# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_LTH482
_database_code_depnum_ccdc_archive 'CCDC 2373010'
loop_
_audit_author_name
_audit_author_address
'Sergei Ivlev'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2024-07-23 deposited with the CCDC.	2024-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C28 H34 Be N4'
_chemical_formula_sum            'C28 H34 Be N4'
_chemical_formula_weight         435.60

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      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

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

_cell_length_a                   16.1582(15)
_cell_length_b                   8.6300(5)
_cell_length_c                   17.5982(15)
_cell_angle_alpha                90
_cell_angle_beta                 95.030(7)
_cell_angle_gamma                90
_cell_volume                     2444.5(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100
_cell_measurement_reflns_used    10424
_cell_measurement_theta_min      2.75
_cell_measurement_theta_max      76.07

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.184
_exptl_crystal_F_000             936
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.531
_shelx_estimated_absorpt_T_min   0.816
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4104
_exptl_absorpt_correction_T_max  0.7612
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;

_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'

_diffrn_detector                 Pilatus300K
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_detector_area_resol_mean 5.81

_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_radiation_probe          x-ray
_diffrn_source_voltage           50
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.5 mm diameter'

_diffrn_ambient_temperature      100

_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 2899 frames, detector distance = 60 mm
;

_diffrn_reflns_number            15241
_diffrn_reflns_av_unetI/netI     0.0259
_diffrn_reflns_av_R_equivalents  0.0257
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         5.046
_diffrn_reflns_theta_max         76.127
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             2534
_reflns_number_gt                1981
_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       
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_cell_refinement       
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_reduction        
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image
processing, for the correction and scaling of reflection intensities and
for outlier rejection, version 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0609P)²+0.2685P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.00074(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2534
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0380
_refine_ls_wR_factor_ref         0.1085
_refine_ls_wR_factor_gt          0.1043
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.064
_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 0.31259(8) 0.61204(13) 0.56893(6) 0.0334(3) Uani 1 1 d . . . . .
H1 H 0.3092(9) 0.5495(18) 0.6123(9) 0.040 Uiso 1 1 d . U . . .
N2 N 0.18898(6) 0.39459(12) 0.55068(5) 0.0247(2) Uani 1 1 d . . . . .
C1 C 0.34488(8) 0.75462(14) 0.59214(7) 0.0249(3) Uani 1 1 d . . . . .
C2 C 0.35928(7) 0.79027(15) 0.67139(6) 0.0234(3) Uani 1 1 d . . . . .
C3 C 0.39012(7) 0.93421(15) 0.69484(7) 0.0258(3) Uani 1 1 d . . . . .
H3 H 0.397872 0.956186 0.747882 0.031 Uiso 1 1 calc R U . . .
C4 C 0.41013(7) 1.04780(15) 0.64298(7) 0.0259(3) Uani 1 1 d . . . . .
C5 C 0.39919(7) 1.00952(15) 0.56589(7) 0.0259(3) Uani 1 1 d . . . . .
H5 H 0.413656 1.084055 0.529599 0.031 Uiso 1 1 calc R U . . .
C6 C 0.36805(8) 0.86710(15) 0.53953(7) 0.0270(3) Uani 1 1 d . . . . .
C7 C 0.34226(8) 0.66836(16) 0.72960(7) 0.0287(3) Uani 1 1 d . . . . .
H7A H 0.284176 0.635053 0.721393 0.043 Uiso 1 1 calc R U . . .
H7B H 0.352708 0.711709 0.781017 0.043 Uiso 1 1 calc R U . . .
H7C H 0.378836 0.579204 0.724161 0.043 Uiso 1 1 calc R U . . .
C8 C 0.36276(11) 0.83392(17) 0.45504(7) 0.0406(4) Uani 1 1 d . . . . .
H8A H 0.379204 0.726346 0.446768 0.061 Uiso 1 1 calc R U . . .
H8B H 0.400058 0.903926 0.430495 0.061 Uiso 1 1 calc R U . . .
H8C H 0.305583 0.849942 0.432988 0.061 Uiso 1 1 calc R U . . .
C9 C 0.44234(9) 1.20532(16) 0.66898(8) 0.0340(3) Uani 1 1 d . . . . .
H9A H 0.396911 1.266110 0.687372 0.051 Uiso 1 1 calc R U . . .
H9B H 0.464411 1.259308 0.626120 0.051 Uiso 1 1 calc R U . . .
H9C H 0.486566 1.192634 0.710305 0.051 Uiso 1 1 calc R U . . .
C10 C 0.22567(8) 0.28244(16) 0.59443(7) 0.0286(3) Uani 1 1 d . . . . .
H10 H 0.283998 0.268906 0.594248 0.034 Uiso 1 1 calc R U . . .
C11 C 0.18292(10) 0.18591(17) 0.63962(8) 0.0383(3) Uani 1 1 d . . . . .
H11 H 0.211265 0.108215 0.670014 0.046 Uiso 1 1 calc R U . . .
C12 C 0.09794(10) 0.20447(19) 0.63980(8) 0.0435(4) Uani 1 1 d . . . . .
H12 H 0.066815 0.139808 0.670437 0.052 Uiso 1 1 calc R U . . .
C13 C 0.05924(9) 0.3181(2) 0.59488(9) 0.0431(4) Uani 1 1 d . . . . .
H13 H 0.000937 0.333210 0.594114 0.052 Uiso 1 1 calc R U . . .
C14 C 0.10616(8) 0.40986(17) 0.55096(7) 0.0329(3) Uani 1 1 d . . . . .
H14 H 0.078825 0.487148 0.519569 0.040 Uiso 1 1 calc R U . . .
Be1 Be 0.250000 0.5332(3) 0.500000 0.0277(5) Uani 1 2 d S T 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 C1 1.3841(15) . ?
N1 Be1 1.6557(14) . ?
N1 H1 0.941(16) . ?
N2 C10 1.3420(15) . ?
N2 C14 1.3451(16) . ?
N2 Be1 1.8312(19) . ?
C1 C6 1.4144(16) . ?
C1 C2 1.4272(16) . ?
C2 C3 1.3876(17) . ?
C2 C7 1.5104(16) . ?
C3 C4 1.3964(17) . ?
C3 H3 0.9500 . ?
C4 C5 1.3924(16) . ?
C4 C9 1.5121(17) . ?
C5 C6 1.3922(17) . ?
C5 H5 0.9500 . ?
C6 C8 1.5093(16) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.3783(18) . ?
C10 H10 0.9500 . ?
C11 C12 1.383(2) . ?
C11 H11 0.9500 . ?
C12 C13 1.375(2) . ?
C12 H12 0.9500 . ?
C13 C14 1.379(2) . ?
C13 H13 0.9500 . ?
C14 H14 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
C1 N1 Be1 140.50(12) . . ?
C1 N1 H1 108.5(10) . . ?
Be1 N1 H1 106.5(10) . . ?
C10 N2 C14 117.26(12) . . ?
C10 N2 Be1 121.41(9) . . ?
C14 N2 Be1 121.07(10) . . ?
N1 C1 C6 122.10(11) . . ?
N1 C1 C2 120.34(11) . . ?
C6 C1 C2 117.51(11) . . ?
C3 C2 C1 120.47(11) . . ?
C3 C2 C7 120.26(10) . . ?
C1 C2 C7 119.26(11) . . ?
C2 C3 C4 122.13(11) . . ?
C2 C3 H3 118.9 . . ?
C4 C3 H3 118.9 . . ?
C5 C4 C3 116.96(12) . . ?
C5 C4 C9 121.27(12) . . ?
C3 C4 C9 121.78(11) . . ?
C6 C5 C4 123.05(12) . . ?
C6 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C5 C6 C1 119.77(11) . . ?
C5 C6 C8 118.91(11) . . ?
C1 C6 C8 121.29(11) . . ?
C2 C7 H7A 109.5 . . ?
C2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N2 C10 C11 123.26(13) . . ?
N2 C10 H10 118.4 . . ?
C11 C10 H10 118.4 . . ?
C10 C11 C12 118.64(14) . . ?
C10 C11 H11 120.7 . . ?
C12 C11 H11 120.7 . . ?
C13 C12 C11 118.87(13) . . ?
C13 C12 H12 120.6 . . ?
C11 C12 H12 120.6 . . ?
C12 C13 C14 119.15(13) . . ?
C12 C13 H13 120.4 . . ?
C14 C13 H13 120.4 . . ?
N2 C14 C13 122.81(14) . . ?
N2 C14 H14 118.6 . . ?
C13 C14 H14 118.6 . . ?
N1 Be1 N1 131.50(17) . 2_556 ?
N1 Be1 N2 107.74(6) . 2_556 ?
N1 Be1 N2 103.42(6) 2_556 2_556 ?
N1 Be1 N2 103.41(6) . . ?
N1 Be1 N2 107.75(6) 2_556 . ?
N2 Be1 N2 98.40(13) 2_556 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Be1 N1 C1 C6 -37.4(2) . . . . ?
Be1 N1 C1 C2 145.33(13) . . . . ?
N1 C1 C2 C3 -178.74(11) . . . . ?
C6 C1 C2 C3 3.88(17) . . . . ?
N1 C1 C2 C7 2.51(18) . . . . ?
C6 C1 C2 C7 -174.87(11) . . . . ?
C1 C2 C3 C4 -1.58(18) . . . . ?
C7 C2 C3 C4 177.15(11) . . . . ?
C2 C3 C4 C5 -1.13(18) . . . . ?
C2 C3 C4 C9 178.95(11) . . . . ?
C3 C4 C5 C6 1.49(18) . . . . ?
C9 C4 C5 C6 -178.59(12) . . . . ?
C4 C5 C6 C1 0.89(19) . . . . ?
C4 C5 C6 C8 -176.85(12) . . . . ?
N1 C1 C6 C5 179.14(12) . . . . ?
C2 C1 C6 C5 -3.52(18) . . . . ?
N1 C1 C6 C8 -3.2(2) . . . . ?
C2 C1 C6 C8 174.16(12) . . . . ?
C14 N2 C10 C11 -1.04(19) . . . . ?
Be1 N2 C10 C11 173.13(12) . . . . ?
N2 C10 C11 C12 0.4(2) . . . . ?
C10 C11 C12 C13 0.1(2) . . . . ?
C11 C12 C13 C14 0.1(2) . . . . ?
C10 N2 C14 C13 1.29(18) . . . . ?
Be1 N2 C14 C13 -172.91(11) . . . . ?
C12 C13 C14 N2 -0.8(2) . . . . ?
C1 N1 Be1 N1 -9.47(14) . . . 2_556 ?
C1 N1 Be1 N2 117.99(18) . . . 2_556 ?
C1 N1 Be1 N2 -138.47(16) . . . . ?
C10 N2 Be1 N1 -56.71(15) . . . . ?
C14 N2 Be1 N1 117.24(11) . . . . ?
C10 N2 Be1 N1 160.96(11) . . . 2_556 ?
C14 N2 Be1 N1 -25.09(15) . . . 2_556 ?
C10 N2 Be1 N2 53.89(9) . . . 2_556 ?
C14 N2 Be1 N2 -132.16(11) . . . 2_556 ?

_refine_diff_density_max         0.242
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.036



# start Validation Reply Form
_vrf_PLAT420_LTH482              
;
PROBLEM: D-H Bond Without Acceptor  N1       --H1       .     Please Check
RESPONSE: Chemically plausible, no acceptor is expected.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_LTH501
_database_code_depnum_ccdc_archive 'CCDC 2373012'
loop_
_audit_author_name
_audit_author_address
'Sergei Ivlev'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2024-07-23 deposited with the CCDC.	2024-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C48 H56 Be2 N4'
_chemical_formula_sum            'C48 H56 Be2 N4'
_chemical_formula_weight         706.98

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      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                   9.4884(9)
_cell_length_b                   9.8022(7)
_cell_length_c                   22.2345(19)
_cell_angle_alpha                90
_cell_angle_beta                 99.949(7)
_cell_angle_gamma                90
_cell_volume                     2036.9(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    14748
_cell_measurement_theta_min      4.05
_cell_measurement_theta_max      76.08

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_F_000             760
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.150
_exptl_absorpt_coefficient_mu    0.499
_shelx_estimated_absorpt_T_min   0.916
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2189
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;

_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'

_diffrn_detector                 Pilatus300K
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_detector_area_resol_mean 5.81

_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_radiation_probe          x-ray
_diffrn_source_voltage           50
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.5 mm diameter'

_diffrn_ambient_temperature      100

_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 2890 frames, detector distance = 60 mm
;

_diffrn_reflns_number            24532
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_av_R_equivalents  0.0535
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         4.037
_diffrn_reflns_theta_max         76.128
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             4152
_reflns_number_gt                3226
_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       
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_cell_refinement       
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_reduction        
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image
processing, for the correction and scaling of reflection intensities and
for outlier rejection, version 1.90, Darmstadt 2020
;

_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_refine_special_details          
; Terminal C3H7 group refined disordered
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1090P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0035(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4152
_refine_ls_number_parameters     283
_refine_ls_number_restraints     69
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0518
_refine_ls_wR_factor_ref         0.1578
_refine_ls_wR_factor_gt          0.1488
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.061
_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
N2 N 0.60094(12) 0.45552(12) 0.54079(5) 0.0277(3) Uani 1 1 d . . . . .
N1 N 0.59528(13) 0.36769(12) 0.40829(5) 0.0300(3) Uani 1 1 d . . . . .
C7 C 0.71458(15) 0.28334(14) 0.40755(6) 0.0298(3) Uani 1 1 d . . . . .
C13 C 0.63594(15) 0.34278(14) 0.58248(6) 0.0285(3) Uani 1 1 d . . . . .
C1 C 0.50236(16) 0.38243(15) 0.35013(6) 0.0321(3) Uani 1 1 d . . . . .
C12 C 0.78662(16) 0.22506(14) 0.46181(7) 0.0328(3) Uani 1 1 d . . . . .
H12 H 0.750943 0.239227 0.498695 0.039 Uiso 1 1 calc R U . . .
C14 C 0.76858(16) 0.33989(15) 0.62228(6) 0.0318(3) Uani 1 1 d . . . . .
C18 C 0.53536(17) 0.23723(15) 0.58300(7) 0.0343(3) Uani 1 1 d . . . . .
C11 C 0.90873(17) 0.14724(16) 0.46272(7) 0.0374(4) Uani 1 1 d . . . . .
H11 H 0.956670 0.110501 0.500271 0.045 Uiso 1 1 calc R U . . .
C8 C 0.76847(17) 0.25595(16) 0.35377(7) 0.0354(3) Uani 1 1 d . . . . .
H8 H 0.721037 0.292143 0.316020 0.042 Uiso 1 1 calc R U . . .
C19 C 0.87089(15) 0.46129(16) 0.62624(6) 0.0332(3) Uani 1 1 d . . . . .
H19 H 0.811705 0.545779 0.625934 0.040 Uiso 1 1 calc R U . . .
C15 C 0.80072(17) 0.22596(17) 0.65962(7) 0.0389(4) Uani 1 1 d . . . . .
H15 H 0.890907 0.221113 0.685864 0.047 Uiso 1 1 calc R U . . .
C6 C 0.5054(2) 0.49887(17) 0.31450(7) 0.0412(4) Uani 1 1 d . . . . .
H6 H 0.572389 0.569226 0.327824 0.049 Uiso 1 1 calc R U . . .
C10 C 0.96201(17) 0.12223(16) 0.40932(8) 0.0400(4) Uani 1 1 d . . . . .
H10 H 1.045902 0.068949 0.410003 0.048 Uiso 1 1 calc R U . . .
C9 C 0.89028(17) 0.17658(17) 0.35515(8) 0.0393(4) Uani 1 1 d . . . . .
H9 H 0.924921 0.159312 0.318267 0.047 Uiso 1 1 calc R U . . .
C2 C 0.40569(18) 0.27966(17) 0.32937(7) 0.0403(4) Uani 1 1 d . . . . .
H2A H 0.403328 0.199022 0.352880 0.048 Uiso 1 1 calc R U . . .
C17 C 0.57293(18) 0.12623(16) 0.62215(7) 0.0396(4) Uani 1 1 d . . . . .
H17 H 0.506317 0.054189 0.622976 0.048 Uiso 1 1 calc R U . . .
C16 C 0.70453(19) 0.11961(17) 0.65944(7) 0.0422(4) Uani 1 1 d . . . . .
H16 H 0.729295 0.042468 0.684949 0.051 Uiso 1 1 calc R U . . .
C20 C 0.94938(17) 0.47043(17) 0.57110(7) 0.0390(4) Uani 1 1 d . . . . .
H20A H 1.010185 0.389855 0.570333 0.059 Uiso 1 1 calc R U . . .
H20B H 1.008778 0.552802 0.574662 0.059 Uiso 1 1 calc R U . . .
H20C H 0.879016 0.474448 0.533276 0.059 Uiso 1 1 calc R U . . .
C21 C 0.98158(18) 0.46379(19) 0.68512(8) 0.0445(4) Uani 1 1 d . . . . .
H21A H 0.932844 0.454689 0.720349 0.067 Uiso 1 1 calc R U . . .
H21B H 1.034022 0.550331 0.687884 0.067 Uiso 1 1 calc R U . . .
H21C H 1.048762 0.387944 0.684843 0.067 Uiso 1 1 calc R U . . .
C5 C 0.4115(2) 0.5129(2) 0.25983(8) 0.0503(5) Uani 1 1 d . . . . .
H5 H 0.414131 0.593105 0.236051 0.060 Uiso 1 1 calc R U . . .
C3 C 0.3118(2) 0.2943(2) 0.27401(8) 0.0522(5) Uani 1 1 d . . . . .
H3 H 0.245895 0.223561 0.259890 0.063 Uiso 1 1 calc R U . . .
C4 C 0.3146(2) 0.4117(2) 0.23970(8) 0.0549(5) Uani 1 1 d . . . . .
H4 H 0.249715 0.422315 0.202351 0.066 Uiso 1 1 calc R U . . .
Be1 Be 0.5470(2) 0.44358(19) 0.46372(8) 0.0289(4) Uani 1 1 d . . . . .
H2 H 0.678(2) 0.5168(18) 0.5476(8) 0.037(5) Uiso 1 1 d . . . . .
C22_1 C 0.3803(5) 0.2477(6) 0.5480(2) 0.0323(9) Uani 0.650(13) 1 d D U P A 1
H22_1 H 0.361000 0.346463 0.538734 0.039 Uiso 0.650(13) 1 calc R U P A 1
C23_1 C 0.3659(5) 0.1740(8) 0.48711(16) 0.0516(13) Uani 0.650(13) 1 d D U P A 1
H23A_1 H 0.278211 0.203974 0.460397 0.077 Uiso 0.650(13) 1 calc R U P A 1
H23B_1 H 0.361321 0.075350 0.493814 0.077 Uiso 0.650(13) 1 calc R U P A 1
H23C_1 H 0.448758 0.194969 0.467876 0.077 Uiso 0.650(13) 1 calc R U P A 1
C24_1 C 0.2640(5) 0.1976(5) 0.5824(2) 0.0354(9) Uani 0.650(13) 1 d D U P A 1
H24A_1 H 0.169667 0.214378 0.557690 0.053 Uiso 0.650(13) 1 calc R U P A 1
H24B_1 H 0.271680 0.246605 0.621247 0.053 Uiso 0.650(13) 1 calc R U P A 1
H24C_1 H 0.276106 0.099552 0.590362 0.053 Uiso 0.650(13) 1 calc R U P A 1
C22_2 C 0.4044(10) 0.2286(10) 0.5339(5) 0.0329(16) Uani 0.350(13) 1 d D U P A 2
H2_2 H 0.398997 0.314671 0.509453 0.040 Uiso 0.350(13) 1 calc R U P A 2
C23_2 C 0.3957(8) 0.1104(10) 0.4900(3) 0.0404(15) Uani 0.350(13) 1 d D U P A 2
H3A_2 H 0.308333 0.118233 0.459479 0.061 Uiso 0.350(13) 1 calc R U P A 2
H3B_2 H 0.393863 0.024615 0.512525 0.061 Uiso 0.350(13) 1 calc R U P A 2
H3C_2 H 0.479325 0.111525 0.469612 0.061 Uiso 0.350(13) 1 calc R U P A 2
C24_2 C 0.2801(12) 0.2285(16) 0.5682(6) 0.064(3) Uani 0.350(13) 1 d D U P A 2
H1A_2 H 0.190312 0.238576 0.539259 0.096 Uiso 0.350(13) 1 calc R U P A 2
H1B_2 H 0.290467 0.304556 0.597261 0.096 Uiso 0.350(13) 1 calc R U P A 2
H1C_2 H 0.278826 0.142237 0.590421 0.096 Uiso 0.350(13) 1 calc R U P A 2


