Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2002

data_a
_database_code_CSD                  154905

_journal_coden_Cambridge      186


loop_
_publ_author_name
'C., Vinas'
'Gemma, Barbera'
'Georgina M, Rosair'
'Francesc, Teixidor'
'Alan, Welch'

_publ_contact_author_name     	'C. Vinas'  
_publ_contact_author_address 
;
ICMAB
CSIC
Campus UAB
Bellaterra
Catalonia
08193
SPAIN
;

_publ_contact_author_email       'CLARA@ICMAB.ES'

_publ_requested_journal       'Dalton Transactions'


_publ_section_title		
;
Self-assembly of carborane molecules via C-H...I
hydrogen bonding:  The molecular and crystal structures of
3-I-1,2-closo-C2B10H11
;


_audit_creation_method            SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
'C2 H11 B10 I'
_chemical_formula_weight          270.11

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'
'I'  'I'  -0.4742   1.8119
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting            Orthorhombic
_symmetry_space_group_name_H-M    Pnma

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

_cell_length_a                    20.011(3)
_cell_length_b                    8.0039(10)
_cell_length_c                    6.4946(14)
_cell_angle_alpha                 90.00
_cell_angle_beta                  90.00
_cell_angle_gamma                 90.00
_cell_volume                      1040.2(3)
_cell_formula_units_Z             4
_cell_measurement_temperature     160(2)
_cell_measurement_reflns_used     35
_cell_measurement_theta_min       4.17
_cell_measurement_theta_max       12.44

_exptl_crystal_description        BLOCK
_exptl_crystal_colour             COLOURLESS
_exptl_crystal_size_max           0.36
_exptl_crystal_size_mid           0.68
_exptl_crystal_size_min           0.44
_exptl_crystal_density_meas       ?
_exptl_crystal_density_diffrn     1.725
_exptl_crystal_density_method     'not measured'
_exptl_crystal_F_000              504
_exptl_absorpt_coefficient_mu     3.009
_exptl_absorpt_correction_type    psi-scans
_exptl_absorpt_correction_T_min   0.7260
_exptl_absorpt_correction_T_max   0.8372
_exptl_absorpt_process_details    'North et al., 1968'

_exptl_special_details
;
?
;

_diffrn_ambient_temperature       160(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   'Bruker P4'
_diffrn_measurement_method        '\w scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_standards_number          3
_diffrn_standards_interval_count  97
_diffrn_standards_interval_time   ?
_diffrn_standards_decay_%         ?
_diffrn_reflns_number             1417
_diffrn_reflns_av_R_equivalents   0.0480
_diffrn_reflns_av_sigmaI/netI     0.0474
_diffrn_reflns_limit_h_min        -23
_diffrn_reflns_limit_h_max        1
_diffrn_reflns_limit_k_min        -9
_diffrn_reflns_limit_k_max        1
_diffrn_reflns_limit_l_min        -1
_diffrn_reflns_limit_l_max        7
_diffrn_reflns_theta_min          3.26
_diffrn_reflns_theta_max          25.02
_reflns_number_total              990
_reflns_number_gt                 872
_reflns_threshold_expression      >2sigma(I)

_computing_data_collection        'Bruker XSCANS'
_computing_cell_refinement        'Bruker XSCANS'
_computing_data_reduction         'Bruker SHELXTL'
_computing_structure_solution     'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement   'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics     'Bruker SHELXTL'
_computing_publication_material   'Bruker SHELXTL'

_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.
;

_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^)+(0.0467P)^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     mixed
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        ?
_refine_ls_number_reflns          990
_refine_ls_number_parameters      85
_refine_ls_number_restraints      4
_refine_ls_R_factor_all           0.0373
_refine_ls_R_factor_gt            0.0320
_refine_ls_wR_factor_ref          0.0802
_refine_ls_wR_factor_gt           0.0773
_refine_ls_goodness_of_fit_ref    1.042
_refine_ls_restrained_S_all       1.041
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000

