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_7129423
_publ_section_title
;
 Derivatization of an especially electron-rich diborane
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC06359F
_journal_year                    2022
_chemical_formula_moiety         'C16 H24 B2 N8 S2'
_chemical_formula_sum            'C16 H24 B2 N8 S2'
_chemical_formula_weight         414.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-04-21
_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                 91.214(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.739(2)
_cell_length_b                   15.667(3)
_cell_length_c                   10.1279(18)
_cell_measurement_reflns_used    9900
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.78
_cell_measurement_theta_min      2.60
_cell_volume                     2020.9(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v2018.7-2 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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 2014/5 (Sheldrick, 2014)'
_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  0.0726
_diffrn_reflns_av_unetI/netI     0.0508
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24812
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.487
_diffrn_reflns_theta_min         2.011
_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    0.284
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6015
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1270 before and 0.0897 after correction.
The Ratio of minimum to maximum transmission is 0.8065.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.361
_exptl_crystal_description       block
_exptl_crystal_F_000             872
_exptl_crystal_size_max          0.203
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.148
_refine_diff_density_max         0.459
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.086
_refine_ls_abs_structure_details
;
 Flack x determined using 1820 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.10(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     263
_refine_ls_number_reflns         4620
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0672
_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^)+(0.1096P)^2^+7.0419P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1832
_refine_ls_wR_factor_ref         0.2000
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.994
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                4127
_reflns_number_total             4620
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc06359f2.cif
_cod_data_source_block           mo_dv236_01
_cod_database_code               7129423
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.945
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.854(4)
 0.146(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
3. Others
 Fixed Sof: H12A(0.55) H12B(0.55) H12C(0.45) H12D(0.45) H14A(0.55) H14B(0.55)
 H14C(0.45) H14D(0.45) C13(0.55) H13A(0.55) H13B(0.55) C13B(0.45) H13C(0.45)
 H13D(0.45)
4.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B),
 C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C12(H12C,H12D),
 C14(H14A,H14B), C14(H14C,H14D), C13(H13A,H13B), C13B(H13C,H13D)
;
_shelx_res_checksum              25520
_olex2_submission_special_instructions 'No special instructions were received'