# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_thiostannate_structure1
_database_code_depnum_ccdc_archive 'CCDC 1032729'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_audit_creation_date             2015-01-16
_audit_creation_method           
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4713)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '8(C2 H7 N2), S6 Sn2, S4 Sn'
_chemical_formula_sum            'C16 H56 N16 S10 Sn3'
_chemical_formula_weight         1149.43
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C16H56N16S10Sn3 '
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_H-M_alt        'C 1 2/m 1'
_space_group_name_Hall           '-C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'

_cell_length_a                   23.7739(6)
_cell_length_b                   16.0647(3)
_cell_length_c                   11.8936(3)
_cell_angle_alpha                90
_cell_angle_beta                 99.029(3)
_cell_angle_gamma                90
_cell_volume                     4486.14(19)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14398
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.2715
_cell_measurement_theta_min      2.2077
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.156
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64267
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.702
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2296
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0619
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            51708
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.336
_diffrn_reflns_theta_min         2.212
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -63.00   36.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864  -38.0000   60.0000 99

#__ type_ start__ end____ width___ exp.time_
  2 omega  -22.00   85.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864   77.0000    0.0000 107

#__ type_ start__ end____ width___ exp.time_
  3 omega  -46.00   24.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9364   77.0000 -180.0000 70

#__ type_ start__ end____ width___ exp.time_
  4 omega   35.00  101.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864  178.0000   30.0000 66

#__ type_ start__ end____ width___ exp.time_
  5 omega  -16.00   87.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864   38.0000  120.0000 103

#__ type_ start__ end____ width___ exp.time_
  6 omega  -19.00   85.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864   57.0000 -150.0000 104

#__ type_ start__ end____ width___ exp.time_
  7 omega  -20.00   53.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864  -99.0000 -180.0000 73

#__ type_ start__ end____ width___ exp.time_
  8 omega  -19.00   85.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864   57.0000    0.0000 104

#__ type_ start__ end____ width___ exp.time_
  9 omega -100.00  -34.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -      -11.9364  178.0000  -90.0000 66