_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
N2 C13 1.4439(17) . ?
N2 Be1 1.705(2) . ?
N2 Be1 1.706(2) 3_666 ?
N2 H2 0.935(19) . ?
N1 C7 1.4042(18) . ?
N1 C1 1.4411(17) . ?
N1 Be1 1.574(2) . ?
C7 C12 1.401(2) . ?
C7 C8 1.405(2) . ?
C13 C14 1.4082(19) . ?
C13 C18 1.409(2) . ?
C1 C2 1.387(2) . ?
C1 C6 1.392(2) . ?
C12 C11 1.384(2) . ?
C12 H12 0.9500 . ?
C14 C15 1.393(2) . ?
C14 C19 1.529(2) . ?
C18 C17 1.400(2) . ?
C18 C22_2 1.508(10) . ?
C18 C22_1 1.545(5) . ?
C11 C10 1.390(2) . ?
C11 H11 0.9500 . ?
C8 C9 1.389(2) . ?
C8 H8 0.9500 . ?
C19 C21 1.531(2) . ?
C19 C20 1.543(2) . ?
C19 H19 1.0000 . ?
C15 C16 1.385(2) . ?
C15 H15 0.9500 . ?
C6 C5 1.384(2) . ?
C6 H6 0.9500 . ?
C10 C9 1.383(2) . ?
C10 H10 0.9500 . ?
C9 H9 0.9500 . ?
C2 C3 1.397(2) . ?
C2 H2A 0.9500 . ?
C17 C16 1.376(2) . ?
C17 H17 0.9500 . ?
C16 H16 0.9500 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C5 C4 1.374(3) . ?
C5 H5 0.9500 . ?
C3 C4 1.383(3) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
Be1 Be1 2.263(4) 3_666 ?
C22_1 C23_1 1.520(5) . ?
C22_1 C24_1 1.528(4) . ?
C22_1 H22_1 1.0000 . ?
C23_1 H23A_1 0.9800 . ?
C23_1 H23B_1 0.9800 . ?
C23_1 H23C_1 0.9800 . ?
C24_1 H24A_1 0.9800 . ?
C24_1 H24B_1 0.9800 . ?
C24_1 H24C_1 0.9800 . ?
C22_2 C23_2 1.508(8) . ?
C22_2 C24_2 1.511(8) . ?
C22_2 H2_2 1.0000 . ?
C23_2 H3A_2 0.9800 . ?
C23_2 H3B_2 0.9800 . ?
C23_2 H3C_2 0.9800 . ?
C24_2 H1A_2 0.9800 . ?
C24_2 H1B_2 0.9800 . ?
C24_2 H1C_2 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
C13 N2 Be1 126.04(11) . . ?
C13 N2 Be1 125.24(11) . 3_666 ?
Be1 N2 Be1 83.10(10) . 3_666 ?
C13 N2 H2 107.6(11) . . ?
Be1 N2 H2 107.2(11) . . ?
Be1 N2 H2 104.2(11) 3_666 . ?
C7 N1 C1 114.70(11) . . ?
C7 N1 Be1 129.18(12) . . ?
C1 N1 Be1 116.09(12) . . ?
C12 C7 N1 120.27(12) . . ?
C12 C7 C8 117.36(14) . . ?
N1 C7 C8 122.36(13) . . ?
C14 C13 C18 120.88(13) . . ?
C14 C13 N2 120.02(13) . . ?
C18 C13 N2 119.10(12) . . ?
C2 C1 C6 118.92(14) . . ?
C2 C1 N1 119.53(13) . . ?
C6 C1 N1 121.55(14) . . ?
C11 C12 C7 121.31(14) . . ?
C11 C12 H12 119.3 . . ?
C7 C12 H12 119.3 . . ?
C15 C14 C13 118.05(14) . . ?
C15 C14 C19 121.21(13) . . ?
C13 C14 C19 120.68(13) . . ?
C17 C18 C13 118.40(14) . . ?
C17 C18 C22_2 119.7(4) . . ?
C13 C18 C22_2 120.7(4) . . ?
C17 C18 C22_1 118.9(2) . . ?
C13 C18 C22_1 122.3(2) . . ?
C12 C11 C10 120.76(15) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C9 C8 C7 120.79(15) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C14 C19 C21 113.38(12) . . ?
C14 C19 C20 112.85(12) . . ?
C21 C19 C20 108.94(13) . . ?
C14 C19 H19 107.1 . . ?
C21 C19 H19 107.1 . . ?
C20 C19 H19 107.1 . . ?
C16 C15 C14 121.68(15) . . ?
C16 C15 H15 119.2 . . ?
C14 C15 H15 119.2 . . ?
C5 C6 C1 120.52(17) . . ?
C5 C6 H6 119.7 . . ?
C1 C6 H6 119.7 . . ?
C9 C10 C11 118.60(14) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C10 C9 C8 121.14(14) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
C1 C2 C3 120.21(16) . . ?
C1 C2 H2A 119.9 . . ?
C3 C2 H2A 119.9 . . ?
C16 C17 C18 121.22(15) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C17 C16 C15 119.68(14) . . ?
C17 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C4 C5 C6 120.48(17) . . ?
C4 C5 H5 119.8 . . ?
C6 C5 H5 119.8 . . ?
C4 C3 C2 120.10(18) . . ?
C4 C3 H3 120.0 . . ?
C2 C3 H3 120.0 . . ?
C5 C4 C3 119.76(16) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.1 . . ?
N1 Be1 N2 137.89(14) . . ?
N1 Be1 N2 125.15(12) . 3_666 ?
N2 Be1 N2 96.90(10) . 3_666 ?
N1 Be1 Be1 173.37(17) . 3_666 ?
N2 Be1 Be1 48.46(8) . 3_666 ?
N2 Be1 Be1 48.44(8) 3_666 3_666 ?
C23_1 C22_1 C24_1 109.4(4) . . ?
C23_1 C22_1 C18 110.4(3) . . ?
C24_1 C22_1 C18 115.7(4) . . ?
C23_1 C22_1 H22_1 107.0 . . ?
C24_1 C22_1 H22_1 107.0 . . ?
C18 C22_1 H22_1 107.0 . . ?
C22_1 C23_1 H23A_1 109.5 . . ?
C22_1 C23_1 H23B_1 109.5 . . ?
H23A_1 C23_1 H23B_1 109.5 . . ?
C22_1 C23_1 H23C_1 109.5 . . ?
H23A_1 C23_1 H23C_1 109.5 . . ?
H23B_1 C23_1 H23C_1 109.5 . . ?
C22_1 C24_1 H24A_1 109.5 . . ?
C22_1 C24_1 H24B_1 109.5 . . ?
H24A_1 C24_1 H24B_1 109.5 . . ?
C22_1 C24_1 H24C_1 109.5 . . ?
H24A_1 C24_1 H24C_1 109.5 . . ?
H24B_1 C24_1 H24C_1 109.5 . . ?
C23_2 C22_2 C18 117.2(6) . . ?
C23_2 C22_2 C24_2 111.5(8) . . ?
C18 C22_2 C24_2 104.6(7) . . ?
C23_2 C22_2 H2_2 107.7 . . ?
C18 C22_2 H2_2 107.7 . . ?
C24_2 C22_2 H2_2 107.7 . . ?
C22_2 C23_2 H3A_2 109.5 . . ?
C22_2 C23_2 H3B_2 109.5 . . ?
H3A_2 C23_2 H3B_2 109.5 . . ?
C22_2 C23_2 H3C_2 109.5 . . ?
H3A_2 C23_2 H3C_2 109.5 . . ?
H3B_2 C23_2 H3C_2 109.5 . . ?
C22_2 C24_2 H1A_2 109.5 . . ?
C22_2 C24_2 H1B_2 109.5 . . ?
H1A_2 C24_2 H1B_2 109.5 . . ?
C22_2 C24_2 H1C_2 109.5 . . ?
H1A_2 C24_2 H1C_2 109.5 . . ?
H1B_2 C24_2 H1C_2 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 N1 C7 C12 -159.41(13) . . . . ?
Be1 N1 C7 C12 18.4(2) . . . . ?
C1 N1 C7 C8 21.91(19) . . . . ?
Be1 N1 C7 C8 -160.29(15) . . . . ?
Be1 N2 C13 C14 126.45(15) . . . . ?
Be1 N2 C13 C14 -124.15(15) 3_666 . . . ?
Be1 N2 C13 C18 -54.09(19) . . . . ?
Be1 N2 C13 C18 55.31(18) 3_666 . . . ?
C7 N1 C1 C2 79.11(17) . . . . ?
Be1 N1 C1 C2 -98.99(17) . . . . ?
C7 N1 C1 C6 -102.03(16) . . . . ?
Be1 N1 C1 C6 79.87(18) . . . . ?
N1 C7 C12 C11 -176.69(13) . . . . ?
C8 C7 C12 C11 2.1(2) . . . . ?
C18 C13 C14 C15 3.6(2) . . . . ?
N2 C13 C14 C15 -176.92(13) . . . . ?
C18 C13 C14 C19 -173.67(13) . . . . ?
N2 C13 C14 C19 5.8(2) . . . . ?
C14 C13 C18 C17 -2.8(2) . . . . ?
N2 C13 C18 C17 177.76(13) . . . . ?
C14 C13 C18 C22_2 -170.1(4) . . . . ?
N2 C13 C18 C22_2 10.4(5) . . . . ?
C14 C13 C18 C22_1 169.8(3) . . . . ?
N2 C13 C18 C22_1 -9.7(3) . . . . ?
C7 C12 C11 C10 -1.3(2) . . . . ?
C12 C7 C8 C9 -1.4(2) . . . . ?
N1 C7 C8 C9 177.32(14) . . . . ?
C15 C14 C19 C21 -17.3(2) . . . . ?
C13 C14 C19 C21 159.92(14) . . . . ?
C15 C14 C19 C20 107.17(16) . . . . ?
C13 C14 C19 C20 -75.61(17) . . . . ?
C13 C14 C15 C16 -1.9(2) . . . . ?
C19 C14 C15 C16 175.43(15) . . . . ?
C2 C1 C6 C5 1.2(2) . . . . ?
N1 C1 C6 C5 -177.63(15) . . . . ?
C12 C11 C10 C9 -0.1(2) . . . . ?
C11 C10 C9 C8 0.8(2) . . . . ?
C7 C8 C9 C10 0.0(2) . . . . ?
C6 C1 C2 C3 -0.9(2) . . . . ?
N1 C1 C2 C3 177.96(15) . . . . ?
C13 C18 C17 C16 0.1(2) . . . . ?
C22_2 C18 C17 C16 167.5(5) . . . . ?
C22_1 C18 C17 C16 -172.7(3) . . . . ?
C18 C17 C16 C15 1.7(3) . . . . ?
C14 C15 C16 C17 -0.8(3) . . . . ?
C1 C6 C5 C4 -0.4(3) . . . . ?
C1 C2 C3 C4 -0.2(3) . . . . ?
C6 C5 C4 C3 -0.7(3) . . . . ?
C2 C3 C4 C5 1.0(3) . . . . ?
C7 N1 Be1 N2 -3.4(3) . . . . ?
C1 N1 Be1 N2 174.40(16) . . . . ?
C7 N1 Be1 N2 179.87(13) . . . 3_666 ?
C1 N1 Be1 N2 -2.4(2) . . . 3_666 ?
C13 N2 Be1 N1 -48.2(3) . . . . ?
Be1 N2 Be1 N1 -177.3(3) 3_666 . . . ?
C13 N2 Be1 N2 129.11(14) . . . 3_666 ?
Be1 N2 Be1 N2 0.000(2) 3_666 . . 3_666 ?
C13 N2 Be1 Be1 129.11(14) . . . 3_666 ?
C17 C18 C22_1 C23_1 -89.3(5) . . . . ?
C13 C18 C22_1 C23_1 98.2(4) . . . . ?
C17 C18 C22_1 C24_1 35.5(5) . . . . ?
C13 C18 C22_1 C24_1 -137.0(4) . . . . ?
C17 C18 C22_2 C23_2 -55.1(10) . . . . ?
C13 C18 C22_2 C23_2 112.1(7) . . . . ?
C17 C18 C22_2 C24_2 68.9(10) . . . . ?
C13 C18 C22_2 C24_2 -124.0(8) . . . . ?

_refine_diff_density_max         0.288
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.055



# start Validation Reply Form
_vrf_PLAT414_LTH501              
;
PROBLEM: Short Intra D-H..H-X       H2       ..H19      .       1.99 Ang.
RESPONSE: Position of H19 atom was calculated using the riding model approach
which may lead to a slightly suboptimal results.
;
_vrf_PLAT420_LTH501              
;
PROBLEM: D-H Bond Without Acceptor  N2       --H2       .     Please Check
RESPONSE: Chemically plausible. No acceptor is expected.
;
_vrf_PLAT911_LTH501              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         23 Report
RESPONSE: A few reflections could not be collected using the selected
measurement strategy and the instrument.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_LTH516
_database_code_depnum_ccdc_archive 'CCDC 2373011'
loop_
_audit_author_name
_audit_author_address
'Sergei Ivlev'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2024-07-23 deposited with the CCDC.	2024-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C48 H72 Be2 N4'
_chemical_formula_sum            'C48 H72 Be2 N4'
_chemical_formula_weight         723.11

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      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                   9.5804(3)
_cell_length_b                   16.0927(5)
_cell_length_c                   14.6676(5)
_cell_angle_alpha                90
_cell_angle_beta                 102.993(2)
_cell_angle_gamma                90
_cell_volume                     2203.47(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    9809
_cell_measurement_theta_min      4.1370
_cell_measurement_theta_max      74.4251

_exptl_crystal_description       needle
_exptl_crystal_colour            colorless
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.090
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.221
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.053
_exptl_absorpt_coefficient_mu    0.462
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.976
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8868
_exptl_absorpt_correction_T_max  0.9967
_exptl_absorpt_process_details   
;  SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
 --------------------------------------------------------------------------

 Reference: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10.
;

_diffrn_ambient_temperature      100
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus X-ray tube'
_diffrn_measurement_device_type  'Bruker D8 VENTURE'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_detector                 'PHOTON III C14'
_diffrn_source_voltage           50.0
_diffrn_source_current           1.10
_diffrn_source_power             0.055
_diffrn_radiation_collimation    '0.8 mm diameter'

_diffrn_reflns_number            68071
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         4.137
_diffrn_reflns_theta_max         74.576
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4499
_reflns_number_gt                4060
_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       'APEX5 v2023.9-2 (Bruker AXS, 2023)'
_computing_cell_refinement       'APEX5 v2023.9-2 (Bruker AXS, 2023)'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_computing_molecular_graphics    'Diamond v4.6.8 (Brandenburg, 2022)'
_computing_publication_material  'XCIF v2014/2 (Bruker AXS, 2014)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0516P)²+0.5994P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4499
_refine_ls_number_parameters     258
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.0978
_refine_ls_wR_factor_gt          0.0946
_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
C4 C 0.00255(12) 0.33235(7) 0.15184(8) 0.0254(2) Uani 1 1 d . . . . .
H4 H -0.073473 0.304522 0.110324 0.030 Uiso 1 1 calc R U . . .
C5 C 0.03466(11) 0.31381(6) 0.24659(7) 0.0222(2) Uani 1 1 d . . . . .
H5 H -0.019876 0.272705 0.269502 0.027 Uiso 1 1 calc R U . . .
C6 C 0.14522(10) 0.35414(6) 0.30900(7) 0.01624(19) Uani 1 1 d . . . . .
C7 C 0.27529(11) 0.50175(7) 0.13850(7) 0.0215(2) Uani 1 1 d . . . . .
H7 H 0.376720 0.500736 0.175294 0.026 Uiso 1 1 calc R U . . .
C8 C 0.21265(15) 0.58691(7) 0.15443(9) 0.0342(3) Uani 1 1 d . . . . .
H8A H 0.271593 0.630858 0.136035 0.051 Uiso 1 1 calc R U . . .
H8B H 0.211809 0.593141 0.220765 0.051 Uiso 1 1 calc R U . . .
H8C H 0.114570 0.591092 0.116657 0.051 Uiso 1 1 calc R U . . .
C9 C 0.27855(13) 0.49051(8) 0.03523(8) 0.0309(3) Uani 1 1 d . . . . .
H9A H 0.181930 0.498330 -0.003638 0.046 Uiso 1 1 calc R U . . .
H9B H 0.312344 0.434430 0.025506 0.046 Uiso 1 1 calc R U . . .
H9C H 0.343454 0.531582 0.017801 0.046 Uiso 1 1 calc R U . . .
C10 C 0.17028(10) 0.33737(6) 0.41319(7) 0.0175(2) Uani 1 1 d . . . . .
H10 H 0.273352 0.349258 0.441538 0.021 Uiso 1 1 calc R U . . .
C11 C 0.08000(11) 0.39782(7) 0.45658(7) 0.0231(2) Uani 1 1 d . . . . .
H11A H 0.105663 0.455061 0.444446 0.035 Uiso 1 1 calc R U . . .
H11B H 0.098388 0.388442 0.524251 0.035 Uiso 1 1 calc R U . . .
H11C H -0.021796 0.388617 0.428797 0.035 Uiso 1 1 calc R U . . .
C12 C 0.13953(14) 0.24841(7) 0.43943(8) 0.0292(2) Uani 1 1 d . . . . .
H12A H 0.036453 0.237527 0.420099 0.044 Uiso 1 1 calc R U . . .
H12B H 0.171080 0.241233 0.507295 0.044 Uiso 1 1 calc R U . . .
H12C H 0.191349 0.209422 0.407706 0.044 Uiso 1 1 calc R U . . .
C13 C 0.41900(9) 0.40054(6) 0.61231(6) 0.01362(18) Uani 1 1 d . . . . .
C14 C 0.50247(10) 0.33005(6) 0.60426(6) 0.01650(19) Uani 1 1 d . . . . .
C15 C 0.50598(11) 0.26443(6) 0.66695(7) 0.0210(2) Uani 1 1 d . . . . .
H15 H 0.563287 0.217078 0.662492 0.025 Uiso 1 1 calc R U . . .
C16 C 0.42779(12) 0.26699(7) 0.73531(7) 0.0243(2) Uani 1 1 d . . . . .
H16 H 0.431325 0.221883 0.777559 0.029 Uiso 1 1 calc R U . . .
C17 C 0.34401(11) 0.33611(7) 0.74167(7) 0.0230(2) Uani 1 1 d . . . . .
H17 H 0.289613 0.337353 0.788401 0.028 Uiso 1 1 calc R U . . .
C18 C 0.33722(10) 0.40388(6) 0.68147(6) 0.01648(19) Uani 1 1 d . . . . .
C19 C 0.58997(11) 0.32311(6) 0.53000(7) 0.0211(2) Uani 1 1 d . . . . .
H19 H 0.547153 0.362381 0.478453 0.025 Uiso 1 1 calc R U . . .
C20 C 0.74559(12) 0.35007(7) 0.56809(9) 0.0292(2) Uani 1 1 d . . . . .
H20A H 0.798381 0.346272 0.518241 0.044 Uiso 1 1 calc R U . . .
H20B H 0.790318 0.313623 0.619988 0.044 Uiso 1 1 calc R U . . .
H20C H 0.747587 0.407555 0.590396 0.044 Uiso 1 1 calc R U . . .
C21 C 0.58507(14) 0.23625(7) 0.48704(8) 0.0316(3) Uani 1 1 d . . . . .
H21A H 0.485214 0.218113 0.466963 0.047 Uiso 1 1 calc R U . . .
H21B H 0.637667 0.197296 0.533715 0.047 Uiso 1 1 calc R U . . .
H21C H 0.629193 0.237681 0.432912 0.047 Uiso 1 1 calc R U . . .
C22 C 0.23975(10) 0.47746(6) 0.69012(7) 0.0196(2) Uani 1 1 d . . . . .
H22 H 0.199273 0.498222 0.625304 0.023 Uiso 1 1 calc R U . . .
C23 C 0.32098(12) 0.55009(7) 0.74575(9) 0.0312(3) Uani 1 1 d . . . . .
H23A H 0.396619 0.568971 0.715415 0.047 Uiso 1 1 calc R U . . .
H23B H 0.363873 0.531794 0.809632 0.047 Uiso 1 1 calc R U . . .
H23C H 0.254354 0.595907 0.747746 0.047 Uiso 1 1 calc R U . . .
C24 C 0.11247(12) 0.45349(8) 0.73221(8) 0.0276(2) Uani 1 1 d . . . . .
H24A H 0.045685 0.500338 0.726336 0.041 Uiso 1 1 calc R U . . .
H24B H 0.147204 0.439503 0.798470 0.041 Uiso 1 1 calc R U . . .
H24C H 0.063252 0.405323 0.698717 0.041 Uiso 1 1 calc R U . . .
Be1 Be 0.42884(13) 0.46991(7) 0.43622(8) 0.0151(2) Uani 1 1 d . . . . .
N1 N 0.34073(9) 0.45598(5) 0.33448(6) 0.01639(17) Uani 1 1 d . . . . .
H1 H 0.3809(15) 0.4884(9) 0.3015(10) 0.025 Uiso 1 1 d . U . . .
C1 C 0.22748(10) 0.41497(6) 0.27497(6) 0.01462(19) Uani 1 1 d . . . . .
N2 N 0.41808(8) 0.46941(5) 0.54951(5) 0.01353(16) Uani 1 1 d . . . . .
H2 H 0.3439(14) 0.5025(8) 0.5540(9) 0.020 Uiso 1 1 d . U . . .
C2 C 0.19481(10) 0.43356(6) 0.17743(7) 0.01648(19) Uani 1 1 d . . . . .
C3 C 0.08285(11) 0.39207(6) 0.11846(7) 0.0209(2) Uani 1 1 d . . . . .
H3 H 0.060659 0.404896 0.053580 0.025 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
C4 C5 1.3866(15) . ?
C4 C3 1.3872(15) . ?
C5 C6 1.3947(14) . ?
C6 C1 1.4161(13) . ?
C6 C10 1.5168(13) . ?
C7 C2 1.5240(13) . ?
C7 C9 1.5327(14) . ?
C7 C8 1.5348(16) . ?
C10 C12 1.5282(13) . ?
C10 C11 1.5319(13) . ?
C13 C14 1.4081(13) . ?
C13 C18 1.4153(13) . ?
C13 N2 1.4399(11) . ?
C14 C15 1.3956(13) . ?
C14 C19 1.5206(13) . ?
C15 C16 1.3806(15) . ?
C16 C17 1.3870(15) . ?
C17 C18 1.3955(14) . ?
C18 C22 1.5308(13) . ?
C19 C21 1.5297(14) . ?
C19 C20 1.5325(15) . ?
C22 C23 1.5336(15) . ?
C22 C24 1.5348(14) . ?
Be1 N1 1.5567(14) . ?
Be1 N2 1.6879(14) . ?
Be1 N2 1.7350(14) 3_666 ?
Be1 Be1 2.269(2) 3_666 ?
N1 C1 1.3960(12) . ?
C1 C2 1.4258(13) . ?
C2 C3 1.3883(14) . ?

