# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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 1982295'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2020-02-06 deposited with the CCDC.	2020-05-04 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            'Be4 H51 I2 N19'
_chemical_formula_weight         607.43

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      trigonal
_space_group_IT_number           143
_space_group_name_H-M_alt        'P 3'
_space_group_name_Hall           'P 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   9.77560(10)
_cell_length_b                   9.77560(10)
_cell_length_c                   8.7186(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     721.55(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9830
_cell_measurement_theta_min      10.15
_cell_measurement_theta_max      154.18

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_F_000             306
_exptl_transmission_factor_min   0.0301
_exptl_transmission_factor_max   0.1060
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    17.294
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_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            4283
_diffrn_reflns_av_unetI/netI     0.0155
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.073
_diffrn_reflns_theta_max         75.826
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             1779
_reflns_number_gt                1767
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.964
_reflns_Friedel_fraction_max     0.964
_reflns_Friedel_fraction_full    0.981

_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          
;
 Refined as a 2-component 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)+(0.0903P)²+2.1179P] 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_abs_structure_details 
;
 Flack x determined using 751 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.413(17)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1779
_refine_ls_number_parameters     79
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0447
_refine_ls_wR_factor_ref         0.1277
_refine_ls_wR_factor_gt          0.1274
_refine_ls_goodness_of_fit_ref   1.164
_refine_ls_restrained_S_all      1.160
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.003

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 0.3333 0.6667 0.19097(19) 0.0261(7) Uani 1 3 d S T P . .
I2 I 0.0000 0.0000 0.84022(10) 0.0199(5) Uani 1 3 d S T P . .
N1 N 0.844(3) 0.478(2) 1.140(2) 0.033(5) Uani 1 1 d . . . . .
H1A H 0.8635 0.5745 1.1741 0.040 Uiso 1 1 calc R U . . .
H1B H 0.9236 0.4637 1.1748 0.040 Uiso 1 1 calc R U . . .
N2 N 0.816(2) 0.3010(19) 0.8791(19) 0.020(3) Uani 1 1 d . . . . .
H2A H 0.8960 0.2831 0.9067 0.024 Uiso 1 1 calc R U . . .
H2B H 0.8118 0.3024 0.7749 0.024 Uiso 1 1 calc R U . . .
N3 N 0.6667 0.3333 1.428(2) 0.027(4) Uani 1 3 d S T P . .
H3A H 0.5656 0.2759 1.4627 0.041 Uiso 0.3333 1 calc R U P . .
H3B H 0.7102 0.4344 1.4627 0.041 Uiso 0.3333 1 calc R U P . .
H3C H 0.7241 0.2898 1.4627 0.041 Uiso 0.3333 1 calc R U P . .
N4 N 1.0378(16) 0.6293(17) 0.8838(16) 0.034(3) Uani 1 1 d . . . . .
H4A H 1.0370 0.7209 0.8679 0.051 Uiso 1 1 calc R U . . .
H4B H 1.0580 0.5957 0.7937 0.051 Uiso 1 1 calc R U . . .
H4C H 1.1142 0.6461 0.9532 0.051 Uiso 1 1 calc R U . . .
N5 N 0.529(2) 0.5475(19) 0.5113(19) 0.041(3) Uani 1 1 d . . . . .
N7 N 0.943(2) 0.771(2) 1.460(2) 0.046(4) Uani 1 1 d . . . . .
N6 N 0.787(2) 0.812(2) 1.228(2) 0.050(4) Uani 1 1 d . . . . .
Be1 Be 0.848(2) 0.481(2) 0.956(2) 0.028(4) Uani 1 1 d . U . . .
Be2 Be 0.6667 0.3333 1.222(3) 0.022(6) Uani 1 3 d S TU P . .


_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 1.60(3) . ?
N1 Be2 1.75(2) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 Be1 1.76(3) . ?
N2 Be1 1.78(3) 3_665 ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N3 Be2 1.79(3) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N3 H3C 0.9100 . ?
N4 Be1 1.81(2) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N4 H4C 0.9100 . ?
Be1 N2 1.78(3) 2_655 ?
Be2 N1 1.75(2) 3_665 ?
Be2 N1 1.75(2) 2_655 ?

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 Be2 115.2(16) . . ?
Be1 N1 H1A 108.5 . . ?
Be2 N1 H1A 108.5 . . ?
Be1 N1 H1B 108.5 . . ?
Be2 N1 H1B 108.5 . . ?
H1A N1 H1B 107.5 . . ?
Be1 N2 Be1 105.7(16) . 3_665 ?
Be1 N2 H2A 110.6 . . ?
Be1 N2 H2A 110.6 3_665 . ?
Be1 N2 H2B 110.6 . . ?
Be1 N2 H2B 110.6 3_665 . ?
H2A N2 H2B 108.7 . . ?
Be2 N3 H3A 109.5 . . ?
Be2 N3 H3B 109.5 . . ?
H3A N3 H3B 109.5 . . ?
Be2 N3 H3C 109.5 . . ?
H3A N3 H3C 109.5 . . ?
H3B N3 H3C 109.5 . . ?
Be1 N4 H4A 109.5 . . ?
Be1 N4 H4B 109.5 . . ?
H4A N4 H4B 109.5 . . ?
Be1 N4 H4C 109.5 . . ?
H4A N4 H4C 109.5 . . ?
H4B N4 H4C 109.5 . . ?
N1 Be1 N2 112.2(14) . . ?
N1 Be1 N2 111.4(14) . 2_655 ?
N2 Be1 N2 107.2(15) . 2_655 ?
N1 Be1 N4 111.6(14) . . ?
N2 Be1 N4 105.3(12) . . ?
N2 Be1 N4 108.8(13) 2_655 . ?
N1 Be2 N1 104.6(12) 3_665 . ?
N1 Be2 N1 104.6(12) 3_665 2_655 ?
N1 Be2 N1 104.6(12) . 2_655 ?
N1 Be2 N3 114.0(10) 3_665 . ?
N1 Be2 N3 114.0(10) . . ?
N1 Be2 N3 114.0(10) 2_655 . ?

_refine_diff_density_max         0.972
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.182

####################################################################### 
# 
# 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 1982298'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2020-02-06 deposited with the CCDC.	2020-05-04 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         'Be4 H42 N22'
_chemical_formula_sum            'Be4 H42 N22'
_chemical_formula_weight         386.59

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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'-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                   13.4543(3)
_cell_length_b                   10.5289(3)
_cell_length_c                   16.9967(4)
_cell_angle_alpha                90
_cell_angle_beta                 111.134(2)
_cell_angle_gamma                90
_cell_volume                     2245.79(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    14461
_cell_measurement_theta_min      10.97
_cell_measurement_theta_max      152.26

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.143
_exptl_crystal_F_000             848
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    0.695
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.3649
_exptl_absorpt_correction_T_max  0.9687
_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            11750
_diffrn_reflns_av_unetI/netI     0.0136
_diffrn_reflns_av_R_equivalents  0.0156
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         5.484
_diffrn_reflns_theta_max         75.650
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2312
_reflns_number_gt                1887
_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)+(0.0640P)²+0.7085P] 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_number_reflns         2312
_refine_ls_number_parameters     203
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0480
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.1079
_refine_ls_wR_factor_gt          0.1005
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_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 0.56940(8) 0.40613(11) 0.66468(7) 0.0240(2) Uani 1 1 d . . . . .
N2 N 0.500000 0.59703(13) 0.750000 0.0243(3) Uani 1 2 d S T P . .
N3 N 0.64024(8) 0.41086(10) 0.84092(7) 0.0241(2) Uani 1 1 d . . . . .
N4 N 0.500000 0.22099(14) 0.750000 0.0245(3) Uani 1 2 d S T P . .
N5 N 0.42630(9) 0.59984(11) 0.56851(7) 0.0284(3) Uani 1 1 d . . . . .
N6 N 0.71607(9) 0.21319(11) 0.76241(8) 0.0278(3) Uani 1 1 d . . . . .
N7 N 0.31984(10) 0.82654(13) 0.62268(9) 0.0458(3) Uani 1 1 d . . . . .
N8 N 0.29684(9) 0.93212(12) 0.60252(7) 0.0337(3) Uani 1 1 d . . . . .
N9 N 0.27364(11) 1.03668(13) 0.58277(9) 0.0457(3) Uani 1 1 d . . . . .
N10 N 0.13670(11) 0.61356(13) 0.56942(8) 0.0378(3) Uani 1 1 d . . . . .
N11 N 0.92158(11) 0.39228(13) 0.82227(10) 0.0394(3) Uani 1 1 d . . . . .
N12 N 0.10711(10) 1.26325(14) 0.51275(10) 0.0395(3) Uani 1 1 d . . . . .
Be1 Be 0.46597(11) 0.50331(14) 0.66192(10) 0.0237(3) Uani 1 1 d . . . . .
Be2 Be 0.60579(11) 0.31463(15) 0.75391(10) 0.0240(3) Uani 1 1 d . . . . .
H2 H 0.4501(12) 0.6432(16) 0.7466(10) 0.034(4) Uiso 1 1 d . . . . .
H1A H 0.6163(14) 0.4459(16) 0.6629(11) 0.032(4) Uiso 1 1 d . . . . .
H1B H 0.5530(13) 0.3582(17) 0.6250(12) 0.034(4) Uiso 1 1 d . . . . .
H4 H 0.4828(13) 0.1715(16) 0.7084(10) 0.035(4) Uiso 1 1 d . . . . .
H3A H 0.6644(13) 0.3661(16) 0.8862(11) 0.033(4) Uiso 1 1 d . . . . .
H3B H 0.6846(15) 0.4512(17) 0.8423(11) 0.037(5) Uiso 1 1 d . . . . .
H5A H 0.4772(14) 0.6272(16) 0.5577(11) 0.037(4) Uiso 1 1 d . . . . .
H5B H 0.3916(13) 0.6598(17) 0.5765(10) 0.031(4) Uiso 1 1 d . . . . .
H5C H 0.3834(15) 0.5557(18) 0.5233(13) 0.048(5) Uiso 1 1 d . . . . .
H6A H 0.7066(13) 0.1753(16) 0.7166(12) 0.036(4) Uiso 1 1 d . . . . .
H6B H 0.7241(13) 0.1600(17) 0.8012(11) 0.034(4) Uiso 1 1 d . . . . .
H6C H 0.7672(14) 0.2531(16) 0.7708(11) 0.034(4) Uiso 1 1 d . . . . .
H10A H 0.1852(14) 0.6787(18) 0.5740(11) 0.042(5) Uiso 1 1 d . . . . .
H10B H 0.1443(18) 0.559(2) 0.5343(15) 0.068(7) Uiso 1 1 d . . . . .
H10C H 0.0715(17) 0.6477(19) 0.5475(12) 0.052(5) Uiso 1 1 d . . . . .
H12 H 0.1494(14) 1.1974(16) 0.5301(11) 0.036(4) Uiso 1 1 d . . . . .
H11A H 0.9000(15) 0.4072(17) 0.7688(14) 0.043(5) Uiso 1 1 d . . . . .
H11B H 0.9124(13) 0.4621(17) 0.8432(11) 0.030(4) Uiso 1 1 d . . . . .
H11C H 0.9912(16) 0.3806(16) 0.8420(12) 0.044(5) Uiso 1 1 d . . . . .
H12A H 0.1281(13) 1.3161(17) 0.4819(12) 0.038(4) Uiso 1 1 d . . . . .
H12B H 0.1138(14) 1.3013(17) 0.5562(13) 0.046(5) Uiso 1 1 d . . . . .


_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 Be2 1.7125(19) . ?
N1 Be1 1.7143(17) . ?
N2 Be1 1.7117(18) 2_656 ?
N2 Be1 1.7118(18) . ?
N3 Be2 1.7129(19) . ?
N3 Be1 1.7152(18) 2_656 ?
N4 Be2 1.7129(17) . ?
N4 Be2 1.7129(17) 2_656 ?
N5 Be1 1.7966(18) . ?
N6 Be2 1.7912(18) . ?
N7 N8 1.1715(18) . ?
N8 N9 1.1605(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
Be2 N1 Be1 109.27(9) . . ?
Be1 N2 Be1 109.59(13) 2_656 . ?
Be2 N3 Be1 110.37(9) . 2_656 ?
Be2 N4 Be2 109.72(13) . 2_656 ?
N9 N8 N7 179.62(16) . . ?
N2 Be1 N1 111.20(9) . . ?
N2 Be1 N3 108.01(10) . 2_656 ?
N1 Be1 N3 108.77(10) . 2_656 ?
N2 Be1 N5 110.32(10) . . ?
N1 Be1 N5 109.96(10) . . ?
N3 Be1 N5 108.49(9) 2_656 . ?
N1 Be2 N4 108.74(9) . . ?
N1 Be2 N3 109.50(10) . . ?
N4 Be2 N3 109.65(10) . . ?
N1 Be2 N6 111.77(10) . . ?
N4 Be2 N6 108.21(10) . . ?
N3 Be2 N6 108.94(10) . . ?

