# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_DMeAEt_4_SnBr10
_database_code_depnum_ccdc_archive 'CCDC 1497737'
_audit_update_record             
;
2016-08-04 deposited with the CCDC.
2017-11-21 downloaded from the CCDC.
;
_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_cell_length_a                   10.2070(4)
_cell_length_b                   10.6944(4)
_cell_length_c                   18.5996(6)
_cell_angle_alpha                94.043(3)
_cell_angle_beta                 102.847(3)
_cell_angle_gamma                97.904(3)
_cell_volume                     1949.89(12)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  ?

_cell_formula_units_Z            2

# Given Formula = C16 H56 Br10 N8 Sn1 
# Dc =      2.18 Fooo =   1216.00 Mu =    109.22 M =   1278.40
# Found Formula = C16 H56 Br10 N8 Sn1 
# Dc =      2.18 FOOO =   1216.00 Mu =    109.22 M =   1278.40

_chemical_formula_sum            'C16 H56 Br10 N8 Sn1'
_chemical_formula_moiety         'C16 H56 Br10 N8 Sn1'
_chemical_compound_source        ?
_chemical_formula_weight         1278.40

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Br -0.2901 2.4595 17.1789 2.1723 5.2358 16.5796 5.6377 0.2609 3.9851 41.4328
2.9557 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sn -0.6537 1.4246 19.1889 5.8303 19.1005 0.5031 4.4585 26.8909 2.4663 83.9572
4.7821 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_measurement_reflns_used    15194
_cell_measurement_theta_min      3
_cell_measurement_theta_max      34
_cell_measurement_temperature    120

_exptl_crystal_description       ?
_exptl_crystal_colour            clear
_exptl_crystal_size_min          0.105
_exptl_crystal_size_mid          0.241
_exptl_crystal_size_max          0.269

_exptl_crystal_density_diffrn    2.177
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1216
_exptl_absorpt_coefficient_mu    10.922

# Sheldrick geometric approximatio 0.07 0.32 
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
; 
 Gaussian Integration (Busing and Levy, 1957) 
;
_exptl_absorpt_correction_T_min  0.07
_exptl_absorpt_correction_T_max  0.32
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      120
_diffrn_reflns_number            57392
_reflns_number_total             15194
_diffrn_reflns_av_R_equivalents  0.088
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 15194 
# Theoretical number of reflections is about 23100 

_diffrn_reflns_theta_min         2.815
_diffrn_reflns_theta_max         34.220
_diffrn_measured_fraction_theta_max 0.939

_diffrn_reflns_theta_full        30.798
_diffrn_measured_fraction_theta_full 0.995

_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_reflns_limit_h_min              -16
_reflns_limit_h_max              15
_reflns_limit_k_min              -16
_reflns_limit_k_max              16
_reflns_limit_l_min              0
_reflns_limit_l_max              28

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -2.23
_refine_diff_density_max         1.92

# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 

# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         11532
_refine_ls_number_restraints     240
_refine_ls_number_parameters     540
_oxford_refine_ls_R_factor_ref   0.0651
_refine_ls_wR_factor_ref         0.0511
_refine_ls_goodness_of_fit_ref   0.9933
_refine_ls_shift/su_max          0.0012271
_refine_ls_shift/su_mean         0.0000387

# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11532
_refine_ls_R_factor_all          0.0651
_refine_ls_wR_factor_all         0.0511

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                8737
_refine_ls_R_factor_gt           0.0441
_refine_ls_wR_factor_gt          0.0479

