#------------------------------------------------------------------------------
#$Date: 2016-03-25 10:37:47 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179757 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/53/7005391.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7005391
loop_
_publ_author_name
'Teixidor, Francesc'
'Barberà, Gemma'
'Kivekäs, Raikko'
'Sillanpää, Reijo'
'Viñas, Clara'
_publ_section_title
;
 "Water-stable boron-iodinated dicarbollide dianions
 [7,8-nido-C2H2B9I9]2- and [7,8-nido-C2H2B9I8H]2-".
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1668
_journal_page_last               1670
_journal_paper_doi               10.1039/b701787a
_journal_year                    2007
_chemical_formula_moiety         'C2 H3 B9 I8 2-, 2(C3 H10 N 1+)'
_chemical_formula_sum            'C8 H23 B9 I8 N2'
_chemical_formula_weight         1259.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           40
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      40
_symmetry_space_group_name_Hall  'A 2 -2a'
_symmetry_space_group_name_H-M   'A m a 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.1115(6)
_cell_length_b                   14.8951(8)
_cell_length_c                   17.5202(9)
_cell_measurement_reflns_used    1204
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.682
_cell_measurement_theta_min      2.91
_cell_volume                     2899.7(3)
_computing_cell_refinement       'HKL Scalepack (Otwinowsky & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
HKL Denzo and Scalepack (Otwinowsky & Minor, 1997)
;
_computing_molecular_graphics    'SHELXTL/PC (Sheldrick, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_monochromator  'horizonally mounted graphite crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Mok\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0684
_diffrn_reflns_av_sigmaI/netI    0.0569
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            6423
_diffrn_reflns_theta_full        25.66
_diffrn_reflns_theta_max         25.66
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    8.559
_exptl_absorpt_correction_T_max  0.6013
_exptl_absorpt_correction_T_min  0.1918
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Sheldrick, G.M. (anon) SHELX97 Release 97-2 (1998)
I/sigma threshold for reflections = 5.000
Delta(U)/lambda**2 = 0.000
Highest even order spherical harmonic = 6
Highest odd order spherical harmonic = 3
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2216
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.809
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.44(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2364
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_gt           0.0407
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
w=1/[σ²(Fo²)+(0.0360P)²+24.2974P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0923
_reflns_number_gt                1974
_reflns_number_total             2364
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b701787a.txt
_cod_data_source_block           '[HNMe3]2[3]'
_cod_database_code               7005391
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_rmerge_before     0.0914
_exptl_absorpt_rmerge_after      0.0486
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/2, -y, z'
'-x+1/2, y, z'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.2500 0.79243(10) 1.0000 0.0500(5) Uani 1 d S . .
I2 I 0.54439(12) 0.64866(7) 0.92218(12) 0.0523(4) Uani 1 d . . .
I6 I 0.43060(7) 0.88663(5) 0.81601(12) 0.0469(2) Uani 1 d . . .
I10 I 0.2500 0.81354(10) 0.62452(9) 0.0517(5) Uani 1 d S . .
I11 I 0.54332(12) 0.65479(7) 0.69260(11) 0.0511(4) Uani 1 d . . .
B1 B 0.2500 0.7157(15) 0.8915(13) 0.039(7) Uani 1 d S . .
B2 B 0.3791(19) 0.6627(11) 0.8603(10) 0.033(4) Uani 1 d D . .
B3 B 0.2500 0.6025(13) 0.8859(11) 0.033(5) Uani 1 d SD . .
H3 H 0.2500 0.5579 0.9374 0.039 Uiso 1 calc SR . .
B6 B 0.3318(11) 0.7602(8) 0.8064(11) 0.033(3) Uani 1 d . . .
C7 C 0.3204(10) 0.5787(8) 0.7997(8) 0.035(3) Uani 1 d D . .
H7 H 0.374(4) 0.515(2) 0.794(3) 0.042 Uiso 1 d D . .
B10 B 0.2500 0.7300(16) 0.7262(12) 0.025(5) Uani 1 d S . .
B11 B 0.372(2) 0.6647(11) 0.7556(11) 0.038(5) Uani 1 d . . .
N13 N 0.2500 0.6205(13) 1.1529(11) 0.061(5) Uani 1 d SD . .
H13 H 0.2500 0.6787 1.1337 0.073 Uiso 1 calc SR . .
C14 C 0.2500 0.6318(18) 1.2362(14) 0.076(8) Uani 1 d SD . .