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
N5 H5A N12 0.822(19) 2.580(19) 3.3821(19) 165.6(15) 3_545 yes
N5 H5B N7 0.825(18) 2.275(18) 3.0899(18) 169.5(15) . yes
N5 H5C N8 0.91(2) 2.59(2) 3.3591(16) 142.6(15) 7_566 yes
N5 H5C N9 0.91(2) 2.43(2) 3.3055(18) 162.2(16) 7_566 yes
N6 H6A N10 0.842(19) 2.42(2) 3.2365(19) 162.6(15) 3_545 yes
N6 H6B N9 0.842(19) 2.352(19) 3.1835(19) 169.4(15) 2_646 yes
N6 H6C N11 0.774(18) 2.433(19) 3.1949(18) 168.5(16) . yes
N10 H10A N7 0.930(19) 2.304(19) 3.211(2) 164.8(16) . yes
N10 H10C N12 0.90(2) 2.44(2) 3.3301(19) 179.0(18) 5_576 yes
N12 H12 N9 0.878(18) 2.319(18) 3.194(2) 174.6(15) . yes
N11 H11A N7 0.86(2) 2.47(2) 3.242(2) 148.7(16) 3_545 yes
N11 H11A N8 0.86(2) 2.68(2) 3.5246(19) 168.5(16) 3_545 yes
N11 H11B N10 0.845(18) 2.428(18) 3.236(2) 160.5(14) 2_656 yes
N11 H11C N7 0.88(2) 2.46(2) 3.333(2) 170.9(16) 4_646 yes
N12 H12A N9 0.879(19) 2.530(19) 3.395(2) 168.0(15) 7_576 yes
N12 H12B N11 0.82(2) 2.47(2) 3.262(2) 162.5(17) 2_666 yes

_refine_diff_density_max         0.225
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.038

####################################################################### 
# 
# 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_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 1982296'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2020-02-06 deposited with the CCDC.	2020-05-04 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         '[Be4(NH2)6(NH3)4]+4NH3'
_chemical_formula_sum            'Be4 H36 Br2 N14'
_chemical_formula_weight         428.29

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      trigonal
_space_group_IT_number           143
_space_group_name_H-M_alt        'P 3'
_space_group_name_Hall           'P 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   14.2177(13)
_cell_length_b                   14.2177(13)
_cell_length_c                   8.5600(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1498.5(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    16758
_cell_measurement_theta_min      7.12
_cell_measurement_theta_max      150.00

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.424
_exptl_crystal_F_000             660
_exptl_transmission_factor_min   0.0728
_exptl_transmission_factor_max   1.0000
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    5.228
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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.
;
_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            12189
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_theta_min         3.590
_diffrn_reflns_theta_max         75.476
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_point_group_measured_fraction_full 0.937
_reflns_number_total             3765
_reflns_number_gt                3698
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_max     0.859
_reflns_Friedel_fraction_full    0.876

_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          
;
 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)+(0.1581P)²+1.0011P] 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_abs_structure_details 
;
 Twinning involves inversion, so Flack parameter cannot be determined
;
_refine_ls_abs_structure_Flack   ?
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3765
_refine_ls_number_parameters     188
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0697
_refine_ls_wR_factor_ref         0.1768
_refine_ls_wR_factor_gt          0.1757
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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
Br1 Br 0.31057(8) 0.40765(7) 0.57976(9) 0.0183(3) Uani 1 1 d . . . . .
Br2 Br 0.67986(8) 0.58655(8) 1.22812(7) 0.0197(3) Uani 1 1 d . . . . .
N1 N 0.1307(6) 0.0683(6) 0.2785(9) 0.0172(15) Uani 1 1 d . . . . .
H1A H 0.1644 0.1379 0.2428 0.021 Uiso 1 1 calc R U . . .
H1B H 0.1677 0.0360 0.2417 0.021 Uiso 1 1 calc R U . . .
N2 N 0.0634(6) 0.1309(6) 0.5464(9) 0.0160(14) Uani 1 1 d . . . . .
H2A H 0.0974 0.2012 0.5135 0.019 Uiso 1 1 calc R U . . .
H2B H 0.0634 0.1308 0.6527 0.019 Uiso 1 1 calc R U . . .
N3 N 0.5973(7) 0.3956(7) 0.5893(9) 0.0172(14) Uani 1 1 d . . . . .
H3A H 0.6291 0.4648 0.5521 0.021 Uiso 1 1 calc R U . . .
H3B H 0.5276 0.3590 0.5542 0.021 Uiso 1 1 calc R U . . .
N4 N 0.5340(6) 0.2646(6) 0.8558(10) 0.0174(14) Uani 1 1 d . . . . .
H4A H 0.5326 0.2638 0.9621 0.021 Uiso 1 1 calc R U . . .
H4B H 0.4643 0.2287 0.8205 0.021 Uiso 1 1 calc R U . . .
N5 N 0.2574(7) 0.5356(6) 0.9338(9) 0.0171(15) Uani 1 1 d . . . . .
H5A H 0.2847 0.4945 0.8949 0.021 Uiso 1 1 calc R U . . .
H5B H 0.1876 0.5067 0.9004 0.021 Uiso 1 1 calc R U . . .
N6 N 0.2017(6) 0.6071(6) 1.2004(9) 0.0176(15) Uani 1 1 d . . . . .
H6A H 0.2003 0.6064 1.3067 0.021 Uiso 1 1 calc R U . . .
H6B H 0.1320 0.5756 1.1654 0.021 Uiso 1 1 calc R U . . .
N7 N 0.0000 0.0000 0.0023(14) 0.018(2) Uani 1 3 d S T P . .
H7A H -0.0087 -0.0642 -0.0332 0.027 Uiso 0.3333 1 calc R U P . .
H7B H 0.0642 0.0555 -0.0332 0.027 Uiso 0.3333 1 calc R U P . .
H7C H -0.0555 0.0087 -0.0332 0.027 Uiso 0.3333 1 calc R U P . .
N8 N 0.2691(6) 0.1384(5) 0.5484(8) 0.0180(13) Uani 1 1 d . . . . .
H8A H 0.2971 0.2112 0.5371 0.027 Uiso 1 1 calc R U . . .
H8B H 0.3097 0.1171 0.4925 0.027 Uiso 1 1 calc R U . . .
H8C H 0.2702 0.1225 0.6511 0.027 Uiso 1 1 calc R U . . .
N9 N 0.6667 0.3333 0.3151(15) 0.018(2) Uani 1 3 d S T P . .
H9A H 0.6587 0.3893 0.2797 0.026 Uiso 0.3333 1 calc R U P . .
H9B H 0.6107 0.2694 0.2797 0.026 Uiso 0.3333 1 calc R U P . .
H9C H 0.7306 0.3413 0.2797 0.026 Uiso 0.3333 1 calc R U P . .
N10 N 0.5309(6) 0.4670(6) 0.8594(9) 0.0211(14) Uani 1 1 d . . . . .
H10A H 0.4584 0.4260 0.8398 0.032 Uiso 1 1 calc R U . . .
H10B H 0.5580 0.5321 0.8099 0.032 Uiso 1 1 calc R U . . .
H10C H 0.5418 0.4781 0.9642 0.032 Uiso 1 1 calc R U . . .
N11 N 0.3333 0.6667 0.6584(14) 0.015(2) Uani 1 3 d S T P . .
H11A H 0.2984 0.5970 0.6229 0.022 Uiso 0.3333 1 calc R U P . .
H11B H 0.4030 0.7014 0.6229 0.022 Uiso 0.3333 1 calc R U P . .
H11C H 0.2986 0.7016 0.6229 0.022 Uiso 0.3333 1 calc R U P . .
N12 N 0.1866(6) 0.3980(6) 1.2061(9) 0.0192(13) Uani 1 1 d . . . . .
H12A H 0.2031 0.3967 1.3085 0.029 Uiso 1 1 calc R U . . .
H12B H 0.2050 0.3552 1.1498 0.029 Uiso 1 1 calc R U . . .
H12C H 0.1141 0.3727 1.1963 0.029 Uiso 1 1 calc R U . . .
N13 N 0.0626(9) 0.4206(7) 0.5925(14) 0.023(2) Uani 1 1 d . . . . .
N14 N -0.0113(11) 0.2384(9) 0.8711(13) 0.0251(19) Uani 1 1 d . . . . .
N15 N 0.2272(9) 0.2310(8) 0.9258(12) 0.0260(19) Uani 1 1 d . . . . .
N16 N 0.4055(13) 0.3467(8) 1.2122(15) 0.031(2) Uani 1 1 d . . . . .
Be1 Be 0.0000 0.0000 0.2106(19) 0.016(3) Uani 1 3 d S T P . .
Be2 Be 0.1326(8) 0.0686(8) 0.4787(11) 0.0151(17) Uani 1 1 d . . . . .
Be3 Be 0.6667 0.3333 0.523(2) 0.018(3) Uani 1 3 d S T P . .
Be4 Be 0.5987(8) 0.3973(8) 0.7893(13) 0.020(2) Uani 1 1 d . . . . .
Be5 Be 0.3333 0.6667 0.868(2) 0.017(3) Uani 1 3 d S T P . .
Be6 Be 0.2607(8) 0.5345(8) 1.1346(12) 0.0173(18) Uani 1 1 d . . . . .


_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 1.712(9) . ?
N1 Be2 1.714(12) . ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 Be2 1.721(12) . ?
N2 Be2 1.726(12) 2 ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N3 Be4 1.712(13) . ?
N3 Be3 1.718(10) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N4 Be4 1.722(13) 2_655 ?
N4 Be4 1.730(13) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N5 Be5 1.716(10) . ?
N5 Be6 1.719(13) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N6 Be6 1.718(13) . ?
N6 Be6 1.725(12) 3_565 ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
N7 Be1 1.78(2) . ?
N7 H7A 0.9100 . ?
N7 H7B 0.9100 . ?
N7 H7C 0.9100 . ?
N8 Be2 1.783(12) . ?
N8 H8A 0.9100 . ?
N8 H8B 0.9100 . ?
N8 H8C 0.9100 . ?
N9 Be3 1.78(2) . ?
N9 H9A 0.9100 . ?
N9 H9B 0.9100 . ?
N9 H9C 0.9100 . ?
N10 Be4 1.797(12) . ?
N10 H10A 0.9100 . ?
N10 H10B 0.9100 . ?
N10 H10C 0.9100 . ?
N11 Be5 1.79(2) . ?
N11 H11A 0.9100 . ?
N11 H11B 0.9100 . ?
N11 H11C 0.9100 . ?
N12 Be6 1.791(12) . ?
N12 H12A 0.9100 . ?
N12 H12B 0.9100 . ?
N12 H12C 0.9100 . ?
Be1 N1 1.712(9) 3 ?
Be1 N1 1.712(9) 2 ?
Be2 N2 1.726(12) 3 ?
Be3 N3 1.718(10) 3_665 ?
Be3 N3 1.718(10) 2_655 ?
Be4 N4 1.722(13) 3_665 ?
Be5 N5 1.716(10) 3_565 ?
Be5 N5 1.716(10) 2_665 ?
Be6 N6 1.725(12) 2_665 ?

