Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2007

data_global
_journal_name_full               'Dalton Trans.'

_journal_coden_Cambridge         0222

_publ_contact_author_name        'Clara Vinas'
_publ_contact_author_address     
;
Laboratori de Materials Inorganics i Catalisi
CSIC/ICMAB
Campus UAB
Bellaterra
08193
SPAIN
;

_publ_contact_author_email       CLARA@ICMAB.ES

_publ_section_title              
;
Synthesis and investigation of the boron
cluster anion [7(2'-pyridyl)-7,8-nido-dicarbaundecaborate]
and its protonated form
;
loop_
_publ_author_name
'Clara Vinas'
'Hana Horakova'
'Ales Langauf'
'Anna Laromaine'
'I. Mata'
'Elies Molins'
;
F.Teixidor
;
'Radim Vespalec'

data_tex6
_database_code_depnum_ccdc_archive 'CCDC 642890'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C7 H16 B9 N'
_chemical_formula_weight         211.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 c 1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   7.513
_cell_length_b                   18.803
_cell_length_c                   8.653
_cell_angle_alpha                90.00
_cell_angle_beta                 99.12
_cell_angle_gamma                90.00
_cell_volume                     1206.9
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    25
_cell_measurement_theta_min      5.3
_cell_measurement_theta_max      9.2

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             440
_exptl_absorpt_coefficient_mu    0.056
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            1950
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0922
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         30.42
_reflns_number_total             1950
_reflns_number_gt                1193
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CAD-4 (Enraf-Nonius, 1989)'
_computing_cell_refinement       'CAD-4 (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms and Wocadlo, 1995)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WINGX (Farrugia, 1999)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
The following restrains have been to the bond distances:
d(B-H)=1.100
d(C8-H8)=0.930
d(N16-H16)=0.860
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1950
_refine_ls_number_parameters     203
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1381
_refine_ls_wR_factor_gt          0.1159
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_restrained_S_all      1.041
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.003

