#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:28:27 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179379 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/76/4327682.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_4327682
loop_
_publ_author_name
'Jens Beckmann'
'Monique Biesemans'
'Karl Hassler'
'Klaus Jurkschat'
'Jose C. Martins'
'Markus Schürmann'
'Rudolph Willem'
_publ_section_title
;
 Reactions of [t-Bu2SnO]3 with [t-BuX2Si]2 (X = F, Cl). Syntheses and
 Structures of Novel Stannasiloxanes and of [(t-Bu2FSn)2O]2, the First
 Fluorine-Containing Tetraorganodistannoxane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4891
_journal_page_last               4897
_journal_paper_doi               10.1021/ic971504+
_journal_volume                  37
_journal_year                    1998
_chemical_formula_moiety         'C32 H72 F4 O4 Si4 Sn2'
_chemical_formula_sum            'C32 H72 F4 O4 Si4 Sn2'
_chemical_formula_weight         946.64
_chemical_melting_point          430
_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
_cell_angle_alpha                114.010(1)
_cell_angle_beta                 92.040(1)
_cell_angle_gamma                108.230(1)
_cell_formula_units_Z            1
_cell_length_a                   9.706(1)
_cell_length_b                   11.732(1)
_cell_length_c                   11.818(1)
_cell_measurement_reflns_used    13411
_cell_measurement_temperature    291(1)
_cell_measurement_theta_max      25.69
_cell_measurement_theta_min      4.50
_cell_volume                     1146.82(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      291(1)
_diffrn_detector_area_resol_mean '19 vertical, 18 horizontal'
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method
; 
360 frames via ω-rotation (Δω=1°) and two times 10s per frame
;
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_av_sigmaI/netI    0.0726
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -110
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13411
_diffrn_reflns_theta_max         25.69
_diffrn_reflns_theta_min         4.50
_diffrn_standards_decay_%        0
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    1.239
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.371
_exptl_crystal_density_meas      1.407(5)
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.949
_refine_ls_goodness_of_fit_obs   1.040
_refine_ls_matrix_type           full
_refine_ls_number_parameters     221
_refine_ls_number_reflns         3998
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_restrained_S_obs      1.040
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_obs          0.0347
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0268P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0774
_refine_ls_wR_factor_obs         0.0732
_reflns_number_observed          3033
_reflns_number_total             3998
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715042B_2.cif
_cod_data_source_block           (7)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0268P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1146.8(2)
_cod_database_code               4327682
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 0.07226(3) 0.24237(2) 0.19235(2) 0.04337(10) Uani 1 d .
Si1 Si 0.10548(11) -0.00623(10) 0.25893(9) 0.0435(2) Uani 1 d .
Si2 Si 0.04888(11) 0.22260(10) -0.10587(9) 0.0441(2) Uani 1 d .
F1 F 0.0182(2) 0.0371(2) 0.3732(2) 0.0625(6) Uani 1 d .
O1 O 0.1333(3) 0.1007(2) 0.2024(2) 0.0500(6) Uani 1 d .
O2 O 0.1033(3) 0.2174(3) 0.0214(2) 0.0515(6) Uani 1 d .
F2 F -0.0525(3) 0.3133(2) -0.0743(2) 0.0651(6) Uani 1 d .
C1 C -0.1601(4) 0.1983(4) 0.2010(4) 0.0564(10) Uani 1 d .
C2 C -0.1842(5) 0.2075(5) 0.3306(4) 0.0792(14) Uani 1 d .
H2A H -0.1546 0.1426 0.3443 0.096(3) Uiso 1 calc R
H2B H -0.2868 0.1901 0.3350 0.096(3) Uiso 1 calc R
H2C H -0.1263 0.2954 0.3942 0.096(3) Uiso 1 calc R
C3 C -0.2113(6) 0.2983(6) 0.1785(5) 0.091(2) Uani 1 d .
H3A H -0.1508 0.3873 0.2383 0.096(3) Uiso 1 calc R
H3B H -0.3123 0.2824 0.1885 0.096(3) Uiso 1 calc R
H3C H -0.2033 0.2884 0.0945 0.096(3) Uiso 1 calc R
C4 C -0.2459(5) 0.0577(5) 0.0981(5) 0.0813(15) Uani 1 d .
H4A H -0.2173 -0.0059 0.1151 0.096(3) Uiso 1 calc R
H4B H -0.2245 0.0523 0.0178 0.096(3) Uiso 1 calc R
H4C H -0.3498 0.0383 0.0968 0.096(3) Uiso 1 calc R
C5 C 0.2459(5) 0.4289(4) 0.3171(4) 0.0589(11) Uani 1 d .
C6 C 0.2501(6) 0.4464(5) 0.4529(4) 0.085(2) Uani 1 d .