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 Be2 110.6(8) . . ?
Be1 N1 H1A 109.5 . . ?
Be2 N1 H1A 109.5 . . ?
Be1 N1 H1B 109.5 . . ?
Be2 N1 H1B 109.5 . . ?
H1A N1 H1B 108.1 . . ?
Be2 N2 Be2 110.3(7) . 2 ?
Be2 N2 H2A 109.6 . . ?
Be2 N2 H2A 109.6 2 . ?
Be2 N2 H2B 109.6 . . ?
Be2 N2 H2B 109.6 2 . ?
H2A N2 H2B 108.1 . . ?
Be4 N3 Be3 109.3(8) . . ?
Be4 N3 H3A 109.8 . . ?
Be3 N3 H3A 109.8 . . ?
Be4 N3 H3B 109.8 . . ?
Be3 N3 H3B 109.8 . . ?
H3A N3 H3B 108.3 . . ?
Be4 N4 Be4 109.2(8) 2_655 . ?
Be4 N4 H4A 109.8 2_655 . ?
Be4 N4 H4A 109.8 . . ?
Be4 N4 H4B 109.8 2_655 . ?
Be4 N4 H4B 109.8 . . ?
H4A N4 H4B 108.3 . . ?
Be5 N5 Be6 109.4(8) . . ?
Be5 N5 H5A 109.8 . . ?
Be6 N5 H5A 109.8 . . ?
Be5 N5 H5B 109.8 . . ?
Be6 N5 H5B 109.8 . . ?
H5A N5 H5B 108.2 . . ?
Be6 N6 Be6 110.2(8) . 3_565 ?
Be6 N6 H6A 109.6 . . ?
Be6 N6 H6A 109.6 3_565 . ?
Be6 N6 H6B 109.6 . . ?
Be6 N6 H6B 109.6 3_565 . ?
H6A N6 H6B 108.1 . . ?
Be1 N7 H7A 109.5 . . ?
Be1 N7 H7B 109.5 . . ?
H7A N7 H7B 109.5 . . ?
Be1 N7 H7C 109.5 . . ?
H7A N7 H7C 109.5 . . ?
H7B N7 H7C 109.5 . . ?
Be2 N8 H8A 109.5 . . ?
Be2 N8 H8B 109.5 . . ?
H8A N8 H8B 109.5 . . ?
Be2 N8 H8C 109.5 . . ?
H8A N8 H8C 109.5 . . ?
H8B N8 H8C 109.5 . . ?
Be3 N9 H9A 109.5 . . ?
Be3 N9 H9B 109.5 . . ?
H9A N9 H9B 109.5 . . ?
Be3 N9 H9C 109.5 . . ?
H9A N9 H9C 109.5 . . ?
H9B N9 H9C 109.5 . . ?
Be4 N10 H10A 109.5 . . ?
Be4 N10 H10B 109.5 . . ?
H10A N10 H10B 109.5 . . ?
Be4 N10 H10C 109.5 . . ?
H10A N10 H10C 109.5 . . ?
H10B N10 H10C 109.5 . . ?
Be5 N11 H11A 109.5 . . ?
Be5 N11 H11B 109.5 . . ?
H11A N11 H11B 109.5 . . ?
Be5 N11 H11C 109.5 . . ?
H11A N11 H11C 109.5 . . ?
H11B N11 H11C 109.5 . . ?
Be6 N12 H12A 109.5 . . ?
Be6 N12 H12B 109.5 . . ?
H12A N12 H12B 109.5 . . ?
Be6 N12 H12C 109.5 . . ?
H12A N12 H12C 109.5 . . ?
H12B N12 H12C 109.5 . . ?
N1 Be1 N1 109.1(6) 3 2 ?
N1 Be1 N1 109.1(6) 3 . ?
N1 Be1 N1 109.1(6) 2 . ?
N1 Be1 N7 109.9(6) 3 . ?
N1 Be1 N7 109.9(6) 2 . ?
N1 Be1 N7 109.8(6) . . ?
N1 Be2 N2 109.0(6) . . ?
N1 Be2 N2 109.5(6) . 3 ?
N2 Be2 N2 108.3(7) . 3 ?
N1 Be2 N8 110.3(6) . . ?
N2 Be2 N8 110.1(6) . . ?
N2 Be2 N8 109.6(6) 3 . ?
N3 Be3 N3 109.7(6) . 3_665 ?
N3 Be3 N3 109.7(6) . 2_655 ?
N3 Be3 N3 109.7(6) 3_665 2_655 ?
N3 Be3 N9 109.2(6) . . ?
N3 Be3 N9 109.2(6) 3_665 . ?
N3 Be3 N9 109.2(6) 2_655 . ?
N3 Be4 N4 109.9(7) . 3_665 ?
N3 Be4 N4 108.5(7) . . ?
N4 Be4 N4 110.1(7) 3_665 . ?
N3 Be4 N10 109.7(7) . . ?
N4 Be4 N10 108.0(6) 3_665 . ?
N4 Be4 N10 110.6(7) . . ?
N5 Be5 N5 109.8(6) . 3_565 ?
N5 Be5 N5 109.8(6) . 2_665 ?
N5 Be5 N5 109.8(6) 3_565 2_665 ?
N5 Be5 N11 109.2(6) . . ?
N5 Be5 N11 109.2(6) 3_565 . ?
N5 Be5 N11 109.2(6) 2_665 . ?
N6 Be6 N5 107.4(7) . . ?
N6 Be6 N6 109.5(8) . 2_665 ?
N5 Be6 N6 110.5(6) . 2_665 ?
N6 Be6 N12 109.8(6) . . ?
N5 Be6 N12 110.3(7) . . ?
N6 Be6 N12 109.3(7) 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
N2 H2A Br1 0.91 3.04 3.753(7) 136.8 .
N4 H4A Br2 0.91 3.13 3.854(8) 137.4 2_655
N5 H5A Br1 0.91 3.06 3.799(8) 139.1 .
N7 H7A N15 0.91 2.44 3.323(10) 164.7 3_554
N7 H7B N15 0.91 2.44 3.323(10) 164.7 1_554
N7 H7C N15 0.91 2.44 3.323(10) 164.7 2_554
N8 H8A Br1 0.91 2.73 3.580(7) 156.6 .
N8 H8B Br2 0.91 2.81 3.668(7) 157.0 2_654
N8 H8C N14 0.91 2.38 3.236(14) 156.5 3
N9 H9A Br2 0.91 2.70 3.588(3) 164.5 1_554
N9 H9B Br2 0.91 2.70 3.588(3) 164.5 2_654
N9 H9C Br2 0.91 2.70 3.588(3) 164.5 3_664
N10 H10A Br1 0.91 2.98 3.689(8) 135.8 .
N10 H10B N13 0.91 2.35 3.190(14) 153.3 2_665
N10 H10C Br2 0.91 2.88 3.706(8) 151.2 .
N11 H11A Br1 0.91 2.81 3.595(3) 145.7 .
N11 H11B Br1 0.91 2.81 3.595(3) 145.7 2_665
N11 H11C Br1 0.91 2.81 3.595(3) 145.7 3_565
N12 H12A Br1 0.91 2.74 3.621(8) 163.2 1_556
N12 H12C Br2 0.91 2.67 3.563(7) 167.4 3_565

_refine_diff_density_max         1.946
_refine_diff_density_min         -1.089
_refine_diff_density_rms         0.275

####################################################################### 
# 
# 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_11
_database_code_depnum_ccdc_archive 'CCDC 1982300'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2020-02-06 deposited with the CCDC.	2020-05-04 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            'Be4 H36 Cl2 N14'
_chemical_formula_weight         339.37

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      trigonal
_space_group_IT_number           143
_space_group_name_H-M_alt        'P 3'
_space_group_name_Hall           'P 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   13.93420(10)
_cell_length_b                   13.93420(10)
_cell_length_c                   8.37270(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1407.86(3)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    25538
_cell_measurement_theta_min      7.04
_cell_measurement_theta_max      150.10

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_F_000             552
_exptl_transmission_factor_min   0.0892
_exptl_transmission_factor_max   0.3535
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_absorpt_coefficient_mu    3.195
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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            19167
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_theta_min         3.663
_diffrn_reflns_theta_max         78.738
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3314
_reflns_number_gt                3183
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.993
_reflns_Friedel_fraction_max     0.991
_reflns_Friedel_fraction_full    1.000

_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          
;
 Refined as a 2-component 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)+(0.0258P)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-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00106(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 1127 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.126(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3314
_refine_ls_number_parameters     327
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0189
_refine_ls_R_factor_gt           0.0175
_refine_ls_wR_factor_ref         0.0395
_refine_ls_wR_factor_gt          0.0392
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_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
Cl1 Cl 0.25422(4) 0.23366(4) -0.12249(4) 0.01694(12) Uani 1 1 d . . . . .
Cl2 Cl 0.35852(4) -0.07644(4) 0.54095(4) 0.01520(11) Uani 1 1 d . . . . .
N1 N 0.05752(16) 0.13311(16) 0.5270(2) 0.0136(3) Uani 1 1 d . . . . .
N2 N 0.13412(17) 0.07425(16) 0.2558(2) 0.0150(3) Uani 1 1 d . . . . .
N3 N 0.38682(15) 0.58672(15) 0.1864(2) 0.0128(3) Uani 1 1 d . . . . .
N4 N 0.25596(15) 0.53304(16) -0.0855(2) 0.0127(3) Uani 1 1 d . . . . .
N5 N 0.59462(16) 0.39458(17) 0.5680(2) 0.0137(4) Uani 1 1 d . . . . .
N6 N 0.53292(18) 0.25976(17) 0.8420(2) 0.0132(4) Uani 1 1 d . . . . .
N7 N 0.0000 0.0000 0.8093(3) 0.0138(5) Uani 1 3 d S T P . .
N8 N 0.12357(16) 0.27429(13) 0.2533(2) 0.0227(3) Uani 1 1 d . . . . .
N9 N 0.3333 0.6667 0.4686(3) 0.0129(4) Uani 1 3 d S T P . .
N10 N 0.44944(12) 0.50962(12) -0.09428(18) 0.0147(3) Uani 1 1 d . . . . .
N11 N 0.6667 0.3333 1.1239(3) 0.0167(5) Uani 1 3 d S T P . .
N12 N 0.39209(12) 0.18484(12) 0.56763(18) 0.0147(3) Uani 1 1 d . . . . .
N13 N 0.43914(18) 0.0919(2) 0.1875(3) 0.0215(4) Uani 1 1 d . . . . .
N14 N 0.4081(2) 0.3128(2) 0.2355(3) 0.0207(4) Uani 1 1 d . . . . .
N15 N 0.30839(18) 0.3957(2) 0.5218(3) 0.0194(5) Uani 1 1 d . . . . .
N16 N 0.0223(2) 0.2754(2) -0.1018(3) 0.0230(5) Uani 1 1 d . . . . .
Be1 Be 0.0000 0.0000 0.5950(4) 0.0129(6) Uani 1 3 d S T P . .
Be2 Be 0.05939(18) 0.13367(18) 0.3228(3) 0.0148(4) Uani 1 1 d . . . . .
Be3 Be 0.3333 0.6667 0.2533(4) 0.0120(6) Uani 1 3 d S T P . .
Be4 Be 0.38921(17) 0.58919(16) -0.0187(3) 0.0128(4) Uani 1 1 d . . . . .
Be5 Be 0.53261(17) 0.26090(16) 0.6369(3) 0.0134(4) Uani 1 1 d . . . . .
Be6 Be 0.6667 0.3333 0.9086(4) 0.0139(6) Uani 1 3 d S T P . .
H1A H 0.022(2) 0.162(2) 0.565(3) 0.029(7) Uiso 1 1 d . . . . .
H1B H 0.123(2) 0.174(2) 0.571(3) 0.029(7) Uiso 1 1 d . . . . .
H2A H 0.141(3) 0.076(3) 0.162(4) 0.039(9) Uiso 1 1 d . . . . .
H2B H 0.200(2) 0.110(2) 0.282(3) 0.034(7) Uiso 1 1 d . . . . .
H3A H 0.344(2) 0.516(2) 0.224(3) 0.029(6) Uiso 1 1 d . . . . .
H3B H 0.452(2) 0.609(2) 0.234(3) 0.021(6) Uiso 1 1 d . . . . .
H4A H 0.255(2) 0.531(2) -0.188(3) 0.029(7) Uiso 1 1 d . . . . .
H4B H 0.2187(19) 0.468(2) -0.055(3) 0.023(6) Uiso 1 1 d . . . . .
H6A H 0.505(2) 0.192(2) 0.876(3) 0.032(7) Uiso 1 1 d . . . . .
H6B H 0.487(2) 0.282(2) 0.877(3) 0.032(7) Uiso 1 1 d . . . . .
H7 H 0.062(2) 0.057(2) 0.850(3) 0.025(7) Uiso 1 1 d . . . . .
H5A H 0.559(2) 0.429(2) 0.589(3) 0.025(6) Uiso 1 1 d . . . . .
H5B H 0.592(2) 0.392(2) 0.472(3) 0.026(6) Uiso 1 1 d . . . . .
H9 H 0.338(2) 0.7297(19) 0.506(3) 0.019(6) Uiso 1 1 d . . . . .
H8A H 0.116(3) 0.280(4) 0.165(5) 0.082(13) Uiso 1 1 d . . . . .
H8B H 0.190(3) 0.310(3) 0.284(4) 0.050(9) Uiso 1 1 d . . . . .
H8C H 0.094(3) 0.313(3) 0.300(4) 0.070(10) Uiso 1 1 d . . . . .
H11 H 0.7325(19) 0.343(3) 1.157(3) 0.039(7) Uiso 1 1 d . . . . .
H10A H 0.477(2) 0.535(2) -0.191(3) 0.037(7) Uiso 1 1 d . . . . .
H10B H 0.396(2) 0.436(2) -0.103(3) 0.032(6) Uiso 1 1 d . . . . .
H10C H 0.502(2) 0.513(2) -0.038(3) 0.023(6) Uiso 1 1 d . . . . .
H12A H 0.387(2) 0.210(2) 0.467(3) 0.037(7) Uiso 1 1 d . . . . .
H12B H 0.374(2) 0.117(2) 0.562(3) 0.034(7) Uiso 1 1 d . . . . .
H12C H 0.349(2) 0.1953(19) 0.637(3) 0.026(6) Uiso 1 1 d . . . . .
H13A H 0.387(3) 0.054(3) 0.124(4) 0.039(9) Uiso 1 1 d . . . . .
H13B H 0.426(2) 0.056(3) 0.268(4) 0.028(7) Uiso 1 1 d . . . . .
H13C H 0.425(2) 0.150(3) 0.213(3) 0.034(9) Uiso 1 1 d . . . . .
H14A H 0.464(2) 0.362(2) 0.210(3) 0.016(7) Uiso 1 1 d . . . . .
H14B H 0.373(3) 0.333(3) 0.307(4) 0.040(9) Uiso 1 1 d . . . . .
H14C H 0.362(2) 0.291(2) 0.138(4) 0.036(8) Uiso 1 1 d . . . . .
H15A H 0.305(3) 0.355(3) 0.589(4) 0.042(10) Uiso 1 1 d . . . . .
H15B H 0.374(3) 0.463(3) 0.519(4) 0.040(10) Uiso 1 1 d . . . . .
H15C H 0.250(3) 0.410(3) 0.529(4) 0.035(9) Uiso 1 1 d . . . . .
H16A H 0.026(2) 0.312(2) -0.199(3) 0.029(8) Uiso 1 1 d . . . . .
H16B H 0.067(3) 0.256(3) -0.118(4) 0.040(10) Uiso 1 1 d . . . . .
H16C H -0.040(3) 0.216(3) -0.117(4) 0.022(8) Uiso 1 1 d . . . . .