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 191. 144. 60.6 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Sn1 Sn 0.50513(4) 0.73268(3) 0.25379(2) 0.0165 1.0000 Uani . . . . . .
Br1 Br 0.63291(5) 0.68065(5) 0.39545(3) 0.0213 1.0000 Uani . . . . . .
Br2 Br 0.36628(5) 0.47903(5) 0.22695(3) 0.0201 1.0000 Uani . . . . . .
Br3 Br 0.71126(5) 0.65033(5) 0.18028(3) 0.0189 1.0000 Uani . . . . . .
Br4 Br 0.28362(5) 0.82142(5) 0.32885(3) 0.0209 1.0000 Uani . . . . . .
Br5 Br 0.65333(6) 1.02790(5) 0.28467(3) 0.0259 1.0000 Uani . . . . . .
Br6 Br 0.35651(6) 0.77645(5) 0.08009(3) 0.0238 1.0000 Uani . . . . . .
Br7 Br 0.89569(6) 1.31403(5) 0.15163(3) 0.0199 1.0000 Uani . . . . . .
Br8 Br 0.89768(6) 1.30727(5) 0.48454(3) 0.0208 1.0000 Uani . . . . . .
Br9 Br -0.12538(6) 0.79197(5) -0.02452(3) 0.0216 1.0000 Uani . . . . . .
Br10 Br 0.14702(6) 0.16762(5) 0.35492(3) 0.0264 1.0000 Uani . . . . . .
N1 N -0.1487(4) 0.3684(4) 0.3152(2) 0.0185 1.0000 Uani D . . . . .
N2 N 0.1579(4) 0.4614(4) 0.4116(2) 0.0173 1.0000 Uani D . . . . .
N3 N 0.8478(4) 1.0173(4) 0.0913(2) 0.0186 1.0000 Uani D . . . . .
N4 N 1.1552(4) 1.1009(4) 0.1836(2) 0.0202 1.0000 Uani D . . . . .
N5 N 0.4943(5) 1.0797(4) 0.4118(2) 0.0258 1.0000 Uani D . . . . .
N6 N 0.5755(4) 0.3819(4) 0.0600(2) 0.0193 1.0000 Uani D . . . . .
N7 N 1.0250(4) 0.9133(4) 0.4135(2) 0.0201 1.0000 Uani D . . . . .
N8 N 0.1107(4) 0.5285(4) 0.0968(2) 0.0197 1.0000 Uani D . . . . .
C9 C -0.0652(5) 0.4954(5) 0.3320(3) 0.0182 1.0000 Uani D . . . . .
C10 C 0.0849(5) 0.4963(5) 0.3395(3) 0.0212 1.0000 Uani D . . . . .
C11 C 0.3103(5) 0.4950(5) 0.4238(3) 0.0230 1.0000 Uani D . . . . .
C12 C -0.2975(5) 0.3758(5) 0.3025(3) 0.0207 1.0000 Uani D . . . . .
C13 C 0.9227(5) 0.9734(5) 0.1602(3) 0.0203 1.0000 Uani D . . . . .
C14 C 1.0719(6) 0.9736(5) 0.1650(3) 0.0220 1.0000 Uani D . . . . .
C15 C 1.3043(6) 1.0942(5) 0.1964(3) 0.0246 1.0000 Uani D . . . . .
C16 C 0.6981(6) 0.9905(5) 0.0830(3) 0.0268 1.0000 Uani D . . . . .
C17 C 0.5067(6) 1.2206(6) 0.4308(3) 0.0305 1.0000 Uani D . . . . .
C18 C 0.5471(6) 1.0070(5) 0.4745(3) 0.0263 1.0000 Uani D . . . . .
C19 C 0.4689(5) 0.4533(5) 0.0221(3) 0.0207 1.0000 Uani D . . . . .
C20 C 0.5201(6) 0.2788(5) 0.1004(3) 0.0249 1.0000 Uani D . . . . .
C21 C 0.9498(5) 0.9674(5) 0.4659(3) 0.0189 1.0000 Uani D . . . . .
C22 C 0.9346(5) 0.8435(5) 0.3441(3) 0.0206 1.0000 Uani D . . . . .
C23 C 0.0734(5) 0.5268(5) 0.0151(3) 0.0167 1.0000 Uani D . . . . .
C24 C 0.0588(6) 0.6265(5) 0.1381(3) 0.0228 1.0000 Uani D . . . . .
H91 H -0.081(3) 0.532(3) 0.3771(13) 0.022(2) 1.0000 Uiso D . . . . .
H92 H -0.097(2) 0.542(2) 0.2916(14) 0.022(2) 1.0000 Uiso D . . . . .
H101 H 0.124(2) 0.580(2) 0.3343(16) 0.025(2) 1.0000 Uiso D . . . . .
H102 H 0.096(3) 0.435(3) 0.3013(13) 0.026(2) 1.0000 Uiso D . . . . .
H111 H 0.357(3) 0.463(4) 0.4678(16) 0.036(2) 1.0000 Uiso D . . . . .
H112 H 0.337(3) 0.5871(19) 0.429(2) 0.035(2) 1.0000 Uiso D . . . . .
H113 H 0.337(3) 0.458(4) 0.3828(16) 0.035(2) 1.0000 Uiso D . . . . .
H123 H -0.350(3) 0.293(2) 0.288(2) 0.031(2) 1.0000 Uiso D . . . . .
H122 H -0.318(3) 0.412(4) 0.3468(14) 0.031(2) 1.0000 Uiso D . . . . .
H121 H -0.323(3) 0.427(3) 0.2635(17) 0.031(2) 1.0000 Uiso D . . . . .
H131 H 0.913(3) 1.029(3) 0.2012(12) 0.025(2) 1.0000 Uiso D . . . . .
H132 H 0.883(2) 0.888(2) 0.1617(16) 0.025(2) 1.0000 Uiso D . . . . .
H141 H 1.105(3) 0.924(2) 0.2044(14) 0.026(2) 1.0000 Uiso D . . . . .
H142 H 1.087(3) 0.940(3) 0.1188(13) 0.026(2) 1.0000 Uiso D . . . . .
H151 H 1.355(3) 1.178(2) 0.211(2) 0.037(2) 1.0000 Uiso D . . . . .
H152 H 1.322(3) 1.058(4) 0.1514(14) 0.037(2) 1.0000 Uiso D . . . . .
H153 H 1.328(3) 1.042(3) 0.2353(18) 0.037(2) 1.0000 Uiso D . . . . .
H163 H 0.651(3) 1.023(4) 0.0395(16) 0.039(2) 1.0000 Uiso D . . . . .
H162 H 0.675(3) 1.031(4) 0.1248(16) 0.039(2) 1.0000 Uiso D . . . . .
H161 H 0.666(3) 0.900(2) 0.079(2) 0.039(2) 1.0000 Uiso D . . . . .
H173 H 0.463(4) 1.257(3) 0.3877(14) 0.044(2) 1.0000 Uiso D . . . . .
H172 H 0.601(2) 1.255(3) 0.446(2) 0.045(2) 1.0000 Uiso D . . . . .
H171 H 0.462(4) 1.237(3) 0.4705(19) 0.045(2) 1.0000 Uiso D . . . . .
H181 H 0.634(2) 1.052(3) 0.5003(13) 0.030(2) 1.0000 Uiso D . . . . .
H182 H 0.560(3) 0.925(2) 0.4537(14) 0.030(2) 1.0000 Uiso D . . . . .
H191 H 0.436(3) 0.500(2) 0.0596(13) 0.025(2) 1.0000 Uiso D . . . . .
H192 H 0.397(2) 0.395(2) -0.0089(14) 0.025(2) 1.0000 Uiso D . . . . .
H203 H 0.591(3) 0.234(3) 0.123(2) 0.035(2) 1.0000 Uiso D . . . . .
H202 H 0.479(4) 0.313(3) 0.1381(18) 0.036(2) 1.0000 Uiso D . . . . .
H201 H 0.453(3) 0.220(3) 0.0662(14) 0.036(2) 1.0000 Uiso D . . . . .
H211 H 0.901(3) 1.028(2) 0.4411(13) 0.024(2) 1.0000 Uiso D . . . . .
H212 H 0.892(3) 0.899(2) 0.4794(14) 0.024(2) 1.0000 Uiso D . . . . .
H223 H 0.988(3) 0.804(3) 0.3149(16) 0.029(2) 1.0000 Uiso D . . . . .
H222 H 0.888(3) 0.903(2) 0.3172(16) 0.029(2) 1.0000 Uiso D . . . . .
H221 H 0.868(3) 0.782(3) 0.3574(15) 0.029(2) 1.0000 Uiso D . . . . .
H231 H 0.089(3) 0.613(2) 0.0028(14) 0.020(2) 1.0000 Uiso D . . . . .
H232 H 0.126(2) 0.475(3) -0.0067(13) 0.021(2) 1.0000 Uiso D . . . . .
H243 H 0.108(3) 0.636(3) 0.1880(12) 0.035(2) 1.0000 Uiso D . . . . .
H242 H 0.073(4) 0.704(2) 0.1169(18) 0.035(2) 1.0000 Uiso D . . . . .
H241 H -0.036(2) 0.600(3) 0.135(2) 0.035(2) 1.0000 Uiso D . . . . .
H11 H -0.126(2) 0.325(2) 0.3526(13) 0.028(2) 1.0000 Uiso D . . . . .
H12 H -0.133(2) 0.327(2) 0.2764(13) 0.027(2) 1.0000 Uiso D . . . . .
H21 H 0.129(2) 0.498(3) 0.4479(12) 0.026(2) 1.0000 Uiso D . . . . .
H22 H 0.139(2) 0.3787(19) 0.4125(15) 0.026(2) 1.0000 Uiso D . . . . .
H31 H 0.873(2) 1.0995(19) 0.0918(15) 0.029(2) 1.0000 Uiso D . . . . .
H32 H 0.870(2) 0.980(3) 0.0524(12) 0.029(2) 1.0000 Uiso D . . . . .
H41 H 1.131(2) 1.145(2) 0.1472(13) 0.031(2) 1.0000 Uiso D . . . . .
H42 H 1.138(2) 1.140(2) 0.2225(13) 0.031(2) 1.0000 Uiso D . . . . .
H51 H 0.541(3) 1.068(2) 0.3776(14) 0.039(2) 1.0000 Uiso D . . . . .
H52 H 0.410(2) 1.046(2) 0.3915(16) 0.039(2) 1.0000 Uiso D . . . . .
H61 H 0.642(2) 0.434(2) 0.0903(13) 0.028(2) 1.0000 Uiso D . . . . .
H62 H 0.619(3) 0.350(2) 0.0275(13) 0.028(2) 1.0000 Uiso D . . . . .
H71 H 1.083(3) 0.976(2) 0.4017(14) 0.030(2) 1.0000 Uiso D . . . . .
H72 H 1.075(3) 0.861(2) 0.4371(12) 0.030(2) 1.0000 Uiso D . . . . .
H81 H 0.200(2) 0.533(3) 0.1126(13) 0.029(2) 1.0000 Uiso D . . . . .
H82 H 0.080(3) 0.4518(19) 0.1078(13) 0.028(2) 1.0000 Uiso D . . . . .


