# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_Pb2
_database_code_depnum_ccdc_archive 'CCDC 1469593'
_audit_update_record             
;
2016-03-26 deposited with the CCDC.
2016-07-06 downloaded from the CCDC.
;


# start Validation Reply Form
_vrf_PLAT971_Pb2                 
;
PROBLEM: Check Calcd Residual Density  0.73A From      N2       3.27 eA-3  
RESPONSE: This resiudal density maximum may correspond to an alternative
          site of N2, however no stable disorder model reflecting this
          idea could be established.  
;
# end Validation Reply Form 


_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[K(Kryptofix-2,2,2)]2[Pb2(mBDCA-5t)]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H132 K2 N12 O18 Pb2'
_chemical_formula_weight         2090.59

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   13.2463(16)
_cell_length_b                   13.2463(16)
_cell_length_c                   29.783(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4525.7(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9928
_cell_measurement_theta_min      2.24
_cell_measurement_theta_max      29.83

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_F_000             2140
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    3.881
_shelx_estimated_absorpt_T_min   0.892
_shelx_estimated_absorpt_T_max   0.962
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4842
_exptl_absorpt_correction_T_max  0.5282
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   
'I\mS micro-focus sealed tube, multilayer optics'
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            113659
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_av_R_equivalents  0.0853
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         1.367
_diffrn_reflns_theta_max         31.502
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5130
_reflns_number_gt                3431
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0178P)²+8.4443P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5130
_refine_ls_number_parameters     274
_refine_ls_number_restraints     546
_refine_ls_R_factor_all          0.0532
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0612
_refine_ls_wR_factor_gt          0.0517
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      0.967
_refine_ls_shift/su_max          0.003
_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
Pb1 Pb 0.0000 1.0000 0.30922(2) 0.01383(4) Uani 1 3 d S T P . .
O1 O 0.25568(17) 0.92881(17) 0.36436(6) 0.0211(4) Uani 1 1 d . . . . .
N1 N 0.18318(19) 1.04663(19) 0.34096(7) 0.0174(4) Uani 1 1 d D . . . .
N2 N 0.0000 1.0000 0.40512(12) 0.0183(6) Uani 1 3 d S T P . .
C1 C 0.2083(2) 1.1019(2) 0.38521(8) 0.0182(5) Uani 1 1 d . . . . .
H1A H 0.2099 1.1773 0.3832 0.022 Uiso 1 1 calc R U . . .
H1B H 0.2860 1.1177 0.3954 0.022 Uiso 1 1 calc R U . . .
C2 C 0.1161(2) 1.0235(2) 0.41924(8) 0.0204(5) Uani 1 1 d . . . . .
H2A H 0.1162 0.9490 0.4220 0.024 Uiso 1 1 calc R U . . .
H2B H 0.1351 1.0618 0.4490 0.024 Uiso 1 1 calc R U . . .
C3 C 0.2098(2) 0.9622(2) 0.33577(8) 0.0167(5) Uani 1 1 d D U . . .
C4 C 0.1756(9) 0.8990(13) 0.2936(5) 0.0126(16) Uani 0.385(3) 1 d D U P A -1
C5 C 0.2039(15) 0.9605(8) 0.2532(6) 0.0129(13) Uani 0.385(3) 1 d D U P A -1
H5 H 0.2414 1.0432 0.2535 0.015 Uiso 0.385(3) 1 calc R U P A -1
C6 C 0.177(2) 0.9005(13) 0.2122(5) 0.014(2) Uani 0.385(3) 1 d D U P A -1
C7 C 0.1179(17) 0.7782(12) 0.2128(7) 0.014(2) Uani 0.385(3) 1 d D U P A -1
H7 H 0.1003 0.7370 0.1851 0.017 Uiso 0.385(3) 1 calc R U P A -1
C8 C 0.0839(5) 0.7150(4) 0.2532(7) 0.0159(15) Uani 0.385(3) 1 d D U P A -1
C9 C 0.1164(16) 0.7781(12) 0.2930(7) 0.013(2) Uani 0.385(3) 1 d D U P A -1
H9 H 0.0975 0.7371 0.3207 0.016 Uiso 0.385(3) 1 calc R U P A -1
C10 C 0.0061(4) 0.5816(4) 0.2507(7) 0.0187(10) Uani 0.385(3) 1 d D U P A -1
C11 C 0.015(2) 0.5190(19) 0.2925(7) 0.024(3) Uani 0.385(3) 1 d D U P A -1
H11A H 0.0959 0.5377 0.2965 0.036 Uiso 0.385(3) 1 calc R U P A -1
H11B H -0.0352 0.4347 0.2888 0.036 Uiso 0.385(3) 1 calc R U P A -1
H11C H -0.0102 0.5447 0.3190 0.036 Uiso 0.385(3) 1 calc R U P A -1
C12 C -0.1214(5) 0.5542(6) 0.2549(8) 0.025(3) Uani 0.385(3) 1 d D U P A -1
H12A H -0.1737 0.4695 0.2551 0.038 Uiso 0.385(3) 1 calc R U P A -1
H12B H -0.1406 0.5882 0.2294 0.038 Uiso 0.385(3) 1 calc R U P A -1
H12C H -0.1309 0.5874 0.2829 0.038 Uiso 0.385(3) 1 calc R U P A -1
C13 C 0.0378(16) 0.5324(15) 0.2100(6) 0.022(3) Uani 0.385(3) 1 d D U P A -1
H13A H 0.1204 0.5553 0.2115 0.033 Uiso 0.385(3) 1 calc R U P A -1
H13B H 0.0231 0.5632 0.1824 0.033 Uiso 0.385(3) 1 calc R U P A -1
H13C H -0.0099 0.4472 0.2100 0.033 Uiso 0.385(3) 1 calc R U P A -1
C4A C 0.1860(17) 0.9057(18) 0.2927(8) 0.0126(16) Uani 0.115(3) 1 d D U P A -2
C5A C 0.203(5) 0.969(2) 0.2532(9) 0.0129(13) Uani 0.115(3) 1 d D U P A -2
H5A H 0.2294 1.0497 0.2545 0.015 Uiso 0.115(3) 1 calc R U P A -2
C6A C 0.180(7) 0.912(3) 0.2119(9) 0.014(2) Uani 0.115(3) 1 d D U P A -2
C7A C 0.142(5) 0.792(2) 0.2109(12) 0.014(2) Uani 0.115(3) 1 d D U P A -2
H7A H 0.1335 0.7549 0.1828 0.017 Uiso 0.115(3) 1 calc R U P A -2
C8A C 0.1179(17) 0.7273(12) 0.2506(11) 0.0159(15) Uani 0.115(3) 1 d D U P A -2
C9A C 0.147(4) 0.787(2) 0.2914(11) 0.013(2) Uani 0.115(3) 1 d D U P A -2
H9A H 0.1404 0.7464 0.3185 0.016 Uiso 0.115(3) 1 calc R U P A -2
C10A C 0.0772(13) 0.5960(12) 0.2500(12) 0.0211(19) Uani 0.115(3) 1 d D U P A -2
C11A C 0.014(5) 0.537(4) 0.2939(13) 0.024(3) Uani 0.115(3) 1 d D U P A -2
H11D H -0.0180 0.4527 0.2914 0.036 Uiso 0.115(3) 1 calc R U P A -2
H11E H -0.0487 0.5538 0.2994 0.036 Uiso 0.115(3) 1 calc R U P A -2
H11F H 0.0700 0.5673 0.3189 0.036 Uiso 0.115(3) 1 calc R U P A -2
C12A C 0.1858(13) 0.5815(15) 0.253(2) 0.025(3) Uani 0.115(3) 1 d D U P A -2
H12D H 0.2462 0.6372 0.2325 0.038 Uiso 0.115(3) 1 calc R U P A -2
H12E H 0.1644 0.5019 0.2440 0.038 Uiso 0.115(3) 1 calc R U P A -2
H12F H 0.2155 0.5960 0.2836 0.038 Uiso 0.115(3) 1 calc R U P A -2
C13A C -0.007(3) 0.535(3) 0.2112(10) 0.018(5) Uani 0.115(3) 1 d D U P A -2
H13D H 0.0318 0.5685 0.1827 0.026 Uiso 0.115(3) 1 calc R U P A -2
H13E H -0.0752 0.5457 0.2144 0.026 Uiso 0.115(3) 1 calc R U P A -2
H13F H -0.0333 0.4515 0.2118 0.026 Uiso 0.115(3) 1 calc R U P A -2
K1 K 0.3333 0.6667 0.51336(19) 0.0153(5) Uani 0.95(2) 3 d S T P B 1
K1A K 0.3333 0.6667 0.498(3) 0.0153(5) Uani 0.05(2) 3 d S T P B 2
N3 N 0.3333 0.6667 0.41238(12) 0.0161(7) Uani 1 3 d S T P B .
O12 O 0.14070(16) 0.65579(16) 0.46618(6) 0.0183(4) Uani 1 1 d . . . . .
O13 O 0.15398(16) 0.67644(17) 0.56024(6) 0.0205(4) Uani 1 1 d . . . . .
N4 N 0.3333 0.6667 0.61566(13) 0.0181(7) Uani 1 3 d S T P . .
C21 C 0.2176(2) 0.6390(2) 0.39559(8) 0.0189(5) Uani 1 1 d . . . . .
H21A H 0.1645 0.5537 0.3974 0.023 Uiso 1 1 calc R U . B 2
H21B H 0.2247 0.6616 0.3636 0.023 Uiso 1 1 calc R U . B 2
C22 C 0.1643(2) 0.6991(2) 0.42095(9) 0.0203(5) Uani 1 1 d . . . . .
H22A H 0.2187 0.7843 0.4211 0.024 Uiso 1 1 calc R U . B 2
H22B H 0.0911 0.6838 0.4062 0.024 Uiso 1 1 calc R U . B 2
C23 C 0.0816(2) 0.7026(2) 0.49087(9) 0.0223(6) Uani 1 1 d . . . . .
H23A H 0.0104 0.6882 0.4746 0.027 Uiso 1 1 calc R U . . .
H23B H 0.1327 0.7878 0.4945 0.027 Uiso 1 1 calc R U . . .
C24 C 0.0494(2) 0.6450(2) 0.53601(9) 0.0207(5) Uani 1 1 d . . . . .
H24A H 0.0015 0.6707 0.5527 0.025 Uiso 1 1 calc R U . . .
H24B H 0.0033 0.5593 0.5324 0.025 Uiso 1 1 calc R U . . .
C25 C 0.1290(2) 0.6179(2) 0.60269(9) 0.0212(5) Uani 1 1 d . . . . .
H25A H 0.1086 0.5357 0.5984 0.025 Uiso 1 1 calc R U . . .
H25B H 0.0622 0.6189 0.6172 0.025 Uiso 1 1 calc R U . . .
C26 C 0.2363(2) 0.6809(3) 0.63162(9) 0.0218(5) Uani 1 1 d . . . . .
H26A H 0.2614 0.7649 0.6322 0.026 Uiso 1 1 calc R U . . .
H26B H 0.2165 0.6510 0.6627 0.026 Uiso 1 1 calc R U . . .


_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
Pb1 N1 2.380(2) . ?
Pb1 N1 2.380(2) 3_465 ?
Pb1 N1 2.380(2) 2_675 ?
Pb1 Pb1 3.5274(5) 10_556 ?
O1 C3 1.248(3) . ?
N1 C3 1.340(3) . ?
N1 C1 1.463(3) . ?
N2 C2 1.470(3) . ?
N2 C2 1.470(3) 3_465 ?
N2 C2 1.470(3) 2_675 ?
C1 C2 1.526(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4A 1.44(2) . ?
C3 C4 1.450(16) . ?
C4 C9 1.387(12) . ?
C4 C5 1.395(11) . ?
C5 C6 1.403(11) . ?
C5 H5 0.9500 . ?
C6 C7 1.403(12) . ?
C7 C8 1.405(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.390(11) . ?
C8 C10 1.539(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.532(12) . ?
C10 C13 1.533(11) . ?
C10 C12 1.544(7) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C4A C9A 1.387(16) . ?
C4A C5A 1.392(15) . ?
C5A C6A 1.395(16) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.401(16) . ?
C7A C8A 1.404(16) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.396(16) . ?
C8A C10A 1.542(14) . ?
C9A H9A 0.9500 . ?
C10A C13A 1.530(14) . ?
C10A C11A 1.536(15) . ?
C10A C12A 1.546(13) . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C13A H13D 0.9800 . ?
C13A H13E 0.9800 . ?
C13A H13F 0.9800 . ?
K1 O13 2.814(3) 3_565 ?
K1 O13 2.814(3) . ?
K1 O13 2.814(3) 2_665 ?
K1 O12 2.853(3) 3_565 ?
K1 O12 2.853(3) 2_665 ?
K1 O12 2.853(3) . ?
K1 N3 3.008(7) . ?
K1 N4 3.047(7) . ?
K1A N3 2.56(8) . ?
K1A O12 2.66(3) 3_565 ?
K1A O12 2.66(3) 2_665 ?
K1A O12 2.66(3) . ?
K1A O13 3.06(5) 3_565 ?
K1A O13 3.06(5) 2_665 ?
K1A O13 3.06(5) . ?
K1A C21 3.36(7) 3_565 ?
K1A C21 3.36(7) 2_665 ?
K1A C21 3.36(7) . ?
K1A C22 3.38(6) 3_565 ?
K1A C22 3.38(6) 2_665 ?
N3 C21 1.474(3) . ?
N3 C21 1.474(3) 3_565 ?
N3 C21 1.474(3) 2_665 ?
O12 C23 1.423(3) . ?
O12 C22 1.436(3) . ?
O13 C24 1.427(3) . ?
O13 C25 1.433(3) . ?
N4 C26 1.468(3) 3_565 ?
N4 C26 1.468(3) 2_665 ?
N4 C26 1.468(3) . ?
C21 C22 1.504(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.499(4) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.507(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?

