# Supplementary Material (ESI) for Dalton Transactions
# This journal is (c) The Royal Society of Chemistry 2010
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
loop_
_publ_author_address
; Institut f\"ur Anorganische Chemie und Strukturchemie II
Heinrich-Heine-Universit\"at D\"usseldorf
Universit\"atsstrasse 1
D-40225 D\"usseldorf
Germany
;
; Institut f\"ur Anorganische Chemie und Strukturchemie II
Heinrich-Heine-Universit\"at D\"usseldorf
Universit\"atsstrasse 1
D-40225 D\"usseldorf
Germany
;
; Max-Planck-Institut f\"ur Kohlenforschung
Kaiser-Wilhelm-Platz 1
D-45470 M\"ulheim an der Ruhr
Germany
;
_publ_contact_author_name 'Maik Finze'
_publ_contact_author_email MAIK.FINZE@UNI-DUESSELDORF.DE
_publ_section_title
;
Salts of the 1-Cyanocarba-closo-dodecaborate
Anions [1-NC-closo-1-CB11X11]- (X = H, F, Cl, Br, I)
;
_publ_contact_author_address
; Institut fuer Anorganische Chemie und Strukturchemie II
Heinrich Heine Universitaet Duesseldorf
Universitaetsstrasse 1
D-40225 Duesseldorf
Germany
;
_publ_contact_author_fax '049 211 81 14146'
_publ_contact_author_phone '049 211 81 13144'
_publ_author_name 'Maik Finze'
# Attachment 'Et4NNCCB11H11.cif'
data_[Et4N][1-NC-closo-1-CB11H11]
_database_code_depnum_ccdc_archive 'CCDC 752154'
#=================================================================
#DATA 1
#=================================================================
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Tetraethylammonium-1-cyanocarba-closo-dodecaborate
;
_chemical_name_common
Tetraethylammonium-1-cyanocarba-closo-dodecaborate
_chemical_melting_point ?
_chemical_formula_moiety 'C8 H20 N, C2 H11 B11 N'
_chemical_formula_sum 'C10 H31 B11 N2'
_chemical_formula_weight 298.28
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 'P 21/c'
_symmetry_space_group_name_Hall '-P 2ybc'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 9.0592(18)
_cell_length_b 10.065(2)
_cell_length_c 10.736(2)
_cell_angle_alpha 90.00
_cell_angle_beta 99.91(3)
_cell_angle_gamma 90.00
_cell_volume 964.3(3)
_cell_formula_units_Z 2
_cell_measurement_temperature 123(2)
_cell_measurement_reflns_used 2000
_cell_measurement_theta_min 2.28
_cell_measurement_theta_max 25.30
_exptl_crystal_description parallelepiped
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.09
_exptl_crystal_size_mid 0.09
_exptl_crystal_size_min 0.06
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.027
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 320
_exptl_absorpt_coefficient_mu 0.051
_exptl_absorpt_correction_type none
_exptl_absorpt_correction_T_min ?
_exptl_absorpt_correction_T_max ?
_exptl_absorpt_process_details ?
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 123(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 'Stoe IPDS'
_diffrn_measurement_method \f-scans
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 8931
_diffrn_reflns_av_R_equivalents 0.0806
_diffrn_reflns_av_sigmaI/netI 0.0970
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_h_max 10
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 12
_diffrn_reflns_theta_min 2.28
_diffrn_reflns_theta_max 25.30
_reflns_number_total 1751
_reflns_number_gt 735
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'EXPOSE (Stoe & Cie, 1996)'
_computing_cell_refinement 'CELL (Stoe & Cie, 1996)'
_computing_data_reduction 'INTEGRATE (Stoe & Cie, 1996)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Diamond3.1 (Crystal Impact GbR, 2006)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0281P)^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 constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1751
_refine_ls_number_parameters 142
_refine_ls_number_restraints 20
_refine_ls_R_factor_all 0.1257
_refine_ls_R_factor_gt 0.0541
_refine_ls_wR_factor_ref 0.0969
_refine_ls_wR_factor_gt 0.0904
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_restrained_S_all 1.056
_refine_ls_shift/su_max 0.000
_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
C1 C 0.6334(9) 1.0328(7) 0.4533(6) 0.099(5) Uani 0.50 1 d PDU A 1
C2 C 0.7573(7) 1.0649(4) 0.4095(4) 0.0775(13) Uani 0.50 1 d P A 1
N2 N 0.8653(5) 1.0929(4) 0.3716(3) 0.1087(14) Uani 0.50 1 d P A 1
B1 B 0.6568(10) 1.0379(7) 0.4446(6) 0.070(4) Uani 0.50 1 d PDU A 2
H1 H 0.7599 1.0627 0.4084 0.091 Uiso 0.50 1 calc PR A 2
B2 B 0.6260(3) 1.0928(2) 0.5962(2) 0.0824(8) Uani 1 1 d D . .
