Real-Space Indicators for Chemical Bonding. Experimental and Theoretical Electron Density Studies of Four Deltahedral Boranes
Stefan Mebs; Roman Kalinowski; Simon Grabowsky; Diana Förster; Rainer Kickbusch; Eugen Justus; Wolfgang Morgenroth; Carsten Paulmann; Peter Luger; Detlef Gabel; Dieter Lentz; Inorganic Chemistry 50 (2011) 90–103; doi:10.1021/ic1013158

data_4324087
_publ_contact_author
;
    Prof. Dr. Dieter Lentz
    Institut f\"ur  Chemie und Biochemie
    Anorganische Chemie
    Freie Universit\"at Berlin
    Fabeckstr. 34-36
    14195, Berlin
    Germany
;
_publ_contact_author_email       lentz@chemie.fu-berlin.de
_publ_contact_author_fax         0049-30-83852695
_publ_contact_author_phone       0049-30-83852695
_publ_section_title
;
 Real-Space Indicators for Chemical Bonding. Experimental and Theoretical
 Electron Density Studies of Four Deltahedral Boranes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              90
_journal_page_last               103
_journal_paper_doi               10.1021/ic1013158
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration b10
_chemical_formula_moiety         '2(C10 H9 N2), B10 H10, H2 O'
_chemical_formula_sum            'C20 H30 B10 N4 O'
_chemical_formula_weight         450.58
_chemical_name_common
'2,2'-bispyridilium decahydro-closo-decaborate(2-)'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                86.66(3)
_cell_angle_beta                 83.88(3)
_cell_angle_gamma                72.83(3)
_cell_formula_units_Z            2
_cell_length_a                   9.232(2)
_cell_length_b                   9.437(2)
_cell_length_c                   14.613(3)
_cell_measurement_temperature    9(2)
_cell_volume                     1209.0(5)
_computing_cell_refinement       XDS
_computing_data_collection       XDS
_computing_data_reduction        XDS
_computing_molecular_graphics    'Volkov et al, (2006)'
_computing_publication_material  'Volkov et al, (2006)'
_computing_structure_refinement  'Volkov et al, (2006)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      9(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_device_type  'Mar165 CCD'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.5166(2)
_diffrn_reflns_av_R_equivalents  0.0716
_diffrn_reflns_av_sigmaI/netI    0.0779
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            194515
_diffrn_reflns_reduction_process
;
 Scaled and merged with Sortav
 R.H. Blessing, (1987) Cryst. Rev. 1, 3-58
 R.H. Blessing, (1989) J. Appl. Cryst. 22, 396-397
;
_diffrn_reflns_theta_full        18.84
_diffrn_reflns_theta_max         31.80
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.036
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.238(1)
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             472.0
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.226
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.574
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         13527
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.039
_refine_ls_R_factor_gt           0.021
_refine_ls_R_Fsqd_factor         0.032
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
calc w2 = 1/[s^2^(Fo^2^)]
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.048
_reflns_number_gt                13527
_reflns_number_total             19381
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1013158_si_003.cif
_cod_data_source_block           b10h10
_cod_original_cell_volume        1209.0(4)
_cod_database_code               4324087