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 Pb1 N1 105.26(6) . 3_465 ?
N1 Pb1 N1 105.26(6) . 2_675 ?
N1 Pb1 N1 105.26(6) 3_465 2_675 ?
N1 Pb1 Pb1 113.41(5) . 10_556 ?
N1 Pb1 Pb1 113.41(5) 3_465 10_556 ?
N1 Pb1 Pb1 113.41(5) 2_675 10_556 ?
C3 N1 C1 115.7(2) . . ?
C3 N1 Pb1 113.42(16) . . ?
C1 N1 Pb1 115.80(16) . . ?
C2 N2 C2 112.17(15) . 3_465 ?
C2 N2 C2 112.17(15) . 2_675 ?
C2 N2 C2 112.17(15) 3_465 2_675 ?
N1 C1 C2 110.7(2) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 110.5(2) . . ?
N2 C2 H2A 109.5 . . ?
C1 C2 H2A 109.5 . . ?
N2 C2 H2B 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 108.1 . . ?
O1 C3 N1 126.5(2) . . ?
O1 C3 C4A 116.3(9) . . ?
N1 C3 C4A 117.2(9) . . ?
O1 C3 C4 116.9(5) . . ?
N1 C3 C4 116.5(5) . . ?
C9 C4 C5 119.6(12) . . ?
C9 C4 C3 120.7(12) . . ?
C5 C4 C3 119.6(11) . . ?
C4 C5 C6 120.2(6) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C7 C6 C5 118.7(12) . . ?
C6 C7 C8 121.7(12) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 117.5(5) . . ?
C9 C8 C10 124.0(11) . . ?
C7 C8 C10 118.3(11) . . ?
C4 C9 C8 122.1(13) . . ?
C4 C9 H9 118.9 . . ?
C8 C9 H9 118.9 . . ?
C11 C10 C13 107.6(6) . . ?
C11 C10 C8 113.2(12) . . ?
C13 C10 C8 110.9(10) . . ?
C11 C10 C12 100.2(17) . . ?
C13 C10 C12 117.6(15) . . ?
C8 C10 C12 107.0(5) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9A C4A C5A 121(2) . . ?
C9A C4A C3 118.2(18) . . ?
C5A C4A C3 120.9(18) . . ?
C4A C5A C6A 119.7(18) . . ?
C4A C5A H5A 120.1 . . ?
C6A C5A H5A 120.1 . . ?
C5A C6A C7A 119(2) . . ?
C6A C7A C8A 121(2) . . ?
C6A C7A H7A 119.4 . . ?
C8A C7A H7A 119.4 . . ?
C9A C8A C7A 118.2(14) . . ?
C9A C8A C10A 119.4(16) . . ?
C7A C8A C10A 121.7(17) . . ?
C4A C9A C8A 120.4(18) . . ?
C4A C9A H9A 119.8 . . ?
C8A C9A H9A 119.8 . . ?
C13A C10A C11A 108(2) . . ?
C13A C10A C8A 110.8(14) . . ?
C11A C10A C8A 111.0(18) . . ?
C13A C10A C12A 117(2) . . ?
C11A C10A C12A 101(3) . . ?
C8A C10A C12A 108.5(12) . . ?
C10A C11A H11D 109.5 . . ?
C10A C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
C10A C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C10A C12A H12D 109.5 . . ?
C10A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C10A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C10A C13A H13D 109.5 . . ?
C10A C13A H13E 109.5 . . ?
H13D C13A H13E 109.5 . . ?
C10A C13A H13F 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
O13 K1 O13 97.51(14) 3_565 . ?
O13 K1 O13 97.51(14) 3_565 2_665 ?
O13 K1 O13 97.51(14) . 2_665 ?
O13 K1 O12 59.49(5) 3_565 3_565 ?
O13 K1 O12 123.89(5) . 3_565 ?
O13 K1 O12 133.10(5) 2_665 3_565 ?
O13 K1 O12 123.89(5) 3_565 2_665 ?
O13 K1 O12 133.10(5) . 2_665 ?
O13 K1 O12 59.49(5) 2_665 2_665 ?
O12 K1 O12 97.82(14) 3_565 2_665 ?
O13 K1 O12 133.10(5) 3_565 . ?
O13 K1 O12 59.49(5) . . ?
O13 K1 O12 123.89(5) 2_665 . ?
O12 K1 O12 97.82(14) 3_565 . ?
O12 K1 O12 97.82(14) 2_665 . ?
O13 K1 N3 119.75(11) 3_565 . ?
O13 K1 N3 119.75(11) . . ?
O13 K1 N3 119.75(11) 2_665 . ?
O12 K1 N3 60.49(11) 3_565 . ?
O12 K1 N3 60.49(11) 2_665 . ?
O12 K1 N3 60.49(11) . . ?
O13 K1 N4 60.25(11) 3_565 . ?
O13 K1 N4 60.25(11) . . ?
O13 K1 N4 60.25(11) 2_665 . ?
O12 K1 N4 119.51(11) 3_565 . ?
O12 K1 N4 119.51(11) 2_665 . ?
O12 K1 N4 119.51(11) . . ?
N3 K1 N4 180.0 . . ?
N3 K1A O12 69.0(16) . 3_565 ?
N3 K1A O12 69.0(16) . 2_665 ?
O12 K1A O12 107.9(17) 3_565 2_665 ?
N3 K1A O12 69.0(16) . . ?
O12 K1A O12 107.9(17) 3_565 . ?
O12 K1A O12 107.9(17) 2_665 . ?
N3 K1A O13 127.1(12) . 3_565 ?
O12 K1A O13 58.3(4) 3_565 3_565 ?
O12 K1A O13 121.7(8) 2_665 3_565 ?
O12 K1A O13 130.5(9) . 3_565 ?
N3 K1A O13 127.1(12) . 2_665 ?
O12 K1A O13 130.5(9) 3_565 2_665 ?
O12 K1A O13 58.3(4) 2_665 2_665 ?
O12 K1A O13 121.7(8) . 2_665 ?
O13 K1A O13 87.4(18) 3_565 2_665 ?
N3 K1A O13 127.1(12) . . ?
O12 K1A O13 121.7(8) 3_565 . ?
O12 K1A O13 130.5(9) 2_665 . ?
O12 K1A O13 58.3(4) . . ?
O13 K1A O13 87.4(18) 3_565 . ?
O13 K1A O13 87.4(18) 2_665 . ?
N3 K1A C21 24.4(6) . 3_565 ?
O12 K1A C21 45.1(11) 3_565 3_565 ?
O12 K1A C21 86(2) 2_665 3_565 ?
O12 K1A C21 78.6(18) . 3_565 ?
O13 K1A C21 103.4(7) 3_565 3_565 ?
O13 K1A C21 141.8(13) 2_665 3_565 ?
O13 K1A C21 129.0(10) . 3_565 ?
N3 K1A C21 24.4(6) . 2_665 ?
O12 K1A C21 78.6(18) 3_565 2_665 ?
O12 K1A C21 45.1(11) 2_665 2_665 ?
O12 K1A C21 86(2) . 2_665 ?
O13 K1A C21 129.0(10) 3_565 2_665 ?
O13 K1A C21 103.4(7) 2_665 2_665 ?
O13 K1A C21 141.8(13) . 2_665 ?
C21 K1A C21 41.9(10) 3_565 2_665 ?
N3 K1A C21 24.4(6) . . ?
O12 K1A C21 86(2) 3_565 . ?
O12 K1A C21 78.6(18) 2_665 . ?
O12 K1A C21 45.1(11) . . ?
O13 K1A C21 141.8(13) 3_565 . ?
O13 K1A C21 129.0(10) 2_665 . ?
O13 K1A C21 103.4(7) . . ?
C21 K1A C21 41.9(10) 3_565 . ?
C21 K1A C21 41.9(10) 2_665 . ?
N3 K1A C22 47.1(10) . 3_565 ?
O12 K1A C22 23.8(6) 3_565 3_565 ?
O12 K1A C22 88.5(16) 2_665 3_565 ?
O12 K1A C22 102(2) . 3_565 ?
O13 K1A C22 80.1(2) 3_565 3_565 ?
O13 K1A C22 130.4(3) 2_665 3_565 ?
O13 K1A C22 138.9(3) . 3_565 ?
C21 K1A C22 25.8(5) 3_565 3_565 ?
C21 K1A C22 54.8(11) 2_665 3_565 ?
C21 K1A C22 67.6(15) . 3_565 ?
N3 K1A C22 47.1(10) . 2_665 ?
O12 K1A C22 102(2) 3_565 2_665 ?
O12 K1A C22 23.8(6) 2_665 2_665 ?
O12 K1A C22 88.5(16) . 2_665 ?
O13 K1A C22 138.9(3) 3_565 2_665 ?
O13 K1A C22 80.1(2) 2_665 2_665 ?
O13 K1A C22 130.4(3) . 2_665 ?
C21 K1A C22 67.6(15) 3_565 2_665 ?
C21 K1A C22 25.8(5) 2_665 2_665 ?
C21 K1A C22 54.8(11) . 2_665 ?
C22 K1A C22 78.8(15) 3_565 2_665 ?
C21 N3 C21 109.10(17) . 3_565 ?
C21 N3 C21 109.11(17) . 2_665 ?
C21 N3 C21 109.11(17) 3_565 2_665 ?
C21 N3 K1A 109.84(16) . . ?
C21 N3 K1A 109.83(16) 3_565 . ?
C21 N3 K1A 109.83(16) 2_665 . ?
C21 N3 K1 109.84(16) . . ?
C21 N3 K1 109.83(16) 3_565 . ?
C21 N3 K1 109.83(16) 2_665 . ?
C23 O12 C22 111.63(19) . . ?
C23 O12 K1A 120.9(14) . . ?
C22 O12 K1A 107.7(15) . . ?
C23 O12 K1 113.38(17) . . ?
C22 O12 K1 115.52(17) . . ?
C24 O13 C25 111.1(2) . . ?
C24 O13 K1 117.02(17) . . ?
C25 O13 K1 112.64(17) . . ?
C24 O13 K1A 110.1(12) . . ?
C25 O13 K1A 118.9(10) . . ?
C26 N4 C26 110.05(17) 3_565 2_665 ?
C26 N4 C26 110.05(17) 3_565 . ?
C26 N4 C26 110.05(17) 2_665 . ?
C26 N4 K1 108.89(17) 3_565 . ?
C26 N4 K1 108.89(17) 2_665 . ?
C26 N4 K1 108.89(17) . . ?
N3 C21 C22 113.8(2) . . ?
N3 C21 K1A 45.8(6) . . ?
C22 C21 K1A 78.1(5) . . ?
N3 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
K1A C21 H21A 95.7 . . ?
N3 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
K1A C21 H21B 151.1 . . ?
H21A C21 H21B 107.7 . . ?
O12 C22 C21 109.0(2) . . ?
O12 C22 K1A 48.5(9) . . ?
C21 C22 K1A 76.1(10) . . ?
O12 C22 H22A 109.9 . . ?
C21 C22 H22A 109.9 . . ?
K1A C22 H22A 89.5 . . ?
O12 C22 H22B 109.9 . . ?
C21 C22 H22B 109.9 . . ?
K1A C22 H22B 156.9 . . ?
H22A C22 H22B 108.3 . . ?
O12 C23 C24 108.7(2) . . ?
O12 C23 H23A 110.0 . . ?
C24 C23 H23A 110.0 . . ?
O12 C23 H23B 110.0 . . ?
C24 C23 H23B 110.0 . . ?
H23A C23 H23B 108.3 . . ?
O13 C24 C23 108.5(2) . . ?
O13 C24 H24A 110.0 . . ?
C23 C24 H24A 110.0 . . ?
O13 C24 H24B 110.0 . . ?
C23 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
O13 C25 C26 107.8(2) . . ?
O13 C25 H25A 110.1 . . ?
C26 C25 H25A 110.1 . . ?
O13 C25 H25B 110.1 . . ?
C26 C25 H25B 110.1 . . ?
H25A C25 H25B 108.5 . . ?
N4 C26 C25 112.8(2) . . ?
N4 C26 H26A 109.0 . . ?
C25 C26 H26A 109.0 . . ?
N4 C26 H26B 109.0 . . ?
C25 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?

_refine_diff_density_max         3.298
_refine_diff_density_min         -1.673
_refine_diff_density_rms         0.112


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method DMF/Et2O
####################################################################### 
# 
# 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_Sn2
_database_code_depnum_ccdc_archive 'CCDC 1469595'
_audit_update_record             
;
2016-03-26 deposited with the CCDC.
2016-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[K(Kryptofix-2,2,2]2[Sn2(mBDCA-5t)]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H132 K2 N12 O18 Sn2'
_chemical_formula_weight         1913.59

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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'

_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_H-M_alt        'P 63/m'
_space_group_name_Hall           '-P 6c'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -z-1/2'

_cell_length_a                   13.1963(19)
_cell_length_b                   13.1963(19)
_cell_length_c                   29.806(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4495.0(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9780
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      29.56

