N-H deprotonation of a diaminodialkoxido diborane(4) - a structural study on bifunctional Lewis acids/bases and their dimerisation to B(sp<sup>2</sup>)<sub>2</sub>B(sp<sup>3</sup>)<sub>2</sub>N<sub>2</sub> six membered rings.
Drescher, Wiebke; Kleeberg, Christian; Dalton transactions (Cambridge, England : 2003) 50 (2021) 13149–13157; doi:10.1039/d1dt02327f

data_7708184
_publ_section_title
;
 N-H deprotonation of a diaminodialkoxido diborane(4) - a structural study
 on bifunctional Lewis acids/bases and their dimerisation to
 B(sp<sup>2</sup>)<sub>2</sub>B(sp<sup>3</sup>)<sub>2</sub>N<sub>2</sub>
 six membered rings.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13149
_journal_page_last               13157
_journal_paper_doi               10.1039/d1dt02327f
_journal_volume                  50
_journal_year                    2021
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C16 H27 B2 N2 O3, 0.5 (C4 H8 O K), 0.5 (C8 H16 O2 K)'
_chemical_formula_sum            'C22 H39 B2 K N2 O4.5'
_chemical_formula_weight         464.27
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2021-08-24 deposited with the CCDC.	2021-08-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.857(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5005(6)
_cell_length_b                   21.0732(9)
_cell_length_c                   11.8580(6)
_cell_measurement_reflns_used    15591
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75.709
_cell_measurement_theta_min      4.102
_cell_volume                     2607.6(3)
_computing_cell_refinement
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_collection
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_data_reduction
;
 CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
;
_computing_molecular_graphics
;
 K. Brandenburg, 2016, Diamond 4.2.2, Crystal Impact GbR, Bonn, Germany.
;
_computing_publication_material
;
 Olex2 (Dolomanov et al., J. Appl. Cryst., 2009, 42, 339-341)
;
_computing_structure_refinement
;
 SHELXL-2014/7 (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_computing_structure_solution
;
 SHELXT (Ver. 2014/4) (G. M. Sheldrick, Acta Cryst., 2015, A71, 3--8)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3543
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            34751
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.598
_diffrn_reflns_theta_min         4.109
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'Nova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84375
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro 1.171.38.43c (Rigaku Oxford Diffraction, 2015)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.183
_exptl_crystal_description       block
_exptl_crystal_F_000             1000
_exptl_crystal_recrystallization_method
;
 From a solution in THF layered with n-pentane at -40 deg C.
;
_exptl_crystal_size_max          0.259
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.187
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.041
_refine_ls_abs_structure_details
;
 Flack x determined using 2182 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.020(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5235
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0339
_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^)+(0.0433P)^2^+1.0410P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0860
_reflns_Friedel_coverage         0.866
_reflns_Friedel_fraction_full    0.924
_reflns_Friedel_fraction_max     0.910
_reflns_number_gt                5013
_reflns_number_total             5235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02327f2.cif
_cod_data_source_block           wo1wo
_cod_depositor_comments
'Adding full bibliography for 7708180--7708186.cif.'
_cod_original_cell_volume        2607.6(2)
_cod_original_sg_symbol_H-M      'C 2'
_cod_original_formula_sum        'C22 H39 B2 K N2 O4.50'
_cod_database_code               7708184
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              79019