#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:53:43 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179352 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/49/4324967.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_4324967
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 Br14 N2 Si6'
_chemical_formula_weight         1772.20
_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                107.503(6)
_cell_angle_beta                 91.912(6)
_cell_angle_gamma                115.239(6)
_cell_formula_units_Z            1
_cell_length_a                   11.106(4)
_cell_length_b                   12.084(4)
_cell_length_c                   12.741(4)
_cell_measurement_reflns_used    2502
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.42
_cell_volume                     1448.9(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      293(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_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  0.0385
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13955
_diffrn_reflns_theta_full        28.14
_diffrn_reflns_theta_max         28.14
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    9.821
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.154212
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            white
_exptl_crystal_density_diffrn    2.031
_exptl_crystal_description       plate
_exptl_crystal_F_000             852
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.496
_refine_diff_density_min         -1.205
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.983
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.983
_refine_ls_R_factor_all          0.0972
_refine_ls_R_factor_gt           0.0509
_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)+(0.1027P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1371
_refine_ls_wR_factor_ref         0.1710
_reflns_number_gt                4381
_reflns_number_total             6882
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102535n_si_003_4.cif
_cod_data_source_block           Si6Br14
_cod_original_cell_volume        1449.0(9)
_cod_database_code               4324967
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
Br1 Br 0.30368(8) 0.69445(8) 0.68183(6) 0.0473(2) Uani 1 1 d .
Br2 Br 0.32188(8) 0.57760(8) 0.25751(6) 0.0465(2) Uani 1 1 d .
Br3 Br 0.18265(8) 0.13892(7) 0.32002(7) 0.0497(2) Uani 1 1 d .
Br4 Br 0.36993(7) 0.40458(6) 0.59153(5) 0.03441(18) Uani 1 1 d .
Br5 Br 0.51604(8) 0.85898(7) 0.52656(6) 0.0441(2) Uani 1 1 d .
Br6 Br 0.39260(9) 0.28916(9) 0.15905(5) 0.0541(2) Uani 1 1 d .
Br7 Br 0.09922(7) 0.42403(8) 0.41151(6) 0.0454(2) Uani 1 1 d .
Si8 Si 0.36976(18) 0.32491(17) 0.33962(13) 0.0309(4) Uani 1 1 d .
Si9 Si 0.44426(18) 0.67239(17) 0.56401(13) 0.0303(4) Uani 1 1 d .
Si10 Si 0.31724(18) 0.49934(17) 0.39749(13) 0.0298(4) Uani 1 1 d .
N N 0.7237(5) 0.8928(5) 0.2173(4) 0.0316(12) Uani 1 1 d .
C7 C 0.8196(7) 1.0746(7) 0.4131(5) 0.0394(16) Uani 1 1 d .
H7A H 0.7325 1.0738 0.4199 0.047 Uiso 1 1 calc R
H7B H 0.8687 1.1386 0.3791 0.047 Uiso 1 1 calc R
C16 C 0.8167(7) 0.9542(6) 0.1451(5) 0.0368(15) Uani 1 1 d .
H16A H 0.9015 0.9523 0.1616 0.044 Uiso 1 1 calc R
H16B H 0.7767 0.8987 0.0676 0.044 Uiso 1 1 calc R
C4 C 0.6761(7) 0.7466(6) 0.1703(5) 0.0387(16) Uani 1 1 d .
H4A H 0.6095 0.7065 0.2121 0.046 Uiso 1 1 calc R
H4B H 0.6300 0.7144 0.0934 0.046 Uiso 1 1 calc R
C12 C 0.5996(7) 0.9170(7) 0.2180(5) 0.0384(16) Uani 1 1 d .
H12A H 0.5461 0.8792 0.2682 0.046 Uiso 1 1 calc R
H12B H 0.6301 1.0104 0.2482 0.046 Uiso 1 1 calc R
C3 C 0.7825(8) 0.6996(7) 0.1715(6) 0.0466(18) Uani 1 1 d .
H3A H 0.8581 0.7493 0.1415 0.056 Uiso 1 1 calc R
H3B H 0.8161 0.7134 0.2479 0.056 Uiso 1 1 calc R
C8 C 0.7973(7) 0.9429(6) 0.3385(5) 0.0357(15) Uani 1 1 d .
H8A H 0.7464 0.8801 0.3731 0.043 Uiso 1 1 calc R
H8B H 0.8851 0.9441 0.3364 0.043 Uiso 1 1 calc R
C15 C 0.8500(7) 1.0919(7) 0.1541(5) 0.0370(15) Uani 1 1 d .
