#------------------------------------------------------------------------------
#$Date: 2016-02-20 05:06:23 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176774 $
#$URL: svn://www.crystallography.net/cod/cif/2/20/85/2208508.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_2208508
loop_
_publ_author_name
'Puls, Angela'
'Näther, Christian '
'Bensch, Wolfgang'
_publ_section_title
;
 2-Ammoniopropylammonium dodeca-μ-sulfido-tetrasulfidodecaantimony
;
_journal_coeditor_code           BT2015
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m674
_journal_page_last               m676
_journal_paper_doi               10.1107/S1600536806006738
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          '(C3 H12 N2) [Sb10 S16]'
_chemical_formula_moiety         'C3 H12 N2 2+, S16 Sb10 2-'
_chemical_formula_sum            'C3 H12 N2 S16 Sb10'
_chemical_formula_weight         1806.61
_chemical_name_systematic
;
2-Ammoniopropylammonium μ-dodecasulfido-tetrasulfidodecaantimony
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.415(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.480(3)
_cell_length_b                   10.922(2)
_cell_length_c                   18.030(3)
_cell_measurement_reflns_used    92
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      11
_cell_volume                     3204.6(10)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1992)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1992)'
_computing_molecular_graphics
'SHELXTL (Bruker, 1998) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'CIFTAB in SHELXL97'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean n
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe AED-II four-circle'
_diffrn_measurement_method       ω--θ
_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  0.0253
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            11455
_diffrn_reflns_theta_full        27.02
_diffrn_reflns_theta_max         27.02
_diffrn_reflns_theta_min         2.43
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count n
_diffrn_standards_interval_time  120
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    9.336
_exptl_absorpt_correction_T_max  0.401
_exptl_absorpt_correction_T_min  0.345
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE; Stoe & Cie, 1998)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.745
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3240
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.921
_refine_diff_density_min         -0.802
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         6992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0241
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0224P)²+5.0622P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0534
_refine_ls_wR_factor_ref         0.0558
_reflns_number_gt                5739
_reflns_number_total             6992
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bt2015.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3204.5(10)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2208508
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_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
Sb Sb1 1.412206(18) 0.62355(3) -0.111332(18) 0.01877(7) Uani d . 1
Sb Sb2 1.456488(18) 0.86469(3) 0.051461(17) 0.01847(7) Uani d . 1
Sb Sb3 1.245628(17) 0.85087(3) -0.109001(17) 0.01748(7) Uani d . 1
