#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:53:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179352 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/49/4324964.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_4324964
loop_
_publ_author_name
'Xuliang Dai'
'Seok-Bong Choi'
'Christopher W. Braun'
'Pooja Vaidya'
'Svetlana Kilina'
'Angel Ugrinov'
'Douglas L. Schulz'
'Philip Boudjouk'
_publ_contact_author
;
Xuliang Dai
Center for Nanoscale Science and Engineering
North Dakota State University
1735 NDSU Research Park Drive
Fargo, ND 58108
USA
;
_publ_contact_author_email       xuliang.dai@ndsu.edu
_publ_contact_author_fax         'Intl. Code + (000)000-0000'
_publ_contact_author_phone       'Intl. Code + (000)000-0000'
_publ_section_title
;
 Halide Coordination of Perhalocyclohexasilane Si6X12 (X = Cl or Br)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4047
_journal_page_last               4053
_journal_paper_doi               10.1021/ic102535n
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C32 H72 Br12 I2 N2 Si6'
_chemical_formula_weight         1866.18
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                107.899(5)
_cell_angle_beta                 91.885(5)
_cell_angle_gamma                115.169(5)
_cell_formula_units_Z            1
_cell_length_a                   11.083(3)
_cell_length_b                   12.203(4)
_cell_length_c                   12.885(4)
_cell_measurement_reflns_used    4043
_cell_measurement_temperature    253(2)
_cell_measurement_theta_max      28.18
_cell_measurement_theta_min      2.11
_cell_volume                     1473.5(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      253(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0352
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14088
_diffrn_reflns_theta_full        28.22
_diffrn_reflns_theta_max         28.22
_diffrn_reflns_theta_min         1.97
_exptl_absorpt_coefficient_mu    9.350
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.560010
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.103
_exptl_crystal_description       parallelepip
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.74
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.24
_refine_diff_density_max         1.337
_refine_diff_density_min         -4.059
_refine_diff_density_rms         0.263
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         7000
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0671
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0967P)²+14.1034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1788
_refine_ls_wR_factor_ref         0.1922
_reflns_number_gt                5750
_reflns_number_total             7000
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102535n_si_003_1.cif
_cod_data_source_block           Si6Br12I2
_cod_database_code               4324964
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
I1 I 0.14204(6) 0.10135(6) 0.40606(5) 0.04079(18) Uani 1 1 d .
Br6 Br -0.17763(9) 0.07794(9) 0.25713(7) 0.0380(2) Uani 1 1 d .
Br5 Br -0.40319(8) -0.07601(8) 0.40882(8) 0.0367(2) Uani 1 1 d .
Br4 Br -0.19923(9) 0.19596(8) 0.68027(8) 0.0390(2) Uani 1 1 d .
Br3 Br 0.01841(8) 0.36108(7) 0.52715(8) 0.0361(2) Uani 1 1 d .
Br2 Br -0.31805(8) -0.36232(8) 0.31430(8) 0.0405(2) Uani 1 1 d .
Br1 Br -0.10299(10) -0.20979(10) 0.15899(7) 0.0446(2) Uani 1 1 d .
Si3 Si -0.18272(19) -0.00047(18) 0.39688(16) 0.0231(4) Uani 1 1 d .
Si2 Si -0.1293(2) -0.17501(19) 0.33850(16) 0.0242(4) Uani 1 1 d .
Si1 Si -0.05555(19) 0.17262(18) 0.56338(16) 0.0234(4) Uani 1 1 d .
N1 N 0.2252(6) 0.3936(6) 0.2135(5) 0.0248(12) Uani 1 1 d .
C16 C 0.3216(9) 0.5743(8) 0.4089(6) 0.0327(16) Uani 1 1 d .
H16A H 0.2348 0.5748 0.4154 0.039 Uiso 1 1 calc R
H16B H 0.3725 0.6382 0.3765 0.039 Uiso 1 1 calc R
C15 C 0.1007(7) 0.4172(8) 0.2158(6) 0.0312(16) Uani 1 1 d .
H15A H 0.0478 0.3788 0.2651 0.037 Uiso 1 1 calc R
H15B H 0.1310 0.5098 0.2471 0.037 Uiso 1 1 calc R
C14 C 0.3174(8) 0.4549(7) 0.1425(7) 0.0300(15) Uani 1 1 d .
H14A H 0.2779 0.3993 0.0656 0.036 Uiso 1 1 calc R
H14B H 0.4033 0.4547 0.1593 0.036 Uiso 1 1 calc R
C13 C 0.2981(8) 0.4428(8) 0.3340(6) 0.0287(15) Uani 1 1 d .
H13A H 0.2461 0.3806 0.3675 0.034 Uiso 1 1 calc R
H13B H 0.3857 0.4431 0.3323 0.034 Uiso 1 1 calc R
C12 C 0.1759(8) 0.2473(7) 0.1643(7) 0.0336(17) Uani 1 1 d .