H6A H 0.1576 0.4499 0.4771 0.096(3) Uiso 1 calc R
H6B H 0.3285 0.5279 0.5081 0.096(3) Uiso 1 calc R
H6C H 0.2667 0.3722 0.4585 0.096(3) Uiso 1 calc R
C7 C 0.2153(6) 0.5431(4) 0.3048(5) 0.090(2) Uani 1 d .
H7A H 0.1235(17) 0.5466(18) 0.3308(26) 0.096(3) Uiso 1 calc R
H7B H 0.2092(33) 0.5290(16) 0.2186(7) 0.096(3) Uiso 1 calc R
H7C H 0.2937(17) 0.6259(6) 0.3573(22) 0.096(3) Uiso 1 calc R
C8 C 0.3913(5) 0.4232(5) 0.2775(5) 0.0820(15) Uani 1 d .
H8A H 0.3864(13) 0.4088(32) 0.1913(10) 0.096(3) Uiso 1 calc R
H8B H 0.4100(17) 0.3511(19) 0.2859(28) 0.096(3) Uiso 1 calc R
H8C H 0.4695(7) 0.5060(12) 0.3303(20) 0.096(3) Uiso 1 calc R
C11 C 0.2846(4) 0.0006(4) 0.3332(4) 0.0527(10) Uani 1 d .
C12 C 0.2506(5) -0.0912(5) 0.3990(5) 0.085(2) Uani 1 d .
H12A H 0.1953 -0.1813 0.3381 0.096(3) Uiso 1 calc R
H12B H 0.1939 -0.0621 0.4625 0.096(3) Uiso 1 calc R
H12C H 0.3415 -0.0878 0.4376 0.096(3) Uiso 1 calc R
C13 C 0.3763(5) -0.0453(6) 0.2338(5) 0.084(2) Uani 1 d .
H13A H 0.3222 -0.1359 0.1734 0.096(3) Uiso 1 calc R
H13B H 0.4674 -0.0402 0.2736 0.096(3) Uiso 1 calc R
H13C H 0.3970 0.0114 0.1917 0.096(3) Uiso 1 calc R
C14 C 0.3738(5) 0.1427(5) 0.4306(4) 0.0807(15) Uani 1 d .
H14A H 0.3176 0.1719 0.4946 0.096(3) Uiso 1 calc R
H14B H 0.3956 0.2009 0.3902 0.096(3) Uiso 1 calc R
H14C H 0.4643 0.1448 0.4685 0.096(3) Uiso 1 calc R
C16 C 0.2825(5) 0.4570(4) -0.0594(4) 0.0712(13) Uani 1 d .
H16A H 0.2102 0.4990 -0.0408 0.096(3) Uiso 1 calc R
H16B H 0.3589 0.5050 -0.0900 0.096(3) Uiso 1 calc R
H16C H 0.3246 0.4579 0.0158 0.096(3) Uiso 1 calc R
C15 C 0.2085(4) 0.3121(4) -0.1604(4) 0.0533(10) Uani 1 d .
C17 C 0.1531(5) 0.3141(5) -0.2825(4) 0.0719(13) Uani 1 d .
H17A H 0.0799 0.3551 -0.2686 0.096(3) Uiso 1 calc R
H17B H 0.1104 0.2242 -0.3479 0.096(3) Uiso 1 calc R
H17C H 0.2344 0.3642 -0.3074 0.096(3) Uiso 1 calc R
C18 C 0.3230(5) 0.2451(5) -0.1835(5) 0.0734(13) Uani 1 d .
H18A H 0.2772 0.1534 -0.2445 0.096(3) Uiso 1 calc R
H18B H 0.3628 0.2491 -0.1058 0.096(3) Uiso 1 calc R
H18C H 0.4011 0.2906 -0.2146 0.096(3) Uiso 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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Sn Sn -0.6537 1.4246 '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
O2 Sn1 O1 99.97(11) .
O2 Sn1 C1 110.14(13) .
O1 Sn1 C1 109.68(13) .
O2 Sn1 C5 104.72(14) .
O1 Sn1 C5 105.46(13) .
C1 Sn1 C5 124.1(2) .
O1 Si1 F1 107.78(14) .
O1 Si1 C11 111.3(2) .
F1 Si1 C11 105.0(2) .
O1 Si1 Si2 110.92(10) 2
F1 Si1 Si2 106.90(10) 2
C11 Si1 Si2 114.45(13) 2
O2 Si2 F2 108.33(14) .
O2 Si2 C15 111.2(2) .
F2 Si2 C15 104.6(2) .
O2 Si2 Si1 110.57(10) 2
F2 Si2 Si1 106.05(10) 2
C15 Si2 Si1 115.57(13) 2
Si1 O1 Sn1 145.0(2) .
