#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/11/2201188.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2201188
loop_
_publ_author_name
'Howie, R. Alan'
'Wardell, Solange M. S. V.'
_publ_section_title
;
 (2-Carbomethoxyethyl)triiodotin at 120K
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m220
_journal_page_last               m222
_journal_paper_doi               10.1107/S1600536802007080
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '[Sn I3 (C4 H7 O2)]'
_chemical_formula_moiety         'C4 H7 I3 O2 Sn'
_chemical_formula_sum            'C4 H7 I3 O2 Sn'
_chemical_formula_weight         586.49
_chemical_name_systematic
;
 (2-Carbomethoxyethyl)triiodotin at 120K
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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
_cell_angle_beta                 90.4600(8)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   7.39500(10)
_cell_length_b                   25.8407(4)
_cell_length_c                   12.4431(2)
_cell_measurement_reflns_used    14043
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.9
_cell_volume                     2377.70(6)
_computing_cell_refinement       'DENZO and COLLECT'
_computing_data_collection
'DENZO (Otwinowski & Minor, 1997) and COLLECT (Hooft, 1998)'
_computing_data_reduction        'DENZO and COLLECT'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 1990)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.936
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'Enraf-Nonius KappaCCD area-detector'
_diffrn_measurement_method       'φ and ω scans to fill the Ewald sphere'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enraf-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.107
_diffrn_reflns_av_sigmaI/netI    0.066
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20814
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         3.2
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.90
_exptl_absorpt_correction_T_max  0.505
_exptl_absorpt_correction_T_min  0.269
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1995, 1997)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.277
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2048
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.156
_refine_diff_density_min         -2.707
_refine_ls_extinction_coef       0.00204(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.14
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     184
_refine_ls_number_reflns         5138
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.14
_refine_ls_R_factor_all          0.065
_refine_ls_R_factor_gt           0.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0892P)²+21.9385P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.164
_refine_ls_wR_factor_ref         0.168
_reflns_number_gt                4645
_reflns_number_total             5138
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            tk6061.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2201188
_cod_database_fobs_code          2201188
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Sn1A 0.33608(9) 0.63670(2) 0.91984(5) 0.0201(2) Uani d . 1 . . Sn
I1A 0.13667(11) 0.70147(3) 1.04953(6) 0.0354(2) Uani d . 1 . . I
I2A 0.21626(10) 0.54496(2) 0.99356(7) 0.0321(2) Uani d . 1 . . I
I3A 0.19303(10) 0.66415(3) 0.72933(6) 0.0300(2) Uani d . 1 . . I
