#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/57/4085733.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_4085733
loop_
_publ_author_name
'Zitz, Rainer'
'Gatterer, Karl'
'Reinhold, Crispin R. W.'
'Müller, Thomas'
'Baumgartner, Judith'
'Marschner, Christoph'
_publ_section_title
;
 Oligosilanylated Antimony Compounds.
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1419
_journal_page_last               1430
_journal_paper_doi               10.1021/om501075v
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C28 H84 Sb2 Si14'
_chemical_formula_weight         1057.71
_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   constr
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.44(3)
_cell_angle_beta                 107.99(3)
_cell_angle_gamma                105.41(3)
_cell_formula_units_Z            1
_cell_length_a                   9.2013(18)
_cell_length_b                   12.006(2)
_cell_length_c                   14.448(3)
_cell_measurement_reflns_used    5713
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      52.527
_cell_measurement_theta_min      4.737
_cell_volume                     1384.3(7)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.972
_diffrn_measured_fraction_theta_max 0.972
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9327
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.86
_exptl_absorpt_coefficient_mu    1.297
_exptl_absorpt_correction_T_max  0.9033
_exptl_absorpt_correction_T_min  0.6596
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.269
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         1.722
_refine_diff_density_min         -2.114
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.291
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     213
_refine_ls_number_reflns         4738
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.291
_refine_ls_R_factor_all          0.0800
_refine_ls_R_factor_gt           0.0726
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0254P)²+11.2910P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1392
_refine_ls_wR_factor_ref         0.1418
_reflns_number_gt                4429
_reflns_number_total             4738
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om501075v_si_002.cif
_cod_data_source_block           3_925j
_cod_depositor_comments
;Adding full bibliography for 4085733--4085739.cif.

 Adding full bibliography for 4085733--4085739.cif.
;
_cod_original_cell_volume        1384.3(5)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4085733
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
Sb1 Sb -0.03778(6) 0.03766(5) 0.08854(4) 0.01364(16) Uani 1 1 d .
Si2 Si 0.3082(3) 0.1451(2) 0.33338(16) 0.0173(5) Uani 1 1 d .
Si3 Si 0.2031(3) 0.24375(19) 0.21770(17) 0.0172(5) Uani 1 1 d .
Si7 Si 0.4086(3) 0.3551(2) 0.17380(17) 0.0195(5) Uani 1 1 d .
Si1 Si 0.1264(3) -0.04981(19) 0.21968(16) 0.0163(5) Uani 1 1 d .
Si4 Si 0.2674(3) -0.1691(2) 0.16546(17) 0.0205(5) Uani 1 1 d .
Si6 Si 0.0872(3) 0.3727(2) 0.29243(17) 0.0200(5) Uani 1 1 d .
Si5 Si -0.0562(3) -0.1502(2) 0.28396(17) 0.0203(5) Uani 1 1 d .
C1 C 0.5314(9) 0.1653(8) 0.3681(7) 0.027(2) Uani 1 1 d .
H1A H 0.5997 0.2466 0.4182 0.041 Uiso 1 1 calc R
H1B H 0.5557 0.1569 0.3061 0.041 Uiso 1 1 calc R
H1C H 0.5545 0.1029 0.3980 0.041 Uiso 1 1 calc R
C12 C 0.5847(10) 0.4587(8) 0.2957(7) 0.030(2) Uani 1 1 d .
H12A H 0.6769 0.4990 0.2795 0.045 Uiso 1 1 calc R
H12B H 0.6177 0.4109 0.3399 0.045 Uiso 1 1 calc R
H12C H 0.5519 0.5206 0.3315 0.045 Uiso 1 1 calc R
C4 C 0.3797(10) -0.2108(8) 0.2769(7) 0.0270(19) Uani 1 1 d .