_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 1.709(2) . ?
N1 Be2 1.710(3) . ?
N1 H1A 0.83(3) . ?
N1 H1B 0.88(3) . ?
N2 Be2 1.710(3) 3 ?
N2 Be2 1.717(3) . ?
N2 H2A 0.79(3) . ?
N2 H2B 0.82(3) . ?
N3 Be3 1.715(2) . ?
N3 Be4 1.718(3) . ?
N3 H3A 0.91(3) . ?
N3 H3B 0.89(3) . ?
N4 Be4 1.709(3) . ?
N4 Be4 1.715(3) 3_565 ?
N4 H4A 0.86(3) . ?
N4 H4B 0.83(2) . ?
N5 Be5 1.714(3) . ?
N5 Be5 1.715(3) 3_665 ?
N5 H5A 0.86(3) . ?
N5 H5B 0.81(3) . ?
N6 Be6 1.710(2) . ?
N6 Be5 1.717(3) . ?
N6 H6A 0.87(3) . ?
N6 H6B 0.89(3) . ?
N7 Be1 1.794(4) . ?
N7 H7 0.89(2) . ?
N8 Be2 1.796(3) . ?
N8 H8A 0.76(4) . ?
N8 H8B 0.84(4) . ?
N8 H8C 0.92(4) . ?
N9 Be3 1.803(4) . ?
N9 H9 0.90(2) . ?
N10 Be4 1.807(2) . ?
N10 H10A 0.89(3) . ?
N10 H10B 0.92(2) . ?
N10 H10C 0.85(3) . ?
N11 Be6 1.802(4) . ?
N11 H11 0.90(2) . ?
N12 Be5 1.794(3) . ?
N12 H12A 0.92(3) . ?
N12 H12B 0.85(3) . ?
N12 H12C 0.90(3) . ?
N13 H13A 0.84(3) . ?
N13 H13B 0.81(3) . ?
N13 H13C 0.95(3) . ?
N14 H14A 0.76(3) . ?
N14 H14B 0.91(3) . ?
N14 H14C 0.99(3) . ?
N15 H15A 0.78(4) . ?
N15 H15B 0.92(4) . ?
N15 H15C 0.93(3) . ?
N16 H16A 0.95(3) . ?
N16 H16B 0.81(4) . ?
N16 H16C 0.86(3) . ?
Be1 N1 1.709(2) 2 ?
Be1 N1 1.709(2) 3 ?
Be2 N2 1.710(3) 2 ?
Be3 N3 1.715(2) 3_565 ?
Be3 N3 1.715(2) 2_665 ?
Be4 N4 1.715(3) 2_665 ?
Be5 N5 1.715(3) 2_655 ?
Be6 N6 1.710(2) 2_655 ?
Be6 N6 1.710(2) 3_665 ?

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 Be2 109.62(17) . . ?
Be1 N1 H1A 108.9(17) . . ?
Be2 N1 H1A 112.9(17) . . ?
Be1 N1 H1B 109.6(17) . . ?
Be2 N1 H1B 114.0(18) . . ?
H1A N1 H1B 102(2) . . ?
Be2 N2 Be2 109.55(17) 3 . ?
Be2 N2 H2A 110(2) 3 . ?
Be2 N2 H2A 114(2) . . ?
Be2 N2 H2B 111.3(18) 3 . ?
Be2 N2 H2B 112.2(18) . . ?
H2A N2 H2B 99(3) . . ?
Be3 N3 Be4 108.90(16) . . ?
Be3 N3 H3A 108.6(15) . . ?
Be4 N3 H3A 111.2(15) . . ?
Be3 N3 H3B 109.0(16) . . ?
Be4 N3 H3B 115.6(17) . . ?
H3A N3 H3B 103(2) . . ?
Be4 N4 Be4 109.71(16) . 3_565 ?
Be4 N4 H4A 109.7(18) . . ?
Be4 N4 H4A 109.8(18) 3_565 . ?
Be4 N4 H4B 110.1(17) . . ?
Be4 N4 H4B 110.9(16) 3_565 . ?
H4A N4 H4B 107(2) . . ?
Be5 N5 Be5 109.75(17) . 3_665 ?
Be5 N5 H5A 114.7(16) . . ?
Be5 N5 H5A 111.1(16) 3_665 . ?
Be5 N5 H5B 107.9(18) . . ?
Be5 N5 H5B 112.0(17) 3_665 . ?
H5A N5 H5B 101(2) . . ?
Be6 N6 Be5 109.13(18) . . ?
Be6 N6 H6A 108.0(17) . . ?
Be5 N6 H6A 109.7(16) . . ?
Be6 N6 H6B 116.3(17) . . ?
Be5 N6 H6B 108.6(16) . . ?
H6A N6 H6B 105(2) . . ?
Be1 N7 H7 112.2(15) . . ?
Be2 N8 H8A 114(3) . . ?
Be2 N8 H8B 111(2) . . ?
H8A N8 H8B 114(4) . . ?
Be2 N8 H8C 113(2) . . ?
H8A N8 H8C 102(4) . . ?
H8B N8 H8C 102(3) . . ?
Be3 N9 H9 110.6(14) . . ?
Be4 N10 H10A 108.8(18) . . ?
Be4 N10 H10B 110.6(15) . . ?
H10A N10 H10B 108(2) . . ?
Be4 N10 H10C 115.3(17) . . ?
H10A N10 H10C 107(2) . . ?
H10B N10 H10C 107(2) . . ?
Be6 N11 H11 108.1(15) . . ?
Be5 N12 H12A 109.6(17) . . ?
Be5 N12 H12B 107.6(17) . . ?
H12A N12 H12B 109(2) . . ?
Be5 N12 H12C 108.5(16) . . ?
H12A N12 H12C 110(2) . . ?
H12B N12 H12C 112(2) . . ?
H13A N13 H13B 106(3) . . ?
H13A N13 H13C 101(3) . . ?
H13B N13 H13C 106(3) . . ?
H14A N14 H14B 111(3) . . ?
H14A N14 H14C 105(3) . . ?
H14B N14 H14C 105(3) . . ?
H15A N15 H15B 115(3) . . ?
H15A N15 H15C 111(3) . . ?
H15B N15 H15C 108(3) . . ?
H16A N16 H16B 101(3) . . ?
H16A N16 H16C 98(3) . . ?
H16B N16 H16C 104(3) . . ?
N1 Be1 N1 109.48(12) . 2 ?
N1 Be1 N1 109.48(12) . 3 ?
N1 Be1 N1 109.48(12) 2 3 ?
N1 Be1 N7 109.46(12) . . ?
N1 Be1 N7 109.46(12) 2 . ?
N1 Be1 N7 109.46(12) 3 . ?
N1 Be2 N2 108.42(15) . 2 ?
N1 Be2 N2 109.66(14) . . ?
N2 Be2 N2 110.08(18) 2 . ?
N1 Be2 N8 109.10(14) . . ?
N2 Be2 N8 110.37(14) 2 . ?
N2 Be2 N8 109.20(14) . . ?
N3 Be3 N3 109.88(12) . 3_565 ?
N3 Be3 N3 109.88(12) . 2_665 ?
N3 Be3 N3 109.88(12) 3_565 2_665 ?
N3 Be3 N9 109.06(12) . . ?
N3 Be3 N9 109.06(12) 3_565 . ?
N3 Be3 N9 109.06(12) 2_665 . ?
N4 Be4 N4 110.02(17) . 2_665 ?
N4 Be4 N3 108.20(14) . . ?
N4 Be4 N3 110.08(14) 2_665 . ?
N4 Be4 N10 109.65(13) . . ?
N4 Be4 N10 108.53(13) 2_665 . ?
N3 Be4 N10 110.37(13) . . ?
N5 Be5 N5 108.82(18) . 2_655 ?
N5 Be5 N6 110.14(14) . . ?
N5 Be5 N6 109.08(14) 2_655 . ?
N5 Be5 N12 109.96(13) . . ?
N5 Be5 N12 109.87(14) 2_655 . ?
N6 Be5 N12 108.96(14) . . ?
N6 Be6 N6 109.90(13) 2_655 3_665 ?
N6 Be6 N6 109.90(13) 2_655 . ?
N6 Be6 N6 109.90(13) 3_665 . ?
N6 Be6 N11 109.04(13) 2_655 . ?
N6 Be6 N11 109.04(13) 3_665 . ?
N6 Be6 N11 109.04(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
N3 H3B Cl2 0.89(3) 2.93(3) 3.6970(18) 145(2) 3_665
N6 H6B Cl1 0.89(3) 2.97(3) 3.727(2) 145(2) 1_556
N7 H7 Cl1 0.89(2) 2.59(2) 3.4557(7) 163(2) 1_556
N5 H5A Cl2 0.86(3) 2.95(2) 3.671(2) 143(2) 3_665
N9 H9 Cl2 0.90(2) 2.59(2) 3.4708(7) 165.8(19) 1_565
N8 H8A N16 0.76(4) 2.57(4) 3.294(3) 161(4) .
N8 H8B N15 0.84(4) 2.48(3) 3.193(3) 143(3) .
N8 H8C Cl2 0.92(4) 2.73(4) 3.5657(19) 153(3) 2
N11 H11 N13 0.90(2) 2.43(2) 3.315(2) 166(2) 2_656
N10 H10A Cl2 0.89(3) 2.63(3) 3.5127(16) 170(2) 3_664
N10 H10B Cl1 0.92(2) 2.51(3) 3.4324(16) 179(2) .
N10 H10C N13 0.85(3) 2.65(3) 3.475(3) 163(2) 3_665
N12 H12A N14 0.92(3) 2.34(3) 3.250(3) 167(2) .
N12 H12B Cl2 0.85(3) 2.60(3) 3.4381(15) 169(2) .
N12 H12C Cl1 0.90(3) 2.61(3) 3.4917(15) 169(2) 1_556
N13 H13A N16 0.84(3) 2.49(4) 3.316(4) 167(3) 3
N13 H13B Cl2 0.81(3) 2.78(3) 3.590(2) 174(3) .
N13 H13C N14 0.95(3) 2.40(3) 3.340(4) 170(2) .
N14 H14B N15 0.91(3) 2.36(3) 3.259(3) 170(3) .
N14 H14C Cl1 0.99(3) 2.54(3) 3.526(2) 175(2) .
N15 H15A Cl1 0.78(4) 2.83(3) 3.582(3) 163(3) 1_556
N15 H15B Cl2 0.92(4) 2.59(4) 3.507(2) 172(3) 3_665
N15 H15C Cl2 0.93(3) 2.61(3) 3.541(2) 176(3) 2
N16 H16A Cl2 0.95(3) 2.64(3) 3.575(3) 169(2) 2_554
N16 H16B Cl1 0.81(4) 2.78(4) 3.562(3) 165(3) .
N16 H16C Cl1 0.86(3) 2.71(3) 3.563(2) 172(3) 2

_refine_diff_density_max         0.178
_refine_diff_density_min         -0.120
_refine_diff_density_rms         0.032

####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 1982299'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2020-02-06 deposited with the CCDC.	2020-05-04 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         '[Be4(NH2)6(NH3)4]2I6(NH3)'
_chemical_formula_sum            'Be4 H42 I2 N16'
_chemical_formula_weight         556.33

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           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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'
'-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                   14.0852(2)
_cell_length_b                   10.17190(10)
_cell_length_c                   18.4646(2)
_cell_angle_alpha                90
_cell_angle_beta                 112.2170(10)
_cell_angle_gamma                90
_cell_volume                     2449.08(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    39920
_cell_measurement_theta_min      10.35
_cell_measurement_theta_max      152.92