#__ type_ start__ end____ width___ exp.time_
 10 omega  -20.00    5.00   1.0000   45.0000
omega____ theta____ kappa____ phi______ frames
    -       10.6864  -99.0000   90.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0230454000
_diffrn_orient_matrix_UB_12      -0.0068489000
_diffrn_orient_matrix_UB_13      0.0446401000
_diffrn_orient_matrix_UB_21      0.0188367000
_diffrn_orient_matrix_UB_22      -0.0037294000
_diffrn_orient_matrix_UB_23      -0.0404572000
_diffrn_orient_matrix_UB_31      0.0052384000
_diffrn_orient_matrix_UB_32      0.0434625000
_diffrn_orient_matrix_UB_33      0.0035854000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4911
_reflns_number_total             6020
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_data_collection       
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_data_reduction        
'CrysAlisPro, Agilent Technologies, Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET) (compiled Sep 14 2012,17:21:16)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         3.439
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         6020
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0538
_refine_ls_R_factor_gt           0.0369
_refine_ls_restrained_S_all      1.051
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0280P)²+20.3285P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0785
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H12A(0.5) H12B(0.5) H12C(0.5) H10A(0.5) H10B(0.5) H10C(0.5)
 H5C(0.5) H5D(0.5) H5E(0.5) H2C(0.5) H2D(0.5) H2E(0.5)
 Fixed U12: C11(0) C12(0) C9(0) C10(0) C6(0) C5(0) C2(0) C1(0) S3(0) S4(0)
 S6(0) S7(0) Sn2(0)
 Fixed U23: C11(0) C12(0) C9(0) C10(0) C6(0) C5(0) C2(0) C1(0) S3(0) S4(0)
 S6(0) S7(0) Sn2(0)
 Fixed Uiso: H5A(0.033) H5B(0.033) H1A(0.035) H1B(0.035) H2A(0.028) H2B(0.028)
 H3D(0.025) H3E(0.025)
3.a X=CH2 refined with riding coordinates:
 N7(H7D,H7E), N6(H6A,H6B)
3.b Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C7(H7A,H7B,H7C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C),
 C5(H5C,H5D,H5E), C2(H2C,H2D,H2E)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5060(2) 1.0000 0.1969(4) 0.0222(11) Uani 1 2 d S T P . .
C2 C 0.4561(2) 1.0000 0.2571(4) 0.0225(11) Uani 1 2 d S T P . .
C3 C 0.27455(16) 0.8402(3) 0.3398(3) 0.0299(9) Uani 1 1 d . . . . .
C4 C 0.32608(15) 0.8285(2) 0.2851(3) 0.0210(7) Uani 1 1 d . . . . .
C5 C 0.6146(2) 1.0000 0.4836(5) 0.0295(13) Uani 1 2 d S T P . .
C6 C 0.6504(2) 1.0000 0.3907(4) 0.0194(10) Uani 1 2 d S T P . .
C7 C 0.6025(2) 0.6340(3) 0.0753(4) 0.0514(14) Uani 1 1 d . . . . .
C8 C 0.63575(18) 0.7110(2) 0.0780(3) 0.0286(9) Uani 1 1 d . . . . .
C9 C 0.6660(2) 0.5000 0.5039(4) 0.0189(10) Uani 1 2 d S T P . .
C10 C 0.6333(2) 0.5000 0.3872(5) 0.0277(12) Uani 1 2 d S T P . .
C11 C 0.4214(2) 0.5000 0.2112(4) 0.0176(10) Uani 1 2 d S T P . .
C12 C 0.4847(2) 0.5000 0.2278(5) 0.0228(11) Uani 1 2 d S T P . .
H1A H 0.360(2) 0.575(3) 0.205(4) 0.035 Uiso 1 1 d . . . . .
H1B H 0.4164(19) 0.617(3) 0.206(4) 0.035 Uiso 1 1 d . . . . .
H2A H 0.6976(18) 0.426(3) 0.626(4) 0.028 Uiso 1 1 d . . . . .
H2B H 0.6700(17) 0.382(3) 0.510(4) 0.028 Uiso 1 1 d . . . . .
H2C H 0.4225 1.0144 0.2047 0.034 Uiso 0.5 1 calc GR . P . .
H2D H 0.4618 1.0400 0.3178 0.034 Uiso 0.5 1 calc GR . P . .
H2E H 0.4514 0.9456 0.2878 0.034 Uiso 0.5 1 calc GR . P . .
H3A H 0.2484 0.7953 0.3185 0.045 Uiso 1 1 calc GR . . . .
H3B H 0.2566 0.8921 0.3152 0.045 Uiso 1 1 calc GR . . . .
H3C H 0.2853 0.8408 0.4211 0.045 Uiso 1 1 calc GR . . . .
H3D H 0.6894(17) 1.074(2) 0.300(3) 0.025 Uiso 1 1 d . . . . .
H3E H 0.6560(18) 1.113(3) 0.374(4) 0.025 Uiso 1 1 d . . . . .
H4A H 0.3976(18) 0.771(2) 0.303(3) 0.021(11) Uiso 1 1 d . . . . .
H4B H 0.3642(19) 0.762(3) 0.400(4) 0.031(12) Uiso 1 1 d . . . . .
H5A H 0.3564(19) 0.860(3) 0.156(4) 0.033 Uiso 1 1 d . . . . .
H5B H 0.3060(19) 0.901(3) 0.161(4) 0.033 Uiso 1 1 d . . . . .
H5C H 0.5846 1.0402 0.4665 0.044 Uiso 0.5 1 calc GR . P . .
H5D H 0.6379 1.0141 0.5545 0.044 Uiso 0.5 1 calc GR . P . .
H5E H 0.5985 0.9457 0.4894 0.044 Uiso 0.5 1 calc GR . P . .
H6A H 0.7087 0.7547 0.0765 0.050 Uiso 1 1 calc R . . . .
H6B H 0.7065 0.6621 0.0696 0.050 Uiso 1 1 calc R . . . .
H7A H 0.5920 0.6243 0.1489 0.077 Uiso 1 1 calc GR . . . .
H7B H 0.6250 0.5881 0.0556 0.077 Uiso 1 1 calc GR . . . .
H7C H 0.5687 0.6390 0.0197 0.077 Uiso 1 1 calc GR . . . .
H7D H 0.6264 0.8285 0.0875 0.041 Uiso 1 1 calc R . . . .
H7E H 0.5723 0.7817 0.0875 0.041 Uiso 1 1 calc R . . . .
H8A H 0.5125(19) 1.123(3) 0.183(4) 0.040(13) Uiso 1 1 d . . . . .
H8B H 0.553(2) 1.069(3) 0.131(4) 0.041(14) Uiso 1 1 d . . . . .
H10A H 0.5974 0.4727 0.3876 0.042 Uiso 0.5 1 calc GR . P . .
H10B H 0.6544 0.4709 0.3370 0.042 Uiso 0.5 1 calc GR . P . .
H10C H 0.6268 0.5563 0.3615 0.042 Uiso 0.5 1 calc GR . P . .
H12A H 0.4993 0.5134 0.3055 0.034 Uiso 0.5 1 calc GR . P . .
H12B H 0.4976 0.5407 0.1785 0.034 Uiso 0.5 1 calc GR . P . .
H12C H 0.4981 0.4459 0.2100 0.034 Uiso 0.5 1 calc GR . P . .
N1 N 0.39470(14) 0.5717(2) 0.2035(3) 0.0236(7) Uani 1 1 d . . . . .
N2 N 0.67997(14) 0.42836(19) 0.5533(3) 0.0233(7) Uani 1 1 d . . . . .
N3 N 0.66623(14) 1.07094(19) 0.3521(3) 0.0211(7) Uani 1 1 d . . . . .
N4 N 0.36655(15) 0.7786(2) 0.3327(3) 0.0256(7) Uani 1 1 d . . . . .
N5 N 0.32907(15) 0.8655(2) 0.1885(3) 0.0280(7) Uani 1 1 d . . . . .
N6 N 0.68965(17) 0.7090(2) 0.0743(3) 0.0413(9) Uani 1 1 d . . . . .
N7 N 0.60825(15) 0.7820(2) 0.0852(3) 0.0338(8) Uani 1 1 d . . . . .
N8 N 0.52830(16) 1.0702(2) 0.1701(4) 0.0329(9) Uani 1 1 d . . . . .
S1 S 0.52150(4) 0.74190(5) 0.79885(8) 0.01980(18) Uani 1 1 d . . . . .
S2 S 0.36867(4) 0.73422(5) 0.60515(8) 0.01852(18) Uani 1 1 d . . . . .
S3 S 0.5000 0.84576(7) 0.5000 0.0160(2) Uani 1 2 d S T P . .
S4 S 0.5000 0.62331(7) 0.5000 0.0201(3) Uani 1 2 d S T P . .
S5 S 0.25831(4) 0.62054(5) 0.18275(7) 0.01897(18) Uani 1 1 d . . . . .
S6 S 0.26990(5) 0.5000 -0.09513(11) 0.0199(3) Uani 1 2 d S T P . .
S7 S 0.12638(6) 0.5000 0.02394(12) 0.0292(3) Uani 1 2 d S T P . .
Sn1 Sn 0.46759(2) 0.73446(2) 0.61522(2) 0.01477(7) Uani 1 1 d . . . . .
Sn2 Sn 0.22729(2) 0.5000 0.07348(3) 0.01590(8) Uani 1 2 d S T P . .
_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N8 1.306(4) 6_575 ?
C1 N8 1.307(4) . ?
C2 C1 1.480(7) . ?
C4 C3 1.487(5) . ?
C4 N4 1.310(5) . ?
C4 N5 1.306(5) . ?
C6 C5 1.497(7) . ?
C6 N3 1.305(4) 6_575 ?
C6 N3 1.305(4) . ?
C7 C8 1.466(6) . ?
C9 C10 1.481(7) . ?
C9 N2 1.311(4) . ?
C9 N2 1.311(4) 6_565 ?
C11 C12 1.487(7) . ?
C11 N1 1.312(4) 6_565 ?
C11 N1 1.312(4) . ?
N6 C8 1.289(5) . ?
N7 C8 1.325(5) . ?
S1 Sn1 2.3556(9) . ?
S2 Sn1 2.3359(9) . ?
S3 Sn1 2.4495(8) 2_656 ?
S3 Sn1 2.4495(8) . ?
S4 Sn1 2.4477(9) 2_656 ?
S4 Sn1 2.4477(9) . ?
S5 Sn2 2.3836(9) . ?
S6 Sn2 2.3844(13) . ?
S7 Sn2 2.3790(13) . ?
Sn2 S5 2.3836(9) 6_565 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag

N1 C11 C12 118.6(2) 6_565 . ?
N1 C11 C12 118.6(2) . . ?
N1 C11 N1 122.8(5) 6_565 . ?
N2 C9 C10 118.6(2) . . ?
N2 C9 C10 118.6(2) 6_565 . ?
N2 C9 N2 122.8(5) . 6_565 ?
N3 C6 C5 119.2(2) . . ?
N3 C6 C5 119.2(2) 6_575 . ?
N3 C6 N3 121.6(5) . 6_575 ?
N4 C4 C3 119.2(3) . . ?
N5 C4 C3 119.3(3) . . ?
N5 C4 N4 121.4(4) . . ?
N6 C8 C7 121.0(4) . . ?
N6 C8 N7 121.7(4) . . ?
N7 C8 C7 117.3(4) . . ?
N8 C1 C2 120.3(3) . . ?
N8 C1 C2 120.3(3) 6_575 . ?
N8 C1 N8 119.4(5) 6_575 . ?
S1 Sn1 S3 107.97(2) . . ?
S1 Sn1 S4 112.51(2) . . ?
S2 Sn1 S3 112.03(2) . . ?
S2 Sn1 S4 111.90(2) . . ?
S2 Sn1 S1 116.40(3) . . ?
S4 Sn1 S3 93.73(3) . . ?
S5 Sn2 S5 108.66(4) 6_565 . ?
S5 Sn2 S6 108.82(3) . . ?
S5 Sn2 S6 108.82(3) 6_565 . ?
S7 Sn2 S5 110.41(3) . . ?
S7 Sn2 S5 110.41(3) . 6_565 ?
S7 Sn2 S6 109.68(5) . . ?
Sn1 S3 Sn1 86.23(4) 2_656 . ?
Sn1 S4 Sn1 86.31(4) 2_656 . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_thiostannate_structure2
_database_code_depnum_ccdc_archive 'CCDC 1032730'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_audit_creation_date             2014-11-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C2 H8 N, S3 Sn, H4 N'
_chemical_formula_sum            'C2 H12 N2 S3 Sn'
_chemical_formula_weight         279.01
_chemical_absolute_configuration .
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C2 H12 N2 S3 Sn'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'