H4A H 0.3008 -0.2667 0.2939 0.041 Uiso 1 1 calc R
H4B H 0.4454 -0.1367 0.3365 0.041 Uiso 1 1 calc R
H4C H 0.4516 -0.2508 0.2586 0.041 Uiso 1 1 calc R
C7 C 0.0507(12) -0.2035(9) 0.3896(7) 0.032(2) Uani 1 1 d .
H7A H 0.1381 -0.1331 0.4458 0.048 Uiso 1 1 calc R
H7B H 0.0978 -0.2608 0.3627 0.048 Uiso 1 1 calc R
H7C H -0.0281 -0.2443 0.4153 0.048 Uiso 1 1 calc R
C13 C 0.3389(10) 0.4529(8) 0.0993(7) 0.028(2) Uani 1 1 d .
H13A H 0.3177 0.5162 0.1428 0.043 Uiso 1 1 calc R
H13B H 0.2383 0.4025 0.0389 0.043 Uiso 1 1 calc R
H13C H 0.4241 0.4913 0.0769 0.043 Uiso 1 1 calc R
C14 C 0.4817(11) 0.2511(8) 0.0989(7) 0.029(2) Uani 1 1 d .
H14A H 0.3900 0.1950 0.0354 0.043 Uiso 1 1 calc R
H14B H 0.5262 0.2041 0.1403 0.043 Uiso 1 1 calc R
H14C H 0.5672 0.2997 0.0817 0.043 Uiso 1 1 calc R
C11 C -0.0156(11) 0.4484(8) 0.2069(7) 0.031(2) Uani 1 1 d .
H11A H -0.0508 0.5059 0.2457 0.046 Uiso 1 1 calc R
H11B H -0.1111 0.3865 0.1486 0.046 Uiso 1 1 calc R
H11C H 0.0611 0.4927 0.1815 0.046 Uiso 1 1 calc R
C2 C 0.2894(11) 0.1882(8) 0.4618(6) 0.028(2) Uani 1 1 d .
H2A H 0.3208 0.1338 0.4995 0.042 Uiso 1 1 calc R
H2B H 0.1760 0.1801 0.4507 0.042 Uiso 1 1 calc R
H2C H 0.3618 0.2728 0.5019 0.042 Uiso 1 1 calc R
C3 C 0.4187(11) -0.0863(9) 0.1184(7) 0.033(2) Uani 1 1 d .
H3A H 0.5038 -0.0154 0.1753 0.049 Uiso 1 1 calc R
H3B H 0.3623 -0.0587 0.0633 0.049 Uiso 1 1 calc R
H3C H 0.4688 -0.1414 0.0919 0.049 Uiso 1 1 calc R
C8 C -0.1504(10) -0.0453(8) 0.3372(7) 0.0268(19) Uani 1 1 d .
H8A H -0.1976 -0.0101 0.2854 0.040 Uiso 1 1 calc R
H8B H -0.0663 0.0204 0.3987 0.040 Uiso 1 1 calc R
H8C H -0.2366 -0.0913 0.3553 0.040 Uiso 1 1 calc R
C6 C -0.2267(10) -0.2867(8) 0.1796(7) 0.032(2) Uani 1 1 d .
H6A H -0.3079 -0.3212 0.2063 0.048 Uiso 1 1 calc R
H6B H -0.1825 -0.3483 0.1566 0.048 Uiso 1 1 calc R
H6C H -0.2788 -0.2617 0.1215 0.048 Uiso 1 1 calc R
C5 C 0.1187(12) -0.3125(8) 0.0587(7) 0.034(2) Uani 1 1 d .
H5A H 0.1784 -0.3624 0.0368 0.050 Uiso 1 1 calc R
H5B H 0.0582 -0.2914 0.0004 0.050 Uiso 1 1 calc R
H5C H 0.0418 -0.3587 0.0830 0.050 Uiso 1 1 calc R
C9 C -0.0709(12) 0.2859(9) 0.3314(8) 0.041(2) Uani 1 1 d .