C1A 0.6052(14) 0.6572(4) 0.9700(9) 0.027(2) Uani d . 1 . . C
H1A1 0.6236 0.6946 0.9572 0.032 Uiso calc R 1 . . H
H1A2 0.6174 0.6510 1.0482 0.032 Uiso calc R 1 . . H
C2A 0.7492(16) 0.6277(6) 0.9133(11) 0.041(3) Uani d . 1 . . C
H2A1 0.8272 0.6528 0.8754 0.049 Uiso calc R 1 . . H
H2A2 0.8253 0.6102 0.9681 0.049 Uiso calc R 1 . . H
C3A 0.6881(14) 0.5881(4) 0.8339(9) 0.026(2) Uani d . 1 . . C
O1A 0.5295(10) 0.5820(3) 0.8070(7) 0.0305(17) Uani d . 1 . . O
O2A 0.8200(12) 0.5605(3) 0.7940(7) 0.038(2) Uani d . 1 . . O
C4A 0.7682(19) 0.5219(5) 0.7141(11) 0.042(3) Uani d . 1 . . C
H4A1 0.6549 0.5053 0.7356 0.064 Uiso calc R 1 . . H
H4A2 0.8635 0.4957 0.7089 0.064 Uiso calc R 1 . . H
H4A3 0.7514 0.5387 0.6441 0.064 Uiso calc R 1 . . H
Sn1B 0.14771(10) 0.34482(2) 0.63933(6) 0.0235(2) Uani d . 1 . . Sn
I1B 0.33283(13) 0.26872(3) 0.74346(7) 0.0382(2) Uani d . 1 . . I
I2B 0.23598(11) 0.42592(2) 0.76633(6) 0.0288(2) Uani d . 1 . . I
I3B 0.32701(12) 0.34466(3) 0.45298(6) 0.0374(2) Uani d . 1 . . I
C1B -0.1341(17) 0.3264(4) 0.6440(10) 0.033(3) Uani d . 1 . . C
H1B1 -0.1676 0.3065 0.5788 0.040 Uiso calc R 1 . . H
H1B2 -0.1581 0.3043 0.7074 0.040 Uiso calc R 1 . . H
C2B -0.2493(15) 0.3747(4) 0.6500(11) 0.034(3) Uani d . 1 . . C
H2B1 -0.3781 0.3654 0.6391 0.040 Uiso calc R 1 . . H
H2B2 -0.2362 0.3906 0.7220 0.040 Uiso calc R 1 . . H
C3B -0.1932(16) 0.4125(4) 0.5660(9) 0.029(2) Uani d . 1 . . C
O1B -0.0368(10) 0.4159(3) 0.5339(6) 0.0268(16) Uani d . 1 . . O
O2B -0.3236(11) 0.4425(3) 0.5296(7) 0.0351(19) Uani d . 1 . . O
C4B -0.2761(17) 0.4781(5) 0.4425(11) 0.035(3) Uani d . 1 . . C
H4B1 -0.1802 0.5015 0.4671 0.053 Uiso calc R 1 . . H
H4B2 -0.3829 0.4983 0.4215 0.053 Uiso calc R 1 . . H
H4B3 -0.2335 0.4582 0.3806 0.053 Uiso calc R 1 . . H
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'
I I -0.4742 1.8119 '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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1A Sn1A O1A 76.5(3)
C1A Sn1A I3A 123.3(3)
O1A Sn1A I3A 82.80(19)
C1A Sn1A I2A 115.1(3)
O1A Sn1A I2A 83.3(2)
I3A Sn1A I2A 113.89(3)
C1A Sn1A I1A 100.3(3)
O1A Sn1A I1A 176.67(19)
I3A Sn1A I1A 98.48(3)
I2A Sn1A I1A 98.96(3)
C2A C1A Sn1A 113.6(7)
C2A C1A H1A1 108.8
Sn1A C1A H1A1 108.8
C2A C1A H1A2 108.8
Sn1A C1A H1A2 108.8
H1A1 C1A H1A2 107.7
C3A C2A C1A 116.8(10)
C3A C2A H2A1 108.1
C1A C2A H2A1 108.1
C3A C2A H2A2 108.1
C1A C2A H2A2 108.1
H2A1 C2A H2A2 107.3
O1A C3A O2A 122.8(10)
O1A C3A C2A 123.5(10)
O2A C3A C2A 113.7(9)
C3A O1A Sn1A 109.3(7)
C3A O2A C4A 116.0(10)
O2A C4A H4A1 109.5
O2A C4A H4A2 109.5
H4A1 C4A H4A2 109.5
O2A C4A H4A3 109.5
H4A1 C4A H4A3 109.5
H4A2 C4A H4A3 109.5
C1B Sn1B O1B 70.6(3)
C1B Sn1B I3B 120.8(3)
O1B Sn1B I3B 80.09(17)
C1B Sn1B I2B 112.8(3)
O1B Sn1B I2B 82.66(17)
I3B Sn1B I2B 112.85(4)
C1B Sn1B I1B 108.2(3)
O1B Sn1B I1B 177.89(17)
I3B Sn1B I1B 99.24(4)
I2B Sn1B I1B 99.43(3)
C2B C1B Sn1B 111.5(7)
C2B C1B H1B1 109.3
Sn1B C1B H1B1 109.3
C2B C1B H1B2 109.3
Sn1B C1B H1B2 109.3
H1B1 C1B H1B2 108.0
C3B C2B C1B 110.2(10)
C3B C2B H2B1 109.6
C1B C2B H2B1 109.6
C3B C2B H2B2 109.6
C1B C2B H2B2 109.6
H2B1 C2B H2B2 108.1
O1B C3B O2B 122.3(10)
O1B C3B C2B 122.8(10)
O2B C3B C2B 114.9(10)
C3B O1B Sn1B 105.9(6)
C3B O2B C4B 116.4(9)
O2B C4B H4B1 109.5
O2B C4B H4B2 109.5
H4B1 C4B H4B2 109.5
O2B C4B H4B3 109.5
H4B1 C4B H4B3 109.5
H4B2 C4B H4B3 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1A C1A . 2.147(10) ?