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.420
_exptl_crystal_F_000             2012
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.086
_exptl_absorpt_coefficient_mu    0.723
_shelx_estimated_absorpt_T_min   0.836
_shelx_estimated_absorpt_T_max   0.940
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5888
_exptl_absorpt_correction_T_max  0.6483
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   
'I\mS micro-focus sealed tube, multilayer optics'
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            186032
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_av_R_equivalents  0.0604
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         1.366
_diffrn_reflns_theta_max         31.504
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5098
_reflns_number_gt                4179
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0490P)²+4.9624P] 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     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5098
_refine_ls_number_parameters     274
_refine_ls_number_restraints     546
_refine_ls_R_factor_all          0.0481
_refine_ls_R_factor_gt           0.0372
_refine_ls_wR_factor_ref         0.1008
_refine_ls_wR_factor_gt          0.0931
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.001
_refine_ls_shift/su_max          0.002
_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
Sn1 Sn 0.0000 1.0000 0.30934(2) 0.01654(7) Uani 1 3 d S T P . .
O1 O 0.25912(12) 0.93134(12) 0.36191(4) 0.0246(3) Uani 1 1 d . . . . .
N1 N 0.16625(14) 1.03462(14) 0.34383(5) 0.0212(3) Uani 1 1 d D . . . .
N2 N 0.0000 1.0000 0.41388(11) 0.0212(5) Uani 1 3 d S T P . .
C1 C 0.20248(16) 1.09635(16) 0.38678(6) 0.0214(3) Uani 1 1 d . . . . .
H1A H 0.2056 1.1727 0.3842 0.026 Uiso 1 1 calc R U . . .
H1B H 0.2819 1.1116 0.3945 0.026 Uiso 1 1 calc R U . . .
C2 C 0.11738(16) 1.02440(17) 0.42397(6) 0.0224(3) Uani 1 1 d . . . . .
H2A H 0.1173 0.9498 0.4276 0.027 Uiso 1 1 calc R U . . .
H2B H 0.1435 1.0678 0.4526 0.027 Uiso 1 1 calc R U . . .
C3 C 0.20202(15) 0.95694(15) 0.33563(6) 0.0193(3) Uani 1 1 d D U . . .
C4 C 0.1664(8) 0.8931(11) 0.2934(5) 0.0160(14) Uani 0.389(2) 1 d D U P A -1
C5 C 0.1943(11) 0.9544(6) 0.2532(5) 0.0155(11) Uani 0.389(2) 1 d D U P A -1
H5 H 0.2331 1.0374 0.2536 0.019 Uiso 0.389(2) 1 calc R U P A -1
C6 C 0.1655(15) 0.8949(11) 0.2119(5) 0.0149(16) Uani 0.389(2) 1 d D U P A -1
C7 C 0.1059(15) 0.7715(10) 0.2132(5) 0.0186(19) Uani 0.389(2) 1 d D U P A -1
H7 H 0.0878 0.7295 0.1857 0.022 Uiso 0.389(2) 1 calc R U P A -1
C8 C 0.0726(4) 0.7089(3) 0.2535(5) 0.0174(12) Uani 0.389(2) 1 d D U P A -1
C9 C 0.1068(13) 0.7717(10) 0.2934(5) 0.0163(18) Uani 0.389(2) 1 d D U P A -1
H9 H 0.0890 0.7309 0.3211 0.020 Uiso 0.389(2) 1 calc R U P A -1
C10 C -0.0036(3) 0.5748(3) 0.2508(7) 0.0236(8) Uani 0.389(2) 1 d D U P A -1
C11 C 0.007(2) 0.5165(17) 0.2935(6) 0.027(2) Uani 0.389(2) 1 d D U P A -1
H11A H 0.0883 0.5362 0.2976 0.041 Uiso 0.389(2) 1 calc R U P A -1
H11B H -0.0431 0.4314 0.2909 0.041 Uiso 0.389(2) 1 calc R U P A -1
H11C H -0.0182 0.5445 0.3194 0.041 Uiso 0.389(2) 1 calc R U P A -1
C12 C -0.1317(4) 0.5448(5) 0.2550(5) 0.0316(19) Uani 0.389(2) 1 d D U P A -1
H12A H -0.1829 0.4597 0.2547 0.047 Uiso 0.389(2) 1 calc R U P A -1
H12B H -0.1516 0.5793 0.2298 0.047 Uiso 0.389(2) 1 calc R U P A -1
H12C H -0.1423 0.5765 0.2833 0.047 Uiso 0.389(2) 1 calc R U P A -1
C13 C 0.0293(15) 0.5227(16) 0.2113(5) 0.027(2) Uani 0.389(2) 1 d D U P A -1
H13A H 0.1123 0.5462 0.2133 0.041 Uiso 0.389(2) 1 calc R U P A -1
H13B H 0.0147 0.5513 0.1831 0.041 Uiso 0.389(2) 1 calc R U P A -1
H13C H -0.0182 0.4371 0.2123 0.041 Uiso 0.389(2) 1 calc R U P A -1
C4A C 0.1779(14) 0.8998(18) 0.2923(7) 0.0160(14) Uani 0.111(2) 1 d D U P A -2
C5A C 0.197(4) 0.966(2) 0.2535(8) 0.0155(11) Uani 0.111(2) 1 d D U P A -2
H5A H 0.2235 1.0471 0.2551 0.019 Uiso 0.111(2) 1 calc R U P A -2
C6A C 0.176(5) 0.909(2) 0.2124(9) 0.0149(16) Uani 0.111(2) 1 d D U P A -2
C7A C 0.132(4) 0.789(2) 0.2113(11) 0.0186(19) Uani 0.111(2) 1 d D U P A -2
H7A H 0.1186 0.7511 0.1830 0.022 Uiso 0.111(2) 1 calc R U P A -2
C8A C 0.1065(13) 0.7201(11) 0.2503(10) 0.0174(12) Uani 0.111(2) 1 d D U P A -2
C9A C 0.133(3) 0.7799(19) 0.2911(10) 0.0163(18) Uani 0.111(2) 1 d D U P A -2
H9A H 0.1201 0.7379 0.3183 0.020 Uiso 0.111(2) 1 calc R U P A -2
C10A C 0.0704(10) 0.5895(9) 0.2487(10) 0.0249(17) Uani 0.111(2) 1 d D U P A -2
C11A C 0.009(5) 0.528(4) 0.2923(12) 0.027(2) Uani 0.111(2) 1 d D U P A -2
H11D H -0.0175 0.4441 0.2900 0.041 Uiso 0.111(2) 1 calc R U P A -2
H11E H -0.0593 0.5379 0.2972 0.041 Uiso 0.111(2) 1 calc R U P A -2
H11F H 0.0629 0.5618 0.3175 0.041 Uiso 0.111(2) 1 calc R U P A -2
C12A C 0.1795(11) 0.5766(12) 0.251(3) 0.0316(19) Uani 0.111(2) 1 d D U P A -2
H12D H 0.2397 0.6333 0.2310 0.047 Uiso 0.111(2) 1 calc R U P A -2
H12E H 0.1590 0.4971 0.2422 0.047 Uiso 0.111(2) 1 calc R U P A -2
H12F H 0.2095 0.5911 0.2820 0.047 Uiso 0.111(2) 1 calc R U P A -2
C13A C -0.018(2) 0.528(2) 0.2112(9) 0.022(4) Uani 0.111(2) 1 d D U P A -2
H13D H 0.0224 0.5486 0.1822 0.033 Uiso 0.111(2) 1 calc R U P A -2
H13E H -0.0773 0.5515 0.2118 0.033 Uiso 0.111(2) 1 calc R U P A -2
H13F H -0.0558 0.4427 0.2154 0.033 Uiso 0.111(2) 1 calc R U P A -2
K1 K 0.3333 0.6667 0.5115(3) 0.0177(5) Uani 0.87(4) 3 d S T P B 1
K1A K 0.3333 0.6667 0.5019(11) 0.0177(5) Uani 0.13(4) 3 d S T P B 2
N3 N 0.3333 0.6667 0.41002(9) 0.0184(5) Uani 1 3 d S T P B .
O12 O 0.13958(12) 0.65629(12) 0.46386(4) 0.0217(3) Uani 1 1 d . . . . .
O13 O 0.15334(13) 0.67754(13) 0.55766(4) 0.0258(3) Uani 1 1 d . . . . .
N4 N 0.3333 0.6667 0.61291(10) 0.0248(5) Uani 1 3 d S T P . .
C21 C 0.21704(16) 0.63841(17) 0.39351(6) 0.0218(3) Uani 1 1 d . . . . .
H21A H 0.1639 0.5528 0.3956 0.026 Uiso 1 1 calc R U . B 2
H21B H 0.2236 0.6603 0.3614 0.026 Uiso 1 1 calc R U . B 2
C22 C 0.16345(17) 0.69905(17) 0.41875(6) 0.0237(4) Uani 1 1 d . . . . .
H22A H 0.2180 0.7846 0.4188 0.028 Uiso 1 1 calc R U . B 2
H22B H 0.0900 0.6837 0.4039 0.028 Uiso 1 1 calc R U . B 2
C23 C 0.08103(18) 0.70453(18) 0.48840(7) 0.0255(4) Uani 1 1 d . . . . .
H23A H 0.0098 0.6905 0.4721 0.031 Uiso 1 1 calc R U . . .
H23B H 0.1330 0.7900 0.4919 0.031 Uiso 1 1 calc R U . . .
C24 C 0.04861(17) 0.64731(18) 0.53358(7) 0.0257(4) Uani 1 1 d . . . . .
H24A H 0.0016 0.6743 0.5502 0.031 Uiso 1 1 calc R U . . .
H24B H 0.0012 0.5613 0.5301 0.031 Uiso 1 1 calc R U . . .
C25 C 0.12814(18) 0.61826(19) 0.60002(7) 0.0277(4) Uani 1 1 d . . . . .
H25A H 0.1077 0.5358 0.5957 0.033 Uiso 1 1 calc R U . . .
H25B H 0.0612 0.6192 0.6146 0.033 Uiso 1 1 calc R U . . .
C26 C 0.23612(19) 0.6814(2) 0.62880(7) 0.0295(4) Uani 1 1 d . . . . .
H26A H 0.2616 0.7659 0.6292 0.035 Uiso 1 1 calc R U . . .
H26B H 0.2163 0.6519 0.6599 0.035 Uiso 1 1 calc R U . . .


_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
Sn1 N1 2.2531(16) . ?
Sn1 N1 2.2531(16) 2_675 ?
Sn1 N1 2.2531(16) 3_465 ?
O1 C3 1.245(2) . ?
N1 C3 1.348(2) . ?
N1 C1 1.463(2) . ?
N2 C2 1.447(2) . ?
N2 C2 1.447(2) 3_465 ?
N2 C2 1.447(2) 2_675 ?
C1 C2 1.525(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4A 1.447(19) . ?
C3 C4 1.456(15) . ?
C4 C9 1.387(11) . ?
C4 C5 1.388(9) . ?
C5 C6 1.407(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.411(11) . ?
C7 C8 1.398(9) . ?
C7 H7 0.9500 . ?
C8 C9 1.390(9) . ?
C8 C10 1.539(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.527(12) . ?
C10 C13 1.532(11) . ?
C10 C12 1.536(6) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C4A C9A 1.385(15) . ?
C4A C5A 1.393(15) . ?
C5A C6A 1.388(15) . ?
C5A H5A 0.9500 . ?
C6A C7A 1.398(15) . ?
C7A C8A 1.407(15) . ?
C7A H7A 0.9500 . ?
C8A C9A 1.394(15) . ?
C8A C10A 1.542(13) . ?
C9A H9A 0.9500 . ?
C10A C13A 1.525(14) . ?
C10A C12A 1.534(12) . ?
C10A C11A 1.534(15) . ?
C11A H11D 0.9800 . ?
C11A H11E 0.9800 . ?
C11A H11F 0.9800 . ?
C12A H12D 0.9800 . ?
C12A H12E 0.9800 . ?
C12A H12F 0.9800 . ?
C13A H13D 0.9800 . ?
C13A H13E 0.9800 . ?
C13A H13F 0.9800 . ?
K1 O13 2.810(5) 3_565 ?
K1 O13 2.810(5) . ?
K1 O13 2.810(5) 2_665 ?
K1 O12 2.867(5) . ?
K1 O12 2.867(5) 3_565 ?
K1 O12 2.867(5) 2_665 ?
K1 N4 3.023(9) . ?
K1 N3 3.024(9) . ?
K1A O12 2.737(13) . ?
K1A O12 2.737(13) 3_565 ?
K1A O12 2.737(13) 2_665 ?
K1A N3 2.74(3) . ?
K1A O13 2.961(18) 3_565 ?
K1A O13 2.961(18) 2_665 ?
K1A O13 2.961(18) . ?
K1A N4 3.31(3) . ?
K1A C22 3.51(2) . ?
K1A C22 3.51(2) 3_565 ?
K1A C22 3.51(2) 2_665 ?
K1A C21 3.52(3) . ?
N3 C21 1.471(2) . ?
N3 C21 1.471(2) 3_565 ?
N3 C21 1.471(2) 2_665 ?
O12 C23 1.424(2) . ?
O12 C22 1.431(2) . ?
O13 C24 1.426(2) . ?
O13 C25 1.434(2) . ?
N4 C26 1.469(2) . ?
N4 C26 1.469(2) 3_565 ?
N4 C26 1.469(2) 2_665 ?
C21 C22 1.507(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.498(3) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C26 1.508(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?

