#------------------------------------------------------------------------------
#$Date: 2021-11-06 19:46:11 +0100 (Sat 06 de Nov de 2021) $
#$Revision: 270353 $
#$URL: svn://www.crystallography.net/cod/cif/7/12/90/7129027.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_7129027
loop_
_publ_author_name
'Frenette, Brandon L.'
'Omaña, Alvaro A'
'Ferguson, Michael J.'
'Zhou, Yuqiao'
'Rivard, Eric'
_publ_section_title
;
 Access to adducts of parent iminoborane isomers, HBNH and
 NBH₂, using frustrated Lewis pair chelation.
;
_journal_issue                   83
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              10895
_journal_page_last               10898
_journal_paper_doi               10.1039/d1cc04923b
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C2 H6 B I3 S'
_chemical_formula_sum            'C2 H6 B I3 S'
_chemical_formula_weight         453.64
_chemical_name_common            'boron trichloride dimethyl sulfide'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-09-18 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.749(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0765(4)
_cell_length_b                   7.2293(3)
_cell_length_c                   18.9898(9)
_cell_measurement_reflns_used    9876
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      74.02
_cell_measurement_theta_min      4.66
_cell_volume                     970.36(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0628
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37103
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.732
_diffrn_reflns_theta_min         4.662
_exptl_absorpt_coefficient_mu    77.206
_exptl_absorpt_correction_T_max  0.1985
_exptl_absorpt_correction_T_min  0.0409
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
; 
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., 
 J. Appl. Cryst. 48 (2015) 3-10 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.105
_exptl_crystal_description       block
_exptl_crystal_F_000             792
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexanes at -30C'
_exptl_crystal_size_max          0.066
_exptl_crystal_size_mid          0.065
_exptl_crystal_size_min          0.056
_refine_diff_density_max         1.551
_refine_diff_density_min         -1.295
_refine_diff_density_rms         0.179
_refine_ls_extinction_coef       0.00096(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     67
_refine_ls_number_reflns         1973
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0297
_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)+(0.0455P)²+3.8870P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0780
_refine_ls_wR_factor_ref         0.0787
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1912
_reflns_number_total             1973
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc04923b2.cif
_cod_data_source_block           Me2S-BI3
_cod_depositor_comments
'Adding full bibliography for 7129027--7129035.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7129027
_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. 
;
_shelx_estimated_absorpt_t_min   0.080
_shelx_estimated_absorpt_t_max   0.098
_shelx_res_file
; 
TITL riv2065 in P2(1)/c 
    riv2065.res 
    created by SHELXL-2018/3 at 11:00:36 on 23-Oct-2020 
CELL 1.54178   7.07650   7.22930  18.98980  90.0000  92.7490  90.0000 
ZERR    4.00   0.00040   0.00030   0.00090   0.0000   0.0023   0.0000 
LATT  1 
SYMM -X, 0.5+Y, 0.5-Z 
SFAC C H B S I 
UNIT 8 24 4 4 12 
TEMP -100.000 
SIZE 0.056 0.065 0.066 
  
L.S. 4 
ACTA 
CONF 2 
WGHT    0.045500    3.887000 
EXTI    0.000964 
FVAR       0.08518 
I1    5    0.753859    0.389404    0.369281    11.00000    0.04828    0.02106 = 
         0.04555    0.00041    0.00798    0.00123 
I2    5    0.853704    0.829350    0.280630    11.00000    0.03818    0.03518 = 
         0.03761    0.00704    0.00923   -0.00693 
I3    5    0.782122    0.824206    0.470040    11.00000    0.04611    0.04096 = 
         0.03183   -0.01042   -0.00704   -0.00238 
S1    4    0.439031    0.720652    0.340128    11.00000    0.02866    0.02870 = 
         0.03191    0.00098   -0.00171   -0.00541 
C1    1    0.390931    0.964680    0.346948    11.00000    0.04229    0.03376 = 
         0.04678    0.00152   -0.00018    0.00431 
AFIX 137 
H1A   2    0.254599    0.986161    0.339898    11.00000   -1.20000 
H1B   2    0.458065    1.031594    0.310867    11.00000   -1.20000 
H1C   2    0.433977    1.008957    0.393787    11.00000   -1.20000 
AFIX   0 
C2    1    0.312002    0.631513    0.414550    11.00000    0.03233    0.06039 = 
         0.06246    0.01324    0.01006   -0.00009 
AFIX 137 
H2A   2    0.177321    0.661728    0.407921    11.00000   -1.20000 
H2B   2    0.363153    0.688077    0.458326    11.00000   -1.20000 
H2C   2    0.327440    0.496953    0.417297    11.00000   -1.20000 
AFIX   0 
B1    3    0.705065    0.694396    0.367131    11.00000    0.02957    0.01679 = 
         0.02238   -0.00267    0.00008   -0.00460 
  
HKLF 4 
  
  
  
  
REM  riv2065 in P2(1)/c 
REM wR2 = 0.078693, GooF = S = 1.05314, Restrained GooF = 1.05314 for all data 
REM R1 = 0.029655 for 1912 Fo > 4sig(Fo) and 0.030503 for all 1973 data 
REM 67 parameters refined using 0 restraints 
  
