#------------------------------------------------------------------------------
#$Date: 2025-08-21 00:01:10 +0200 (Thu 21 de Aug de 2025) $
#$Revision: 301838 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/98/4329867.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_4329867
loop_
_publ_author_name
'Alasdair P. M. Robertson'
'Mairi F. Haddow'
'Ian Manners'
_publ_section_title
;
 Synthesis and the Thermal and Catalytic Dehydrogenation Reactions of
 Amine-Thioboranes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8254
_journal_page_last               8264
_journal_paper_doi               10.1021/ic3008188
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C2 H12 B N2, C6 F5 S'
_chemical_formula_sum            'C16 H24 B2 F10 N4 S2'
_chemical_formula_weight         548.13
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.932(3)
_cell_length_b                   9.0064(19)
_cell_length_c                   24.933(5)
_cell_measurement_reflns_used    4853
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.48
_cell_volume                     2454.9(10)
_computing_cell_refinement       'Bruker Apex II'
_computing_data_collection       'Bruker Apex II'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker ShelXTL'
_computing_publication_material  'Bruker ShelXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_av_sigmaI/netI    0.0552
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            17215
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.305
_exptl_absorpt_correction_T_max  0.9422
_exptl_absorpt_correction_T_min  0.6872
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.600
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0721
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0786P)²+5.2189P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1781
_refine_ls_wR_factor_ref         0.1906
_reflns_number_gt                2056
_reflns_number_total             2819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3008188_si_002_12.cif
_cod_data_source_block           '[(Me2NH2)BH2][SC6F5]'
_cod_original_cell_volume        2455.0(9)
_cod_database_code               4329867
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C -0.0112(3) 1.0075(4) 0.38178(14) 0.0192(7) Uani 1 1 d .
C2 C -0.0399(3) 0.9018(4) 0.42002(15) 0.0213(8) Uani 1 1 d .
C3 C 0.0376(4) 0.8590(5) 0.46049(15) 0.0288(9) Uani 1 1 d .
C4 C 0.1512(4) 0.9242(5) 0.46429(17) 0.0341(10) Uani 1 1 d .
C5 C 0.1831(3) 1.0309(5) 0.42819(19) 0.0346(11) Uani 1 1 d .
C6 C 0.1042(3) 1.0713(4) 0.38776(17) 0.0261(8) Uani 1 1 d .
F1 F -0.15077(19) 0.8352(2) 0.41858(9) 0.0278(5) Uani 1 1 d .
F2 F 0.0040(2) 0.7553(3) 0.49613(10) 0.0406(7) Uani 1 1 d .
F3 F 0.2277(3) 0.8831(3) 0.50374(12) 0.0542(8) Uani 1 1 d .
F4 F 0.2936(2) 1.0974(3) 0.43168(14) 0.0554(9) Uani 1 1 d .
F5 F 0.1404(2) 1.1769(3) 0.35292(11) 0.0405(7) Uani 1 1 d .
S1 S -0.11142(8) 1.05602(10) 0.33010(3) 0.0198(2) Uani 1 1 d .
B1 B 0.9650(4) 0.4811(5) 0.30811(18) 0.0235(9) Uani 1 1 d .
H1 H 0.933(4) 0.596(4) 0.2967(14) 0.018(10) Uiso 1 1 d .
H2 H 1.065(4) 0.475(5) 0.3215(15) 0.027(11) Uiso 1 1 d .
C7 C 0.8312(4) 0.3551(4) 0.23388(15) 0.0277(9) Uani 1 1 d .
H7A H 0.7727 0.3155 0.2600 0.042 Uiso 1 1 calc R
H7B H 0.8369 0.2875 0.2032 0.042 Uiso 1 1 calc R
H7C H 0.8036 0.4529 0.2216 0.042 Uiso 1 1 calc R
C8 C 0.9273(4) 0.4679(5) 0.40926(15) 0.0293(9) Uani 1 1 d .
H8A H 1.0100 0.4305 0.4160 0.044 Uiso 1 1 calc R
H8B H 0.8717 0.4301 0.4369 0.044 Uiso 1 1 calc R
H8C H 0.9278 0.5767 0.4103 0.044 Uiso 1 1 calc R
N1 N 0.9535(3) 0.3696(4) 0.25955(13) 0.0209(7) Uani 1 1 d .
H1A H 1.006(4) 0.411(5) 0.2337(16) 0.025 Uiso 1 1 d .
