#------------------------------------------------------------------------------
#$Date: 2016-03-26 14:31:31 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180266 $
#$URL: svn://www.crystallography.net/cod/cif/7/11/52/7115292.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_7115292
loop_
_publ_author_name
'Alasdair P. M. Robertson'
'Jordan N. Friedmann'
'Hilary A. Jenkins'
'Neil Burford'
_publ_section_title
;
 Exploring structural trends for complexes of Me2E(OSO2CF3)2 (E = Si, Ge,
 Sn) with pyridine derivatives
;
_journal_name_full               Chem.Commun.
_journal_page_first              7979
_journal_paper_doi               10.1039/C4CC01109K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C18 H26 F6 N4 O6 S2 Sn'
_chemical_formula_sum            'C18 H26 F6 N4 O6 S2 Sn'
_chemical_formula_weight         691.24
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 100.452(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.4758(5)
_cell_length_b                   13.6913(6)
_cell_length_c                   21.1332(12)
_cell_measurement_reflns_used    8995
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.64
_cell_volume                     2696.2(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            32769
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.308
_diffrn_reflns_theta_min         1.960
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  0.9525
_exptl_absorpt_correction_T_min  0.8654
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.703
_exptl_crystal_description       block
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.078
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     168
_refine_ls_number_reflns         5618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0359
_refine_ls_R_factor_gt           0.0251
_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)+(0.0291P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0553
_refine_ls_wR_factor_ref         0.0570
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4648
_reflns_number_total             5618
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c4cc01109k2.cif
_cod_data_source_block           cc
_cod_database_code               7115292
#BEGIN Tags that were not found in dictionaries:
_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. 
;
_shelxl_version_number           2013-3
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Sn1 Sn 0.0000 0.28717(2) 0.2500 0.01810(4) Uani 1 2 d S T P
S1 S 0.01949(4) 0.12162(2) 0.39064(2) 0.02401(7) Uani 1 1 d . . .
F1 F 0.11031(11) -0.03333(7) 0.33783(6) 0.0515(3) Uani 1 1 d . . .
F2 F -0.11474(11) -0.00324(8) 0.30743(5) 0.0528(3) Uani 1 1 d . . .
F3 F -0.03708(11) -0.06337(7) 0.40104(6) 0.0525(3) Uani 1 1 d . . .
O1 O 0.13042(13) 0.10956(9) 0.44579(5) 0.0423(3) Uani 1 1 d . . .
O2 O -0.11869(12) 0.15060(8) 0.40200(5) 0.0380(3) Uani 1 1 d . . .
O3 O 0.06781(11) 0.17409(8) 0.33832(5) 0.0337(2) Uani 1 1 d . . .
N1 N 0.02779(12) 0.40335(8) 0.32381(5) 0.0210(2) Uani 1 1 d . . .
N2 N 0.06649(12) 0.62247(8) 0.46284(5) 0.0251(2) Uani 1 1 d . . .
C1 C 0.21563(15) 0.25857(11) 0.24412(7) 0.0283(3) Uani 1 1 d . . .
H1B H 0.2367 0.2860 0.2051 0.042 Uiso 1 1 calc R U .
H1C H 0.2312 0.1893 0.2443 0.042 Uiso 1 1 calc R U .
H1D H 0.2773 0.2874 0.2804 0.042 Uiso 1 1 calc R U .
C3 C -0.06181(14) 0.48124(10) 0.31771(6) 0.0238(3) Uani 1 1 d . . .
H3A H -0.1331 0.4851 0.2812 0.029 Uiso 1 1 calc R U .
C4 C -0.05332(14) 0.55442(10) 0.36209(6) 0.0245(3) Uani 1 1 d . . .
H4B H -0.1178 0.6062 0.3552 0.029 Uiso 1 1 calc R U .
C5 C 0.05334(13) 0.55177(9) 0.41859(6) 0.0205(2) Uani 1 1 d . . .
C6 C 0.14431(14) 0.46832(9) 0.42534(6) 0.0222(2) Uani 1 1 d . . .
H6A H 0.2149 0.4610 0.4618 0.027 Uiso 1 1 calc R U .
C7 C 0.12797(13) 0.39907(9) 0.37825(6) 0.0218(2) Uani 1 1 d . . .
H7A H 0.1894 0.3456 0.3839 0.026 Uiso 1 1 calc R U .
C8 C 0.18154(15) 0.61983(11) 0.51890(6) 0.0296(3) Uani 1 1 d . . .
H8A H 0.1739 0.5611 0.5429 0.044 Uiso 1 1 calc R U .
H8B H 0.1739 0.6756 0.5456 0.044 Uiso 1 1 calc R U .
H8C H 0.2726 0.6211 0.5051 0.044 Uiso 1 1 calc R U .
C9 C -0.02448(19) 0.70880(10) 0.45249(8) 0.0365(3) Uani 1 1 d . . .
H9A H -0.1232 0.6898 0.4487 0.055 Uiso 1 1 calc R U .
H9B H -0.0109 0.7410 0.4137 0.055 Uiso 1 1 calc R U .
H9C H 0.0006 0.7526 0.4882 0.055 Uiso 1 1 calc R U .
C10 C -0.00719(16) -0.00107(10) 0.35708(8) 0.0322(3) Uani 1 1 d . . .
