# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_5

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C15 H30 N2 Pb Se Si2'
_chemical_formula_sum            'C15 H30 N2 Pb Se Si2'
_chemical_formula_weight         580.74
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8755(2)
_cell_length_b                   12.2474(2)
_cell_length_c                   13.0612(2)
_cell_angle_alpha                63.6070(10)
_cell_angle_beta                 70.8920(10)
_cell_angle_gamma                75.5130(10)
_cell_volume                     1192.50(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9034
_cell_measurement_theta_min      3.07
_cell_measurement_theta_max      27.47
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.07
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             556
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    8.698
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.305
_exptl_absorpt_correction_T_max  0.544


#----------------------------------------------------------------------------#
#                   SQUEEZE RESULTS                                          #
#----------------------------------------------------------------------------#

# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.370 0.401 0.993 284 52 ' '
_platon_squeeze_details          ?

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0432
_diffrn_reflns_number            8413
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_reflns_number_total             5371
_reflns_number_gt                4938
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0397P)²+0.5851P] 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_number_reflns         5371
_refine_ls_number_parameters     198
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.027
_refine_ls_wR_factor_ref         0.0813
_refine_ls_wR_factor_gt          0.0803
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_restrained_S_all      1.139
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.193
_refine_diff_density_min         -1.01
_refine_diff_density_rms         0.232