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.509
_exptl_crystal_F_000             1104
_exptl_transmission_factor_min   0.0003
_exptl_transmission_factor_max   0.0089
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    20.295
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_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            21462
_diffrn_reflns_av_unetI/netI     0.0160
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         5.175
_diffrn_reflns_theta_max         75.696
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2547
_reflns_number_gt                2518
_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)+(0.0689P)²+3.9091P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.00068(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2547
_refine_ls_number_parameters     140
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0343
_refine_ls_wR_factor_ref         0.0886
_refine_ls_wR_factor_gt          0.0885
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.072
_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
Be1 Be 0.4021(2) 0.5935(3) 0.25341(18) 0.0152(6) Uani 1 1 d . . . . .
Be2 Be 0.5456(3) 0.7889(4) 0.3322(2) 0.0172(6) Uani 1 1 d . . . . .
I1 I 0.54487(2) 0.76760(2) 0.59443(2) 0.02094(13) Uani 1 1 d . . . . .
N1 N 0.35734(16) 0.6885(2) 0.17052(13) 0.0178(4) Uani 1 1 d . . . . .
H1A H 0.3036 0.7382 0.1705 0.021 Uiso 1 1 calc R U . . .
H1B H 0.3350 0.6360 0.1274 0.021 Uiso 1 1 calc R U . . .
N2 N 0.44771(16) 0.6917(2) 0.33529(12) 0.0165(4) Uani 1 1 d . . . . .
H2A H 0.3961 0.7432 0.3376 0.020 Uiso 1 1 calc R U . . .
H2B H 0.4708 0.6406 0.3790 0.020 Uiso 1 1 calc R U . . .
N3 N 0.5000 0.8865(3) 0.2500 0.0177(6) Uani 1 2 d S T P . .
H3A H 0.5512 0.9390 0.2479 0.021 Uiso 0.5 1 calc R U P . .
H3B H 0.4488 0.9390 0.2521 0.021 Uiso 0.5 1 calc R U P . .
N4 N 0.5000 0.4965(3) 0.2500 0.0157(6) Uani 1 2 d S T P . .
H4A H 0.4765 0.4441 0.2069 0.019 Uiso 0.5 1 calc R U P . .
H4B H 0.5235 0.4441 0.2931 0.019 Uiso 0.5 1 calc R U P . .
N5 N 0.30204(16) 0.4918(2) 0.25973(12) 0.0174(4) Uani 1 1 d . . . . .
H5A H 0.2610 0.5404 0.2774 0.026 Uiso 1 1 calc R U . . .
H5B H 0.3300 0.4243 0.2934 0.026 Uiso 1 1 calc R U . . .
H5C H 0.2642 0.4589 0.2116 0.026 Uiso 1 1 calc R U . . .
N6 N 0.40822(18) 0.8909(3) 0.08252(13) 0.0205(5) Uani 1 1 d . . . . .
H6A H 0.3428 0.9165 0.0735 0.031 Uiso 1 1 calc R U . . .
H6B H 0.4094 0.8450 0.0406 0.031 Uiso 1 1 calc R U . . .
H6C H 0.4490 0.9631 0.0902 0.031 Uiso 1 1 calc R U . . .
N7 N 0.18421(19) 0.4064(3) 0.08284(14) 0.0231(5) Uani 1 1 d . . . . .
N8 N 0.1618(2) 0.6722(3) 0.31711(16) 0.0243(5) Uani 1 1 d . . . . .
N9 N 0.8269(2) 1.0159(3) 0.47837(19) 0.0319(6) Uani 1 1 d . . . . .
H1 H 0.156(4) 0.476(5) 0.089(3) 0.042(12) Uiso 1 1 d . . . . .
H2 H 0.137(3) 0.351(5) 0.049(3) 0.036(11) Uiso 1 1 d . . . . .
H3 H 0.228(3) 0.420(5) 0.061(3) 0.038(11) Uiso 1 1 d . . . . .
H4 H 0.126(4) 0.690(6) 0.265(3) 0.056(14) Uiso 1 1 d . . . . .
H5 H 0.114(3) 0.666(5) 0.338(2) 0.037(11) Uiso 1 1 d . . . . .
H6 H 0.200(3) 0.736(4) 0.333(3) 0.018(10) Uiso 1 1 d . . . . .
H7 H 0.802(5) 1.054(8) 0.442(4) 0.09(2) Uiso 1 1 d . . . . .
H8 H 0.852(3) 0.955(5) 0.470(2) 0.029(10) Uiso 1 1 d . . . . .
H9 H 0.873(3) 1.073(4) 0.510(3) 0.032(10) Uiso 1 1 d . . . . .


_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
Be1 N1 1.716(4) . ?
Be1 N4 1.716(4) . ?
Be1 N2 1.721(4) . ?
Be1 N5 1.787(4) . ?
Be2 N2 1.715(4) . ?
Be2 N3 1.722(4) . ?
Be2 N1 1.723(4) 2_655 ?
Be2 N6 1.791(4) 2_655 ?
N1 Be2 1.722(4) 2_655 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
N3 Be2 1.722(4) 2_655 ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N4 Be1 1.716(4) 2_655 ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
N5 H5C 0.9100 . ?
N6 Be2 1.791(4) 2_655 ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
N6 H6C 0.9100 . ?
N7 H1 0.84(5) . ?
N7 H2 0.91(5) . ?
N7 H3 0.87(5) . ?
N8 H4 0.93(6) . ?
N8 H5 0.89(4) . ?
N8 H6 0.83(4) . ?
N9 H7 0.74(8) . ?
N9 H8 0.76(5) . ?
N9 H9 0.90(5) . ?

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 N4 108.67(19) . . ?
N1 Be1 N2 110.3(2) . . ?
N4 Be1 N2 109.12(19) . . ?
N1 Be1 N5 110.58(19) . . ?
N4 Be1 N5 109.5(2) . . ?
N2 Be1 N5 108.68(19) . . ?
N2 Be2 N3 109.0(2) . . ?
N2 Be2 N1 108.4(2) . 2_655 ?
N3 Be2 N1 110.6(2) . 2_655 ?
N2 Be2 N6 109.5(2) . 2_655 ?
N3 Be2 N6 109.3(2) . 2_655 ?
N1 Be2 N6 109.9(2) 2_655 2_655 ?
Be1 N1 Be2 109.4(2) . 2_655 ?
Be1 N1 H1A 109.8 . . ?
Be2 N1 H1A 109.8 2_655 . ?
Be1 N1 H1B 109.8 . . ?
Be2 N1 H1B 109.8 2_655 . ?
H1A N1 H1B 108.2 . . ?
Be2 N2 Be1 110.0(2) . . ?
Be2 N2 H2A 109.7 . . ?
Be1 N2 H2A 109.7 . . ?
Be2 N2 H2B 109.7 . . ?
Be1 N2 H2B 109.7 . . ?
H2A N2 H2B 108.2 . . ?
Be2 N3 Be2 109.5(3) . 2_655 ?
Be2 N3 H3A 109.8 . . ?
Be2 N3 H3A 109.8 2_655 . ?
Be2 N3 H3B 109.8 . . ?
Be2 N3 H3B 109.8 2_655 . ?
H3A N3 H3B 108.2 . . ?
Be1 N4 Be1 109.8(3) . 2_655 ?
Be1 N4 H4A 109.7 . . ?
Be1 N4 H4A 109.7 2_655 . ?
Be1 N4 H4B 109.7 . . ?
Be1 N4 H4B 109.7 2_655 . ?
H4A N4 H4B 108.2 . . ?
Be1 N5 H5A 109.5 . . ?
Be1 N5 H5B 109.5 . . ?
H5A N5 H5B 109.5 . . ?
Be1 N5 H5C 109.5 . . ?
H5A N5 H5C 109.5 . . ?
H5B N5 H5C 109.5 . . ?
Be2 N6 H6A 109.5 2_655 . ?
Be2 N6 H6B 109.5 2_655 . ?
H6A N6 H6B 109.5 . . ?
Be2 N6 H6C 109.5 2_655 . ?
H6A N6 H6C 109.5 . . ?
H6B N6 H6C 109.5 . . ?
H1 N7 H2 111(4) . . ?
H1 N7 H3 112(4) . . ?
H2 N7 H3 104(4) . . ?
H4 N8 H5 105(4) . . ?
H4 N8 H6 104(5) . . ?
H5 N8 H6 113(4) . . ?
H7 N9 H8 110(6) . . ?
H7 N9 H9 103(6) . . ?
H8 N9 H9 113(4) . . ?

_refine_diff_density_max         1.605
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.161

####################################################################### 
# 
# 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_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 1982297'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2020-02-06 deposited with the CCDC.	2020-05-04 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 H33 Be4 N15 S2'
_chemical_formula_sum            'C2 H33 Be4 N15 S2'
_chemical_formula_weight         367.59

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      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                   9.9563(2)
_cell_length_b                   8.58430(10)
_cell_length_c                   24.7099(4)
_cell_angle_alpha                90
_cell_angle_beta                 97.4540(10)
_cell_angle_gamma                90
_cell_volume                     2094.06(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    24774
_cell_measurement_theta_min      7.21
_cell_measurement_theta_max      159.36

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.166
_exptl_crystal_F_000             792
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_exptl_absorpt_coefficient_mu    2.446
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2652
_exptl_absorpt_correction_T_max  0.8966
_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            24637
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.608
_diffrn_reflns_theta_max         78.973
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4449
_reflns_number_gt                3534
_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)+(0.0397P)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_number_reflns         4449
_refine_ls_number_parameters     340
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0355
_refine_ls_R_factor_gt           0.0239
_refine_ls_wR_factor_ref         0.0597
_refine_ls_wR_factor_gt          0.0567
_refine_ls_goodness_of_fit_ref   0.905
_refine_ls_restrained_S_all      0.905
_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
S1 S 0.04816(3) 0.19720(4) 0.27429(2) 0.02560(7) Uani 1 1 d . . . . .
S2 S 1.33932(3) 0.79885(3) 0.46356(2) 0.02347(7) Uani 1 1 d . . . . .
N1 N 0.60628(9) 0.53293(11) 0.40233(3) 0.01529(17) Uani 1 1 d . . . . .
N2 N 0.64512(9) 0.74444(10) 0.32009(3) 0.01561(17) Uani 1 1 d . . . . .
N3 N 0.91266(9) 0.79616(10) 0.36936(3) 0.01509(17) Uani 1 1 d . . . . .
N4 N 0.87043(9) 0.58837(11) 0.45247(3) 0.01484(17) Uani 1 1 d . . . . .
N5 N 0.82378(9) 0.49502(10) 0.34267(4) 0.01585(17) Uani 1 1 d . . . . .
N6 N 0.69450(10) 0.83846(10) 0.42877(4) 0.01608(18) Uani 1 1 d . . . . .
N7 N 0.55559(10) 0.43423(11) 0.29071(4) 0.01874(19) Uani 1 1 d . . . . .
N8 N 0.74062(11) 1.05621(11) 0.34507(4) 0.02083(19) Uani 1 1 d . . . . .
N9 N 1.09438(9) 0.53947(11) 0.39248(4) 0.01752(18) Uani 1 1 d . . . . .
N10 N 0.64894(10) 0.63181(11) 0.51423(4) 0.01685(18) Uani 1 1 d . . . . .
N11 N 0.23156(11) 0.44847(12) 0.28418(4) 0.0293(2) Uani 1 1 d . . . . .
N12 N 1.14369(11) 0.80022(12) 0.53620(5) 0.0332(2) Uani 1 1 d . . . . .
N13 N 0.72216(12) 0.32847(15) 0.19132(5) 0.0306(2) Uani 1 1 d . . . . .
N14 N 0.43831(12) 1.14780(14) 0.35501(5) 0.0305(2) Uani 1 1 d . . . . .
N15 N 0.86060(11) 0.84220(12) 0.58096(4) 0.0228(2) Uani 1 1 d . . . . .
C1 C 0.15526(11) 0.34459(14) 0.28023(4) 0.0222(2) Uani 1 1 d . . . . .
C2 C 1.22411(11) 0.79999(12) 0.50612(4) 0.0217(2) Uani 1 1 d . . . . .
Be1 Be 0.65909(14) 0.55323(16) 0.33909(5) 0.0155(2) Uani 1 1 d . . . . .
Be2 Be 0.74740(14) 0.85609(15) 0.36580(5) 0.0153(2) Uani 1 1 d . . . . .
Be3 Be 0.92305(13) 0.60597(15) 0.38950(5) 0.0143(2) Uani 1 1 d . . . . .
Be4 Be 0.70618(14) 0.64746(15) 0.44857(5) 0.0147(2) Uani 1 1 d . . . . .
H1A H 0.5230(15) 0.5578(16) 0.4014(5) 0.029(4) Uiso 1 1 d . . . . .
H1B H 0.6154(15) 0.4363(17) 0.4128(6) 0.032(4) Uiso 1 1 d . . . . .
H7A H 0.5439(15) 0.3420(19) 0.3036(6) 0.036(4) Uiso 1 1 d . . . . .
H7B H 0.4721(15) 0.4711(16) 0.2819(5) 0.027(4) Uiso 1 1 d . . . . .
H7C H 0.5892(14) 0.4216(16) 0.2614(6) 0.031(4) Uiso 1 1 d . . . . .
H2A H 0.5615(15) 0.7730(15) 0.3177(5) 0.026(4) Uiso 1 1 d . . . . .
H2B H 0.6669(14) 0.7576(15) 0.2869(6) 0.026(4) Uiso 1 1 d . . . . .
H8B H 0.6591(16) 1.0933(17) 0.3426(6) 0.034(4) Uiso 1 1 d . . . . .
H8C H 0.7899(15) 1.1153(18) 0.3684(6) 0.035(4) Uiso 1 1 d . . . . .
H9A H 1.1198(15) 0.5380(17) 0.3592(6) 0.035(4) Uiso 1 1 d . . . . .
H9B H 1.1544(15) 0.6009(18) 0.4129(6) 0.035(4) Uiso 1 1 d . . . . .
H9C H 1.1050(16) 0.4440(19) 0.4056(6) 0.041(4) Uiso 1 1 d . . . . .
H4B H 0.9176(14) 0.6439(16) 0.4767(5) 0.025(4) Uiso 1 1 d . . . . .
H4A H 0.8806(14) 0.4959(18) 0.4628(5) 0.027(4) Uiso 1 1 d . . . . .
H10B H 0.5689(14) 0.6734(15) 0.5140(5) 0.023(3) Uiso 1 1 d . . . . .
H10A H 0.6457(14) 0.5332(18) 0.5249(5) 0.032(4) Uiso 1 1 d . . . . .
H5A H 0.8363(15) 0.4004(18) 0.3495(6) 0.036(4) Uiso 1 1 d . . . . .
H5B H 0.8542(15) 0.5033(17) 0.3112(6) 0.033(4) Uiso 1 1 d . . . . .
H6A H 0.6137(17) 0.8732(18) 0.4294(6) 0.038(4) Uiso 1 1 d . . . . .
H3A H 0.9408(15) 0.8084(17) 0.3373(6) 0.037(4) Uiso 1 1 d . . . . .
H3B H 0.9628(15) 0.8558(18) 0.3916(6) 0.038(4) Uiso 1 1 d . . . . .
H15B H 0.8830(16) 0.8479(18) 0.6159(6) 0.039(4) Uiso 1 1 d . . . . .
H15A H 0.8183(17) 0.9308(19) 0.5708(6) 0.044(5) Uiso 1 1 d . . . . .
H15C H 0.9371(17) 0.8459(19) 0.5656(6) 0.044(5) Uiso 1 1 d . . . . .
H10C H 0.7003(16) 0.6835(18) 0.5401(6) 0.039(4) Uiso 1 1 d . . . . .
H6B H 0.7431(16) 0.8961(18) 0.4534(6) 0.038(4) Uiso 1 1 d . . . . .
H8A H 0.7715(16) 1.0679(18) 0.3117(7) 0.043(4) Uiso 1 1 d . . . . .
H14C H 0.4508(19) 1.130(2) 0.3915(8) 0.065(6) Uiso 1 1 d . . . . .
H14B H 0.3770(19) 1.226(2) 0.3496(7) 0.060(5) Uiso 1 1 d . . . . .
H14A H 0.401(2) 1.069(2) 0.3408(8) 0.067(6) Uiso 1 1 d . . . . .
H13B H 0.793(2) 0.383(2) 0.2041(8) 0.065(6) Uiso 1 1 d . . . . .
H13C H 0.7390(18) 0.239(2) 0.2030(7) 0.056(6) Uiso 1 1 d . . . . .
H13A H 0.7248(17) 0.3249(19) 0.1557(7) 0.046(5) Uiso 1 1 d . . . . .