_cell_length_a                   5.93925(12)
_cell_length_b                   12.1816(2)
_cell_length_c                   12.4709(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     902.26(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4699
_cell_measurement_temperature    99.98(10)
_cell_measurement_theta_max      30.8341
_cell_measurement_theta_min      2.3325
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.447
_exptl_absorpt_correction_T_max  0.621
_exptl_absorpt_correction_T_min  0.209
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.054
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.4862
_exptl_crystal_size_mid          0.0934
_exptl_crystal_size_min          0.0744
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0261
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.918
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            6136
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.903
_diffrn_reflns_theta_min         2.337
_diffrn_ambient_temperature      99.98(10)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.918
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -4.00   56.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4966   38.0000  120.0000 60

#__ type_ start__ end____ width___ exp.time_
  2 omega  -70.00    8.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      -15.7466  -57.0000  -30.0000 78

#__ type_ start__ end____ width___ exp.time_
  3 omega   34.00   59.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4966 -178.0000  -60.0000 25

#__ type_ start__ end____ width___ exp.time_
  4 omega   34.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -       14.4966 -178.0000  120.0000 69
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0117678000
_diffrn_orient_matrix_UB_12      -0.0555633000
_diffrn_orient_matrix_UB_13      0.0160342000
_diffrn_orient_matrix_UB_21      -0.0133124000
_diffrn_orient_matrix_UB_22      0.0157723000
_diffrn_orient_matrix_UB_23      0.0543907000
_diffrn_orient_matrix_UB_31      -0.1180901000
_diffrn_orient_matrix_UB_32      -0.0073248000
_diffrn_orient_matrix_UB_33      -0.0045339000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.651
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.831
_reflns_number_gt                2473
_reflns_number_total             2525
_reflns_odcompleteness_completeness 99.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         1.624
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.172
_refine_ls_abs_structure_details 
'Flack, H. D. (1983). Acta Cryst. A39, 876-881.'
_refine_ls_abs_structure_Flack   0.45(9)
_refine_ls_extinction_coef       0.0044(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.242
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     89
_refine_ls_number_reflns         2525
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0326
_refine_ls_R_factor_gt           0.0316
_refine_ls_restrained_S_all      1.241
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+4.4107P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0747
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed Sof: Sn1(0.82) Sn1A(0.18)
 Fixed Uiso: H1A(0.022) H1B(0.022) H2A(0.016) H1C(0.022) H2B(0.016) H3A(0.024)
 H3B(0.024) H3C(0.024) H1D(0.021) H1E(0.021) H1F(0.021) H1G(0.021)
 Fixed X: H1A(1.0098) H1B(1.1251) H2A(1.1399) H1C(0.8621) H2B(0.8953)
 H3A(1.1315) H3B(1.0197) H3C(0.8686)
 Fixed Y: H1A(0.7166) H1B(0.8297) H2A(0.7887) H1C(0.8219) H2B(0.7851)
 H3A(0.9724) H3B(0.9487) H3C(0.9678)
 Fixed Z: H1A(0.0673) H1B(0.0432) H2A(0.222) H1C(0.0504) H2B(0.2279)
 H3A(0.1827) H3B(0.2942) H3C(0.1928)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 1.0014(11) 0.7945(5) 0.0788(5) 0.0153(12) Uani 1 1 d . . . . .
C2 C 1.0077(13) 0.9372(5) 0.2184(5) 0.0160(13) Uani 1 1 d . . . . .
H1A H 1.0098 0.7166 0.0673 0.022 Uiso 1 1 d . . . . .
H1B H 1.1251 0.8297 0.0432 0.022 Uiso 1 1 d . . . . .
H1C H 0.8621 0.8219 0.0504 0.022 Uiso 1 1 d . . . . .
H1D H 0.097(10) 0.511(5) 0.569(4) 0.021 Uiso 1 1 d D . . . .
H1E H -0.130(6) 0.496(6) 0.593(5) 0.021 Uiso 1 1 d D . . . .
H1F H 0.038(12) 0.447(4) 0.664(5) 0.021 Uiso 1 1 d D . . . .
H1G H 0.000(12) 0.567(3) 0.664(5) 0.021 Uiso 1 1 d D . . . .
H2A H 1.1399 0.7887 0.2220 0.016 Uiso 1 1 d . . . . .
H2B H 0.8953 0.7851 0.2279 0.016 Uiso 1 1 d . . . . .
H3A H 1.1315 0.9724 0.1827 0.024 Uiso 1 1 d . . . . .
H3B H 1.0197 0.9487 0.2942 0.024 Uiso 1 1 d . . . . .
H3C H 0.8686 0.9678 0.1928 0.024 Uiso 1 1 d . . . . .
N1 N 1.0125(9) 0.8177(4) 0.1951(4) 0.0134(10) Uani 1 1 d . . . . .
N2 N 0.0029(10) 0.5055(4) 0.6246(4) 0.0133(10) Uani 1 1 d D . . . .
S1 S 0.0183(3) 0.69132(11) 0.43425(13) 0.0125(3) Uani 1 1 d . . . . .
S2 S 0.5035(3) 0.49216(11) 0.48474(12) 0.0101(3) Uani 1 1 d . . . . .
S3 S 0.5132(3) 0.73384(12) 0.25528(12) 0.0109(3) Uani 1 1 d . . . . .
Sn1 Sn 0.43811(8) 0.67258(4) 0.43135(4) 0.00617(13) Uani 0.82 1 d . . P A 1
Sn1A Sn 0.5618(4) 0.67281(17) 0.43135(18) 0.00617(13) Uani 0.18 1 d . . P A 2
_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.479(8) . ?
C2 N1 1.484(8) . ?
S1 Sn1 2.4052(16) 3_466 ?
S1 Sn1 2.5041(16) . ?
S1 Sn1A 2.370(3) 3_466 ?
S1 Sn1A 2.721(3) 1_455 ?
S2 Sn1 2.3291(14) . ?
S2 Sn1A 2.325(2) . ?
S3 Sn1 2.3616(16) . ?
S3 Sn1A 2.336(3) . ?
Sn1 S1 2.4051(16) 3_566 ?
Sn1A S1 2.721(3) 1_655 ?
Sn1A S1 2.370(3) 3_566 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 N1 C2 112.3(5) . . ?
S1 Sn1 S1 97.14(5) 3_566 . ?
S1 Sn1A S1 92.36(9) 3_566 1_655 ?
S2 Sn1 S1 104.36(5) . . ?
S2 Sn1 S1 114.72(5) . 3_566 ?
S2 Sn1 S3 122.18(6) . . ?
S2 Sn1A S1 102.88(9) . 1_655 ?
S2 Sn1A S1 116.25(10) . 3_566 ?
S2 Sn1A S3 123.51(11) . . ?
S3 Sn1 S1 99.94(6) . . ?
S3 Sn1 S1 113.12(5) . 3_566 ?
S3 Sn1A S1 115.41(10) . 3_566 ?
S3 Sn1A S1 96.27(10) . 1_655 ?
Sn1 S1 Sn1 105.67(6) 3_466 . ?
Sn1A S1 Sn1A 100.13(9) 3_466 1_455 ?

loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 -1 -1 0.0348 -0.0002 -0.9999 -1.0003 0.0395 -0.0702 0.0119
-1 -1 0 0.1624 -1.0000 -1.0002 0.0002 0.0438 -0.0025 0.1254
0 -1 1 0.0508 -0.0000 -1.0000 0.9999 0.0716 0.0386 0.0028
0 1 -1 0.0426 0.0000 1.0000 -0.9999 -0.0716 -0.0386 -0.0028
1 0 0 0.2958 0.9999 0.0002 -0.0003 0.0117 -0.0133 -0.1181
-1 0 1 0.1543 -0.9998 -0.0003 1.0004 0.0043 0.0677 0.1135
0 1 1 0.0396 0.0002 0.9999 1.0003 -0.0395 0.0702 -0.0119

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_thiostanante_structure3
_database_code_depnum_ccdc_archive 'CCDC 1032731'
_audit_update_record             
;
2015-02-11 deposited with the CCDC.
2015-02-16 downloaded from the CCDC.
;
_audit_creation_date             2014-11-04
_audit_creation_method           
;
Olex2 1.2
(compiled 2014.09.19 svn.r3010 for OlexSys, GUI svn.r4874)
;
_shelxl_version_number           2014-3
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         '3(S9 Sn3), 18(H4 N), 4(H2 O)'
_chemical_formula_sum            'H80 N18 O4 S27 Sn9'
_chemical_formula_weight         2330.65
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'H20 N4 O1 S6 Sn2'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
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'
O O 0.0106 0.0060 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'C 1 2 1'
_space_group_name_Hall           'C 2y'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'

