#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/61/2236193.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_2236193
loop_
_publ_author_name
'Ye, Fei'
'Reuter, Hans'
_publ_section_title
;
 Diaquatetrabromidotin(IV) trihydrate
;
_journal_coeditor_code           FJ2592
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              i70
_journal_paper_doi               10.1107/S1600536812036434
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Sn Br4 (H2 O)2], 3H2 O'
_chemical_formula_moiety         'Br4 H4 O2 Sn, 3(H2 O)'
_chemical_formula_sum            'Br4 H10 O5 Sn'
_chemical_formula_weight         528.41
_chemical_name_systematic
;
Diaquatetrabromidotin(IV) trihydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 104.4620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6484(5)
_cell_length_b                   10.1647(4)
_cell_length_c                   8.8683(4)
_cell_measurement_reflns_used    8700
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      2.60
_cell_volume                     1104.04(8)
_computing_cell_refinement       'SAINT (Bruker, 2009)'
_computing_data_collection       'APEX2 (Bruker, 2009)'
_computing_data_reduction        'SAINT (Bruker, 2009)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006) and Mercury (Macrae et al.,
2008)
;
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'φ and ω scans'
_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  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0168
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16999
_diffrn_reflns_theta_full        29.99
_diffrn_reflns_theta_max         29.99
_diffrn_reflns_theta_min         3.23
_exptl_absorpt_coefficient_mu    16.767
_exptl_absorpt_correction_T_max  0.2342
_exptl_absorpt_correction_T_min  0.1484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2009)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.179
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.409
_refine_ls_extinction_coef       0.00035(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     51
_refine_ls_number_reflns         1618
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.096
_refine_ls_R_factor_all          0.0151
_refine_ls_R_factor_gt           0.0133
_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)+(0.0089P)²+1.3814P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0276
_refine_ls_wR_factor_ref         0.0279
_reflns_number_gt                1523
_reflns_number_total             1618
_reflns_threshold_expression     I>2sigma(I)
_iucr_refine_instructions_details
;
TITL HR282_0ma in C2/c
CELL 0.71073  12.6484  10.1647   8.8683  90.000 104.462  90.000
ZERR    4.00   0.0005   0.0004   0.0004   0.000   0.001   0.000
LATT 7
SYMM -X, Y, 0.5-Z
SFAC O  H  Br Sn
UNIT 20  40  16  4
OMIT -3 60
L.S. 10
EXTI 0.000377
ACTA
BOND $H
FMAP 2
PLAN 5
Size 0.122 0.154 0.184
EQIV $4  -x+1, -y, -z+1
EQIV $3  -x+1/2, -y+1/2, -z+1
EQIV $2  x-1, y, z
EQIV $1  x, -y+1, z-1/2
HTAB O3 Br2_$4
HTAB O2 Br2_$3
HTAB O2 Br1_$3
HTAB O2 O3_$2
HTAB O1 O2_$1
HTAB O1 O2
HTAB
WGHT   0.008900   1.381400
FVAR 0.057500 0.058640 0.039620 0.057140
TEMP -173
MOLE 1
Sn1    4   0.000000   0.259476   0.250000  10.500000   0.008290 =
           0.008240   0.007030   0.000000   0.002380   0.000000
Br1    3   0.143864   0.280599   0.095769  11.000000   0.011080 =
           0.014130   0.009880   0.001300   0.005070   0.001550
Br2    3   0.117876   0.098464   0.438945  11.000000   0.013230 =
           0.012390   0.012040   0.003560   0.002370   0.002080
O1     1   0.078374   0.422527   0.384910  11.000000   0.015230 =
           0.012030   0.008600  -0.001480   0.001920  -0.004450
AFIX 3
H11    2   0.102470   0.427411   0.496349  11.000000  21.000000
H12    2   0.106331   0.500737   0.348055  11.000000  21.000000
AFIX 0
O2     1   0.135327   0.390303   0.700573  11.000000   0.012760 =
           0.014010   0.012520   0.000610   0.002600   0.003190
AFIX 3
H21    2   0.095423   0.312090   0.711748  11.000000  31.000000
H22    2   0.210344   0.363172   0.723092  11.000000  31.000000
AFIX 0
O3     1   1.000000   0.190513   0.750000  10.500000   0.024890 =
           0.014470   0.009480   0.000000   0.002150   0.000000
AFIX 3
H3     2   0.975639   0.131009   0.664258  11.000000  41.000000
AFIX
HKLF 4
END
HKLF 4
REM  HR282_0ma in C2/c
REM R1=  0.0135 for   1523 Fo > 4sig(Fo)  and  0.0153 for all   1618 data
REM     51 parameters refined using      0 restraints
REM XShell GPWARNING : The following atoms were created either by GROW or PACK.