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Si Si 0.0817 0.0704 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.75165(2) 0.968021(15) 0.609292(15) 0.01913(7) Uani 1 1 d . . .
Se2 Se 0.92705(6) 1.15218(4) 0.55435(4) 0.02241(11) Uani 1 1 d . . .
Si1 Si 0.65122(17) 0.73149(12) 0.86728(12) 0.0240(3) Uani 1 1 d . . .
Si2 Si 0.89157(17) 0.87637(12) 0.85898(12) 0.0232(3) Uani 1 1 d . . .
N1 N 0.7736(5) 0.8475(4) 0.7947(3) 0.0213(8) Uani 1 1 d . . .
C2 C 0.5376(7) 0.7327(5) 0.7678(5) 0.0365(13) Uani 1 1 d . . .
H2A H 0.4763 0.8138 0.7373 0.055 Uiso 1 1 calc R . .
H2B H 0.4638 0.6702 0.8125 0.055 Uiso 1 1 calc R . .
H2C H 0.6136 0.7149 0.7017 0.055 Uiso 1 1 calc R . .
C3 C 0.4999(8) 0.7457(5) 0.9985(5) 0.0407(14) Uani 1 1 d . . .
H3A H 0.5542 0.7371 1.0565 0.061 Uiso 1 1 calc R . .
H3B H 0.4297 0.6811 1.0335 0.061 Uiso 1 1 calc R . .
H3C H 0.4353 0.8263 0.9752 0.061 Uiso 1 1 calc R . .
C4 C 0.7633(7) 0.5724(5) 0.9179(5) 0.0359(13) Uani 1 1 d . . .
H4A H 0.8187 0.5512 0.8496 0.054 Uiso 1 1 calc R . .
H4B H 0.6873 0.5135 0.9735 0.054 Uiso 1 1 calc R . .
H4C H 0.8422 0.5697 0.957 0.054 Uiso 1 1 calc R . .
C5 C 0.9246(9) 0.7456(6) 0.9984(6) 0.0463(16) Uani 1 1 d . . .
H5A H 0.8231 0.7353 1.0594 0.069 Uiso 1 1 calc R . .
H5B H 1.0042 0.7627 1.0248 0.069 Uiso 1 1 calc R . .
H5C H 0.9638 0.6701 0.9841 0.069 Uiso 1 1 calc R . .
C6 C 1.0992(6) 0.9005(6) 0.7625(6) 0.0369(13) Uani 1 1 d . . .
H6A H 1.1521 0.8255 0.75 0.055 Uiso 1 1 calc R . .
H6B H 1.161 0.9204 0.8007 0.055 Uiso 1 1 calc R . .
H6C H 1.0936 0.9685 0.6864 0.055 Uiso 1 1 calc R . .
C7 C 0.8017(8) 1.0127(5) 0.8981(5) 0.0350(13) Uani 1 1 d . . .
H7A H 0.7897 1.0857 0.8264 0.053 Uiso 1 1 calc R . .
H7B H 0.8723 1.0258 0.9346 0.053 Uiso 1 1 calc R . .
H7C H 0.6961 0.998 0.9536 0.053 Uiso 1 1 calc R . .
N11 N 0.5043(5) 1.1293(4) 0.6572(4) 0.0230(9) Uani 1 1 d . . .
C12 C 0.4223(7) 1.0789(6) 0.7840(5) 0.0381(13) Uani 1 1 d . . .
H12A H 0.4965 1.0668 0.8307 0.057 Uiso 1 1 calc R . .
H12B H 0.3877 1 0.8052 0.057 Uiso 1 1 calc R . .
H12C H 0.3284 1.1365 0.8003 0.057 Uiso 1 1 calc R . .
C13 C 0.3991(6) 1.1370(5) 0.5862(5) 0.0320(12) Uani 1 1 d . . .
H13A H 0.3013 1.1932 0.5984 0.048 Uiso 1 1 calc R . .
H13B H 0.3701 1.0552 0.6107 0.048 Uiso 1 1 calc R . .
H13C H 0.456 1.1675 0.5025 0.048 Uiso 1 1 calc R . .
C14 C 0.5475(6) 1.2517(4) 0.6253(5) 0.0258(11) Uani 1 1 d . . .
H14A H 0.6166 1.2429 0.6753 0.031 Uiso 1 1 calc R . .
H14B H 0.4483 1.306 0.6427 0.031 Uiso 1 1 calc R . .
C15 C 0.6347(6) 1.3119(4) 0.4969(5) 0.0251(11) Uani 1 1 d . . .
C16 C 0.5514(7) 1.4073(5) 0.4184(5) 0.0308(12) Uani 1 1 d . . .
H16 H 0.4403 1.4305 0.4463 0.037 Uiso 1 1 calc R . .
C17 C 0.6267(8) 1.4683(5) 0.3014(5) 0.0374(14) Uani 1 1 d . . .
H17 H 0.5685 1.5339 0.25 0.045 Uiso 1 1 calc R . .
C18 C 0.7876(8) 1.4333(5) 0.2596(5) 0.0362(13) Uani 1 1 d . . .
H18 H 0.84 1.4742 0.179 0.043 Uiso 1 1 calc R . .
C19 C 0.8730(7) 1.3377(5) 0.3356(5) 0.0309(12) Uani 1 1 d . . .
H19 H 0.9834 1.3138 0.3065 0.037 Uiso 1 1 calc R . .
C20 C 0.7981(6) 1.2776(4) 0.4529(4) 0.0228(10) Uani 1 1 d . . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.251(4) . ?
Pb1 N11 2.673(4) . ?
Pb1 Se2 2.7589(5) . ?
Se2 C20 1.931(5) . ?
Si1 N1 1.731(4) . ?
Si1 C3 1.847(6) . ?
Si1 C2 1.881(5) . ?
Si1 C4 1.881(6) . ?
Si2 N1 1.718(4) . ?
Si2 C5 1.868(6) . ?
Si2 C6 1.869(6) . ?
Si2 C7 1.873(5) . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
N11 C12 1.476(7) . ?
N11 C13 1.479(6) . ?
N11 C14 1.482(6) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C15 1.514(7) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.401(7) . ?
C15 C20 1.405(7) . ?
C16 C17 1.381(8) . ?
C16 H16 0.95 . ?
C17 C18 1.383(9) . ?
C17 H17 0.95 . ?
C18 C19 1.395(8) . ?
C18 H18 0.95 . ?
C19 C20 1.381(7) . ?
C19 H19 0.95 . ?


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 N11 98.66(14) . . ?
N1 Pb1 Se2 100.60(10) . . ?
N11 Pb1 Se2 82.59(9) . . ?
C20 Se2 Pb1 93.89(14) . . ?
N1 Si1 C3 112.7(2) . . ?
N1 Si1 C2 111.1(2) . . ?
C3 Si1 C2 106.8(3) . . ?
N1 Si1 C4 114.0(2) . . ?
C3 Si1 C4 106.9(3) . . ?
C2 Si1 C4 104.9(3) . . ?
N1 Si2 C5 113.3(2) . . ?
N1 Si2 C6 112.0(2) . . ?
C5 Si2 C6 103.8(3) . . ?
N1 Si2 C7 112.1(2) . . ?
C5 Si2 C7 106.2(3) . . ?
C6 Si2 C7 109.0(3) . . ?
Si2 N1 Si1 124.1(2) . . ?
Si2 N1 Pb1 122.2(2) . . ?
Si1 N1 Pb1 113.63(19) . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C12 N11 C13 110.1(4) . . ?
C12 N11 C14 108.7(4) . . ?
C13 N11 C14 111.3(4) . . ?
C12 N11 Pb1 109.8(3) . . ?
C13 N11 Pb1 102.1(3) . . ?
C14 N11 Pb1 114.7(3) . . ?
N11 C12 H12A 109.5 . . ?
N11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C13 H13A 109.5 . . ?
N11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N11 C14 C15 113.4(4) . . ?
N11 C14 H14A 108.9 . . ?
C15 C14 H14A 108.9 . . ?
N11 C14 H14B 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
C16 C15 C20 118.1(5) . . ?
C16 C15 C14 119.3(5) . . ?
C20 C15 C14 122.6(4) . . ?
C17 C16 C15 121.6(5) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 119.5(5) . . ?
C16 C17 H17 120.3 . . ?
C18 C17 H17 120.3 . . ?
C17 C18 C19 120.0(5) . . ?
C17 C18 H18 120 . . ?
C19 C18 H18 120 . . ?
C20 C19 C18 120.5(5) . . ?
C20 C19 H19 119.8 . . ?
C18 C19 H19 119.8 . . ?
C19 C20 C15 120.3(5) . . ?
C19 C20 Se2 118.0(4) . . ?
C15 C20 Se2 121.7(4) . . ?


