#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:20:45 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179056 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/18/4301883.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_4301883
loop_
_publ_author_name
'Michael Wolff'
'Thomas Harmening'
'Rainer Pöttgen'
'Claus Feldmann'
_publ_section_title
;
Sn3I8.2(18-crown-6): a Mixed-Valent Tin-Crown-Ether Complex
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3153
_journal_page_last               3156
_journal_paper_doi               10.1021/ic8024183
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C24 H48 I8 O12 Sn3'
_chemical_formula_weight         1899.9679
_chemical_name_systematic
; 
 ?
;
_space_group_IT_number           13
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.03(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.418(3)
_cell_length_b                   7.9111(16)
_cell_length_c                   24.586(5)
_cell_measurement_reflns_used    2000
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      52.1
_cell_measurement_theta_min      3.3
_cell_volume                     2413.8(9)
_computing_cell_refinement       'CELL, SELECT (STOE)'
_computing_data_collection       'EXPOSE (STOE)'
_computing_data_reduction        'INTEGRATE (STOE)'
_computing_molecular_graphics    'DIAMOND, Crystal Impact'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_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  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0287
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            18916
_diffrn_reflns_theta_full        25.93
_diffrn_reflns_theta_max         25.93
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    6.700
_exptl_absorpt_correction_T_max  0.3229
_exptl_absorpt_correction_T_min  0.1917
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
 The numerical absoption correction was performed using 
 X-RED (V1.19, STOE, 1999) and X-SHAPE (V1.06, STOE, 1999)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.6139
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1724
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.937
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.138
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     216
_refine_ls_number_reflns         4628
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0265
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0354P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0600
_reflns_number_gt                3834
_reflns_number_total             4628
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8024183_si_001.cif
_cod_data_source_block           '[Sn2I3(18-crown-6)2][SnI5]'
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Numerical' changed to 'numerical'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 2/n'
_cod_database_code               4301883
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.73959(2) 0.47137(4) 0.386373(12) 0.02373(8) Uani 1 1 d . . .
Sn2 Sn 0.7500 0.05110(6) 0.7500 0.02141(10) Uani 1 2 d S . .
I4 I 0.56024(2) 0.22503(5) 0.742399(13) 0.03416(9) Uani 1 1 d . . .
I3 I 0.76010(2) 0.04515(5) 0.633441(12) 0.03320(9) Uani 1 1 d . . .
I1 I 0.76936(3) 0.29031(4) 0.487024(13) 0.03122(9) Uani 1 1 d . . .
I5 I 0.7500 -0.29595(6) 0.7500 0.03718(12) Uani 1 2 d S . .
I2 I 0.7500 0.61720(8) 0.2500 0.04727(14) Uani 1 2 d S . .
O1 O 0.6332(3) 0.1935(5) 0.35373(15) 0.0391(9) Uani 1 1 d . . .
O4 O 0.8316(2) 0.7418(4) 0.44199(14) 0.0302(7) Uani 1 1 d . . .
O5 O 0.6134(3) 0.6962(4) 0.45470(15) 0.0334(8) Uani 1 1 d . . .
O3 O 0.9496(3) 0.4921(5) 0.39236(16) 0.0355(8) Uani 1 1 d . . .
O6 O 0.5155(2) 0.4701(5) 0.38599(15) 0.0326(8) Uani 1 1 d . . .
O2 O 0.8496(2) 0.2286(4) 0.34089(14) 0.0311(7) Uani 1 1 d . . .
C5 C 0.9920(4) 0.6599(7) 0.4003(2) 0.0407(13) Uani 1 1 d . . .
H5A H 0.9720 0.7308 0.3694 0.049(4) Uiso 1 1 calc R . .
H5B H 1.0700 0.6563 0.4040 0.049(4) Uiso 1 1 calc R . .
C2 C 0.8012(4) 0.0654(7) 0.3396(2) 0.0370(12) Uani 1 1 d . . .
H2A H 0.8019 0.0174 0.3760 0.049(4) Uiso 1 1 calc R . .
H2B H 0.8408 -0.0095 0.3163 0.049(4) Uiso 1 1 calc R . .
C3 C 0.9627(4) 0.2213(8) 0.3555(3) 0.0438(14) Uani 1 1 d . . .
H3A H 0.9999 0.1493 0.3303 0.049(4) Uiso 1 1 calc R . .
H3B H 0.9734 0.1756 0.3919 0.049(4) Uiso 1 1 calc R . .
C11 C 0.4659(4) 0.3099(8) 0.3773(3) 0.0476(16) Uani 1 1 d . . .
H11A H 0.3907 0.3245 0.3662 0.049(4) Uiso 1 1 calc R . .
H11B H 0.4694 0.2443 0.4107 0.049(4) Uiso 1 1 calc R . .
C6 C 0.9464(4) 0.7289(8) 0.4503(2) 0.0394(13) Uani 1 1 d . . .
H6A H 0.9635 0.6549 0.4809 0.049(4) Uiso 1 1 calc R . .