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 Sn1 N1 100.82(5) . 2_675 ?
N1 Sn1 N1 100.82(5) . 3_465 ?
N1 Sn1 N1 100.82(5) 2_675 3_465 ?
C3 N1 C1 116.15(15) . . ?
C3 N1 Sn1 116.02(12) . . ?
C1 N1 Sn1 121.74(11) . . ?
C2 N2 C2 115.80(10) . 3_465 ?
C2 N2 C2 115.80(10) . 2_675 ?
C2 N2 C2 115.80(10) 3_465 2_675 ?
N1 C1 C2 110.82(15) . . ?
N1 C1 H1A 109.5 . . ?
C2 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
C2 C1 H1B 109.5 . . ?
H1A C1 H1B 108.1 . . ?
N2 C2 C1 111.14(17) . . ?
N2 C2 H2A 109.4 . . ?
C1 C2 H2A 109.4 . . ?
N2 C2 H2B 109.4 . . ?
C1 C2 H2B 109.4 . . ?
H2A C2 H2B 108.0 . . ?
O1 C3 N1 125.58(17) . . ?
O1 C3 C4A 115.1(8) . . ?
N1 C3 C4A 119.2(8) . . ?
O1 C3 C4 116.8(4) . . ?
N1 C3 C4 117.6(4) . . ?
C9 C4 C5 120.3(11) . . ?
C9 C4 C3 120.1(11) . . ?
C5 C4 C3 119.6(10) . . ?
C4 C5 C6 120.7(5) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C7 117.4(10) . . ?
C8 C7 C6 122.3(10) . . ?
C8 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C9 C8 C7 118.1(4) . . ?
C9 C8 C10 124.0(10) . . ?
C7 C8 C10 117.9(10) . . ?
C4 C9 C8 121.1(10) . . ?
C4 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C11 C10 C13 107.3(7) . . ?
C11 C10 C12 99.6(15) . . ?
C13 C10 C12 118.0(12) . . ?
C11 C10 C8 111.5(11) . . ?
C13 C10 C8 112.7(10) . . ?
C12 C10 C8 107.1(4) . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C10 C12 H12A 109.5 . . ?
C10 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C10 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C10 C13 H13A 109.5 . . ?
C10 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C10 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9A C4A C5A 122(2) . . ?
C9A C4A C3 118.5(17) . . ?
C5A C4A C3 119.4(17) . . ?
C6A C5A C4A 118.3(17) . . ?
C6A C5A H5A 120.8 . . ?
C4A C5A H5A 120.8 . . ?
C5A C6A C7A 119.2(19) . . ?
C6A C7A C8A 123(2) . . ?
C6A C7A H7A 118.5 . . ?
C8A C7A H7A 118.5 . . ?
C9A C8A C7A 116.4(14) . . ?
C9A C8A C10A 120.7(16) . . ?
C7A C8A C10A 122.2(17) . . ?
C4A C9A C8A 120.9(18) . . ?
C4A C9A H9A 119.5 . . ?
C8A C9A H9A 119.5 . . ?
C13A C10A C12A 119(2) . . ?
C13A C10A C11A 106(2) . . ?
C12A C10A C11A 100(3) . . ?
C13A C10A C8A 110.4(13) . . ?
C12A C10A C8A 109.8(10) . . ?
C11A C10A C8A 110.6(18) . . ?
C10A C11A H11D 109.5 . . ?
C10A C11A H11E 109.5 . . ?
H11D C11A H11E 109.5 . . ?
C10A C11A H11F 109.5 . . ?
H11D C11A H11F 109.5 . . ?
H11E C11A H11F 109.5 . . ?
C10A C12A H12D 109.5 . . ?
C10A C12A H12E 109.5 . . ?
H12D C12A H12E 109.5 . . ?
C10A C12A H12F 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C10A C13A H13D 109.5 . . ?
C10A C13A H13E 109.5 . . ?
H13D C13A H13E 109.5 . . ?
C10A C13A H13F 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
O13 K1 O13 98.1(2) 3_565 . ?
O13 K1 O13 98.1(2) 3_565 2_665 ?
O13 K1 O13 98.1(2) . 2_665 ?
O13 K1 O12 133.14(4) 3_565 . ?
O13 K1 O12 59.24(4) . . ?
O13 K1 O12 123.71(4) 2_665 . ?
O13 K1 O12 59.24(4) 3_565 3_565 ?
O13 K1 O12 123.71(4) . 3_565 ?
O13 K1 O12 133.14(4) 2_665 3_565 ?
O12 K1 O12 97.6(2) . 3_565 ?
O13 K1 O12 123.71(4) 3_565 2_665 ?
O13 K1 O12 133.14(4) . 2_665 ?
O13 K1 O12 59.24(4) 2_665 2_665 ?
O12 K1 O12 97.6(2) . 2_665 ?
O12 K1 O12 97.6(2) 3_565 2_665 ?
O13 K1 N4 60.68(16) 3_565 . ?
O13 K1 N4 60.68(16) . . ?
O13 K1 N4 60.68(16) 2_665 . ?
O12 K1 N4 119.68(16) . . ?
O12 K1 N4 119.68(16) 3_565 . ?
O12 K1 N4 119.68(16) 2_665 . ?
O13 K1 N3 119.32(16) 3_565 . ?
O13 K1 N3 119.32(16) . . ?
O13 K1 N3 119.32(16) 2_665 . ?
O12 K1 N3 60.32(16) . . ?
O12 K1 N3 60.32(16) 3_565 . ?
O12 K1 N3 60.32(16) 2_665 . ?
N4 K1 N3 180.0 . . ?
O12 K1A O12 104.0(7) . 3_565 ?
O12 K1A O12 104.0(7) . 2_665 ?
O12 K1A O12 104.0(7) 3_565 2_665 ?
O12 K1A N3 65.5(6) . . ?
O12 K1A N3 65.5(6) 3_565 . ?
O12 K1A N3 65.5(6) 2_665 . ?
O12 K1A O13 132.2(2) . 3_565 ?
O12 K1A O13 58.86(11) 3_565 3_565 ?
O12 K1A O13 122.90(19) 2_665 3_565 ?
N3 K1A O13 124.2(5) . 3_565 ?
O12 K1A O13 122.90(19) . 2_665 ?
O12 K1A O13 132.2(2) 3_565 2_665 ?
O12 K1A O13 58.86(11) 2_665 2_665 ?
N3 K1A O13 124.2(5) . 2_665 ?
O13 K1A O13 91.6(7) 3_565 2_665 ?
O12 K1A O13 58.86(11) . . ?
O12 K1A O13 122.90(19) 3_565 . ?
O12 K1A O13 132.2(2) 2_665 . ?
N3 K1A O13 124.2(5) . . ?
O13 K1A O13 91.6(7) 3_565 . ?
O13 K1A O13 91.6(7) 2_665 . ?
O12 K1A N4 114.5(6) . . ?
O12 K1A N4 114.5(6) 3_565 . ?
O12 K1A N4 114.5(6) 2_665 . ?
N3 K1A N4 180.0 . . ?
O13 K1A N4 55.8(5) 3_565 . ?
O13 K1A N4 55.8(5) 2_665 . ?
O13 K1A N4 55.8(5) . . ?
O12 K1A C22 22.4(2) . . ?
O12 K1A C22 85.1(6) 3_565 . ?
O12 K1A C22 97.6(8) 2_665 . ?
N3 K1A C22 45.1(4) . . ?
O13 K1A C22 129.6(2) 3_565 . ?
O13 K1A C22 137.6(2) 2_665 . ?
O13 K1A C22 79.26(15) . . ?
N4 K1A C22 134.9(4) . . ?
O12 K1A C22 97.6(8) . 3_565 ?
O12 K1A C22 22.4(2) 3_565 3_565 ?
O12 K1A C22 85.1(6) 2_665 3_565 ?
N3 K1A C22 45.1(4) . 3_565 ?
O13 K1A C22 79.26(15) 3_565 3_565 ?
O13 K1A C22 129.6(2) 2_665 3_565 ?
O13 K1A C22 137.6(2) . 3_565 ?
N4 K1A C22 134.9(4) . 3_565 ?
C22 K1A C22 75.6(6) . 3_565 ?
O12 K1A C22 85.1(6) . 2_665 ?
O12 K1A C22 97.6(8) 3_565 2_665 ?
O12 K1A C22 22.4(2) 2_665 2_665 ?
N3 K1A C22 45.1(4) . 2_665 ?
O13 K1A C22 137.6(2) 3_565 2_665 ?
O13 K1A C22 79.26(15) 2_665 2_665 ?
O13 K1A C22 129.6(2) . 2_665 ?
N4 K1A C22 134.9(4) . 2_665 ?
C22 K1A C22 75.6(6) . 2_665 ?
C22 K1A C22 75.6(6) 3_565 2_665 ?
O12 K1A C21 42.8(4) . . ?
O12 K1A C21 81.6(7) 3_565 . ?
O12 K1A C21 74.8(7) 2_665 . ?
N3 K1A C21 23.2(2) . . ?
O13 K1A C21 138.8(6) 3_565 . ?
O13 K1A C21 126.4(4) 2_665 . ?
O13 K1A C21 101.7(3) . . ?
N4 K1A C21 156.8(2) . . ?
C22 K1A C21 24.79(19) . . ?
C22 K1A C21 64.6(5) 3_565 . ?
C22 K1A C21 52.4(4) 2_665 . ?
C21 N3 C21 109.40(12) . 3_565 ?
C21 N3 C21 109.40(12) . 2_665 ?
C21 N3 C21 109.40(12) 3_565 2_665 ?
C21 N3 K1A 109.54(12) . . ?
C21 N3 K1A 109.54(12) 3_565 . ?
C21 N3 K1A 109.54(12) 2_665 . ?
C21 N3 K1 109.54(12) . . ?
C21 N3 K1 109.54(12) 3_565 . ?
C21 N3 K1 109.54(12) 2_665 . ?
C23 O12 C22 111.58(14) . . ?
C23 O12 K1A 117.8(5) . . ?
C22 O12 K1A 110.7(6) . . ?
C23 O12 K1 113.23(18) . . ?
C22 O12 K1 115.55(18) . . ?
C24 O13 C25 111.25(15) . . ?
C24 O13 K1 117.72(18) . . ?
C25 O13 K1 112.00(18) . . ?
C24 O13 K1A 113.1(5) . . ?
C25 O13 K1A 116.1(5) . . ?
C26 N4 C26 110.13(13) . 3_565 ?
C26 N4 C26 110.13(13) . 2_665 ?
C26 N4 C26 110.12(13) 3_565 2_665 ?
C26 N4 K1 108.81(14) . . ?
C26 N4 K1 108.81(14) 3_565 . ?
C26 N4 K1 108.81(14) 2_665 . ?
C26 N4 K1A 108.81(14) . . ?
C26 N4 K1A 108.81(14) 3_565 . ?
C26 N4 K1A 108.81(14) 2_665 . ?
N3 C21 C22 113.92(15) . . ?
N3 C21 K1A 47.2(2) . . ?
C22 C21 K1A 77.35(19) . . ?
N3 C21 H21A 108.8 . . ?
C22 C21 H21A 108.8 . . ?
K1A C21 H21A 94.9 . . ?
N3 C21 H21B 108.8 . . ?
C22 C21 H21B 108.8 . . ?
K1A C21 H21B 152.5 . . ?
H21A C21 H21B 107.7 . . ?
O12 C22 C21 109.19(15) . . ?
O12 C22 K1A 46.9(3) . . ?
C21 C22 K1A 77.9(4) . . ?
O12 C22 H22A 109.8 . . ?
C21 C22 H22A 109.8 . . ?
K1A C22 H22A 89.6 . . ?
O12 C22 H22B 109.8 . . ?
C21 C22 H22B 109.8 . . ?
K1A C22 H22B 155.6 . . ?
H22A C22 H22B 108.3 . . ?
O12 C23 C24 108.56(16) . . ?
O12 C23 H23A 110.0 . . ?
C24 C23 H23A 110.0 . . ?
O12 C23 H23B 110.0 . . ?
C24 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
O13 C24 C23 108.59(16) . . ?
O13 C24 H24A 110.0 . . ?
C23 C24 H24A 110.0 . . ?
O13 C24 H24B 110.0 . . ?
C23 C24 H24B 110.0 . . ?
H24A C24 H24B 108.4 . . ?
O13 C25 C26 107.58(17) . . ?
O13 C25 H25A 110.2 . . ?
C26 C25 H25A 110.2 . . ?
O13 C25 H25B 110.2 . . ?
C26 C25 H25B 110.2 . . ?
H25A C25 H25B 108.5 . . ?
N4 C26 C25 112.94(17) . . ?
N4 C26 H26A 109.0 . . ?
C25 C26 H26A 109.0 . . ?
N4 C26 H26B 109.0 . . ?
C25 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?

_refine_diff_density_max         1.307
_refine_diff_density_min         -1.035
_refine_diff_density_rms         0.091


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method DMF/Et2O
####################################################################### 
# 
# 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_x13160_sq
_database_code_depnum_ccdc_archive 'CCDC 1469596'
_audit_update_record             
;
2016-03-20 deposited with the CCDC.
2016-07-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        '[K2(DMF)3][Se6Sn2(mBDCA-5t)]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H60 K2 N8 O7.50 Se6 Sn2'
_chemical_formula_weight         1658.38

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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+1/2, -z'

_cell_length_a                   13.2183(19)
_cell_length_b                   18.536(3)
_cell_length_c                   16.295(2)
_cell_angle_alpha                90
_cell_angle_beta                 113.704(2)
_cell_angle_gamma                90
_cell_volume                     3655.7(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9910
_cell_measurement_theta_min      2.20
_cell_measurement_theta_max      27.48

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_F_000             1612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    3.828
_shelx_estimated_absorpt_T_min   0.546
_shelx_estimated_absorpt_T_max   0.894
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.1025
_exptl_absorpt_correction_T_max  0.1524
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   
'I\mS micro-focus sealed tube, multilayer optics'
_diffrn_measurement_device_type  'Bruker Smart APEX2 CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.3
_diffrn_reflns_number            62975
_diffrn_reflns_av_unetI/netI     0.0766
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         1.365
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14765
_reflns_number_gt                10913
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.938
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
; 
 Reflections were merged by SHELXL according to the crystal 
 class for the calculation of statistics and refinement. 
  
 Structure factors included contributions from the .fab file. 
  