_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 1.6489(13) . ?
S2 C2 1.6538(12) . ?
N1 Be1 1.7211(15) . ?
N1 Be4 1.7223(16) . ?
N2 Be1 1.7080(16) . ?
N2 Be2 1.7127(16) . ?
N3 Be3 1.7060(16) . ?
N3 Be2 1.7153(16) . ?
N4 Be4 1.7030(16) . ?
N4 Be3 1.7116(15) . ?
N5 Be1 1.7054(16) . ?
N5 Be3 1.7107(15) . ?
N6 Be4 1.7106(15) . ?
N6 Be2 1.7128(16) . ?
N7 Be1 1.7931(16) . ?
N8 Be2 1.7914(16) . ?
N9 Be3 1.7912(16) . ?
N10 Be4 1.7930(16) . ?
N11 C1 1.1673(16) . ?
N12 C2 1.1611(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 Be4 109.05(8) . . ?
Be1 N2 Be2 109.65(8) . . ?
Be3 N3 Be2 108.87(8) . . ?
Be4 N4 Be3 109.10(7) . . ?
Be1 N5 Be3 109.82(8) . . ?
Be4 N6 Be2 109.09(8) . . ?
N11 C1 S1 179.54(11) . . ?
N12 C2 S2 179.61(12) . . ?
N5 Be1 N2 109.83(9) . . ?
N5 Be1 N1 109.16(8) . . ?
N2 Be1 N1 108.86(8) . . ?
N5 Be1 N7 109.46(8) . . ?
N2 Be1 N7 110.18(8) . . ?
N1 Be1 N7 109.32(8) . . ?
N2 Be2 N6 108.85(8) . . ?
N2 Be2 N3 110.50(9) . . ?
N6 Be2 N3 109.44(8) . . ?
N2 Be2 N8 110.54(8) . . ?
N6 Be2 N8 109.87(8) . . ?
N3 Be2 N8 107.62(8) . . ?
N3 Be3 N5 109.12(8) . . ?
N3 Be3 N4 109.61(8) . . ?
N5 Be3 N4 110.35(8) . . ?
N3 Be3 N9 109.78(8) . . ?
N5 Be3 N9 108.29(8) . . ?
N4 Be3 N9 109.68(8) . . ?
N4 Be4 N6 109.32(9) . . ?
N4 Be4 N1 109.58(8) . . ?
N6 Be4 N1 110.21(8) . . ?
N4 Be4 N10 110.00(8) . . ?
N6 Be4 N10 108.23(8) . . ?
N1 Be4 N10 109.48(8) . . ?

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
N7 H7A N14 0.867(16) 2.417(16) 3.2271(15) 155.7(13) 1_545 yes
N7 H7B N11 0.890(15) 2.411(15) 3.2115(15) 149.9(12) . yes
N7 H7C N13 0.844(15) 2.446(15) 3.2654(15) 164.0(13) . yes
N2 H2B N11 0.882(14) 2.694(14) 3.4690(13) 147.4(11) 2_655 yes
N8 H8B N14 0.866(16) 2.306(16) 3.1511(16) 164.9(13) . yes
N8 H8C N12 0.870(15) 2.473(15) 3.2519(15) 149.4(13) 3_776 yes
N9 H9A N11 0.892(15) 2.408(15) 3.2535(13) 158.4(13) 1_655 yes
N9 H9B S2 0.902(15) 2.691(15) 3.5886(10) 173.6(12) . yes
N9 H9C N15 0.883(16) 2.497(17) 3.3601(14) 166.0(13) 3_766 yes
N4 H4A N12 0.836(15) 2.554(15) 3.3520(14) 160.1(12) 3_766 yes
N10 H10B S2 0.872(14) 2.683(14) 3.4821(10) 152.9(11) 1_455 yes
N10 H10A S2 0.889(15) 2.866(16) 3.7370(10) 166.7(12) 3_766 yes
N5 H5B S1 0.873(15) 2.951(15) 3.7345(10) 150.2(12) 2_655 yes
N6 H6A S2 0.860(16) 3.030(16) 3.7615(10) 144.3(12) 1_455 yes
N3 H3A S1 0.880(15) 2.934(15) 3.7194(9) 149.6(12) 2_655 yes
N15 H15B S1 0.865(16) 2.739(16) 3.5903(10) 168.6(13) 3_666 yes
N15 H15A S2 0.890(17) 2.867(17) 3.7548(11) 175.0(14) 3_776 yes
N15 H15C N12 0.894(17) 2.302(17) 3.1790(15) 166.6(14) . yes
N10 H10C N15 0.884(16) 2.238(17) 3.0855(13) 160.7(14) . yes
N8 H8A N11 0.921(16) 2.579(16) 3.3708(14) 144.4(12) 2_655 yes
N14 H14A N13 0.83(2) 2.48(2) 3.3019(17) 173.1(17) 2_655 yes
N13 H13C N11 0.831(19) 2.525(19) 3.3388(17) 166.5(16) 2_645 yes
N13 H13A S2 0.884(17) 2.942(17) 3.8050(12) 165.7(14) 2_745 yes

_refine_diff_density_max         0.224
_refine_diff_density_min         -0.138
_refine_diff_density_rms         0.035

####################################################################### 
# 
# 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 1982301'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2020-02-06 deposited with the CCDC.	2020-05-04 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            'C8 H16 Be N6'
_chemical_formula_weight         205.28

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      tetragonal
_space_group_IT_number           94
_space_group_name_H-M_alt        'P 42 21 2'
_space_group_name_Hall           'P 4n 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'
'-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, x, -z'
'-y, -x, -z'

_cell_length_a                   9.9478(3)
_cell_length_b                   9.9478(3)
_cell_length_c                   5.4077(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     535.14(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4208
_cell_measurement_theta_min      12.58
_cell_measurement_theta_max      151.23

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             220
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_exptl_absorpt_coefficient_mu    0.667
_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            3136
_diffrn_reflns_av_unetI/netI     0.0231
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -6
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_theta_min         6.292
_diffrn_reflns_theta_max         75.716
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             555
_reflns_number_gt                484
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.552
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    1.000

_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          
;
 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)+(0.0651P)²+0.0470P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.2(11)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         555
_refine_ls_number_parameters     42
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0369
_refine_ls_wR_factor_ref         0.0996
_refine_ls_wR_factor_gt          0.0954
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.083
_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 0.35858(15) 0.51531(17) 0.3292(3) 0.0219(5) Uani 1 1 d . . . . .
H1 H 0.336(3) 0.455(3) 0.215(5) 0.031(7) Uiso 1 1 d . . . . .
Be1 Be 0.5000 0.5000 0.5000 0.0205(10) Uani 1 4 d S T P . .
C1 C 0.27281(19) 0.61413(18) 0.3414(4) 0.0206(5) Uani 1 1 d . . . . .
N2 N 0.28001(16) 0.71999(16) 0.5000 0.0226(6) Uani 1 2 d S T P . .
C2 C 0.1535(2) 0.6158(2) 0.1703(5) 0.0266(5) Uani 1 1 d . . . . .
H2A H 0.0858 0.6784 0.2339 0.040 Uiso 1 1 calc R U . . .
H2B H 0.1149 0.5253 0.1603 0.040 Uiso 1 1 calc R U . . .
H2C H 0.1822 0.6447 0.0053 0.040 Uiso 1 1 calc R U . . .


_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 C1 1.303(2) . ?
N1 Be1 1.6897(17) . ?
N1 H1 0.89(3) . ?
Be1 N1 1.6898(17) 8_666 ?
Be1 N1 1.6898(17) 2_665 ?
Be1 N1 1.6898(17) 7_556 ?
C1 N2 1.360(2) . ?
C1 C2 1.505(3) . ?
N2 C1 1.360(2) 8_666 ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?

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
C1 N1 Be1 125.82(15) . . ?
C1 N1 H1 112.5(17) . . ?
Be1 N1 H1 121.6(17) . . ?
N1 Be1 N1 98.55(12) . 8_666 ?
N1 Be1 N1 113.73(12) . 2_665 ?
N1 Be1 N1 116.67(11) 8_666 2_665 ?
N1 Be1 N1 116.67(11) . 7_556 ?
N1 Be1 N1 113.73(12) 8_666 7_556 ?
N1 Be1 N1 98.55(12) 2_665 7_556 ?
N1 C1 N2 125.56(19) . . ?
N1 C1 C2 119.55(19) . . ?
N2 C1 C2 114.89(18) . . ?
C1 N2 C1 118.6(2) 8_666 . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?

_refine_diff_density_max         0.148
_refine_diff_density_min         -0.147
_refine_diff_density_rms         0.039

####################################################################### 
# 
# 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 1982302'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2020-02-06 deposited with the CCDC.	2020-05-04 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         ?
_chemical_formula_sum            'C2 H36 Be4 N16'
_chemical_formula_weight         320.51

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      trigonal
_space_group_IT_number           143
_space_group_name_H-M_alt        'P 3'
_space_group_name_Hall           'P 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'

_cell_length_a                   14.1334(3)
_cell_length_b                   14.1334(3)
_cell_length_c                   8.5563(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     1480.16(8)
_cell_formula_units_Z            3
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    29697
_cell_measurement_theta_min      7.22
_cell_measurement_theta_max      158.92

_exptl_crystal_description       Cuboctahedron
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_F_000             528
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    0.616
_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            31215
_diffrn_reflns_av_unetI/netI     0.0210
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         3.611
_diffrn_reflns_theta_max         79.077
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.977
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4168
_reflns_number_gt                3657
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.970
_reflns_Friedel_fraction_max     0.962
_reflns_Friedel_fraction_full    0.995