H9A H -0.1305 0.3373 0.3508 0.061 Uiso 1 1 calc R
H9B H -0.0178 0.2625 0.3902 0.061 Uiso 1 1 calc R
H9C H -0.1476 0.2124 0.2738 0.061 Uiso 1 1 calc R
C10 C 0.2538(12) 0.4959(9) 0.4079(7) 0.039(2) Uani 1 1 d .
H10A H 0.3294 0.5482 0.3864 0.059 Uiso 1 1 calc R
H10B H 0.3133 0.4594 0.4538 0.059 Uiso 1 1 calc R
H10C H 0.2064 0.5451 0.4444 0.059 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'
H H 0.0000 0.0000 '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'
Sb Sb -0.5866 1.5461 '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
Si1 Sb1 Si3 80.48(7) .
Si1 Sb1 Sb1 103.10(6) 2
Si3 Sb1 Sb1 107.65(6) 2
C2 Si2 C1 104.1(4) .
C2 Si2 Si1 114.7(3) .
C1 Si2 Si1 113.9(3) .
C2 Si2 Si3 116.0(3) .
C1 Si2 Si3 115.9(3) .
Si1 Si2 Si3 92.68(11) .
Si7 Si3 Si6 110.80(12) .
Si7 Si3 Si2 110.99(11) .
Si6 Si3 Si2 109.34(12) .
Si7 Si3 Sb1 123.30(11) .
Si6 Si3 Sb1 108.12(10) .
Si2 Si3 Sb1 92.53(9) .
C13 Si7 C14 109.5(4) .
C13 Si7 C12 107.3(4) .
C14 Si7 C12 108.6(4) .
C13 Si7 Si3 112.2(3) .
C14 Si7 Si3 111.1(3) .
C12 Si7 Si3 108.1(3) .
Si4 Si1 Si5 112.48(12) .
Si4 Si1 Si2 111.17(11) .
Si5 Si1 Si2 113.41(12) .
Si4 Si1 Sb1 118.44(10) .
Si5 Si1 Sb1 106.53(10) .
Si2 Si1 Sb1 93.53(9) .
C4 Si4 C5 109.0(4) .
C4 Si4 C3 108.9(4) .
C5 Si4 C3 108.5(4) .
C4 Si4 Si1 108.3(3) .
C5 Si4 Si1 109.9(3) .
C3 Si4 Si1 112.3(3) .
C11 Si6 C9 106.0(4) .
C11 Si6 C10 107.2(5) .
C9 Si6 C10 109.5(5) .
C11 Si6 Si3 114.7(3) .
C9 Si6 Si3 111.0(3) .
C10 Si6 Si3 108.3(3) .
C8 Si5 C6 107.6(4) .
C8 Si5 C7 108.1(4) .
C6 Si5 C7 108.3(4) .
C8 Si5 Si1 110.4(3) .
C6 Si5 Si1 111.0(3) .
C7 Si5 Si1 111.3(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sb1 Si1 2.628(2) .
Sb1 Si3 2.657(3) .
Sb1 Sb1 2.8779(13) 2
Si2 C2 1.891(8) .
Si2 C1 1.890(8) .
Si2 Si1 2.354(3) .
Si2 Si3 2.365(3) .
Si3 Si7 2.351(3) .
Si3 Si6 2.359(3) .
Si7 C13 1.862(8) .
Si7 C14 1.870(8) .
Si7 C12 1.870(9) .
Si1 Si4 2.341(3) .
Si1 Si5 2.347(3) .
Si4 C4 1.872(8) .
Si4 C5 1.875(9) .
Si4 C3 1.879(9) .
Si6 C11 1.862(9) .
Si6 C9 1.863(9) .
Si6 C10 1.864(9) .
Si5 C8 1.872(8) .
Si5 C6 1.878(9) .
Si5 C7 1.879(8) .
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
C2 Si2 Si3 Si7 120.6(3) .
C1 Si2 Si3 Si7 -2.0(3) .
Si1 Si2 Si3 Si7 -120.28(12) .
C2 Si2 Si3 Si6 -2.0(3) .