 _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       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_structure_solution    'SHELXS-2015 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
; 
 Refined as a 2-component inversion twin.
 Tructure is plagued by extensive disorder and the overal structre quality 
 is low. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1252P)²+10.9744P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Refined as an inversion twin. 
;
_refine_ls_abs_structure_Flack   0.27(2)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         14765
_refine_ls_number_parameters     1264
_refine_ls_number_restraints     5504
_refine_ls_R_factor_all          0.1017
_refine_ls_R_factor_gt           0.0718
_refine_ls_wR_factor_ref         0.2100
_refine_ls_wR_factor_gt          0.1873
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.009
_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
Sn1 Sn 0.14590(9) -0.00369(5) 0.11464(7) 0.0373(3) Uani 1 1 d D U . . .
Sn2 Sn 0.35013(9) -0.16363(6) 0.36967(7) 0.0426(3) Uani 1 1 d D U . . .
Se1 Se 0.29832(14) -0.08373(9) 0.22704(11) 0.0334(4) Uani 0.893(3) 1 d D U P A
1
Se2 Se 0.3114(2) 0.01153(14) 0.05646(16) 0.0569(6) Uani 0.893(3) 1 d D U P A 1
Se3 Se 0.3168(3) -0.10535(15) 0.00557(19) 0.0725(8) Uani 0.893(3) 1 d D U P A 1
Se4 Se 0.4889(2) -0.15182(16) 0.0999(2) 0.0821(8) Uani 0.893(3) 1 d D U P A 1
Se5 Se 0.4852(3) -0.23060(14) 0.2105(2) 0.0780(8) Uani 0.893(3) 1 d D U P A 1
Se6 Se 0.53935(18) -0.16445(14) 0.34243(17) 0.0619(6) Uani 0.893(3) 1 d D U P A
1
Se1A Se 0.2120(13) -0.0801(7) 0.2604(8) 0.046(3) Uani 0.107(3) 1 d D U P A 2
Se2A Se 0.265(2) -0.0260(15) 0.0373(16) 0.081(5) Uani 0.107(3) 1 d D U P A 2
Se3A Se 0.400(2) -0.0855(15) 0.019(2) 0.113(7) Uani 0.107(3) 1 d D U P A 2
Se4A Se 0.386(2) -0.1971(14) 0.0802(18) 0.109(7) Uani 0.107(3) 1 d D U P A 2
Se5A Se 0.550(2) -0.197(2) 0.2089(16) 0.121(7) Uani 0.107(3) 1 d D U P A 2
Se6A Se 0.4848(18) -0.2089(12) 0.3167(15) 0.077(5) Uani 0.107(3) 1 d D U P A 2
N1 N -0.0128(16) 0.000(2) 0.1339(17) 0.042(4) Uani 0.583(15) 1 d D U P A 1
N5 N 0.214(2) -0.1777(13) 0.417(2) 0.048(4) Uani 0.583(15) 1 d D U P A 1
O1 O -0.096(2) 0.0826(16) 0.187(2) 0.059(9) Uani 0.583(15) 1 d D U P A 1
O4 O 0.197(4) -0.131(2) 0.5358(19) 0.088(10) Uani 0.583(15) 1 d D U P A 1
C1 C -0.102(2) 0.0095(15) 0.0437(18) 0.044(5) Uani 0.583(15) 1 d D U P A 1
H1A H -0.1728 0.0180 0.0498 0.053 Uiso 0.583(15) 1 calc R U P A 1
H1B H -0.1098 -0.0356 0.0092 0.053 Uiso 0.583(15) 1 calc R U P A 1
C2 C -0.0804(17) 0.0722(15) -0.0081(19) 0.049(5) Uani 0.583(15) 1 d D U P A 1
H2A H -0.1355 0.0711 -0.0709 0.058 Uiso 0.583(15) 1 calc R U P A 1
H2B H -0.0891 0.1184 0.0189 0.058 Uiso 0.583(15) 1 calc R U P A 1
C7 C 0.228(2) -0.2518(14) 0.4517(19) 0.049(5) Uani 0.583(15) 1 d D U P A 1
H7A H 0.2186 -0.2861 0.4025 0.059 Uiso 0.583(15) 1 calc R U P A 1
H7B H 0.1714 -0.2625 0.4750 0.059 Uiso 0.583(15) 1 calc R U P A 1
C8 C 0.3432(18) -0.2614(16) 0.5265(18) 0.062(5) Uani 0.583(15) 1 d D U P A 1
H8A H 0.3510 -0.2302 0.5780 0.074 Uiso 0.583(15) 1 calc R U P A 1
H8B H 0.3537 -0.3121 0.5472 0.074 Uiso 0.583(15) 1 calc R U P A 1
C21 C -0.015(2) 0.0410(14) 0.1971(17) 0.041(5) Uani 0.583(15) 1 d D U P A 1
C22 C 0.0577(18) 0.0277(14) 0.2919(16) 0.039(4) Uani 0.583(15) 1 d D U P A 1
C23 C 0.089(2) 0.0860(15) 0.352(2) 0.045(5) Uani 0.583(15) 1 d D U P A 1
H23 H 0.0604 0.1323 0.3288 0.054 Uiso 0.583(15) 1 calc R U P A 1
C24 C 0.158(4) 0.0806(16) 0.442(2) 0.059(6) Uani 0.583(15) 1 d D U P A 1
C25 C 0.194(4) 0.0118(15) 0.473(2) 0.054(6) Uani 0.583(15) 1 d D U P A 1
H25 H 0.2370 0.0056 0.5355 0.065 Uiso 0.583(15) 1 calc R U P A 1
C26 C 0.168(3) -0.0486(13) 0.4180(19) 0.055(6) Uani 0.583(15) 1 d D U P A 1
C27 C 0.102(3) -0.0402(13) 0.3251(17) 0.046(5) Uani 0.583(15) 1 d D U P A 1
H27 H 0.0879 -0.0803 0.2857 0.055 Uiso 0.583(15) 1 calc R U P A 1
C28 C 0.179(3) 0.1516(15) 0.4968(19) 0.068(6) Uani 0.583(15) 1 d D U P A 1
C29 C 0.264(3) 0.135(2) 0.590(2) 0.073(9) Uani 0.583(15) 1 d D U P A 1
H29A H 0.2366 0.0971 0.6171 0.109 Uiso 0.583(15) 1 calc R U P A 1
H29B H 0.3332 0.1197 0.5867 0.109 Uiso 0.583(15) 1 calc R U P A 1
H29C H 0.2781 0.1790 0.6272 0.109 Uiso 0.583(15) 1 calc R U P A 1
C30 C 0.220(4) 0.2106(19) 0.454(3) 0.070(9) Uani 0.583(15) 1 d D U P A 1
H30A H 0.2897 0.1954 0.4510 0.106 Uiso 0.583(15) 1 calc R U P A 1
H30B H 0.1650 0.2202 0.3937 0.106 Uiso 0.583(15) 1 calc R U P A 1
H30C H 0.2332 0.2546 0.4904 0.106 Uiso 0.583(15) 1 calc R U P A 1
C31 C 0.072(3) 0.175(2) 0.502(3) 0.076(8) Uani 0.583(15) 1 d D U P A 1
H31A H 0.0454 0.1372 0.5294 0.114 Uiso 0.583(15) 1 calc R U P A 1
H31B H 0.0853 0.2194 0.5378 0.114 Uiso 0.583(15) 1 calc R U P A 1
H31C H 0.0171 0.1850 0.4411 0.114 Uiso 0.583(15) 1 calc R U P A 1
C32 C 0.200(2) -0.1222(14) 0.4596(19) 0.055(5) Uani 0.583(15) 1 d D U P A 1
N2 N 0.184(3) 0.1103(10) 0.163(2) 0.048(5) Uani 0.583(15) 1 d D U P A 1
N6 N 0.455(3) -0.0917(11) 0.4834(15) 0.060(5) Uani 0.583(15) 1 d D U P A 1
O2 O 0.279(3) 0.2047(14) 0.247(3) 0.074(8) Uani 0.583(15) 1 d D U P A 1
O5 O 0.503(2) 0.0131(10) 0.5653(12) 0.057(5) Uani 0.583(15) 1 d D U P A 1
C3 C 0.107(3) 0.1641(15) 0.1008(18) 0.054(6) Uani 0.583(15) 1 d D U P A 1
H3A H 0.1409 0.2127 0.1124 0.065 Uiso 0.583(15) 1 calc R U P A 1
H3B H 0.0371 0.1662 0.1097 0.065 Uiso 0.583(15) 1 calc R U P A 1
C4 C 0.083(3) 0.1407(11) 0.0051(17) 0.056(6) Uani 0.583(15) 1 d D U P A 1
H4A H 0.0322 0.1750 -0.0385 0.067 Uiso 0.583(15) 1 calc R U P A 1
H4B H 0.1529 0.1390 -0.0043 0.067 Uiso 0.583(15) 1 calc R U P A 1
C9 C 0.484(3) -0.1291(14) 0.5711(18) 0.067(6) Uani 0.583(15) 1 d D U P A 1
H9A H 0.4193 -0.1312 0.5866 0.080 Uiso 0.583(15) 1 calc R U P A 1
H9B H 0.5441 -0.1025 0.6191 0.080 Uiso 0.583(15) 1 calc R U P A 1
C10 C 0.523(2) -0.2050(13) 0.5622(18) 0.064(6) Uani 0.583(15) 1 d D U P A 1
H10A H 0.5860 -0.2032 0.5443 0.077 Uiso 0.583(15) 1 calc R U P A 1
H10B H 0.5461 -0.2311 0.6200 0.077 Uiso 0.583(15) 1 calc R U P A 1
C41 C 0.269(2) 0.1385(14) 0.2280(18) 0.048(5) Uani 0.583(15) 1 d D U P A 1
C42 C 0.366(2) 0.0958(12) 0.2858(16) 0.046(4) Uani 0.583(15) 1 d D U P A 1
C43 C 0.457(3) 0.0946(17) 0.264(2) 0.057(5) Uani 0.583(15) 1 d D U P A 1
H43 H 0.4523 0.1189 0.2110 0.069 Uiso 0.583(15) 1 calc R U P A 1
C44 C 0.554(3) 0.059(2) 0.316(3) 0.064(5) Uani 0.583(15) 1 d D U P A 1
C45 C 0.554(3) 0.019(3) 0.389(3) 0.059(5) Uani 0.583(15) 1 d D U P A 1
H45 H 0.6165 -0.0095 0.4226 0.071 Uiso 0.583(15) 1 calc R U P A 1
C46 C 0.463(2) 0.0214(19) 0.4131(19) 0.051(4) Uani 0.583(15) 1 d D U P A 1
C47 C 0.368(2) 0.056(2) 0.359(2) 0.040(5) Uani 0.583(15) 1 d D U P A 1
H47 H 0.3041 0.0532 0.3717 0.048 Uiso 0.583(15) 1 calc R U P A 1
C48 C 0.654(2) 0.0591(16) 0.2874(19) 0.076(5) Uani 0.583(15) 1 d D U P A 1
C49 C 0.692(3) -0.0180(17) 0.289(3) 0.079(8) Uani 0.583(15) 1 d D U P A 1
H49A H 0.7131 -0.0380 0.3490 0.118 Uiso 0.583(15) 1 calc R U P A 1
H49B H 0.6312 -0.0466 0.2458 0.118 Uiso 0.583(15) 1 calc R U P A 1
H49C H 0.7552 -0.0194 0.2720 0.118 Uiso 0.583(15) 1 calc R U P A 1
C50 C 0.622(3) 0.089(2) 0.193(2) 0.092(9) Uani 0.583(15) 1 d D U P A 1
H50A H 0.5972 0.1390 0.1915 0.138 Uiso 0.583(15) 1 calc R U P A 1
H50B H 0.6854 0.0871 0.1771 0.138 Uiso 0.583(15) 1 calc R U P A 1
H50C H 0.5614 0.0599 0.1509 0.138 Uiso 0.583(15) 1 calc R U P A 1
C51 C 0.742(3) 0.108(2) 0.353(3) 0.079(9) Uani 0.583(15) 1 d D U P A 1
H51A H 0.7131 0.1568 0.3486 0.119 Uiso 0.583(15) 1 calc R U P A 1
H51B H 0.7637 0.0895 0.4138 0.119 Uiso 0.583(15) 1 calc R U P A 1
H51C H 0.8072 0.1084 0.3378 0.119 Uiso 0.583(15) 1 calc R U P A 1
C52 C 0.475(2) -0.0226(12) 0.4927(15) 0.053(5) Uani 0.583(15) 1 d D U P A 1
N3 N 0.057(5) -0.0751(14) -0.0031(14) 0.048(5) Uani 0.583(15) 1 d D U P A 1
N7 N 0.320(3) -0.2758(10) 0.312(2) 0.048(5) Uani 0.583(15) 1 d D U P A 1
O3 O -0.029(2) -0.1760(15) -0.0786(18) 0.062(8) Uani 0.583(15) 1 d D U P A 1
O6 O 0.208(3) -0.3715(13) 0.247(2) 0.060(9) Uani 0.583(15) 1 d D U P A 1
C5 C 0.005(4) -0.0429(14) -0.0944(19) 0.059(7) Uani 0.583(15) 1 d D U P A 1
H5A H -0.0758 -0.0502 -0.1188 0.070 Uiso 0.583(15) 1 calc R U P A 1
H5B H 0.0338 -0.0672 -0.1349 0.070 Uiso 0.583(15) 1 calc R U P A 1
C6 C 0.031(3) 0.0370(13) -0.0900(15) 0.057(5) Uani 0.583(15) 1 d D U P A 1
H6A H 0.1035 0.0443 -0.0931 0.068 Uiso 0.583(15) 1 calc R U P A 1
H6B H -0.0259 0.0618 -0.1419 0.068 Uiso 0.583(15) 1 calc R U P A 1
C11 C 0.385(4) -0.3338(16) 0.373(2) 0.059(7) Uani 0.583(15) 1 d D U P A 1
H11A H 0.4247 -0.3611 0.3431 0.071 Uiso 0.583(15) 1 calc R U P A 1
H11B H 0.3332 -0.3676 0.3838 0.071 Uiso 0.583(15) 1 calc R U P A 1
C12 C 0.467(3) -0.3060(14) 0.4619(19) 0.066(6) Uani 0.583(15) 1 d D U P A 1
H12A H 0.4824 -0.3445 0.5075 0.079 Uiso 0.583(15) 1 calc R U P A 1
H12B H 0.5369 -0.2942 0.4565 0.079 Uiso 0.583(15) 1 calc R U P A 1
C61 C 0.024(3) -0.1411(13) -0.0061(17) 0.052(5) Uani 0.583(15) 1 d D U P A 1
C62 C 0.038(2) -0.1811(12) 0.0765(15) 0.041(4) Uani 0.583(15) 1 d D U P A 1
C63 C -0.048(2) -0.1761(16) 0.105(2) 0.047(5) Uani 0.583(15) 1 d D U P A 1
H63 H -0.1102 -0.1472 0.0715 0.057 Uiso 0.583(15) 1 calc R U P A 1
C64 C -0.046(3) -0.212(2) 0.181(2) 0.052(5) Uani 0.583(15) 1 d D U P A 1
C65 C 0.047(3) -0.254(2) 0.225(3) 0.048(5) Uani 0.583(15) 1 d D U P A 1
H65 H 0.0510 -0.2809 0.2757 0.058 Uiso 0.583(15) 1 calc R U P A 1
C66 C 0.136(2) -0.258(2) 0.198(2) 0.046(4) Uani 0.583(15) 1 d D U P A 1
C67 C 0.135(2) -0.218(2) 0.127(2) 0.043(5) Uani 0.583(15) 1 d D U P A 1
H67 H 0.1977 -0.2157 0.1126 0.052 Uiso 0.583(15) 1 calc R U P A 1
C68 C -0.141(2) -0.2090(15) 0.2108(18) 0.065(5) Uani 0.583(15) 1 d D U P A 1
C69 C -0.227(3) -0.156(2) 0.150(2) 0.084(9) Uani 0.583(15) 1 d D U P A 1
