#------------------------------------------------------------------------------
#$Date: 2019-11-23 02:14:45 +0200 (Sat, 23 Nov 2019) $
#$Revision: 231854 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/65/4346578.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_4346578
loop_
_publ_author_name
'Tillmann, Jan'
'Moxter, Maximilian'
'Bolte, Michael'
'Lerner, Hans-Wolfram'
'Wagner, Matthias'
_publ_section_title
;
 Lewis acidity of Si6Cl12 and its role as convenient SiCl2 source.
;
_journal_issue                   19
_journal_name_full               'Inorganic chemistry'
_journal_page_first              9611
_journal_page_last               9618
_journal_paper_doi               10.1021/acs.inorgchem.5b01703
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety         'Si6 Cl12, C Cl4'
_chemical_formula_sum            'C Cl16 Si6'
_chemical_formula_weight         747.75
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   12.6663(11)
_cell_length_b                   12.6663(11)
_cell_length_c                   27.782(3)
_cell_measurement_reflns_used    5473
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.7
_cell_measurement_theta_min      3.9
_cell_volume                     3860.1(6)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP in SHELXTL-Plus (Sheldrick, 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            3307
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.570
_diffrn_reflns_theta_min         3.898
_diffrn_source                   'Genix 3D I\mS microfocus X-ray source'
_exptl_absorpt_coefficient_mu    1.977
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.410
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'X-Area (Stoe & Cie, 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_description       block
_exptl_crystal_F_000             2172
_exptl_crystal_size_max          0.570
_exptl_crystal_size_mid          0.520
_exptl_crystal_size_min          0.470
_refine_diff_density_max         0.523
_refine_diff_density_min         -0.385
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.206
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     42
_refine_ls_number_reflns         977
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.206
_refine_ls_R_factor_all          0.0400
_refine_ls_R_factor_gt           0.0375
_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)+(0.0424P)²+7.9343P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0912
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                932
_reflns_number_total             977
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ic5b01703_si_002.cif
_cod_data_source_block           wa2073
_cod_original_cell_volume        3860.1(8)
_cod_database_code               4346578
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.399
_shelx_estimated_absorpt_t_max   0.457
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+5/6'
'x-y+2/3, -y+1/3, -z+5/6'
'-x+2/3, -x+y+1/3, -z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+7/6'
'x-y+1/3, -y+2/3, -z+7/6'
'-x+1/3, -x+y+2/3, -z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z-1/6'
'-x+y+2/3, y+1/3, z-1/6'
'x+2/3, x-y+1/3, z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+1/6'
'-x+y+1/3, y+2/3, z+1/6'
'x+1/3, x-y+2/3, z+1/6'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Si1 Si 0.63265(5) 0.49141(5) 0.34570(2) 0.01850(19) Uani 1 1 d . . .
Cl1 Cl 0.62924(5) 0.49249(5) 0.41908(2) 0.0307(2) Uani 1 1 d . . .
Cl2 Cl 0.60523(6) 0.62500(5) 0.31835(2) 0.0325(2) Uani 1 1 d . . .
C1 C 0.3333 0.6667 0.4167 0.0333(12) Uani 1 6 d S T P
Cl3 Cl 0.3333 0.6667 0.35337(10) 0.0744(10) Uani 0.5 3 d S T P
Cl4 Cl 0.3152(2) 0.52709(18) 0.39688(8) 0.0670(5) Uani 0.5 1 d . . P
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'
Cl Cl 0.1484 0.1585 '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'
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
Cl2 Si1 Cl1 110.75(3) . .
Cl2 Si1 Si1 109.88(4) . 33_545
Cl1 Si1 Si1 106.80(3) . 33_545
Cl2 Si1 Si1 109.24(4) . 32
Cl1 Si1 Si1 108.32(3) . 32
Si1 Si1 Si1 111.83(2) 33_545 32
Cl4 C1 Cl4 136.20(14) 12 3_565
Cl4 C1 Cl4 110.54(14) 12 2_665
Cl4 C1 Cl4 110.64(7) 3_565 2_665
Cl4 C1 Cl4 38.97(14) 12 .
Cl4 C1 Cl4 110.64(7) 3_565 .
Cl4 C1 Cl4 110.64(7) 2_665 .
Cl4 C1 Cl4 110.64(7) 12 11_565
Cl4 C1 Cl4 110.53(14) 3_565 11_565
Cl4 C1 Cl4 38.97(14) 2_665 11_565
Cl4 C1 Cl4 136.20(14) . 11_565
Cl4 C1 Cl4 110.64(7) 12 10_455
Cl4 C1 Cl4 38.97(14) 3_565 10_455
Cl4 C1 Cl4 136.20(14) 2_665 10_455
Cl4 C1 Cl4 110.54(14) . 10_455
Cl4 C1 Cl4 110.64(7) 11_565 10_455
Cl4 C1 Cl3 108.28(7) 12 .