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C7 C 0.5115(4) 0.25298(12) 0.4516(3) 0.0281(6) Uani 1 1 d . . .
C8 C 0.6168(4) 0.28823(14) 0.3305(3) 0.0343(6) Uani 1 1 d D . .
H8 H 0.678(4) 0.2579(14) 0.267(3) 0.041 Uiso 1 1 d D . .
C11 C 0.5179(4) 0.17432(13) 0.4623(3) 0.0306(6) Uani 1 1 d . . .
C12 C 0.6476(5) 0.13261(16) 0.4130(5) 0.0428(7) Uani 1 1 d . . .
H12 H 0.735(5) 0.1494(17) 0.382(5) 0.051 Uiso 1 1 d . . .
C13 C 0.6446(5) 0.05990(17) 0.4275(5) 0.0520(9) Uani 1 1 d . . .
H13 H 0.733(5) 0.0339(18) 0.374(5) 0.062 Uiso 1 1 d . . .
C14 C 0.5107(5) 0.02744(16) 0.4902(4) 0.0476(8) Uani 1 1 d . . .
H14 H 0.520(5) -0.0239(19) 0.510(4) 0.057 Uiso 1 1 d . . .
C15 C 0.3798(5) 0.06835(16) 0.5381(4) 0.0432(8) Uani 1 1 d . . .
H15 H 0.275(5) 0.0544(17) 0.573(4) 0.052 Uiso 1 1 d . . .
N16 N 0.3875(3) 0.14020(12) 0.5219(3) 0.0385(6) Uani 1 1 d D . .
H16 H 0.301(4) 0.1643(15) 0.558(4) 0.046 Uiso 1 1 d D . .
B1 B 0.6490(5) 0.37848(18) 0.5822(5) 0.0407(8) Uani 1 1 d D . .
H1 H 0.718(5) 0.4073(16) 0.682(3) 0.049 Uiso 1 1 d D . .
B2 B 0.5243(5) 0.30308(17) 0.6210(4) 0.0351(7) Uani 1 1 d D . .
H2 H 0.517(4) 0.2757(14) 0.732(3) 0.042 Uiso 1 1 d D . .
B3 B 0.7156(4) 0.29369(17) 0.5259(4) 0.0353(7) Uani 1 1 d D . .
H3 H 0.831(3) 0.2600(14) 0.570(4) 0.042 Uiso 1 1 d D . .
B4 B 0.7189(5) 0.36674(18) 0.3977(5) 0.0385(8) Uani 1 1 d D . .
H4 H 0.849(3) 0.3792(17) 0.359(4) 0.046 Uiso 1 1 d D . .
B5 B 0.5296(5) 0.42048(17) 0.4089(5) 0.0396(8) Uani 1 1 d D . .
H5 H 0.527(4) 0.4780(10) 0.391(4) 0.048 Uiso 1 1 d D . .
B6 B 0.4076(5) 0.38059(17) 0.5501(4) 0.0378(8) Uani 1 1 d D . .
H6 H 0.341(4) 0.4164(14) 0.623(4) 0.045 Uiso 1 1 d D . .
B9 B 0.5228(5) 0.36009(18) 0.2522(4) 0.0366(7) Uani 1 1 d D . .
H9 H 0.536(5) 0.3796(16) 0.135(3) 0.044 Uiso 1 1 d D . .
B10 B 0.3265(5) 0.37465(18) 0.3466(4) 0.0350(7) Uani 1 1 d D . .
H10A H 0.203(3) 0.4033(15) 0.306(4) 0.042 Uiso 1 1 d D . .
H10B H 0.320(7) 0.3226(16) 0.293(6) 0.109(17) Uiso 1 1 d D . .
B11 B 0.3308(5) 0.29767(16) 0.4715(4) 0.0310(7) Uani 1 1 d D . .
H11 H 0.211(3) 0.2713(14) 0.501(4) 0.037 Uiso 1 1 d D . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C7 0.0292(13) 0.0244(11) 0.0302(14) -0.0017(11) 0.0038(11) 0.0014(12)
C8 0.0327(14) 0.0322(14) 0.0375(16) -0.0040(12) 0.0041(12) -0.0004(12)
C11 0.0314(14) 0.0284(11) 0.0307(15) -0.0026(12) 0.0010(12) -0.0031(12)
C12 0.0388(16) 0.0348(15) 0.057(2) 0.0014(14) 0.0155(15) 0.0010(14)
C13 0.055(2) 0.0342(16) 0.068(2) -0.0094(17) 0.0130(18) 0.0105(15)
C14 0.0579(18) 0.0278(13) 0.054(2) -0.0045(14) 0.0002(17) -0.0025(16)
C15 0.0482(19) 0.0318(15) 0.050(2) -0.0035(14) 0.0081(16) -0.0093(14)
N16 0.0435(15) 0.0287(12) 0.0444(16) -0.0036(11) 0.0102(12) 0.0009(11)
B1 0.0456(19) 0.0302(16) 0.042(2) -0.0042(15) -0.0068(17) -0.0037(14)
B2 0.0423(18) 0.0320(16) 0.0302(17) -0.0003(13) 0.0032(15) 0.0044(14)
B3 0.0342(17) 0.0328(15) 0.0367(17) 0.0017(13) -0.0015(14) 0.0023(13)
B4 0.0342(16) 0.0346(16) 0.044(2) 0.0029(14) -0.0012(16) -0.0093(13)
B5 0.0431(18) 0.0267(15) 0.047(2) 0.0030(14) -0.0007(16) -0.0012(14)
B6 0.0444(19) 0.0308(15) 0.0374(19) -0.0015(14) 0.0043(16) 0.0070(15)
B9 0.0359(17) 0.0404(17) 0.0326(17) 0.0040(14) 0.0026(14) -0.0022(14)
B10 0.0322(16) 0.0323(16) 0.0394(19) 0.0040(14) 0.0023(14) 0.0037(13)
B11 0.0340(15) 0.0288(14) 0.0297(16) 0.0000(12) 0.0033(13) 0.0061(12)