H69A H -0.2532 -0.1720 0.0880 0.126 Uiso 0.583(15) 1 calc R U P A 1
H69B H -0.2895 -0.1538 0.1683 0.126 Uiso 0.583(15) 1 calc R U P A 1
H69C H -0.1938 -0.1080 0.1563 0.126 Uiso 0.583(15) 1 calc R U P A 1
C70 C -0.189(3) -0.2846(17) 0.200(3) 0.078(8) Uani 0.583(15) 1 d D U P A 1
H70A H -0.2177 -0.2988 0.1371 0.117 Uiso 0.583(15) 1 calc R U P A 1
H70B H -0.1310 -0.3185 0.2360 0.117 Uiso 0.583(15) 1 calc R U P A 1
H70C H -0.2489 -0.2854 0.2211 0.117 Uiso 0.583(15) 1 calc R U P A 1
C71 C -0.097(2) -0.1878(18) 0.3079(18) 0.060(7) Uani 0.583(15) 1 d D U P A 1
H71A H -0.0660 -0.1391 0.3150 0.090 Uiso 0.583(15) 1 calc R U P A 1
H71B H -0.1572 -0.1887 0.3285 0.090 Uiso 0.583(15) 1 calc R U P A 1
H71C H -0.0393 -0.2218 0.3434 0.090 Uiso 0.583(15) 1 calc R U P A 1
C72 C 0.227(2) -0.3045(13) 0.2552(18) 0.047(5) Uani 0.583(15) 1 d D U P A 1
N1A N -0.016(2) -0.003(3) 0.129(2) 0.045(4) Uani 0.417(15) 1 d D U P A 2
N5A N 0.222(3) -0.1826(19) 0.423(3) 0.050(4) Uani 0.417(15) 1 d D U P A 2
O1A O -0.115(3) 0.060(2) 0.186(3) 0.051(10) Uani 0.417(15) 1 d D U P A 2
O4A O 0.152(4) -0.145(2) 0.519(3) 0.069(10) Uani 0.417(15) 1 d D U P A 2
C1A C -0.098(4) -0.006(3) 0.034(3) 0.050(6) Uani 0.417(15) 1 d D U P A 2
H1C H -0.1735 -0.0050 0.0329 0.060 Uiso 0.417(15) 1 calc R U P A 2
H1D H -0.0892 -0.0520 0.0068 0.060 Uiso 0.417(15) 1 calc R U P A 2
C2A C -0.0835(19) 0.057(2) -0.020(3) 0.054(6) Uani 0.417(15) 1 d D U P A 2
H2C H -0.1285 0.0483 -0.0846 0.065 Uiso 0.417(15) 1 calc R U P A 2
H2D H -0.1114 0.1016 -0.0029 0.065 Uiso 0.417(15) 1 calc R U P A 2
C7A C 0.230(3) -0.247(2) 0.479(3) 0.062(6) Uani 0.417(15) 1 d D U P A 2
H7C H 0.1742 -0.2825 0.4432 0.074 Uiso 0.417(15) 1 calc R U P A 2
H7D H 0.2142 -0.2329 0.5310 0.074 Uiso 0.417(15) 1 calc R U P A 2
C8A C 0.343(2) -0.280(2) 0.511(3) 0.063(6) Uani 0.417(15) 1 d D U P A 2
H8C H 0.3702 -0.2867 0.5771 0.076 Uiso 0.417(15) 1 calc R U P A 2
H8D H 0.3349 -0.3292 0.4846 0.076 Uiso 0.417(15) 1 calc R U P A 2
C21A C -0.029(3) 0.027(2) 0.195(2) 0.046(5) Uani 0.417(15) 1 d D U P A 2
C22A C 0.044(2) 0.0159(19) 0.291(2) 0.051(6) Uani 0.417(15) 1 d D U P A 2
C23A C 0.076(3) 0.075(2) 0.348(3) 0.051(7) Uani 0.417(15) 1 d D U P A 2
H23A H 0.0506 0.1216 0.3236 0.061 Uiso 0.417(15) 1 calc R U P A 2
C24A C 0.143(5) 0.071(2) 0.439(3) 0.061(6) Uani 0.417(15) 1 d D U P A 2
C25A C 0.178(5) 0.001(2) 0.469(3) 0.055(7) Uani 0.417(15) 1 d D U P A 2
H25A H 0.2215 -0.0060 0.5308 0.067 Uiso 0.417(15) 1 calc R U P A 2
C26A C 0.152(5) -0.0593(17) 0.413(2) 0.054(6) Uani 0.417(15) 1 d D U P A 2
C27A C 0.090(5) -0.0512(19) 0.321(2) 0.055(5) Uani 0.417(15) 1 d D U P A 2
H27A H 0.0793 -0.0903 0.2807 0.066 Uiso 0.417(15) 1 calc R U P A 2
C28A C 0.180(3) 0.135(2) 0.503(3) 0.076(7) Uani 0.417(15) 1 d D U P A 2
C29A C 0.293(4) 0.121(3) 0.579(4) 0.086(12) Uani 0.417(15) 1 d D U P A 2
H29D H 0.2893 0.0763 0.6103 0.128 Uiso 0.417(15) 1 calc R U P A 2
H29E H 0.3486 0.1154 0.5540 0.128 Uiso 0.417(15) 1 calc R U P A 2
H29F H 0.3122 0.1613 0.6207 0.128 Uiso 0.417(15) 1 calc R U P A 2
C30A C 0.187(6) 0.203(2) 0.455(4) 0.084(12) Uani 0.417(15) 1 d D U P A 2
H30D H 0.2425 0.1971 0.4299 0.126 Uiso 0.417(15) 1 calc R U P A 2
H30E H 0.1150 0.2132 0.4067 0.126 Uiso 0.417(15) 1 calc R U P A 2
H30F H 0.2084 0.2432 0.4978 0.126 Uiso 0.417(15) 1 calc R U P A 2
C31A C 0.095(4) 0.142(3) 0.543(4) 0.092(11) Uani 0.417(15) 1 d D U P A 2
H31D H 0.0914 0.0969 0.5730 0.139 Uiso 0.417(15) 1 calc R U P A 2
H31E H 0.1154 0.1817 0.5858 0.139 Uiso 0.417(15) 1 calc R U P A 2
H31F H 0.0221 0.1518 0.4947 0.139 Uiso 0.417(15) 1 calc R U P A 2
C32A C 0.180(3) -0.1320(18) 0.455(2) 0.052(5) Uani 0.417(15) 1 d D U P A 2
N2A N 0.195(5) 0.1094(12) 0.165(3) 0.052(6) Uani 0.417(15) 1 d D U P A 2
N6A N 0.428(3) -0.0868(15) 0.4855(17) 0.056(5) Uani 0.417(15) 1 d D U P A 2
O2A O 0.263(4) 0.202(2) 0.263(3) 0.064(9) Uani 0.417(15) 1 d D U P A 2
O5A O 0.573(3) -0.008(2) 0.558(2) 0.072(8) Uani 0.417(15) 1 d D U P A 2
C3A C 0.097(5) 0.156(2) 0.115(2) 0.055(7) Uani 0.417(15) 1 d D U P A 2
H3C H 0.1159 0.2073 0.1311 0.066 Uiso 0.417(15) 1 calc R U P A 2
H3D H 0.0350 0.1428 0.1315 0.066 Uiso 0.417(15) 1 calc R U P A 2
C4A C 0.065(4) 0.1445(12) 0.015(2) 0.056(6) Uani 0.417(15) 1 d D U P A 2
H4C H 0.0023 0.1763 -0.0198 0.068 Uiso 0.417(15) 1 calc R U P A 2
H4D H 0.1280 0.1565 -0.0005 0.068 Uiso 0.417(15) 1 calc R U P A 2
C9A C 0.443(5) -0.1274(17) 0.568(2) 0.061(6) Uani 0.417(15) 1 d D U P A 2
H9C H 0.3696 -0.1366 0.5697 0.073 Uiso 0.417(15) 1 calc R U P A 2
H9D H 0.4873 -0.0986 0.6218 0.073 Uiso 0.417(15) 1 calc R U P A 2
C10A C 0.501(3) -0.1988(16) 0.569(2) 0.066(7) Uani 0.417(15) 1 d D U P A 2
H10D H 0.5718 -0.1900 0.5644 0.079 Uiso 0.417(15) 1 calc R U P A 2
H10C H 0.5154 -0.2249 0.6259 0.079 Uiso 0.417(15) 1 calc R U P A 2
C41A C 0.269(3) 0.1386(18) 0.237(2) 0.045(6) Uani 0.417(15) 1 d D U P A 2
C42A C 0.368(3) 0.0965(16) 0.294(2) 0.048(5) Uani 0.417(15) 1 d D U P A 2
C43A C 0.459(3) 0.103(2) 0.272(3) 0.059(6) Uani 0.417(15) 1 d D U P A 2
H43A H 0.4522 0.1306 0.2211 0.071 Uiso 0.417(15) 1 calc R U P A 2
C44A C 0.560(4) 0.071(3) 0.322(4) 0.065(5) Uani 0.417(15) 1 d D U P A 2
C45A C 0.563(4) 0.024(3) 0.390(4) 0.059(6) Uani 0.417(15) 1 d D U P A 2
H45A H 0.6289 -0.0012 0.4238 0.071 Uiso 0.417(15) 1 calc R U P A 2
C46A C 0.469(3) 0.014(2) 0.410(3) 0.051(5) Uani 0.417(15) 1 d D U P A 2
C47A C 0.374(3) 0.052(3) 0.365(3) 0.042(6) Uani 0.417(15) 1 d D U P A 2
H47A H 0.3128 0.0482 0.3811 0.050 Uiso 0.417(15) 1 calc R U P A 2
C48A C 0.661(3) 0.072(2) 0.295(2) 0.072(6) Uani 0.417(15) 1 d D U P A 2
C49A C 0.652(4) 0.010(3) 0.231(3) 0.084(10) Uani 0.417(15) 1 d D U P A 2
H49D H 0.5834 0.0144 0.1773 0.126 Uiso 0.417(15) 1 calc R U P A 2
H49E H 0.7153 0.0113 0.2143 0.126 Uiso 0.417(15) 1 calc R U P A 2
H49F H 0.6520 -0.0361 0.2609 0.126 Uiso 0.417(15) 1 calc R U P A 2
C50A C 0.654(4) 0.143(2) 0.248(3) 0.069(9) Uani 0.417(15) 1 d D U P A 2
H50D H 0.5861 0.1450 0.1932 0.103 Uiso 0.417(15) 1 calc R U P A 2
H50E H 0.6552 0.1825 0.2878 0.103 Uiso 0.417(15) 1 calc R U P A 2
H50F H 0.7181 0.1475 0.2316 0.103 Uiso 0.417(15) 1 calc R U P A 2
C51A C 0.765(3) 0.067(3) 0.379(3) 0.084(11) Uani 0.417(15) 1 d D U P A 2
H51D H 0.7683 0.1074 0.4184 0.126 Uiso 0.417(15) 1 calc R U P A 2
H51E H 0.7661 0.0213 0.4098 0.126 Uiso 0.417(15) 1 calc R U P A 2
H51F H 0.8295 0.0687 0.3632 0.126 Uiso 0.417(15) 1 calc R U P A 2
C52A C 0.491(3) -0.0312(16) 0.4905(19) 0.055(6) Uani 0.417(15) 1 d D U P A 2
N3A N 0.067(7) -0.0735(18) -0.0071(17) 0.050(5) Uani 0.417(15) 1 d D U P A 2
N7A N 0.320(5) -0.2785(13) 0.324(3) 0.054(6) Uani 0.417(15) 1 d D U P A 2
O3A O 0.013(3) -0.182(2) -0.079(2) 0.053(8) Uani 0.417(15) 1 d D U P A 2
O6A O 0.233(3) -0.3712(18) 0.230(3) 0.047(9) Uani 0.417(15) 1 d D U P A 2
C5A C 0.035(5) -0.0367(17) -0.095(2) 0.048(6) Uani 0.417(15) 1 d D U P A 2
H5C H -0.0445 -0.0459 -0.1324 0.057 Uiso 0.417(15) 1 calc R U P A 2
H5D H 0.0780 -0.0570 -0.1272 0.057 Uiso 0.417(15) 1 calc R U P A 2
C6A C 0.054(4) 0.0440(17) -0.0843(19) 0.054(5) Uani 0.417(15) 1 d D U P A 2
H6C H 0.1313 0.0552 -0.0749 0.065 Uiso 0.417(15) 1 calc R U P A 2
H6D H 0.0040 0.0694 -0.1390 0.065 Uiso 0.417(15) 1 calc R U P A 2
C11A C 0.407(5) -0.330(2) 0.376(3) 0.062(8) Uani 0.417(15) 1 d D U P A 2
H11C H 0.4478 -0.3456 0.3399 0.075 Uiso 0.417(15) 1 calc R U P A 2
H11D H 0.3730 -0.3729 0.3904 0.075 Uiso 0.417(15) 1 calc R U P A 2
C12A C 0.488(3) -0.2960(18) 0.463(2) 0.062(6) Uani 0.417(15) 1 d D U P A 2
H12C H 0.5194 -0.3336 0.5099 0.074 Uiso 0.417(15) 1 calc R U P A 2
H12D H 0.5499 -0.2727 0.4535 0.074 Uiso 0.417(15) 1 calc R U P A 2
C61A C 0.046(3) -0.1422(17) -0.009(2) 0.047(5) Uani 0.417(15) 1 d D U P A 2
C62A C 0.056(3) -0.1840(15) 0.071(2) 0.044(5) Uani 0.417(15) 1 d D U P A 2
C63A C -0.035(3) -0.182(2) 0.093(3) 0.048(6) Uani 0.417(15) 1 d D U P A 2
H63A H -0.0979 -0.1550 0.0555 0.058 Uiso 0.417(15) 1 calc R U P A 2
C64A C -0.040(4) -0.216(3) 0.167(3) 0.052(5) Uani 0.417(15) 1 d D U P A 2
C65A C 0.051(4) -0.260(3) 0.215(3) 0.052(6) Uani 0.417(15) 1 d D U P A 2
H65A H 0.0478 -0.2908 0.2605 0.063 Uiso 0.417(15) 1 calc R U P A 2
C66A C 0.146(3) -0.260(3) 0.197(3) 0.048(5) Uani 0.417(15) 1 d D U P A 2
C67A C 0.149(3) -0.223(3) 0.124(3) 0.049(6) Uani 0.417(15) 1 d D U P A 2
H67A H 0.2129 -0.2236 0.1115 0.059 Uiso 0.417(15) 1 calc R U P A 2
C68A C -0.147(3) -0.2144(18) 0.183(2) 0.065(6) Uani 0.417(15) 1 d D U P A 2
C69A C -0.176(4) -0.1354(19) 0.188(4) 0.071(10) Uani 0.417(15) 1 d D U P A 2
H69D H -0.1902 -0.1120 0.1301 0.106 Uiso 0.417(15) 1 calc R U P A 2
H69E H -0.2420 -0.1322 0.2006 0.106 Uiso 0.417(15) 1 calc R U P A 2
H69F H -0.1140 -0.1113 0.2352 0.106 Uiso 0.417(15) 1 calc R U P A 2
C70A C -0.242(3) -0.249(3) 0.105(3) 0.077(10) Uani 0.417(15) 1 d D U P A 2
H70D H -0.2535 -0.2221 0.0495 0.115 Uiso 0.417(15) 1 calc R U P A 2
H70E H -0.2232 -0.2990 0.0980 0.115 Uiso 0.417(15) 1 calc R U P A 2
H70F H -0.3091 -0.2471 0.1158 0.115 Uiso 0.417(15) 1 calc R U P A 2
C71A C -0.124(4) -0.253(3) 0.270(3) 0.074(9) Uani 0.417(15) 1 d D U P A 2
H71D H -0.0631 -0.2287 0.3183 0.111 Uiso 0.417(15) 1 calc R U P A 2
H71E H -0.1905 -0.2511 0.2829 0.111 Uiso 0.417(15) 1 calc R U P A 2
H71F H -0.1046 -0.3029 0.2651 0.111 Uiso 0.417(15) 1 calc R U P A 2
C72A C 0.238(3) -0.3057(18) 0.254(2) 0.049(6) Uani 0.417(15) 1 d D U P A 2
N4 N 0.0332(11) 0.0683(6) -0.0067(9) 0.053(3) Uani 1 1 d D U . . .
N8 N 0.4269(11) -0.2418(7) 0.4922(9) 0.060(3) Uani 1 1 d D U . . .
K1 K 0.1454(7) 0.3157(3) 0.2450(4) 0.115(3) Uani 1 1 d D U . . .
K2 K 0.3174(7) 0.5054(3) 0.2799(3) 0.106(2) Uani 1 1 d D U . . .
O1S O 0.210(2) 0.4287(10) 0.3627(16) 0.119(7) Uani 0.75 1 d D U P A .
O2S O 0.291(2) 0.3801(10) 0.1866(17) 0.124(7) Uani 0.75 1 d D U P A .


