#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/69/2206947.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_2206947
loop_
_publ_author_name
'Hai-Tang Li'
'Rui Sun'
'He-Ping Shi'
'Shu-Ping Huang'
_publ_section_title
;
 2-(2-Ammoniophenylamino)ethanaminium hexachlorostannate(IV)
 monohydrate
;
_journal_coeditor_code           FL6183
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m2088
_journal_page_last               m2089
_journal_paper_doi               10.1107/S1600536805029454
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C8 H15 N3) [Sn Cl6], H2 O'
_chemical_formula_moiety         'C8 H17 Cl6 N3 O Sn'
_chemical_formula_sum            'C8 H17 Cl6 N3 O Sn'
_chemical_formula_weight         502.64
_chemical_name_systematic
;
2-(2-Ammoniophenylamino)ethanaminium hexachlorostannate(IV) monohydrate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 92.985(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2640(17)
_cell_length_b                   22.960(6)
_cell_length_c                   10.270(2)
_cell_measurement_reflns_used    3683
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.791
_cell_measurement_theta_min      2.945
_cell_volume                     1710.5(7)
_computing_cell_refinement       'SAINT (Bruker, 1998)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Bruker, 1998)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '100x100 microns'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX CCD area-detector'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'oil  sealed '
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0246
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6951
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_diffrn_standards_interval_count no
_diffrn_standards_interval_time  'no standards in IP'
_diffrn_standards_number         no
_exptl_absorpt_coefficient_mu    2.425
_exptl_absorpt_correction_T_max  0.6426
_exptl_absorpt_correction_T_min  0.5298
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.547
_refine_diff_density_min         -0.435
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         3011
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.032P)²+0.2954P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0688
_refine_ls_wR_factor_ref         0.0714
_reflns_number_gt                2653
_reflns_number_total             3011
_reflns_threshold_expression     I>2\sa(I)
_cod_data_source_file            fl6183.cif
_cod_data_source_block           I
_cod_original_cell_volume        1710.6(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2206947
_cod_database_fobs_code          2206947
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_type_symbol
Sn1 0.14151(3) 0.163024(12) 0.49889(2) 0.03063(10) Uani d . 1 Sn
Cl1 -0.08768(15) 0.13723(6) 0.65369(11) 0.0503(3) Uani d . 1 Cl
Cl2 0.38639(14) 0.14116(5) 0.66354(10) 0.0433(3) Uani d . 1 Cl
Cl3 0.14721(16) 0.06123(5) 0.43106(11) 0.0495(3) Uani d . 1 Cl
Cl4 0.37904(14) 0.18596(6) 0.34964(10) 0.0465(3) Uani d . 1 Cl
Cl5 -0.09794(14) 0.18384(5) 0.33500(10) 0.0471(3) Uani d . 1 Cl
Cl6 0.13422(17) 0.26272(5) 0.57130(11) 0.0526(3) Uani d . 1 Cl
O1 0.8820(6) 0.5558(2) 0.0714(4) 0.0867(13) Uani d D 1 O
N1 0.6904(5) 0.49120(16) 0.2427(3) 0.0517(10) Uani d . 1 N
H1A 0.5698 0.4922 0.2227 0.078 Uiso calc R 1 H
H1B 0.7320 0.4551 0.2322 0.078 Uiso calc R 1 H
H1C 0.7481 0.5153 0.1906 0.078 Uiso calc R 1 H
N2 0.6800(5) 0.40960(16) 0.4421(3) 0.0411(9) Uani d D 1 N
N3 0.6453(5) 0.25960(15) 0.5761(3) 0.0473(9) Uani d . 1 N
H3A 0.7613 0.2546 0.6062 0.071 Uiso calc R 1 H
H3B 0.6039 0.2269 0.5386 0.071 Uiso calc R 1 H
H3C 0.5755 0.2687 0.6418 0.071 Uiso calc R 1 H
C1 0.7692(6) 0.5666(2) 0.4064(5) 0.0489(12) Uani d . 1 C
H1 0.7714 0.5938 0.3395 0.059 Uiso calc R 1 H
C2 0.7257(5) 0.50921(18) 0.3791(4) 0.0352(9) Uani d . 1 C
C3 0.7217(5) 0.46645(17) 0.4746(4) 0.0331(9) Uani d . 1 C
C4 0.7645(5) 0.48447(19) 0.6024(4) 0.0398(10) Uani d . 1 C
H4 0.7636 0.4574 0.6696 0.048 Uiso calc R 1 H
C5 0.8079(6) 0.5415(2) 0.6308(5) 0.0476(12) Uani d . 1 C
H5 0.8368 0.5522 0.7168 0.057 Uiso calc R 1 H
C6 0.8093(6) 0.5831(2) 0.5337(5) 0.0532(12) Uani d . 1 C
H6 0.8370 0.6217 0.5540 0.064 Uiso calc R 1 H
C7 0.6870(6) 0.36435(19) 0.5402(4) 0.0435(11) Uani d . 1 C
H7A 0.6017 0.3734 0.6069 0.052 Uiso calc R 1 H
H7B 0.8101 0.3622 0.5812 0.052 Uiso calc R 1 H
C8 0.6373(7) 0.3075(2) 0.4786(4) 0.0491(12) Uani d . 1 C
H8A 0.7216 0.2991 0.4108 0.059 Uiso calc R 1 H
H8B 0.5138 0.3099 0.4382 0.059 Uiso calc R 1 H
H2 0.596(5) 0.402(3) 0.382(4) 0.09(2) Uiso d D 1 H
H10 0.962(5) 0.5201(12) 0.101(4) 0.048(13) Uiso d D 1 H
H9 0.967(11) 0.591(3) 0.096(8) 0.24(5) Uiso d D 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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
_geom_angle_publ_flag
Cl5 Sn1 Cl6 90.03(4) y
Cl5 Sn1 Cl4 91.54(4) y
Cl6 Sn1 Cl4 90.95(4) y
Cl5 Sn1 Cl1 90.64(4) y
Cl6 Sn1 Cl1 90.15(4) y
Cl4 Sn1 Cl1 177.55(4) y
Cl5 Sn1 Cl3 90.74(4) y
Cl6 Sn1 Cl3 178.55(4) y
Cl4 Sn1 Cl3 90.25(4) y
Cl1 Sn1 Cl3 88.61(4) y
Cl5 Sn1 Cl2 179.34(4) y
Cl6 Sn1 Cl2 90.49(4) y
Cl4 Sn1 Cl2 88.04(4) y
Cl1 Sn1 Cl2 89.77(4) y
Cl3 Sn1 Cl2 88.75(4) y
H10 O1 H9 103(6) ?