_cell_length_a                   16.98717(13)
_cell_length_b                   10.54777(7)
_cell_length_c                   21.08715(19)
_cell_angle_alpha                90
_cell_angle_beta                 108.0389(9)
_cell_angle_gamma                90
_cell_volume                     3592.61(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    32112
_cell_measurement_temperature    99.97(11)
_cell_measurement_theta_max      32.6517
_cell_measurement_theta_min      2.3015
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.891
_exptl_absorpt_correction_T_max  0.778
_exptl_absorpt_correction_T_min  0.602
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.1599
_exptl_crystal_size_mid          0.1065
_exptl_crystal_size_min          0.0788
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            43957
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.922
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.726
_diffrn_reflns_theta_min         2.306
_diffrn_ambient_temperature      99.97(11)
_diffrn_detector_area_resol_mean 10.3590
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0298142000
_diffrn_orient_matrix_UB_12      0.0025238000
_diffrn_orient_matrix_UB_13      -0.0320901000
_diffrn_orient_matrix_UB_21      0.0046933000
_diffrn_orient_matrix_UB_22      -0.0661077000
_diffrn_orient_matrix_UB_23      -0.0038485000
_diffrn_orient_matrix_UB_31      -0.0319004000
_diffrn_orient_matrix_UB_32      -0.0120741000
_diffrn_orient_matrix_UB_33      0.0143651000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.886
_reflns_number_gt                11917
_reflns_number_total             12197
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     30.44
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.21 (release 14-08-2012 CrysAlis171 .NET)
(compiled Sep 14 2012,17:21:16)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.919
_refine_diff_density_min         -0.750
_refine_diff_density_rms         0.098
_refine_ls_abs_structure_details 
;
 Flack x determined using 5368 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.029(5)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         12197
_refine_ls_number_restraints     67
_refine_ls_R_factor_all          0.0180
_refine_ls_R_factor_gt           0.0170
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0130P)²+1.4488P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0335
_refine_ls_wR_factor_ref         0.0338
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Others
 Fixed U12: S14(0) Sn4(0) Sn5(0) N3(0) N10(0)
 Fixed U23: S14(0) Sn4(0) Sn5(0) N3(0) N10(0)
 Fixed Uiso: H2E(0.044) H2F(0.044)
 Fixed X: S14(0.5) Sn4(0.5) N3(0.5) N10(0.5) H2E(0.5821) H2F(0.6024)
 Fixed Y: H2E(0.6392) H2F(0.7499)
 Fixed Z: S14(0) Sn4(0) N3(0.5) N10(0.5) H2E(0.1774) H2F(0.2145)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
H1A H 0.5046(14) 0.292(4) 0.1679(19) 0.041(13) Uiso 1 1 d D . . . .
H1B H 0.534(2) 0.1674(16) 0.1754(17) 0.026(11) Uiso 1 1 d D . . . .
H1C H 0.5951(12) 0.267(4) 0.182(2) 0.044(14) Uiso 1 1 d D . . . .
H1D H 0.553(3) 0.255(4) 0.2339(7) 0.050(15) Uiso 1 1 d D . . . .
H1E H 0.608(3) 0.012(2) 0.4707(16) 0.042(14) Uiso 1 1 d D . . . .
H1F H 0.623(3) 0.057(4) 0.5332(6) 0.042(14) Uiso 1 1 d D . . . .
H2A H 0.340(2) 0.2741(15) 0.003(2) 0.034(12) Uiso 1 1 d D . . . .
H2B H 0.3131(17) 0.405(3) -0.006(2) 0.030(12) Uiso 1 1 d D . . . .
H2C H 0.3985(15) 0.385(4) 0.0306(13) 0.020(10) Uiso 1 1 d D . . . .
H2D H 0.376(3) 0.362(5) -0.0359(14) 0.039(13) Uiso 1 1 d D . . . .
H2E H 0.5821 0.6392 0.1774 0.044 Uiso 1 1 d DG . . . .
H2F H 0.6024 0.7499 0.2145 0.044 Uiso 1 1 d DG . . . .
H3A H 0.4562(11) 0.360(2) 0.489(3) 0.063(18) Uiso 1 1 d D . . . .
H3B H 0.500(3) 0.253(2) 0.4673(13) 0.16(4) Uiso 1 1 d D . . . .
H4A H 0.525(2) -0.010(4) 0.7291(4) 0.028(12) Uiso 1 1 d D . . . .