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
I1 I 0.451856(16) 0.2500 0.35738(6) 0.02348(18) Uani 1 2 d S . . C1 C
0.61414(19) 0.1485(5) 0.3625(6) 0.0191(8) Uani 1 1 d . . . H1 H 0.600(2)
0.109(6) 0.487(7) 0.023 Uiso 1 1 d . . . B3 B 0.5521(3) 0.2500 0.2311(10)
0.0168(12) Uani 1 2 d S . . B4 B 0.5906(2) 0.0697(6) 0.1291(6) 0.0193(9)
Uani 1 1 d D . . H4 H 0.563(2) -0.046(4) 0.123(6) 0.023 Uiso 1 1 d D . . B5
B 0.6760(2) 0.0700(6) 0.2114(7) 0.0231(9) Uani 1 1 d D . . H5 H 0.7001(19)
-0.047(4) 0.254(6) 0.028 Uiso 1 1 d D . . B6 B 0.6906(3) 0.2500 0.3687(9)
0.0205(13) Uani 1 2 d SD . . H6 H 0.720(3) 0.2500 0.510(6) 0.025 Uiso 1 2 d
SD . . B8 B 0.5776(3) 0.2500 -0.0276(9) 0.0180(12) Uani 1 2 d SD . . H8 H
0.538(2) 0.2500 -0.145(7) 0.022 Uiso 1 2 d SD . . B9 B 0.6553(2) 0.1382(6)
-0.0405(7) 0.0213(9) Uani 1 1 d . . . H9 H 0.669(2) 0.068(6) -0.178(6) 0.026
Uiso 1 1 d . . . B10 B 0.7169(3) 0.2500 0.1048(11) 0.0243(15) Uani 1 2 d S .
. H10 H 0.771(3) 0.2500 0.063(10) 0.029 Uiso 1 2 d S . .

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
I1 0.0161(2) 0.0273(2) 0.0270(3) 0.000 0.00719(14) 0.000
C1 0.0168(18) 0.025(2) 0.0159(18) 0.0002(16) 0.0005(14) 0.0000(16) 
B3 0.012(3) 0.021(3) 0.017(3) 0.000 -0.001(2) 0.000 
B4 0.0169(19) 0.022(2) 0.019(2) -0.0040(18) 0.0010(16) 0.0001(18) 
B5 0.019(2) 0.027(2) 0.023(2) 0.001(2) 0.0021(19) 0.0064(19) 
B6 0.015(3) 0.030(3) 0.016(3) 0.000 -0.004(2) 0.000 
B8 0.012(3) 0.028(3) 0.014(3) 0.000 0.001(2) 0.000 
B9 0.0135(19) 0.031(2) 0.019(2) -0.003(2) 0.0018(16) 0.0025(17) 
B10 0.011(3) 0.033(3) 0.029(4) 0.000 -0.001(3) 0.000

_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
I1 B3 2.168(6) . ?
C1 C1 1.624(8) 7_565 ?
C1 B5 1.701(6) . ?
C1 B4 1.708(5) . ?
C1 B3 1.711(6) . ?
C1 B6 1.733(7) . ?
B3 C1 1.711(6) 7_565 ?
B3 B8 1.756(9) . ?
B3 B4 1.764(6) . ?
B3 B4 1.764(6) 7_565 ?
B4 B8 1.784(6) . ?
B4 B9 1.787(6) . ?
B4 B5 1.792(6) . ?
B5 B9 1.773(6) . ?
B5 B6 1.790(6) . ?
B5 B10 1.795(6) . ?
B6 C1 1.733(7) 7_565 ?
B6 B5 1.790(6) 7_565 ?
B6 B10 1.793(9) . ?
B8 B4 1.784(6) 7_565 ?
B8 B9 1.796(6) . ?
B8 B9 1.796(6) 7_565 ?
B9 B9 1.789(9) 7_565 ?
B9 B10 1.791(7) . ?
B10 B9 1.791(7) 7_565 ?
B10 B5 1.795(6) 7_565 ?