C2 N1 H1A 109.5 ?
C2 N1 H1B 109.5 ?
H1A N1 H1B 109.5 ?
C2 N1 H1C 109.5 ?
H1A N1 H1C 109.5 ?
H1B N1 H1C 109.5 ?
C3 N2 C7 120.8(3) y
C3 N2 H2 120(4) ?
C7 N2 H2 111(4) ?
C8 N3 H3A 109.5 ?
C8 N3 H3B 109.5 ?
H3A N3 H3B 109.5 ?
C8 N3 H3C 109.5 ?
H3A N3 H3C 109.5 ?
H3B N3 H3C 109.5 ?
C6 C1 C2 119.4(4) ?
C6 C1 H1 120.3 ?
C2 C1 H1 120.3 ?
C1 C2 C3 122.9(4) ?
C1 C2 N1 119.3(4) ?
C3 C2 N1 117.7(4) ?
N2 C3 C2 120.7(4) ?
N2 C3 C4 123.0(4) ?
C2 C3 C4 116.3(4) ?
C5 C4 C3 121.3(4) ?
C5 C4 H4 119.3 ?
C3 C4 H4 119.3 ?
C4 C5 C6 121.0(4) ?
C4 C5 H5 119.5 ?
C6 C5 H5 119.5 ?
C1 C6 C5 119.1(5) ?
C1 C6 H6 120.5 ?
C5 C6 H6 120.5 ?
N2 C7 C8 109.6(3) ?
N2 C7 H7A 109.8 ?
C8 C7 H7A 109.8 ?
N2 C7 H7B 109.8 ?
C8 C7 H7B 109.8 ?
H7A C7 H7B 108.2 ?
C7 C8 N3 111.3(3) ?
C7 C8 H8A 109.4 ?
N3 C8 H8A 109.4 ?
C7 C8 H8B 109.4 ?
N3 C8 H8B 109.4 ?
H8A C8 H8B 108.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 Cl5 2.4046(11) y
Sn1 Cl6 2.4082(13) y
Sn1 Cl4 2.4247(11) y
Sn1 Cl1 2.4343(11) y
Sn1 Cl3 2.4398(13) y
Sn1 Cl2 2.4418(11) y
O1 H10 1.041(10) y
O1 H9 1.046(10) y
N1 C2 1.470(5) ?
N1 H1A 0.8900 ?
N1 H1B 0.8900 ?
N1 H1C 0.8900 ?
N2 C3 1.377(5) ?
N2 C7 1.446(5) ?
N2 H2 0.862(10) y
N3 C8 1.487(5) ?
N3 H3A 0.8900 ?
N3 H3B 0.8900 ?
N3 H3C 0.8900 ?
C1 C6 1.378(6) ?
C1 C2 1.380(6) ?
C1 H1 0.9300 ?
C2 C3 1.389(5) ?
C3 C4 1.395(5) ?
C4 C5 1.375(6) ?
C4 H4 0.9300 ?
C5 C6 1.381(6) ?
C5 H5 0.9300 ?
C6 H6 0.9300 ?
C7 C8 1.486(6) ?
C7 H7A 0.9700 ?
C7 H7B 0.9700 ?
C8 H8A 0.9700 ?
C8 H8B 0.9700 ?
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_publ_flag
C6 C1 C2 C3 -0.6(6) ?
C6 C1 C2 N1 -177.5(4) ?
C7 N2 C3 C2 176.1(4) y
C7 N2 C3 C4 -3.0(6) y
C1 C2 C3 N2 -179.1(4) y
N1 C2 C3 N2 -2.1(6) y
C1 C2 C3 C4 0.0(6) ?
N1 C2 C3 C4 177.0(3) ?
N2 C3 C4 C5 179.1(4) y
C2 C3 C4 C5 0.0(6) ?
C3 C4 C5 C6 0.5(6) ?
C2 C1 C6 C5 1.0(7) ?
C4 C5 C6 C1 -1.0(7) ?
C3 N2 C7 C8 -179.6(4) ?
N2 C7 C8 N3 179.3(4) y