H12A H 0.1090 0.2065 0.2048 0.040 Uiso 1 1 calc R
H12B H 0.1306 0.2159 0.0879 0.040 Uiso 1 1 calc R
C11 C 0.3481(9) 0.5919(8) 0.1521(7) 0.0322(16) Uani 1 1 d .
H11A H 0.3956 0.6514 0.2267 0.039 Uiso 1 1 calc R
H11B H 0.2639 0.5960 0.1380 0.039 Uiso 1 1 calc R
C10 C 0.2853(9) 0.2038(8) 0.1662(8) 0.0380(18) Uani 1 1 d .
H10A H 0.3204 0.2193 0.2421 0.046 Uiso 1 1 calc R
H10B H 0.3597 0.2521 0.1352 0.046 Uiso 1 1 calc R
C9 C 0.4004(10) 0.6115(9) 0.5255(8) 0.043(2) Uani 1 1 d .
H9A H 0.3560 0.5412 0.5529 0.052 Uiso 1 1 calc R
H9B H 0.4915 0.6222 0.5197 0.052 Uiso 1 1 calc R
C8 C 0.0089(9) 0.3637(9) 0.1037(7) 0.0400(19) Uani 1 1 d .
H8A H -0.0365 0.2698 0.0781 0.048 Uiso 1 1 calc R
H8B H 0.0632 0.3896 0.0500 0.048 Uiso 1 1 calc R
C7 C 0.4364(10) 0.6316(9) 0.0675(8) 0.042(2) Uani 1 1 d .
H7A H 0.5194 0.6253 0.0810 0.051 Uiso 1 1 calc R
H7B H 0.3880 0.5721 -0.0069 0.051 Uiso 1 1 calc R
C6 C 0.2223(11) 0.0587(8) 0.0972(9) 0.050(2) Uani 1 1 d .
H6A H 0.1414 0.0131 0.1236 0.060 Uiso 1 1 calc R
H6B H 0.1948 0.0457 0.0204 0.060 Uiso 1 1 calc R
C5 C -0.0980(10) 0.4138(11) 0.1117(10) 0.053(3) Uani 1 1 d .
H5A H -0.0526 0.5073 0.1475 0.064 Uiso 1 1 calc R
H5B H -0.1425 0.3933 0.0374 0.064 Uiso 1 1 calc R
C4 C 0.4718(12) 0.7682(10) 0.0747(9) 0.054(3) Uani 1 1 d .
H4A H 0.5256 0.7888 0.0201 0.082 Uiso 1 1 calc R
H4B H 0.5224 0.8277 0.1474 0.082 Uiso 1 1 calc R
H4C H 0.3899 0.7748 0.0610 0.082 Uiso 1 1 calc R
C3 C 0.4093(13) 0.7329(10) 0.6071(8) 0.054(3) Uani 1 1 d .
H3A H 0.4586 0.7509 0.6779 0.081 Uiso 1 1 calc R
H3B H 0.3195 0.7226 0.6143 0.081 Uiso 1 1 calc R
H3C H 0.4556 0.8035 0.5816 0.081 Uiso 1 1 calc R
C2 C -0.2039(11) 0.3565(12) 0.1758(10) 0.059(3) Uani 1 1 d .
H2A H -0.2680 0.3905 0.1779 0.088 Uiso 1 1 calc R
H2B H -0.1609 0.3784 0.2502 0.088 Uiso 1 1 calc R
H2C H -0.2504 0.2640 0.1402 0.088 Uiso 1 1 calc R
C1 C 0.3171(15) 0.0013(12) 0.1024(12) 0.073(4) Uani 1 1 d .
H1A H 0.2717 -0.0897 0.0593 0.110 Uiso 1 1 calc R
H1B H 0.3449 0.0137 0.1783 0.110 Uiso 1 1 calc R
H1C H 0.3955 0.0431 0.0731 0.110 Uiso 1 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
H H 0.0000 0.0000 '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
Br5 Si3 Br6 101.07(8) . .
Br5 Si3 Si1 108.09(9) . .
Br6 Si3 Si1 109.30(10) . .
Br5 Si3 Si2 109.35(9) . .
Br6 Si3 Si2 109.14(10) . .
Si1 Si3 Si2 118.48(10) . .
Br2 Si2 Br1 99.32(8) . .
Br2 Si2 Si1 108.88(10) . 2_556
Br1 Si2 Si1 107.87(10) . 2_556
Br2 Si2 Si3 109.28(10) . .
Br1 Si2 Si3 107.67(10) . .
Si1 Si2 Si3 121.53(10) 2_556 .
Br4 Si1 Br3 100.88(8) . .
Br4 Si1 Si3 108.83(10) . .
Br3 Si1 Si3 107.77(10) . .