END 
  
WGHT      0.0455      3.8869 
  
REM Highest difference peak  1.551,  deepest hole -1.295,  1-sigma level  0.179 
Q1    1   0.6729  0.8246  0.4684  11.00000  0.05    1.55 
Q2    1   0.6380  0.3823  0.3685  11.00000  0.05    1.21 
Q3    1   0.7476  0.8274  0.2742  11.00000  0.05    1.18 
Q4    1   0.8714  0.3724  0.3748  11.00000  0.05    1.15 
Q5    1   0.9733  0.8219  0.2818  11.00000  0.05    0.91 
Q6    1   0.7960  0.3088  0.3625  11.00000  0.05    0.81 
Q7    1   0.3022  0.5315  0.4220  11.00000  0.05    0.68 
Q8    1   0.8570  0.8785  0.2460  11.00000  0.05    0.64 
Q9    1   0.7888  0.3793  0.2942  11.00000  0.05    0.63 
Q10   1   0.7103  0.2765  0.3912  11.00000  0.05    0.57 
Q11   1   0.8959  0.8191  0.4787  11.00000  0.05    0.57 
Q12   1   0.8116  0.8759  0.4463  11.00000  0.05    0.52 
Q13   1   0.6150  1.1293  0.3766  11.00000  0.05    0.51 
Q14   1   0.7627  0.9316  0.3940  11.00000  0.05    0.50 
Q15   1   0.8272  0.8406  0.3577  11.00000  0.05    0.49 
Q16   1   0.7518  0.3815  0.4472  11.00000  0.05    0.49 
Q17   1   0.7059  0.5259  0.4103  11.00000  0.05    0.49 
Q18   1   0.6046  0.6429  0.2947  11.00000  0.05    0.48 
Q19   1   0.8242  0.9665  0.3508  11.00000  0.05    0.48 
Q20   1   0.7002  0.9420  0.3706  11.00000  0.05    0.46 
;
_shelx_res_checksum              43713
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'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.75386(6) 0.38940(5) 0.36928(2) 0.03811(14) Uani 1 1 d . . . . .
I2 I 0.85370(5) 0.82935(5) 0.28063(2) 0.03675(14) Uani 1 1 d . . . . .
I3 I 0.78212(6) 0.82421(5) 0.47004(2) 0.03992(15) Uani 1 1 d . . . . .
S1 S 0.43903(17) 0.72065(18) 0.34013(7) 0.0299(3) Uani 1 1 d . . . . .
C1 C 0.3909(9) 0.9647(8) 0.3469(4) 0.0410(13) Uani 1 1 d . . . . .
H1A H 0.254599 0.986161 0.339898 0.049 Uiso 1 1 calc R U . . .
H1B H 0.458065 1.031594 0.310867 0.049 Uiso 1 1 calc R U . . .
H1C H 0.433977 1.008957 0.393787 0.049 Uiso 1 1 calc R U . . .
C2 C 0.3120(9) 0.6315(11) 0.4146(4) 0.0515(17) Uani 1 1 d . . . . .
H2A H 0.177321 0.661728 0.407921 0.062 Uiso 1 1 calc R U . . .
H2B H 0.363153 0.688077 0.458326 0.062 Uiso 1 1 calc R U . . .
H2C H 0.327440 0.496953 0.417297 0.062 Uiso 1 1 calc R U . . .
B1 B 0.7051(8) 0.6944(7) 0.3671(3) 0.0230(10) Uani 1 1 d . . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.0483(2) 0.0211(2) 0.0455(2) 0.00041(13) 0.00798(16) 0.00123(13)
I2 0.0382(2) 0.0352(2) 0.0376(2) 0.00704(13) 0.00923(15) -0.00693(13)
I3 0.0461(2) 0.0410(2) 0.0318(2) -0.01042(14) -0.00704(15) -0.00238(15)
S1 0.0287(6) 0.0287(6) 0.0319(6) 0.0010(5) -0.0017(5) -0.0054(5)
C1 0.042(3) 0.034(3) 0.047(3) 0.002(3) 0.000(3) 0.004(2)
C2 0.032(3) 0.060(4) 0.062(4) 0.013(3) 0.010(3) 0.000(3)
B1 0.030(3) 0.017(2) 0.022(2) -0.0027(18) 0.0001(19) -0.0046(19)
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'
B B 0.0090 0.0039 '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'
I I -0.3257 6.8362 '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
C1 S1 C2 100.8(3) . . ?
C1 S1 B1 105.2(3) . . ?
C2 S1 B1 105.6(3) . . ?
S1 B1 I3 112.8(3) . . ?
S1 B1 I2 104.5(2) . . ?
I3 B1 I2 111.2(2) . . ?
S1 B1 I1 104.4(2) . . ?
I3 B1 I1 111.8(2) . . ?
I2 B1 I1 111.7(2) . . ?
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
I1 B1 2.232(5) . ?
I2 B1 2.219(5) . ?
I3 B1 2.212(5) . ?
S1 C1 1.803(6) . ?
S1 C2 1.828(7) . ?
S1 B1 1.937(6) . ?
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 S1 B1 I3 52.6(3) . . . . ?
C2 S1 B1 I3 -53.5(4) . . . . ?
C1 S1 B1 I2 -68.4(3) . . . . ?
C2 S1 B1 I2 -174.5(3) . . . . ?
C1 S1 B1 I1 174.2(3) . . . . ?
C2 S1 B1 I1 68.1(4) . . . . ?