H15A H 0.7668 1.0978 0.1404 0.044 Uiso 1 1 calc R
H15B H 0.8981 1.1513 0.2291 0.044 Uiso 1 1 calc R
C14 C 0.9364(8) 1.1307(7) 0.0700(6) 0.0449(18) Uani 1 1 d .
H14A H 1.0186 1.1231 0.0834 0.054 Uiso 1 1 calc R
H14B H 0.8876 1.0710 -0.0048 0.054 Uiso 1 1 calc R
C6 C 0.8977(8) 1.1145(8) 0.5278(5) 0.051(2) Uani 1 1 d .
H6A H 0.9880 1.1236 0.5212 0.061 Uiso 1 1 calc R
H6B H 0.8535 1.0457 0.5582 0.061 Uiso 1 1 calc R
C11 C 0.5092(7) 0.8623(8) 0.1046(5) 0.0483(19) Uani 1 1 d .
H11A H 0.4641 0.7677 0.0798 0.058 Uiso 1 1 calc R
H11B H 0.5640 0.8880 0.0504 0.058 Uiso 1 1 calc R
C9 C 0.2988(9) 0.8599(10) 0.1772(7) 0.064(2) Uani 1 1 d .
H9A H 0.2373 0.8967 0.1787 0.095 Uiso 1 1 calc R
H9B H 0.3423 0.8829 0.2524 0.095 Uiso 1 1 calc R
H9C H 0.2496 0.7666 0.1435 0.095 Uiso 1 1 calc R
C13 C 0.9737(10) 1.2683(8) 0.0762(7) 0.065(2) Uani 1 1 d .
H13A H 1.0287 1.2887 0.0215 0.098 Uiso 1 1 calc R
H13B H 1.0235 1.3279 0.1497 0.098 Uiso 1 1 calc R
H13C H 0.8927 1.2758 0.0613 0.098 Uiso 1 1 calc R
C10 C 0.4035(8) 0.9118(9) 0.1105(7) 0.058(2) Uani 1 1 d .
H10A H 0.4493 1.0063 0.1430 0.069 Uiso 1 1 calc R
H10B H 0.3583 0.8882 0.0349 0.069 Uiso 1 1 calc R
C2 C 0.7226(9) 0.5566(8) 0.1021(7) 0.058(2) Uani 1 1 d .
H2A H 0.6432 0.5088 0.1294 0.070 Uiso 1 1 calc R
H2B H 0.6933 0.5446 0.0251 0.070 Uiso 1 1 calc R
C5 C 0.9098(10) 1.2403(9) 0.6085(6) 0.066(3) Uani 1 1 d .
H5A H 0.9608 1.2601 0.6798 0.100 Uiso 1 1 calc R
H5B H 0.8210 1.2315 0.6173 0.100 Uiso 1 1 calc R
H5C H 0.9553 1.3095 0.5800 0.100 Uiso 1 1 calc R
C1 C 0.8176(11) 0.5008(9) 0.1040(8) 0.074(3) Uani 1 1 d .
H1A H 0.7737 0.4101 0.0580 0.110 Uiso 1 1 calc R
H1B H 0.8449 0.5095 0.1796 0.110 Uiso 1 1 calc R
H1C H 0.8959 0.5465 0.0759 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'
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_3
Br3 Si8 Br6 99.82(7) .
Br3 Si8 Si10 108.80(9) .
Br6 Si8 Si10 107.52(8) .
Br3 Si8 Si9 109.06(9) 2_666
Br6 Si8 Si9 107.67(9) 2_666
Si10 Si8 Si9 121.74(9) 2_666
Br1 Si9 Br5 101.33(8) .
Br1 Si9 Si10 108.85(9) .
Br5 Si9 Si10 107.50(8) .
Br1 Si9 Si8 109.26(8) 2_666
Br5 Si9 Si8 108.59(9) 2_666
Si10 Si9 Si8 119.73(10) 2_666
Br7 Si10 Br2 101.40(8) .
Br7 Si10 Si8 109.35(9) .
Br2 Si10 Si8 109.12(8) .
Br7 Si10 Si9 107.88(8) .
Br2 Si10 Si9 109.41(9) .
Si8 Si10 Si9 118.34(10) .
C16 N C4 108.1(5) .
C16 N C12 112.1(5) .
C4 N C12 108.5(5) .
C16 N C8 111.7(5) .
C4 N C8 107.6(5) .
C12 N C8 108.7(5) .
C8 C7 C6 112.4(6) .
C8 C7 H7A 109.1 .
C6 C7 H7A 109.1 .
C8 C7 H7B 109.1 .
C6 C7 H7B 109.1 .