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
C5 C4 C3 119.15(9) . . ?
C4 C5 C6 121.49(9) . . ?
C5 C6 C1 119.40(9) . . ?
C5 C6 C10 120.22(9) . . ?
C1 C6 C10 120.23(8) . . ?
C2 C7 C9 114.19(9) . . ?
C2 C7 C8 109.74(9) . . ?
C9 C7 C8 110.57(9) . . ?
C6 C10 C12 115.12(8) . . ?
C6 C10 C11 109.23(8) . . ?
C12 C10 C11 109.36(8) . . ?
C14 C13 C18 120.47(8) . . ?
C14 C13 N2 119.24(8) . . ?
C18 C13 N2 120.30(8) . . ?
C15 C14 C13 118.97(9) . . ?
C15 C14 C19 118.74(8) . . ?
C13 C14 C19 122.29(8) . . ?
C16 C15 C14 121.29(9) . . ?
C15 C16 C17 119.30(9) . . ?
C16 C17 C18 121.98(9) . . ?
C17 C18 C13 117.98(9) . . ?
C17 C18 C22 119.64(9) . . ?
C13 C18 C22 122.35(8) . . ?
C14 C19 C21 113.05(9) . . ?
C14 C19 C20 111.46(8) . . ?
C21 C19 C20 110.25(9) . . ?
C18 C22 C23 112.80(8) . . ?
C18 C22 C24 113.18(9) . . ?
C23 C22 C24 109.36(9) . . ?
N1 Be1 N2 143.43(9) . . ?
N1 Be1 N2 117.26(8) . 3_666 ?
N2 Be1 N2 96.95(7) . 3_666 ?
N1 Be1 Be1 161.36(11) . 3_666 ?
N2 Be1 Be1 49.37(5) . 3_666 ?
N2 Be1 Be1 47.59(5) 3_666 3_666 ?
C1 N1 Be1 147.69(8) . . ?
N1 C1 C6 121.49(8) . . ?
N1 C1 C2 119.51(8) . . ?
C6 C1 C2 118.99(8) . . ?
C13 N2 Be1 129.83(7) . . ?
C13 N2 Be1 118.20(7) . 3_666 ?
Be1 N2 Be1 83.05(7) . 3_666 ?
C3 C2 C1 119.26(9) . . ?
C3 C2 C7 119.87(9) . . ?
C1 C2 C7 120.77(8) . . ?
C4 C3 C2 121.69(9) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C3 C4 C5 C6 0.36(16) . . . . ?
C4 C5 C6 C1 -0.50(15) . . . . ?
C4 C5 C6 C10 175.22(10) . . . . ?
C5 C6 C10 C12 34.43(13) . . . . ?
C1 C6 C10 C12 -149.88(9) . . . . ?
C5 C6 C10 C11 -89.02(11) . . . . ?
C1 C6 C10 C11 86.67(10) . . . . ?
C18 C13 C14 C15 -1.53(13) . . . . ?
N2 C13 C14 C15 178.29(8) . . . . ?
C18 C13 C14 C19 178.93(8) . . . . ?
N2 C13 C14 C19 -1.26(13) . . . . ?
C13 C14 C15 C16 0.99(15) . . . . ?
C19 C14 C15 C16 -179.45(9) . . . . ?
C14 C15 C16 C17 0.09(16) . . . . ?
C15 C16 C17 C18 -0.64(16) . . . . ?
C16 C17 C18 C13 0.10(15) . . . . ?
C16 C17 C18 C22 178.37(9) . . . . ?
C14 C13 C18 C17 0.99(13) . . . . ?
N2 C13 C18 C17 -178.82(8) . . . . ?
C14 C13 C18 C22 -177.22(8) . . . . ?
N2 C13 C18 C22 2.96(13) . . . . ?
C15 C14 C19 C21 40.42(13) . . . . ?
C13 C14 C19 C21 -140.04(9) . . . . ?
C15 C14 C19 C20 -84.43(11) . . . . ?
C13 C14 C19 C20 95.12(11) . . . . ?
C17 C18 C22 C23 98.72(11) . . . . ?
C13 C18 C22 C23 -83.10(11) . . . . ?
C17 C18 C22 C24 -26.12(13) . . . . ?
C13 C18 C22 C24 152.07(9) . . . . ?
N2 Be1 N1 C1 -29.8(3) . . . . ?
N2 Be1 N1 C1 172.81(12) 3_666 . . . ?
Be1 Be1 N1 C1 -155.0(3) 3_666 . . . ?
Be1 N1 C1 C6 -3.4(2) . . . . ?
Be1 N1 C1 C2 177.60(13) . . . . ?
C5 C6 C1 N1 -178.90(9) . . . . ?
C10 C6 C1 N1 5.37(13) . . . . ?
C5 C6 C1 C2 0.11(13) . . . . ?
C10 C6 C1 C2 -175.61(8) . . . . ?
C14 C13 N2 Be1 34.37(13) . . . . ?
C18 C13 N2 Be1 -145.81(9) . . . . ?
C14 C13 N2 Be1 -71.19(11) . . . 3_666 ?
C18 C13 N2 Be1 108.62(10) . . . 3_666 ?
N1 Be1 N2 C13 78.92(17) . . . . ?
N2 Be1 N2 C13 -121.21(10) 3_666 . . . ?
Be1 Be1 N2 C13 -121.21(10) 3_666 . . . ?
N1 Be1 N2 Be1 -159.87(18) . . . 3_666 ?
N2 Be1 N2 Be1 -0.001(1) 3_666 . . 3_666 ?
N1 C1 C2 C3 179.45(9) . . . . ?
C6 C1 C2 C3 0.41(13) . . . . ?
N1 C1 C2 C7 -4.21(13) . . . . ?
C6 C1 C2 C7 176.76(8) . . . . ?
C9 C7 C2 C3 -28.99(13) . . . . ?
C8 C7 C2 C3 95.79(11) . . . . ?
C9 C7 C2 C1 154.69(9) . . . . ?
C8 C7 C2 C1 -80.53(11) . . . . ?
C5 C4 C3 C2 0.19(16) . . . . ?
C1 C2 C3 C4 -0.57(15) . . . . ?
C7 C2 C3 C4 -176.95(10) . . . . ?

_refine_diff_density_max         0.282
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.035



# start Validation Reply Form
_vrf_PLAT414_LTH516              
;
PROBLEM: Short Intra D-H..H-X       H1       ..H7       .       1.85 Ang.
RESPONSE: One of the two H atoms was refined using the riding model which
may lead to shorter D-H..H-X distances.
;
_vrf_PLAT420_LTH516              
;
PROBLEM: D-H Bond Without Acceptor  N1       --H1       .     Please Check
RESPONSE: Chemically correct, no acceptor is expected.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_LTH473
_database_code_depnum_ccdc_archive 'CCDC 2373014'
loop_
_audit_author_name
_audit_author_address
'Sergei Ivlev'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2024-07-23 deposited with the CCDC.	2024-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C54 H72 Be3 N6, C6 H6'
_chemical_formula_sum            'C60 H78 Be3 N6'
_chemical_formula_weight         910.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Be Be 0.0038 0.0014 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   14.2365(15)
_cell_length_b                   14.6407(15)
_cell_length_c                   15.7210(18)
_cell_angle_alpha                63.743(8)
_cell_angle_beta                 71.969(9)
_cell_angle_gamma                72.777(8)
_cell_volume                     2745.2(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    20991
_cell_measurement_theta_min      2.95
_cell_measurement_theta_max      75.93

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.101
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.476
_shelx_estimated_absorpt_T_min   0.911
_shelx_estimated_absorpt_T_max   0.954
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.2940
_exptl_absorpt_correction_T_max  0.9137
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;

_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'

_diffrn_detector                 Pilatus300K
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_detector_area_resol_mean 5.81

_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_radiation_probe          x-ray
_diffrn_source_voltage           50
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.5 mm diameter'

_diffrn_ambient_temperature      100

_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 5283 frames, detector distance = 60 mm
;