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
N1 Pb1 Se2 C20 -148.01(18) . . . . ?
N11 Pb1 Se2 C20 -50.53(17) . . . . ?
C5 Si2 N1 Si1 17.2(4) . . . . ?
C6 Si2 N1 Si1 134.2(3) . . . . ?
C7 Si2 N1 Si1 -102.9(3) . . . . ?
C5 Si2 N1 Pb1 -167.3(3) . . . . ?
C6 Si2 N1 Pb1 -50.3(3) . . . . ?
C7 Si2 N1 Pb1 72.6(3) . . . . ?
C3 Si1 N1 Si2 58.7(4) . . . . ?
C2 Si1 N1 Si2 178.5(3) . . . . ?
C4 Si1 N1 Si2 -63.3(4) . . . . ?
C3 Si1 N1 Pb1 -117.1(3) . . . . ?
C2 Si1 N1 Pb1 2.7(3) . . . . ?
C4 Si1 N1 Pb1 120.9(3) . . . . ?
N11 Pb1 N1 Si2 -89.0(2) . . . . ?
Se2 Pb1 N1 Si2 -5.0(2) . . . . ?
N11 Pb1 N1 Si1 86.9(2) . . . . ?
Se2 Pb1 N1 Si1 170.89(18) . . . . ?
N1 Pb1 N11 C12 -16.4(3) . . . . ?
Se2 Pb1 N11 C12 -116.1(3) . . . . ?
N1 Pb1 N11 C13 -133.2(3) . . . . ?
Se2 Pb1 N11 C13 127.2(3) . . . . ?
N1 Pb1 N11 C14 106.3(3) . . . . ?
Se2 Pb1 N11 C14 6.6(3) . . . . ?
C12 N11 C14 C15 179.3(4) . . . . ?
C13 N11 C14 C15 -59.3(5) . . . . ?
Pb1 N11 C14 C15 55.9(5) . . . . ?
N11 C14 C15 C16 103.8(5) . . . . ?
N11 C14 C15 C20 -77.4(6) . . . . ?
C20 C15 C16 C17 -1.3(7) . . . . ?
C14 C15 C16 C17 177.5(5) . . . . ?
C15 C16 C17 C18 1.4(8) . . . . ?
C16 C17 C18 C19 -0.7(8) . . . . ?
C17 C18 C19 C20 -0.1(8) . . . . ?
C18 C19 C20 C15 0.2(7) . . . . ?
C18 C19 C20 Se2 -176.8(4) . . . . ?
C16 C15 C20 C19 0.5(7) . . . . ?
C14 C15 C20 C19 -178.3(4) . . . . ?
C16 C15 C20 Se2 177.4(4) . . . . ?
C14 C15 C20 Se2 -1.4(6) . . . . ?
Pb1 Se2 C20 C19 -119.0(4) . . . . ?
Pb1 Se2 C20 C15 64.1(4) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006879'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_6

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C15 H30 N2 Pb S Si2'
_chemical_formula_sum            'C15 H30 N2 Pb S Si2'
_chemical_formula_weight         533.84
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.8858(4)
_cell_length_b                   12.1481(6)
_cell_length_c                   12.9552(6)
_cell_angle_alpha                63.6440(10)
_cell_angle_beta                 71.551(2)
_cell_angle_gamma                75.792(2)
_cell_volume                     1179.59(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9914
_cell_measurement_theta_min      2.61
_cell_measurement_theta_max      27.53
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    7.339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.251
_exptl_absorpt_correction_T_max  0.480