_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C7 C11 1.482(3) . ?
C7 C8 1.557(4) . ?
C7 B11 1.629(4) . ?
C7 B2 1.732(4) . ?
C7 B3 1.743(4) . ?
C8 B9 1.622(5) . ?
C8 B4 1.722(4) . ?
C8 B3 1.739(4) . ?
C11 N16 1.341(4) . ?
C11 C12 1.371(4) . ?
C12 C13 1.373(4) . ?
C13 C14 1.361(5) . ?
C14 C15 1.364(5) . ?
C15 N16 1.360(4) . ?
B1 B2 1.760(5) . ?
B1 B3 1.763(5) . ?
B1 B4 1.772(6) . ?
B1 B6 1.791(5) . ?
B1 B5 1.803(5) . ?
B2 B6 1.760(5) . ?
B2 B3 1.774(5) . ?
B2 B11 1.789(5) . ?
B3 B4 1.768(5) . ?
B4 B5 1.760(5) . ?
B4 B9 1.784(5) . ?
B5 B10 1.761(5) . ?
B5 B9 1.763(5) . ?
B5 B6 1.803(5) . ?
B6 B11 1.761(5) . ?
B6 B10 1.774(6) . ?
B9 B10 1.816(5) . ?
B10 B11 1.804(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 C7 C8 116.8(2) . . ?
C11 C7 B11 121.8(2) . . ?
C8 C7 B11 111.8(2) . . ?
C11 C7 B2 119.5(2) . . ?
C8 C7 B2 111.8(2) . . ?
B11 C7 B2 64.25(19) . . ?
C11 C7 B3 113.4(2) . . ?
C8 C7 B3 63.29(19) . . ?
B11 C7 B3 115.7(2) . . ?
B2 C7 B3 61.41(19) . . ?
C7 C8 B9 113.7(2) . . ?
C7 C8 B4 112.6(2) . . ?
B9 C8 B4 64.42(19) . . ?
C7 C8 B3 63.57(18) . . ?
B9 C8 B3 116.6(2) . . ?
B4 C8 B3 61.4(2) . . ?
N16 C11 C12 116.4(2) . . ?
N16 C11 C7 118.9(2) . . ?
C12 C11 C7 124.7(3) . . ?
C11 C12 C13 121.2(3) . . ?
C14 C13 C12 120.5(3) . . ?
C13 C14 C15 118.9(3) . . ?
N16 C15 C14 119.0(3) . . ?
C11 N16 C15 124.1(3) . . ?
B2 B1 B3 60.48(19) . . ?
B2 B1 B4 108.3(2) . . ?
B3 B1 B4 60.0(2) . . ?
B2 B1 B6 59.4(2) . . ?
B3 B1 B6 107.6(2) . . ?
B4 B1 B6 107.5(2) . . ?
B2 B1 B5 107.6(2) . . ?
B3 B1 B5 107.0(3) . . ?
B4 B1 B5 59.0(2) . . ?
B6 B1 B5 60.2(2) . . ?
C7 B2 B6 101.4(2) . . ?
C7 B2 B1 103.7(3) . . ?
B6 B2 B1 61.2(2) . . ?
C7 B2 B3 59.60(18) . . ?
B6 B2 B3 108.4(2) . . ?
B1 B2 B3 59.8(2) . . ?
C7 B2 B11 55.08(17) . . ?
B6 B2 B11 59.49(19) . . ?
B1 B2 B11 107.7(2) . . ?
B3 B2 B11 106.5(2) . . ?
C8 B3 C7 53.14(16) . . ?
C8 B3 B1 103.1(2) . . ?
C7 B3 B1 103.1(2) . . ?
C8 B3 B4 58.82(19) . . ?
C7 B3 B4 102.1(2) . . ?
B1 B3 B4 60.2(2) . . ?
C8 B3 B2 101.8(2) . . ?
C7 B3 B2 58.99(18) . . ?
B1 B3 B2 59.7(2) . . ?
B4 B3 B2 107.8(2) . . ?
C8 B4 B5 100.9(2) . . ?
C8 B4 B3 59.74(18) . . ?
B5 B4 B3 108.7(3) . . ?
C8 B4 B1 103.4(2) . . ?
B5 B4 B1 61.4(2) . . ?
B3 B4 B1 59.7(2) . . ?
C8 B4 B9 55.07(18) . . ?
B5 B4 B9 59.6(2) . . ?
B3 B4 B9 107.2(2) . . ?
B1 B4 B9 108.3(3) . . ?
B4 B5 B10 111.8(2) . . ?
B4 B5 B9 60.9(2) . . ?
B10 B5 B9 62.0(2) . . ?
B4 B5 B6 107.5(2) . . ?
B10 B5 B6 59.7(2) . . ?
B9 B5 B6 107.3(2) . . ?
B4 B5 B1 59.6(2) . . ?
B10 B5 B1 109.5(2) . . ?
B9 B5 B1 107.9(3) . . ?
B6 B5 B1 59.6(2) . . ?
B2 B6 B11 61.08(18) . . ?
B2 B6 B10 111.6(3) . . ?
B11 B6 B10 61.4(2) . . ?
B2 B6 B1 59.4(2) . . ?
B11 B6 B1 107.6(2) . . ?
B10 B6 B1 109.4(3) . . ?
B2 B6 B5 107.6(3) . . ?
B11 B6 B5 106.1(2) . . ?
B10 B6 B5 59.0(2) . . ?
B1 B6 B5 60.2(2) . . ?
C8 B9 B5 104.9(3) . . ?
C8 B9 B4 60.51(19) . . ?
B5 B9 B4 59.5(2) . . ?
C8 B9 B10 105.6(2) . . ?
B5 B9 B10 58.9(2) . . ?
B4 B9 B10 108.1(3) . . ?
B5 B10 B6 61.3(2) . . ?
B5 B10 B11 106.1(3) . . ?
B6 B10 B11 58.98(19) . . ?
B5 B10 B9 59.0(2) . . ?
B6 B10 B9 106.3(3) . . ?
B11 B10 B9 102.1(2) . . ?
C7 B11 B6 105.7(2) . . ?
C7 B11 B2 60.67(19) . . ?
B6 B11 B2 59.44(19) . . ?
C7 B11 B10 106.7(2) . . ?
B6 B11 B10 59.7(2) . . ?
B2 B11 B10 108.8(2) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        30.42
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.220
_refine_diff_density_min         -0.178
_refine_diff_density_rms         0.050