_diffrn_reflns_number            67425
_diffrn_reflns_av_unetI/netI     0.0598
_diffrn_reflns_av_R_equivalents  0.0661
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.205
_diffrn_reflns_theta_max         76.230
_diffrn_reflns_theta_full        67.686
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             11226
_reflns_number_gt                6113
_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       
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_cell_refinement       
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_reduction        
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image
processing, for the correction and scaling of reflection intensities and
for outlier rejection, version 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'
_refine_special_details          
; Parts of molecule refined disordered
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0733P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.00201(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11226
_refine_ls_number_parameters     927
_refine_ls_number_restraints     2052
_refine_ls_R_factor_all          0.0942
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1377
_refine_ls_wR_factor_gt          0.1183
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_restrained_S_all      0.838
_refine_ls_shift/su_max          0.015
_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
N2B N 0.4718(3) 0.5068(2) 0.8264(3) 0.0420(9) Uani 0.456(2) 1 d D U P A 2
H2NB H 0.423(4) 0.554(4) 0.828(4) 0.063 Uiso 0.456(2) 1 d . U P A 2
N2A N 0.5655(2) 0.4381(2) 0.8230(2) 0.0399(7) Uani 0.544(2) 1 d D U P A 1
H2NA H 0.634(3) 0.400(3) 0.828(3) 0.060 Uiso 0.544(2) 1 d . U P A 1
N2 N 0.73983(11) 0.74484(11) 0.59053(12) 0.0395(3) Uani 1 1 d . U . . .
H2N H 0.6941(15) 0.7991(16) 0.6016(15) 0.059 Uiso 1 1 d . U . . .
N3A N 0.83002(19) 0.8604(2) 0.4080(2) 0.0439(6) Uani 0.644(2) 1 d D U P A 1
H3NA H 0.831(3) 0.883(3) 0.445(3) 0.066 Uiso 0.644(2) 1 d . U P A 1
N3B N 0.8049(3) 0.8153(4) 0.3596(3) 0.0463(12) Uani 0.356(2) 1 d D U P A 2
H3NB H 0.773(5) 0.794(5) 0.323(5) 0.069 Uiso 0.356(2) 1 d . U P A 2
N5 N 0.53993(12) 0.67172(13) 0.66956(12) 0.0444(4) Uani 1 1 d . U . . .
H5N H 0.5014(16) 0.6714(17) 0.6323(16) 0.067 Uiso 1 1 d . U . . .
N1 N 0.68648(13) 0.69712(12) 0.47678(13) 0.0491(4) Uani 1 1 d . U . . .
H1N H 0.7240(17) 0.6433(18) 0.4650(17) 0.074 Uiso 1 1 d . U . . .
N4 N 0.69580(15) 0.52855(12) 0.67570(14) 0.0560(5) Uani 1 1 d . U . . .
H4N H 0.7383(18) 0.5260(19) 0.7106(18) 0.084 Uiso 1 1 d . U . . .
C8 C 0.40048(16) 0.88335(17) 0.22551(16) 0.0587(6) Uani 1 1 d . . . . .
H8A H 0.358223 0.945074 0.236501 0.088 Uiso 1 1 calc R U . . .
H8B H 0.358249 0.833734 0.240941 0.088 Uiso 1 1 calc R U . . .
H8C H 0.435646 0.903280 0.157399 0.088 Uiso 1 1 calc R U . . .
C1 C 0.61605(14) 0.74253(14) 0.41271(14) 0.0414(4) Uani 1 1 d . . . . .
C9 C 0.68813(15) 0.59881(14) 0.34740(15) 0.0461(5) Uani 1 1 d . . . . .
H9A H 0.671878 0.575707 0.304761 0.069 Uiso 1 1 calc R U . . .
H9B H 0.684539 0.543934 0.412524 0.069 Uiso 1 1 calc R U . . .
H9C H 0.756219 0.614252 0.321622 0.069 Uiso 1 1 calc R U . . .
C10 C 0.82536(13) 0.72644(14) 0.63049(14) 0.0410(4) Uani 1 1 d . . . . .
C11 C 0.91316(14) 0.65806(15) 0.60951(15) 0.0452(5) Uani 1 1 d . . . . .
C12 C 0.99466(15) 0.64073(18) 0.64918(17) 0.0584(6) Uani 1 1 d . . . . .
H12 H 1.053342 0.593134 0.635979 0.070 Uiso 1 1 calc R U . . .
C13 C 0.99395(17) 0.6899(2) 0.70713(19) 0.0694(7) Uani 1 1 d . . . . .
C14 C 0.90791(17) 0.7603(2) 0.72309(17) 0.0662(7) Uani 1 1 d . . . . .
H14 H 0.905910 0.795742 0.761881 0.079 Uiso 1 1 calc R U . . .
C15 C 0.82445(15) 0.78142(16) 0.68497(15) 0.0495(5) Uani 1 1 d . . . . .
C16 C 0.92497(15) 0.60944(16) 0.53858(16) 0.0528(5) Uani 1 1 d . . . . .
H16A H 0.927760 0.663291 0.472983 0.079 Uiso 1 1 calc R U . . .
H16B H 0.867559 0.575944 0.556529 0.079 Uiso 1 1 calc R U . . .
H16C H 0.987240 0.557632 0.540326 0.079 Uiso 1 1 calc R U . . .
C17 C 1.0845(2) 0.6696(3) 0.7493(2) 0.1114(12) Uani 1 1 d . . . . .
H17A H 1.141288 0.626666 0.721656 0.167 Uiso 1 1 calc R U . . .
H17B H 1.067728 0.633250 0.819873 0.167 Uiso 1 1 calc R U . . .
H17C H 1.102637 0.735634 0.733449 0.167 Uiso 1 1 calc R U . . .
C18 C 0.73813(16) 0.86847(16) 0.69586(18) 0.0616(6) Uani 1 1 d . . . . .
H18A H 0.748992 0.894667 0.738970 0.092 Uiso 1 1 calc R U . . .
H18B H 0.674905 0.842318 0.723512 0.092 Uiso 1 1 calc R U . . .
H18C H 0.734716 0.924682 0.632127 0.092 Uiso 1 1 calc R U . . .
C19 C 0.73043(16) 0.44041(13) 0.64779(15) 0.0498(5) Uani 1 1 d . . . . .
C20 C 0.82030(16) 0.37098(14) 0.66878(15) 0.0476(5) Uani 1 1 d . . . . .
C21 C 0.85099(15) 0.28815(14) 0.63967(14) 0.0476(5) Uani 1 1 d . . . . .
H21 H 0.911837 0.241367 0.653893 0.057 Uiso 1 1 calc R U . . .
C22 C 0.79598(16) 0.27092(15) 0.59034(15) 0.0500(5) Uani 1 1 d . . . . .
C23 C 0.70555(16) 0.33827(14) 0.57443(15) 0.0503(5) Uani 1 1 d . . . . .
H23 H 0.665713 0.326907 0.542699 0.060 Uiso 1 1 calc R U . . .
C24 C 0.67090(16) 0.42156(13) 0.60299(15) 0.0490(5) Uani 1 1 d . . . . .
C25 C 0.87913(17) 0.37915(15) 0.72991(17) 0.0565(6) Uani 1 1 d . . . . .
H25A H 0.891855 0.449886 0.703043 0.085 Uiso 1 1 calc R U . . .
H25B H 0.943320 0.330264 0.729568 0.085 Uiso 1 1 calc R U . . .
H25C H 0.840252 0.362585 0.796629 0.085 Uiso 1 1 calc R U . . .
C26 C 0.83192(18) 0.18100(17) 0.55786(18) 0.0632(6) Uani 1 1 d . . . . .
H26A H 0.776467 0.170550 0.540648 0.095 Uiso 1 1 calc R U . . .
H26B H 0.855120 0.118038 0.610668 0.095 Uiso 1 1 calc R U . . .
H26C H 0.887460 0.196191 0.501229 0.095 Uiso 1 1 calc R U . . .
C27 C 0.56604(16) 0.48385(14) 0.59253(16) 0.0551(6) Uani 1 1 d . . . . .
H27A H 0.569869 0.556903 0.552545 0.083 Uiso 1 1 calc R U . . .
H27B H 0.524247 0.477501 0.656773 0.083 Uiso 1 1 calc R U . . .
H27C H 0.536235 0.457404 0.561499 0.083 Uiso 1 1 calc R U . . .
C28 C 0.48229(13) 0.74430(15) 0.71349(14) 0.0441(4) Uani 1 1 d . . . . .
C29 C 0.39181(14) 0.80801(16) 0.68602(15) 0.0518(5) Uani 1 1 d . . . . .
C30 C 0.34065(15) 0.88008(17) 0.72711(16) 0.0596(6) Uani 1 1 d . . . . .
H30 H 0.279755 0.922835 0.708511 0.072 Uiso 1 1 calc R U . . .
C31 C 0.37479(15) 0.89225(16) 0.79424(15) 0.0560(6) Uani 1 1 d . . . . .
C32 C 0.46149(14) 0.82467(15) 0.82437(14) 0.0506(5) Uani 1 1 d . . . . .
H32 H 0.484980 0.830088 0.872015 0.061 Uiso 1 1 calc R U . . .
C33 C 0.51447(13) 0.74963(14) 0.78662(14) 0.0437(4) Uani 1 1 d . . . . .
C34 C 0.34809(16) 0.79630(18) 0.61587(17) 0.0658(7) Uani 1 1 d . . . . .
H34A H 0.286293 0.847941 0.604767 0.099 Uiso 1 1 calc R U . . .
H34B H 0.332741 0.726580 0.643169 0.099 Uiso 1 1 calc R U . . .
H34C H 0.396907 0.806814 0.554219 0.099 Uiso 1 1 calc R U . . .
C35 C 0.31996(18) 0.97424(19) 0.83558(17) 0.0756(8) Uani 1 1 d . . . . .
H35A H 0.344491 1.039165 0.793485 0.113 Uiso 1 1 calc R U . . .
H35B H 0.332252 0.951046 0.900640 0.113 Uiso 1 1 calc R U . . .
H35C H 0.247651 0.985563 0.839364 0.113 Uiso 1 1 calc R U . . .
C36 C 0.60017(13) 0.67023(15) 0.83149(14) 0.0445(4) Uani 1 1 d . . . . .
H36A H 0.660198 0.667684 0.780350 0.067 Uiso 1 1 calc R U . . .
H36B H 0.581005 0.601847 0.865575 0.067 Uiso 1 1 calc R U . . .
H36C H 0.614627 0.689891 0.877517 0.067 Uiso 1 1 calc R U . . .
C2 C 0.55257(14) 0.83800(13) 0.40715(14) 0.0410(4) Uani 1 1 d . . . . .
C3 C 0.48376(14) 0.88063(13) 0.34687(13) 0.0415(4) Uani 1 1 d . . . . .
H3 H 0.439877 0.944382 0.344704 0.050 Uiso 1 1 calc R U . . .
C4 C 0.47659(14) 0.83391(14) 0.28980(14) 0.0427(4) Uani 1 1 d . . . . .
C5 C 0.54380(14) 0.74225(14) 0.29255(14) 0.0417(4) Uani 1 1 d . . . . .
H5 H 0.542295 0.710156 0.252170 0.050 Uiso 1 1 calc R U . . .
C6 C 0.61332(14) 0.69581(13) 0.35252(14) 0.0406(4) Uani 1 1 d . . . . .
C7 C 0.55987(15) 0.89888(13) 0.46028(14) 0.0435(4) Uani 1 1 d . . . . .
H7A H 0.626015 0.918874 0.436299 0.065 Uiso 1 1 calc R U . . .
H7B H 0.551048 0.856068 0.529876 0.065 Uiso 1 1 calc R U . . .
H7C H 0.507295 0.961293 0.449235 0.065 Uiso 1 1 calc R U . . .
Be1 Be 0.66527(18) 0.66060(17) 0.6032(2) 0.0403(5) Uani 1 1 d . . . . .
Be2A Be 0.7583(6) 0.7792(5) 0.4743(4) 0.0388(12) Uani 0.644(2) 1 d D U P A 1
Be2B Be 0.7586(13) 0.7580(10) 0.4669(8) 0.043(2) Uani 0.356(2) 1 d D U P A 2
Be3A Be 0.5889(6) 0.5401(6) 0.7370(7) 0.0454(15) Uani 0.544(2) 1 d D U P A 1
Be3B Be 0.5604(7) 0.5543(8) 0.7387(8) 0.0494(19) Uani 0.456(2) 1 d D U P A 2
C1_1 C 0.9162(3) 0.8557(3) 0.2488(3) 0.0383(9) Uani 0.644(2) 1 d D U P A 1
C2_1 C 0.9898(4) 0.8863(4) 0.1658(4) 0.0488(11) Uani 0.644(2) 1 d D U P A 1
H2_1 H 1.000524 0.859063 0.118099 0.059 Uiso 0.644(2) 1 calc R U P A 1
C3_1 C 1.0485(4) 0.9554(4) 0.1498(4) 0.0529(12) Uani 0.644(2) 1 d D U P A 1
C4_1 C 1.0300(3) 0.9943(3) 0.2202(4) 0.0513(10) Uani 0.644(2) 1 d D U P A 1
H4_1 H 1.069139 1.042034 0.210293 0.062 Uiso 0.644(2) 1 calc R U P A 1
C5_1 C 0.9560(3) 0.9667(3) 0.3057(3) 0.0414(8) Uani 0.644(2) 1 d D U P A 1
C6_1 C 0.8990(3) 0.8945(3) 0.3213(3) 0.0388(9) Uani 0.644(2) 1 d D U P A 1
C7_1 C 0.8575(2) 0.7785(2) 0.2624(2) 0.0472(8) Uani 0.644(2) 1 d D U P A 1
H7A_1 H 0.785684 0.808992 0.270022 0.071 Uiso 0.644(2) 1 calc R U P A 1
H7B_1 H 0.869162 0.716127 0.320390 0.071 Uiso 0.644(2) 1 calc R U P A 1
H7C_1 H 0.879394 0.760040 0.205520 0.071 Uiso 0.644(2) 1 calc R U P A 1
C8_1 C 1.1326(3) 0.9827(4) 0.0607(3) 0.0824(14) Uani 0.644(2) 1 d D U P A 1
H8A_1 H 1.126325 0.958283 0.014257 0.124 Uiso 0.644(2) 1 calc R U P A 1
H8B_1 H 1.197664 0.949430 0.079783 0.124 Uiso 0.644(2) 1 calc R U P A 1
H8C_1 H 1.128087 1.058072 0.030674 0.124 Uiso 0.644(2) 1 calc R U P A 1
C9_1 C 0.9406(2) 1.0105(2) 0.3805(2) 0.0508(8) Uani 0.644(2) 1 d D U P A 1
H9A_1 H 0.985515 1.059944 0.356885 0.076 Uiso 0.644(2) 1 calc R U P A 1
H9B_1 H 0.955706 0.954059 0.441047 0.076 Uiso 0.644(2) 1 calc R U P A 1
H9C_1 H 0.870649 1.045874 0.392215 0.076 Uiso 0.644(2) 1 calc R U P A 1
C1_2 C 0.9259(7) 0.8651(6) 0.2049(6) 0.0491(19) Uani 0.356(2) 1 d D U P A 2
C2_2 C 1.0017(7) 0.9198(6) 0.1453(7) 0.055(2) Uani 0.356(2) 1 d D U P A 2
H2_2 H 1.031327 0.915151 0.083949 0.066 Uiso 0.356(2) 1 calc R U P A 2
C3_2 C 1.0369(7) 0.9814(8) 0.1707(7) 0.060(2) Uani 0.356(2) 1 d D U P A 2
C4_2 C 0.9919(6) 0.9882(6) 0.2598(6) 0.0473(18) Uani 0.356(2) 1 d D U P A 2
H4_2 H 1.013615 1.031075 0.278154 0.057 Uiso 0.356(2) 1 calc R U P A 2
C5_2 C 0.9159(6) 0.9344(6) 0.3232(5) 0.0458(17) Uani 0.356(2) 1 d D U P A 2
C6_2 C 0.8827(5) 0.8724(6) 0.2958(5) 0.0421(15) Uani 0.356(2) 1 d D U P A 2
C7_2 C 0.8919(5) 0.7961(5) 0.1752(4) 0.0582(16) Uani 0.356(2) 1 d D U P A 2
H7A_2 H 0.822740 0.825149 0.165455 0.087 Uiso 0.356(2) 1 calc R U P A 2
H7B_2 H 0.894623 0.726319 0.226335 0.087 Uiso 0.356(2) 1 calc R U P A 2
H7C_2 H 0.936303 0.792410 0.114705 0.087 Uiso 0.356(2) 1 calc R U P A 2
C8_2 C 1.1244(5) 1.0347(7) 0.1047(6) 0.086(3) Uani 0.356(2) 1 d D U P A 2
H8A_2 H 1.123753 1.052575 0.037008 0.130 Uiso 0.356(2) 1 calc R U P A 2
H8B_2 H 1.187667 0.988032 0.120081 0.130 Uiso 0.356(2) 1 calc R U P A 2
H8C_2 H 1.118415 1.098026 0.114465 0.130 Uiso 0.356(2) 1 calc R U P A 2
C9_2 C 0.8705(4) 0.9433(5) 0.4204(4) 0.0500(14) Uani 0.356(2) 1 d D U P A 2
H9A_2 H 0.889436 1.002447 0.420323 0.075 Uiso 0.356(2) 1 calc R U P A 2
H9B_2 H 0.895515 0.879582 0.471580 0.075 Uiso 0.356(2) 1 calc R U P A 2
H9C_2 H 0.797102 0.953508 0.432351 0.075 Uiso 0.356(2) 1 calc R U P A 2
C1_3 C 0.3882(4) 0.4223(3) 0.8751(3) 0.0384(10) Uani 0.544(2) 1 d D U P A 1
C2_3 C 0.3160(3) 0.3599(4) 0.9232(3) 0.0427(9) Uani 0.544(2) 1 d D U P A 1
H2_3 H 0.247193 0.390945 0.923369 0.051 Uiso 0.544(2) 1 calc R U P A 1
C3_3 C 0.3418(4) 0.2525(4) 0.9715(4) 0.0461(10) Uani 0.544(2) 1 d D U P A 1
C4_3 C 0.4432(4) 0.2108(4) 0.9691(4) 0.0417(11) Uani 0.544(2) 1 d D U P A 1
H4_3 H 0.462600 0.137964 1.000597 0.050 Uiso 0.544(2) 1 calc R U P A 1
C5_3 C 0.5178(3) 0.2705(4) 0.9229(3) 0.0368(10) Uani 0.544(2) 1 d D U P A 1
C6_3 C 0.4901(4) 0.3787(4) 0.8740(3) 0.0338(9) Uani 0.544(2) 1 d D U P A 1
C7_3 C 0.3575(3) 0.5369(3) 0.8218(3) 0.0474(9) Uani 0.544(2) 1 d D U P A 1
H7A_3 H 0.382684 0.554860 0.751984 0.071 Uiso 0.544(2) 1 calc R U P A 1
H7B_3 H 0.385832 0.574540 0.843335 0.071 Uiso 0.544(2) 1 calc R U P A 1
H7C_3 H 0.284000 0.556167 0.835452 0.071 Uiso 0.544(2) 1 calc R U P A 1
C8_3 C 0.2614(3) 0.1862(3) 1.0213(3) 0.0670(13) Uani 0.544(2) 1 d D U P A 1
H8A_3 H 0.236542 0.180995 0.972292 0.100 Uiso 0.544(2) 1 calc R U P A 1
H8B_3 H 0.205744 0.217835 1.060705 0.100 Uiso 0.544(2) 1 calc R U P A 1
H8C_3 H 0.290062 0.116714 1.063019 0.100 Uiso 0.544(2) 1 calc R U P A 1
C9_3 C 0.6267(3) 0.2195(3) 0.9238(3) 0.0447(9) Uani 0.544(2) 1 d D U P A 1
H9A_3 H 0.665668 0.237578 0.857018 0.067 Uiso 0.544(2) 1 calc R U P A 1
H9B_3 H 0.632000 0.144073 0.955754 0.067 Uiso 0.544(2) 1 calc R U P A 1
H9C_3 H 0.653212 0.243666 0.959203 0.067 Uiso 0.544(2) 1 calc R U P A 1
C1_4 C 0.3433(4) 0.4009(4) 0.8853(4) 0.0391(11) Uani 0.456(2) 1 d D U P A 2
C2_4 C 0.3168(4) 0.3029(5) 0.9286(4) 0.0492(12) Uani 0.456(2) 1 d D U P A 2
H2_4 H 0.249668 0.297604 0.935725 0.059 Uiso 0.456(2) 1 calc R U P A 2
C3_4 C 0.3871(6) 0.2132(4) 0.9614(4) 0.0516(14) Uani 0.456(2) 1 d D U P A 2
C4_4 C 0.4841(5) 0.2241(5) 0.9518(4) 0.0445(14) Uani 0.456(2) 1 d D U P A 2
H4_4 H 0.532655 0.163792 0.975420 0.053 Uiso 0.456(2) 1 calc R U P A 2
C5_4 C 0.5116(4) 0.3196(5) 0.9092(4) 0.0368(12) Uani 0.456(2) 1 d D U P A 2
C6_4 C 0.4421(5) 0.4097(4) 0.8734(3) 0.0338(12) Uani 0.456(2) 1 d D U P A 2
C7_4 C 0.2665(3) 0.4972(3) 0.8445(3) 0.0502(11) Uani 0.456(2) 1 d D U P A 2
H7A_4 H 0.291968 0.533456 0.775128 0.075 Uiso 0.456(2) 1 calc R U P A 2
H7B_4 H 0.255050 0.543297 0.878281 0.075 Uiso 0.456(2) 1 calc R U P A 2
H7C_4 H 0.203141 0.477008 0.853994 0.075 Uiso 0.456(2) 1 calc R U P A 2
C8_4 C 0.3572(5) 0.1081(4) 1.0020(4) 0.0806(19) Uani 0.456(2) 1 d D U P A 2
H8A_4 H 0.320459 0.107041 0.959202 0.121 Uiso 0.456(2) 1 calc R U P A 2
H8B_4 H 0.314236 0.095508 1.066800 0.121 Uiso 0.456(2) 1 calc R U P A 2
H8C_4 H 0.417795 0.053942 1.006311 0.121 Uiso 0.456(2) 1 calc R U P A 2
C9_4 C 0.6178(3) 0.3233(4) 0.9063(4) 0.0531(12) Uani 0.456(2) 1 d D U P A 2
H9A_4 H 0.660092 0.327363 0.842734 0.080 Uiso 0.456(2) 1 calc R U P A 2
H9B_4 H 0.644744 0.260538 0.957015 0.080 Uiso 0.456(2) 1 calc R U P A 2
H9C_4 H 0.617188 0.384412 0.917189 0.080 Uiso 0.456(2) 1 calc R U P A 2
C1_5 C 0.1571(7) 0.5267(4) 1.0828(4) 0.0839(19) Uani 0.637(11) 1 d D U P B 1
H1_5 H 0.173313 0.455748 1.123432 0.101 Uiso 0.637(11) 1 calc R U P B 1
C2_5 C 0.0592(7) 0.5715(7) 1.0737(6) 0.109(3) Uani 0.637(11) 1 d D U P B 1
H2_5 H 0.007958 0.531324 1.109126 0.131 Uiso 0.637(11) 1 calc R U P B 1
C3_5 C 0.0347(7) 0.6730(7) 1.0145(7) 0.135(3) Uani 0.637(11) 1 d D U P B 1
H3_5 H -0.033315 0.703571 1.009556 0.162 Uiso 0.637(11) 1 calc R U P B 1
C4_5 C 0.1089(6) 0.7301(6) 0.9626(8) 0.095(3) Uani 0.637(11) 1 d D U P B 1
H4_5 H 0.091927 0.800583 0.921087 0.114 Uiso 0.637(11) 1 calc R U P B 1
C5_5 C 0.2084(7) 0.6871(6) 0.9693(9) 0.079(2) Uani 0.637(11) 1 d D U P B 1
H5_5 H 0.259827 0.726685 0.931113 0.094 Uiso 0.637(11) 1 calc R U P B 1
C6_5 C 0.2317(6) 0.5852(5) 1.0327(5) 0.088(2) Uani 0.637(11) 1 d D U P B 1
H6_5 H 0.298771 0.555722 1.041617 0.105 Uiso 0.637(11) 1 calc R U P B 1
C1_6 C 0.2046(11) 0.6793(11) 0.9643(15) 0.079(4) Uani 0.363(11) 1 d D U P B 2
H1_6 H 0.269398 0.697248 0.937696 0.095 Uiso 0.363(11) 1 calc R U P B 2
C2_6 C 0.1242(10) 0.7565(10) 0.9423(13) 0.081(3) Uani 0.363(11) 1 d D U P B 2
H2_6 H 0.131794 0.825651 0.900285 0.097 Uiso 0.363(11) 1 calc R U P B 2
C3_6 C 0.0318(9) 0.7294(11) 0.9839(11) 0.115(4) Uani 0.363(11) 1 d D U P B 2
H3_6 H -0.026954 0.779953 0.968943 0.138 Uiso 0.363(11) 1 calc R U P B 2
C4_6 C 0.0232(9) 0.6295(12) 1.0471(13) 0.112(5) Uani 0.363(11) 1 d D U P B 2
H4_6 H -0.042131 0.613658 1.077688 0.134 Uiso 0.363(11) 1 calc R U P B 2
C5_6 C 0.1051(9) 0.5514(11) 1.0682(9) 0.073(3) Uani 0.363(11) 1 d D U P B 2
H5_6 H 0.097292 0.482838 1.112254 0.088 Uiso 0.363(11) 1 calc R U P B 2
C6_6 C 0.1995(7) 0.5767(9) 1.0224(8) 0.062(2) Uani 0.363(11) 1 d D U P B 2
H6_6 H 0.258732 0.525178 1.030826 0.075 Uiso 0.363(11) 1 calc R U P B 2


_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
N2B C6_4 1.406(5) . ?
N2B Be3B 1.604(9) . ?
N2A C6_3 1.398(5) . ?
N2A Be3A 1.549(7) . ?
N2 C10 1.442(2) . ?
N2 Be2A 1.621(6) . ?
N2 Be1 1.765(3) . ?
N2 Be2B 1.806(12) . ?
N3A C6_1 1.389(4) . ?
N3A Be2A 1.583(6) . ?
N3B C6_2 1.432(8) . ?
N3B Be2B 1.540(11) . ?
N5 C28 1.436(3) . ?
N5 Be3B 1.570(10) . ?
N5 Be1 1.768(3) . ?
N5 Be3A 1.783(7) . ?
N1 C1 1.449(2) . ?
N1 Be2B 1.482(13) . ?
N1 Be1 1.764(3) . ?
N1 Be2A 1.775(6) . ?
N4 C19 1.446(2) . ?
N4 Be3A 1.535(8) . ?
N4 Be1 1.756(3) . ?
N4 Be3B 1.885(9) . ?
C8 C4 1.512(3) . ?
C1 C2 1.404(2) . ?
C1 C6 1.406(2) . ?
C9 C6 1.520(2) . ?
C10 C11 1.403(2) . ?
C10 C15 1.407(3) . ?
C11 C12 1.390(3) . ?
C11 C16 1.515(3) . ?
C12 C13 1.385(3) . ?
C13 C14 1.384(3) . ?
C13 C17 1.521(3) . ?
C14 C15 1.388(3) . ?
C15 C18 1.516(3) . ?
C19 C24 1.404(2) . ?
C19 C20 1.405(3) . ?
C20 C21 1.387(3) . ?
C20 C25 1.516(2) . ?
C21 C22 1.395(3) . ?
C22 C23 1.386(3) . ?
C22 C26 1.513(3) . ?
C23 C24 1.387(3) . ?
C24 C27 1.517(3) . ?
C28 C33 1.401(3) . ?
C28 C29 1.411(3) . ?
C29 C30 1.385(3) . ?
C29 C34 1.513(3) . ?
C30 C31 1.385(3) . ?
C31 C32 1.397(3) . ?
C31 C35 1.515(3) . ?
C32 C33 1.392(3) . ?
C33 C36 1.518(2) . ?
C2 C3 1.392(3) . ?
C2 C7 1.507(2) . ?
C3 C4 1.387(2) . ?
C4 C5 1.390(2) . ?
C5 C6 1.394(3) . ?
Be1 Be2B 2.247(11) . ?
Be1 Be3A 2.271(8) . ?
Be1 Be2A 2.337(6) . ?
Be1 Be3B 2.379(9) . ?
C1_1 C2_1 1.384(5) . ?
C1_1 C6_1 1.414(5) . ?
C1_1 C7_1 1.503(4) . ?
C2_1 C3_1 1.389(5) . ?
C3_1 C4_1 1.381(5) . ?
C3_1 C8_1 1.518(5) . ?
C4_1 C5_1 1.406(5) . ?
C5_1 C6_1 1.411(4) . ?
C5_1 C9_1 1.504(4) . ?
C1_2 C2_2 1.381(8) . ?
C1_2 C6_2 1.408(7) . ?
C1_2 C7_2 1.525(8) . ?
C2_2 C3_2 1.389(10) . ?
C3_2 C4_2 1.384(9) . ?
C3_2 C8_2 1.516(9) . ?
C4_2 C5_2 1.388(7) . ?
C5_2 C6_2 1.400(8) . ?
C5_2 C9_2 1.511(8) . ?
C1_3 C2_3 1.388(5) . ?
C1_3 C6_3 1.400(5) . ?
C1_3 C7_3 1.502(5) . ?
C2_3 C3_3 1.399(5) . ?
C3_3 C4_3 1.388(6) . ?
C3_3 C8_3 1.515(5) . ?
C4_3 C5_3 1.389(5) . ?
C5_3 C6_3 1.413(5) . ?
C5_3 C9_3 1.510(5) . ?
C1_4 C6_4 1.399(6) . ?
C1_4 C2_4 1.400(6) . ?
C1_4 C7_4 1.521(6) . ?
C2_4 C3_4 1.390(7) . ?
C3_4 C4_4 1.391(7) . ?
C3_4 C8_4 1.518(6) . ?
C4_4 C5_4 1.376(6) . ?
C5_4 C6_4 1.397(6) . ?
C5_4 C9_4 1.514(6) . ?
C1_5 C2_5 1.375(7) . ?
C1_5 C6_5 1.380(7) . ?
C2_5 C3_5 1.366(8) . ?
C3_5 C4_5 1.366(9) . ?
C4_5 C5_5 1.387(8) . ?
C5_5 C6_5 1.388(7) . ?
C1_6 C2_6 1.357(12) . ?
C1_6 C6_6 1.380(11) . ?
C2_6 C3_6 1.365(11) . ?
C3_6 C4_6 1.374(11) . ?
C4_6 C5_6 1.375(11) . ?
C5_6 C6_6 1.386(9) . ?