Br4 Si1 Si2 108.94(10) . 2_556
Br3 Si1 Si2 108.89(9) . 2_556
Si3 Si1 Si2 119.86(10) . 2_556
C14 N1 C15 112.5(6) . .
C14 N1 C12 108.1(6) . .
C15 N1 C12 107.9(6) . .
C14 N1 C13 112.3(6) . .
C15 N1 C13 107.8(5) . .
C12 N1 C13 108.1(6) . .
C13 C16 C9 111.3(7) . .
C13 C16 H16A 109.4 . .
C9 C16 H16A 109.4 . .
C13 C16 H16B 109.4 . .
C9 C16 H16B 109.4 . .
H16A C16 H16B 108.0 . .
C8 C15 N1 115.1(6) . .
C8 C15 H15A 108.5 . .
N1 C15 H15A 108.5 . .
C8 C15 H15B 108.5 . .
N1 C15 H15B 108.5 . .
H15A C15 H15B 107.5 . .
N1 C14 C11 118.6(6) . .
N1 C14 H14A 107.7 . .
C11 C14 H14A 107.7 . .
N1 C14 H14B 107.7 . .
C11 C14 H14B 107.7 . .
H14A C14 H14B 107.1 . .
C16 C13 N1 117.7(6) . .
C16 C13 H13A 107.9 . .
N1 C13 H13A 107.9 . .
C16 C13 H13B 107.9 . .
N1 C13 H13B 107.9 . .
H13A C13 H13B 107.2 . .
C10 C12 N1 115.6(6) . .
C10 C12 H12A 108.4 . .
N1 C12 H12A 108.4 . .
C10 C12 H12B 108.4 . .
N1 C12 H12B 108.4 . .
H12A C12 H12B 107.4 . .
C14 C11 C7 109.8(7) . .
C14 C11 H11A 109.7 . .
C7 C11 H11A 109.7 . .
C14 C11 H11B 109.7 . .
C7 C11 H11B 109.7 . .
H11A C11 H11B 108.2 . .
C12 C10 C6 108.3(8) . .
C12 C10 H10A 110.0 . .
C6 C10 H10A 110.0 . .
C12 C10 H10B 110.0 . .
C6 C10 H10B 110.0 . .
H10A C10 H10B 108.4 . .
C3 C9 C16 113.1(8) . .
C3 C9 H9A 109.0 . .
C16 C9 H9A 109.0 . .
C3 C9 H9B 109.0 . .
C16 C9 H9B 109.0 . .
H9A C9 H9B 107.8 . .
C15 C8 C5 110.8(7) . .
C15 C8 H8A 109.5 . .
C5 C8 H8A 109.5 . .
C15 C8 H8B 109.5 . .
C5 C8 H8B 109.5 . .
H8A C8 H8B 108.1 . .
C4 C7 C11 112.0(8) . .
C4 C7 H7A 109.2 . .
C11 C7 H7A 109.2 . .
C4 C7 H7B 109.2 . .
C11 C7 H7B 109.2 . .
H7A C7 H7B 107.9 . .
C1 C6 C10 113.2(9) . .
C1 C6 H6A 108.9 . .
C10 C6 H6A 108.9 . .
C1 C6 H6B 108.9 . .
C10 C6 H6B 108.9 . .
H6A C6 H6B 107.7 . .
C2 C5 C8 112.9(9) . .
C2 C5 H5A 109.0 . .
C8 C5 H5A 109.0 . .
C2 C5 H5B 109.0 . .
C8 C5 H5B 109.0 . .
H5A C5 H5B 107.8 . .
C7 C4 H4A 109.5 . .
C7 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C7 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C9 C3 H3A 109.5 . .
C9 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
C9 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C5 C2 H2A 109.5 . .
C5 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C5 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C6 C1 H1A 109.5 . .
C6 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C6 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br6 Si3 2.276(2) .
Br5 Si3 2.245(2) .
Br4 Si1 2.273(2) .
Br3 Si1 2.293(2) .
Br2 Si2 2.269(2) .
Br1 Si2 2.272(2) .
Si3 Si1 2.353(3) .
Si3 Si2 2.360(3) .
Si2 Si1 2.357(3) 2_556
Si1 Si2 2.357(3) 2_556
N1 C14 1.507(10) .
N1 C15 1.524(9) .
N1 C12 1.530(9) .
N1 C13 1.535(9) .
C16 C13 1.501(11) .
C16 C9 1.544(11) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C15 C8 1.520(11) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C14 C11 1.521(11) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C12 C10 1.518(12) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C11 C7 1.540(11) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C10 C6 1.534(11) .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C9 C3 1.490(13) .
C9 H9A 0.9700 .
C9 H9B 0.9700 .
C8 C5 1.541(13) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C7 C4 1.513(13) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C6 C1 1.500(15) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C5 C2 1.506(17) .
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C3 H3A 0.9600 .
C3 H3B 0.9600 .
C3 H3C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
