder_group
C1A C 0.1423(2) 0.5436(2) 0.8334(4) 0.0421(7) Uani 0.16(3) 1 d . . P A 1
N1A N 0.1719(3) 0.6202(2) 0.7748(4) 0.0433(8) Uani 0.16(3) 1 d . . P A 1
N2A N 0.4948(3) 0.3345(2) 0.8715(4) 0.0435(8) Uani 0.60(4) 1 d . . P B 1
C2A C 0.4988(3) 0.3074(2) 0.7207(5) 0.0463(8) Uani 0.60(4) 1 d . . P B 1
C1B C 0.1719(3) 0.6202(2) 0.7748(4) 0.0433(8) Uani 0.84(3) 1 d . . P A 2
N1B N 0.1423(2) 0.5436(2) 0.8334(4) 0.0421(7) Uani 0.84(3) 1 d . . P A 2
C2B C 0.4948(3) 0.3345(2) 0.8715(4) 0.0435(8) Uani 0.40(4) 1 d . . P B 2
N2B N 0.4988(3) 0.3074(2) 0.7207(5) 0.0463(8) Uani 0.40(4) 1 d . . P B 2
Be1 Be 0.2507(3) 0.4158(2) 0.3127(6) 0.0273(5) Uani 1 1 d . . . . .
N3 N 0.1989(2) 0.36476(18) 0.5341(4) 0.0332(5) Uani 1 1 d . . . . .
H3A H 0.111(5) 0.324(3) 0.525(6) 0.055(10) Uiso 1 1 d . . . . .
H3B H 0.189(3) 0.415(3) 0.626(5) 0.046(9) Uiso 1 1 d . . . . .
H3C H 0.267(5) 0.316(3) 0.596(6) 0.075(12) Uiso 1 1 d . . . . .
N4 N 0.1840(3) 0.33828(17) 0.1298(3) 0.0344(5) Uani 1 1 d . . . . .
H4A H 0.222(6) 0.357(4) 0.001(8) 0.107(17) Uiso 1 1 d . . . . .
H4B H 0.079(6) 0.328(3) 0.124(6) 0.076(12) Uiso 1 1 d . . . . .
H4C H 0.222(5) 0.272(3) 0.136(6) 0.081(13) Uiso 1 1 d . . . . .
N6 N 0.1798(2) 0.54219(15) 0.2890(3) 0.0319(4) Uani 1 1 d . . . . .
H6A H 0.181(4) 0.572(3) 0.147(7) 0.076(12) Uiso 1 1 d . . . . .
H6B H 0.218(3) 0.592(3) 0.357(6) 0.051(9) Uiso 1 1 d . . . . .
H6C H 0.085(4) 0.541(3) 0.303(7) 0.073(11) Uiso 1 1 d . . . . .
N5 N 0.44016(19) 0.41708(17) 0.2999(4) 0.0302(4) Uani 1 1 d . . . . .
H5 H 0.481(4) 0.377(3) 0.395(6) 0.053(10) Uiso 1 1 d . . . . .
H5B H 0.483(3) 0.488(3) 0.292(7) 0.056(9) Uiso 1 1 d . . . . .
H5C H 0.470(4) 0.392(3) 0.172(6) 0.067(11) Uiso 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
C1A 0.0433(11) 0.0466(17) 0.0365(14) 0.0002(11) -0.0001(10) -0.0008(10)
N1A 0.0369(11) 0.0456(17) 0.0473(17) -0.0072(14) -0.0022(12) 0.0027(11)
N2A 0.0328(12) 0.0411(13) 0.057(2) 0.0138(13) 0.0042(11) 0.0050(11)
C2A 0.0428(14) 0.0435(14) 0.0526(19) -0.0030(12) -0.0071(12) 0.0104(11)
C1B 0.0369(11) 0.0456(17) 0.0473(17) -0.0072(14) -0.0022(12) 0.0027(11)
N1B 0.0433(11) 0.0466(17) 0.0365(14) 0.0002(11) -0.0001(10) -0.0008(10)
C2B 0.0328(12) 0.0411(13) 0.057(2) 0.0138(13) 0.0042(11) 0.0050(11)
N2B 0.0428(14) 0.0435(14) 0.0526(19) -0.0030(12) -0.0071(12) 0.0104(11)
Be1 0.0278(11) 0.0231(12) 0.0309(15) -0.0002(11) -0.0016(13) 0.0006(10)
N3 0.0314(11) 0.0339(10) 0.0343(11) 0.0018(9) 0.0024(9) -0.0013(9)
N4 0.0357(11) 0.0335(11) 0.0340(11) -0.0055(9) -0.0054(10) -0.0034(10)
N6 0.0323(9) 0.0282(9) 0.0351(12) -0.0016(9) -0.0021(10) 0.0017(8)
N5 0.0282(8) 0.0303(10) 0.0321(11) 0.0008(9) 0.0014(9) 0.0005(7)

_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1A N1A 1.082(3) . ?
N2A C2A 1.096(4) . ?
C1B N1B 1.082(3) . ?
C2B N2B 1.096(4) . ?
Be1 N4 1.708(4) . ?
Be1 N3 1.724(5) . ?
Be1 N6 1.728(3) . ?
Be1 N5 1.730(3) . ?

