#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/56/2205650.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_2205650
loop_
_publ_author_name
'Puls, Angela'
'Näther, Christian'
'Bensch, Wolfgang'
_publ_section_title
;
 Bis(2-aminoethylammonium) (ethylenediammonium)
 (di-μ-sulfido-κ²S:S)bis[dithiostannate(IV)]
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m868
_journal_page_last               m870
_journal_paper_doi               10.1107/S1600536805010871
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          '(C2 H10 N2) (C2 H9 N2)2 [Sn2 S6]'
_chemical_formula_moiety         'C2 H10 N2 2+ , 2C2 H9 N2 + , S6 Sn2 4-'
_chemical_formula_sum            'C6 H28 N6 S6 Sn2'
_chemical_formula_weight         614.08
_chemical_name_systematic
;
Bis(2-aminoethylammonium)(ethylenediammonium)(di-μ-sulfido-
κ²S:S)bis[disulfidotin(IV)]
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                74.845(10)
_cell_angle_beta                 72.997(10)
_cell_angle_gamma                88.978(10)
_cell_formula_units_Z            2
_cell_length_a                   8.7638(7)
_cell_length_b                   10.7287(10)
_cell_length_c                   12.2216(10)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    170(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.5
_cell_volume                     1058.54(18)
_computing_cell_refinement       IPDS
_computing_data_collection       'IPDS (Stoe & Cie, 1998)'
_computing_data_reduction        IPDS
_computing_molecular_graphics    'XP in SHELXTL (Bruker, 1998)'
_computing_publication_material  'CIFTAB in SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      170(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Stoe IPDS-1'
_diffrn_measurement_method       φ
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11088
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.950
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.927
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             604
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.912
_refine_diff_density_min         -1.800
_refine_ls_extinction_coef       0.0039(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     186
_refine_ls_number_reflns         4820
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0291
_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)+(0.0472P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                3926
_reflns_number_total             4820
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt6643.cif
_cod_data_source_block           I
_cod_original_cell_volume        1058.54(16)
_cod_database_code               2205650
_cod_database_fobs_code          2205650
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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 0.34747(2) 0.63752(2) 0.154153(17) 0.00856(8) Uani d . 1 Sn
Sn2 0.13770(2) 0.36405(2) 0.334696(17) 0.00832(8) Uani d . 1 Sn
S1 0.58686(9) 0.70422(8) 0.17769(7) 0.01206(16) Uani d . 1 S