_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)+(0.0564P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_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         4168
_refine_ls_number_parameters     255
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.0862
_refine_ls_wR_factor_gt          0.0840
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_restrained_S_all      0.995
_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 0.27026(13) 0.73620(13) 0.09275(19) 0.0230(4) Uani 1 1 d . . . . .
H1A H 0.269536 0.736966 0.199082 0.028 Uiso 1 1 calc R U . . .
H1B H 0.236960 0.772997 0.057439 0.028 Uiso 1 1 calc R U . . .
N2 N 0.20160(14) 0.60606(14) -0.17386(19) 0.0244(4) Uani 1 1 d . . . . .
H2A H 0.162968 0.536600 -0.211249 0.029 Uiso 1 1 calc R U . . .
H2B H 0.169195 0.643878 -0.208493 0.029 Uiso 1 1 calc R U . . .
N3 N 0.06673(13) 0.13183(13) 0.53579(17) 0.0224(3) Uani 1 1 d . . . . .
H3A H 0.033117 0.167950 0.498986 0.027 Uiso 1 1 calc R U . . .
H3B H 0.136824 0.166756 0.500318 0.027 Uiso 1 1 calc R U . . .
N4 N 0.13166(13) 0.06603(13) 0.80382(18) 0.0225(4) Uani 1 1 d . . . . .
H4A H 0.132137 0.066282 0.910174 0.027 Uiso 1 1 calc R U . . .
H4B H 0.202155 0.101351 0.770017 0.027 Uiso 1 1 calc R U . . .
N5 N 0.79875(13) 0.40612(13) 1.4391(2) 0.0246(3) Uani 1 1 d . . . . .
H5A H 0.868752 0.444785 1.403734 0.030 Uiso 1 1 calc R U . . .
H5B H 0.800290 0.406926 1.545388 0.030 Uiso 1 1 calc R U . . .
N6 N 0.74172(14) 0.27638(13) 1.1729(2) 0.0241(3) Uani 1 1 d . . . . .
H6A H 0.712983 0.207105 1.135553 0.029 Uiso 1 1 calc R U . . .
H6B H 0.811837 0.316175 1.138451 0.029 Uiso 1 1 calc R U . . .
N7 N 0.333333 0.666667 -0.4519(3) 0.0273(6) Uani 1 3 d S T P . .
H7A H 0.394080 0.666752 -0.487335 0.041 Uiso 0.3333 1 calc R U P . .
H7B H 0.333248 0.727328 -0.487335 0.041 Uiso 0.3333 1 calc R U P . .
H7C H 0.272672 0.605920 -0.487335 0.041 Uiso 0.3333 1 calc R U P . .
N8 N 0.06348(13) 0.53649(14) 0.0961(2) 0.0261(4) Uani 1 1 d . . . . .
H8A H 0.035168 0.581457 0.084489 0.039 Uiso 1 1 calc R U . . .
H8B H 0.062267 0.519457 0.198889 0.039 Uiso 1 1 calc R U . . .
H8C H 0.022866 0.474211 0.040125 0.039 Uiso 1 1 calc R U . . .
N9 N 0.000000 0.000000 0.2594(3) 0.0249(6) Uani 1 3 d S T P . .
H9A H 0.065038 0.055159 0.223929 0.037 Uiso 0.3333 1 calc R U P . .
H9B H -0.055159 0.009879 0.223929 0.037 Uiso 0.3333 1 calc R U P . .
H9C H -0.009879 -0.065038 0.223929 0.037 Uiso 0.3333 1 calc R U P . .
N10 N 0.13428(13) 0.27054(12) 0.80520(18) 0.0246(4) Uani 1 1 d . . . . .
H10A H 0.206084 0.293218 0.822005 0.037 Uiso 1 1 calc R U . . .
H10B H 0.103034 0.274516 0.896119 0.037 Uiso 1 1 calc R U . . .
H10C H 0.128400 0.314162 0.732220 0.037 Uiso 1 1 calc R U . . .
N11 N 0.666667 0.333333 0.8961(3) 0.0264(6) Uani 1 3 d S T P . .
H11A H 0.675382 0.277458 0.860610 0.040 Uiso 0.3333 1 calc R U P . .
H11B H 0.722542 0.397924 0.860610 0.040 Uiso 0.3333 1 calc R U P . .
H11C H 0.602076 0.324618 0.860610 0.040 Uiso 0.3333 1 calc R U P . .
N12 N 0.81395(13) 0.21219(13) 1.4511(2) 0.0279(3) Uani 1 1 d . . . . .
H12A H 0.791399 0.189250 1.550600 0.042 Uiso 1 1 calc R U . . .
H12B H 0.886686 0.261888 1.451208 0.042 Uiso 1 1 calc R U . . .
H12C H 0.801340 0.153999 1.390765 0.042 Uiso 1 1 calc R U . . .
N13 N -0.06914(16) 0.36022(17) -0.1638(3) 0.0326(4) Uani 1 1 d . . . . .
N14 N -0.22297(16) 0.00086(17) 0.1762(2) 0.0347(4) Uani 1 1 d . . . . .
N15 N -0.38765(19) -0.05827(19) 0.4707(3) 0.0388(5) Uani 1 1 d . . . . .
N16 N 0.00750(18) 0.25622(18) 1.1265(2) 0.0323(4) Uani 1 1 d . . . . .
N17 N 0.4369(2) 0.3028(2) 0.7873(3) 0.0510(6) Uani 1 1 d . . . . .
N18 N 0.0885(2) 0.3957(2) 0.5228(3) 0.0564(7) Uani 1 1 d . . . . .
C1 C 0.3820(2) 0.3176(2) 0.8571(3) 0.0463(6) Uani 1 1 d . . . . .
C2 C 0.0872(2) 0.4467(2) 0.4310(3) 0.0451(6) Uani 1 1 d . . . . .
Be1 Be 0.333333 0.666667 -0.2409(5) 0.0243(8) Uani 1 3 d S T P . .
Be2 Be 0.20120(19) 0.60393(19) 0.0267(3) 0.0226(5) Uani 1 1 d . . . . .
Be3 Be 0.000000 0.000000 0.4692(5) 0.0223(8) Uani 1 3 d S T P . .
Be4 Be 0.06615(19) 0.13253(19) 0.7370(3) 0.0221(5) Uani 1 1 d . . . . .
Be5 Be 0.666667 0.333333 1.1061(5) 0.0233(7) Uani 1 3 d S T P . .
Be6 Be 0.73957(19) 0.2744(2) 1.3734(3) 0.0243(5) Uani 1 1 d . . . . .
H13A H -0.126(2) 0.302(2) -0.166(3) 0.036(7) Uiso 1 1 d . . . . .
H13B H -0.083(3) 0.422(3) -0.185(4) 0.061(9) Uiso 1 1 d . . . . .
H13C H -0.025(3) 0.358(3) -0.240(4) 0.060(9) Uiso 1 1 d . . . . .
H14A H -0.249(2) 0.018(2) 0.091(3) 0.037(7) Uiso 1 1 d . . . . .
H14B H -0.258(3) 0.001(3) 0.253(4) 0.060(10) Uiso 1 1 d . . . . .
H14C H -0.230(2) -0.070(3) 0.148(4) 0.056(9) Uiso 1 1 d . . . . .
H15A H -0.456(2) -0.079(2) 0.454(3) 0.024(6) Uiso 1 1 d . . . . .
H15B H -0.396(3) -0.131(3) 0.485(4) 0.064(10) Uiso 1 1 d . . . . .
H15C H -0.371(3) -0.032(3) 0.572(4) 0.092(14) Uiso 1 1 d . . . . .
H16A H -0.022(2) 0.288(2) 1.060(3) 0.053(9) Uiso 1 1 d . . . . .
H16B H -0.043(2) 0.197(2) 1.160(3) 0.038(8) Uiso 1 1 d . . . . .
H16C H 0.022(2) 0.294(2) 1.222(3) 0.046(8) Uiso 1 1 d . . . . .


_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 Be2 1.715(3) . ?
N1 Be2 1.718(3) 3_565 ?
N2 Be1 1.713(2) . ?
N2 Be2 1.717(3) . ?
N3 Be3 1.711(2) . ?
N3 Be4 1.721(3) . ?
N4 Be4 1.714(3) . ?
N4 Be4 1.716(3) 3 ?
N5 Be6 1.710(3) . ?
N5 Be6 1.716(3) 2_655 ?
N6 Be6 1.715(3) . ?
N6 Be5 1.719(2) . ?
N7 Be1 1.806(5) . ?
N8 Be2 1.787(3) . ?
N9 Be3 1.795(5) . ?
N10 Be4 1.787(3) . ?
N11 Be5 1.798(5) . ?
N12 Be6 1.801(3) . ?
N17 C1 1.079(3) . ?
N18 C2 1.072(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
Be2 N1 Be2 109.44(17) . 3_565 ?
Be1 N2 Be2 109.67(18) . . ?
Be3 N3 Be4 109.72(17) . . ?
Be4 N4 Be4 109.98(17) . 3 ?
Be6 N5 Be6 109.64(18) . 2_655 ?
Be6 N6 Be5 109.27(18) . . ?
N2 Be1 N2 109.39(14) 3_565 2_665 ?
N2 Be1 N2 109.39(14) 3_565 . ?
N2 Be1 N2 109.39(14) 2_665 . ?
N2 Be1 N7 109.55(14) 3_565 . ?
N2 Be1 N7 109.55(14) 2_665 . ?
N2 Be1 N7 109.55(14) . . ?
N1 Be2 N2 108.36(15) . . ?
N1 Be2 N1 110.02(17) . 2_665 ?
N2 Be2 N1 109.92(15) . 2_665 ?
N1 Be2 N8 110.28(15) . . ?
N2 Be2 N8 109.53(15) . . ?
N1 Be2 N8 108.72(14) 2_665 . ?
N3 Be3 N3 109.50(13) 2 3 ?
N3 Be3 N3 109.50(13) 2 . ?
N3 Be3 N3 109.50(13) 3 . ?
N3 Be3 N9 109.44(13) 2 . ?
N3 Be3 N9 109.44(13) 3 . ?
N3 Be3 N9 109.44(13) . . ?
N4 Be4 N4 108.93(16) . 2 ?
N4 Be4 N3 108.97(14) . . ?
N4 Be4 N3 109.71(15) 2 . ?
N4 Be4 N10 110.21(15) . . ?
N4 Be4 N10 109.65(14) 2 . ?
N3 Be4 N10 109.35(14) . . ?
N6 Be5 N6 109.52(14) . 3_665 ?
N6 Be5 N6 109.52(14) . 2_655 ?
N6 Be5 N6 109.52(14) 3_665 2_655 ?
N6 Be5 N11 109.42(14) . . ?
N6 Be5 N11 109.42(14) 3_665 . ?
N6 Be5 N11 109.42(14) 2_655 . ?
N5 Be6 N6 108.41(15) . . ?
N5 Be6 N5 109.94(17) . 3_665 ?
N6 Be6 N5 110.02(15) . 3_665 ?
N5 Be6 N12 108.84(15) . . ?
N6 Be6 N12 111.54(15) . . ?
N5 Be6 N12 108.08(15) 3_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
N8 H8C N13 0.91 2.29 3.161(3) 160.7 . yes
N9 H9A N14 0.91 2.35 3.237(2) 165.9 3 yes
N9 H9B N14 0.91 2.35 3.237(2) 165.9 . yes
N9 H9C N14 0.91 2.35 3.237(2) 165.9 2 yes
N10 H10B N16 0.91 2.33 3.232(3) 171.4 . yes
N10 H10C N18 0.91 2.35 3.245(3) 169.3 . yes
N11 H11A N17 0.91 2.28 3.193(3) 176.5 2_655 yes
N11 H11B N17 0.91 2.28 3.193(3) 176.5 3_665 yes
N11 H11C N17 0.91 2.28 3.193(3) 176.5 . yes
N12 H12A N17 0.91 2.33 3.224(3) 166.1 2_656 yes
N12 H12B N18 0.91 2.59 3.478(3) 166.3 1_656 yes
N13 H13A N17 0.81(3) 2.47(3) 3.277(3) 172(2) 2_554 yes
N13 H13B N17 0.99(3) 2.46(3) 3.446(3) 173(3) 3_564 yes
N13 H13C N18 0.92(3) 2.47(3) 3.360(3) 163(3) 1_554 yes
N14 H14B N15 0.82(3) 2.45(3) 3.243(3) 163(3) . yes
N14 H14C N16 0.98(3) 2.38(3) 3.345(3) 170(3) 2_554 yes
N15 H15B N18 0.98(3) 2.51(3) 3.491(4) 174(3) 2 yes
N16 H16A N13 0.94(3) 2.42(3) 3.331(3) 165(3) 1_556 yes
N16 H16B N14 0.83(3) 2.67(3) 3.473(3) 162(3) 1_556 yes

_refine_diff_density_max         0.213
_refine_diff_density_min         -0.188
_refine_diff_density_rms         0.030

####################################################################### 
# 
# 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_6_sq
_database_code_depnum_ccdc_archive 'CCDC 1982303'
loop_
_audit_author_name
_audit_author_address
'Matthias Mueller'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2020-02-06 deposited with the CCDC.	2020-05-04 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         'C45 H69 Be8 I2 N21 O + 5(C5H5N)'
_chemical_formula_sum            'C20 H44 Be8 I2 N16 O'
_chemical_formula_weight         850.59

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'
I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           66
_space_group_name_H-M_alt        'C c c m'
_space_group_name_Hall           '-C 2 2c'

_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'
'-x, y, -z+1/2'
'x, -y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z-1/2'
'-x, y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z-1/2'

_cell_length_a                   20.1994(2)
_cell_length_b                   21.2118(2)
_cell_length_c                   23.3361(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9998.72(19)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    73657
_cell_measurement_theta_min      6.04
_cell_measurement_theta_max      152.20