C1 Si2 Si3 Si6 -124.5(3) .
Si1 Si2 Si3 Si6 117.20(12) .
C2 Si2 Si3 Sb1 -112.2(3) .
C1 Si2 Si3 Sb1 125.3(3) .
Si1 Si2 Si3 Sb1 6.98(9) .
Si1 Sb1 Si3 Si7 110.92(13) .
Sb1 Sb1 Si3 Si7 10.10(13) 2
Si1 Sb1 Si3 Si6 -117.63(11) .
Sb1 Sb1 Si3 Si6 141.55(9) 2
Si1 Sb1 Si3 Si2 -6.33(8) .
Sb1 Sb1 Si3 Si2 -107.15(8) 2
Si6 Si3 Si7 C13 -49.5(3) .
Si2 Si3 Si7 C13 -171.2(3) .
Sb1 Si3 Si7 C13 80.8(3) .
Si6 Si3 Si7 C14 -172.4(3) .
Si2 Si3 Si7 C14 65.9(3) .
Sb1 Si3 Si7 C14 -42.1(3) .
Si6 Si3 Si7 C12 68.6(3) .
Si2 Si3 Si7 C12 -53.1(3) .
Sb1 Si3 Si7 C12 -161.1(3) .
C2 Si2 Si1 Si4 -124.4(3) .
C1 Si2 Si1 Si4 -4.6(3) .
Si3 Si2 Si1 Si4 115.31(12) .
C2 Si2 Si1 Si5 3.5(3) .
C1 Si2 Si1 Si5 123.3(3) .
Si3 Si2 Si1 Si5 -116.78(12) .
C2 Si2 Si1 Sb1 113.2(3) .
C1 Si2 Si1 Sb1 -127.0(3) .
Si3 Si2 Si1 Sb1 -7.07(9) .
Si3 Sb1 Si1 Si4 -110.04(12) .
Sb1 Sb1 Si1 Si4 -3.99(12) 2
Si3 Sb1 Si1 Si5 122.06(11) .
Sb1 Sb1 Si1 Si5 -131.88(9) 2
Si3 Sb1 Si1 Si2 6.37(8) .
Sb1 Sb1 Si1 Si2 112.43(8) 2
Si5 Si1 Si4 C4 -57.7(3) .
Si2 Si1 Si4 C4 70.7(3) .
Sb1 Si1 Si4 C4 177.2(3) .
Si5 Si1 Si4 C5 61.2(3) .
Si2 Si1 Si4 C5 -170.4(3) .
Sb1 Si1 Si4 C5 -63.8(3) .
Si5 Si1 Si4 C3 -178.0(3) .
Si2 Si1 Si4 C3 -49.6(3) .
Sb1 Si1 Si4 C3 57.0(3) .
Si7 Si3 Si6 C11 61.8(4) .
Si2 Si3 Si6 C11 -175.6(3) .
Sb1 Si3 Si6 C11 -76.1(3) .
Si7 Si3 Si6 C9 -178.1(4) .
Si2 Si3 Si6 C9 -55.5(4) .
Sb1 Si3 Si6 C9 44.0(4) .
Si7 Si3 Si6 C10 -57.9(4) .
Si2 Si3 Si6 C10 64.8(4) .
Sb1 Si3 Si6 C10 164.2(4) .
Si4 Si1 Si5 C8 174.7(3) .
Si2 Si1 Si5 C8 47.5(3) .
Sb1 Si1 Si5 C8 -53.9(3) .
Si4 Si1 Si5 C6 -66.0(3) .
Si2 Si1 Si5 C6 166.8(3) .
Sb1 Si1 Si5 C6 65.4(3) .
Si4 Si1 Si5 C7 54.7(4) .
Si2 Si1 Si5 C7 -72.5(3) .
Sb1 Si1 Si5 C7 -174.0(3) .
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.062 0.450 0.556 7 1 ' '
2 0.937 0.550 0.444 7 1 ' '