_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
Sn1 N3 2.235(16) . ?
Sn1 N1A 2.24(2) . ?
Sn1 N2 2.243(16) . ?
Sn1 N1 2.243(17) . ?
Sn1 N3A 2.245(19) . ?
Sn1 N2A 2.250(19) . ?
Sn1 N4 2.354(14) . ?
Sn1 Se2A 2.418(17) . ?
Sn1 Se1 2.5784(19) . ?
Sn1 Se1A 2.597(11) . ?
Sn1 Se2 2.727(3) . ?
Sn2 N5A 2.23(2) . ?
Sn2 N7A 2.239(19) . ?
Sn2 N5 2.241(18) . ?
Sn2 N7 2.248(17) . ?
Sn2 N6 2.251(16) . ?
Sn2 N6A 2.256(19) . ?
Sn2 N8 2.343(14) . ?
Sn2 Se6A 2.420(17) . ?
Sn2 Se1A 2.507(11) . ?
Sn2 Se1 2.605(2) . ?
Sn2 Se6 2.710(3) . ?
Se2 Se3 2.331(4) . ?
Se3 Se4 2.338(4) . ?
Se4 Se5 2.336(5) . ?
Se5 Se6 2.323(4) . ?
Se1A C27A 2.27(6) . ?
Se2A Se3A 2.22(2) . ?
Se3A Se4A 2.34(2) . ?
Se4A Se5A 2.34(2) . ?
Se5A Se6A 2.26(2) . ?
N1 C21 1.285(19) . ?
N1 C1 1.48(2) . ?
N5 C32 1.30(2) . ?
N5 C7 1.47(2) . ?
O1 C21 1.267(19) . ?
O4 C32 1.27(2) . ?
C1 C2 1.53(2) . ?
C2 N4 1.495(19) . ?
C7 C8 1.53(2) . ?
C8 N8 1.47(2) . ?
C21 C22 1.476(19) . ?
C22 C23 1.401(19) . ?
C22 C27 1.402(19) . ?
C23 C24 1.39(2) . ?
C24 C25 1.38(2) . ?
C24 C28 1.56(3) . ?
C25 C26 1.39(2) . ?
C26 C27 1.420(19) . ?
C26 C32 1.505(19) . ?
C28 C30 1.51(2) . ?
C28 C31 1.51(2) . ?
C28 C29 1.52(2) . ?
N2 C41 1.302(19) . ?
N2 C3 1.49(2) . ?
N6 C52 1.305(19) . ?
N6 C9 1.49(2) . ?
O2 C41 1.259(18) . ?
O2 K1 2.70(3) . ?
O5 C52 1.274(19) . ?
O5 K2 2.68(2) 2_646 ?
C3 C4 1.53(2) . ?
C4 N4 1.475(19) . ?
C9 C10 1.52(2) . ?
C10 N8 1.486(19) . ?
C41 C42 1.479(19) . ?
C42 C43 1.39(2) . ?
C42 C47 1.393(19) . ?
C43 C44 1.39(2) . ?
C44 C45 1.40(2) . ?
C44 C48 1.57(3) . ?
C45 C46 1.41(2) . ?
C46 C47 1.368(19) . ?
C46 C52 1.486(19) . ?
C48 C49 1.51(2) . ?
C48 C50 1.52(2) . ?
C48 C51 1.52(2) . ?
N3 C61 1.297(18) . ?
N3 C5 1.49(2) . ?
N7 C72 1.318(19) . ?
N7 C11 1.48(2) . ?
O3 C61 1.279(19) . ?
O3 K1 2.53(3) 2_545 ?
O6 C72 1.264(19) . ?
O6 K2 2.64(3) 1_545 ?
C5 C6 1.52(2) . ?
C6 N4 1.464(19) . ?
C11 C12 1.51(2) . ?
C11 K2 3.30(3) 1_545 ?
C12 N8 1.466(19) . ?
C61 C62 1.481(19) . ?
C62 C67 1.391(18) . ?
C62 C63 1.39(2) . ?
C63 C64 1.39(2) . ?
C64 C65 1.39(2) . ?
C64 C68 1.52(3) . ?
C65 C66 1.40(2) . ?
C66 C67 1.376(19) . ?
C66 C72 1.473(19) . ?
C68 C71 1.50(2) . ?
C68 C70 1.52(2) . ?
C68 C69 1.53(2) . ?
N1A C21A 1.29(2) . ?
N1A C1A 1.49(2) . ?
N5A C32A 1.29(2) . ?
N5A C7A 1.47(2) . ?
O1A C21A 1.26(2) . ?
O4A C32A 1.27(2) . ?
C1A C2A 1.53(2) . ?
C2A N4 1.48(2) . ?
C7A C8A 1.50(2) . ?
C8A N8 1.46(2) . ?
C21A C22A 1.48(2) . ?
C22A C27A 1.38(2) . ?
C22A C23A 1.40(2) . ?
C23A C24A 1.39(2) . ?
C24A C25A 1.39(2) . ?
C24A C28A 1.52(4) . ?
C25A C26A 1.39(2) . ?
C26A C27A 1.41(2) . ?
C26A C32A 1.49(2) . ?
C28A C30A 1.51(2) . ?
C28A C31A 1.52(2) . ?
C28A C29A 1.53(2) . ?
N2A C41A 1.31(2) . ?
N2A C3A 1.49(2) . ?
N6A C52A 1.30(2) . ?
N6A C9A 1.49(2) . ?
O2A C41A 1.26(2) . ?
O2A K1 2.57(4) . ?
O5A C52A 1.27(2) . ?
O5A K2 2.46(3) 2_646 ?
C3A C4A 1.53(2) . ?
C4A N4 1.48(2) . ?
C9A C10A 1.53(2) . ?
C10A N8 1.47(2) . ?
C41A C42A 1.48(2) . ?
C42A C43A 1.39(2) . ?
C42A C47A 1.39(2) . ?
C43A C44A 1.39(2) . ?
C44A C45A 1.39(2) . ?
C44A C48A 1.56(4) . ?
C45A C46A 1.41(2) . ?
C46A C47A 1.37(2) . ?
C46A C52A 1.49(2) . ?
C48A C51A 1.51(2) . ?
C48A C49A 1.51(2) . ?
C48A C50A 1.52(2) . ?
N3A C61A 1.30(2) . ?
N3A C5A 1.49(2) . ?
N7A C72A 1.31(2) . ?
N7A C11A 1.48(2) . ?
O3A C61A 1.27(2) . ?
O3A K1 2.68(4) 2_545 ?
O6A C72A 1.27(2) . ?
O6A K2 2.53(4) 1_545 ?
C5A C6A 1.52(2) . ?
C6A N4 1.47(2) . ?
C11A C12A 1.53(2) . ?
C11A K2 3.42(4) 1_545 ?
C12A N8 1.48(2) . ?
C61A C62A 1.48(2) . ?
C62A C67A 1.38(2) . ?
C62A C63A 1.40(2) . ?
C63A C64A 1.39(2) . ?
C64A C65A 1.40(2) . ?
C64A C68A 1.53(4) . ?
C65A C66A 1.40(2) . ?
C66A C67A 1.38(2) . ?
C66A C72A 1.47(2) . ?
C68A C71A 1.50(2) . ?
C68A C70A 1.52(2) . ?
C68A C69A 1.52(2) . ?
K1 O3 2.53(3) 2 ?
K1 O3A 2.68(4) 2 ?
K1 O1S 2.735(18) . ?
K1 O2S 2.74(2) . ?
K1 K2 4.102(11) . ?
K2 O5A 2.46(3) 2_656 ?
K2 O6A 2.53(4) 1_565 ?
K2 O6 2.64(3) 1_565 ?
K2 O5 2.68(2) 2_656 ?
K2 O2S 2.720(19) . ?
K2 O1S 2.72(2) . ?
K2 C11 3.30(3) 1_565 ?
K2 C11A 3.42(4) 1_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
N3 Sn1 N2 145.8(11) . . ?
N3 Sn1 N1 86.8(18) . . ?
N2 Sn1 N1 90.3(17) . . ?
N1A Sn1 N3A 88(3) . . ?
N1A Sn1 N2A 96(2) . . ?
N3A Sn1 N2A 145.4(16) . . ?
N3 Sn1 N4 71.2(10) . . ?
N1A Sn1 N4 77.0(12) . . ?
N2 Sn1 N4 74.9(7) . . ?
N1 Sn1 N4 77.7(9) . . ?
N3A Sn1 N4 70.8(13) . . ?
N2A Sn1 N4 76.7(9) . . ?
N1A Sn1 Se2A 154.7(13) . . ?
N3A Sn1 Se2A 67(2) . . ?
N2A Sn1 Se2A 101(2) . . ?
N4 Sn1 Se2A 89.1(6) . . ?
N3 Sn1 Se1 105.0(11) . . ?
N2 Sn1 Se1 107.0(7) . . ?
N1 Sn1 Se1 115.4(8) . . ?
N4 Sn1 Se1 166.6(3) . . ?
N1A Sn1 Se1A 83.9(12) . . ?
N3A Sn1 Se1A 111.1(9) . . ?
N2A Sn1 Se1A 103.5(13) . . ?
N4 Sn1 Se1A 160.8(5) . . ?
Se2A Sn1 Se1A 109.5(7) . . ?
N3 Sn1 Se2 88.8(15) . . ?
N2 Sn1 Se2 86.0(15) . . ?
N1 Sn1 Se2 166.2(8) . . ?
N4 Sn1 Se2 88.5(3) . . ?
Se1 Sn1 Se2 78.43(7) . . ?
N5A Sn2 N7A 85(2) . . ?
N5 Sn2 N7 90.1(15) . . ?
N5 Sn2 N6 95.8(13) . . ?
N7 Sn2 N6 146.8(9) . . ?
N5A Sn2 N6A 86.4(17) . . ?
N7A Sn2 N6A 147.2(14) . . ?
N5A Sn2 N8 72.8(11) . . ?
N7A Sn2 N8 69.8(12) . . ?
N5 Sn2 N8 76.6(8) . . ?
N7 Sn2 N8 74.1(9) . . ?
N6 Sn2 N8 75.6(7) . . ?
N6A Sn2 N8 77.4(9) . . ?
N5A Sn2 Se6A 150.6(11) . . ?
N7A Sn2 Se6A 67(2) . . ?
N6A Sn2 Se6A 111.2(13) . . ?
N8 Sn2 Se6A 87.8(6) . . ?
N5A Sn2 Se1A 85.6(11) . . ?
N7A Sn2 Se1A 111.6(9) . . ?
N6A Sn2 Se1A 99.4(10) . . ?
N8 Sn2 Se1A 158.3(5) . . ?
Se6A Sn2 Se1A 113.0(6) . . ?
N5 Sn2 Se1 114.4(7) . . ?
N7 Sn2 Se1 102.5(9) . . ?
N6 Sn2 Se1 104.6(6) . . ?
N8 Sn2 Se1 168.7(4) . . ?
N5 Sn2 Se6 168.0(7) . . ?
N7 Sn2 Se6 87.0(12) . . ?
N6 Sn2 Se6 80.5(10) . . ?
N8 Sn2 Se6 91.4(4) . . ?
Se1 Sn2 Se6 77.64(7) . . ?
Sn1 Se1 Sn2 144.20(8) . . ?
Se3 Se2 Sn1 99.84(12) . . ?
Se2 Se3 Se4 105.62(15) . . ?
Se5 Se4 Se3 114.89(16) . . ?
Se6 Se5 Se4 106.86(15) . . ?
Se5 Se6 Sn2 101.13(12) . . ?
C27A Se1A Sn2 106.3(10) . . ?
C27A Se1A Sn1 103.4(10) . . ?
Sn2 Se1A Sn1 150.2(8) . . ?
Se3A Se2A Sn1 152.1(13) . . ?
Se2A Se3A Se4A 100.2(13) . . ?
Se5A Se4A Se3A 100.4(14) . . ?
Se6A Se5A Se4A 100.9(13) . . ?
Se5A Se6A Sn2 144.3(12) . . ?
C21 N1 C1 118(2) . . ?
C21 N1 Sn1 117(2) . . ?
C1 N1 Sn1 106.5(16) . . ?
C32 N5 C7 124(2) . . ?
C32 N5 Sn2 114(2) . . ?
C7 N5 Sn2 104.1(16) . . ?
N1 C1 C2 112(2) . . ?
N4 C2 C1 111.4(18) . . ?
N5 C7 C8 111(2) . . ?
N8 C8 C7 109.0(19) . . ?
O1 C21 N1 122(2) . . ?
O1 C21 C22 113.7(19) . . ?
N1 C21 C22 121.7(18) . . ?
C23 C22 C27 117.7(17) . . ?
C23 C22 C21 118.9(18) . . ?
C27 C22 C21 123.3(17) . . ?
C24 C23 C22 124(2) . . ?
C25 C24 C23 116(2) . . ?
C25 C24 C28 127(2) . . ?
C23 C24 C28 116(2) . . ?
C24 C25 C26 123(2) . . ?
C25 C26 C27 119.2(17) . . ?
C25 C26 C32 119.1(18) . . ?
C27 C26 C32 121.3(17) . . ?
C22 C27 C26 119.5(16) . . ?
C30 C28 C31 109(2) . . ?
C30 C28 C29 110(2) . . ?
C31 C28 C29 110(2) . . ?
C30 C28 C24 111(2) . . ?
C31 C28 C24 109(3) . . ?
C29 C28 C24 108(2) . . ?
O4 C32 N5 119(2) . . ?
O4 C32 C26 117(2) . . ?
N5 C32 C26 123(2) . . ?
C41 N2 C3 114(2) . . ?
C41 N2 Sn1 131.4(19) . . ?
C3 N2 Sn1 113.2(15) . . ?
C52 N6 C9 112.4(19) . . ?