_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.8825(6)

loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 . Br1 . 2.7985(6) yes
Sn1 . Br2 . 2.8379(6) yes
Sn1 . Br3 . 2.9479(7) yes
Sn1 . Br4 . 3.1255(7) yes
Sn1 . Br6 . 3.3447(7) yes
Sn1 . Br5 . 3.2604(7) yes
N1 . C9 . 1.473(6) yes
N1 . C12 . 1.499(7) yes
N1 . H11 . 0.873(19) no
N1 . H12 . 0.876(19) no
N2 . C10 . 1.482(6) yes
N2 . C11 . 1.510(7) yes
N2 . H21 . 0.884(19) no
N2 . H22 . 0.881(19) no
N3 . C13 . 1.482(6) yes
N3 . C16 . 1.486(7) yes
N3 . H31 . 0.881(19) no
N3 . H32 . 0.890(19) no
N4 . C14 . 1.476(7) yes
N4 . C15 . 1.500(7) yes
N4 . H41 . 0.865(19) no
N4 . H42 . 0.876(19) no
N5 . C17 . 1.505(7) yes
N5 . C18 . 1.490(7) yes
N5 . H51 . 0.890(19) no
N5 . H52 . 0.875(19) no
N6 . C19 . 1.492(6) yes
N6 . C20 . 1.496(7) yes
N6 . H61 . 0.883(19) no
N6 . H62 . 0.900(19) no
N7 . C21 . 1.500(6) yes
N7 . C22 . 1.490(6) yes
N7 . H71 . 0.903(19) no
N7 . H72 . 0.888(19) no
N8 . C23 . 1.482(6) yes
N8 . C24 . 1.479(6) yes
N8 . H81 . 0.886(19) no
N8 . H82 . 0.892(19) no
C9 . C10 . 1.506(7) yes
C9 . H91 . 0.958(19) no
C9 . H92 . 0.954(19) no
C10 . H101 . 0.953(19) no
C10 . H102 . 0.967(19) no
C11 . H111 . 0.962(19) no
C11 . H112 . 0.977(19) no
C11 . H113 . 0.948(19) no
C12 . H123 . 0.952(19) no
C12 . H122 . 0.962(19) no
C12 . H121 . 0.954(19) no
C13 . C14 . 1.505(7) yes
C13 . H131 . 0.960(19) no
C13 . H132 . 0.950(19) no
C14 . H141 . 0.962(19) no
C14 . H142 . 0.960(19) no
C15 . H151 . 0.956(19) no
C15 . H152 . 0.961(19) no
C15 . H153 . 0.957(19) no
C16 . H163 . 0.954(19) no
C16 . H162 . 0.956(19) no
C16 . H161 . 0.969(19) no
C17 . H173 . 0.964(19) no
C17 . H172 . 0.958(19) no
C17 . H171 . 0.966(19) no
C18 . C18 2_676 1.493(11) yes
C18 . H181 . 0.953(19) no
C18 . H182 . 0.976(19) no
C19 . C19 2_665 1.499(10) yes
C19 . H191 . 0.974(19) no
C19 . H192 . 0.947(19) no
C20 . H203 . 0.959(19) no
C20 . H202 . 0.965(19) no
C20 . H201 . 0.949(19) no
C21 . C21 2_776 1.499(10) yes
C21 . H211 . 0.951(19) no
C21 . H212 . 0.957(19) no
C22 . H223 . 0.964(19) no
C22 . H222 . 0.952(19) no
C22 . H221 . 0.967(19) no
C23 . C23 2_565 1.494(9) yes
C23 . H231 . 0.962(19) no
C23 . H232 . 0.950(19) no
C24 . H243 . 0.944(19) no
C24 . H242 . 0.947(19) no
C24 . H241 . 0.964(19) no

loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Br1 . Sn1 . Br2 . 88.676(19) yes
Br1 . Sn1 . Br3 . 95.392(19) yes
Br2 . Sn1 . Br3 . 88.541(19) yes
Br1 . Sn1 . Br4 . 85.693(19) yes
Br2 . Sn1 . Br4 . 91.524(19) yes
Br3 . Sn1 . Br4 . 178.91(2) yes
Br1 . Sn1 . Br6 . 176.22(2) yes
Br2 . Sn1 . Br6 . 88.611(18) yes
Br3 . Sn1 . Br6 . 81.906(17) yes
Br4 . Sn1 . Br6 . 97.012(18) yes
Br1 . Sn1 . Br5 . 92.123(19) yes
Br2 . Sn1 . Br5 . 177.75(2) yes
Br3 . Sn1 . Br5 . 93.475(19) yes
Br4 . Sn1 . Br5 . 86.442(17) yes
Br6 . Sn1 . Br5 . 90.686(18) yes
C9 . N1 . C12 . 111.7(4) yes
C9 . N1 . H11 . 108.5(16) no
C12 . N1 . H11 . 108.8(16) no
C9 . N1 . H12 . 111.4(16) no
C12 . N1 . H12 . 109.5(16) no
H11 . N1 . H12 . 106.8(17) no
C10 . N2 . C11 . 112.1(4) yes
C10 . N2 . H21 . 109.8(16) no
C11 . N2 . H21 . 111.0(16) no
C10 . N2 . H22 . 109.1(16) no
C11 . N2 . H22 . 107.6(16) no
H21 . N2 . H22 . 107.1(17) no
C13 . N3 . C16 . 111.9(4) yes
C13 . N3 . H31 . 109.4(16) no
C16 . N3 . H31 . 109.3(16) no
C13 . N3 . H32 . 109.5(16) no
C16 . N3 . H32 . 109.8(16) no
H31 . N3 . H32 . 106.9(17) no
C14 . N4 . C15 . 111.7(4) yes
C14 . N4 . H41 . 108.1(16) no
C15 . N4 . H41 . 109.9(16) no
C14 . N4 . H42 . 110.3(16) no
C15 . N4 . H42 . 110.4(16) no
H41 . N4 . H42 . 106.2(17) no
C17 . N5 . C18 . 115.6(4) yes
C17 . N5 . H51 . 107.5(16) no
C18 . N5 . H51 . 107.3(16) no
C17 . N5 . H52 . 111.2(16) no
C18 . N5 . H52 . 108.4(16) no
H51 . N5 . H52 . 106.5(17) no
C19 . N6 . C20 . 112.8(4) yes
C19 . N6 . H61 . 110.4(16) no
C20 . N6 . H61 . 110.6(16) no
C19 . N6 . H62 . 110.8(16) no
C20 . N6 . H62 . 110.0(16) no
H61 . N6 . H62 . 101.7(17) no
C21 . N7 . C22 . 113.9(4) yes
C21 . N7 . H71 . 109.8(16) no
C22 . N7 . H71 . 109.2(16) no
C21 . N7 . H72 . 107.8(16) no
C22 . N7 . H72 . 109.0(16) no
H71 . N7 . H72 . 107.0(17) no
C23 . N8 . C24 . 115.2(4) yes
C23 . N8 . H81 . 110.0(16) no
C24 . N8 . H81 . 111.4(16) no
C23 . N8 . H82 . 107.4(16) no
C24 . N8 . H82 . 109.5(16) no
H81 . N8 . H82 . 102.5(17) no
N1 . C9 . C10 . 114.8(4) yes
N1 . C9 . H91 . 106.9(15) no
C10 . C9 . H91 . 110.2(15) no
N1 . C9 . H92 . 106.2(15) no
C10 . C9 . H92 . 108.1(15) no
H91 . C9 . H92 . 110.8(17) no
C9 . C10 . N2 . 114.5(4) yes
C9 . C10 . H101 . 107.5(15) no
N2 . C10 . H101 . 107.7(15) no
C9 . C10 . H102 . 107.8(15) no
N2 . C10 . H102 . 107.2(15) no
H101 . C10 . H102 . 112.3(17) no
N2 . C11 . H111 . 111.4(16) no
N2 . C11 . H112 . 110.4(16) no
H111 . C11 . H112 . 108.2(17) no
N2 . C11 . H113 . 108.8(16) no
H111 . C11 . H113 . 107.9(17) no
H112 . C11 . H113 . 110.2(17) no
N1 . C12 . H123 . 110.3(16) no
N1 . C12 . H122 . 110.5(16) no
H123 . C12 . H122 . 109.4(17) no
N1 . C12 . H121 . 109.8(16) no
H123 . C12 . H121 . 108.0(17) no
H122 . C12 . H121 . 108.9(17) no
N3 . C13 . C14 . 114.7(4) yes
N3 . C13 . H131 . 107.5(15) no
C14 . C13 . H131 . 108.5(15) no
N3 . C13 . H132 . 107.4(15) no
C14 . C13 . H132 . 106.8(15) no
H131 . C13 . H132 . 112.2(17) no
C13 . C14 . N4 . 113.9(4) yes
C13 . C14 . H141 . 107.5(15) no
N4 . C14 . H141 . 106.7(16) no
C13 . C14 . H142 . 111.2(15) no
N4 . C14 . H142 . 106.3(15) no
H141 . C14 . H142 . 111.2(17) no
N4 . C15 . H151 . 109.2(16) no
N4 . C15 . H152 . 108.7(16) no
H151 . C15 . H152 . 110.8(17) no
N4 . C15 . H153 . 108.5(16) no
H151 . C15 . H153 . 109.4(17) no
H152 . C15 . H153 . 110.2(17) no
N3 . C16 . H163 . 110.8(16) no
N3 . C16 . H162 . 109.6(16) no
H163 . C16 . H162 . 107.9(17) no
N3 . C16 . H161 . 111.4(16) no
H163 . C16 . H161 . 107.9(17) no
H162 . C16 . H161 . 109.1(17) no
N5 . C17 . H173 . 108.9(16) no
N5 . C17 . H172 . 108.2(16) no
H173 . C17 . H172 . 110.7(17) no
N5 . C17 . H171 . 109.6(16) no
H173 . C17 . H171 . 108.9(17) no
H172 . C17 . H171 . 110.5(17) no
C18 2_676 C18 . N5 . 111.4(6) yes
C18 2_676 C18 . H181 . 110.6(16) no
N5 . C18 . H181 . 107.4(16) no
C18 2_676 C18 . H182 . 111.5(15) no
N5 . C18 . H182 . 107.9(16) no
H181 . C18 . H182 . 107.8(17) no
C19 2_665 C19 . N6 . 109.0(5) yes
C19 2_665 C19 . H191 . 108.9(16) no
N6 . C19 . H191 . 108.7(16) no
C19 2_665 C19 . H192 . 111.1(16) no
N6 . C19 . H192 . 109.1(15) no
H191 . C19 . H192 . 110.1(17) no
N6 . C20 . H203 . 110.2(16) no
N6 . C20 . H202 . 111.0(16) no
H203 . C20 . H202 . 109.4(17) no
N6 . C20 . H201 . 109.3(16) no
H203 . C20 . H201 . 107.9(17) no
H202 . C20 . H201 . 109.0(17) no
N7 . C21 . C21 2_776 109.2(5) yes
N7 . C21 . H211 . 106.8(16) no
C21 2_776 C21 . H211 . 109.5(16) no
N7 . C21 . H212 . 108.2(16) no
C21 2_776 C21 . H212 . 109.3(16) no
H211 . C21 . H212 . 113.8(17) no
N7 . C22 . H223 . 110.1(16) no
N7 . C22 . H222 . 107.9(16) no
H223 . C22 . H222 . 110.3(17) no
N7 . C22 . H221 . 108.5(16) no
H223 . C22 . H221 . 111.7(17) no
H222 . C22 . H221 . 108.2(17) no
C23 2_565 C23 . N8 . 110.7(5) yes
C23 2_565 C23 . H231 . 108.8(15) no
N8 . C23 . H231 . 108.5(15) no
C23 2_565 C23 . H232 . 107.9(15) no
N8 . C23 . H232 . 109.9(15) no
H231 . C23 . H232 . 111.1(17) no
N8 . C24 . H243 . 108.4(16) no
N8 . C24 . H242 . 108.1(16) no
H243 . C24 . H242 . 109.9(17) no
N8 . C24 . H241 . 109.3(16) no
H243 . C24 . H241 . 109.8(17) no
H242 . C24 . H241 . 111.4(17) no

####################################################################### 
# 
# 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_Pr2SbCl5
_database_code_depnum_ccdc_archive 'CCDC 1538293'
_audit_update_record             
;
2017-03-15 deposited with the CCDC.
2017-11-21 downloaded from the CCDC.
;
_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_cell_length_a                   8.75618(18)
_cell_length_b                   27.2439(5)
_cell_length_c                   10.64297(18)
_cell_angle_alpha                90
_cell_angle_beta                 97.3536(17)
_cell_angle_gamma                90
_cell_volume                     2518.02(8)
_cell_formula_units_Z            4

# Given Formula = C18 H40 Cl5 N2 Sb1 
# Dc =      1.54 Fooo =   1192.00 Mu =     16.33 M =    583.54
# Found Formula = C18 H40 Cl5 N2 Sb1 
# Dc =      1.54 FOOO =   1192.00 Mu =     16.33 M =    583.54

_chemical_formula_sum            'C18 H40 Cl5 N2 Sb1'
_chemical_formula_moiety         'C18 H40 Cl5 N2 Sb1'
_chemical_compound_source        ?
_chemical_formula_weight         583.54

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  ?

loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Sb -0.5866 1.5461 19.6418 5.3034 19.0455 0.4607 5.0371 27.9074 2.6827 75.2825
4.5909 'International Tables Vol C 4.2.6.8 and 6.1.1.4'

_cell_measurement_reflns_used    8177
_cell_measurement_theta_min      3
_cell_measurement_theta_max      32
_cell_measurement_temperature    100

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_size_min          0.270
_exptl_crystal_size_mid          0.403
_exptl_crystal_size_max          0.507

_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1192
_exptl_absorpt_coefficient_mu    1.633

# Sheldrick geometric approximatio 0.52 0.64 
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_absorpt_correction_T_min  0.52
_exptl_absorpt_correction_T_max  0.64
_diffrn_measurement_device_type  'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       'φ & ω scans'

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'Xcalibur, (Oxford Diffraction, 2002)'
_computing_cell_refinement       'CrysAlisPro, (Agilent, 2011)'
_computing_data_reduction        'CrysAlisPro, (Agilent, 2011)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      100
_diffrn_reflns_number            32635
_reflns_number_total             8177
_diffrn_reflns_av_R_equivalents  0.055
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 8177 
# Theoretical number of reflections is about 17459 


_diffrn_reflns_theta_min         2.782
_diffrn_reflns_theta_max         31.981
_diffrn_measured_fraction_theta_max 0.938