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
C6_4 N2B Be3B 135.1(6) . . ?
C6_3 N2A Be3A 142.6(4) . . ?
C10 N2 Be2A 117.6(3) . . ?
C10 N2 Be1 131.69(14) . . ?
Be2A N2 Be1 87.2(2) . . ?
C10 N2 Be2B 119.8(6) . . ?
Be1 N2 Be2B 78.0(4) . . ?
C6_1 N3A Be2A 145.8(3) . . ?
C6_2 N3B Be2B 143.9(7) . . ?
C28 N5 Be3B 117.3(5) . . ?
C28 N5 Be1 130.55(14) . . ?
Be3B N5 Be1 90.7(4) . . ?
C28 N5 Be3A 123.5(4) . . ?
Be1 N5 Be3A 79.5(3) . . ?
C1 N1 Be2B 119.5(6) . . ?
C1 N1 Be1 130.36(16) . . ?
Be2B N1 Be1 87.1(5) . . ?
C1 N1 Be2A 117.7(3) . . ?
Be1 N1 Be2A 82.7(2) . . ?
C19 N4 Be3A 117.2(4) . . ?
C19 N4 Be1 129.06(17) . . ?
Be3A N4 Be1 87.0(3) . . ?
C19 N4 Be3B 118.6(4) . . ?
Be1 N4 Be3B 81.5(3) . . ?
C2 C1 C6 119.25(17) . . ?
C2 C1 N1 119.15(16) . . ?
C6 C1 N1 121.52(16) . . ?
C11 C10 C15 119.33(18) . . ?
C11 C10 N2 119.75(17) . . ?
C15 C10 N2 120.79(17) . . ?
C12 C11 C10 118.96(19) . . ?
C12 C11 C16 118.85(18) . . ?
C10 C11 C16 122.00(18) . . ?
C13 C12 C11 122.8(2) . . ?
C14 C13 C12 116.9(2) . . ?
C14 C13 C17 121.5(2) . . ?
C12 C13 C17 121.6(2) . . ?
C13 C14 C15 123.0(2) . . ?
C14 C15 C10 118.86(19) . . ?
C14 C15 C18 119.66(19) . . ?
C10 C15 C18 121.31(19) . . ?
C24 C19 C20 119.63(18) . . ?
C24 C19 N4 119.32(18) . . ?
C20 C19 N4 120.98(17) . . ?
C21 C20 C19 118.90(18) . . ?
C21 C20 C25 119.41(18) . . ?
C19 C20 C25 121.47(18) . . ?
C20 C21 C22 122.54(19) . . ?
C23 C22 C21 117.09(18) . . ?
C23 C22 C26 121.34(19) . . ?
C21 C22 C26 121.55(19) . . ?
C22 C23 C24 122.62(18) . . ?
C23 C24 C19 119.06(19) . . ?
C23 C24 C27 118.77(17) . . ?
C19 C24 C27 121.97(18) . . ?
C33 C28 C29 119.60(19) . . ?
C33 C28 N5 119.68(16) . . ?
C29 C28 N5 120.69(19) . . ?
C30 C29 C28 118.9(2) . . ?
C30 C29 C34 119.67(19) . . ?
C28 C29 C34 121.4(2) . . ?
C29 C30 C31 122.6(2) . . ?
C30 C31 C32 117.6(2) . . ?
C30 C31 C35 121.8(2) . . ?
C32 C31 C35 120.5(2) . . ?
C33 C32 C31 121.9(2) . . ?
C32 C33 C28 119.11(18) . . ?
C32 C33 C36 119.02(18) . . ?
C28 C33 C36 121.67(17) . . ?
C3 C2 C1 119.08(17) . . ?
C3 C2 C7 118.59(16) . . ?
C1 C2 C7 122.26(17) . . ?
C4 C3 C2 122.75(17) . . ?
C5 C4 C3 117.17(18) . . ?
C5 C4 C8 122.08(17) . . ?
C3 C4 C8 120.73(17) . . ?
C4 C5 C6 122.26(17) . . ?
C5 C6 C1 119.34(16) . . ?
C5 C6 C9 119.13(16) . . ?
C1 C6 C9 121.45(17) . . ?
N4 Be1 N1 118.17(16) . . ?
N4 Be1 N2 118.10(15) . . ?
N1 Be1 N2 92.73(14) . . ?
N4 Be1 N5 92.93(15) . . ?
N1 Be1 N5 118.62(16) . . ?
N2 Be1 N5 118.62(16) . . ?
N4 Be1 Be2B 128.7(5) . . ?
N1 Be1 Be2B 41.2(4) . . ?
N2 Be1 Be2B 51.8(3) . . ?
N5 Be1 Be2B 137.9(5) . . ?
N4 Be1 Be3A 42.5(2) . . ?
N1 Be1 Be3A 135.7(3) . . ?
N2 Be1 Be3A 131.2(3) . . ?
N5 Be1 Be3A 50.5(2) . . ?
N4 Be1 Be2A 133.4(3) . . ?
N1 Be1 Be2A 48.88(17) . . ?
N2 Be1 Be2A 43.86(17) . . ?
N5 Be1 Be2A 133.5(3) . . ?
Be3A Be1 Be2A 173.7(3) . . ?
N4 Be1 Be3B 51.6(3) . . ?
N1 Be1 Be3B 133.7(4) . . ?
N2 Be1 Be3B 133.2(4) . . ?
N5 Be1 Be3B 41.3(3) . . ?
Be2B Be1 Be3B 174.9(5) . . ?
N3A Be2A N2 116.9(4) . . ?
N3A Be2A N1 145.6(4) . . ?
N2 Be2A N1 97.4(3) . . ?
N3A Be2A Be1 165.7(4) . . ?
N2 Be2A Be1 48.95(17) . . ?
N1 Be2A Be1 48.47(15) . . ?
N1 Be2B N3B 111.1(8) . . ?
N1 Be2B N2 101.5(6) . . ?
N3B Be2B N2 146.6(8) . . ?
N1 Be2B Be1 51.6(4) . . ?
N3B Be2B Be1 162.8(9) . . ?
N2 Be2B Be1 50.2(3) . . ?
N4 Be3A N2A 113.3(5) . . ?
N4 Be3A N5 100.4(4) . . ?
N2A Be3A N5 146.1(5) . . ?
N4 Be3A Be1 50.6(2) . . ?
N2A Be3A Be1 163.9(5) . . ?
N5 Be3A Be1 50.0(2) . . ?
N5 Be3B N2B 119.1(6) . . ?
N5 Be3B N4 94.9(4) . . ?
N2B Be3B N4 146.0(7) . . ?
N5 Be3B Be1 48.0(2) . . ?
N2B Be3B Be1 167.1(7) . . ?
N4 Be3B Be1 46.9(2) . . ?
C2_1 C1_1 C6_1 120.1(3) . . ?
C2_1 C1_1 C7_1 119.3(4) . . ?
C6_1 C1_1 C7_1 120.6(4) . . ?
C3_1 C2_1 C1_1 122.3(5) . . ?
C2_1 C3_1 C4_1 117.3(4) . . ?
C2_1 C3_1 C8_1 121.1(4) . . ?
C4_1 C3_1 C8_1 121.6(4) . . ?
C3_1 C4_1 C5_1 123.1(4) . . ?
C4_1 C5_1 C6_1 118.6(4) . . ?
C4_1 C5_1 C9_1 120.6(4) . . ?
C6_1 C5_1 C9_1 120.8(4) . . ?
N3A C6_1 C5_1 119.9(4) . . ?
N3A C6_1 C1_1 121.3(4) . . ?
C5_1 C6_1 C1_1 118.7(3) . . ?
C2_2 C1_2 C6_2 118.0(8) . . ?
C2_2 C1_2 C7_2 121.3(8) . . ?
C6_2 C1_2 C7_2 120.7(8) . . ?
C1_2 C2_2 C3_2 123.2(8) . . ?
C4_2 C3_2 C2_2 117.5(7) . . ?
C4_2 C3_2 C8_2 121.6(9) . . ?
C2_2 C3_2 C8_2 120.8(9) . . ?
C5_2 C4_2 C3_2 122.0(7) . . ?
C4_2 C5_2 C6_2 119.1(7) . . ?
C4_2 C5_2 C9_2 119.9(8) . . ?
C6_2 C5_2 C9_2 121.0(7) . . ?
C5_2 C6_2 C1_2 120.2(7) . . ?
C5_2 C6_2 N3B 120.7(7) . . ?
C1_2 C6_2 N3B 119.1(8) . . ?
C2_3 C1_3 C6_3 120.3(4) . . ?
C2_3 C1_3 C7_3 120.1(5) . . ?
C6_3 C1_3 C7_3 119.6(5) . . ?
C1_3 C2_3 C3_3 121.9(4) . . ?
C2_3 C3_3 C4_3 116.9(4) . . ?
C2_3 C3_3 C8_3 120.6(5) . . ?
C4_3 C3_3 C8_3 122.5(5) . . ?
C5_3 C4_3 C3_3 123.2(5) . . ?
C4_3 C5_3 C6_3 118.9(5) . . ?
C4_3 C5_3 C9_3 120.1(5) . . ?
C6_3 C5_3 C9_3 121.0(5) . . ?
C1_3 C6_3 N2A 122.1(5) . . ?
C1_3 C6_3 C5_3 118.9(4) . . ?
N2A C6_3 C5_3 119.0(5) . . ?
C6_4 C1_4 C2_4 120.0(5) . . ?
C6_4 C1_4 C7_4 119.8(6) . . ?
C2_4 C1_4 C7_4 120.0(6) . . ?
C3_4 C2_4 C1_4 121.2(5) . . ?
C2_4 C3_4 C4_4 117.8(5) . . ?
C2_4 C3_4 C8_4 119.6(6) . . ?
C4_4 C3_4 C8_4 122.5(6) . . ?
C5_4 C4_4 C3_4 121.9(6) . . ?
C6_4 C5_4 C4_4 120.5(5) . . ?
C6_4 C5_4 C9_4 121.8(6) . . ?
C4_4 C5_4 C9_4 117.7(6) . . ?
C5_4 C6_4 C1_4 118.6(4) . . ?
C5_4 C6_4 N2B 120.2(6) . . ?
C1_4 C6_4 N2B 121.2(6) . . ?
C2_5 C1_5 C6_5 119.8(6) . . ?
C3_5 C2_5 C1_5 121.0(8) . . ?
C2_5 C3_5 C4_5 119.3(8) . . ?
C3_5 C4_5 C5_5 121.2(7) . . ?
C6_5 C5_5 C4_5 118.8(8) . . ?
C5_5 C6_5 C1_5 119.8(7) . . ?
C2_6 C1_6 C6_6 125.0(12) . . ?
C1_6 C2_6 C3_6 116.4(11) . . ?
C2_6 C3_6 C4_6 120.3(11) . . ?
C5_6 C4_6 C3_6 122.9(11) . . ?
C4_6 C5_6 C6_6 117.3(10) . . ?
C1_6 C6_6 C5_6 117.9(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Be2B N1 C1 C2 -55.2(6) . . . . ?
Be1 N1 C1 C2 58.8(3) . . . . ?
Be2A N1 C1 C2 -46.0(3) . . . . ?
Be2B N1 C1 C6 121.6(6) . . . . ?
Be1 N1 C1 C6 -124.4(2) . . . . ?
Be2A N1 C1 C6 130.7(3) . . . . ?
Be2A N2 C10 C11 -52.7(3) . . . . ?
Be1 N2 C10 C11 60.3(3) . . . . ?
Be2B N2 C10 C11 -40.5(5) . . . . ?
Be2A N2 C10 C15 123.0(3) . . . . ?
Be1 N2 C10 C15 -124.0(2) . . . . ?
Be2B N2 C10 C15 135.2(5) . . . . ?
C15 C10 C11 C12 4.7(3) . . . . ?
N2 C10 C11 C12 -179.58(17) . . . . ?
C15 C10 C11 C16 -170.22(18) . . . . ?
N2 C10 C11 C16 5.5(3) . . . . ?
C10 C11 C12 C13 -1.5(3) . . . . ?
C16 C11 C12 C13 173.6(2) . . . . ?
C11 C12 C13 C14 -1.3(4) . . . . ?
C11 C12 C13 C17 -179.8(2) . . . . ?
C12 C13 C14 C15 0.8(4) . . . . ?
C17 C13 C14 C15 179.4(2) . . . . ?
C13 C14 C15 C10 2.4(3) . . . . ?
C13 C14 C15 C18 -172.8(2) . . . . ?
C11 C10 C15 C14 -5.1(3) . . . . ?
N2 C10 C15 C14 179.20(18) . . . . ?
C11 C10 C15 C18 170.01(18) . . . . ?
N2 C10 C15 C18 -5.7(3) . . . . ?
Be3A N4 C19 C24 51.6(5) . . . . ?
Be1 N4 C19 C24 -58.2(3) . . . . ?
Be3B N4 C19 C24 44.8(5) . . . . ?
Be3A N4 C19 C20 -125.5(4) . . . . ?
Be1 N4 C19 C20 124.7(2) . . . . ?
Be3B N4 C19 C20 -132.3(4) . . . . ?
C24 C19 C20 C21 3.6(3) . . . . ?
N4 C19 C20 C21 -179.34(19) . . . . ?
C24 C19 C20 C25 -170.94(19) . . . . ?
N4 C19 C20 C25 6.2(3) . . . . ?
C19 C20 C21 C22 -0.1(3) . . . . ?
C25 C20 C21 C22 174.55(19) . . . . ?
C20 C21 C22 C23 -2.6(3) . . . . ?
C20 C21 C22 C26 179.0(2) . . . . ?
C21 C22 C23 C24 1.9(3) . . . . ?
C26 C22 C23 C24 -179.7(2) . . . . ?
C22 C23 C24 C19 1.5(3) . . . . ?
C22 C23 C24 C27 -173.33(19) . . . . ?
C20 C19 C24 C23 -4.3(3) . . . . ?
N4 C19 C24 C23 178.58(19) . . . . ?
C20 C19 C24 C27 170.42(19) . . . . ?
N4 C19 C24 C27 -6.7(3) . . . . ?
Be3B N5 C28 C33 56.3(5) . . . . ?
Be1 N5 C28 C33 -61.1(3) . . . . ?
Be3A N5 C28 C33 45.1(4) . . . . ?
Be3B N5 C28 C29 -121.6(5) . . . . ?
Be1 N5 C28 C29 121.0(2) . . . . ?
Be3A N5 C28 C29 -132.8(4) . . . . ?
C33 C28 C29 C30 4.8(3) . . . . ?
N5 C28 C29 C30 -177.29(17) . . . . ?
C33 C28 C29 C34 -172.93(17) . . . . ?
N5 C28 C29 C34 5.0(3) . . . . ?
C28 C29 C30 C31 0.0(3) . . . . ?
C34 C29 C30 C31 177.78(18) . . . . ?
C29 C30 C31 C32 -3.4(3) . . . . ?
C29 C30 C31 C35 177.63(19) . . . . ?
C30 C31 C32 C33 2.1(3) . . . . ?
C35 C31 C32 C33 -178.94(19) . . . . ?
C31 C32 C33 C28 2.6(3) . . . . ?
C31 C32 C33 C36 -172.40(17) . . . . ?
C29 C28 C33 C32 -6.0(3) . . . . ?
N5 C28 C33 C32 176.02(16) . . . . ?
C29 C28 C33 C36 168.81(17) . . . . ?
N5 C28 C33 C36 -9.1(3) . . . . ?
C6 C1 C2 C3 4.3(3) . . . . ?
N1 C1 C2 C3 -178.89(17) . . . . ?
C6 C1 C2 C7 -172.51(17) . . . . ?
N1 C1 C2 C7 4.3(3) . . . . ?
C1 C2 C3 C4 -1.6(3) . . . . ?
C7 C2 C3 C4 175.31(17) . . . . ?
C2 C3 C4 C5 -1.8(3) . . . . ?
C2 C3 C4 C8 179.97(18) . . . . ?
C3 C4 C5 C6 2.5(3) . . . . ?
C8 C4 C5 C6 -179.27(18) . . . . ?
C4 C5 C6 C1 0.1(3) . . . . ?
C4 C5 C6 C9 -176.68(17) . . . . ?
C2 C1 C6 C5 -3.6(3) . . . . ?
N1 C1 C6 C5 179.65(17) . . . . ?
C2 C1 C6 C9 173.17(17) . . . . ?
N1 C1 C6 C9 -3.6(3) . . . . ?
C19 N4 Be1 N1 -5.1(3) . . . . ?
Be3A N4 Be1 N1 -128.1(5) . . . . ?
Be3B N4 Be1 N1 -125.2(5) . . . . ?
C19 N4 Be1 N2 -115.4(2) . . . . ?
Be3A N4 Be1 N2 121.6(5) . . . . ?
Be3B N4 Be1 N2 124.5(5) . . . . ?
C19 N4 Be1 N5 119.8(2) . . . . ?
Be3A N4 Be1 N5 -3.3(5) . . . . ?
Be3B N4 Be1 N5 -0.3(5) . . . . ?
C19 N4 Be1 Be2B -53.4(5) . . . . ?
Be3B N4 Be1 Be2B -173.6(7) . . . . ?
C19 N4 Be1 Be3A 123.1(5) . . . . ?
C19 N4 Be1 Be2A -63.7(3) . . . . ?
Be3A N4 Be1 Be2A 173.2(5) . . . . ?
C19 N4 Be1 Be3B 120.1(5) . . . . ?
C1 N1 Be1 N4 115.0(2) . . . . ?
Be2B N1 Be1 N4 -117.7(7) . . . . ?
Be2A N1 Be1 N4 -124.6(3) . . . . ?
C1 N1 Be1 N2 -120.87(18) . . . . ?
Be2B N1 Be1 N2 6.4(7) . . . . ?
Be2A N1 Be1 N2 -0.5(3) . . . . ?
C1 N1 Be1 N5 4.0(3) . . . . ?
Be2B N1 Be1 N5 131.3(7) . . . . ?
Be2A N1 Be1 N5 124.4(3) . . . . ?
C1 N1 Be1 Be2B -127.3(7) . . . . ?
C1 N1 Be1 Be3A 65.5(4) . . . . ?
Be2A N1 Be1 Be3A -174.1(4) . . . . ?
C1 N1 Be1 Be2A -120.4(3) . . . . ?
C1 N1 Be1 Be3B 52.6(4) . . . . ?
Be2B N1 Be1 Be3B 179.8(8) . . . . ?
C10 N2 Be1 N4 -0.6(3) . . . . ?
Be2A N2 Be1 N4 124.7(4) . . . . ?
Be2B N2 Be1 N4 118.8(6) . . . . ?
C10 N2 Be1 N1 -124.72(19) . . . . ?
Be2A N2 Be1 N1 0.6(3) . . . . ?
Be2B N2 Be1 N1 -5.4(6) . . . . ?
C10 N2 Be1 N5 110.4(2) . . . . ?
Be2A N2 Be1 N5 -124.4(4) . . . . ?
Be2B N2 Be1 N5 -130.3(6) . . . . ?
C10 N2 Be1 Be2B -119.4(6) . . . . ?
C10 N2 Be1 Be3A 49.3(4) . . . . ?
Be2A N2 Be1 Be3A 174.6(4) . . . . ?
C10 N2 Be1 Be2A -125.3(4) . . . . ?
C10 N2 Be1 Be3B 61.8(4) . . . . ?
Be2B N2 Be1 Be3B -178.9(7) . . . . ?
C28 N5 Be1 N4 128.28(18) . . . . ?
Be3B N5 Be1 N4 0.4(6) . . . . ?
Be3A N5 Be1 N4 2.8(4) . . . . ?
C28 N5 Be1 N1 -107.2(2) . . . . ?
Be3B N5 Be1 N1 124.9(6) . . . . ?
Be3A N5 Be1 N1 127.3(4) . . . . ?
C28 N5 Be1 N2 3.9(3) . . . . ?
Be3B N5 Be1 N2 -124.0(6) . . . . ?
Be3A N5 Be1 N2 -121.6(4) . . . . ?
C28 N5 Be1 Be2B -59.6(6) . . . . ?
Be3B N5 Be1 Be2B 172.5(8) . . . . ?
C28 N5 Be1 Be3A 125.4(4) . . . . ?
C28 N5 Be1 Be2A -48.2(4) . . . . ?
Be3A N5 Be1 Be2A -173.6(5) . . . . ?
C28 N5 Be1 Be3B 127.9(6) . . . . ?
C6_1 N3A Be2A N2 149.1(5) . . . . ?
C6_1 N3A Be2A N1 -26.3(16) . . . . ?
C6_1 N3A Be2A Be1 142.7(17) . . . . ?
C10 N2 Be2A N3A -41.4(6) . . . . ?
Be1 N2 Be2A N3A -177.9(5) . . . . ?
C10 N2 Be2A N1 136.0(3) . . . . ?
Be1 N2 Be2A N1 -0.6(3) . . . . ?
C10 N2 Be2A Be1 136.5(2) . . . . ?
C1 N1 Be2A N3A -51.5(11) . . . . ?
Be1 N1 Be2A N3A 176.4(10) . . . . ?
C1 N1 Be2A N2 132.6(3) . . . . ?
Be1 N1 Be2A N2 0.6(3) . . . . ?
C1 N1 Be2A Be1 132.0(2) . . . . ?
C1 N1 Be2B N3B -43.0(12) . . . . ?
Be1 N1 Be2B N3B -178.9(10) . . . . ?
C1 N1 Be2B N2 129.4(5) . . . . ?
Be1 N1 Be2B N2 -6.4(7) . . . . ?
C1 N1 Be2B Be1 135.8(3) . . . . ?
C6_2 N3B Be2B N1 -168.2(7) . . . . ?
C6_2 N3B Be2B N2 25(3) . . . . ?
C6_2 N3B Be2B Be1 -171(3) . . . . ?
C10 N2 Be2B N1 137.9(6) . . . . ?
Be1 N2 Be2B N1 6.5(7) . . . . ?
C10 N2 Be2B N3B -55(2) . . . . ?
Be1 N2 Be2B N3B 174(2) . . . . ?
C10 N2 Be2B Be1 131.4(2) . . . . ?
C19 N4 Be3A N2A 46.8(8) . . . . ?
Be1 N4 Be3A N2A 179.8(7) . . . . ?
C19 N4 Be3A N5 -129.7(4) . . . . ?
Be1 N4 Be3A N5 3.3(5) . . . . ?
C19 N4 Be3A Be1 -133.0(2) . . . . ?
C6_3 N2A Be3A N4 -139.7(5) . . . . ?
C6_3 N2A Be3A N5 34(2) . . . . ?
C6_3 N2A Be3A Be1 -139(2) . . . . ?
C28 N5 Be3A N4 -135.4(4) . . . . ?
Be1 N5 Be3A N4 -3.3(5) . . . . ?
C28 N5 Be3A N2A 50.4(15) . . . . ?
Be1 N5 Be3A N2A -177.5(15) . . . . ?
C28 N5 Be3A Be1 -132.1(2) . . . . ?
C28 N5 Be3B N2B 41.0(12) . . . . ?
Be1 N5 Be3B N2B 178.6(9) . . . . ?
C28 N5 Be3B N4 -137.9(4) . . . . ?
Be1 N5 Be3B N4 -0.4(5) . . . . ?
C28 N5 Be3B Be1 -137.6(3) . . . . ?
C6_4 N2B Be3B N5 146.2(7) . . . . ?
C6_4 N2B Be3B N4 -36(2) . . . . ?
C6_4 N2B Be3B Be1 151(4) . . . . ?
C19 N4 Be3B N5 -129.7(5) . . . . ?
Be1 N4 Be3B N5 0.4(5) . . . . ?
C19 N4 Be3B N2B 51.9(18) . . . . ?
Be1 N4 Be3B N2B -178.0(18) . . . . ?
C19 N4 Be3B Be1 -130.1(2) . . . . ?
C6_1 C1_1 C2_1 C3_1 -0.3(6) . . . . ?
C7_1 C1_1 C2_1 C3_1 -178.4(4) . . . . ?
C1_1 C2_1 C3_1 C4_1 -0.8(6) . . . . ?
C1_1 C2_1 C3_1 C8_1 176.5(5) . . . . ?
C2_1 C3_1 C4_1 C5_1 0.4(7) . . . . ?
C8_1 C3_1 C4_1 C5_1 -176.9(5) . . . . ?
C3_1 C4_1 C5_1 C6_1 1.1(7) . . . . ?
C3_1 C4_1 C5_1 C9_1 178.9(4) . . . . ?
Be2A N3A C6_1 C5_1 -169.1(7) . . . . ?
Be2A N3A C6_1 C1_1 8.7(9) . . . . ?
C4_1 C5_1 C6_1 N3A 175.7(4) . . . . ?
C9_1 C5_1 C6_1 N3A -2.2(5) . . . . ?
C4_1 C5_1 C6_1 C1_1 -2.2(6) . . . . ?
C9_1 C5_1 C6_1 C1_1 180.0(3) . . . . ?
C2_1 C1_1 C6_1 N3A -176.0(4) . . . . ?
C7_1 C1_1 C6_1 N3A 2.0(6) . . . . ?
C2_1 C1_1 C6_1 C5_1 1.8(6) . . . . ?
C7_1 C1_1 C6_1 C5_1 179.8(3) . . . . ?
C6_2 C1_2 C2_2 C3_2 -0.2(9) . . . . ?
C7_2 C1_2 C2_2 C3_2 -178.2(7) . . . . ?
C1_2 C2_2 C3_2 C4_2 -0.8(9) . . . . ?
C1_2 C2_2 C3_2 C8_2 176.4(8) . . . . ?
C2_2 C3_2 C4_2 C5_2 1.4(11) . . . . ?
C8_2 C3_2 C4_2 C5_2 -175.9(8) . . . . ?
C3_2 C4_2 C5_2 C6_2 -0.9(11) . . . . ?
C3_2 C4_2 C5_2 C9_2 179.0(7) . . . . ?
C4_2 C5_2 C6_2 C1_2 -0.2(11) . . . . ?
C9_2 C5_2 C6_2 C1_2 179.9(6) . . . . ?
C4_2 C5_2 C6_2 N3B 179.7(6) . . . . ?
C9_2 C5_2 C6_2 N3B -0.2(10) . . . . ?
C2_2 C1_2 C6_2 C5_2 0.7(10) . . . . ?
C7_2 C1_2 C6_2 C5_2 178.8(7) . . . . ?
C2_2 C1_2 C6_2 N3B -179.2(6) . . . . ?
C7_2 C1_2 C6_2 N3B -1.1(10) . . . . ?
Be2B N3B C6_2 C5_2 -32.2(15) . . . . ?
Be2B N3B C6_2 C1_2 147.7(12) . . . . ?
C6_3 C1_3 C2_3 C3_3 -0.2(6) . . . . ?
C7_3 C1_3 C2_3 C3_3 178.3(4) . . . . ?
C1_3 C2_3 C3_3 C4_3 0.0(6) . . . . ?
C1_3 C2_3 C3_3 C8_3 -178.5(4) . . . . ?
C2_3 C3_3 C4_3 C5_3 0.9(7) . . . . ?
C8_3 C3_3 C4_3 C5_3 179.3(5) . . . . ?
C3_3 C4_3 C5_3 C6_3 -1.5(8) . . . . ?
C3_3 C4_3 C5_3 C9_3 179.8(4) . . . . ?
C2_3 C1_3 C6_3 N2A 177.2(3) . . . . ?
C7_3 C1_3 C6_3 N2A -1.3(6) . . . . ?
C2_3 C1_3 C6_3 C5_3 -0.4(6) . . . . ?
C7_3 C1_3 C6_3 C5_3 -178.9(4) . . . . ?
Be3A N2A C6_3 C1_3 -23.7(10) . . . . ?
Be3A N2A C6_3 C5_3 153.9(8) . . . . ?
C4_3 C5_3 C6_3 C1_3 1.1(7) . . . . ?
C9_3 C5_3 C6_3 C1_3 179.9(4) . . . . ?
C4_3 C5_3 C6_3 N2A -176.5(4) . . . . ?
C9_3 C5_3 C6_3 N2A 2.2(6) . . . . ?
C6_4 C1_4 C2_4 C3_4 0.7(7) . . . . ?
C7_4 C1_4 C2_4 C3_4 176.3(5) . . . . ?
C1_4 C2_4 C3_4 C4_4 1.5(7) . . . . ?
C1_4 C2_4 C3_4 C8_4 -176.0(5) . . . . ?
C2_4 C3_4 C4_4 C5_4 -1.7(9) . . . . ?
C8_4 C3_4 C4_4 C5_4 175.7(5) . . . . ?
C3_4 C4_4 C5_4 C6_4 -0.3(9) . . . . ?
C3_4 C4_4 C5_4 C9_4 177.4(5) . . . . ?
C4_4 C5_4 C6_4 C1_4 2.4(8) . . . . ?
C9_4 C5_4 C6_4 C1_4 -175.1(5) . . . . ?
C4_4 C5_4 C6_4 N2B -177.5(5) . . . . ?
C9_4 C5_4 C6_4 N2B 5.0(7) . . . . ?
C2_4 C1_4 C6_4 C5_4 -2.6(7) . . . . ?
C7_4 C1_4 C6_4 C5_4 -178.2(4) . . . . ?
C2_4 C1_4 C6_4 N2B 177.2(4) . . . . ?
C7_4 C1_4 C6_4 N2B 1.6(7) . . . . ?
Be3B N2B C6_4 C5_4 52.2(10) . . . . ?
Be3B N2B C6_4 C1_4 -127.7(8) . . . . ?
C6_5 C1_5 C2_5 C3_5 1.0(10) . . . . ?
C1_5 C2_5 C3_5 C4_5 1.0(12) . . . . ?
C2_5 C3_5 C4_5 C5_5 -0.4(14) . . . . ?
C3_5 C4_5 C5_5 C6_5 -2.3(14) . . . . ?
C4_5 C5_5 C6_5 C1_5 4.2(13) . . . . ?
C2_5 C1_5 C6_5 C5_5 -3.7(11) . . . . ?
C6_6 C1_6 C2_6 C3_6 2.0(18) . . . . ?
C1_6 C2_6 C3_6 C4_6 2.4(15) . . . . ?
C2_6 C3_6 C4_6 C5_6 -3(2) . . . . ?
C3_6 C4_6 C5_6 C6_6 0(2) . . . . ?
C2_6 C1_6 C6_6 C5_6 -5(2) . . . . ?
C4_6 C5_6 C6_6 C1_6 4(2) . . . . ?