H2 H 0.7106 1.1534 0.6566 0.107 Uiso 1 1 calc R A 1
B3 B 0.6566(3) 0.9209(2) 0.5686(2) 0.0835(8) Uani 1 1 d D . .
H3 H 0.7611 0.8709 0.6113 0.109 Uiso 1 1 calc R B 1
B4 B 0.5653(3) 0.8823(2) 0.4130(2) 0.0839(8) Uani 1 1 d D . .
H4 H 0.6110 0.8073 0.3555 0.109 Uiso 1 1 calc R A 1
B5 B 0.4790(3) 1.0296(2) 0.3432(2) 0.0822(8) Uani 1 1 d D . .
H5 H 0.4694 1.0495 0.2414 0.107 Uiso 1 1 calc R C 1
B6 B 0.5160(3) 1.1593(2) 0.4569(2) 0.0861(8) Uani 1 1 d . . .
H6 H 0.5298 1.2627 0.4277 0.112 Uiso 1 1 calc R D 1
N1 N 1.0000 0.5000 0.5000 0.0551(6) Uani 1 2 d S . .
C10 C 1.0642(5) 0.4427(3) 0.6242(3) 0.0705(8) Uani 0.50 1 d P E -1
H10A H 1.0135 0.4822 0.6877 0.092 Uiso 0.50 1 calc PR E -1
H10B H 1.1689 0.4682 0.6443 0.092 Uiso 0.50 1 calc PR E -1
C11 C 1.054(2) 0.2930(18) 0.6345(19) 0.086(3) Uani 0.50 1 d P E -1
H11A H 1.0998 0.2655 0.7179 0.129 Uiso 0.50 1 calc PR E -1
H11B H 1.1058 0.2523 0.5734 0.129 Uiso 0.50 1 calc PR E -1
H11C H 0.9510 0.2664 0.6186 0.129 Uiso 0.50 1 calc PR E -1
C12 C 1.0258(4) 0.6525(4) 0.5097(3) 0.0705(8) Uani 0.50 1 d P E -1
H12A H 0.9736 0.6863 0.5748 0.092 Uiso 0.50 1 calc PR E -1
H12B H 1.1319 0.6679 0.5382 0.092 Uiso 0.50 1 calc PR E -1
C13 C 0.978(2) 0.7321(19) 0.3937(18) 0.086(3) Uani 0.50 1 d P E -1
H13A H 0.9996 0.8242 0.4117 0.129 Uiso 0.50 1 calc PR E -1
H13B H 0.8724 0.7209 0.3654 0.129 Uiso 0.50 1 calc PR E -1
H13C H 1.0315 0.7028 0.3288 0.129 Uiso 0.50 1 calc PR E -1
C14 C 0.8360(4) 0.4704(4) 0.4579(3) 0.0720(8) Uani 0.50 1 d P E -1
H14A H 0.8023 0.5154 0.3782 0.094 Uiso 0.50 1 calc PR E -1
H14B H 0.8245 0.3757 0.4425 0.094 Uiso 0.50 1 calc PR E -1
C15 C 0.738(3) 0.510(2) 0.5473(19) 0.096(3) Uani 0.50 1 d P E -1
H15A H 0.6364 0.4859 0.5133 0.144 Uiso 0.50 1 calc PR E -1
H15B H 0.7447 0.6038 0.5606 0.144 Uiso 0.50 1 calc PR E -1
H15C H 0.7690 0.4646 0.6263 0.144 Uiso 0.50 1 calc PR E -1
C16 C 1.0799(4) 0.4478(4) 0.3957(3) 0.0720(8) Uani 0.50 1 d P E -1
H16A H 1.0579 0.3538 0.3847 0.094 Uiso 0.50 1 calc PR E -1