_diffrn_reflns_theta_full        28.783
_diffrn_measured_fraction_theta_full 0.995


_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_reflns_limit_h_min              -12
_reflns_limit_h_max              12
_reflns_limit_k_min              0
_reflns_limit_k_max              39
_reflns_limit_l_min              0
_reflns_limit_l_max              15

_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom,iterative
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.90
_refine_diff_density_max         1.12


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         8159
_refine_ls_number_restraints     174
_refine_ls_number_parameters     395
_oxford_refine_ls_R_factor_ref   0.0418
_refine_ls_wR_factor_ref         0.0542
_refine_ls_goodness_of_fit_ref   0.9984
_refine_ls_shift/su_max          0.0042682
_refine_ls_shift/su_mean         0.0000648


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        8161
_refine_ls_R_factor_all          0.0418
_refine_ls_wR_factor_all         0.0542

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                7386
_refine_ls_R_factor_gt           0.0371
_refine_ls_wR_factor_gt          0.0529

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    mixed #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 190. 222. 74.2 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint

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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Sb1 Sb 0.69469(2) 0.617573(6) 0.704002(16) 0.0146 1.0000 Uani . . . . . .
Cl1 Cl 0.90348(7) 0.64305(2) 0.85508(6) 0.0197 1.0000 Uani . . . . . .
Cl2 Cl 0.89245(8) 0.60436(2) 0.54405(6) 0.0223 1.0000 Uani . . . . . .
Cl3 Cl 0.65685(8) 0.70796(2) 0.62752(7) 0.0224 1.0000 Uani . . . . . .
Cl4 Cl 0.51366(7) 0.63457(2) 0.87714(6) 0.0209 1.0000 Uani . . . . . .
Cl5 Cl 0.74205(7) 0.52839(2) 0.79729(6) 0.0191 1.0000 Uani . . . . . .
N1 N 0.6923(2) 0.76716(8) 1.0395(2) 0.0162 1.0000 Uani D . . . . .
C11 C 0.5231(3) 0.76010(11) 1.0037(3) 0.0231 1.0000 Uani D . . . . .
C12 C 0.7217(3) 0.80458(10) 1.1450(3) 0.0202 1.0000 Uani D . . . . .
C13 C 0.6880(3) 0.77630(11) 1.2627(3) 0.0247 1.0000 Uani D . . . . .
C14 C 0.7197(3) 0.72199(10) 1.2350(3) 0.0227 1.0000 Uani D . . . . .
C15 C 0.7627(3) 0.72097(9) 1.1011(3) 0.0209 1.0000 Uani D . . . . .
C16 C 0.7709(3) 0.77882(10) 0.9252(3) 0.0197 1.0000 Uani D . . . . .
C17 C 0.6976(3) 0.81971(10) 0.8401(2) 0.0196 1.0000 Uani D . . . . .
C18 C 0.8007(3) 0.83001(10) 0.7377(3) 0.0215 1.0000 Uani D . . . . .
C19 C 0.7305(4) 0.86599(13) 0.6370(3) 0.0317 1.0000 Uani D . . . . .
N2 N 0.2121(2) 0.49319(8) 0.8262(2) 0.0163 1.0000 Uani D . . . . .
C21 C 0.2050(4) 0.53918(10) 0.9020(3) 0.0229 1.0000 Uani D . . . . .
C22 C 0.3609(3) 0.46566(10) 0.8617(2) 0.0190 1.0000 Uani D . . . . .
C23 C 0.3271(3) 0.41422(9) 0.8082(3) 0.0203 1.0000 Uani D . . . . .
C24 C 0.1537(3) 0.40672(9) 0.8153(3) 0.0191 1.0000 Uani D . . . . .
C25 C 0.0947(3) 0.45585(9) 0.8581(2) 0.0177 1.0000 Uani D . . . . .
C26 C 0.1813(3) 0.50469(9) 0.6859(2) 0.0178 1.0000 Uani D . . . . .
C27 C 0.3009(3) 0.53776(10) 0.6377(2) 0.0192 1.0000 Uani D . . . . .
C28 C 0.2732(3) 0.54086(10) 0.4939(2) 0.0193 1.0000 Uani D . . . . .
C29 C 0.4049(3) 0.56648(10) 0.4405(3) 0.0234 1.0000 Uani D . . . . .
H113 H 0.509(3) 0.7376(8) 0.935(2) 0.0351(19) 1.0000 Uiso D . . . . .
H112 H 0.477(2) 0.7908(7) 0.980(2) 0.0351(19) 1.0000 Uiso D . . . . .
H111 H 0.479(3) 0.7466(9) 1.0733(19) 0.0352(19) 1.0000 Uiso D . . . . .
H121 H 0.831(2) 0.8140(8) 1.152(2) 0.0244(19) 1.0000 Uiso D . . . . .
H122 H 0.654(2) 0.8322(7) 1.128(2) 0.0245(19) 1.0000 Uiso D . . . . .
H131 H 0.753(2) 0.7877(8) 1.3376(18) 0.0302(19) 1.0000 Uiso D . . . . .
H132 H 0.582(2) 0.7806(8) 1.275(2) 0.0299(19) 1.0000 Uiso D . . . . .
H141 H 0.802(2) 0.7088(8) 1.2949(19) 0.0300(19) 1.0000 Uiso D . . . . .
H142 H 0.630(2) 0.7032(8) 1.238(2) 0.0290(19) 1.0000 Uiso D . . . . .
H151 H 0.875(2) 0.7222(8) 1.098(2) 0.0261(19) 1.0000 Uiso D . . . . .
H152 H 0.721(3) 0.6922(7) 1.0561(19) 0.0262(19) 1.0000 Uiso D . . . . .
H161 H 0.874(2) 0.7873(8) 0.9575(19) 0.0255(19) 1.0000 Uiso D . . . . .
H162 H 0.776(3) 0.7491(7) 0.8743(19) 0.0256(19) 1.0000 Uiso D . . . . .
H171 H 0.685(3) 0.8493(7) 0.8905(19) 0.0241(19) 1.0000 Uiso D . . . . .
H172 H 0.595(2) 0.8093(8) 0.800(2) 0.0251(19) 1.0000 Uiso D . . . . .
H181 H 0.894(2) 0.8437(8) 0.7791(19) 0.0267(19) 1.0000 Uiso D . . . . .
H182 H 0.822(3) 0.7997(7) 0.6953(19) 0.0255(19) 1.0000 Uiso D . . . . .
H193 H 0.803(3) 0.8713(10) 0.576(2) 0.048(2) 1.0000 Uiso D . . . . .
H192 H 0.708(3) 0.8979(8) 0.677(2) 0.048(2) 1.0000 Uiso D . . . . .
H191 H 0.635(3) 0.8521(9) 0.595(2) 0.049(2) 1.0000 Uiso D . . . . .
H213 H 0.106(2) 0.5555(8) 0.874(2) 0.0341(19) 1.0000 Uiso D . . . . .
H212 H 0.287(2) 0.5599(8) 0.884(2) 0.0349(19) 1.0000 Uiso D . . . . .
H211 H 0.215(3) 0.5315(8) 0.9906(17) 0.0343(19) 1.0000 Uiso D . . . . .
H221 H 0.385(2) 0.4643(8) 0.9535(16) 0.0226(19) 1.0000 Uiso D . . . . .
H222 H 0.441(2) 0.4827(7) 0.827(2) 0.0221(19) 1.0000 Uiso D . . . . .
H231 H 0.389(2) 0.3910(7) 0.8595(19) 0.0250(19) 1.0000 Uiso D . . . . .
H232 H 0.350(2) 0.4124(8) 0.7224(17) 0.0256(19) 1.0000 Uiso D . . . . .
H241 H 0.133(2) 0.3817(7) 0.8759(19) 0.0244(19) 1.0000 Uiso D . . . . .
H242 H 0.103(2) 0.3982(8) 0.7310(17) 0.0255(19) 1.0000 Uiso D . . . . .
H251 H 0.093(3) 0.4563(8) 0.9484(16) 0.0233(19) 1.0000 Uiso D . . . . .
H252 H -0.005(2) 0.4646(7) 0.818(2) 0.0222(19) 1.0000 Uiso D . . . . .
H261 H 0.081(2) 0.5196(8) 0.671(2) 0.0214(19) 1.0000 Uiso D . . . . .
H262 H 0.179(3) 0.4739(7) 0.6399(19) 0.0215(19) 1.0000 Uiso D . . . . .
H271 H 0.294(3) 0.5707(7) 0.674(2) 0.0233(19) 1.0000 Uiso D . . . . .
H272 H 0.403(2) 0.5257(8) 0.661(2) 0.0239(19) 1.0000 Uiso D . . . . .
H281 H 0.177(2) 0.5583(8) 0.469(2) 0.0241(19) 1.0000 Uiso D . . . . .
H282 H 0.265(3) 0.5069(7) 0.459(2) 0.0239(19) 1.0000 Uiso D . . . . .
H293 H 0.381(3) 0.5684(9) 0.3490(17) 0.0344(19) 1.0000 Uiso D . . . . .
H292 H 0.412(3) 0.5994(7) 0.474(2) 0.0339(19) 1.0000 Uiso D . . . . .
H291 H 0.502(2) 0.5502(8) 0.465(2) 0.0344(19) 1.0000 Uiso D . . . . .


loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sb1 . Cl1 . 2.3784(6) yes
Sb1 . Cl2 . 2.6039(7) yes
Sb1 . Cl3 . 2.6013(7) yes
Sb1 . Cl4 . 2.6212(7) yes
Sb1 . Cl5 . 2.6374(6) yes
N1 . C11 . 1.495(3) yes
N1 . C12 . 1.515(3) yes
N1 . C15 . 1.513(3) yes
N1 . C16 . 1.506(3) yes
C11 . H113 . 0.952(17) no
C11 . H112 . 0.948(17) no
C11 . H111 . 0.952(17) no
C12 . C13 . 1.531(4) yes
C12 . H121 . 0.982(17) no
C12 . H122 . 0.960(17) no
C13 . C14 . 1.541(4) yes
C13 . H131 . 0.969(17) no
C13 . H132 . 0.959(17) no
C14 . C15 . 1.520(4) yes
C14 . H141 . 0.966(17) no
C14 . H142 . 0.938(17) no
C15 . H151 . 0.984(17) no
C15 . H152 . 0.965(17) no
C16 . C17 . 1.524(4) yes
C16 . H161 . 0.955(17) no
C16 . H162 . 0.979(17) no
C17 . C18 . 1.527(4) yes
C17 . H171 . 0.981(17) no
C17 . H172 . 0.987(17) no
C18 . C19 . 1.523(4) yes
C18 . H181 . 0.957(17) no
C18 . H182 . 0.971(17) no
C19 . H193 . 0.977(18) no
C19 . H192 . 1.000(18) no
C19 . H191 . 0.975(18) no
N2 . C21 . 1.496(3) yes
N2 . C22 . 1.509(3) yes
N2 . C25 . 1.516(3) yes
N2 . C26 . 1.515(3) yes
C21 . H213 . 0.987(17) no
C21 . H212 . 0.951(17) no
C21 . H211 . 0.959(17) no
C22 . C23 . 1.527(4) yes
C22 . H221 . 0.974(17) no
C22 . H222 . 0.957(17) no
C23 . C24 . 1.543(4) yes
C23 . H231 . 0.957(17) no
C23 . H232 . 0.962(17) no
C24 . C25 . 1.525(4) yes
C24 . H241 . 0.971(17) no
C24 . H242 . 0.977(17) no
C25 . H251 . 0.963(17) no
C25 . H252 . 0.949(17) no
C26 . C27 . 1.520(4) yes
C26 . H261 . 0.960(17) no
C26 . H262 . 0.971(17) no
C27 . C28 . 1.520(4) yes
C27 . H271 . 0.981(17) no
C27 . H272 . 0.955(17) no
C28 . C29 . 1.519(4) yes
C28 . H281 . 0.972(17) no
C28 . H282 . 0.996(17) no
C29 . H293 . 0.971(17) no
C29 . H292 . 0.965(17) no
C29 . H291 . 0.967(17) no

loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
Cl1 . Sb1 . Cl2 . 87.96(2) yes
Cl1 . Sb1 . Cl3 . 89.51(2) yes
Cl2 . Sb1 . Cl3 . 89.71(2) yes
Cl1 . Sb1 . Cl4 . 87.41(2) yes
Cl2 . Sb1 . Cl4 . 175.28(2) yes
Cl3 . Sb1 . Cl4 . 89.34(2) yes
Cl1 . Sb1 . Cl5 . 86.80(2) yes
Cl2 . Sb1 . Cl5 . 91.90(2) yes
Cl3 . Sb1 . Cl5 . 175.92(2) yes
Cl4 . Sb1 . Cl5 . 88.75(2) yes
C11 . N1 . C12 . 110.1(2) yes
C11 . N1 . C15 . 109.8(2) yes
C12 . N1 . C15 . 102.55(19) yes
C11 . N1 . C16 . 111.2(2) yes
C12 . N1 . C16 . 113.9(2) yes
C15 . N1 . C16 . 108.8(2) yes
N1 . C11 . H113 . 107.6(14) no
N1 . C11 . H112 . 109.4(14) no
H113 . C11 . H112 . 111.0(15) no
N1 . C11 . H111 . 109.8(14) no
H113 . C11 . H111 . 109.2(15) no
H112 . C11 . H111 . 109.8(15) no
N1 . C12 . C13 . 103.6(2) yes
N1 . C12 . H121 . 107.4(13) no
C13 . C12 . H121 . 111.2(13) no
N1 . C12 . H122 . 110.3(13) no
C13 . C12 . H122 . 111.5(13) no
H121 . C12 . H122 . 112.3(15) no
C12 . C13 . C14 . 105.6(2) yes
C12 . C13 . H131 . 111.0(13) no
C14 . C13 . H131 . 111.3(13) no
C12 . C13 . H132 . 109.9(13) no
C14 . C13 . H132 . 110.1(13) no
H131 . C13 . H132 . 109.0(15) no
C13 . C14 . C15 . 105.6(2) yes
C13 . C14 . H141 . 111.6(13) no
C15 . C14 . H141 . 111.1(13) no
C13 . C14 . H142 . 110.2(13) no
C15 . C14 . H142 . 109.4(13) no
H141 . C14 . H142 . 108.8(15) no
C14 . C15 . N1 . 104.8(2) yes
C14 . C15 . H151 . 113.3(13) no
N1 . C15 . H151 . 108.1(13) no
C14 . C15 . H152 . 111.0(13) no
N1 . C15 . H152 . 110.8(13) no
H151 . C15 . H152 . 108.9(15) no
N1 . C16 . C17 . 115.6(2) yes
N1 . C16 . H161 . 105.6(13) no
C17 . C16 . H161 . 110.1(13) no
N1 . C16 . H162 . 109.2(13) no
C17 . C16 . H162 . 108.8(12) no
H161 . C16 . H162 . 107.1(15) no
C16 . C17 . C18 . 108.4(2) yes
C16 . C17 . H171 . 110.1(12) no
C18 . C17 . H171 . 110.8(13) no
C16 . C17 . H172 . 109.8(13) no
C18 . C17 . H172 . 109.3(13) no
H171 . C17 . H172 . 108.4(15) no
C17 . C18 . C19 . 113.5(2) yes
C17 . C18 . H181 . 107.1(13) no
C19 . C18 . H181 . 108.5(13) no
C17 . C18 . H182 . 110.2(13) no
C19 . C18 . H182 . 107.7(13) no
H181 . C18 . H182 . 109.8(15) no
C18 . C19 . H193 . 109.0(14) no
C18 . C19 . H192 . 110.0(14) no
H193 . C19 . H192 . 109.7(16) no
C18 . C19 . H191 . 108.7(14) no
H193 . C19 . H191 . 110.3(16) no
H192 . C19 . H191 . 109.2(16) no
C21 . N2 . C22 . 112.0(2) yes
C21 . N2 . C25 . 111.4(2) yes
C22 . N2 . C25 . 101.48(19) yes
C21 . N2 . C26 . 110.13(19) yes
C22 . N2 . C26 . 112.8(2) yes
C25 . N2 . C26 . 108.64(19) yes
N2 . C21 . H213 . 107.9(13) no
N2 . C21 . H212 . 107.6(14) no
H213 . C21 . H212 . 109.1(15) no
N2 . C21 . H211 . 110.1(13) no
H213 . C21 . H211 . 111.3(15) no
H212 . C21 . H211 . 110.8(15) no
N2 . C22 . C23 . 104.1(2) yes
N2 . C22 . H221 . 109.7(13) no
C23 . C22 . H221 . 110.2(12) no
N2 . C22 . H222 . 108.5(13) no
C23 . C22 . H222 . 114.8(13) no
H221 . C22 . H222 . 109.4(14) no
C22 . C23 . C24 . 104.4(2) yes
C22 . C23 . H231 . 109.1(13) no
C24 . C23 . H231 . 111.8(13) no
C22 . C23 . H232 . 110.2(13) no
C24 . C23 . H232 . 111.5(13) no
H231 . C23 . H232 . 109.8(15) no
C23 . C24 . C25 . 105.8(2) yes
C23 . C24 . H241 . 113.0(12) no
C25 . C24 . H241 . 108.6(13) no
C23 . C24 . H242 . 108.9(13) no
C25 . C24 . H242 . 110.5(13) no
H241 . C24 . H242 . 109.9(14) no
C24 . C25 . N2 . 104.9(2) yes
C24 . C25 . H251 . 111.1(13) no
N2 . C25 . H251 . 108.1(13) no
C24 . C25 . H252 . 114.2(13) no
N2 . C25 . H252 . 109.8(13) no
H251 . C25 . H252 . 108.6(15) no
N2 . C26 . C27 . 114.3(2) yes
N2 . C26 . H261 . 107.3(13) no
C27 . C26 . H261 . 110.2(12) no
N2 . C26 . H262 . 107.9(12) no
C27 . C26 . H262 . 108.3(12) no
H261 . C26 . H262 . 108.7(15) no
C26 . C27 . C28 . 110.2(2) yes
C26 . C27 . H271 . 109.4(13) no
C28 . C27 . H271 . 109.6(13) no
C26 . C27 . H272 . 111.9(13) no
C28 . C27 . H272 . 107.4(13) no
H271 . C27 . H272 . 108.3(15) no
C27 . C28 . C29 . 111.8(2) yes
C27 . C28 . H281 . 108.8(13) no
C29 . C28 . H281 . 110.2(13) no
C27 . C28 . H282 . 108.6(12) no
C29 . C28 . H282 . 108.2(12) no
H281 . C28 . H282 . 109.2(15) no
C28 . C29 . H293 . 109.0(13) no
C28 . C29 . H292 . 107.7(13) no
H293 . C29 . H292 . 108.4(15) no
C28 . C29 . H291 . 112.0(13) no
H293 . C29 . H291 . 110.9(15) no
H292 . C29 . H291 . 108.6(15) no

####################################################################### 
# 
# 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_ma12a
_database_code_depnum_ccdc_archive 'CCDC 1580794'
_audit_update_record             
;
2017-10-19 deposited with the CCDC.
2017-11-21 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ' I6 Sn, 4(C4 H14 N2), 4(I)'
_chemical_formula_sum            'C16 H56 I10 N8 Sn'
_chemical_formula_weight         1748.37

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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.7464(7)
_cell_length_b                   10.8924(7)
_cell_length_c                   11.1796(7)
_cell_angle_alpha                64.2658(7)
_cell_angle_beta                 80.1825(7)
_cell_angle_gamma                72.8331(7)
_cell_volume                     1124.94(12)
_cell_formula_units_Z            1
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9499
_cell_measurement_theta_min      2.27
_cell_measurement_theta_max      29.23