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'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 '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_1
_geom_angle_site_symmetry_3
C1 Sn1 C1 158.57(8) . 2
C1 Sn1 N1 94.87(5) . 2
C1 Sn1 N1 100.53(5) 2 2
C1 Sn1 N1 100.53(5) . .
C1 Sn1 N1 94.87(5) 2 .
N1 Sn1 N1 87.92(6) 2 .
C1 Sn1 O3 87.72(5) . 2
C1 Sn1 O3 78.57(5) 2 2
N1 Sn1 O3 86.28(4) 2 2
N1 Sn1 O3 170.29(4) . 2
C1 Sn1 O3 78.57(5) . .
C1 Sn1 O3 87.72(5) 2 .
N1 Sn1 O3 170.29(4) 2 .
N1 Sn1 O3 86.28(4) . .
O3 Sn1 O3 100.47(5) 2 .
O2 S1 O1 117.08(7) . .
O2 S1 O3 114.41(7) . .
O1 S1 O3 112.88(7) . .
O2 S1 C10 104.74(7) . .
O1 S1 C10 103.89(7) . .
O3 S1 C10 101.49(7) . .
S1 O3 Sn1 145.37(7) . .
C3 N1 C7 116.47(11) . .
C3 N1 Sn1 120.48(9) . .
C7 N1 Sn1 122.97(8) . .
C5 N2 C9 120.37(12) . .
C5 N2 C8 120.80(11) . .
C9 N2 C8 118.52(11) . .
Sn1 C1 H1B 109.5 . .
Sn1 C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
Sn1 C1 H1D 109.5 . .
H1B C1 H1D 109.5 . .
H1C C1 H1D 109.5 . .
N1 C3 C4 123.70(12) . .
N1 C3 H3A 118.1 . .
C4 C3 H3A 118.1 . .
C3 C4 C5 120.26(12) . .
C3 C4 H4B 119.9 . .
C5 C4 H4B 119.9 . .
N2 C5 C4 122.18(12) . .
N2 C5 C6 122.26(12) . .
C4 C5 C6 115.55(11) . .
C7 C6 C5 119.93(12) . .
C7 C6 H6A 120.0 . .
C5 C6 H6A 120.0 . .
N1 C7 C6 124.04(12) . .
N1 C7 H7A 118.0 . .
C6 C7 H7A 118.0 . .
N2 C8 H8A 109.5 . .
N2 C8 H8B 109.5 . .
H8A C8 H8B 109.5 . .
N2 C8 H8C 109.5 . .
H8A C8 H8C 109.5 . .
H8B C8 H8C 109.5 . .
N2 C9 H9A 109.5 . .
N2 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
N2 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
F2 C10 F1 108.50(13) . .
F2 C10 F3 107.98(12) . .
F1 C10 F3 107.30(12) . .
F2 C10 S1 111.19(10) . .
F1 C10 S1 111.15(10) . .
F3 C10 S1 110.58(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 C1 2.1062(13) .
Sn1 C1 2.1062(13) 2
Sn1 N1 2.2097(10) 2
Sn1 N1 2.2098(10) .
Sn1 O3 2.4204(10) 2
Sn1 O3 2.4204(10) .
S1 O2 1.4296(11) .
S1 O1 1.4305(11) .
S1 O3 1.4601(10) .
S1 C10 1.8231(15) .
F1 C10 1.3284(17) .
F2 C10 1.3239(18) .
F3 C10 1.3290(18) .
N1 C3 1.3547(16) .
N1 C7 1.3535(16) .
N2 C5 1.3360(16) .
N2 C9 1.4559(18) .
N2 C8 1.4576(18) .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C1 H1D 0.9600 .
C3 C4 1.3647(18) .
C3 H3A 0.9300 .
C4 C5 1.4180(18) .
C4 H4B 0.9300 .
C5 C6 1.4227(17) .
C6 C7 1.3630(18) .
C6 H6A 0.9300 .
C7 H7A 0.9300 .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
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
O2 S1 O3 Sn1 -9.01(15)
O1 S1 O3 Sn1 -146.24(11)
C10 S1 O3 Sn1 103.16(12)
C7 N1 C3 C4 1.6(2)
Sn1 N1 C3 C4 178.33(10)
N1 C3 C4 C5 -0.2(2)
C9 N2 C5 C4 -3.7(2)
C8 N2 C5 C4 -177.08(12)
C9 N2 C5 C6 177.06(13)
C8 N2 C5 C6 3.64(19)
C3 C4 C5 N2 179.16(12)
C3 C4 C5 C6 -1.51(18)
N2 C5 C6 C7 -178.88(12)
C4 C5 C6 C7 1.79(18)
C3 N1 C7 C6 -1.25(19)
Sn1 N1 C7 C6 -177.93(10)
C5 C6 C7 N1 -0.4(2)
O2 S1 C10 F2 52.46(12)
O1 S1 C10 F2 175.82(11)
O3 S1 C10 F2 -66.86(11)
O2 S1 C10 F1 173.45(11)
O1 S1 C10 F1 -63.19(13)
O3 S1 C10 F1 54.13(13)
O2 S1 C10 F3 -67.49(12)
O1 S1 C10 F3 55.88(12)
O3 S1 C10 F3 173.20(10)