Sb Sb4 1.028169(17) 0.85960(3) -0.264660(17) 0.01896(7) Uani d . 1
Sb Sb5 0.959911(19) 1.01239(3) -0.125205(19) 0.02475(8) Uani d . 1
Sb Sb6 0.806578(18) 0.94820(3) -0.045737(19) 0.02295(8) Uani d . 1
Sb Sb7 0.581883(17) 0.85275(3) -0.153428(18) 0.01867(7) Uani d . 1
Sb Sb8 0.654826(18) 0.64710(3) 0.035937(17) 0.01761(7) Uani d . 1
Sb Sb9 0.865630(17) 0.65213(3) 0.193069(17) 0.01834(7) Uani d . 1
Sb Sb10 0.700860(17) 0.88025(3) 0.200136(18) 0.01978(7) Uani d . 1
S S1 1.41676(7) 0.84261(10) -0.12516(7) 0.0191(2) Uani d . 1
S S2 1.47171(7) 0.64314(10) 0.04170(6) 0.0197(2) Uani d . 1
S S3 1.26256(6) 0.62939(10) -0.12057(7) 0.0189(2) Uani d . 1
S S4 1.30889(7) 0.83937(11) 0.04254(7) 0.0215(2) Uani d . 1
S S5 1.10046(6) 0.81489(12) -0.11902(6) 0.0233(2) Uani d . 1
S S6 1.01318(7) 0.64130(11) -0.29682(7) 0.0227(2) Uani d . 1
S S7 0.89314(7) 0.87887(13) -0.24672(7) 0.0265(3) Uani d . 1
S S8 0.93861(7) 0.85049(12) -0.04018(7) 0.0254(3) Uani d . 1
S S9 0.83685(7) 1.11761(12) -0.12197(8) 0.0279(3) Uani d . 1
S S10 0.71678(7) 0.85217(12) -0.17184(7) 0.0262(3) Uani d . 1
S S11 0.51176(7) 0.81046(13) -0.29719(7) 0.0249(3) Uani d . 1
S S12 0.59004(7) 0.63760(10) -0.11502(7) 0.0201(2) Uani d . 1
S S13 0.80123(7) 0.67173(11) 0.04206(6) 0.0209(2) Uani d . 1
S S14 0.63598(7) 0.86680(10) 0.04556(6) 0.0195(2) Uani d . 1
S S15 0.84821(7) 0.87393(11) 0.20742(7) 0.0201(2) Uani d . 1
S S16 0.69557(6) 0.66100(10) 0.21088(6) 0.0192(2) Uani d . 1
C C1 1.1854(6) 0.4301(6) 0.1499(5) 0.078(3) Uani d . 1
H H1A 1.1663 0.3708 0.1069 0.093 Uiso calc R 1
H H1B 1.2435 0.4152 0.1781 0.093 Uiso calc R 1
C C2 1.1759(4) 0.5554(5) 0.1135(3) 0.0405(14) Uani d . 1
H H2 1.1837 0.6168 0.1553 0.049 Uiso calc R 1
C C3 1.0954(4) 0.5793(8) 0.0463(4) 0.067(2) Uani d . 1
H H3A 1.0948 0.6616 0.0273 0.101 Uiso calc R 1
H H3B 1.0510 0.5688 0.0650 0.101 Uiso calc R 1
H H3C 1.0891 0.5228 0.0036 0.101 Uiso calc R 1
N N1 1.1441(5) 0.4070(6) 0.2031(4) 0.089(2) Uani d . 1
H H1C 1.1544 0.3307 0.2214 0.134 Uiso calc R 1
H H1D 1.0902 0.4165 0.1776 0.134 Uiso calc R 1
H H1E 1.1617 0.4593 0.2437 0.134 Uiso calc R 1
N N2 1.2422(3) 0.5689(5) 0.0810(3) 0.0542(14) Uani d . 1
H H2A 1.2907 0.5551 0.1194 0.081 Uiso calc R 1
H H2B 1.2413 0.6445 0.0622 0.081 Uiso calc R 1
H H2C 1.2345 0.5152 0.0418 0.081 Uiso calc R 1
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'
Sb Sb -0.5866 1.5461 '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
S1 Sb1 S3 . . 92.29(4) y
S1 Sb1 S2 . . 90.73(4) y
S3 Sb1 S2 . . 94.07(4) y
S2 Sb2 S4 . . 91.28(4) y
S2 Sb2 S6 . 4_676 92.40(4) y
S4 Sb2 S6 . 4_676 93.04(4) y
S3 Sb3 S5 . . 89.41(4) y
S3 Sb3 S4 . . 91.37(4) y
S5 Sb3 S4 . . 95.80(4) y
S6 Sb4 S7 . . 95.06(4) y
S6 Sb4 S5 . . 91.59(4) y
S7 Sb4 S5 . . 91.11(4) y
S8 Sb5 S9 . . 89.34(4) y
S8 Sb5 S7 . . 89.91(5) y
S9 Sb5 S7 . . 99.13(4) y
S9 Sb6 S10 . . 89.95(5) y
S9 Sb6 S8 . . 87.72(4) y
S10 Sb6 S8 . . 97.01(4) y
S12 Sb7 S11 . . 94.18(4) y
S12 Sb7 S10 . . 94.30(4) y
S11 Sb7 S10 . . 89.48(4) y
S14 Sb8 S13 . . 93.03(4) y
S14 Sb8 S12 . . 95.60(4) y
S13 Sb8 S12 . . 95.68(4) y
S15 Sb9 S11 . 4_676 89.67(4) y
S15 Sb9 S13 . . 90.36(4) y
S11 Sb9 S13 4_676 . 95.83(4) y
S16 Sb10 S15 . . 92.12(4) y
S16 Sb10 S14 . . 90.89(4) y
S15 Sb10 S14 . . 95.24(4) y
Sb2 S2 Sb1 . . 98.46(4) ?
Sb3 S3 Sb1 . . 99.85(4) ?
Sb2 S4 Sb3 . . 95.49(4) ?
Sb3 S5 Sb4 . . 98.88(4) ?
Sb4 S6 Sb2 . 4_575 104.22(4) ?
Sb4 S7 Sb5 . . 90.10(4) ?
Sb5 S8 Sb6 . . 90.90(4) ?
Sb5 S9 Sb6 . . 91.72(4) ?