S2 0.25563(9) 0.77505(8) 0.00775(7) 0.01272(16) Uani d . 1 S
S3 0.34584(9) 0.41326(8) 0.14064(6) 0.01217(16) Uani d . 1 S
S4 0.12997(9) 0.58798(8) 0.34600(7) 0.01226(16) Uani d . 1 S
S5 0.24852(9) 0.22744(8) 0.47117(7) 0.01222(16) Uani d . 1 S
S6 -0.10768(9) 0.28440(8) 0.32975(7) 0.01187(16) Uani d . 1 S
N1 0.4617(3) 0.1191(3) 0.2382(3) 0.0172(6) Uani d . 1 N
H1N1 0.3919 0.0876 0.2080 0.026 Uiso calc R 1 H
H2N1 0.5356 0.1758 0.1785 0.026 Uiso calc R 1 H
H3N1 0.4075 0.1603 0.2928 0.026 Uiso calc R 1 H
C1 0.5430(4) 0.0112(4) 0.2955(3) 0.0185(7) Uani d . 1 C
H1A 0.6289 0.0465 0.3186 0.022 Uiso calc R 1 H
H1B 0.5931 -0.0387 0.2380 0.022 Uiso calc R 1 H
C2 0.4283(4) -0.0776(4) 0.4039(3) 0.0183(7) Uani d . 1 C
H2A 0.4870 -0.1481 0.4405 0.022 Uiso calc R 1 H
H2B 0.3813 -0.0287 0.4628 0.022 Uiso calc R 1 H
N2 0.3002(3) -0.1333(3) 0.3732(3) 0.0196(6) Uani d . 1 N
H1N2 0.2409 -0.1942 0.4383 0.029 Uiso d R 1 H
H2N2 0.3452 -0.1736 0.3156 0.029 Uiso d R 1 H
N3 0.0231(4) -0.0186(3) 0.3250(3) 0.0209(7) Uani d . 1 N
H1N3 0.1225 -0.0389 0.3300 0.031 Uiso calc R 1 H
H2N3 -0.0515 -0.0737 0.3856 0.031 Uiso calc R 1 H
H3N3 0.0069 0.0641 0.3298 0.031 Uiso calc R 1 H
C3 0.0089(4) -0.0303(4) 0.2093(4) 0.0257(9) Uani d . 1 C
H3A -0.1039 -0.0229 0.2096 0.031 Uiso calc R 1 H
H3B 0.0411 -0.1165 0.1993 0.031 Uiso calc R 1 H
C4 0.1134(5) 0.0740(5) 0.1061(3) 0.0277(9) Uani d . 1 C
H4A 0.0949 0.0683 0.0314 0.033 Uiso calc R 1 H
H4B 0.0837 0.1602 0.1174 0.033 Uiso calc R 1 H
N4 0.2832(4) 0.0595(3) 0.0970(3) 0.0220(7) Uani d . 1 N
H1N4 0.3453 0.1211 0.0340 0.033 Uiso d R 1 H
H2N4 0.3099 -0.0195 0.0857 0.033 Uiso d R 1 H
N5 0.7907(3) 0.4613(3) 1.1043(2) 0.0136(6) Uani d . 1 N
H1N5 0.7591 0.4119 1.0636 0.020 Uiso calc R 1 H
H2N5 0.7114 0.5131 1.1279 0.020 Uiso calc R 1 H
H3N5 0.8118 0.4089 1.1693 0.020 Uiso calc R 1 H
C5 0.9384(4) 0.5432(3) 1.0258(3) 0.0148(7) Uani d . 1 C
H5A 0.9813 0.5888 1.0723 0.018 Uiso calc R 1 H
H5B 0.9128 0.6088 0.9610 0.018 Uiso calc R 1 H
N6 0.2903(3) 0.4523(3) 0.6009(2) 0.0140(6) Uani d . 1 N
H1N6 0.2649 0.3974 0.5626 0.021 Uiso calc R 1 H
H2N6 0.2055 0.5000 0.6230 0.021 Uiso calc R 1 H
H3N6 0.3151 0.4059 0.6666 0.021 Uiso calc R 1 H
C6 0.4303(4) 0.5403(3) 0.5202(3) 0.0146(7) Uani d . 1 C
H6A 0.4607 0.5986 0.5622 0.018 Uiso calc R 1 H
H6B 0.4024 0.5941 0.4504 0.018 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'
N N 0.0061 0.0033 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
S2 Sn1 S1 . . 117.06(3) y
S2 Sn1 S3 . . 111.51(3) y
S1 Sn1 S3 . . 112.48(3) y
S2 Sn1 S4 . . 109.00(3) y
S1 Sn1 S4 . . 110.79(3) y
S3 Sn1 S4 . . 93.46(3) y
S5 Sn2 S6 . . 114.80(3) y
S5 Sn2 S4 . . 113.84(3) y
S6 Sn2 S4 . . 112.12(3) y
S5 Sn2 S3 . . 106.50(3) y
S6 Sn2 S3 . . 113.35(3) y
S4 Sn2 S3 . . 94.34(3) y
Sn1 S3 Sn2 . . 86.14(3) y
Sn2 S4 Sn1 . . 85.98(3) y
C1 N1 H1N1 . . 109.5 n
C1 N1 H2N1 . . 109.5 n
H1N1 N1 H2N1 . . 109.5 n
C1 N1 H3N1 . . 109.5 n
H1N1 N1 H3N1 . . 109.5 n
H2N1 N1 H3N1 . . 109.5 n
N1 C1 C2 . . 111.6(3) n
N1 C1 H1A . . 109.3 n