H16B H 1.0375 0.4918 0.3173 0.094 Uiso 0.50 1 calc PR E -1
C17 C 1.249(3) 0.465(2) 0.416(2) 0.096(3) Uani 0.50 1 d P E -1
H17A H 1.2880 0.4280 0.3461 0.144 Uiso 0.50 1 calc PR E -1
H17B H 1.2939 0.4211 0.4928 0.144 Uiso 0.50 1 calc PR E -1
H17C H 1.2734 0.5584 0.4229 0.144 Uiso 0.50 1 calc PR E -1
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
C1 0.097(5) 0.102(5) 0.096(5) -0.006(3) 0.014(3) 0.001(3)
C2 0.087(4) 0.085(3) 0.060(3) -0.012(2) 0.010(3) -0.009(3)
N2 0.105(3) 0.139(4) 0.085(3) -0.006(2) 0.026(2) -0.020(3)
B1 0.071(5) 0.071(4) 0.064(4) -0.011(2) -0.001(3) 0.004(3)
B2 0.088(2) 0.0798(17) 0.0717(15) -0.0155(13) -0.0073(14) 0.0059(15)
B3 0.087(2) 0.0758(17) 0.0769(16) -0.0033(14) -0.0174(14) 0.0177(16)
B4 0.092(2) 0.0697(16) 0.0826(16) -0.0173(14) -0.0059(14) 0.0136(16)
B5 0.084(2) 0.0873(17) 0.0666(14) -0.0059(13) -0.0122(13) 0.0111(15)
B6 0.101(2) 0.0637(17) 0.0862(18) -0.0052(13) -0.0047(15) 0.0151(15)
N1 0.0563(16) 0.0574(15) 0.0492(13) -0.0062(11) 0.0024(11) -0.0011(12)
C10 0.076(2) 0.069(2) 0.0634(17) 0.0007(14) 0.0045(15) -0.0017(16)
C11 0.076(8) 0.077(5) 0.099(7) 0.017(4) -0.001(5) -0.001(4)
C12 0.076(2) 0.069(2) 0.0634(17) 0.0007(14) 0.0045(15) -0.0017(16)
C13 0.076(8) 0.077(5) 0.099(7) 0.017(4) -0.001(5) -0.001(4)
C14 0.069(2) 0.0742(18) 0.0709(17) -0.0060(14) 0.0053(16) 0.0012(16)
C15 0.083(3) 0.087(8) 0.125(10) -0.003(6) 0.041(6) 0.011(4)
C16 0.069(2) 0.0742(18) 0.0709(17) -0.0060(14) 0.0053(16) 0.0012(16)
C17 0.083(3) 0.087(8) 0.125(10) -0.003(6) 0.041(6) 0.011(4)
_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
C1 C2 1.329(8) . ?
C1 B3 1.661(6) . ?
C1 B2 1.661(7) . ?
C1 B6 1.664(8) . ?
C1 B4 1.665(6) . ?
C1 B5 1.669(7) . ?
C2 N2 1.157(5) . ?
B1 B4 1.778(7) . ?
B1 B3 1.778(7) . ?
B1 B5 1.784(8) . ?
B1 B2 1.785(8) . ?
B1 B6 1.788(9) . ?
B1 H1 1.1000 . ?
B2 B4 1.737(3) 3_676 ?
B2 B5 1.749(3) 3_676 ?
B2 B6 1.779(3) . ?
B2 B3 1.785(3) . ?
B2 H2 1.1000 . ?
B3 B6 1.739(4) 3_676 ?
