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#$Date: 2023-09-14 01:51:06 +0300 (Thu, 14 Sep 2023) $
#$Revision: 286328 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/39/7713949.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_7713949
loop_
_publ_author_name
'Berthold, Chantsalmaa'
'Müller, Matthias'
'Ivlev, Sergei'
'Andrada, Diego M.'
'Buchner, Magnus Richard'
_publ_section_title
;
 Gauging ambiphilicity of pseudo-halides via beryllium-trispyrazolylborato
 compounds
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02857G
_journal_year                    2023
_chemical_formula_moiety         'C6 H12 Be N2 S4'
_chemical_formula_sum            'C6 H12 Be N2 S4'
_chemical_formula_weight         249.43
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-06-22 deposited with the CCDC.	2023-09-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.362(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.4275(3)
_cell_length_b                   14.7872(5)
_cell_length_c                   10.3424(4)
_cell_measurement_reflns_used    16639
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      149.73
_cell_measurement_theta_min      10.61
_cell_volume                     1258.98(8)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20425
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.862
_diffrn_reflns_theta_min         5.303
_diffrn_source                   'GeniX 3D HF Cu'
_exptl_absorpt_coefficient_mu    6.605
_exptl_absorpt_correction_T_max  0.4499
_exptl_absorpt_correction_T_min  0.0680
_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    1.316
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.085
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0594P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2130
_reflns_number_total             2564
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt02857g2.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7713949
_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
S1 S 0.83134(7) 0.49614(4) 0.85287(5) 0.03213(16) Uani 1 1 d . . . . .
S2 S 1.05019(7) 0.80553(4) 0.38953(5) 0.03245(16) Uani 1 1 d . . . . .
S3 S 0.45544(6) 0.67100(3) 0.41914(5) 0.02414(14) Uani 1 1 d . . . . .
S4 S 0.64644(6) 0.48916(4) 0.31936(5) 0.02478(14) Uani 1 1 d . . . . .
N1 N 0.7337(2) 0.56594(12) 0.59891(16) 0.0247(4) Uani 1 1 d . . . . .
N2 N 0.8220(2) 0.67491(13) 0.40857(17) 0.0290(4) Uani 1 1 d . . . . .
C1 C 0.7731(2) 0.53613(14) 0.70537(19) 0.0220(4) Uani 1 1 d . . . . .
C2 C 0.9166(3) 0.72851(15) 0.39999(18) 0.0255(4) Uani 1 1 d . . . . .
C3 C 0.5105(3) 0.77034(19) 0.5204(3) 0.0390(6) Uani 1 1 d . . . . .
C4 C 0.4268(3) 0.71997(18) 0.2564(2) 0.0334(5) Uani 1 1 d . . . . .
C5 C 0.6828(4) 0.5265(2) 0.1623(2) 0.0390(6) Uani 1 1 d . . . . .
C6 C 0.8270(3) 0.4236(2) 0.3785(3) 0.0396(6) Uani 1 1 d . . . . .
Be1 Be 0.6897(3) 0.60451(19) 0.4478(3) 0.0245(5) Uani 1 1 d . . . . .
H3A H 0.524(3) 0.748(2) 0.610(3) 0.049(8) Uiso 1 1 d . . . . .
H3B H 0.619(4) 0.798(2) 0.501(3) 0.065(10) Uiso 1 1 d . . . . .
H3C H 0.434(4) 0.810(2) 0.513(3) 0.057(9) Uiso 1 1 d . . . . .
H4A H 0.356(3) 0.766(2) 0.250(3) 0.041(7) Uiso 1 1 d . . . . .
H4B H 0.388(4) 0.671(2) 0.194(3) 0.057(9) Uiso 1 1 d . . . . .
H4C H 0.532(4) 0.743(2) 0.244(3) 0.048(8) Uiso 1 1 d . . . . .
H5A H 0.594(4) 0.567(2) 0.128(3) 0.061(10) Uiso 1 1 d . . . . .
H5B H 0.690(3) 0.474(2) 0.109(3) 0.044(8) Uiso 1 1 d . . . . .
H5C H 0.779(4) 0.556(2) 0.171(3) 0.045(8) Uiso 1 1 d . . . . .
H6A H 0.821(4) 0.365(2) 0.323(3) 0.066(10) Uiso 1 1 d . . . . .
H6B H 0.917(4) 0.463(2) 0.378(3) 0.060(10) Uiso 1 1 d . . . . .
H6C H 0.828(4) 0.406(2) 0.472(3) 0.059(9) 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'
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
C4 S3 C3 100.44(13) . . ?
C4 S3 Be1 104.24(11) . . ?
C3 S3 Be1 100.14(11) . . ?
C6 S4 C5 100.19(13) . . ?
C6 S4 Be1 101.47(12) . . ?
C5 S4 Be1 105.97(12) . . ?
C1 N1 Be1 176.1(2) . . ?
C2 N2 Be1 169.8(2) . . ?
N1 C1 S1 178.76(19) . . ?
N2 C2 S2 179.1(2) . . ?
N1 Be1 N2 115.64(18) . . ?
N1 Be1 S4 106.81(15) . . ?
N2 Be1 S4 112.73(15) . . ?
N1 Be1 S3 107.64(14) . . ?
N2 Be1 S3 109.02(16) . . ?
S4 Be1 S3 104.29(11) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
S1 C1 1.611(2) . ?
S2 C2 1.621(2) . ?
S3 C4 1.800(2) . ?
S3 C3 1.806(3) . ?
S3 Be1 2.168(3) . ?
S4 C6 1.798(2) . ?
S4 C5 1.803(2) . ?
S4 Be1 2.145(3) . ?
N1 C1 1.166(3) . ?
N1 Be1 1.630(3) . ?
N2 C2 1.141(3) . ?
N2 Be1 1.638(3) . ?
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
C3 H3A S2 0.97(3) 2.96(3) 3.924(3) 175(2) 4_576 yes
