#------------------------------------------------------------------------------
#$Date: 2021-06-05 22:01:18 +0300 (Sat, 05 Jun 2021) $
#$Revision: 266105 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/72/7707224.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7707224
loop_
_publ_author_name
'Buchner, Magnus R.'
'Müller, Matthias'
_publ_section_title
;
 Ethylenediamine complexes of the beryllium halides and pseudo-halides.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7246
_journal_page_last               7255
_journal_paper_doi               10.1039/d1dt01154e
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         '[Be3(OH)3(en)3][NH3C2H4NH2](SCN)4'
_chemical_formula_sum            'C12 H36 Be3 N12 O3 S4'
_chemical_formula_weight         551.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-04-07 deposited with the CCDC.	2021-04-27 downloaded from the CCDC.
;
_cell_angle_alpha                104.350(2)
_cell_angle_beta                 109.886(2)
_cell_angle_gamma                97.482(2)
_cell_formula_units_Z            2
_cell_length_a                   10.5372(3)
_cell_length_b                   11.0027(3)
_cell_length_c                   13.3669(3)
_cell_measurement_reflns_used    28243
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      159.45
_cell_measurement_theta_min      8.54
_cell_volume                     1372.15(7)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25752
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.056
_diffrn_reflns_theta_min         3.703
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    3.501
_exptl_absorpt_correction_T_max  0.9827
_exptl_absorpt_correction_T_min  0.2291
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(μ₂-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.275
_refine_diff_density_min         -0.284
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0307
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0409P)²+0.5787P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4827
_reflns_number_total             5678
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1dt01154e2.cif
_cod_data_source_block           2_CCDC2
_cod_depositor_comments
'Adding full bibliography for 7707219--7707225.cif.'
_cod_database_code               7707224
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S -0.12505(4) 0.67621(4) 0.35405(3) 0.02356(9) Uani 1 1 d . . . . .
S2 S 0.22199(5) 1.08312(4) 1.09037(3) 0.02461(10) Uani 1 1 d . . . . .
S3 S 0.28406(4) 0.34043(4) 0.96066(3) 0.02518(10) Uani 1 1 d . . . . .
S4 S 0.62140(4) -0.28328(4) 0.52753(4) 0.02665(10) Uani 1 1 d . . . . .
O1 O 0.65626(12) 0.35089(10) 0.76567(9) 0.0174(2) Uani 1 1 d . . . . .
O2 O 0.72036(11) 0.13408(10) 0.78182(9) 0.0191(2) Uani 1 1 d . . . . .
O3 O 0.88812(12) 0.30487(10) 0.75455(9) 0.0178(2) Uani 1 1 d . . . . .
N1 N 0.56163(14) 0.22380(12) 0.89714(11) 0.0180(3) Uani 1 1 d . . . . .
N2 N 0.43999(14) 0.12763(13) 0.68055(11) 0.0186(3) Uani 1 1 d . . . . .
N3 N 0.88857(15) 0.56231(12) 0.84503(11) 0.0201(3) Uani 1 1 d . . . . .
N4 N 0.76172(14) 0.45289(13) 0.62785(11) 0.0188(3) Uani 1 1 d . . . . .
N5 N 0.80133(15) 0.05239(13) 0.60445(11) 0.0214(3) Uani 1 1 d . . . . .
N6 N 0.98345(14) 0.09101(12) 0.80600(11) 0.0187(3) Uani 1 1 d . . . . .
N7 N 0.26743(14) 0.68362(13) 0.75763(11) 0.0214(3) Uani 1 1 d . . . . .
H7B H 0.213785 0.673413 0.685128 0.032 Uiso 1 1 calc R U . . .
H7C H 0.247845 0.747487 0.803897 0.032 Uiso 1 1 calc R U . . .
H7D H 0.249451 0.608495 0.772748 0.032 Uiso 1 1 calc R U . . .
N8 N 0.46608(15) 0.50064(13) 0.77563(13) 0.0226(3) Uani 1 1 d . . . . .