B3 B5 1.747(3) 3_676 ?
B3 B4 1.775(3) . ?
B3 H3 1.1000 . ?
B4 B2 1.737(3) 3_676 ?
B4 B6 1.738(4) 3_676 ?
B4 B5 1.780(3) . ?
B4 H4 1.1000 . ?
B5 B3 1.747(3) 3_676 ?
B5 B2 1.749(3) 3_676 ?
B5 B6 1.779(3) . ?
B5 H5 1.1000 . ?
B6 B4 1.738(4) 3_676 ?
B6 B3 1.739(4) 3_676 ?
B6 H6 1.1000 . ?
N1 C10 1.477(4) 3_766 ?
N1 C10 1.477(4) . ?
N1 C14 1.507(4) . ?
N1 C14 1.507(4) 3_766 ?
N1 C16 1.528(4) . ?
N1 C16 1.528(4) 3_766 ?
N1 C12 1.553(4) 3_766 ?
N1 C12 1.553(4) . ?
C10 C11 1.515(19) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.48(2) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C15 1.47(2) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17 1.52(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
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
C2 C1 B3 115.0(5) . . ?
C2 C1 B2 114.2(4) . . ?
B3 C1 B2 65.0(3) . . ?
C2 C1 B6 113.9(5) . . ?
B3 C1 B6 120.0(5) . . ?
B2 C1 B6 64.7(3) . . ?
C2 C1 B4 115.3(5) . . ?
B3 C1 B4 64.5(3) . . ?
B2 C1 B4 119.9(4) . . ?
B6 C1 B4 119.5(5) . . ?
C2 C1 B5 114.2(4) . . ?
B3 C1 B5 119.9(4) . . ?
B2 C1 B5 119.9(5) . . ?
B6 C1 B5 64.5(3) . . ?
B4 C1 B5 64.6(3) . . ?
N2 C2 C1 179.9(6) . . ?
B4 B1 B3 59.9(2) . . ?
B4 B1 B5 60.0(2) . . ?
B3 B1 B5 108.0(5) . . ?
B4 B1 B2 107.8(5) . . ?
B3 B1 B2 60.1(3) . . ?
B5 B1 B2 107.7(5) . . ?
B4 B1 B6 107.5(5) . . ?
B3 B1 B6 107.7(5) . . ?
B5 B1 B6 59.7(3) . . ?
B2 B1 B6 59.7(3) . . ?
B4 B1 H1 121.9 . . ?
B3 B1 H1 121.7 . . ?
B5 B1 H1 121.8 . . ?
B2 B1 H1 121.8 . . ?
B6 B1 H1 122.1 . . ?
C1 B2 B4 101.5(3) . 3_676 ?
C1 B2 B5 101.5(3) . 3_676 ?
B4 B2 B5 61.41(14) 3_676 3_676 ?
C1 B2 B6 57.7(3) . . ?
B4 B2 B6 59.26(14) 3_676 . ?
B5 B2 B6 108.41(18) 3_676 . ?
C1 B2 B3 57.5(2) . . ?
B4 B2 B3 108.20(18) 3_676 . ?
B5 B2 B3 59.26(13) 3_676 . ?
B6 B2 B3 107.82(15) . . ?
C1 B2 B1 7.3(4) . . ?
B4 B2 B1 107.7(3) 3_676 . ?
B5 B2 B1 107.6(3) 3_676 . ?
B6 B2 B1 60.2(3) . . ?
B3 B2 B1 59.8(2) . . ?
B4 B2 H2 122.7 3_676 . ?
B5 B2 H2 122.6 3_676 . ?
B6 B2 H2 121.4 . . ?
B3 B2 H2 121.5 . . ?
B1 B2 H2 120.5 . . ?
C1 B3 B6 101.7(3) . 3_676 ?
C1 B3 B5 101.6(3) . 3_676 ?
B6 B3 B5 61.37(15) 3_676 3_676 ?
C1 B3 B4 57.8(2) . . ?
B6 B3 B4 59.29(14) 3_676 . ?
B5 B3 B4 108.37(19) 3_676 . ?