_refine_diff_density_max         0.201
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.046



# start Validation Reply Form
_vrf_PLAT220_LTH473              
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        3.3 Ratio
RESPONSE: Due to disorder.
;
_vrf_PLAT420_LTH473              
;
PROBLEM: D-H Bond Without Acceptor  N1       --H1N      .     Please Check
RESPONSE: Chemically correct, no acceptor is expected.
;
_vrf_PLAT906_LTH473              
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.356 Check
RESPONSE: Likely due to disorder.
;
_vrf_PLAT911_LTH473              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         82 Report
RESPONSE: A few reflections could not be collected using the selected
measurement strategy and the instrument.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_LTH435
_database_code_depnum_ccdc_archive 'CCDC 2373013'
loop_
_audit_author_name
_audit_author_address
'Sergei Ivlev'
;Philipps Universitaet Marburg
Germany
;
_audit_update_record             
;
2024-07-23 deposited with the CCDC.	2024-08-27 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2019/1
_shelx_SHELXL_version_number     2019/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C78 H60 Be3 N6'
_chemical_formula_sum            'C78 H60 Be3 N6'
_chemical_formula_weight         1108.35

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      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.9415(6)
_cell_length_b                   15.0952(7)
_cell_length_c                   23.1922(13)
_cell_angle_alpha                71.835(4)
_cell_angle_beta                 87.988(6)
_cell_angle_gamma                71.142(4)
_cell_volume                     3121.1(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100
_cell_measurement_reflns_used    38162
_cell_measurement_theta_min      3.34
_cell_measurement_theta_max      76.02

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.179
_exptl_crystal_F_000             1164
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.522
_shelx_estimated_absorpt_T_min   0.859
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4010
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_process_details   
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens in: F. R. Ahmed (Editor), "Crystallographic Computing", Munksgaard,
Copenhagen (1970), 255 - 270. Afterwards scaling of reflection intensities was
performed within STOE LANA. J. Koziskova, F. Hahn, J. Richter, J. Kozisek, Acta
Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Finally a spherical absorption correction was done within STOE LANA.
;

_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'

_diffrn_detector                 Pilatus300K
_diffrn_detector_type            'DECTRIS PILATUS 300K'
_diffrn_detector_area_resol_mean 5.81

_diffrn_source                   'GeniX 3D HF Cu'
_diffrn_radiation_probe          x-ray
_diffrn_source_voltage           50
_diffrn_source_current           0.600
_diffrn_source_power             0.030
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54186
_diffrn_radiation_monochromator  'Graded multilayer mirror'
_diffrn_radiation_polarisn_norm  270
_diffrn_radiation_collimation    '0.5 mm diameter'

_diffrn_ambient_temperature      100

_diffrn_measurement_method       'rotation method, ω scans'
_diffrn_measurement_details      
; 5207 frames, detector distance = 60 mm
;