H7A C7 H7B 107.9 .
C15 C16 N 119.0(5) .
C15 C16 H16A 107.6 .
N C16 H16A 107.6 .
C15 C16 H16B 107.6 .
N C16 H16B 107.6 .
H16A C16 H16B 107.0 .
C3 C4 N 117.5(6) .
C3 C4 H4A 107.9 .
N C4 H4A 107.9 .
C3 C4 H4B 107.9 .
N C4 H4B 107.9 .
H4A C4 H4B 107.2 .
C11 C12 N 115.0(5) .
C11 C12 H12A 108.5 .
N C12 H12A 108.5 .
C11 C12 H12B 108.5 .
N C12 H12B 108.5 .
H12A C12 H12B 107.5 .
C2 C3 C4 110.1(7) .
C2 C3 H3A 109.6 .
C4 C3 H3A 109.6 .
C2 C3 H3B 109.6 .
C4 C3 H3B 109.6 .
H3A C3 H3B 108.2 .
C7 C8 N 117.7(5) .
C7 C8 H8A 107.9 .
N C8 H8A 107.9 .
C7 C8 H8B 107.9 .
N C8 H8B 107.9 .
H8A C8 H8B 107.2 .
C14 C15 C16 110.2(6) .
C14 C15 H15A 109.6 .
C16 C15 H15A 109.6 .
C14 C15 H15B 109.6 .
C16 C15 H15B 109.6 .
H15A C15 H15B 108.1 .
C13 C14 C15 112.4(6) .
C13 C14 H14A 109.1 .
C15 C14 H14A 109.1 .
C13 C14 H14B 109.1 .
C15 C14 H14B 109.1 .
H14A C14 H14B 107.9 .
C7 C6 C5 113.7(7) .
C7 C6 H6A 108.8 .
C5 C6 H6A 108.8 .
C7 C6 H6B 108.8 .
C5 C6 H6B 108.8 .
H6A C6 H6B 107.7 .
C12 C11 C10 110.9(6) .
C12 C11 H11A 109.5 .
C10 C11 H11A 109.5 .
C12 C11 H11B 109.5 .
C10 C11 H11B 109.5 .
H11A C11 H11B 108.1 .
C10 C9 H9A 109.5 .
C10 C9 H9B 109.5 .
H9A C9 H9B 109.5 .
C10 C9 H9C 109.5 .
H9A C9 H9C 109.5 .
H9B C9 H9C 109.5 .
C14 C13 H13A 109.5 .
C14 C13 H13B 109.5 .
H13A C13 H13B 109.5 .
C14 C13 H13C 109.5 .
H13A C13 H13C 109.5 .
H13B C13 H13C 109.5 .
C9 C10 C11 114.2(7) .
C9 C10 H10A 108.7 .
C11 C10 H10A 108.7 .
C9 C10 H10B 108.7 .
C11 C10 H10B 108.7 .
H10A C10 H10B 107.6 .
C1 C2 C3 113.6(8) .
C1 C2 H2A 108.8 .
C3 C2 H2A 108.8 .
C1 C2 H2B 108.8 .
C3 C2 H2B 108.8 .
H2A C2 H2B 107.7 .
C6 C5 H5A 109.5 .
C6 C5 H5B 109.5 .
H5A C5 H5B 109.5 .
C6 C5 H5C 109.5 .
H5A C5 H5C 109.5 .
H5B C5 H5C 109.5 .
C2 C1 H1A 109.5 .
C2 C1 H1B 109.5 .
H1A C1 H1B 109.5 .
C2 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
Br1 Si9 2.2433(19) .
Br2 Si10 2.2487(19) .
Br3 Si8 2.253(2) .
Br5 Si9 2.256(2) .
Br6 Si8 2.2535(19) .
Br7 Si10 2.229(2) .
Si8 Si10 2.339(3) .
Si8 Si9 2.350(3) 2_666
Si9 Si10 2.341(2) .
Si9 Si8 2.350(3) 2_666
N C16 1.512(7) .
N C4 1.517(8) .
N C12 1.525(8) .
N C8 1.533(7) .
C7 C8 1.495(9) .
C7 C6 1.502(9) .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C16 C15 1.509(9) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C4 C3 1.515(10) .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C12 C11 1.515(9) .
C12 H12A 0.9700 .
C12 H12B 0.9700 .
C3 C2 1.508(10) .
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C15 C14 1.508(9) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C14 C13 1.508(10) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C6 C5 1.504(10) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C11 C10 1.523(10) .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C9 C10 1.494(12) .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C10 H10A 0.9700 .
C10 H10B 0.9700 .
C2 C1 1.478(12) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
