An Experimental Solution to the "Missing Hydrogens" Question Surrounding the Macropolyhedral 19-Vertex Boron Hydride Monoanion [B19H22]-, a Simplification of Its Synthesis, and Its Use As an Intermediate in the First Example of syn-B18H22 to anti-B18H22 Isomer Conversion
Michael G. S. Londesborough; Jonathan Bould; Tomáš Baše; Drahomír Hnyk; Mario Bakardjiev; Josef Holub; Ivana Císařová; John D. Kennedy; Inorganic Chemistry 49 (2010) 4092–4098; doi:10.1021/ic901976y

data_4315441
_publ_contact_author_name        'Cisarova Ivana'
_publ_section_title
;
 An Experimental Solution to the "Missing Hydrogens" Question Surrounding
 the Macropolyhedral 19-Vertex Boron Hydride Monoanion [B19H22]-, a
 Simplification of Its Synthesis, and Its Use As an Intermediate in the
 First Example of syn-B18H22 to anti-B18H22 Isomer Conversion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4092
_journal_page_last               4098
_journal_paper_doi               10.1021/ic901976y
_journal_volume                  49
_journal_year                    2010
_chemical_absolute_configuration unk
_chemical_compound_source        'synthesized by the authors'
_chemical_formula_moiety         'B19 H21, 2(C14 H20 B N2)'
_chemical_formula_sum            'C28 H61 B21 N4'
_chemical_formula_weight         680.82
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                81.11(3)
_cell_angle_beta                 81.85(3)
_cell_angle_gamma                75.56(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8508(18)
_cell_length_b                   10.575(2)
_cell_length_c                   11.461(2)
_cell_measurement_temperature    150(2)
_cell_volume                     1020.4(4)
_computing_cell_refinement
;
 APEX 2 software, Bruker Nonius 2004
;
_computing_data_collection
;
 APEX 2 software, Bruker Nonius 2004
;
_computing_data_reduction
;
 SAINT - Bruker Integration program embedded in
 APEX 2 software, Bruker Nonius 2004
;
_computing_molecular_graphics    'ORTEP-III Version 1.08 (Farrugia, 2005)'
_computing_structure_refinement
;
SHELXL-97 (Sheldrick, G. M.     Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_computing_structure_solution
;
SHELXS-97 (Sheldrick, G. M.     Acta Cryst. (2008). A64, 112)
XSeed (L.J.Barbour, J.Supramol. Chem., 2003, 1, 189.)
;
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean
;
  120 microns
;
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type
;
Mach3 kappa-type 4-circle goniostat.
;
_diffrn_measurement_method       'rotation images'
_diffrn_radiation_detector       'ApexII camera'
_diffrn_radiation_monochromator
;
 graphite model mounted in "parallel" mode
;
_diffrn_radiation_source
;
  Bruker Nonius FR591 rotating anode generator
;
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0628
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            28061
_diffrn_reflns_theta_full        29.72
_diffrn_reflns_theta_max         29.72
_diffrn_reflns_theta_min         1.81
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  0.9899
_exptl_absorpt_correction_T_min  0.9805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

 See Sheldrick, G. M. (2002). SADABS.
 University of Gottingen, Germany.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.108
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             362
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.446
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   4(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         10214
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.2218*P+(0.0782P)^2^+0.0000sin\q/\l] 
 where P = 0.00000Fo^2^ + 1.00000Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1494
_refine_ls_wR_factor_ref         0.1667
_reflns_number_gt                7722
_reflns_number_total             10214
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic901976y_si_001_1.cif
_cod_data_source_block           jdk_mgsl
_cod_database_code               4315441