H14A H 0.2009 0.5846 1.2596 0.114 Uiso 0.50 calc PR . .
H14B H 0.2165 0.6907 1.2492 0.114 Uiso 0.50 calc PR . .
H14C H 0.3327 0.6276 1.2554 0.114 Uiso 0.50 calc PR . .
C15 C 0.360(2) 0.5769(13) 1.1178(12) 0.077(6) Uani 1 d . . .
H15A H 0.3610 0.5129 1.1308 0.115 Uiso 1 calc R . .
H15B H 0.4327 0.6058 1.1375 0.115 Uiso 1 calc R . .
H15C H 0.3569 0.5837 1.0622 0.115 Uiso 1 calc R . .
N16 N 0.2500 0.6003(15) 0.5357(12) 0.088(7) Uani 1 d SDU . .
H16 H 0.2500 0.6567 0.5585 0.106 Uiso 1 calc SR . .
C17 C 0.2500 0.5336(16) 0.6011(13) 0.070(7) Uani 1 d SD . .
H17A H 0.3316 0.5283 0.6219 0.105 Uiso 0.50 calc PR . .
H17B H 0.2231 0.4749 0.5825 0.105 Uiso 0.50 calc PR . .
H17C H 0.1953 0.5546 0.6412 0.105 Uiso 0.50 calc PR . .
C18 C 0.370(3) 0.592(2) 0.497(2) 0.179(16) Uani 1 d DU . .
H18A H 0.4327 0.6168 0.5298 0.268 Uiso 1 calc R . .
H18B H 0.3679 0.6264 0.4487 0.268 Uiso 1 calc R . .
H18C H 0.3866 0.5292 0.4857 0.268 Uiso 1 calc R . .
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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
B3 B1 B2 61.6(9) . 4 ?
B3 B1 B2 61.6(9) . . ?
B2 B1 B2 112.3(16) 4 . ?
B3 B1 B6 107.9(12) . 4 ?
B2 B1 B6 60.3(9) 4 4 ?
B2 B1 B6 108.3(14) . 4 ?
B3 B1 B6 107.9(12) . . ?
B2 B1 B6 108.3(14) 4 . ?
B2 B1 B6 60.3(9) . . ?
B6 B1 B6 58.2(11) 4 . ?
B3 B1 I1 124.4(15) . . ?
B2 B1 I1 120.5(9) 4 . ?
B2 B1 I1 120.5(9) . . ?
B6 B1 I1 120.1(11) 4 . ?
B6 B1 I1 120.1(11) . . ?
B1 B2 B3 58.1(11) . . ?
B1 B2 C7 102.0(12) . . ?
B3 B2 C7 59.2(9) . . ?
B1 B2 B6 63.7(12) . . ?
B3 B2 B6 107.9(12) . . ?
C7 B2 B6 98.5(10) . . ?
B1 B2 B11 105.9(16) . . ?
B3 B2 B11 103.3(16) . . ?
C7 B2 B11 52.8(9) . . ?
B6 B2 B11 56.9(10) . . ?
B1 B2 I2 126.6(11) . . ?
B3 B2 I2 121.5(10) . . ?
C7 B2 I2 123.5(10) . . ?
B6 B2 I2 126.2(10) . . ?
B11 B2 I2 122.9(17) . . ?
B1 B3 C7 104.7(12) . 4 ?
B1 B3 C7 104.7(12) . . ?
C7 B3 C7 53.6(10) 4 . ?
B1 B3 B2 60.3(8) . . ?
C7 B3 B2 104.5(12) 4 . ?
C7 B3 B2 60.8(8) . . ?
B1 B3 B2 60.3(8) . 4 ?
C7 B3 B2 60.8(8) 4 4 ?
C7 B3 B2 104.5(12) . 4 ?
B2 B3 B2 110.1(16) . 4 ?
B1 B3 H3 123.0 . . ?
C7 B3 H3 125.4 4 . ?
C7 B3 H3 125.4 . . ?
B2 B3 H3 120.7 . . ?
B2 B3 H3 120.7 4 . ?
B10 B6 B11 60.5(11) . . ?
B10 B6 B2 111.5(12) . . ?
B11 B6 B2 62.3(7) . . ?
B10 B6 B6 58.3(6) . 4 ?
B11 B6 B6 105.0(9) . 4 ?
B2 B6 B6 106.8(8) . 4 ?