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
_geom_angle_publ_flag
N4 Be1 N3 110.10(19) . . ?
N4 Be1 N6 108.9(2) . . ?
N3 Be1 N6 109.0(2) . . ?
N4 Be1 N5 108.8(2) . . ?
N3 Be1 N5 108.8(2) . . ?
N6 Be1 N5 111.10(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
N3 H3A N2B^b 0.95(4) 2.37(4) 3.115(4) 135(3) 3_455 yes
N3 H3B N1B^b 0.90(4) 2.20(4) 3.102(4) 173(3) . yes
N3 H3C N2B^b 0.97(4) 2.29(5) 3.109(4) 142(3) . yes
N4 H4A N2A^a 0.98(6) 2.66(5) 3.349(4) 128(4) 1_554 yes
N4 H4A N1B^b 0.98(6) 2.73(5) 3.322(4) 119(3) 1_554 yes
N4 H4B N1A^a 0.97(5) 2.59(5) 3.436(3) 145(3) 2_564 yes
N4 H4C N1A^a 0.90(4) 2.35(4) 3.207(4) 158(4) 4_544 yes
N6 H6A N1A^a 1.05(5) 2.64(5) 3.684(4) 172(3) 1_554 yes
N6 H6A N1B^b 1.05(5) 2.22(4) 3.164(3) 148(3) 1_554 yes
N6 H6C N1B^b 0.87(4) 2.34(3) 3.145(3) 154(3) 2_564 yes
N5 H5 N2B^b 0.91(4) 2.42(4) 3.261(4) 155(3) . yes
N5 H5B N2A^a 0.97(3) 2.32(3) 3.226(3) 155(3) 2_664 yes
N5 H5B N2B^b 0.97(3) 2.63(3) 3.560(4) 159(3) 2_664 yes
N5 H5C N2A^a 0.98(4) 2.21(4) 3.174(4) 170(3) 1_554 yes

_refine_diff_density_max         0.134
_refine_diff_density_min         -0.155
_refine_diff_density_rms         0.037

_shelx_res_file                  
;
TITL 4_a.res in Pna2(1)
    FVAR2.res
    created by SHELXL-2018/3 at 14:12:17 on 05-Jul-2019
REM Old TITL 4 in Pna2(1)
REM SHELXT solution in Pna2(1): R1 0.097, Rweak 0.011, Alpha 0.030
REM <I/s>   0.299 for  102 systematic absences,  Orientation as input
REM Flack x =  0.217 ( 0.231 ) from   306 Parsons' quotients
REM Formula found by SHELXT:  C2 Be N6
CELL  1.54178   9.1188  12.6103   6.9022   90.000   90.000   90.000
ZERR    4.000   0.0003   0.0006   0.0003    0.000    0.000    0.000
LATT -1
SYMM -X, -Y, 1/2+Z
SYMM 1/2+X, 1/2-Y, Z
SYMM 1/2-X, 1/2+Y, 1/2+Z
SFAC C H BE N
UNIT 8 48 4 24
L.S. 10
BOND
LIST 4
ACTA
OMIT 1 6 -8
TEMP -173.15
TWIN
FMAP 2
PLAN 20
EXYZ N1A C1B
EADP N1A C1B
EXYZ N1B C1A
EADP N1B C1A
EXYZ N2A C2B
EADP N2A C2B
EXYZ N2B C2A
EADP N2B C2A
HTAB
EQIV $1 x-1/2, -y+1/2, z
HTAB N3 N2B_$1
HTAB N3 N1B
HTAB N3 N2B
EQIV $2 x, y, z-1
HTAB N4 N2A_$2
HTAB N4 N1B_$2
EQIV $3 -x, -y+1, z-1/2
HTAB N4 N1A_$3
EQIV $4 -x+1/2, y-1/2, z-1/2
HTAB N4 N1A_$4
HTAB N6 N1A_$2
HTAB N6 N1B_$2
HTAB N6 N1B_$3
HTAB N5 N2B
EQIV $5 -x+1, -y+1, z-1/2
HTAB N5 N2A_$5
HTAB N5 N2B_$5
HTAB N5 N2A_$2
REM EXTI 0.004549
WGHT    0.050500
BASF   0.42801
FVAR       1.09285   0.16020   0.59885
PART 1
C1A   1    0.142258    0.543626    0.833355    21.00000    0.04334    0.04661 =
         0.03649    0.00025   -0.00006   -0.00084
N1A   4    0.171867    0.620247    0.774792    21.00000    0.03689    0.04558 =
         0.04732   -0.00721   -0.00225    0.00273
N2A   4    0.494845    0.334495    0.871474    31.00000    0.03283    0.04109 =
         0.05668    0.01383    0.00418    0.00505
C2A   1    0.498840    0.307438    0.720680    31.00000    0.04283    0.04345 =
         0.05258   -0.00303   -0.00707    0.01035
PART 2
C1B   1    0.171867    0.620247    0.774792   -21.00000    0.03689    0.04558 =
         0.04732   -0.00721   -0.00225    0.00273
N1B   4    0.142258    0.543626    0.833355   -21.00000    0.04334    0.04661 =
         0.03649    0.00025   -0.00006   -0.00084
C2B   1    0.494845    0.334495    0.871474   -31.00000    0.03283    0.04109 =
         0.05668    0.01383    0.00418    0.00505
N2B   4    0.498840    0.307438    0.720680   -31.00000    0.04283    0.04345 =
         0.05258   -0.00303   -0.00707    0.01035
PART 0
BE1   3    0.250718    0.415790    0.312697    11.00000    0.02785    0.02305 =
         0.03090   -0.00017   -0.00159    0.00057
N3    4    0.198871    0.364760    0.534051    11.00000    0.03135    0.03389 =
         0.03432    0.00178    0.00239   -0.00128
H3A   2    0.111423    0.324175    0.525088    11.00000    0.05477
H3B   2    0.189472    0.415152    0.626274    11.00000    0.04579
H3C   2    0.267066    0.315860    0.595600    11.00000    0.07528
N4    4    0.184038    0.338283    0.129822    11.00000    0.03567    0.03347 =
         0.03396   -0.00552   -0.00541   -0.00340
H4A   2    0.222208    0.356565    0.000727    11.00000    0.10668
H4B   2    0.078806    0.327719    0.124499    11.00000    0.07567
H4C   2    0.221576    0.272337    0.135605    11.00000    0.08079
N6    4    0.179847    0.542191    0.288991    11.00000    0.03229    0.02823 =
         0.03512   -0.00163   -0.00212    0.00167
H6A   2    0.181205    0.572172    0.146930    11.00000    0.07591
H6B   2    0.218275    0.592309    0.357143    11.00000    0.05059
H6C   2    0.085367    0.540985    0.303123    11.00000    0.07260
N5    4    0.440164    0.417084    0.299875    11.00000    0.02818    0.03028 =
         0.03207    0.00076    0.00138    0.00048
H5    2    0.480727    0.376891    0.395271    11.00000    0.05293
H5B   2    0.483032    0.487719    0.292047    11.00000    0.05610
H5C   2    0.469622    0.391909    0.171998    11.00000    0.06699
HKLF 4