C52 N6 Sn2 134.9(17) . . ?
C9 N6 Sn2 110.6(15) . . ?
C41 O2 K1 137(3) . . ?
C52 O5 K2 131.6(18) . 2_646 ?
N2 C3 C4 108(2) . . ?
N4 C4 C3 106.7(19) . . ?
N6 C9 C10 108(2) . . ?
N8 C10 C9 106.4(19) . . ?
O2 C41 N2 124(2) . . ?
O2 C41 C42 112.8(19) . . ?
N2 C41 C42 123.1(17) . . ?
C43 C42 C47 119.4(17) . . ?
C43 C42 C41 117.6(19) . . ?
C47 C42 C41 123.0(19) . . ?
C42 C43 C44 122(2) . . ?
C43 C44 C45 117(2) . . ?
C43 C44 C48 120(2) . . ?
C45 C44 C48 123(2) . . ?
C44 C45 C46 121(2) . . ?
C47 C46 C45 119.9(18) . . ?
C47 C46 C52 124.6(19) . . ?
C45 C46 C52 115.2(19) . . ?
C46 C47 C42 119.9(17) . . ?
C49 C48 C50 109(2) . . ?
C49 C48 C51 113(2) . . ?
C50 C48 C51 109(2) . . ?
C49 C48 C44 108(2) . . ?
C50 C48 C44 112(2) . . ?
C51 C48 C44 107(2) . . ?
O5 C52 N6 126(2) . . ?
O5 C52 C46 114(2) . . ?
N6 C52 C46 119(2) . . ?
C61 N3 C5 109.0(19) . . ?
C61 N3 Sn1 130.2(18) . . ?
C5 N3 Sn1 119.5(15) . . ?
C72 N7 C11 108(2) . . ?
C72 N7 Sn2 129(2) . . ?
C11 N7 Sn2 115.9(15) . . ?
C61 O3 K1 153(2) . 2_545 ?
C72 O6 K2 139(2) . 1_545 ?
N3 C5 C6 109.8(19) . . ?
N4 C6 C5 110.6(19) . . ?
N7 C11 C12 113(2) . . ?
N7 C11 K2 112.0(13) . 1_545 ?
C12 C11 K2 134.9(17) . 1_545 ?
N8 C12 C11 113(2) . . ?
O3 C61 N3 124(2) . . ?
O3 C61 C62 114.2(17) . . ?
N3 C61 C62 121.4(17) . . ?
C67 C62 C63 121.1(17) . . ?
C67 C62 C61 122.3(18) . . ?
C63 C62 C61 116.5(18) . . ?
C64 C63 C62 123(2) . . ?
C63 C64 C65 115(2) . . ?
C63 C64 C68 123(2) . . ?
C65 C64 C68 121(2) . . ?
C64 C65 C66 123(2) . . ?
C67 C66 C65 120.6(17) . . ?
C67 C66 C72 124.9(18) . . ?
C65 C66 C72 114.4(18) . . ?
C66 C67 C62 117.1(17) . . ?
C71 C68 C70 109(2) . . ?
C71 C68 C64 109(2) . . ?
C70 C68 C64 107(2) . . ?
C71 C68 C69 112(2) . . ?
C70 C68 C69 111(2) . . ?
C64 C68 C69 108(2) . . ?
O6 C72 N7 124(2) . . ?
O6 C72 C66 116(2) . . ?
N7 C72 C66 120(2) . . ?
C21A N1A C1A 127(3) . . ?
C21A N1A Sn1 123(3) . . ?
C1A N1A Sn1 103(2) . . ?
C32A N5A C7A 106(3) . . ?
C32A N5A Sn2 124(3) . . ?
C7A N5A Sn2 119(2) . . ?
N1A C1A C2A 111(3) . . ?
N4 C2A C1A 113(2) . . ?
N5A C7A C8A 112(2) . . ?
N8 C8A C7A 117(2) . . ?
O1A C21A N1A 122(3) . . ?
O1A C21A C22A 112(2) . . ?
N1A C21A C22A 125(2) . . ?
C27A C22A C23A 120(2) . . ?
C27A C22A C21A 120(2) . . ?
C23A C22A C21A 120(2) . . ?
C24A C23A C22A 124(2) . . ?
C23A C24A C25A 114(2) . . ?
C23A C24A C28A 125(3) . . ?
C25A C24A C28A 121(3) . . ?
C26A C25A C24A 124(2) . . ?
C25A C26A C27A 120(2) . . ?
C25A C26A C32A 119(2) . . ?
C27A C26A C32A 121(2) . . ?
C22A C27A C26A 117.6(19) . . ?
C22A C27A Se1A 110(3) . . ?
C26A C27A Se1A 103(3) . . ?
C30A C28A C31A 111(3) . . ?
C30A C28A C24A 112(3) . . ?
C31A C28A C24A 106(3) . . ?
C30A C28A C29A 108(2) . . ?
C31A C28A C29A 108(3) . . ?
C24A C28A C29A 111(3) . . ?
O4A C32A N5A 120(3) . . ?
O4A C32A C26A 116(2) . . ?
N5A C32A C26A 123(2) . . ?
C41A N2A C3A 115(3) . . ?
C41A N2A Sn1 136(2) . . ?
C3A N2A Sn1 106(2) . . ?
C52A N6A C9A 120(3) . . ?
C52A N6A Sn2 128(2) . . ?
C9A N6A Sn2 106.7(19) . . ?
C41A O2A K1 147(3) . . ?
C52A O5A K2 153(3) . 2_646 ?
N2A C3A C4A 108(3) . . ?
N4 C4A C3A 109(2) . . ?
N6A C9A C10A 109(3) . . ?
N8 C10A C9A 108(2) . . ?
O2A C41A N2A 124(3) . . ?
O2A C41A C42A 116(2) . . ?
N2A C41A C42A 120(2) . . ?
C43A C42A C47A 120(2) . . ?
C43A C42A C41A 116(2) . . ?
C47A C42A C41A 124(2) . . ?
C44A C43A C42A 123(2) . . ?
C43A C44A C45A 116(3) . . ?
C43A C44A C48A 124(3) . . ?
C45A C44A C48A 119(3) . . ?
C44A C45A C46A 121(2) . . ?
C47A C46A C45A 121(2) . . ?
C47A C46A C52A 125(2) . . ?
C45A C46A C52A 114(2) . . ?
C46A C47A C42A 118.7(19) . . ?
C51A C48A C49A 111(3) . . ?
C51A C48A C50A 111(3) . . ?
C49A C48A C50A 110(2) . . ?
C51A C48A C44A 108(3) . . ?
C49A C48A C44A 110(3) . . ?
C50A C48A C44A 106(3) . . ?
O5A C52A N6A 128(3) . . ?
O5A C52A C46A 112(2) . . ?
N6A C52A C46A 120(2) . . ?
C61A N3A C5A 117(2) . . ?
C61A N3A Sn1 127(2) . . ?
C5A N3A Sn1 116.1(17) . . ?
C72A N7A C11A 116(2) . . ?
C72A N7A Sn2 129(2) . . ?
C11A N7A Sn2 115(2) . . ?
C61A O3A K1 140(3) . 2_545 ?
C72A O6A K2 144(3) . 1_545 ?
N3A C5A C6A 112(2) . . ?
N4 C6A C5A 109(2) . . ?
N7A C11A C12A 112(2) . . ?
N7A C11A K2 105.2(18) . 1_545 ?
C12A C11A K2 141(2) . 1_545 ?
N8 C12A C11A 108(2) . . ?
O3A C61A N3A 126(3) . . ?
O3A C61A C62A 111(2) . . ?
N3A C61A C62A 123(2) . . ?
C67A C62A C63A 120(2) . . ?
C67A C62A C61A 125(2) . . ?
C63A C62A C61A 116(2) . . ?
C64A C63A C62A 124(2) . . ?
C63A C64A C65A 115(2) . . ?
C63A C64A C68A 120(3) . . ?
C65A C64A C68A 124(3) . . ?
C64A C65A C66A 122(2) . . ?
C67A C66A C65A 121(2) . . ?
C67A C66A C72A 122(2) . . ?
C65A C66A C72A 117(2) . . ?
C62A C67A C66A 118.2(19) . . ?
C71A C68A C70A 112(2) . . ?
C71A C68A C69A 111(2) . . ?
C70A C68A C69A 108(2) . . ?
C71A C68A C64A 107(3) . . ?
C70A C68A C64A 111(3) . . ?
C69A C68A C64A 107(3) . . ?
O6A C72A N7A 124(3) . . ?
O6A C72A C66A 115(2) . . ?
N7A C72A C66A 121(2) . . ?
C6 N4 C4 108.7(17) . . ?
C6A N4 C4A 112(2) . . ?
C6A N4 C2A 112(2) . . ?
C4A N4 C2A 110(2) . . ?
C6 N4 C2 111.1(18) . . ?
C4 N4 C2 110.8(18) . . ?
C6 N4 Sn1 108.9(14) . . ?
C6A N4 Sn1 106.0(16) . . ?
C4 N4 Sn1 107.8(13) . . ?
C4A N4 Sn1 108.5(15) . . ?
C2A N4 Sn1 108.3(14) . . ?
C2 N4 Sn1 109.4(12) . . ?
C12 N8 C8 110.8(19) . . ?
C8A N8 C10A 113(2) . . ?
C8A N8 C12A 107(2) . . ?
C10A N8 C12A 112(2) . . ?
C12 N8 C10 108.6(17) . . ?
C8 N8 C10 111.2(19) . . ?
C8A N8 Sn2 112.4(14) . . ?
C12 N8 Sn2 107.8(14) . . ?
C8 N8 Sn2 110.0(12) . . ?
C10A N8 Sn2 107.6(15) . . ?
C12A N8 Sn2 104.7(16) . . ?
C10 N8 Sn2 108.3(13) . . ?
O2A K1 O3A 108.7(13) . 2 ?
O3 K1 O2 100.0(11) 2 . ?
O3 K1 O1S 126.1(9) 2 . ?
O2A K1 O1S 123.0(11) . . ?
O3A K1 O1S 126.4(10) 2 . ?
O2 K1 O1S 123.8(9) . . ?
O3 K1 O2S 79.1(10) 2 . ?
O2A K1 O2S 85.5(15) . . ?
O3A K1 O2S 90.6(11) 2 . ?
O2 K1 O2S 78.0(11) . . ?
O1S K1 O2S 81.1(7) . . ?
O3 K1 K2 99.3(7) 2 . ?
O2A K1 K2 114.3(12) . . ?
O3A K1 K2 106.8(8) 2 . ?
O2 K1 K2 109.2(9) . . ?
O1S K1 K2 41.1(5) . . ?
O2S K1 K2 41.1(4) . . ?
O5A K2 O6A 115.3(13) 2_656 1_565 ?
O6 K2 O5 110.4(8) 1_565 2_656 ?
O5A K2 O2S 113.7(10) 2_656 . ?
O6A K2 O2S 130.6(11) 1_565 . ?
O6 K2 O2S 133.5(9) 1_565 . ?
O5 K2 O2S 116.0(8) 2_656 . ?
O5A K2 O1S 67.3(12) 2_656 . ?
O6A K2 O1S 112.3(12) 1_565 . ?
O6 K2 O1S 101.5(10) 1_565 . ?
O5 K2 O1S 90.1(8) 2_656 . ?
O2S K2 O1S 81.6(7) . . ?
O6 K2 C11 48.3(8) 1_565 1_565 ?
O5 K2 C11 63.1(7) 2_656 1_565 ?
O2S K2 C11 168.1(11) . 1_565 ?
O1S K2 C11 110.0(10) . 1_565 ?
O5A K2 C11A 69.6(12) 2_656 1_565 ?
O6A K2 C11A 50.7(10) 1_565 1_565 ?
O2S K2 C11A 164.2(14) . 1_565 ?
O1S K2 C11A 113.2(14) . 1_565 ?
O5A K2 K1 96.7(11) 2_656 . ?
O6A K2 K1 125.6(9) 1_565 . ?
O6 K2 K1 119.1(7) 1_565 . ?
O5 K2 K1 114.0(5) 2_656 . ?
O2S K2 K1 41.4(5) . . ?
O1S K2 K1 41.4(4) . . ?
C11 K2 K1 150.5(10) 1_565 . ?
C11A K2 K1 154.1(14) 1_565 . ?
K2 O1S K1 97.5(7) . . ?
K2 O2S K1 97.5(8) . . ?

_refine_diff_density_max         1.928
_refine_diff_density_min         -1.128
_refine_diff_density_rms         0.179

_shelxl_version_number           2014/6



_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'DMF, Et2O'