N9 N 0.10302(18) 0.7007(2) 0.54806(13) 0.0414(4) Uani 1 1 d . . . . .
N10 N 0.23529(16) 0.88887(14) 0.91548(12) 0.0280(3) Uani 1 1 d . . . . .
N11 N 0.20093(16) 0.55854(13) 0.91022(12) 0.0273(3) Uani 1 1 d . . . . .
N12 N 0.42190(17) -0.14720(14) 0.55671(13) 0.0312(3) Uani 1 1 d . . . . .
C1 C 0.45198(17) 0.10386(14) 0.85842(13) 0.0206(3) Uani 1 1 d . . . . .
H1A H 0.402198 0.108020 0.909599 0.025 Uiso 1 1 calc R U . . .
H1AB H 0.493093 0.027771 0.855813 0.025 Uiso 1 1 calc R U . . .
C2 C 0.35339(16) 0.09480(15) 0.74195(13) 0.0218(3) Uani 1 1 d . . . . .
H2A H 0.293843 0.006357 0.702587 0.026 Uiso 1 1 calc R U . . .
H2AB H 0.292961 0.155920 0.746896 0.026 Uiso 1 1 calc R U . . .
C3 C 0.89016(17) 0.64971(14) 0.77611(14) 0.0224(3) Uani 1 1 d . . . . .
H3A H 0.977759 0.717473 0.812168 0.027 Uiso 1 1 calc R U . . .
H3AB H 0.811405 0.691943 0.767687 0.027 Uiso 1 1 calc R U . . .
C4 C 0.87797(17) 0.56662(14) 0.66277(14) 0.0218(3) Uani 1 1 d . . . . .
H4A H 0.857777 0.614870 0.607956 0.026 Uiso 1 1 calc R U . . .
H4AB H 0.965326 0.539182 0.668537 0.026 Uiso 1 1 calc R U . . .
C5 C 0.92163(18) -0.00524(15) 0.60743(13) 0.0231(3) Uani 1 1 d . . . . .
H5A H 0.994749 0.054729 0.600782 0.028 Uiso 1 1 calc R U . . .
H5AB H 0.892736 -0.087190 0.545351 0.028 Uiso 1 1 calc R U . . .
C6 C 0.97455(18) -0.02931(15) 0.72010(14) 0.0227(3) Uani 1 1 d . . . . .
H6A H 0.909918 -0.103109 0.720178 0.027 Uiso 1 1 calc R U . . .
H6AB H 1.067084 -0.049022 0.735918 0.027 Uiso 1 1 calc R U . . .
C7 C 0.41628(17) 0.71866(15) 0.77575(14) 0.0232(3) Uani 1 1 d . . . . .
H7A H 0.472788 0.753748 0.857215 0.028 Uiso 1 1 calc R U . . .
H7AB H 0.430492 0.787320 0.742110 0.028 Uiso 1 1 calc R U . . .
C8 C 0.46635(19) 0.60427(16) 0.72503(14) 0.0251(3) Uani 1 1 d . . . . .
H8A H 0.406829 0.567741 0.644217 0.030 Uiso 1 1 calc R U . . .
H8AB H 0.562056 0.636056 0.731570 0.030 Uiso 1 1 calc R U . . .
C9 C 0.00702(18) 0.68995(16) 0.46907(14) 0.0240(3) Uani 1 1 d . . . . .
C10 C 0.22846(16) 0.96876(15) 0.98734(13) 0.0205(3) Uani 1 1 d . . . . .
C11 C 0.23669(16) 0.46879(14) 0.93114(12) 0.0197(3) Uani 1 1 d . . . . .
C12 C 0.50446(17) -0.20418(14) 0.54526(13) 0.0217(3) Uani 1 1 d . . . . .
Be1 Be 0.6080(2) 0.21770(18) 0.78092(16) 0.0164(4) Uani 1 1 d . . . . .
Be2 Be 0.8437(2) 0.15682(18) 0.74238(16) 0.0167(4) Uani 1 1 d . . . . .