C2 C1 H1A . . 109.3 n
N1 C1 H1B . . 109.3 n
C2 C1 H1B . . 109.3 n
H1A C1 H1B . . 108.0 n
N2 C2 C1 . . 111.0(3) n
N2 C2 H2A . . 109.4 n
C1 C2 H2A . . 109.4 n
N2 C2 H2B . . 109.4 n
C1 C2 H2B . . 109.4 n
H2A C2 H2B . . 108.0 n
C2 N2 H1N2 . . 108.8 n
C2 N2 H2N2 . . 108.6 n
H1N2 N2 H2N2 . . 107.9 n
C3 N3 H1N3 . . 109.5 n
C3 N3 H2N3 . . 109.5 n
H1N3 N3 H2N3 . . 109.5 n
C3 N3 H3N3 . . 109.5 n
H1N3 N3 H3N3 . . 109.5 n
H2N3 N3 H3N3 . . 109.5 n
N3 C3 C4 . . 111.2(3) n
N3 C3 H3A . . 109.4 n
C4 C3 H3A . . 109.4 n
N3 C3 H3B . . 109.4 n
C4 C3 H3B . . 109.4 n
H3A C3 H3B . . 108.0 n
N4 C4 C3 . . 110.9(3) n
N4 C4 H4A . . 109.5 n
C3 C4 H4A . . 109.5 n
N4 C4 H4B . . 109.5 n
C3 C4 H4B . . 109.5 n
H4A C4 H4B . . 108.0 n
C4 N4 H1N4 . . 110.5 n
C4 N4 H2N4 . . 108.9 n
H1N4 N4 H2N4 . . 108.3 n
C5 N5 H1N5 . . 109.5 n
C5 N5 H2N5 . . 109.5 n
H1N5 N5 H2N5 . . 109.5 n
C5 N5 H3N5 . . 109.5 n
H1N5 N5 H3N5 . . 109.5 n
H2N5 N5 H3N5 . . 109.5 n
N5 C5 C5 . 2_767 108.8(3) n
N5 C5 H5A . . 109.9 n
C5 C5 H5A 2_767 . 109.9 n
N5 C5 H5B . . 109.9 n
C5 C5 H5B 2_767 . 109.9 n
H5A C5 H5B . . 108.3 n
C6 N6 H1N6 . . 109.5 n
C6 N6 H2N6 . . 109.5 n
H1N6 N6 H2N6 . . 109.5 n
C6 N6 H3N6 . . 109.5 n
H1N6 N6 H3N6 . . 109.5 n
H2N6 N6 H3N6 . . 109.5 n
N6 C6 C6 . 2_666 109.1(4) n
N6 C6 H6A . . 109.9 n
C6 C6 H6A 2_666 . 109.9 n
N6 C6 H6B . . 109.9 n
C6 C6 H6B 2_666 . 109.9 n
H6A C6 H6B . . 108.3 n
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 S2 . 2.3337(9) y
Sn1 S1 . 2.3474(8) y
Sn1 S3 . 2.4549(9) y
Sn1 S4 . 2.4868(8) y
Sn2 S5 . 2.3434(9) y
Sn2 S6 . 2.3509(8) y
Sn2 S4 . 2.4409(9) y
Sn2 S3 . 2.4659(8) y
N1 C1 . 1.475(5) n
N1 H1N1 . 0.9100 n
N1 H2N1 . 0.9100 n
N1 H3N1 . 0.9100 n
C1 C2 . 1.507(5) n
C1 H1A . 0.9900 n
C1 H1B . 0.9900 n
C2 N2 . 1.465(4) n
C2 H2A . 0.9900 n
C2 H2B . 0.9900 n
N2 H1N2 . 0.9100 n
N2 H2N2 . 0.9100 n
N3 C3 . 1.491(5) n
N3 H1N3 . 0.9100 n
N3 H2N3 . 0.9100 n
N3 H3N3 . 0.9100 n
C3 C4 . 1.517(6) n
C3 H3A . 0.9900 n
C3 H3B . 0.9900 n
C4 N4 . 1.468(5) n
C4 H4A . 0.9900 n
C4 H4B . 0.9900 n
N4 H1N4 . 0.9100 n
N4 H2N4 . 0.9100 n
N5 C5 . 1.497(4) n
N5 H1N5 . 0.9100 n
N5 H2N5 . 0.9100 n
N5 H3N5 . 0.9100 n
C5 C5 2_767 1.514(7) n
C5 H5A . 0.9900 n
C5 H5B . 0.9900 n
N6 C6 . 1.489(4) n
N6 H1N6 . 0.9100 n
N6 H2N6 . 0.9100 n
N6 H3N6 . 0.9100 n
C6 C6 2_666 1.521(6) n
C6 H6A . 0.9900 n
C6 H6B . 0.9900 n
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
N1 H1N1 N4 . 0.91 1.95 2.833(4) 162
N1 H2N1 S2 2_665 0.91 2.40 3.228(3) 151
N1 H3N1 S5 . 0.91 2.49 3.390(3) 168
N2 H1N2 S6 2_556 0.91 2.65 3.477(3) 152
N2 H2N2 S1 1_545 0.91 2.83 3.683(3) 157
N3 H1N3 N2 . 0.91 1.97 2.849(5) 162
N3 H2N3 S5 2_556 0.91 2.36 3.271(3) 174
N3 H3N3 S6 . 0.91 2.55 3.436(4) 164
N4 H1N4 S1 2_665 0.91 2.68 3.523(3) 155
N4 H2N4 S2 1_545 0.91 2.72 3.533(3) 150
N5 H1N5 S2 2_666 0.91 2.41 3.263(3) 157
N5 H2N5 S1 1_556 0.91 2.44 3.303(3) 159
N5 H3N5 S6 1_656 0.91 2.35 3.260(3) 174
N6 H1N6 S5 . 0.91 2.40 3.293(3) 167
N6 H2N6 S6 2_566 0.91 2.60 3.399(3) 147
N6 H3N6 S1 2_666 0.91 2.35 3.250(3) 173