H6B H 0.9768 0.8395 0.4582 0.049(4) Uiso 1 1 calc R . .
C10 C 0.4528(4) 0.5723(7) 0.4207(2) 0.0368(12) Uani 1 1 d . . .
H10A H 0.4426 0.5145 0.4549 0.049(4) Uiso 1 1 calc R . .
H10B H 0.3825 0.5935 0.4036 0.049(4) Uiso 1 1 calc R . .
C1 C 0.6881(4) 0.0849(8) 0.3181(3) 0.0482(15) Uani 1 1 d . . .
H1A H 0.6876 0.1329 0.2818 0.049(4) Uiso 1 1 calc R . .
H1B H 0.6528 -0.0244 0.3162 0.049(4) Uiso 1 1 calc R . .
C12 C 0.5243(4) 0.2212(9) 0.3341(3) 0.0564(19) Uani 1 1 d . . .
H12A H 0.4897 0.1140 0.3256 0.049(4) Uiso 1 1 calc R . .
H12B H 0.5237 0.2893 0.3013 0.049(4) Uiso 1 1 calc R . .
C7 C 0.7807(4) 0.7963(7) 0.4899(2) 0.0348(11) Uani 1 1 d . . .
H7A H 0.8187 0.8928 0.5056 0.049(4) Uiso 1 1 calc R . .
H7B H 0.7816 0.7061 0.5166 0.049(4) Uiso 1 1 calc R . .
C4 C 1.0049(4) 0.3955(8) 0.3532(3) 0.0446(14) Uani 1 1 d . . .
H4A H 1.0818 0.3963 0.3617 0.049(4) Uiso 1 1 calc R . .
H4B H 0.9924 0.4425 0.3171 0.049(4) Uiso 1 1 calc R . .
C9 C 0.5100(4) 0.7338(7) 0.4305(2) 0.0386(12) Uani 1 1 d . . .
H9A H 0.5180 0.7937 0.3965 0.049(4) Uiso 1 1 calc R . .
H9B H 0.4696 0.8048 0.4546 0.049(4) Uiso 1 1 calc R . .
C8 C 0.6674(4) 0.8438(6) 0.4747(2) 0.0344(11) Uani 1 1 d . . .
H8A H 0.6317 0.8873 0.5063 0.049(4) Uiso 1 1 calc R . .
H8B H 0.6664 0.9309 0.4470 0.049(4) 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'
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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 '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
_geom_angle_publ_flag
I4 Sn2 I4 119.46(3) . 2_656 ?
I4 Sn2 I5 120.272(13) . . ?
I4 Sn2 I5 120.272(13) 2_656 . ?
I4 Sn2 I3 90.46(3) . . ?
I4 Sn2 I3 90.49(3) 2_656 . ?
I5 Sn2 I3 89.061(12) . . ?
I4 Sn2 I3 90.49(3) . 2_656 ?
I4 Sn2 I3 90.46(3) 2_656 2_656 ?
I5 Sn2 I3 89.061(12) . 2_656 ?
I3 Sn2 I3 178.12(2) . 2_656 ?
C1 O1 C12 110.7(4) . . ?
C7 O4 C6 111.8(4) . . ?
C8 O5 C9 112.2(4) . . ?
C4 O3 C5 113.9(4) . . ?
C11 O6 C10 110.6(4) . . ?
C2 O2 C3 112.1(4) . . ?
O3 C5 C6 107.8(4) . . ?
O2 C2 C1 107.8(5) . . ?
O2 C3 C4 107.3(4) . . ?
O6 C11 C12 108.0(5) . . ?
O4 C6 C5 108.4(4) . . ?
O6 C10 C9 108.5(4) . . ?
O1 C1 C2 108.2(4) . . ?
O1 C12 C11 108.1(5) . . ?
O4 C7 C8 108.2(4) . . ?
O3 C4 C3 107.2(4) . . ?
O5 C9 C10 108.0(4) . . ?
O5 C8 C7 108.0(4) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 I1 2.8718(6) . ?
Sn2 I4 2.7295(6) . ?
Sn2 I4 2.7295(6) 2_656 ?
Sn2 I5 2.7456(9) . ?
Sn2 I3 2.8733(7) . ?
Sn2 I3 2.8733(6) 2_656 ?
O1 C1 1.419(6) . ?
O1 C12 1.436(6) . ?
O4 C7 1.423(6) . ?
O4 C6 1.437(6) . ?
O5 C8 1.426(6) . ?
O5 C9 1.426(6) . ?
O3 C4 1.424(6) . ?
O3 C5 1.439(6) . ?
O6 C11 1.422(7) . ?
O6 C10 1.427(6) . ?
O2 C2 1.424(6) . ?
O2 C3 1.439(6) . ?
C5 C6 1.476(8) . ?
C2 C1 1.491(7) . ?
C3 C4 1.476(8) . ?
C11 C12 1.483(8) . ?
C10 C9 1.478(8) . ?
C7 C8 1.490(7) . ?