Q1     1   0.092700   0.463600   0.348600  11.000000   0.050000
Q2     1   0.191000   0.366100   0.740100  11.000000   0.050000
Q3     1   0.132700   0.233100  -0.006100  11.000000   0.050000
Q4     1   0.090700   0.432100   0.457100  11.000000   0.050000
Q5     1   0.083300   0.257900   0.227000  11.000000   0.050000
MOLE
HKLF 4
END
;
_cod_data_source_file            fj2592.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2236193
_cod_database_fobs_code          2236193
loop_
_symmetry_equiv_pos_as_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_type_symbol
_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_symmetry_multiplicity
Sn Sn1 0.0000 0.259481(16) 0.2500 0.00769(5) Uani d S 1 2
Br Br1 0.143871(16) 0.280603(17) 0.09578(2) 0.01115(5) Uani d . 1 1
Br Br2 0.117864(16) 0.098459(17) 0.43896(2) 0.01257(5) Uani d . 1 1
O O1 0.07836(11) 0.42263(12) 0.38481(14) 0.0123(3) Uani d . 1 1
H H11 0.1025 0.4275 0.4963 0.048(6) Uiso d R 1 1
H H12 0.1063 0.5008 0.3480 0.048(6) Uiso d R 1 1
O O2 0.13528(11) 0.39033(13) 0.70061(15) 0.0134(3) Uani d . 1 1
H H21 0.0954 0.3121 0.7118 0.038(5) Uiso d R 1 1
H H22 0.2103 0.3632 0.7231 0.038(5) Uiso d R 1 1
O O3 1.0000 0.19063(19) 0.7500 0.0170(4) Uani d S 1 2
H H3 0.9756 0.1311 0.6643 0.056(10) Uiso d R 1 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Sn1 0.00819(9) 0.00818(8) 0.00695(8) 0.000 0.00236(6) 0.000
Br1 0.01097(10) 0.01404(9) 0.00975(8) 0.00156(7) 0.00504(7) 0.00131(6)
Br2 0.01312(10) 0.01227(9) 0.01191(9) 0.00208(6) 0.00235(7) 0.00356(6)
O1 0.0151(7) 0.0124(6) 0.0087(6) -0.0042(5) 0.0017(5) -0.0013(5)
O2 0.0131(7) 0.0143(6) 0.0126(6) 0.0033(5) 0.0027(5) 0.0009(5)
O3 0.0250(12) 0.0150(9) 0.0102(9) 0.000 0.0026(8) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
Br Br -0.2901 2.4595 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Sn1 O1 2 . 78.26(7)
O1 Sn1 Br2 2 2 90.98(4)
O1 Sn1 Br2 . 2 169.06(4)
O1 Sn1 Br2 2 . 169.06(4)
O1 Sn1 Br2 . . 90.98(4)
Br2 Sn1 Br2 2 . 99.837(10)
O1 Sn1 Br1 2 . 85.86(4)
O1 Sn1 Br1 . . 86.63(4)
Br2 Sn1 Br1 2 . 94.612(7)
Br2 Sn1 Br1 . . 91.621(7)
O1 Sn1 Br1 2 2 86.63(4)
O1 Sn1 Br1 . 2 85.86(4)
Br2 Sn1 Br1 2 2 91.620(7)
Br2 Sn1 Br1 . 2 94.613(7)
Br1 Sn1 Br1 . 2 170.317(10)
Sn1 O1 H11 . . 126.8
Sn1 O1 H12 . . 127.6
H11 O1 H12 . . 105.0
H21 O2 H22 . . 105.0
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
Sn1 O1 2 2.1378(12) ?
Sn1 O1 . 2.1378(12) y
Sn1 Br2 2 2.5420(2) ?
Sn1 Br2 . 2.5420(2) y
Sn1 Br1 . 2.5439(2) y
Sn1 Br1 2 2.5439(2) ?
O1 H11 . 0.9600 ?
O1 H12 . 0.9600 ?
O2 H21 . 0.9600 ?
O2 H22 . 0.9600 ?
O3 H3 . 0.9602 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
O3 H3 Br2 5_656 0.96 2.67 3.5239(16) 148
O2 H22 Br2 7_556 0.96 2.92 3.6365(14) 133
O2 H22 Br1 7_556 0.96 2.58 3.4004(13) 144
O2 H21 O3 1_455 0.96 1.82 2.7595(19) 167
O1 H12 O2 6_565 0.96 1.82 2.7182(18) 155
O1 H11 O2 . 0.96 1.80 2.7318(18) 164