H4B H 0.497(2) 0.0828(14) 0.677(2) 0.027(11) Uiso 1 1 d D . . . .
H4C H 0.4694(17) -0.039(4) 0.6600(13) 0.038(13) Uiso 1 1 d D . . . .
H4D H 0.5600(16) -0.015(3) 0.676(2) 0.038(13) Uiso 1 1 d D . . . .
H5A H 0.373(3) 0.663(6) 0.0951(4) 0.09(2) Uiso 1 1 d D . . . .
H5B H 0.3445(18) 0.692(3) 0.153(2) 0.031(12) Uiso 1 1 d D . . . .
H5C H 0.4318(16) 0.697(4) 0.1624(17) 0.044(15) Uiso 1 1 d D . . . .
H5D H 0.395(3) 0.5774(14) 0.149(2) 0.051(15) Uiso 1 1 d D . . . .
H6A H 0.270(3) 0.026(2) 0.182(2) 0.048(15) Uiso 1 1 d D . . . .
H6B H 0.249(3) 0.090(4) 0.1219(7) 0.048(16) Uiso 1 1 d D . . . .
H6C H 0.215(2) 0.138(4) 0.176(3) 0.067(18) Uiso 1 1 d D . . . .
H6D H 0.297(2) 0.158(4) 0.1842(18) 0.057(16) Uiso 1 1 d D . . . .
H7A H 0.705(2) 0.242(5) 0.4118(6) 0.039(13) Uiso 1 1 d D . . . .
H7B H 0.7645(8) 0.259(5) 0.4803(14) 0.047(15) Uiso 1 1 d D . . . .
H7C H 0.694(3) 0.3316(16) 0.461(3) 0.052(16) Uiso 1 1 d D . . . .
H7D H 0.683(3) 0.192(3) 0.466(3) 0.066(18) Uiso 1 1 d D . . . .
H8A H 0.346(2) 0.614(3) 0.6288(11) 0.026(11) Uiso 1 1 d D . . . .
H8B H 0.2902(8) 0.533(3) 0.653(2) 0.028(12) Uiso 1 1 d D . . . .
H8C H 0.3788(15) 0.500(2) 0.662(2) 0.030(12) Uiso 1 1 d D . . . .
H8D H 0.353(3) 0.596(3) 0.7009(8) 0.032(12) Uiso 1 1 d D . . . .
H9A H 0.194(3) 0.5812(19) 0.1564(16) 0.034(13) Uiso 1 1 d D . . . .
H9B H 0.1344(11) 0.479(4) 0.139(2) 0.042(14) Uiso 1 1 d D . . . .
H9C H 0.175(3) 0.510(4) 0.0919(5) 0.063(18) Uiso 1 1 d D . . . .
H9D H 0.2248(15) 0.453(3) 0.153(2) 0.042(14) Uiso 1 1 d D . . . .
H10A H 0.535(3) 0.677(3) 0.488(3) 0.11(3) Uiso 1 1 d D . . . .
H10B H 0.476(3) 0.786(3) 0.470(2) 0.10(2) Uiso 1 1 d D . . . .
N1 N 0.54835(17) 0.2459(3) 0.19063(14) 0.0155(5) Uani 1 1 d D . . . .
N2 N 0.35590(17) 0.3533(3) -0.00190(16) 0.0172(6) Uani 1 1 d D . . . .
N3 N 0.5000 0.3072(5) 0.5000 0.0296(10) Uani 1 2 d DS T P . .
N4 N 0.51377(17) 0.0027(3) 0.68546(15) 0.0154(5) Uani 1 1 d D . . . .
N5 N 0.38469(19) 0.6593(3) 0.13929(17) 0.0194(6) Uani 1 1 d D . . . .
N6 N 0.2565(2) 0.1032(3) 0.16512(17) 0.0221(6) Uani 1 1 d D . . . .
N7 N 0.71154(17) 0.2541(3) 0.45488(15) 0.0170(5) Uani 1 1 d D . . . .
N8 N 0.34196(18) 0.5609(3) 0.66065(16) 0.0194(6) Uani 1 1 d D . . . .
N9 N 0.18304(17) 0.5066(3) 0.13571(15) 0.0166(5) Uani 1 1 d D . . . .
N10 N 0.5000 0.7278(5) 0.5000 0.0269(9) Uani 1 2 d DS T P . .
O1 O 0.60490(18) 0.0789(3) 0.49243(14) 0.0264(6) Uani 1 1 d D . . . .
O2 O 0.61820(17) 0.6751(3) 0.20959(15) 0.0295(6) Uani 1 1 d . . . . .
S1 S 0.19622(4) 0.58990(7) 0.30623(4) 0.01153(13) Uani 1 1 d . . . . .
S2 S 0.34910(5) 0.51572(7) 0.48968(4) 0.01428(14) Uani 1 1 d . . . . .
S3 S 0.13844(5) 0.33519(7) 0.40757(4) 0.01345(14) Uani 1 1 d . . . . .
S4 S 0.32171(5) 0.27586(7) 0.34210(5) 0.01781(16) Uani 1 1 d . . . . .
S5 S 0.54154(4) 0.30379(7) 0.33916(4) 0.01318(14) Uani 1 1 d . . . . .
S6 S 0.35952(5) 0.36300(7) 0.17555(4) 0.01284(14) Uani 1 1 d . . . . .
S7 S 0.43373(4) 0.61602(7) 0.32033(4) 0.01339(14) Uani 1 1 d . . . . .
S8 S 0.24389(5) 0.79726(7) 0.18532(4) 0.01346(14) Uani 1 1 d . . . . .
S9 S 0.33929(5) 0.89790(8) 0.37431(4) 0.01722(15) Uani 1 1 d . . . . .
S10 S 0.53012(5) 0.49757(8) 0.09343(4) 0.01721(16) Uani 1 1 d . . . . .
S11 S 0.38118(4) 0.76834(7) -0.01415(4) 0.01112(13) Uani 1 1 d . . . . .
S12 S 0.50033(5) 0.93354(8) 0.16238(4) 0.01433(14) Uani 1 1 d . . . . .
S13 S 0.29185(4) 1.06597(7) 0.01971(4) 0.01222(14) Uani 1 1 d . . . . .
S14 S 0.5000 1.10040(10) 0.0000 0.0123(2) Uani 1 2 d S T P . .
Sn1 Sn 0.25561(2) 0.43409(2) 0.39219(2) 0.00978(4) Uani 1 1 d . . . . .
Sn2 Sn 0.41018(2) 0.39323(2) 0.29175(2) 0.00892(4) Uani 1 1 d . . . . .
Sn3 Sn 0.30450(2) 0.73178(2) 0.29726(2) 0.00941(4) Uani 1 1 d . . . . .
Sn4 Sn 0.5000 0.63035(3) 0.0000 0.00910(5) Uani 1 2 d S T P . .
Sn5 Sn 0.42082(2) 0.96293(2) 0.05065(2) 0.00850(4) Uani 1 1 d . . . . .
_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag

S1 Sn3 2.4236(7) . ?
S1 Sn1 2.4233(8) . ?
S2 Sn1 2.3384(8) . ?
S5 Sn2 2.3425(7) . ?
S4 Sn2 2.4303(8) . ?
S6 Sn2 2.3539(8) . ?
S7 Sn3 2.4260(7) . ?
S7 Sn2 2.4282(8) . ?
S8 Sn3 2.3672(8) . ?
S9 Sn3 2.3376(8) . ?
S10 Sn4 2.3410(8) . ?
S11 Sn4 2.4307(7) . ?
S11 Sn5 2.4420(7) . ?
S12 Sn5 2.3454(8) . ?
S13 Sn5 2.3497(7) . ?
S14 Sn5 2.4377(6) . ?
S14 Sn5 2.4377(6) 2_655 ?
Sn1 S3 2.3568(7) . ?
Sn1 S4 2.4283(8) . ?
Sn4 S10 2.3410(8) 2_655 ?
Sn4 S11 2.4307(7) 2_655 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
S1 Sn3 S7 109.58(3) . . ?
S1 Sn1 S4 106.39(3) . . ?
S2 Sn1 S1 114.84(3) . . ?
S2 Sn1 S3 114.50(3) . . ?
S2 Sn1 S4 110.85(3) . . ?
S3 Sn1 S1 103.26(3) . . ?
S3 Sn1 S4 106.24(3) . . ?
S5 Sn2 S7 102.82(3) . . ?
S5 Sn2 S6 112.49(3) . . ?
S5 Sn2 S4 104.16(3) . . ?
S6 Sn2 S7 111.62(3) . . ?
S6 Sn2 S4 108.03(3) . . ?
S7 Sn2 S4 117.47(3) . . ?
S8 Sn3 S7 115.72(3) . . ?
S8 Sn3 S1 98.72(3) . . ?
S9 Sn3 S7 102.68(3) . . ?
S9 Sn3 S1 116.31(3) . . ?
S9 Sn3 S8 114.37(3) . . ?
S10 Sn4 S10 106.51(4) 2_655 . ?
S10 Sn4 S11 107.35(3) 2_655 . ?
S10 Sn4 S11 114.73(3) . . ?
S10 Sn4 S11 107.35(3) . 2_655 ?
S10 Sn4 S11 114.73(3) 2_655 2_655 ?
S11 Sn4 S11 106.43(3) 2_655 . ?
S12 Sn5 S14 107.13(2) . . ?
S12 Sn5 S13 122.51(3) . . ?
S12 Sn5 S11 115.10(3) . . ?
S13 Sn5 S14 101.35(2) . . ?
S13 Sn5 S11 99.30(3) . . ?
S14 Sn5 S11 110.41(2) . . ?
Sn1 S4 Sn2 105.77(3) . . ?
Sn1 S1 Sn3 109.08(3) . . ?
Sn3 S7 Sn2 111.59(3) . . ?
Sn4 S11 Sn5 111.10(3) . . ?
Sn5 S14 Sn5 107.00(4) . 2_655 ?
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
0 1 0 0.0487 -0.0000 1.0000 -0.0000 0.0025 -0.0661 -0.0121
1 0 -1 0.0612 1.0000 -0.0000 -1.0000 0.0023 0.0085 -0.0463
-1 0 1 0.0453 -1.0000 0.0000 1.0000 -0.0023 -0.0085 0.0463
-1 0 -2 0.0708 -1.0000 -0.0000 -2.0000 0.0940 0.0030 0.0032
0 -1 0 0.0301 0.0000 -1.0000 0.0000 -0.0025 0.0661 0.0121
1 0 2 0.0869 1.0000 0.0000 2.0000 -0.0940 -0.0030 -0.0032
2 1 -1 0.0521 2.0000 1.0000 -1.0000 -0.0250 -0.0529 -0.0902
-1 -1 2 0.0441 -1.0000 -1.0000 2.0000 -0.0369 0.0537 0.0727
1 1 -2 0.0594 1.0000 1.0000 -2.0000 0.0369 -0.0537 -0.0727
-3 2 1 0.0521 -3.0000 2.0000 0.9999 0.0624 -0.1501 0.0859
2 2 1 0.0581 2.0000 2.0000 1.0000 -0.0867 -0.1267 -0.0736

_olex2_submission_special_instructions 'No special instructions were received'