C1 B3 B1 7.4(5) . . ?
B6 B3 B1 107.8(3) 3_676 . ?
B5 B3 B1 108.0(3) 3_676 . ?
B4 B3 B1 60.0(2) . . ?
C1 B3 B2 57.5(3) . . ?
B6 B3 B2 108.36(18) 3_676 . ?
B5 B3 B2 59.36(13) 3_676 . ?
B4 B3 B2 107.91(15) . . ?
B1 B3 B2 60.1(3) . . ?
B6 B3 H3 122.6 3_676 . ?
B5 B3 H3 122.7 3_676 . ?
B4 B3 H3 121.3 . . ?
B1 B3 H3 120.2 . . ?
B2 B3 H3 121.4 . . ?
C1 B4 B2 101.8(3) . 3_676 ?
C1 B4 B6 101.5(3) . 3_676 ?
B2 B4 B6 61.57(14) 3_676 3_676 ?
C1 B4 B3 57.6(2) . . ?
B2 B4 B3 108.69(18) 3_676 . ?
B6 B4 B3 59.30(14) 3_676 . ?
C1 B4 B1 7.5(5) . . ?
B2 B4 B1 108.2(3) 3_676 . ?
B6 B4 B1 107.9(3) 3_676 . ?
B3 B4 B1 60.1(2) . . ?
C1 B4 B5 57.8(3) . . ?
B2 B4 B5 59.64(13) 3_676 . ?
B6 B4 B5 108.84(17) 3_676 . ?
B3 B4 B5 108.28(15) . . ?
B1 B4 B5 60.2(3) . . ?
B2 B4 H4 122.4 3_676 . ?
B6 B4 H4 122.6 3_676 . ?
B3 B4 H4 121.3 . . ?
B1 B4 H4 120.2 . . ?
B5 B4 H4 121.0 . . ?
C1 B5 B3 101.1(3) . 3_676 ?
C1 B5 B2 101.2(3) . 3_676 ?
B3 B5 B2 61.38(14) 3_676 3_676 ?
C1 B5 B6 57.6(3) . . ?
B3 B5 B6 59.07(14) 3_676 . ?
B2 B5 B6 108.14(18) 3_676 . ?
C1 B5 B4 57.6(2) . . ?
B3 B5 B4 107.94(17) 3_676 . ?
B2 B5 B4 58.95(13) 3_676 . ?
B6 B5 B4 107.76(15) . . ?
C1 B5 B1 7.4(4) . . ?
B3 B5 B1 107.5(3) 3_676 . ?
B2 B5 B1 107.3(3) 3_676 . ?
B6 B5 B1 60.2(3) . . ?
B4 B5 B1 59.8(2) . . ?
B3 B5 H5 122.9 3_676 . ?
B2 B5 H5 122.9 3_676 . ?
B6 B5 H5 121.5 . . ?
B4 B5 H5 121.6 . . ?
B1 B5 H5 120.5 . . ?
C1 B6 B4 101.3(3) . 3_676 ?
C1 B6 B3 101.7(3) . 3_676 ?
B4 B6 B3 61.40(15) 3_676 3_676 ?
C1 B6 B2 57.6(2) . . ?
B4 B6 B2 59.17(14) 3_676 . ?
B3 B6 B2 108.45(19) 3_676 . ?
C1 B6 B5 57.9(2) . . ?
B4 B6 B5 108.60(18) 3_676 . ?
B3 B6 B5 59.56(14) 3_676 . ?
B2 B6 B5 108.23(16) . . ?
C1 B6 B1 7.3(4) . . ?
B4 B6 B1 107.5(3) 3_676 . ?
B3 B6 B1 107.8(3) 3_676 . ?
B2 B6 B1 60.1(2) . . ?
B5 B6 B1 60.0(2) . . ?
B4 B6 H6 122.8 3_676 . ?
B3 B6 H6 122.5 3_676 . ?
B2 B6 H6 121.4 . . ?
B5 B6 H6 121.0 . . ?
B1 B6 H6 120.5 . . ?