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_F_000             3376
_exptl_transmission_factor_min   0.0913
_exptl_transmission_factor_max   0.3520
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_exptl_absorpt_coefficient_mu    10.116
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_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            72530
_diffrn_reflns_av_unetI/netI     0.0105
_diffrn_reflns_av_R_equivalents  0.0319
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.021
_diffrn_reflns_theta_max         76.241
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5329
_reflns_number_gt                4864
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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 2014/5 (Sheldrick, 2014)'
_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)+(0.0371P)²+25.2398P] 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         5329
_refine_ls_number_parameters     215
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0270
_refine_ls_wR_factor_ref         0.0732
_refine_ls_wR_factor_gt          0.0710
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
I1 I 0.01218(2) 0.14321(2) 0.500000 0.02837(7) Uani 1 2 d S T P . .
Be1 Be 0.28963(16) 0.35261(15) 0.82463(14) 0.0276(6) Uani 1 1 d . . . . .
Be2 Be 0.31303(16) 0.22766(15) 0.79677(14) 0.0275(6) Uani 1 1 d . . . . .
O O 0.250000 0.250000 0.75459(9) 0.0264(5) Uani 1 2 d S T P . .
N1 N 0.32561(10) 0.28575(10) 0.84920(9) 0.0283(4) Uani 1 1 d . . . . .
H1A H 0.306871 0.273801 0.882955 0.034 Uiso 1 1 calc R U . . .
H1B H 0.369670 0.292013 0.854997 0.034 Uiso 1 1 calc R U . . .
C1 C 0.03878(13) 0.36956(12) 0.66363(11) 0.0326(5) Uani 1 1 d . . . . .
H1 H 0.059628 0.393634 0.692836 0.039 Uiso 1 1 calc R U . . .
N2 N 0.20655(10) 0.34444(9) 0.82869(9) 0.0277(4) Uani 1 1 d . . . . .
H2A H 0.186068 0.376578 0.809905 0.033 Uiso 1 1 calc R U . . .
H2B H 0.193173 0.344813 0.865928 0.033 Uiso 1 1 calc R U . . .
I2 I 0.13657(2) 0.500000 0.750000 0.02592(7) Uani 1 2 d S T P . .
C2 C -0.01875(14) 0.39230(13) 0.63974(13) 0.0361(6) Uani 1 1 d . . . . .
H2 H -0.036933 0.431251 0.652219 0.043 Uiso 1 1 calc R U . . .
N3 N 0.31094(12) 0.36663(10) 0.75547(9) 0.0329(5) Uani 1 1 d . . . . .
H3A H 0.355673 0.364271 0.751339 0.040 Uiso 1 1 calc R U . . .
H3B H 0.297591 0.405917 0.744901 0.040 Uiso 1 1 calc R U . . .
N4 N 0.20227(11) 0.34110(10) 0.67980(9) 0.0304(4) Uani 1 1 d . . . . .
H4A H 0.190492 0.378034 0.696820 0.036 Uiso 1 1 calc R U . . .
H4B H 0.210594 0.348782 0.642113 0.036 Uiso 1 1 calc R U . . .
C4 C -0.02171(16) 0.30098(14) 0.58073(13) 0.0434(7) Uani 1 1 d . . . . .
H4 H -0.042151 0.275707 0.552160 0.052 Uiso 1 1 calc R U . . .
Be4 Be 0.14020(17) 0.28747(16) 0.68640(14) 0.0315(7) Uani 1 1 d . . . . .
N5 N 0.11597(11) 0.27981(10) 0.75563(8) 0.0295(4) Uani 1 1 d . . . . .
H5A H 0.089884 0.245136 0.759788 0.035 Uiso 1 1 calc R U . . .
H5B H 0.092494 0.314306 0.766796 0.035 Uiso 1 1 calc R U . . .
C5 C 0.03666(16) 0.28167(13) 0.60648(12) 0.0409(7) Uani 1 1 d . . . . .
H5 H 0.056019 0.243103 0.594340 0.049 Uiso 1 1 calc R U . . .
N6 N 0.16972(12) 0.21748(10) 0.66154(9) 0.0343(5) Uani 1 1 d . . . . .
H6A H 0.189808 0.222906 0.626986 0.041 Uiso 1 1 calc R U . . .
H6B H 0.136073 0.189341 0.657257 0.041 Uiso 1 1 calc R U . . .
C10 C 0.37044(12) 0.42190(13) 0.90049(11) 0.0329(5) Uani 1 1 d . . . . .
H10 H 0.392299 0.383090 0.907895 0.039 Uiso 1 1 calc R U . . .
C3 C -0.04975(14) 0.35758(14) 0.59725(12) 0.0392(6) Uani 1 1 d . . . . .
H3 H -0.089360 0.372311 0.579858 0.047 Uiso 1 1 calc R U . . .
Be3 Be 0.27265(18) 0.31022(15) 0.71282(14) 0.0310(7) Uani 1 1 d . . . . .
C6 C 0.28768(15) 0.47664(13) 0.85597(15) 0.0459(8) Uani 1 1 d . . . . .
H6 H 0.250131 0.477536 0.831467 0.055 Uiso 1 1 calc R U . . .
C7 C 0.3091(2) 0.53233(15) 0.8797(2) 0.0838(17) Uani 1 1 d . . . . .
H7 H 0.286839 0.570699 0.871498 0.101 Uiso 1 1 calc R U . . .
N7 N 0.06701(11) 0.31459(10) 0.64751(9) 0.0320(5) Uani 1 1 d . . . . .
N8 N 0.31702(10) 0.42169(10) 0.86571(9) 0.0284(4) Uani 1 1 d . . . . .
C8 C 0.3635(2) 0.53193(16) 0.9157(2) 0.0769(15) Uani 1 1 d . . . . .
H8 H 0.378781 0.569719 0.933074 0.092 Uiso 1 1 calc R U . . .
C9 C 0.39463(15) 0.47583(15) 0.92567(13) 0.0439(7) Uani 1 1 d . . . . .
H9 H 0.432545 0.474078 0.949709 0.053 Uiso 1 1 calc R U . . .


_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
Be1 N2 1.690(4) . ?
Be1 N1 1.694(4) . ?
Be1 N3 1.696(4) . ?
Be1 N8 1.836(4) . ?
Be2 O 1.678(3) . ?
Be2 N5 1.733(4) 6 ?
Be2 N2 1.746(4) 6 ?
Be2 N1 1.755(4) . ?
Be2 Be2 2.717(6) 6 ?
O Be3 1.671(4) . ?
O Be3 1.671(4) 6 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
C1 N7 1.351(3) . ?
C1 C2 1.376(4) . ?
C1 H1 0.9500 . ?
N2 H2A 0.9100 . ?
N2 H2B 0.9100 . ?
C2 C3 1.385(4) . ?
C2 H2 0.9500 . ?
N3 Be3 1.738(4) . ?
N3 H3A 0.9100 . ?
N3 H3B 0.9100 . ?
N4 Be4 1.700(4) . ?
N4 Be3 1.745(4) . ?
N4 H4A 0.9100 . ?
N4 H4B 0.9100 . ?
C4 C3 1.382(4) . ?
C4 C5 1.385(4) . ?
C4 H4 0.9500 . ?
Be4 N5 1.696(4) . ?
Be4 N6 1.702(4) . ?
Be4 N7 1.828(4) . ?
N5 H5A 0.9100 . ?
N5 H5B 0.9100 . ?
C5 N7 1.334(3) . ?
C5 H5 0.9500 . ?
N6 Be3 1.770(4) 6 ?
N6 H6A 0.9100 . ?
N6 H6B 0.9100 . ?
C10 N8 1.350(3) . ?
C10 C9 1.376(4) . ?
C10 H10 0.9500 . ?
C3 H3 0.9500 . ?
Be3 Be3 2.714(7) 6 ?
C6 N8 1.327(3) . ?
C6 C7 1.375(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.382(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.366(5) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?

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 108.7(2) . . ?
N2 Be1 N3 108.9(2) . . ?
N1 Be1 N3 111.1(2) . . ?
N2 Be1 N8 110.59(19) . . ?
N1 Be1 N8 111.23(19) . . ?
N3 Be1 N8 106.3(2) . . ?
O Be2 N5 109.20(19) . 6 ?
O Be2 N2 109.0(2) . 6 ?
N5 Be2 N2 110.09(19) 6 6 ?
O Be2 N1 108.70(19) . . ?
N5 Be2 N1 109.3(2) 6 . ?
N2 Be2 N1 110.51(19) 6 . ?
O Be2 Be2 35.93(12) . 6 ?
N5 Be2 Be2 143.85(14) 6 6 ?
N2 Be2 Be2 95.34(19) 6 6 ?
N1 Be2 Be2 83.73(15) . 6 ?
Be3 O Be3 108.6(3) . 6 ?
Be3 O Be2 110.52(17) . . ?
Be3 O Be2 109.53(16) 6 . ?
Be3 O Be2 109.53(16) . 6 ?
Be3 O Be2 110.52(17) 6 6 ?
Be2 O Be2 108.1(2) . 6 ?
Be1 N1 Be2 106.85(18) . . ?
Be1 N1 H1A 110.4 . . ?
Be2 N1 H1A 110.4 . . ?
Be1 N1 H1B 110.4 . . ?
Be2 N1 H1B 110.4 . . ?
H1A N1 H1B 108.6 . . ?
N7 C1 C2 123.1(2) . . ?
N7 C1 H1 118.5 . . ?
C2 C1 H1 118.5 . . ?
Be1 N2 Be2 106.90(18) . 6 ?
Be1 N2 H2A 110.3 . . ?
Be2 N2 H2A 110.3 6 . ?
Be1 N2 H2B 110.3 . . ?
Be2 N2 H2B 110.3 6 . ?
H2A N2 H2B 108.6 . . ?
C1 C2 C3 119.1(2) . . ?
C1 C2 H2 120.5 . . ?
C3 C2 H2 120.5 . . ?
Be1 N3 Be3 108.1(2) . . ?
Be1 N3 H3A 110.1 . . ?
Be3 N3 H3A 110.1 . . ?
Be1 N3 H3B 110.1 . . ?
Be3 N3 H3B 110.1 . . ?
H3A N3 H3B 108.4 . . ?
Be4 N4 Be3 108.04(19) . . ?
Be4 N4 H4A 110.1 . . ?
Be3 N4 H4A 110.1 . . ?
Be4 N4 H4B 110.1 . . ?
Be3 N4 H4B 110.1 . . ?
H4A N4 H4B 108.4 . . ?
C3 C4 C5 119.0(3) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
N5 Be4 N4 111.3(2) . . ?
N5 Be4 N6 110.0(2) . . ?
N4 Be4 N6 107.1(2) . . ?
N5 Be4 N7 105.7(2) . . ?
N4 Be4 N7 109.9(2) . . ?
N6 Be4 N7 112.9(2) . . ?
Be4 N5 Be2 107.3(2) . 6 ?
Be4 N5 H5A 110.2 . . ?
Be2 N5 H5A 110.3 6 . ?
Be4 N5 H5B 110.2 . . ?
Be2 N5 H5B 110.2 6 . ?
H5A N5 H5B 108.5 . . ?
N7 C5 C4 123.2(3) . . ?
N7 C5 H5 118.4 . . ?
C4 C5 H5 118.4 . . ?
Be4 N6 Be3 106.83(19) . 6 ?
Be4 N6 H6A 110.4 . . ?
Be3 N6 H6A 110.4 6 . ?
Be4 N6 H6B 110.4 . . ?
Be3 N6 H6B 110.4 6 . ?
H6A N6 H6B 108.6 . . ?
N8 C10 C9 122.9(3) . . ?
N8 C10 H10 118.5 . . ?
C9 C10 H10 118.5 . . ?
C4 C3 C2 118.4(3) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
O Be3 N3 108.3(2) . . ?
O Be3 N4 108.8(2) . . ?
N3 Be3 N4 110.9(2) . . ?
O Be3 N6 108.72(19) . 6 ?
N3 Be3 N6 108.8(2) . 6 ?
N4 Be3 N6 111.2(2) . 6 ?
O Be3 Be3 35.70(13) . 6 ?
N3 Be3 Be3 142.96(14) . 6 ?
N4 Be3 Be3 94.5(2) . 6 ?
N6 Be3 Be3 84.80(16) 6 6 ?
N8 C6 C7 123.0(3) . . ?
N8 C6 H6 118.5 . . ?
C7 C6 H6 118.5 . . ?
C6 C7 C8 119.4(3) . . ?
C6 C7 H7 120.3 . . ?
C8 C7 H7 120.3 . . ?
C5 N7 C1 117.2(2) . . ?
C5 N7 Be4 124.3(2) . . ?
C1 N7 Be4 118.3(2) . . ?
C6 N8 C10 117.2(2) . . ?
C6 N8 Be1 118.5(2) . . ?
C10 N8 Be1 123.9(2) . . ?
C9 C8 C7 118.3(3) . . ?
C9 C8 H8 120.8 . . ?
C7 C8 H8 120.8 . . ?
C8 C9 C10 119.2(3) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
C1 H1 I2 0.95 3.05 3.952(3) 159.7 . yes
N2 H2A I2 0.91 3.13 4.032(2) 170.6 . yes
N4 H4A I2 0.91 3.07 3.976(2) 174.2 . yes
C4 H4 I1 0.95 3.25 3.901(3) 127.1 . yes
C5 H5 I1 0.95 3.18 3.879(3) 131.7 . yes
C10 H10 I1 0.95 3.29 3.937(2) 127.5 15_556 yes
C6 H6 I2 0.95 3.02 3.959(3) 171.6 . yes
C9 H9 I1 0.95 3.19 3.876(3) 130.9 15_556 yes

_refine_diff_density_max         0.530
_refine_diff_density_min         -0.479
_refine_diff_density_rms         0.071