B10 B6 B1 107.4(8) . . ?
B11 B6 B1 104.1(11) . . ?
B2 B6 B1 55.9(10) . . ?
B6 B6 B1 60.9(5) 4 . ?
B10 B6 I6 123.4(11) . . ?
B11 B6 I6 128.0(11) . . ?
B2 B6 I6 120.4(9) . . ?
B6 B6 I6 120.1(3) 4 . ?
B1 B6 I6 119.2(11) . . ?
C7 C7 B11 111.0(10) 4 . ?
C7 C7 B3 63.2(5) 4 . ?
B11 C7 B3 114.7(11) . . ?
C7 C7 B2 111.7(7) 4 . ?
B11 C7 B2 65.9(7) . . ?
B3 C7 B2 59.9(9) . . ?
C7 C7 H7 122(2) 4 . ?
B11 C7 H7 116(3) . . ?
B3 C7 H7 120(3) . . ?
B2 C7 H7 118(2) . . ?
B6 B10 B6 63.3(13) . 4 ?
B6 B10 B11 108.3(14) . 4 ?
B6 B10 B11 59.9(9) 4 4 ?
B6 B10 B11 59.9(9) . . ?
B6 B10 B11 108.3(14) 4 . ?
B11 B10 B11 101.9(18) 4 . ?
B6 B10 I10 121.1(11) . . ?
B6 B10 I10 121.1(11) 4 . ?
B11 B10 I10 124.1(10) 4 . ?
B11 B10 I10 124.1(10) . . ?
C7 B11 B6 108.3(13) . . ?
C7 B11 B10 107.9(16) . . ?
B6 B11 B10 59.6(11) . . ?
C7 B11 B2 61.3(10) . . ?
B6 B11 B2 60.8(10) . . ?
B10 B11 B2 109.6(16) . . ?
C7 B11 I11 119.9(11) . . ?
B6 B11 I11 122.3(12) . . ?
B10 B11 I11 124.1(11) . . ?
B2 B11 I11 117.6(17) . . ?
C14 N13 C15 117.0(13) . 4 ?
C14 N13 C15 117.0(12) . . ?
C15 N13 C15 107(2) 4 . ?
C14 N13 H13 104.7 . . ?
C15 N13 H13 104.7 4 . ?
C15 N13 H13 104.7 . . ?
N13 C14 H14A 109.5 . . ?
N13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N13 C15 H15A 109.5 . . ?
N13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C18 N16 C18 125(3) 4 . ?
C18 N16 C17 107.1(19) 4 . ?
C18 N16 C17 107.1(18) . . ?
C18 N16 H16 105.5 4 . ?
C18 N16 H16 105.5 . . ?
C17 N16 H16 105.5 . . ?
N16 C17 H17A 109.5 . . ?
N16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N16 C18 H18A 109.5 . . ?
N16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
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 B1 2.22(2) . ?
I2 B2 2.143(19) . ?
I6 B6 2.186(12) . ?
I10 B10 2.17(2) . ?
I11 B11 2.20(2) . ?
B1 B3 1.69(3) . ?
B1 B2 1.73(2) 4 ?
B1 B2 1.73(2) . ?
B1 B6 1.87(3) 4 ?
B1 B6 1.87(3) . ?
B2 B3 1.75(2) . ?
B2 C7 1.76(2) . ?
B2 B6 1.81(2) . ?
B2 B11 1.836(16) . ?
B3 C7 1.74(2) 4 ?
B3 C7 1.74(2) . ?
B3 B2 1.75(2) 4 ?
B3 H3 1.1200 . ?
B6 B10 1.73(2) . ?
B6 B11 1.74(2) . ?
B6 B6 1.82(2) 4 ?
C7 C7 1.57(2) 4 ?
C7 B11 1.60(2) . ?
C7 H7 1.13(2) . ?
B10 B6 1.73(2) 4 ?
B10 B11 1.75(2) 4 ?
B10 B11 1.75(2) . ?
N13 C14 1.47(2) . ?
N13 C15 1.51(2) 4 ?
N13 C15 1.51(2) . ?
N13 H13 0.9300 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
N16 C18 1.50(3) 4 ?
N16 C18 1.50(3) . ?
N16 C17 1.52(2) . ?
N16 H16 0.9300 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N13 H13 I1 0.93 2.89 3.706(19) 147.1 .
N16 H16 I10 0.93 2.61 3.54(2) 179.1 .