Sb6 S10 Sb7 . . 100.93(5) ?
Sb7 S11 Sb9 . 4_575 98.29(4) ?
Sb7 S12 Sb8 . . 102.82(4) ?
Sb8 S13 Sb9 . . 94.74(4) ?
Sb8 S14 Sb10 . . 96.57(4) ?
Sb9 S15 Sb10 . . 100.57(4) ?
N1 C1 C2 . . 117.1(7) ?
N1 C1 H1A . . 108.0 ?
C2 C1 H1A . . 108.0 ?
N1 C1 H1B . . 108.0 ?
C2 C1 H1B . . 108.0 ?
H1A C1 H1B . . 107.3 ?
N2 C2 C1 . . 106.6(6) ?
N2 C2 C3 . . 107.4(5) ?
C1 C2 C3 . . 115.5(7) ?
N2 C2 H2 . . 109.0 ?
C1 C2 H2 . . 109.0 ?
C3 C2 H2 . . 109.0 ?
C2 C3 H3A . . 109.5 ?
C2 C3 H3B . . 109.5 ?
H3A C3 H3B . . 109.5 ?
C2 C3 H3C . . 109.5 ?
H3A C3 H3C . . 109.5 ?
H3B C3 H3C . . 109.5 ?
C1 N1 H1C . . 109.5 ?
C1 N1 H1D . . 109.5 ?
H1C N1 H1D . . 109.5 ?
C1 N1 H1E . . 109.5 ?
H1C N1 H1E . . 109.5 ?
H1D N1 H1E . . 109.5 ?
C2 N2 H2A . . 109.5 ?
C2 N2 H2B . . 109.5 ?
H2A N2 H2B . . 109.5 ?
C2 N2 H2C . . 109.5 ?
H2A N2 H2C . . 109.5 ?
H2B N2 H2C . . 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
Sb1 S1 . 2.4099(12) y
Sb1 S3 . 2.5604(12) y
Sb1 S2 . 2.5777(12) y
Sb2 S2 . 2.4477(12) y
Sb2 S4 . 2.5408(12) y
Sb2 S6 4_676 2.5475(12) y
Sb3 S3 . 2.4551(12) y
Sb3 S5 . 2.5082(12) y
Sb3 S4 . 2.5490(12) y
Sb4 S6 . 2.4451(13) y
Sb4 S7 . 2.5055(13) y
Sb4 S5 . 2.5115(12) y
Sb5 S8 . 2.4561(13) y
Sb5 S9 . 2.4583(13) y
Sb5 S7 . 2.5340(13) y
Sb6 S9 . 2.4747(14) y
Sb6 S10 . 2.4753(13) y
Sb6 S8 . 2.5113(13) y
Sb7 S12 . 2.4392(13) y
Sb7 S11 . 2.4727(12) y
Sb7 S10 . 2.4983(13) y
Sb8 S14 . 2.4368(12) y
Sb8 S13 . 2.5353(12) y
Sb8 S12 . 2.5397(12) y
Sb9 S15 . 2.4669(13) y
Sb9 S11 4_676 2.5288(12) y
Sb9 S13 . 2.5472(12) y
Sb10 S16 . 2.4070(13) y
Sb10 S15 . 2.5317(12) y
Sb10 S14 . 2.6014(12) y
S6 Sb2 4_575 2.5475(12) y
S11 Sb9 4_575 2.5288(12) y
C1 N1 . 1.418(10) ?
C1 C2 . 1.500(9) ?
C1 H1A . 0.9700 ?
C1 H1B . 0.9700 ?
C2 N2 . 1.486(8) ?
C2 C3 . 1.508(9) ?
C2 H2 . 0.9800 ?
C3 H3A . 0.9600 ?
C3 H3B . 0.9600 ?
C3 H3C . 0.9600 ?
N1 H1C . 0.8900 ?
N1 H1D . 0.8900 ?
N1 H1E . 0.8900 ?
N2 H2A . 0.8900 ?
N2 H2B . 0.8900 ?
N2 H2C . 0.8900 ?
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 H1C S7 3_765 0.89 2.53 3.341(7) 151
N1 H1C S10 3_765 0.89 3.37 3.905(8) 121
N2 H2A S7 4_676 0.89 2.53 3.309(5) 147
N2 H2B S4 . 0.89 2.52 3.340(6) 153
N2 H2C S13 3_765 0.89 2.48 3.343(6) 163