C10 N1 C10 180.000(1) 3_766 . ?
C10 N1 C14 65.9(2) 3_766 . ?
C10 N1 C14 114.1(2) . . ?
C10 N1 C14 114.1(2) 3_766 3_766 ?
C10 N1 C14 65.9(2) . 3_766 ?
C14 N1 C14 180.00(11) . 3_766 ?
C10 N1 C16 68.6(2) 3_766 . ?
C10 N1 C16 111.4(2) . . ?
C14 N1 C16 106.23(19) . . ?
C14 N1 C16 73.77(19) 3_766 . ?
C10 N1 C16 111.4(2) 3_766 3_766 ?
C10 N1 C16 68.6(2) . 3_766 ?
C14 N1 C16 73.77(19) . 3_766 ?
C14 N1 C16 106.23(19) 3_766 3_766 ?
C16 N1 C16 180.000(1) . 3_766 ?
C10 N1 C12 107.08(18) 3_766 3_766 ?
C10 N1 C12 72.92(18) . 3_766 ?
C14 N1 C12 69.84(19) . 3_766 ?
C14 N1 C12 110.16(19) 3_766 3_766 ?
C16 N1 C12 72.29(18) . 3_766 ?
C16 N1 C12 107.71(19) 3_766 3_766 ?
C10 N1 C12 72.92(18) 3_766 . ?
C10 N1 C12 107.08(18) . . ?
C14 N1 C12 110.16(19) . . ?
C14 N1 C12 69.84(19) 3_766 . ?
C16 N1 C12 107.71(19) . . ?
C16 N1 C12 72.29(18) 3_766 . ?
C12 N1 C12 180.000(1) 3_766 . ?
N1 C10 C11 115.7(7) . . ?
N1 C10 H10A 108.3 . . ?
C11 C10 H10A 108.3 . . ?
N1 C10 H10B 108.3 . . ?
C11 C10 H10B 108.3 . . ?
H10A C10 H10B 107.4 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C13 C12 N1 117.4(7) . . ?
C13 C12 H12A 108.0 . . ?
N1 C12 H12A 108.0 . . ?
C13 C12 H12B 108.0 . . ?
N1 C12 H12B 108.0 . . ?
H12A C12 H12B 107.2 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N1 115.3(9) . . ?
C15 C14 H14A 108.5 . . ?
N1 C14 H14A 108.5 . . ?
C15 C14 H14B 108.5 . . ?
N1 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 N1 116.5(7) . . ?
C17 C16 H16A 108.2 . . ?
N1 C16 H16A 108.2 . . ?
C17 C16 H16B 108.2 . . ?
N1 C16 H16B 108.2 . . ?
H16A C16 H16B 107.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full 25.30
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max 0.085
_refine_diff_density_min -0.154
_refine_diff_density_rms 0.021
# Attachment 'CsNCCB11Cl11.cif'
data_Cs[1-NC-closo-1-CB11Cl11]
_database_code_depnum_ccdc_archive 'CCDC 752155'
#=================================================================
#DATA 1
#=================================================================
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
Caesium-1-cyanoundecachloridocarba-closo-dodecaborate
;
_chemical_name_common
Caesium-1-cyanoundecachloridocarba-closo-dodecaborate
_chemical_melting_point ?