Sn1A O1A . 2.459(8) ?
Sn1A I3A . 2.6835(9) ?
Sn1A I2A . 2.6944(9) ?
Sn1A I1A . 2.7601(10) ?
C1A C2A . 1.492(16) ?
C1A H1A1 . 0.9900 ?
C1A H1A2 . 0.9900 ?
C2A C3A . 1.491(16) ?
C2A H2A1 . 0.9900 ?
C2A H2A2 . 0.9900 ?
C3A O1A . 1.227(13) ?
C3A O2A . 1.308(14) ?
O2A C4A . 1.458(16) ?
C4A H4A1 . 0.9800 ?
C4A H4A2 . 0.9800 ?
C4A H4A3 . 0.9800 ?
Sn1B C1B . 2.139(12) ?
Sn1B O1B . 2.631(8) ?
Sn1B I3B . 2.6803(11) ?
Sn1B I2B . 2.7016(9) ?
Sn1B I1B . 2.7188(9) ?
C1B C2B . 1.513(16) ?
C1B H1B1 . 0.9900 ?
C1B H1B2 . 0.9900 ?
C2B C3B . 1.493(16) ?
C2B H2B1 . 0.9900 ?
C2B H2B2 . 0.9900 ?
C3B O1B . 1.229(14) ?
C3B O2B . 1.316(13) ?
O2B C4B . 1.465(14) ?
C4B H4B1 . 0.9800 ?
C4B H4B2 . 0.9800 ?
C4B H4B3 . 0.9800 ?
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
O1A Sn1A C1A C2A -1.1(9)
I3A Sn1A C1A C2A -72.9(10)
I2A Sn1A C1A C2A 74.6(10)
I1A Sn1A C1A C2A 179.7(9)
Sn1A C1A C2A C3A -1.6(16)
C1A C2A C3A O1A 6(2)
C1A C2A C3A O2A -174.3(11)
O2A C3A O1A Sn1A 173.9(9)
C2A C3A O1A Sn1A -7.0(14)
C1A Sn1A O1A C3A 4.3(8)
I3A Sn1A O1A C3A 131.2(7)
I2A Sn1A O1A C3A -113.6(7)
O1A C3A O2A C4A 0.5(16)
C2A C3A O2A C4A -178.7(11)
O1B Sn1B C1B C2B -35.0(8)
I3B Sn1B C1B C2B -100.0(8)
I2B Sn1B C1B C2B 37.9(9)
I1B Sn1B C1B C2B 146.9(8)
Sn1B C1B C2B C3B 49.3(11)
C1B C2B C3B O1B -30.9(16)
C1B C2B C3B O2B 149.8(10)
O2B C3B O1B Sn1B -179.8(9)
C2B C3B O1B Sn1B 1.0(13)
C1B Sn1B O1B C3B 19.9(8)
I3B Sn1B O1B C3B 147.7(7)
I2B Sn1B O1B C3B -97.4(7)
I1B Sn1B O1B C3B 76(5)
O1B C3B O2B C4B 4.3(17)
C2B C3B O2B C4B -176.5(10)
