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#$Date: 2016-03-25 16:09:15 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179954 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/49/7024927.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_7024927
loop_
_publ_author_name
'Finze, Maik'
'Sprenger, Jan A. P.'
'Schaack, Bernd Bastian'
_publ_section_title
;
 Salts of the 1-cyanocarba-closo-dodecaborate anions
 [1-NC-closo-1-CB11X11]- (X = H, F, Cl, Br, I).
;
_journal_issue                   10
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2708
_journal_page_last               2716
_journal_paper_doi               10.1039/b922720b
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C2 B11 Cl11 N, Cs'
_chemical_formula_sum            'C2 B11 Cl11 Cs N'
_chemical_formula_weight         679.80
_chemical_name_common
Caesium-1-cyanoundecachloridocarba-closo-dodecaborate
_chemical_name_systematic
;
Caesium-1-cyanoundecachloridocarba-closo-dodecaborate
;
_space_group_IT_number           142
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4bd 2c'
_symmetry_space_group_name_H-M   'I 41/a c d :2'
_atom_sites_solution_hydrogens   none
_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            16
_cell_length_a                   18.638(3)
_cell_length_b                   18.638(3)
_cell_length_c                   24.499(4)
_cell_measurement_reflns_used    3672
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      5.16
_cell_volume                     8510(2)
_computing_cell_refinement       'CrysAlis RED (Kuma 2000)'
_computing_data_collection       'CrysAlis CCD (KUMA, 2000)'
_computing_data_reduction        'CrysAlis RED (Kuma 2000)'
_computing_molecular_graphics    'Diamond 3.1f (Brandeburger, 2008)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Stoe STADI CCD'
_diffrn_measurement_method       omega
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16987
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         5.16
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.112
_exptl_absorpt_correction_T_max  0.7401
_exptl_absorpt_correction_T_min  0.5641
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'X-RED 1.20 (Stoe & Cie, 1996)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5056
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.622
_refine_diff_density_min         -0.549
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     135
_refine_ls_number_reflns         1859
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0382
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0540P)²+3.2000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0842
_reflns_number_gt                1553
_reflns_number_total             1859
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b922720b.txt
_cod_data_source_block           Cs[1-NC-closo-1-CB11Cl11]
_cod_original_cell_volume        8510(3)
_cod_original_sg_symbol_H-M      'I 41/acd'
_cod_database_code               7024927
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'
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
Cs1 Cs 0.2500 0.19668(2) 0.0000 0.05118(17) Uani 1 2 d S . .
B2 B 0.20405(18) 0.26584(19) 0.30902(13) 0.0265(7) Uani 1 1 d . . .
Cl2 Cl 0.15276(5) 0.28508(6) 0.36783(4) 0.0476(3) Uani 1 1 d . . .
B3 B 0.20240(18) 0.2508(2) 0.19040(13) 0.0273(8) Uani 1 1 d . . .
Cl3 Cl 0.15013(5) 0.25409(7) 0.13041(4) 0.0546(3) Uani 1 1 d . A .
B4 B 0.16469(19) 0.21738(18) 0.25343(14) 0.0266(7) Uani 1 1 d . . .
Cl4 Cl 0.07444(4) 0.18892(5) 0.25582(4) 0.0439(2) Uani 1 1 d . . .
B5 B 0.26629(19) 0.33057(19) 0.28065(15) 0.0290(8) Uani 1 1 d . . .
Cl5 Cl 0.27867(5) 0.41552(5) 0.31071(4) 0.0523(3) Uani 1 1 d . . .
B6 B 0.26517(18) 0.32099(19) 0.20765(15) 0.0278(8) Uani 1 1 d . . .
Cl6 Cl 0.27653(6) 0.39594(5) 0.16435(4) 0.0539(3) Uani 1 1 d . . .