REM  4_a.res in Pna2(1)
REM wR2 = 0.0866, GooF = S = 0.998, Restrained GooF = 0.998 for all data
REM R1 = 0.0336 for 1129 Fo > 4sig(Fo) and 0.0457 for all 1390 data
REM 133 parameters refined using 1 restraints

END

WGHT      0.0505      0.0000

REM Instructions for potential hydrogen bonds
HTAB N3 N2B_$1
HTAB N3 N1B
HTAB N3 N2B
HTAB N4 N2A_$2
HTAB N4 N1A_$3
HTAB N4 N1A_$4
HTAB N6 N1A_$2
HTAB N6 N1B_$2
HTAB N6 N1B_$3
HTAB N5 N2B
HTAB N5 N2A_$5
HTAB N5 N2B_$5
HTAB N5 N2A_$2

REM Highest difference peak  0.134,  deepest hole -0.155,  1-sigma level  0.037
Q1    1   0.3612  0.4219  0.4839  11.00000  0.05    0.13
Q2    1   0.5521  0.3350  0.6775  11.00000  0.05    0.13
Q3    1   0.6247  0.3496  0.0518  11.00000  0.05    0.12
Q4    1   0.4409  0.2891  1.0570  11.00000  0.05    0.12
Q5    1   0.5502  0.3511  0.9175  11.00000  0.05    0.11
Q6    1   0.1216  0.6943  0.9882  11.00000  0.05    0.11
Q7    1   0.5853  0.3058  0.5355  11.00000  0.05    0.11
Q8    1   0.2921  0.5662  0.8651  11.00000  0.05    0.10
Q9    1   0.4494  0.3256  0.9132  11.00000  0.05    0.10
Q10   1   0.3482  0.3829  0.8256  11.00000  0.05    0.10
Q11   1   0.0524  0.5318  0.1368  11.00000  0.05    0.09
Q12   1   0.3370  0.4995  0.2368  11.00000  0.05    0.09
Q13   1   0.6203  0.2415  0.8309  11.00000  0.05    0.09
Q14   1   0.3050  0.4745  0.8478  11.00000  0.05    0.09
Q15   1   0.4972  0.3231  0.7986  11.00000  0.05    0.09
Q16   1   0.0261  0.6187  0.2600  11.00000  0.05    0.09
Q17   1   0.0251  0.4485  0.3173  11.00000  0.05    0.09
Q18   1   0.3383  0.3294  0.8194  11.00000  0.05    0.09
Q19   1   0.5568  0.4134  0.6928  11.00000  0.05    0.09
Q20   1   0.3212  0.6842  0.8305  11.00000  0.05    0.09
;
_shelx_res_checksum              29717