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
C1 C1 B5 111.7(2) 7_565 . ?
C1 C1 B4 111.7(2) 7_565 . ?
B5 C1 B4 63.4(3) . . ?
C1 C1 B3 61.66(16) 7_565 . ?
B5 C1 B3 114.6(3) . . ?
B4 C1 B3 62.1(3) . . ?
C1 C1 B6 62.06(17) 7_565 . ?
B5 C1 B6 62.8(3) . . ?
B4 C1 B6 115.9(3) . . ?
B3 C1 B6 115.4(3) . . ?
C1 B3 C1 56.7(3) 7_565 . ?
C1 B3 B8 105.5(3) 7_565 . ?
C1 B3 B8 105.5(3) . . ?
C1 B3 B4 105.0(3) 7_565 . ?
C1 B3 B4 58.9(2) . . ?
B8 B3 B4 60.9(2) . . ?
C1 B3 B4 58.9(2) 7_565 7_565 ?
C1 B3 B4 105.0(3) . 7_565 ?
B8 B3 B4 60.9(2) . 7_565 ?
B4 B3 B4 109.7(4) . 7_565 ?
C1 B3 I1 118.9(3) 7_565 . ?
C1 B3 I1 118.9(3) . . ?
B8 B3 I1 129.1(4) . . ?
B4 B3 I1 123.1(2) . . ?
B4 B3 I1 123.1(2) 7_565 . ?
C1 B4 B3 59.0(3) . . ?
C1 B4 B8 104.3(3) . . ?
B3 B4 B8 59.3(3) . . ?
C1 B4 B9 103.5(3) . . ?
B3 B4 B9 107.3(3) . . ?
B8 B4 B9 60.4(3) . . ?
C1 B4 B5 58.1(2) . . ?
B3 B4 B5 107.6(3) . . ?
B8 B4 B5 107.9(3) . . ?
B9 B4 B5 59.4(2) . . ?
C1 B5 B9 104.4(3) . . ?
C1 B5 B6 59.5(3) . . ?
B9 B5 B6 108.5(3) . . ?
C1 B5 B4 58.5(2) . . ?
B9 B5 B4 60.2(2) . . ?
B6 B5 B4 109.1(3) . . ?
C1 B5 B10 104.9(3) . . ?
B9 B5 B10 60.2(3) . . ?
B6 B5 B10 60.0(3) . . ?
B4 B5 B10 108.7(4) . . ?
C1 B6 C1 55.9(3) . 7_565 ?
C1 B6 B5 57.7(2) . . ?
C1 B6 B5 102.7(4) 7_565 . ?
C1 B6 B5 102.7(4) . 7_565 ?
C1 B6 B5 57.7(2) 7_565 7_565 ?
B5 B6 B5 107.2(4) . 7_565 ?
C1 B6 B10 103.7(4) . . ?
C1 B6 B10 103.7(4) 7_565 . ?
B5 B6 B10 60.1(2) . . ?
B5 B6 B10 60.1(2) 7_565 . ?
B3 B8 B4 59.8(2) . 7_565 ?
B3 B8 B4 59.8(2) . . ?
B4 B8 B4 107.9(4) 7_565 . ?
B3 B8 B9 107.2(3) . . ?
B4 B8 B9 107.7(4) 7_565 . ?
B4 B8 B9 59.9(2) . . ?
B3 B8 B9 107.2(3) . 7_565 ?
B4 B8 B9 59.9(2) 7_565 7_565 ?
B4 B8 B9 107.7(4) . 7_565 ?
B9 B8 B9 59.8(3) . 7_565 ?
B5 B9 B4 60.4(2) . . ?
B5 B9 B9 107.9(2) . 7_565 ?
B4 B9 B9 107.9(2) . 7_565 ?
B5 B9 B10 60.5(3) . . ?
B4 B9 B10 109.1(3) . . ?
B9 B9 B10 60.03(18) 7_565 . ?
B5 B9 B8 108.2(3) . . ?
B4 B9 B8 59.7(2) . . ?
B9 B9 B8 60.12(17) 7_565 . ?
B10 B9 B8 108.8(3) . . ?
B9 B10 B9 59.9(4) . 7_565 ?
B9 B10 B6 107.6(4) . . ?
B9 B10 B6 107.6(4) 7_565 . ?
B9 B10 B5 106.9(4) . 7_565 ?
B9 B10 B5 59.3(2) 7_565 7_565 ?
B6 B10 B5 59.9(3) . 7_565 ?
B9 B10 B5 59.3(2) . . ?
B9 B10 B5 106.9(4) 7_565 . ?
B6 B10 B5 59.9(3) . . ?
B5 B10 B5 106.7(5) 7_565 . ?

_diffrn_measured_fraction_theta_max    0.997
_diffrn_reflns_theta_full              25.02
_diffrn_measured_fraction_theta_full   0.997
_refine_diff_density_max    0.564
_refine_diff_density_min   -1.828
_refine_diff_density_rms    0.160