B1 B 0.1820(19) 0.314(2) 0.247(4) 0.0233(14) Uani 0.50 1 d PD A 1
Cl1 Cl 0.1129(3) 0.3784(2) 0.2423(2) 0.0462(12) Uani 0.50 1 d PDU A 1
C1 C 0.1888(16) 0.3047(18) 0.246(3) 0.0233(14) Uani 0.50 1 d PD A 2
C2 C 0.1312(6) 0.3577(6) 0.2435(7) 0.033(4) Uani 0.50 1 d PD A 2
N1 N 0.0913(7) 0.3973(7) 0.2447(6) 0.042(2) Uani 0.50 1 d P A 2
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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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'
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
N1 Cs1 N1 70.9(5) 10_544 14_444
N1 Cs1 Cl4 131.6(2) 10_544 8
N1 Cs1 Cl4 61.1(2) 14_444 8
N1 Cs1 Cl4 61.1(2) 10_544 4_554
N1 Cs1 Cl4 131.6(2) 14_444 4_554
Cl4 Cs1 Cl4 167.25(3) 8 4_554
N1 Cs1 Cl2 71.2(3) 10_544 25
N1 Cs1 Cl2 100.0(3) 14_444 25
Cl4 Cs1 Cl2 121.87(2) 8 25
Cl4 Cs1 Cl2 59.48(2) 4_554 25
N1 Cs1 Cl2 100.0(3) 10_544 31_554
N1 Cs1 Cl2 71.2(3) 14_444 31_554
Cl4 Cs1 Cl2 59.48(2) 8 31_554
Cl4 Cs1 Cl2 121.87(2) 4_554 31_554
Cl2 Cs1 Cl2 169.53(3) 25 31_554
N1 Cs1 Cl5 157.6(3) 10_544 24
N1 Cs1 Cl5 114.5(2) 14_444 24
Cl4 Cs1 Cl5 60.905(19) 8 24
Cl4 Cs1 Cl5 107.67(2) 4_554 24
Cl2 Cs1 Cl5 86.37(2) 25 24
Cl2 Cs1 Cl5 102.32(2) 31_554 24
N1 Cs1 Cl5 114.5(2) 10_544 20_656
N1 Cs1 Cl5 157.6(3) 14_444 20_656
Cl4 Cs1 Cl5 107.67(2) 8 20_656
Cl4 Cs1 Cl5 60.905(19) 4_554 20_656
Cl2 Cs1 Cl5 102.32(2) 25 20_656
Cl2 Cs1 Cl5 86.37(2) 31_554 20_656
Cl5 Cs1 Cl5 69.34(4) 24 20_656
N1 Cs1 Cl1 1.0(3) 10_544 10_544
N1 Cs1 Cl1 71.7(2) 14_444 10_544
Cl4 Cs1 Cl1 132.30(8) 8 10_544
Cl4 Cs1 Cl1 60.40(8) 4_554 10_544
Cl2 Cs1 Cl1 71.49(9) 25 10_544
Cl2 Cs1 Cl1 99.81(9) 31_554 10_544
Cl5 Cs1 Cl1 157.83(9) 24 10_544
Cl5 Cs1 Cl1 113.58(8) 20_656 10_544
N1 Cs1 Cl1 71.7(2) 10_544 14_444
N1 Cs1 Cl1 1.0(3) 14_444 14_444
Cl4 Cs1 Cl1 60.40(8) 8 14_444
Cl4 Cs1 Cl1 132.30(8) 4_554 14_444
Cl2 Cs1 Cl1 99.81(9) 25 14_444
Cl2 Cs1 Cl1 71.49(9) 31_554 14_444
Cl5 Cs1 Cl1 113.58(8) 24 14_444
Cl5 Cs1 Cl1 157.83(9) 20_656 14_444
Cl1 Cs1 Cl1 72.54(16) 10_544 14_444
N1 Cs1 Cl3 57.4(3) 10_544 7
N1 Cs1 Cl3 94.9(3) 14_444 7
Cl4 Cs1 Cl3 118.53(2) 8 7
Cl4 Cs1 Cl3 65.42(2) 4_554 7
Cl2 Cs1 Cl3 117.43(2) 25 7
Cl2 Cs1 Cl3 59.24(2) 31_554 7
Cl5 Cs1 Cl3 138.83(3) 24 7
Cl5 Cs1 Cl3 72.81(3) 20_656 7
Cl1 Cs1 Cl3 56.63(9) 10_544 7
Cl1 Cs1 Cl3 95.84(9) 14_444 7
N1 Cs1 Cl3 94.9(3) 10_544 .
N1 Cs1 Cl3 57.4(3) 14_444 .
Cl4 Cs1 Cl3 65.42(2) 8 .
Cl4 Cs1 Cl3 118.53(2) 4_554 .
Cl2 Cs1 Cl3 59.24(2) 25 .
Cl2 Cs1 Cl3 117.43(2) 31_554 .
Cl5 Cs1 Cl3 72.81(3) 24 .
Cl5 Cs1 Cl3 138.83(3) 20_656 .
Cl1 Cs1 Cl3 95.84(9) 10_544 .