_diffrn_reflns_number            70021
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.243
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             11726
_reflns_number_gt                9176
_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       
;
X-Area Pilatus3_SV 1.31.170.0 (STOE, 2020)
;
_computing_cell_refinement       
;
X-Area Recipe 1.36.0.0 (STOE, 2020)
;
_computing_data_reduction        
;
X-Area Integrate 1.78.3.0 (STOE, 2020)
X-Area LANA 1.83.8.0 (STOE, 2020)
;
_computing_publication_material  
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image
processing, for the correction and scaling of reflection intensities and
for outlier rejection, version 1.90, Darmstadt 2020
;
_computing_structure_refinement  'SHELXL-2019/1 (Sheldrick, 2019)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0919P)²+0.5194P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_extinction_coef       0.0025(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         11726
_refine_ls_number_parameters     785
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0546
_refine_ls_wR_factor_ref         0.1653
_refine_ls_wR_factor_gt          0.1569
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_restrained_S_all      1.086
_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 0.1655(2) 0.75998(12) 0.66255(7) 0.0657(5) Uani 1 1 d . . . . .
N2 N 0.42402(16) 0.58987(10) 0.67904(6) 0.0449(3) Uani 1 1 d . . . . .
N3 N 0.27235(16) 0.58372(10) 0.76567(6) 0.0463(3) Uani 1 1 d . . . . .
N4 N 0.46034(16) 0.38893(10) 0.74345(6) 0.0436(3) Uani 1 1 d . . . . .
N5 N 0.55419(16) 0.45923(10) 0.80908(6) 0.0448(3) Uani 1 1 d . . . . .
N6 N 0.68589(19) 0.24717(11) 0.83490(7) 0.0580(4) Uani 1 1 d . . . . .
C1 C 0.0741(2) 0.84393(14) 0.63788(8) 0.0594(5) Uani 1 1 d . . . . .
C2 C -0.0739(2) 0.85337(13) 0.61825(8) 0.0558(5) Uani 1 1 d . . . . .
C3 C -0.1382(3) 0.78762(16) 0.65316(11) 0.0707(6) Uani 1 1 d . . . . .
H3 H -0.089247 0.737725 0.689225 0.085 Uiso 1 1 calc R U . . .
C4 C -0.2749(3) 0.7949(2) 0.63521(14) 0.0865(8) Uani 1 1 d . . . . .
H4 H -0.318743 0.749686 0.659125 0.104 Uiso 1 1 calc R U . . .
C5 C -0.3461(3) 0.86658(18) 0.58342(14) 0.0808(7) Uani 1 1 d . . . . .
H5 H -0.439453 0.871230 0.571813 0.097 Uiso 1 1 calc R U . . .
C6 C -0.2841(3) 0.93160(18) 0.54825(12) 0.0756(6) Uani 1 1 d . . . . .
H6 H -0.333516 0.980597 0.511971 0.091 Uiso 1 1 calc R U . . .
C7 C -0.1490(3) 0.92588(16) 0.56561(10) 0.0664(6) Uani 1 1 d . . . . .
H7 H -0.106753 0.971884 0.541400 0.080 Uiso 1 1 calc R U . . .
C8 C 0.1093(2) 0.93582(14) 0.62878(8) 0.0568(5) Uani 1 1 d . . . . .
C9 C 0.2481(3) 0.93502(16) 0.62003(10) 0.0662(5) Uani 1 1 d . . . . .
H9 H 0.318964 0.876686 0.617580 0.079 Uiso 1 1 calc R U . . .
C10 C 0.2849(3) 1.01728(19) 0.61482(12) 0.0764(6) Uani 1 1 d . . . . .
H10 H 0.380325 1.015807 0.608288 0.092 Uiso 1 1 calc R U . . .
C11 C 0.1821(3) 1.10294(18) 0.61913(12) 0.0764(6) Uani 1 1 d . . . . .
H11 H 0.206830 1.160085 0.615591 0.092 Uiso 1 1 calc R U . . .
C12 C 0.0449(3) 1.10352(17) 0.62854(12) 0.0755(7) Uani 1 1 d . . . . .
H12 H -0.025232 1.161284 0.632180 0.091 Uiso 1 1 calc R U . . .
C13 C 0.0072(2) 1.02143(15) 0.63281(10) 0.0632(5) Uani 1 1 d . . . . .
H13 H -0.088740 1.023502 0.638512 0.076 Uiso 1 1 calc R U . . .
C14 C 0.4984(2) 0.58717(12) 0.63307(7) 0.0471(4) Uani 1 1 d . . . . .
C15 C 0.6380(2) 0.50686(12) 0.63803(8) 0.0487(4) Uani 1 1 d . . . . .
C16 C 0.7374(2) 0.47842(14) 0.68665(8) 0.0534(4) Uani 1 1 d . . . . .
H16 H 0.715955 0.510022 0.717026 0.064 Uiso 1 1 calc R U . . .
C17 C 0.8674(2) 0.40463(15) 0.69148(9) 0.0598(5) Uani 1 1 d . . . . .
H17 H 0.934656 0.386464 0.724719 0.072 Uiso 1 1 calc R U . . .
C18 C 0.8987(2) 0.35759(15) 0.64774(10) 0.0634(5) Uani 1 1 d . . . . .
H18 H 0.988015 0.307495 0.650726 0.076 Uiso 1 1 calc R U . . .
C19 C 0.8011(2) 0.38315(14) 0.60010(10) 0.0618(5) Uani 1 1 d . . . . .
H19 H 0.821839 0.349205 0.570882 0.074 Uiso 1 1 calc R U . . .
C20 C 0.6712(2) 0.45892(13) 0.59425(8) 0.0558(5) Uani 1 1 d . . . . .
H20 H 0.605418 0.477783 0.560367 0.067 Uiso 1 1 calc R U . . .
C21 C 0.4519(2) 0.66318(12) 0.57167(7) 0.0493(4) Uani 1 1 d . . . . .
C22 C 0.5502(3) 0.69829(13) 0.53585(8) 0.0576(5) Uani 1 1 d . . . . .
H22 H 0.648377 0.672042 0.549501 0.069 Uiso 1 1 calc R U . . .
C23 C 0.5047(3) 0.77226(14) 0.47971(9) 0.0669(6) Uani 1 1 d . . . . .
H23 H 0.571635 0.796993 0.455408 0.080 Uiso 1 1 calc R U . . .
C24 C 0.3632(3) 0.80902(15) 0.45983(9) 0.0700(6) Uani 1 1 d . . . . .
H24 H 0.333037 0.858484 0.421348 0.084 Uiso 1 1 calc R U . . .
C25 C 0.2640(3) 0.77515(16) 0.49494(9) 0.0676(6) Uani 1 1 d . . . . .
H25 H 0.166128 0.801655 0.480850 0.081 Uiso 1 1 calc R U . . .
C26 C 0.3081(2) 0.70198(14) 0.55108(8) 0.0572(5) Uani 1 1 d . . . . .
H26 H 0.240278 0.678441 0.575398 0.069 Uiso 1 1 calc R U . . .
C27 C 0.2052(2) 0.58547(12) 0.81350(8) 0.0466(4) Uani 1 1 d . . . . .
C28 C 0.0949(2) 0.67687(12) 0.81888(7) 0.0468(4) Uani 1 1 d . . . . .
C29 C 0.1155(2) 0.76748(13) 0.79581(8) 0.0522(4) Uani 1 1 d . . . . .
H29 H 0.200323 0.771684 0.776645 0.063 Uiso 1 1 calc R U . . .
C30 C 0.0127(2) 0.85227(14) 0.80058(9) 0.0626(5) Uani 1 1 d . . . . .
H30 H 0.027162 0.914288 0.784190 0.075 Uiso 1 1 calc R U . . .
C31 C -0.1095(2) 0.84718(16) 0.82879(9) 0.0660(6) Uani 1 1 d . . . . .
H31 H -0.178435 0.905247 0.832681 0.079 Uiso 1 1 calc R U . . .
C32 C -0.1320(2) 0.75780(17) 0.85138(10) 0.0661(5) Uani 1 1 d . . . . .
H32 H -0.217724 0.754350 0.869879 0.079 Uiso 1 1 calc R U . . .
C33 C -0.0291(2) 0.67237(15) 0.84717(9) 0.0589(5) Uani 1 1 d . . . . .
H33 H -0.043933 0.610523 0.863797 0.071 Uiso 1 1 calc R U . . .
C34 C 0.2345(2) 0.49540(12) 0.86841(8) 0.0477(4) Uani 1 1 d . . . . .
C35 C 0.2650(2) 0.40229(13) 0.86245(8) 0.0506(4) Uani 1 1 d . . . . .
H35 H 0.264439 0.395863 0.822999 0.061 Uiso 1 1 calc R U . . .
C36 C 0.2963(2) 0.31865(14) 0.91314(8) 0.0572(5) Uani 1 1 d . . . . .
H36 H 0.317338 0.255388 0.908410 0.069 Uiso 1 1 calc R U . . .
C37 C 0.2969(2) 0.32772(15) 0.97089(8) 0.0618(5) Uani 1 1 d . . . . .
H37 H 0.318197 0.270619 1.005813 0.074 Uiso 1 1 calc R U . . .
C38 C 0.2665(2) 0.41956(15) 0.97745(8) 0.0619(5) Uani 1 1 d . . . . .
H38 H 0.267279 0.425586 1.016998 0.074 Uiso 1 1 calc R U . . .
C39 C 0.2347(2) 0.50335(14) 0.92676(8) 0.0551(5) Uani 1 1 d . . . . .
H39 H 0.212950 0.566477 0.931780 0.066 Uiso 1 1 calc R U . . .
C40 C 0.42317(19) 0.35270(11) 0.70637(7) 0.0435(4) Uani 1 1 d . . . . .
C41 C 0.4997(2) 0.24846(12) 0.70734(7) 0.0456(4) Uani 1 1 d . . . . .
C42 C 0.4237(2) 0.18745(13) 0.70310(8) 0.0549(5) Uani 1 1 d . . . . .
H42 H 0.322656 0.212843 0.697082 0.066 Uiso 1 1 calc R U . . .
C43 C 0.4955(3) 0.08937(14) 0.70768(9) 0.0655(6) Uani 1 1 d . . . . .
H43 H 0.443219 0.047729 0.705295 0.079 Uiso 1 1 calc R U . . .
C44 C 0.6418(3) 0.05255(14) 0.71564(9) 0.0664(6) Uani 1 1 d . . . . .
H44 H 0.690619 -0.014363 0.718592 0.080 Uiso 1 1 calc R U . . .
C45 C 0.7177(2) 0.11287(14) 0.71932(8) 0.0593(5) Uani 1 1 d . . . . .
H45 H 0.818785 0.087343 0.724800 0.071 Uiso 1 1 calc R U . . .
C46 C 0.6473(2) 0.21046(13) 0.71506(7) 0.0495(4) Uani 1 1 d . . . . .
H46 H 0.700306 0.251621 0.717431 0.059 Uiso 1 1 calc R U . . .
C47 C 0.30233(19) 0.41217(12) 0.65846(7) 0.0449(4) Uani 1 1 d . . . . .
C48 C 0.3107(2) 0.40001(13) 0.60107(8) 0.0505(4) Uani 1 1 d . . . . .
H48 H 0.390356 0.351297 0.592990 0.061 Uiso 1 1 calc R U . . .
C49 C 0.2025(2) 0.45904(14) 0.55569(8) 0.0566(5) Uani 1 1 d . . . . .
H49 H 0.209175 0.450955 0.516558 0.068 Uiso 1 1 calc R U . . .
C50 C 0.0856(2) 0.52933(14) 0.56715(9) 0.0568(5) Uani 1 1 d . . . . .
H50 H 0.012165 0.569568 0.535917 0.068 Uiso 1 1 calc R U . . .
C51 C 0.0752(2) 0.54120(14) 0.62414(9) 0.0549(5) Uani 1 1 d . . . . .
H51 H -0.005687 0.589121 0.632207 0.066 Uiso 1 1 calc R U . . .
C52 C 0.1834(2) 0.48285(12) 0.66946(8) 0.0490(4) Uani 1 1 d . . . . .
H52 H 0.176058 0.491295 0.708500 0.059 Uiso 1 1 calc R U . . .
C53 C 0.5946(2) 0.49145(13) 0.84746(8) 0.0497(4) Uani 1 1 d . . . . .
C54 C 0.6939(2) 0.42372(13) 0.90207(8) 0.0488(4) Uani 1 1 d . . . . .
C55 C 0.6701(2) 0.33841(15) 0.93832(8) 0.0601(5) Uani 1 1 d . . . . .
H55 H 0.587119 0.324652 0.930434 0.072 Uiso 1 1 calc R U . . .
C56 C 0.7690(3) 0.27304(19) 0.98640(10) 0.0783(7) Uani 1 1 d . . . . .
H56 H 0.752850 0.214939 1.011701 0.094 Uiso 1 1 calc R U . . .
C57 C 0.8899(3) 0.2928(2) 0.99712(13) 0.0957(10) Uani 1 1 d . . . . .
H57 H 0.957407 0.247966 1.029697 0.115 Uiso 1 1 calc R U . . .
C58 C 0.9133(3) 0.3758(2) 0.96158(17) 0.0994(11) Uani 1 1 d . . . . .
H58 H 0.997047 0.388805 0.969336 0.119 Uiso 1 1 calc R U . . .
C59 C 0.8156(2) 0.44170(18) 0.91395(13) 0.0738(6) Uani 1 1 d . . . . .
H59 H 0.832778 0.499801 0.889271 0.089 Uiso 1 1 calc R U . . .
C60 C 0.5510(2) 0.60004(13) 0.83938(8) 0.0502(4) Uani 1 1 d . . . . .
C61 C 0.5471(2) 0.66810(14) 0.78275(9) 0.0587(5) Uani 1 1 d . . . . .
H61 H 0.570181 0.645860 0.748439 0.070 Uiso 1 1 calc R U . . .
C62 C 0.5102(2) 0.76807(14) 0.77515(10) 0.0624(5) Uani 1 1 d . . . . .
H62 H 0.510222 0.813379 0.736078 0.075 Uiso 1 1 calc R U . . .
C63 C 0.4736(2) 0.80158(15) 0.82408(10) 0.0601(5) Uani 1 1 d . . . . .
H63 H 0.448347 0.869994 0.819032 0.072 Uiso 1 1 calc R U . . .
C64 C 0.4737(2) 0.73494(15) 0.88083(10) 0.0609(5) Uani 1 1 d . . . . .
H64 H 0.446367 0.758033 0.914589 0.073 Uiso 1 1 calc R U . . .
C65 C 0.5135(2) 0.63469(15) 0.88874(9) 0.0556(5) Uani 1 1 d . . . . .
H65 H 0.515128 0.589451 0.928022 0.067 Uiso 1 1 calc R U . . .
C66 C 0.7762(2) 0.16520(14) 0.86210(8) 0.0556(5) Uani 1 1 d . . . . .
C67 C 0.7314(2) 0.08189(14) 0.90224(8) 0.0589(5) Uani 1 1 d . . . . .
C68 C 0.6126(3) 0.06637(15) 0.88416(10) 0.0670(6) Uani 1 1 d . . . . .
H68 H 0.561794 0.107526 0.846229 0.080 Uiso 1 1 calc R U . . .
C69 C 0.5666(4) -0.00834(19) 0.92060(13) 0.0912(8) Uani 1 1 d . . . . .
H69 H 0.485993 -0.019371 0.907173 0.109 Uiso 1 1 calc R U . . .
C70 C 0.6367(4) -0.0664(2) 0.97589(14) 0.0997(10) Uani 1 1 d . . . . .
H70 H 0.602035 -0.115815 1.001442 0.120 Uiso 1 1 calc R U . . .
C71 C 0.7554(4) -0.0542(2) 0.99471(12) 0.0977(10) Uani 1 1 d . . . . .
H71 H 0.805390 -0.096698 1.032573 0.117 Uiso 1 1 calc R U . . .
C72 C 0.8044(3) 0.02085(18) 0.95834(10) 0.0824(8) Uani 1 1 d . . . . .
H72 H 0.886517 0.030209 0.971711 0.099 Uiso 1 1 calc R U . . .
C73 C 0.9324(2) 0.14326(16) 0.85298(9) 0.0599(5) Uani 1 1 d . . . . .
C74 C 0.9907(3) 0.21791(19) 0.83795(10) 0.0739(6) Uani 1 1 d . . . . .
H74 H 0.933595 0.282713 0.836513 0.089 Uiso 1 1 calc R U . . .
C75 C 1.1351(4) 0.1987(2) 0.82462(12) 0.0909(9) Uani 1 1 d . . . . .
H75 H 1.175304 0.250350 0.814016 0.109 Uiso 1 1 calc R U . . .
C76 C 1.2154(3) 0.1060(3) 0.82712(14) 0.0977(9) Uani 1 1 d . . . . .
H76 H 1.311682 0.093521 0.816907 0.117 Uiso 1 1 calc R U . . .
C77 C 1.1612(3) 0.0299(2) 0.84404(15) 0.0953(8) Uani 1 1 d . . . . .
H77 H 1.220402 -0.035170 0.847000 0.114 Uiso 1 1 calc R U . . .
C78 C 1.0203(3) 0.04787(19) 0.85677(12) 0.0748(6) Uani 1 1 d . . . . .
H78 H 0.982466 -0.004946 0.868219 0.090 Uiso 1 1 calc R U . . .
Be1 Be 0.2722(3) 0.66169(16) 0.69629(10) 0.0505(5) Uani 1 1 d . . . . .
Be2 Be 0.4270(3) 0.50530(15) 0.74942(9) 0.0457(5) Uani 1 1 d . . . . .
Be3 Be 0.5841(3) 0.34814(16) 0.80128(10) 0.0464(5) 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 C1 1.264(2) . ?
N1 Be1 1.502(3) . ?
N2 C14 1.280(2) . ?
N2 Be1 1.668(3) . ?
N2 Be2 1.725(2) . ?
N3 C27 1.277(2) . ?
N3 Be1 1.671(3) . ?
N3 Be2 1.723(3) . ?
N4 C40 1.273(2) . ?
N4 Be3 1.674(3) . ?
N4 Be2 1.728(3) . ?
N5 C53 1.270(2) . ?
N5 Be3 1.672(3) . ?
N5 Be2 1.718(3) . ?
N6 C66 1.253(2) . ?
N6 Be3 1.507(3) . ?
C1 C8 1.489(3) . ?
C1 C2 1.505(3) . ?
C2 C3 1.386(3) . ?
C2 C7 1.395(3) . ?
C3 C4 1.396(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.367(4) . ?
C4 H4 0.9500 . ?
C5 C6 1.366(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.384(3) . ?
C6 H6 0.9500 . ?
C7 H7 0.9500 . ?
C8 C9 1.384(3) . ?
C8 C13 1.389(3) . ?
C9 C10 1.374(3) . ?
C9 H9 0.9500 . ?
C10 C11 1.395(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.371(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.381(3) . ?
C12 H12 0.9500 . ?
C13 H13 0.9500 . ?
C14 C21 1.498(2) . ?
C14 C15 1.498(3) . ?
C15 C16 1.391(3) . ?
C15 C20 1.394(3) . ?
C16 C17 1.387(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.384(3) . ?
C17 H17 0.9500 . ?
C18 C19 1.371(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.398(3) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C22 1.389(3) . ?
C21 C26 1.395(3) . ?
C22 C23 1.398(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.371(3) . ?
C23 H23 0.9500 . ?
C24 C25 1.381(3) . ?
C24 H24 0.9500 . ?
C25 C26 1.392(3) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.497(2) . ?
C27 C34 1.499(2) . ?
C28 C29 1.385(2) . ?
C28 C33 1.387(3) . ?
C29 C30 1.389(3) . ?
C29 H29 0.9500 . ?
C30 C31 1.373(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.375(3) . ?
C31 H31 0.9500 . ?
C32 C33 1.392(3) . ?
C32 H32 0.9500 . ?
C33 H33 0.9500 . ?
C34 C35 1.389(2) . ?
C34 C39 1.395(2) . ?
C35 C36 1.385(2) . ?
C35 H35 0.9500 . ?
C36 C37 1.388(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.376(3) . ?
C37 H37 0.9500 . ?
C38 C39 1.386(3) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C47 1.503(2) . ?
C40 C41 1.504(2) . ?
C41 C46 1.387(3) . ?
C41 C42 1.393(3) . ?
C42 C43 1.392(3) . ?
C42 H42 0.9500 . ?
C43 C44 1.376(3) . ?
C43 H43 0.9500 . ?
C44 C45 1.379(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.385(3) . ?
C45 H45 0.9500 . ?
C46 H46 0.9500 . ?
C47 C52 1.391(3) . ?
C47 C48 1.395(2) . ?
C48 C49 1.390(2) . ?
C48 H48 0.9500 . ?
C49 C50 1.380(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.384(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.388(2) . ?
C51 H51 0.9500 . ?
C52 H52 0.9500 . ?
C53 C54 1.501(2) . ?
C53 C60 1.505(2) . ?
C54 C59 1.377(3) . ?
C54 C55 1.389(3) . ?
C55 C56 1.395(3) . ?
C55 H55 0.9500 . ?
C56 C57 1.377(4) . ?
C56 H56 0.9500 . ?
C57 C58 1.354(5) . ?
C57 H57 0.9500 . ?
C58 C59 1.385(4) . ?
C58 H58 0.9500 . ?
C59 H59 0.9500 . ?
C60 C61 1.385(3) . ?
C60 C65 1.393(3) . ?
C61 C62 1.387(3) . ?
C61 H61 0.9500 . ?
C62 C63 1.373(3) . ?
C62 H62 0.9500 . ?
C63 C64 1.385(3) . ?
C63 H63 0.9500 . ?
C64 C65 1.387(3) . ?
C64 H64 0.9500 . ?
C65 H65 0.9500 . ?
C66 C67 1.500(3) . ?
C66 C73 1.502(3) . ?
C67 C68 1.379(3) . ?
C67 C72 1.398(3) . ?
C68 C69 1.381(3) . ?
C68 H68 0.9500 . ?
C69 C70 1.366(4) . ?
C69 H69 0.9500 . ?
C70 C71 1.358(5) . ?
C70 H70 0.9500 . ?
C71 C72 1.402(4) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
C73 C74 1.375(3) . ?
C73 C78 1.399(3) . ?
C74 C75 1.413(4) . ?
