Derivatization of an especially electron-rich diborane
Vogler, Daniel; Haas, Lea; Wolf, Nina; Kaifer, Elisabeth; Himmel, Hans-Jörg; Chemical Communications  (2022) –; doi:10.1039/D1CC06359F

data_7129428
_publ_section_title
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 Derivatization of an especially electron-rich diborane
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06359F
_journal_year                    2022
_chemical_formula_moiety         'C15 H23 B2 Br N7 S'
_chemical_formula_sum            'C15 H23 B2 Br N7 S'
_chemical_formula_weight         434.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2021-05-25
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2021-11-05 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.7035(10)
_cell_length_b                   15.5342(9)
_cell_length_c                   16.8091(10)
_cell_measurement_reflns_used    8115
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      24.34
_cell_measurement_theta_min      2.16
_cell_volume                     4361.5(4)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'APEX 3 V2019.11-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'Bruker Photon III detector'
_diffrn_detector_type            'CPAD detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1664
_diffrn_reflns_av_unetI/netI     0.0578
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            80071
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         2.162
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.994
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6079
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1285 before and 0.0787 after correction.
The Ratio of minimum to maximum transmission is 0.8156.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_description       needle
_exptl_crystal_F_000             1784
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.122
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.959
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         4282
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1105
_refine_ls_R_factor_gt           0.0940
_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/[\s^2^(Fo^2^)+(0.0308P)^2^+73.2237P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2102
_refine_ls_wR_factor_ref         0.2208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3407
_reflns_number_total             4282
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06359f2.cif
_cod_data_source_block           mo_2021_dv294_0ma_pl
_cod_database_code               7129428
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
N7 \\sim C15 \\sim S1: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
C13B \\sim C14 \\sim C12 \\sim C13: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
3. Others
 Sof(H12C)=Sof(H12D)=Sof(H14C)=Sof(H14D)=1-FVAR(1)
 Sof(H12A)=Sof(H12B)=Sof(H14A)=Sof(H14B)=FVAR(1)
 Fixed Sof: C13(0.7) H13A(0.7) H13B(0.7) C13B(0.3) H13C(0.3) H13D(0.3)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B), C9(H9A,H9B),
 C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C12(H12C,H12D), C13(H13A,H13B),
  C13B(H13C,H13D), C14(H14A,H14B), C14(H14C,H14D)
4.b Aromatic/amide H refined with riding coordinates:
 C5(H5)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40562
_shelx_fab_checksum              98879
_olex2_submission_special_instructions 'No special instructions were received'