Cl1 Cs1 Cl3 56.63(9) 14_444 .
Cl3 Cs1 Cl3 147.72(4) 7 .
C1 B2 B6 103.3(15) . 25
C1 B2 Cl2 123.7(12) . .
B6 B2 Cl2 123.4(2) 25 .
C1 B2 B3 104.0(11) . 25
B6 B2 B3 61.4(2) 25 25
Cl2 B2 B3 124.2(2) . 25
C1 B2 B4 57.6(17) . .
B6 B2 B4 59.66(19) 25 .
Cl2 B2 B4 120.1(2) . .
B3 B2 B4 108.7(2) 25 .
C1 B2 B5 59.0(15) . .
B6 B2 B5 108.3(2) 25 .
Cl2 B2 B5 121.6(2) . .
B3 B2 B5 59.28(19) 25 .
B4 B2 B5 107.8(2) . .
C1 B2 B1 6(3) . .
B6 B2 B1 109(2) 25 .
Cl2 B2 B1 117.5(16) . .
B3 B2 B1 108.4(14) 25 .
B4 B2 B1 61(2) . .
B5 B2 B1 59.5(16) . .
B2 Cl2 Cs1 117.66(12) . 25
C1 B3 Cl3 124.1(12) . .
C1 B3 B2 104.0(11) . 25
Cl3 B3 B2 123.8(2) . 25
C1 B3 B5 103.4(16) . 25
Cl3 B3 B5 123.1(2) . 25
B2 B3 B5 61.52(19) 25 25
C1 B3 B6 59.0(15) . .
Cl3 B3 B6 121.8(2) . .
B2 B3 B6 59.12(19) 25 .
B5 B3 B6 108.2(2) 25 .
C1 B3 B4 57.6(18) . .
Cl3 B3 B4 120.6(2) . .
B2 B3 B4 108.4(2) 25 .
B5 B3 B4 59.45(19) 25 .
B6 B3 B4 107.5(2) . .
C1 B3 B1 5(3) . .
Cl3 B3 B1 118.9(16) . .
B2 B3 B1 107.9(13) 25 .
B5 B3 B1 108.4(19) 25 .
B6 B3 B1 59.8(16) . .
B4 B3 B1 60(2) . .
B3 Cl3 Cs1 114.50(12) . .
C1 B4 Cl4 122.9(7) . .
C1 B4 B6 104.5(16) . 25
Cl4 B4 B6 124.4(2) . 25
C1 B4 B5 103.9(16) . 25
Cl4 B4 B5 123.7(2) . 25
B6 B4 B5 60.9(2) 25 25
C1 B4 B2 59(3) . .
Cl4 B4 B2 121.1(2) . .
B6 B4 B2 59.4(2) 25 .
B5 B4 B2 108.3(2) 25 .
C1 B4 B3 58(3) . .
Cl4 B4 B3 120.2(2) . .
B6 B4 B3 108.2(2) 25 .
B5 B4 B3 59.3(2) 25 .
B2 B4 B3 108.5(2) . .
C1 B4 B1 5(2) . .
Cl4 B4 B1 117.7(9) . .
B6 B4 B1 108.4(18) 25 .
B5 B4 B1 108.9(18) 25 .
B2 B4 B1 60(3) . .
B3 B4 B1 61(3) . .
B4 Cl4 Cs1 113.77(11) . 2_545
C1 B5 Cl5 124.1(9) . .
C1 B5 B3 103.3(11) . 25
Cl5 B5 B3 123.9(2) . 25
C1 B5 B4 103.4(18) . 25
Cl5 B5 B4 123.7(2) . 25
B3 B5 B4 61.2(2) 25 25
C1 B5 B6 59(2) . .
Cl5 B5 B6 120.5(2) . .
B3 B5 B6 108.5(2) 25 .
B4 B5 B6 59.36(19) 25 .
C1 B5 B1 7(2) . .
Cl5 B5 B1 117.3(12) . .
B3 B5 B1 109.1(13) 25 .
B4 B5 B1 109(2) 25 .
B6 B5 B1 61(3) . .
C1 B5 B2 58(2) . .
Cl5 B5 B2 121.5(2) . .
B3 B5 B2 59.20(19) 25 .
B4 B5 B2 108.0(2) 25 .
B6 B5 B2 107.9(2) . .
B1 B5 B2 61(2) . .
B5 Cl5 Cs1 108.43(12) . 26_565
C1 B6 B2 103.4(11) . 25
C1 B6 Cl6 124.3(10) . .