H1B H 0.970(4) 0.273(5) 0.2682(16) 0.025 Uiso 1 1 d .
N2 N 0.8853(3) 0.4173(3) 0.35579(12) 0.0173(6) Uani 1 1 d .
H2A H 0.804(4) 0.449(4) 0.3487(15) 0.021 Uiso 1 1 d .
H2B H 0.886(4) 0.315(5) 0.3553(15) 0.021 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 0.0033 0.0016 '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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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
C2 C1 C6 114.5(3)
C2 C1 S1 122.6(3)
C6 C1 S1 122.9(3)
F1 C2 C3 116.6(3)
F1 C2 C1 119.3(3)
C3 C2 C1 124.1(4)
F2 C3 C2 120.9(4)
F2 C3 C4 119.9(4)
C2 C3 C4 119.2(4)
F3 C4 C5 121.2(4)
F3 C4 C3 119.7(4)
C5 C4 C3 119.1(4)
F4 C5 C4 119.9(4)
F4 C5 C6 119.4(4)
C4 C5 C6 120.7(4)
F5 C6 C5 118.3(4)
F5 C6 C1 119.2(4)
C5 C6 C1 122.5(4)
N1 B1 N2 107.5(3)
N1 B1 H1 111.3(19)
N2 B1 H1 110(2)
N1 B1 H2 106(2)
N2 B1 H2 107(2)
H1 B1 H2 115(3)
N1 C7 H7A 109.5
N1 C7 H7B 109.5
H7A C7 H7B 109.5
N1 C7 H7C 109.5
H7A C7 H7C 109.5
H7B C7 H7C 109.5
N2 C8 H8A 109.5
N2 C8 H8B 109.5
H8A C8 H8B 109.5
N2 C8 H8C 109.5
H8A C8 H8C 109.5
H8B C8 H8C 109.5
C7 N1 B1 117.2(3)
C7 N1 H1A 107(3)
B1 N1 H1A 103(2)
C7 N1 H1B 101(3)
B1 N1 H1B 114(3)
H1A N1 H1B 115(4)
C8 N2 B1 113.2(3)
C8 N2 H2A 111(2)
B1 N2 H2A 105(2)
C8 N2 H2B 109(2)
B1 N2 H2B 111(2)
H2A N2 H2B 108(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C2 1.384(5)
C1 C6 1.394(5)
C1 S1 1.747(4)
C2 F1 1.353(4)
C2 C3 1.373(5)
C3 F2 1.341(5)
C3 C4 1.377(6)
C4 F3 1.343(4)
C4 C5 1.362(7)
C5 F4 1.351(5)
C5 C6 1.376(6)
C6 F5 1.347(5)
B1 N1 1.578(5)
B1 N2 1.582(5)
B1 H1 1.13(4)
B1 H2 1.14(4)
C7 N1 1.488(5)
C7 H7A 0.9800
C7 H7B 0.9800
C7 H7C 0.9800
C8 N2 1.482(5)
C8 H8A 0.9800
C8 H8B 0.9800
C8 H8C 0.9800
N1 H1A 0.94(4)
N1 H1B 0.91(4)
N2 H2A 0.95(4)
N2 H2B 0.92(4)
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
C6 C1 C2 F1 178.6(3)
S1 C1 C2 F1 -1.8(5)
C6 C1 C2 C3 -1.0(5)
S1 C1 C2 C3 178.7(3)
F1 C2 C3 F2 0.6(5)
C1 C2 C3 F2 -179.8(3)
F1 C2 C3 C4 -179.3(3)
C1 C2 C3 C4 0.3(6)
F2 C3 C4 F3 0.1(6)
C2 C3 C4 F3 -180.0(3)
F2 C3 C4 C5 -179.0(4)
C2 C3 C4 C5 0.9(6)
F3 C4 C5 F4 0.1(6)
C3 C4 C5 F4 179.2(4)
F3 C4 C5 C6 179.6(4)
C3 C4 C5 C6 -1.3(6)
F4 C5 C6 F5 -0.2(6)
C4 C5 C6 F5 -179.7(4)
F4 C5 C6 C1 -179.9(3)
C4 C5 C6 C1 0.6(6)
C2 C1 C6 F5 -179.2(3)
S1 C1 C6 F5 1.1(5)
C2 C1 C6 C5 0.5(5)
S1 C1 C6 C5 -179.1(3)
N2 B1 N1 C7 66.2(4)
N1 B1 N2 C8 154.7(3)
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139137581