Be3 Be 0.7916(2) 0.40518(17) 0.75118(16) 0.0166(4) Uani 1 1 d . . . . .
H1 H 0.529(2) 0.294(2) 0.9176(18) 0.033(6) Uiso 1 1 d . . . . .
H2 H 0.634(2) 0.227(2) 0.9600(19) 0.035(6) Uiso 1 1 d . . . . .
H3 H 0.400(2) 0.1700(19) 0.6356(16) 0.023(5) Uiso 1 1 d . . . . .
H4 H 0.447(2) 0.059(2) 0.6439(18) 0.031(6) Uiso 1 1 d . . . . .
H5 H 0.856(2) 0.596(2) 0.8968(17) 0.028(5) Uiso 1 1 d . . . . .
H6 H 0.975(3) 0.559(2) 0.8797(19) 0.035(6) Uiso 1 1 d . . . . .
H7 H 0.677(2) 0.476(2) 0.6019(17) 0.031(5) Uiso 1 1 d . . . . .
H8 H 0.764(2) 0.396(2) 0.5720(18) 0.030(5) Uiso 1 1 d . . . . .
H9 H 0.729(2) -0.007(2) 0.5858(18) 0.033(6) Uiso 1 1 d . . . . .
H10 H 0.782(3) 0.091(2) 0.550(2) 0.048(7) Uiso 1 1 d . . . . .
H11 H 1.064(2) 0.144(2) 0.8272(18) 0.034(6) Uiso 1 1 d . . . . .
H12 H 0.982(2) 0.068(2) 0.8653(19) 0.035(6) Uiso 1 1 d . . . . .
H13 H 0.604(3) 0.391(2) 0.763(2) 0.042(7) Uiso 1 1 d . . . . .
H14 H 0.715(2) 0.077(2) 0.8028(18) 0.030(6) Uiso 1 1 d . . . . .
H15 H 0.952(3) 0.322(2) 0.742(2) 0.041(7) Uiso 1 1 d . . . . .
H16 H 0.500(3) 0.531(2) 0.848(2) 0.043(7) Uiso 1 1 d . . . . .
H17 H 0.386(2) 0.455(2) 0.7509(18) 0.030(5) Uiso 1 1 d . . . . .
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'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
Be3 O1 Be1 129.38(12) . . ?
Be2 O2 Be1 127.00(12) . . ?
Be2 O3 Be3 126.38(12) . . ?
C1 N1 Be1 104.09(11) . . ?
C2 N2 Be1 108.25(11) . . ?
C3 N3 Be3 107.49(11) . . ?
C4 N4 Be3 104.29(12) . . ?
C5 N5 Be2 106.82(12) . . ?
C6 N6 Be2 106.80(12) . . ?
N1 C1 C2 106.16(12) . . ?
N2 C2 C1 107.18(12) . . ?
N3 C3 C4 106.81(12) . . ?
N4 C4 C3 105.84(12) . . ?
N5 C5 C6 105.61(13) . . ?
N6 C6 C5 106.76(12) . . ?
N7 C7 C8 112.57(13) . . ?
N8 C8 C7 115.27(14) . . ?
N9 C9 S1 177.52(17) . . ?
N10 C10 S2 178.91(16) . . ?
N11 C11 S3 178.79(15) . . ?
N12 C12 S4 178.97(15) . . ?
O1 Be1 O2 110.69(13) . . ?
O1 Be1 N1 116.52(12) . . ?
O2 Be1 N1 109.95(12) . . ?
O1 Be1 N2 113.74(12) . . ?
O2 Be1 N2 110.96(12) . . ?
N1 Be1 N2 93.96(11) . . ?
O2 Be2 O3 110.00(13) . . ?
O2 Be2 N6 113.19(12) . . ?
O3 Be2 N6 114.15(13) . . ?
O2 Be2 N5 111.16(13) . . ?
O3 Be2 N5 113.05(12) . . ?
N6 Be2 N5 94.56(11) . . ?
O1 Be3 O3 110.99(12) . . ?
O1 Be3 N3 115.43(13) . . ?
O3 Be3 N3 110.96(13) . . ?