_exptl_crystal_description       irregular
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.581
_exptl_crystal_F_000             788
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.083
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.069
_exptl_absorpt_coefficient_mu    7.448
_shelx_estimated_absorpt_T_min   0.577
_shelx_estimated_absorpt_T_max   0.627
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.5505
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14019
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.986
_diffrn_reflns_theta_max         29.408
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.920
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.920
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.920
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5710
_reflns_number_gt                5309
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 ? 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0132P)²+0.2315P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.00028(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         5710
_refine_ls_number_parameters     165
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.0155
_refine_ls_wR_factor_ref         0.0349
_refine_ls_wR_factor_gt          0.0341
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.5313(2) 0.5410(2) 0.4337(2) 0.0167(5) Uani 1 1 d . . . . .
H1A H 0.5665 0.6111 0.4421 0.020 Uiso 1 1 calc R U . . .
H1B H 0.6044 0.4759 0.4073 0.020 Uiso 1 1 calc R U . . .
C2 C 0.4895(2) 0.6867(3) 0.1950(2) 0.0210(5) Uani 1 1 d . . . . .
H2A H 0.5322 0.7540 0.1967 0.031 Uiso 1 1 calc R U . . .
H2B H 0.4203 0.7370 0.1313 0.031 Uiso 1 1 calc R U . . .
H2C H 0.5538 0.6171 0.1682 0.031 Uiso 1 1 calc R U . . .
C3 C 0.9288(2) 0.5307(2) 0.5158(2) 0.0110(4) Uani 1 1 d . . . . .
H3A H 0.8719 0.4898 0.4905 0.013 Uiso 1 1 calc R U . . .
H3B H 0.9147 0.5058 0.6125 0.013 Uiso 1 1 calc R U . . .
C4 C 0.9433(2) 0.7655(2) 0.4969(2) 0.0165(5) Uani 1 1 d . . . . .
H4A H 0.9151 0.7390 0.5909 0.025 Uiso 1 1 calc R U . . .
H4B H 0.9089 0.8668 0.4473 0.025 Uiso 1 1 calc R U . . .
H4C H 1.0388 0.7422 0.4882 0.025 Uiso 1 1 calc R U . . .
C5 C 0.7030(2) 0.8895(3) 0.9118(2) 0.0186(5) Uani 1 1 d . . . . .
H5A H 0.6787 0.9680 0.8260 0.028 Uiso 1 1 calc R U . . .
H5B H 0.6504 0.9121 0.9836 0.028 Uiso 1 1 calc R U . . .
H5C H 0.6874 0.8044 0.9137 0.028 Uiso 1 1 calc R U . . .
C6 C 0.9298(2) 0.8280(3) 0.8240(2) 0.0163(5) Uani 1 1 d . . . . .
H6A H 0.8984 0.9001 0.7362 0.020 Uiso 1 1 calc R U . . .
H6B H 0.9210 0.7367 0.8322 0.020 Uiso 1 1 calc R U . . .
C7 C 1.0728(2) 0.8179(2) 0.8280(2) 0.0168(5) Uani 1 1 d . . . . .
H7A H 1.1162 0.8259 0.7403 0.020 Uiso 1 1 calc R U . . .
H7B H 1.0802 0.8984 0.8432 0.020 Uiso 1 1 calc R U . . .
C8 C 1.2877(2) 0.6627(3) 0.9147(2) 0.0192(5) Uani 1 1 d . . . . .
H8A H 1.3175 0.6523 0.8310 0.029 Uiso 1 1 calc R U . . .
H8B H 1.3293 0.5776 0.9889 0.029 Uiso 1 1 calc R U . . .
H8C H 1.3114 0.7441 0.9123 0.029 Uiso 1 1 calc R U . . .
N1 N 0.43196(18) 0.6141(2) 0.32989(19) 0.0160(4) Uani 1 1 d . . . . .
H1C H 0.3913 0.5443 0.3283 0.019 Uiso 1 1 calc R U . . .
H1D H 0.3626 0.6840 0.3537 0.019 Uiso 1 1 calc R U . . .
N2 N 0.89334(18) 0.68652(19) 0.44224(19) 0.0137(4) Uani 1 1 d . . . . .
H2D H 0.7971 0.7198 0.4416 0.016 Uiso 1 1 calc R U . . .
H2E H 0.9270 0.7102 0.3488 0.016 Uiso 1 1 calc R U . . .
N3 N 1.14323(18) 0.6844(2) 0.93305(19) 0.0146(4) Uani 1 1 d . . . . .
H3C H 1.1146 0.6864 1.0213 0.018 Uiso 1 1 calc R U . . .
H3D H 1.1196 0.6039 0.9313 0.018 Uiso 1 1 calc R U . . .
N4 N 0.84445(18) 0.8648(2) 0.93014(18) 0.0138(4) Uani 1 1 d . . . . .
H4D H 0.8597 0.9507 0.9288 0.017 Uiso 1 1 calc R U . . .
H4E H 0.8680 0.7873 1.0180 0.017 Uiso 1 1 calc R U . . .
Sn2 Sn 0.5000 0.0000 0.5000 0.01152(5) Uani 1 2 d S . P . .
I1 I 0.64754(2) -0.04809(2) 0.24698(2) 0.01492(4) Uani 1 1 d . . . . .
I2 I 0.36726(2) 0.32381(2) 0.30243(2) 0.01490(4) Uani 1 1 d . . . . .
I3 I 0.28216(2) -0.13896(2) 0.48131(2) 0.01328(4) Uani 1 1 d . . . . .
I4 I 0.11755(2) 0.80129(2) 0.17567(2) 0.01393(4) Uani 1 1 d . . . . .
I5 I 0.12191(2) 0.45687(2) 0.80855(2) 0.01387(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
C1 N1 1.496(3) . ?
C1 C1 1.520(5) 2_666 ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 N1 1.489(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 N2 1.488(3) . ?
C3 C3 1.527(4) 2_766 ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 N2 1.498(3) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C5 N4 1.497(3) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 N4 1.495(3) . ?
C6 C7 1.515(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 N3 1.496(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 N3 1.492(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
N1 H1C 0.9900 . ?
N1 H1D 0.9900 . ?
N2 H2D 0.9900 . ?
N2 H2E 0.9900 . ?
N3 H3C 0.9900 . ?
N3 H3D 0.9900 . ?
N4 H4D 0.9900 . ?
N4 H4E 0.9900 . ?
Sn2 I1 3.1712(2) . ?
Sn2 I1 3.1712(2) 2_656 ?
Sn2 I3 3.2168(2) 2_656 ?
Sn2 I3 3.2168(2) . ?

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 C1 C1 109.7(2) . 2_666 ?
N1 C1 H1A 109.7 . . ?
C1 C1 H1A 109.7 2_666 . ?
N1 C1 H1B 109.7 . . ?
C1 C1 H1B 109.7 2_666 . ?
H1A C1 H1B 108.2 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C3 C3 110.6(2) . 2_766 ?
N2 C3 H3A 109.5 . . ?
C3 C3 H3A 109.5 2_766 . ?
N2 C3 H3B 109.5 . . ?
C3 C3 H3B 109.5 2_766 . ?
H3A C3 H3B 108.1 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N4 C5 H5A 109.5 . . ?
N4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
N4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N4 C6 C7 114.38(19) . . ?
N4 C6 H6A 108.7 . . ?
C7 C6 H6A 108.7 . . ?
N4 C6 H6B 108.7 . . ?
C7 C6 H6B 108.7 . . ?
H6A C6 H6B 107.6 . . ?
N3 C7 C6 113.97(19) . . ?
N3 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
N3 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C2 N1 C1 112.39(18) . . ?
C2 N1 H1C 109.1 . . ?
C1 N1 H1C 109.1 . . ?
C2 N1 H1D 109.1 . . ?
C1 N1 H1D 109.1 . . ?
H1C N1 H1D 107.9 . . ?
C3 N2 C4 115.34(17) . . ?
C3 N2 H2D 108.4 . . ?
C4 N2 H2D 108.4 . . ?
C3 N2 H2E 108.4 . . ?
C4 N2 H2E 108.4 . . ?
H2D N2 H2E 107.5 . . ?
C8 N3 C7 112.43(18) . . ?
C8 N3 H3C 109.1 . . ?
C7 N3 H3C 109.1 . . ?
C8 N3 H3D 109.1 . . ?
C7 N3 H3D 109.1 . . ?
H3C N3 H3D 107.9 . . ?
C6 N4 C5 111.86(17) . . ?
C6 N4 H4D 109.2 . . ?
C5 N4 H4D 109.2 . . ?
C6 N4 H4E 109.2 . . ?
C5 N4 H4E 109.2 . . ?
H4D N4 H4E 107.9 . . ?
I1 Sn2 I1 180.0 . 2_656 ?
I1 Sn2 I3 91.714(5) . 2_656 ?
I1 Sn2 I3 88.287(5) 2_656 2_656 ?
I1 Sn2 I3 88.287(5) . . ?
I1 Sn2 I3 91.712(5) 2_656 . ?
I3 Sn2 I3 180.0 2_656 . ?

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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N4 C6 C7 N3 77.6(2) . . . . ?
C1 C1 N1 C2 -175.2(2) 2_666 . . . ?
C3 C3 N2 C4 -75.7(3) 2_766 . . . ?
C6 C7 N3 C8 166.82(19) . . . . ?
C7 C6 N4 C5 173.46(19) . . . . ?

_refine_diff_density_max         0.830
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.106

_shelxl_version_number           2013-4