_chemical_formula_moiety 'C2 B11 Cl11 N, Cs'
_chemical_formula_sum 'C2 B11 Cl11 Cs N'
_chemical_formula_weight 679.80
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'
_symmetry_cell_setting tetragonal
_symmetry_space_group_name_H-M 'I 41/acd'
_symmetry_space_group_name_Hall '-I 4bd 2c'
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'
_cell_length_a 18.638(3)
_cell_length_b 18.638(3)
_cell_length_c 24.499(4)
_cell_angle_alpha 90.00
_cell_angle_beta 90.00
_cell_angle_gamma 90.00
_cell_volume 8510(3)
_cell_formula_units_Z 16
_cell_measurement_temperature 293(2)
_cell_measurement_reflns_used 3672
_cell_measurement_theta_min 5.16
_cell_measurement_theta_max 25.00
_exptl_crystal_description block
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.15
_exptl_crystal_size_mid 0.10
_exptl_crystal_size_min 0.10
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 2.122
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 5056
_exptl_absorpt_coefficient_mu 3.112
_exptl_absorpt_correction_type numerical
_exptl_absorpt_correction_T_min 0.5641
_exptl_absorpt_correction_T_max 0.7401
_exptl_absorpt_process_details 'X-RED 1.20 (Stoe & Cie, 1996)'
_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 'Stoe STADI CCD'
_diffrn_measurement_method omega
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 16987
_diffrn_reflns_av_R_equivalents 0.0512
_diffrn_reflns_av_sigmaI/netI 0.0241
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 22
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_theta_min 5.16
_diffrn_reflns_theta_max 25.00
_reflns_number_total 1859
_reflns_number_gt 1553
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'CrysAlis CCD (KUMA, 2000)'
_computing_cell_refinement 'CrysAlis RED (Kuma 2000)'
_computing_data_reduction 'CrysAlis RED (Kuma 2000)'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics 'Diamond 3.1f (Brandeburger, 2008)'
_computing_publication_material 'SHELXL-97 (Sheldrick, 1997)'
_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^)+(0.0540P)^2^+3.2000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens none
_refine_ls_hydrogen_treatment none
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1859
_refine_ls_number_parameters 135
_refine_ls_number_restraints 8
_refine_ls_R_factor_all 0.0382
_refine_ls_R_factor_gt 0.0292
_refine_ls_wR_factor_ref 0.0842
_refine_ls_wR_factor_gt 0.0801
_refine_ls_goodness_of_fit_ref 1.071
_refine_ls_restrained_S_all 1.085
_refine_ls_shift/su_max 0.004
_refine_ls_shift/su_mean 0.001
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_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
Cs1 0.0357(2) 0.0582(3) 0.0597(3) 0.000 -0.00001(15) 0.000
B2 0.0274(18) 0.0282(18) 0.0241(17) -0.0020(14) 0.0031(14) 0.0009(14)
Cl2 0.0472(5) 0.0620(6) 0.0337(5) -0.0086(4) 0.0158(4) 0.0069(4)
B3 0.0262(18) 0.0332(18) 0.0224(16) -0.0018(14) -0.0028(14) 0.0042(15)
Cl3 0.0495(6) 0.0808(7) 0.0335(5) -0.0017(4) -0.0177(4) 0.0110(5)
B4 0.0266(18) 0.0236(17) 0.0295(18) -0.0028(14) 0.0023(14) 0.0003(15)
Cl4 0.0239(4) 0.0423(5) 0.0655(6) -0.0026(4) 0.0031(4) -0.0053(4)
B5 0.0302(19) 0.0247(18) 0.0320(19) -0.0060(15) -0.0001(15) 0.0010(15)
Cl5 0.0549(6) 0.0341(5) 0.0678(6) -0.0259(4) 0.0073(5) -0.0057(4)
B6 0.0261(18) 0.0271(18) 0.0303(18) 0.0047(15) 0.0046(14) 0.0014(14)
Cl6 0.0616(6) 0.0387(5) 0.0613(6) 0.0258(4) 0.0112(5) 0.0042(4)
B1 0.023(5) 0.017(7) 0.030(2) -0.002(9) 0.003(6) 0.0058(17)
Cl1 0.037(2) 0.038(3) 0.0637(16) 0.001(2) 0.0026(19) 0.0222(16)
C1 0.023(5) 0.017(7) 0.030(2) -0.002(9) 0.003(6) 0.0058(17)
C2 0.031(8) 0.030(8) 0.038(5) -0.006(6) 0.006(5) -0.002(6)
N1 0.054(8) 0.026(6) 0.045(4) -0.004(4) 0.000(6) 0.015(5)
_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
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 ?
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
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 ?
_diffrn_measured_fraction_theta_max 0.988
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.988
_refine_diff_density_max 0.622
_refine_diff_density_min -0.549
_refine_diff_density_rms 0.078