Cl4 C1 Cl3 71.73(7) 3_565 .
Cl4 C1 Cl3 71.73(7) 2_665 .
Cl4 C1 Cl3 71.73(7) . .
Cl4 C1 Cl3 108.28(7) 11_565 .
Cl4 C1 Cl3 108.28(7) 10_455 .
Cl4 C1 Cl3 71.72(7) 12 10_455
Cl4 C1 Cl3 108.27(7) 3_565 10_455
Cl4 C1 Cl3 108.28(7) 2_665 10_455
Cl4 C1 Cl3 108.28(7) . 10_455
Cl4 C1 Cl3 71.72(7) 11_565 10_455
Cl4 C1 Cl3 71.72(7) 10_455 10_455
Cl3 C1 Cl3 180.0 . 10_455
C1 Cl3 Cl4 54.02(8) . 3_565
C1 Cl3 Cl4 54.02(8) . 2_665
Cl4 Cl3 Cl4 88.98(11) 3_565 2_665
C1 Cl3 Cl4 54.02(8) . .
Cl4 Cl3 Cl4 88.98(11) 3_565 .
Cl4 Cl3 Cl4 88.98(11) 2_665 .
Cl4 Cl4 C1 70.52(7) 12 .
Cl4 Cl4 Cl3 121.29(11) 12 .
C1 Cl4 Cl3 54.26(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Si1 Cl2 2.0368(8) .
Si1 Cl1 2.0395(8) .
Si1 Si1 2.3514(6) 33_545
Si1 Si1 2.3515(6) 32
C1 Cl4 1.7533(16) 12
C1 Cl4 1.7534(17) 3_565
C1 Cl4 1.7534(17) 2_665
C1 Cl4 1.7534(17) .
C1 Cl4 1.7534(17) 11_565
C1 Cl4 1.7534(17) 10_455
C1 Cl3 1.759(3) .
C1 Cl3 1.759(3) 10_455
Cl3 Cl4 2.057(3) 3_565
Cl3 Cl4 2.057(3) 2_665
Cl3 Cl4 2.057(3) .
Cl4 Cl4 1.170(4) 12
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Cl4 C1 Cl3 Cl4 133.74(15) 12 3_565
Cl4 C1 Cl3 Cl4 -120.000(1) 2_665 3_565
Cl4 C1 Cl3 Cl4 120.000(1) . 3_565
Cl4 C1 Cl3 Cl4 -106.26(15) 11_565 3_565
Cl4 C1 Cl3 Cl4 13.74(15) 10_455 3_565
Cl4 C1 Cl3 Cl4 -106.26(15) 12 2_665
Cl4 C1 Cl3 Cl4 120.000(0) 3_565 2_665
Cl4 C1 Cl3 Cl4 -120.000(0) . 2_665
Cl4 C1 Cl3 Cl4 13.74(15) 11_565 2_665
Cl4 C1 Cl3 Cl4 133.74(15) 10_455 2_665
Cl4 C1 Cl3 Cl4 13.74(15) 12 .
Cl4 C1 Cl3 Cl4 -120.000(1) 3_565 .
Cl4 C1 Cl3 Cl4 120.000(1) 2_665 .
Cl4 C1 Cl3 Cl4 133.74(15) 11_565 .
Cl4 C1 Cl3 Cl4 -106.26(15) 10_455 .
Cl4 C1 Cl4 Cl4 -139.5(2) 3_565 12
Cl4 C1 Cl4 Cl4 97.5(3) 2_665 12
Cl4 C1 Cl4 Cl4 61.35(19) 11_565 12
Cl4 C1 Cl4 Cl4 -97.8(2) 10_455 12
Cl3 C1 Cl4 Cl4 159.0(2) . 12
Cl3 C1 Cl4 Cl4 -21.0(2) 10_455 12
Cl4 C1 Cl4 Cl3 -159.0(2) 12 .
Cl4 C1 Cl4 Cl3 61.49(9) 3_565 .
Cl4 C1 Cl4 Cl3 -61.49(9) 2_665 .
Cl4 C1 Cl4 Cl3 -97.63(4) 11_565 .
Cl4 C1 Cl4 Cl3 103.24(6) 10_455 .
Cl3 C1 Cl4 Cl3 179.999(1) 10_455 .