C74 H74 0.9500 . ?
C75 C76 1.353(4) . ?
C75 H75 0.9500 . ?
C76 C77 1.368(4) . ?
C76 H76 0.9500 . ?
C77 C78 1.377(4) . ?
C77 H77 0.9500 . ?
C78 H78 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
C1 N1 Be1 175.8(2) . . ?
C14 N2 Be1 138.80(14) . . ?
C14 N2 Be2 133.78(15) . . ?
Be1 N2 Be2 86.73(13) . . ?
C27 N3 Be1 137.56(15) . . ?
C27 N3 Be2 134.80(14) . . ?
Be1 N3 Be2 86.71(13) . . ?
C40 N4 Be3 136.00(15) . . ?
C40 N4 Be2 136.44(13) . . ?
Be3 N4 Be2 86.85(12) . . ?
C53 N5 Be3 135.49(15) . . ?
C53 N5 Be2 136.63(15) . . ?
Be3 N5 Be2 87.26(12) . . ?
C66 N6 Be3 176.7(2) . . ?
N1 C1 C8 120.8(2) . . ?
N1 C1 C2 120.7(2) . . ?
C8 C1 C2 118.42(16) . . ?
C3 C2 C7 118.6(2) . . ?
C3 C2 C1 119.20(18) . . ?
C7 C2 C1 122.23(19) . . ?
C2 C3 C4 119.8(2) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.4(2) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
C6 C5 C4 120.5(3) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C5 C6 C7 119.8(2) . . ?
C5 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C2 120.8(2) . . ?
C6 C7 H7 119.6 . . ?
C2 C7 H7 119.6 . . ?
C9 C8 C13 118.8(2) . . ?
C9 C8 C1 119.88(19) . . ?
C13 C8 C1 121.2(2) . . ?
C10 C9 C8 121.0(2) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 120.0(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C12 C11 C10 119.1(2) . . ?
C12 C11 H11 120.5 . . ?
C10 C11 H11 120.5 . . ?
C11 C12 C13 121.0(2) . . ?
C11 C12 H12 119.5 . . ?
C13 C12 H12 119.5 . . ?
C12 C13 C8 120.1(2) . . ?
C12 C13 H13 120.0 . . ?
C8 C13 H13 120.0 . . ?
N2 C14 C21 122.39(16) . . ?
N2 C14 C15 121.35(14) . . ?
C21 C14 C15 116.26(15) . . ?
C16 C15 C20 118.50(18) . . ?
C16 C15 C14 120.54(16) . . ?
C20 C15 C14 120.96(17) . . ?
C17 C16 C15 121.04(19) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C18 C17 C16 119.8(2) . . ?
C18 C17 H17 120.1 . . ?
C16 C17 H17 120.1 . . ?
C19 C18 C17 120.1(2) . . ?
C19 C18 H18 119.9 . . ?
C17 C18 H18 119.9 . . ?
C18 C19 C20 120.4(2) . . ?
C18 C19 H19 119.8 . . ?
C20 C19 H19 119.8 . . ?
C15 C20 C19 120.16(19) . . ?
C15 C20 H20 119.9 . . ?
C19 C20 H20 119.9 . . ?
C22 C21 C26 119.54(16) . . ?
C22 C21 C14 120.43(18) . . ?
C26 C21 C14 119.98(17) . . ?
C21 C22 C23 120.0(2) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 119.8(2) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 120.95(18) . . ?
C23 C24 H24 119.5 . . ?
C25 C24 H24 119.5 . . ?
C24 C25 C26 119.7(2) . . ?
C24 C25 H25 120.2 . . ?
C26 C25 H25 120.2 . . ?
C25 C26 C21 120.1(2) . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
N3 C27 C28 122.68(15) . . ?
N3 C27 C34 121.50(16) . . ?
C28 C27 C34 115.82(15) . . ?
C29 C28 C33 118.89(18) . . ?
C29 C28 C27 120.30(17) . . ?
C33 C28 C27 120.81(16) . . ?
C28 C29 C30 120.2(2) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C31 C30 C29 120.5(2) . . ?
C31 C30 H30 119.7 . . ?
C29 C30 H30 119.7 . . ?
C30 C31 C32 119.8(2) . . ?
C30 C31 H31 120.1 . . ?
C32 C31 H31 120.1 . . ?
C31 C32 C33 120.0(2) . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C28 C33 C32 120.5(2) . . ?
C28 C33 H33 119.8 . . ?
C32 C33 H33 119.8 . . ?
C35 C34 C39 118.61(16) . . ?
C35 C34 C27 120.94(15) . . ?
C39 C34 C27 120.44(16) . . ?
C36 C35 C34 121.01(17) . . ?
C36 C35 H35 119.5 . . ?
C34 C35 H35 119.5 . . ?
C35 C36 C37 119.70(18) . . ?
C35 C36 H36 120.1 . . ?
C37 C36 H36 120.1 . . ?
C38 C37 C36 119.89(17) . . ?
C38 C37 H37 120.1 . . ?
C36 C37 H37 120.1 . . ?
C37 C38 C39 120.47(18) . . ?
C37 C38 H38 119.8 . . ?
C39 C38 H38 119.8 . . ?
C38 C39 C34 120.32(18) . . ?
C38 C39 H39 119.8 . . ?
C34 C39 H39 119.8 . . ?
N4 C40 C47 121.97(15) . . ?
N4 C40 C41 121.78(14) . . ?
C47 C40 C41 116.24(14) . . ?
C46 C41 C42 119.05(17) . . ?
C46 C41 C40 120.23(16) . . ?
C42 C41 C40 120.67(17) . . ?
C43 C42 C41 120.1(2) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C44 C43 C42 120.2(2) . . ?
C44 C43 H43 119.9 . . ?
C42 C43 H43 119.9 . . ?
C43 C44 C45 119.93(18) . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C44 C45 C46 120.3(2) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C45 C46 C41 120.39(19) . . ?
C45 C46 H46 119.8 . . ?
C41 C46 H46 119.8 . . ?
C52 C47 C48 118.83(16) . . ?
C52 C47 C40 120.94(15) . . ?
C48 C47 C40 120.18(16) . . ?
C49 C48 C47 120.13(18) . . ?
C49 C48 H48 119.9 . . ?
C47 C48 H48 119.9 . . ?
C50 C49 C48 120.39(18) . . ?
C50 C49 H49 119.8 . . ?
C48 C49 H49 119.8 . . ?
C49 C50 C51 120.03(17) . . ?
C49 C50 H50 120.0 . . ?
C51 C50 H50 120.0 . . ?
C50 C51 C52 119.77(19) . . ?
C50 C51 H51 120.1 . . ?
C52 C51 H51 120.1 . . ?
C51 C52 C47 120.85(17) . . ?
C51 C52 H52 119.6 . . ?
C47 C52 H52 119.6 . . ?
N5 C53 C54 121.88(16) . . ?
N5 C53 C60 121.96(15) . . ?
C54 C53 C60 116.11(15) . . ?
C59 C54 C55 119.25(19) . . ?
C59 C54 C53 120.06(19) . . ?
C55 C54 C53 120.50(17) . . ?
C54 C55 C56 119.6(2) . . ?
C54 C55 H55 120.2 . . ?
C56 C55 H55 120.2 . . ?
C57 C56 C55 119.9(3) . . ?
C57 C56 H56 120.0 . . ?
C55 C56 H56 120.0 . . ?
C58 C57 C56 120.5(2) . . ?
C58 C57 H57 119.8 . . ?
C56 C57 H57 119.8 . . ?
C57 C58 C59 120.3(3) . . ?
C57 C58 H58 119.9 . . ?
C59 C58 H58 119.9 . . ?
C54 C59 C58 120.5(3) . . ?
C54 C59 H59 119.7 . . ?
C58 C59 H59 119.7 . . ?
C61 C60 C65 118.28(17) . . ?
C61 C60 C53 120.93(16) . . ?
C65 C60 C53 120.79(16) . . ?
C60 C61 C62 121.31(19) . . ?
C60 C61 H61 119.3 . . ?
C62 C61 H61 119.3 . . ?
C63 C62 C61 120.02(19) . . ?
C63 C62 H62 120.0 . . ?
C61 C62 H62 120.0 . . ?
C62 C63 C64 119.54(18) . . ?
C62 C63 H63 120.2 . . ?
C64 C63 H63 120.2 . . ?
C63 C64 C65 120.49(19) . . ?
C63 C64 H64 119.8 . . ?
C65 C64 H64 119.8 . . ?
C64 C65 C60 120.34(19) . . ?
C64 C65 H65 119.8 . . ?
C60 C65 H65 119.8 . . ?
N6 C66 C67 121.1(2) . . ?
N6 C66 C73 122.01(19) . . ?
C67 C66 C73 116.79(16) . . ?
C68 C67 C72 118.8(2) . . ?
C68 C67 C66 119.19(17) . . ?
C72 C67 C66 122.0(2) . . ?
C67 C68 C69 120.7(2) . . ?
C67 C68 H68 119.6 . . ?
C69 C68 H68 119.6 . . ?
C70 C69 C68 120.1(3) . . ?
C70 C69 H69 119.9 . . ?
C68 C69 H69 119.9 . . ?
C71 C70 C69 120.7(3) . . ?
C71 C70 H70 119.7 . . ?
C69 C70 H70 119.7 . . ?
C70 C71 C72 120.1(2) . . ?
C70 C71 H71 120.0 . . ?
C72 C71 H71 120.0 . . ?
C67 C72 C71 119.5(3) . . ?
C67 C72 H72 120.3 . . ?
C71 C72 H72 120.3 . . ?
C74 C73 C78 118.6(2) . . ?
C74 C73 C66 120.3(2) . . ?
C78 C73 C66 121.0(2) . . ?
C73 C74 C75 120.3(3) . . ?
C73 C74 H74 119.8 . . ?
C75 C74 H74 119.8 . . ?
C76 C75 C74 119.2(3) . . ?
C76 C75 H75 120.4 . . ?
C74 C75 H75 120.4 . . ?
C75 C76 C77 121.5(3) . . ?
C75 C76 H76 119.3 . . ?
C77 C76 H76 119.3 . . ?
C76 C77 C78 119.7(3) . . ?
C76 C77 H77 120.1 . . ?
C78 C77 H77 120.1 . . ?
C77 C78 C73 120.6(3) . . ?
C77 C78 H78 119.7 . . ?
C73 C78 H78 119.7 . . ?
N1 Be1 N2 134.25(18) . . ?
N1 Be1 N3 130.5(2) . . ?
N2 Be1 N3 95.18(13) . . ?
N5 Be2 N3 110.69(14) . . ?
N5 Be2 N2 127.99(16) . . ?
N3 Be2 N2 91.33(12) . . ?
N5 Be2 N4 91.17(12) . . ?
N3 Be2 N4 129.35(16) . . ?
N2 Be2 N4 110.68(14) . . ?
N6 Be3 N5 132.46(17) . . ?
N6 Be3 N4 132.82(17) . . ?
N5 Be3 N4 94.72(13) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 36.0(3) . . . . ?
C8 C1 C2 C3 -142.72(19) . . . . ?
N1 C1 C2 C7 -143.5(2) . . . . ?
C8 C1 C2 C7 37.8(3) . . . . ?
C7 C2 C3 C4 0.1(3) . . . . ?
C1 C2 C3 C4 -179.4(2) . . . . ?
C2 C3 C4 C5 -0.1(4) . . . . ?
C3 C4 C5 C6 0.6(4) . . . . ?
C4 C5 C6 C7 -1.0(4) . . . . ?
C5 C6 C7 C2 1.0(4) . . . . ?
C3 C2 C7 C6 -0.6(3) . . . . ?
C1 C2 C7 C6 178.9(2) . . . . ?
N1 C1 C8 C9 29.8(3) . . . . ?
C2 C1 C8 C9 -151.46(19) . . . . ?
N1 C1 C8 C13 -145.9(2) . . . . ?
C2 C1 C8 C13 32.8(3) . . . . ?
C13 C8 C9 C10 -0.6(3) . . . . ?
C1 C8 C9 C10 -176.44(19) . . . . ?
C8 C9 C10 C11 0.8(4) . . . . ?
C9 C10 C11 C12 0.0(4) . . . . ?
C10 C11 C12 C13 -1.0(4) . . . . ?
C11 C12 C13 C8 1.3(4) . . . . ?
C9 C8 C13 C12 -0.5(3) . . . . ?
C1 C8 C13 C12 175.33(19) . . . . ?
Be1 N2 C14 C21 -2.2(3) . . . . ?
Be2 N2 C14 C21 164.98(17) . . . . ?
Be1 N2 C14 C15 177.89(19) . . . . ?
Be2 N2 C14 C15 -15.0(3) . . . . ?
N2 C14 C15 C16 -45.4(2) . . . . ?
C21 C14 C15 C16 134.63(17) . . . . ?
N2 C14 C15 C20 134.53(18) . . . . ?
C21 C14 C15 C20 -45.4(2) . . . . ?
C20 C15 C16 C17 0.5(3) . . . . ?
C14 C15 C16 C17 -179.53(17) . . . . ?
C15 C16 C17 C18 -0.7(3) . . . . ?
C16 C17 C18 C19 -0.6(3) . . . . ?
C17 C18 C19 C20 2.0(3) . . . . ?
C16 C15 C20 C19 0.9(3) . . . . ?
C14 C15 C20 C19 -179.08(17) . . . . ?
C18 C19 C20 C15 -2.2(3) . . . . ?
N2 C14 C21 C22 140.22(19) . . . . ?
C15 C14 C21 C22 -39.8(2) . . . . ?
N2 C14 C21 C26 -37.3(2) . . . . ?
C15 C14 C21 C26 142.64(17) . . . . ?
C26 C21 C22 C23 0.2(3) . . . . ?
C14 C21 C22 C23 -177.30(17) . . . . ?
C21 C22 C23 C24 -0.9(3) . . . . ?
C22 C23 C24 C25 1.1(3) . . . . ?
C23 C24 C25 C26 -0.6(3) . . . . ?
C24 C25 C26 C21 0.0(3) . . . . ?
C22 C21 C26 C25 0.2(3) . . . . ?
C14 C21 C26 C25 177.73(17) . . . . ?
Be1 N3 C27 C28 -2.9(3) . . . . ?
Be2 N3 C27 C28 162.24(17) . . . . ?
Be1 N3 C27 C34 178.07(19) . . . . ?
Be2 N3 C27 C34 -16.8(3) . . . . ?
N3 C27 C28 C29 -40.3(3) . . . . ?
C34 C27 C28 C29 138.80(17) . . . . ?
N3 C27 C28 C33 140.01(19) . . . . ?
C34 C27 C28 C33 -40.9(2) . . . . ?
C33 C28 C29 C30 -0.6(3) . . . . ?
C27 C28 C29 C30 179.69(17) . . . . ?
C28 C29 C30 C31 0.8(3) . . . . ?
C29 C30 C31 C32 -1.4(3) . . . . ?
C30 C31 C32 C33 1.8(3) . . . . ?
C29 C28 C33 C32 1.0(3) . . . . ?
C27 C28 C33 C32 -179.25(17) . . . . ?
C31 C32 C33 C28 -1.7(3) . . . . ?
N3 C27 C34 C35 -37.0(3) . . . . ?
C28 C27 C34 C35 143.89(18) . . . . ?
N3 C27 C34 C39 141.58(19) . . . . ?
C28 C27 C34 C39 -37.5(2) . . . . ?
C39 C34 C35 C36 -0.6(3) . . . . ?
C27 C34 C35 C36 178.05(18) . . . . ?
C34 C35 C36 C37 0.2(3) . . . . ?
C35 C36 C37 C38 0.0(3) . . . . ?
C36 C37 C38 C39 0.3(3) . . . . ?
C37 C38 C39 C34 -0.6(3) . . . . ?
C35 C34 C39 C38 0.8(3) . . . . ?
C27 C34 C39 C38 -177.86(19) . . . . ?
Be3 N4 C40 C47 179.70(18) . . . . ?
Be2 N4 C40 C47 -13.4(3) . . . . ?
Be3 N4 C40 C41 -1.5(3) . . . . ?
Be2 N4 C40 C41 165.43(18) . . . . ?
N4 C40 C41 C46 -42.0(2) . . . . ?
C47 C40 C41 C46 136.92(16) . . . . ?
N4 C40 C41 C42 135.32(18) . . . . ?
C47 C40 C41 C42 -45.8(2) . . . . ?
C46 C41 C42 C43 1.1(3) . . . . ?
C40 C41 C42 C43 -176.19(16) . . . . ?
C41 C42 C43 C44 -0.8(3) . . . . ?
C42 C43 C44 C45 0.2(3) . . . . ?
C43 C44 C45 C46 0.0(3) . . . . ?
C44 C45 C46 C41 0.3(3) . . . . ?
C42 C41 C46 C45 -0.9(2) . . . . ?
C40 C41 C46 C45 176.45(15) . . . . ?
N4 C40 C47 C52 -34.4(3) . . . . ?
C41 C40 C47 C52 146.74(17) . . . . ?
N4 C40 C47 C48 142.94(18) . . . . ?
C41 C40 C47 C48 -35.9(2) . . . . ?
C52 C47 C48 C49 1.1(3) . . . . ?
C40 C47 C48 C49 -176.30(16) . . . . ?
C47 C48 C49 C50 -0.7(3) . . . . ?
C48 C49 C50 C51 -0.2(3) . . . . ?
C49 C50 C51 C52 0.6(3) . . . . ?
C50 C51 C52 C47 -0.2(3) . . . . ?
C48 C47 C52 C51 -0.7(3) . . . . ?
C40 C47 C52 C51 176.69(16) . . . . ?
Be3 N5 C53 C54 0.1(3) . . . . ?
Be2 N5 C53 C54 168.05(18) . . . . ?
Be3 N5 C53 C60 177.35(19) . . . . ?
Be2 N5 C53 C60 -14.7(3) . . . . ?
N5 C53 C54 C59 127.7(2) . . . . ?
C60 C53 C54 C59 -49.7(3) . . . . ?
N5 C53 C54 C55 -47.3(3) . . . . ?
C60 C53 C54 C55 135.34(19) . . . . ?
C59 C54 C55 C56 0.6(3) . . . . ?
C53 C54 C55 C56 175.62(18) . . . . ?
C54 C55 C56 C57 -0.8(3) . . . . ?
C55 C56 C57 C58 0.5(4) . . . . ?
C56 C57 C58 C59 0.0(4) . . . . ?
C55 C54 C59 C58 -0.2(3) . . . . ?
C53 C54 C59 C58 -175.2(2) . . . . ?
C57 C58 C59 C54 -0.1(4) . . . . ?
N5 C53 C60 C61 -40.7(3) . . . . ?
C54 C53 C60 C61 136.65(19) . . . . ?
N5 C53 C60 C65 139.3(2) . . . . ?
C54 C53 C60 C65 -43.3(3) . . . . ?
C65 C60 C61 C62 1.5(3) . . . . ?
C53 C60 C61 C62 -178.50(19) . . . . ?
C60 C61 C62 C63 -1.4(3) . . . . ?
C61 C62 C63 C64 -0.1(3) . . . . ?
C62 C63 C64 C65 1.4(3) . . . . ?
C63 C64 C65 C60 -1.3(3) . . . . ?
C61 C60 C65 C64 -0.1(3) . . . . ?
C53 C60 C65 C64 179.86(18) . . . . ?
N6 C66 C67 C68 40.0(3) . . . . ?
C73 C66 C67 C68 -136.0(2) . . . . ?
N6 C66 C67 C72 -138.3(2) . . . . ?
C73 C66 C67 C72 45.7(3) . . . . ?
C72 C67 C68 C69 -0.3(3) . . . . ?
C66 C67 C68 C69 -178.6(2) . . . . ?
C67 C68 C69 C70 1.6(4) . . . . ?
C68 C69 C70 C71 -2.7(5) . . . . ?
C69 C70 C71 C72 2.4(5) . . . . ?
C68 C67 C72 C71 0.0(3) . . . . ?
C66 C67 C72 C71 178.3(2) . . . . ?
C70 C71 C72 C67 -1.0(4) . . . . ?
N6 C66 C73 C74 29.0(3) . . . . ?
C67 C66 C73 C74 -155.01(19) . . . . ?
N6 C66 C73 C78 -148.0(2) . . . . ?
C67 C66 C73 C78 28.0(3) . . . . ?
C78 C73 C74 C75 2.2(3) . . . . ?
C66 C73 C74 C75 -174.94(19) . . . . ?
C73 C74 C75 C76 -0.3(4) . . . . ?
C74 C75 C76 C77 -2.0(4) . . . . ?
C75 C76 C77 C78 2.4(5) . . . . ?
C76 C77 C78 C73 -0.5(4) . . . . ?
C74 C73 C78 C77 -1.8(3) . . . . ?
C66 C73 C78 C77 175.3(2) . . . . ?
C14 N2 Be1 N1 -5.4(4) . . . . ?
Be2 N2 Be1 N1 -176.2(3) . . . . ?
C14 N2 Be1 N3 172.2(2) . . . . ?
Be2 N2 Be1 N3 1.50(13) . . . . ?
C27 N3 Be1 N1 -14.2(4) . . . . ?
Be2 N3 Be1 N1 176.3(2) . . . . ?
C27 N3 Be1 N2 168.0(2) . . . . ?
Be2 N3 Be1 N2 -1.50(13) . . . . ?
C53 N5 Be2 N3 -37.8(3) . . . . ?
Be3 N5 Be2 N3 133.79(15) . . . . ?
C53 N5 Be2 N2 71.3(3) . . . . ?
Be3 N5 Be2 N2 -117.2(2) . . . . ?
C53 N5 Be2 N4 -171.0(2) . . . . ?
Be3 N5 Be2 N4 0.51(13) . . . . ?
C27 N3 Be2 N5 -36.7(3) . . . . ?
Be1 N3 Be2 N5 133.27(15) . . . . ?
C27 N3 Be2 N2 -168.57(18) . . . . ?
Be1 N3 Be2 N2 1.45(13) . . . . ?
C27 N3 Be2 N4 73.0(3) . . . . ?
Be1 N3 Be2 N4 -116.98(18) . . . . ?
C14 N2 Be2 N5 69.2(3) . . . . ?
Be1 N2 Be2 N5 -119.3(2) . . . . ?
C14 N2 Be2 N3 -173.00(18) . . . . ?
Be1 N2 Be2 N3 -1.45(13) . . . . ?
C14 N2 Be2 N4 -39.6(3) . . . . ?
Be1 N2 Be2 N4 131.92(16) . . . . ?
C40 N4 Be2 N5 -171.45(19) . . . . ?
Be3 N4 Be2 N5 -0.51(13) . . . . ?
C40 N4 Be2 N3 70.3(3) . . . . ?
Be3 N4 Be2 N3 -118.79(18) . . . . ?
C40 N4 Be2 N2 -39.7(3) . . . . ?
Be3 N4 Be2 N2 131.23(16) . . . . ?
C53 N5 Be3 N6 -8.4(4) . . . . ?
Be2 N5 Be3 N6 179.9(2) . . . . ?
C53 N5 Be3 N4 171.2(2) . . . . ?
Be2 N5 Be3 N4 -0.53(14) . . . . ?
C40 N4 Be3 N6 -8.9(4) . . . . ?
Be2 N4 Be3 N6 -179.9(2) . . . . ?
C40 N4 Be3 N5 171.54(19) . . . . ?
Be2 N4 Be3 N5 0.52(14) . . . . ?

_refine_diff_density_max         0.315
_refine_diff_density_min         -0.236
_refine_diff_density_rms         0.040



# start Validation Reply Form
_vrf_PLAT230_LTH435              
;
PROBLEM: Hirshfeld Test Diff for    C4       --C5       .        5.3 s.u.
RESPONSE: No other atoms are chemically possible at these positions.
;
_vrf_PLAT906_LTH435              
;
PROBLEM: Large K Value in the Analysis of Variance ......      2.877 Check
RESPONSE: Likely due to weakly diffracting crystal and due to possible
very minor disorder of phenyl rings.
;
_vrf_PLAT911_LTH435              
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600         93 Report
RESPONSE: A few reflections could be collected using the selected measurement
strategy and the instrument.
;
# end Validation Reply Form