O1 Be3 N4 114.41(13) . . ?
O3 Be3 N4 109.85(12) . . ?
N3 Be3 N4 94.13(10) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C9 1.6425(17) . ?
S2 C10 1.6467(17) . ?
S3 C11 1.6508(16) . ?
S4 C12 1.6456(18) . ?
O1 Be3 1.566(2) . ?
O1 Be1 1.572(2) . ?
O2 Be2 1.574(2) . ?
O2 Be1 1.590(2) . ?
O3 Be2 1.587(2) . ?
O3 Be3 1.594(2) . ?
N1 C1 1.4838(18) . ?
N1 Be1 1.769(2) . ?
N2 C2 1.486(2) . ?
N2 Be1 1.784(2) . ?
N3 C3 1.4897(19) . ?
N3 Be3 1.789(2) . ?
N4 C4 1.4854(19) . ?
N4 Be3 1.792(2) . ?
N5 C5 1.483(2) . ?
N5 Be2 1.782(2) . ?
N6 C6 1.490(2) . ?
N6 Be2 1.774(2) . ?
N7 C7 1.485(2) . ?
N8 C8 1.463(2) . ?
N9 C9 1.154(2) . ?
N10 C10 1.160(2) . ?
N11 C11 1.165(2) . ?
N12 C12 1.165(2) . ?
C1 C2 1.519(2) . ?
C3 C4 1.516(2) . ?
C5 C6 1.521(2) . ?
C7 C8 1.522(2) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N7 H7B N9 0.91 1.93 2.816(2) 164.5 . yes
N7 H7C N10 0.91 1.92 2.827(2) 171.5 . yes
N7 H7D N11 0.91 2.24 2.943(2) 133.9 . yes
C1 H1A S3 0.99 3.02 3.5854(17) 117.7 . yes
C2 H2AB S1 0.99 2.97 3.8554(17) 149.3 2_566 yes
C3 H3AB S2 0.99 2.86 3.6003(16) 131.8 2_677 yes
C4 H4A S4 0.99 2.85 3.5527(17) 128.7 1_565 yes
C5 H5A S1 0.99 2.92 3.7775(16) 146.0 2_666 yes
N1 H1 S3 0.90(2) 2.91(2) 3.6124(15) 135.9(17) . yes
N1 H2 N10 0.91(2) 2.50(2) 3.312(2) 148.6(18) 2_667 yes
N1 H2 N11 0.91(2) 2.54(2) 3.1025(19) 120.6(17) 2_667 yes
N2 H3 S4 0.88(2) 2.73(2) 3.5374(14) 153.6(17) 2_656 yes
N2 H4 N12 0.82(2) 2.22(2) 3.012(2) 165(2) . yes
N3 H5 S3 0.90(2) 2.79(2) 3.6801(15) 170.0(17) 2_667 yes
N3 H6 N11 0.88(2) 2.28(2) 3.114(2) 159(2) 1_655 yes
N4 H8 N9 0.86(2) 2.60(2) 3.370(2) 150.4(19) 2_666 yes
N5 H9 S4 0.85(2) 2.91(2) 3.6415(14) 144.7(19) . yes
N5 H10 N12 0.90(3) 2.40(3) 3.093(2) 134(2) 2_656 yes
N6 H11 S3 0.87(2) 2.69(2) 3.5082(14) 157.6(19) 1_655 yes
N6 H12 S2 0.89(2) 2.85(2) 3.5427(14) 134.9(18) 2_667 yes
O1 H13 N8 0.74(3) 2.03(3) 2.7715(18) 173(3) . yes
O2 H14 S2 0.75(2) 2.55(2) 3.2702(11) 162(2) 2_667 yes
O3 H15 S1 0.75(2) 2.57(2) 3.2959(12) 162(2) 2_666 yes
N8 H16 S3 0.86(3) 2.67(3) 3.4420(16) 149(2) 2_667 yes
N8 H17 S1 0.84(2) 2.63(2) 3.4604(15) 171.1(19) 2_566 yes