B2 B6 Cl6 123.2(2) 25 .
C1 B6 B4 104.1(18) . 25
B2 B6 B4 60.91(19) 25 25
Cl6 B6 B4 123.7(2) . 25
C1 B6 B5 59(2) . .
B2 B6 B5 108.5(2) 25 .
Cl6 B6 B5 121.2(2) . .
B4 B6 B5 59.69(19) 25 .
C1 B6 B3 58(2) . .
B2 B6 B3 59.4(2) 25 .
Cl6 B6 B3 120.7(2) . .
B4 B6 B3 108.2(2) 25 .
B5 B6 B3 108.2(2) . .
C1 B6 B1 6.4(18) . .
B2 B6 B1 109.5(12) 25 .
Cl6 B6 B1 118.0(12) . .
B4 B6 B1 109(2) 25 .
B5 B6 B1 60(3) . .
B3 B6 B1 61(2) . .
Cl1 B1 B5 123(3) . .
Cl1 B1 B2 123(5) . .
B5 B1 B2 60(2) . .
Cl1 B1 B6 123(4) . .
B5 B1 B6 59.4(13) . .
B2 B1 B6 106.3(14) . .
Cl1 B1 B4 123(3) . .
B5 B1 B4 106(2) . .
B2 B1 B4 58.5(17) . .
B6 B1 B4 105(2) . .
Cl1 B1 B3 123(5) . .
B5 B1 B3 105.8(16) . .
B2 B1 B3 105.1(12) . .
B6 B1 B3 59(2) . .
B4 B1 B3 58.5(17) . .
B1 Cl1 Cs1 171(2) . 12_454
C2 C1 B4 117(2) . .
C2 C1 B3 118(4) . .
B4 C1 B3 64.0(18) . .
C2 C1 B2 116(4) . .
B4 C1 B2 63.0(18) . .
B3 C1 B2 116.1(13) . .
C2 C1 B6 118(3) . .
B4 C1 B6 116(2) . .
B3 C1 B6 63(2) . .
B2 C1 B6 115.0(18) . .
C2 C1 B5 116(3) . .
B4 C1 B5 116(2) . .
B3 C1 B5 115.3(18) . .
B2 C1 B5 63(2) . .
B6 C1 B5 62.3(13) . .
N1 C2 C1 175(4) . .
C2 N1 Cs1 170.7(16) . 12_454
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cs1 N1 3.308(11) 10_544
Cs1 N1 3.308(11) 14_444
Cs1 Cl4 3.5458(11) 8
Cs1 Cl4 3.5458(11) 4_554
Cs1 Cl2 3.7263(11) 25
Cs1 Cl2 3.7263(11) 31_554
Cs1 Cl5 3.8074(12) 24
Cs1 Cl5 3.8074(12) 20_656
Cs1 Cl1 3.843(4) 10_544
Cs1 Cl1 3.843(4) 14_444
Cs1 Cl3 3.8492(11) 7
Cs1 Cl3 3.8492(11) .
B2 C1 1.73(7) .
B2 B6 1.765(5) 25
B2 Cl2 1.766(3) .
B2 B3 1.771(5) 25
B2 B4 1.791(5) .
B2 B5 1.812(5) .
B2 B1 1.82(8) .
Cl2 Cs1 3.7263(11) 25
B3 C1 1.71(7) .
B3 Cl3 1.764(3) .
B3 B2 1.771(5) 25
B3 B5 1.772(5) 25
B3 B6 1.806(5) .
B3 B4 1.807(5) .
B3 B1 1.86(8) .
B4 C1 1.70(4) .
B4 Cl4 1.765(4) .
B4 B6 1.769(5) 25
B4 B5 1.775(5) 25
B4 B1 1.84(4) .
Cl4 Cs1 3.5458(11) 2_545
B5 C1 1.74(5) .
B5 Cl5 1.761(4) .
B5 B3 1.772(5) 25
B5 B4 1.775(5) 25
B5 B6 1.797(5) .
B5 B1 1.80(6) .
Cl5 Cs1 3.8074(12) 26_565
B6 C1 1.73(5) .
B6 B2 1.765(5) 25
B6 Cl6 1.767(4) .
B6 B4 1.769(5) 25
B6 B1 1.82(6) .
B1 Cl1 1.7601(11) .
Cl1 Cs1 3.843(4) 12_454
C1 C2 1.4602(11) .
C2 N1 1.048(14) .
N1 Cs1 3.308(11) 12_454