Si2 O2 Sn1 147.1(2) .
C3 C1 C2 109.1(4) .
C3 C1 C4 109.6(4) .
C2 C1 C4 110.7(4) .
C3 C1 Sn1 109.8(3) .
C2 C1 Sn1 109.6(3) .
C4 C1 Sn1 108.1(3) .
C8 C5 C7 110.0(4) .
C8 C5 C6 110.0(4) .
C7 C5 C6 110.5(4) .
C8 C5 Sn1 108.1(3) .
C7 C5 Sn1 108.9(3) .
C6 C5 Sn1 109.3(3) .
C14 C11 C13 108.8(4) .
C14 C11 C12 108.9(4) .
C13 C11 C12 109.2(4) .
C14 C11 Si1 110.2(3) .
C13 C11 Si1 110.8(3) .
C12 C11 Si1 109.0(3) .
C18 C15 C17 109.2(4) .
C18 C15 C16 108.7(3) .
C17 C15 C16 108.3(3) .
C18 C15 Si2 111.3(3) .
C17 C15 Si2 109.8(3) .
C16 C15 Si2 109.4(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 O2 1.969(2) .
Sn1 O1 1.975(2) .
Sn1 C1 2.166(4) .
Sn1 C5 2.167(4) .
Si1 O1 1.605(3) .
Si1 F1 1.610(2) .
Si1 C11 1.883(4) .
Si1 Si2 2.3772(14) 2
Si2 O2 1.607(2) .
Si2 F2 1.612(2) .
Si2 C15 1.877(4) .
Si2 Si1 2.3772(14) 2
C1 C3 1.518(6) .
C1 C2 1.523(6) .
C1 C4 1.526(6) .
C5 C8 1.514(6) .
C5 C7 1.519(6) .
C5 C6 1.530(6) .
C11 C14 1.522(5) .
C11 C13 1.524(6) .
C11 C12 1.533(6) .
C16 C15 1.535(5) .
C15 C18 1.523(6) .
C15 C17 1.534(5) .
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
F1 Si1 O1 Sn1 -18.0(3) .
C11 Si1 O1 Sn1 -132.7(3) .
Si2 Si1 O1 Sn1 98.7(3) 2
O2 Sn1 O1 Si1 -147.1(3) .
C1 Sn1 O1 Si1 -31.4(3) .
C5 Sn1 O1 Si1 104.4(3) .
F2 Si2 O2 Sn1 19.1(3) .
C15 Si2 O2 Sn1 133.5(3) .
Si1 Si2 O2 Sn1 -96.7(3) 2
O1 Sn1 O2 Si2 145.8(3) .
C1 Sn1 O2 Si2 30.4(3) .
C5 Sn1 O2 Si2 -105.2(3) .
O2 Sn1 C1 C3 -64.6(3) .
O1 Sn1 C1 C3 -173.6(3) .
C5 Sn1 C1 C3 60.6(4) .
O2 Sn1 C1 C2 175.6(3) .
O1 Sn1 C1 C2 66.5(3) .
C5 Sn1 C1 C2 -59.2(3) .
O2 Sn1 C1 C4 54.9(3) .
O1 Sn1 C1 C4 -54.2(3) .
C5 Sn1 C1 C4 -180.0(3) .
O2 Sn1 C5 C8 -50.1(3) .
O1 Sn1 C5 C8 54.8(3) .
C1 Sn1 C5 C8 -177.6(3) .
O2 Sn1 C5 C7 69.3(4) .
O1 Sn1 C5 C7 174.3(3) .
C1 Sn1 C5 C7 -58.1(4) .
O2 Sn1 C5 C6 -169.9(3) .
O1 Sn1 C5 C6 -64.9(3) .
C1 Sn1 C5 C6 62.6(4) .
O1 Si1 C11 C14 54.0(3) .
F1 Si1 C11 C14 -62.4(3) .
Si2 Si1 C11 C14 -179.3(3) 2
O1 Si1 C11 C13 -66.5(3) .
F1 Si1 C11 C13 177.1(3) .
Si2 Si1 C11 C13 60.3(3) 2
O1 Si1 C11 C12 173.4(3) .
F1 Si1 C11 C12 57.1(3) .
Si2 Si1 C11 C12 -59.8(3) 2
O2 Si2 C15 C18 58.3(3) .
F2 Si2 C15 C18 175.0(3) .
Si1 Si2 C15 C18 -68.8(3) 2
O2 Si2 C15 C17 179.4(3) .
F2 Si2 C15 C17 -63.9(3) .
Si1 Si2 C15 C17 52.4(3) 2
O2 Si2 C15 C16 -61.8(3) .
F2 Si2 C15 C16 54.9(3) .
Si1 Si2 C15 C16 171.1(2) 2