#----------------------------------------------------------------------------#
#                   SQUEEZE RESULTS                                          #
#----------------------------------------------------------------------------#

# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.500 204 57 ' '
_platon_squeeze_details          
;
;

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_number            5435
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.81
_diffrn_reflns_theta_max         27.62
_diffrn_reflns_theta_full        27.62
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_reflns_number_total             5435
_reflns_number_gt                4994
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0860P)²+6.2905P] 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_number_reflns         5435
_refine_ls_number_parameters     198
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.036
_refine_ls_wR_factor_ref         0.1244
_refine_ls_wR_factor_gt          0.1217
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.487
_refine_diff_density_min         -1.61
_refine_diff_density_rms         0.318

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.74658(3) 0.031859(19) 0.392439(19) 0.02011(10) Uani 1 1 d . . .
N1 N 0.7256(6) 0.1516(5) 0.2052(5) 0.0210(11) Uani 1 1 d . . .
Si1 Si 0.6055(2) 0.12217(17) 0.14090(16) 0.0230(4) Uani 1 1 d . . .
Si2 Si 0.8468(2) 0.26840(17) 0.13140(17) 0.0241(4) Uani 1 1 d . . .
C2 C 0.6928(11) -0.0155(7) 0.1015(7) 0.0362(17) Uani 1 1 d . . .
H2A H 0.7981 -0.0013 0.0466 0.054 Uiso 1 1 calc R . .
H2B H 0.622 -0.0275 0.0638 0.054 Uiso 1 1 calc R . .
H2C H 0.704 -0.0895 0.1737 0.054 Uiso 1 1 calc R . .
C3 C 0.4003(9) 0.0961(8) 0.2382(8) 0.0364(17) Uani 1 1 d . . .
H3A H 0.407 0.023 0.3119 0.055 Uiso 1 1 calc R . .
H3B H 0.3353 0.083 0.197 0.055 Uiso 1 1 calc R . .
H3C H 0.3509 0.1687 0.2568 0.055 Uiso 1 1 calc R . .
C4 C 0.5740(12) 0.2539(8) -0.0023(8) 0.045(2) Uani 1 1 d . . .
H4A H 0.5156 0.3265 0.0137 0.067 Uiso 1 1 calc R . .
H4B H 0.5121 0.2295 -0.0377 0.067 Uiso 1 1 calc R . .
H4C H 0.6779 0.2742 -0.0574 0.067 Uiso 1 1 calc R . .
C5 C 0.9968(10) 0.2568(8) -0.0025(7) 0.0394(18) Uani 1 1 d . . .
H5A H 1.0728 0.1819 0.0215 0.059 Uiso 1 1 calc R . .
H5B H 1.0544 0.3297 -0.0442 0.059 Uiso 1 1 calc R . .
H5C H 0.9422 0.2526 -0.0554 0.059 Uiso 1 1 calc R . .
C6 C 0.9617(10) 0.2666(8) 0.2322(7) 0.0359(17) Uani 1 1 d . . .
H6A H 0.8866 0.2768 0.3023 0.054 Uiso 1 1 calc R . .
H6B H 1.028 0.3345 0.1897 0.054 Uiso 1 1 calc R . .
H6C H 1.0303 0.1875 0.2571 0.054 Uiso 1 1 calc R . .
C7 C 0.7369(10) 0.4280(7) 0.0799(8) 0.0385(19) Uani 1 1 d . . .
H7A H 0.6588 0.4312 0.0392 0.058 Uiso 1 1 calc R . .
H7B H 0.813 0.4872 0.0251 0.058 Uiso 1 1 calc R . .
H7C H 0.6813 0.4492 0.1484 0.058 Uiso 1 1 calc R . .
N11 N 0.9907(7) -0.1249(5) 0.3422(5) 0.0237(11) Uani 1 1 d . . .
C12 C 1.0731(9) -0.0729(8) 0.2155(7) 0.0333(16) Uani 1 1 d . . .
H12A H 1.1734 -0.1257 0.2014 0.05 Uiso 1 1 calc R . .
H12B H 1.0961 0.0106 0.1936 0.05 Uiso 1 1 calc R . .
H12C H 1.0045 -0.0689 0.1675 0.05 Uiso 1 1 calc R . .
C13 C 1.0969(9) -0.1368(7) 0.4144(7) 0.0307(15) Uani 1 1 d . . .
H13A H 1.0397 -0.1661 0.4982 0.046 Uiso 1 1 calc R . .
H13B H 1.1307 -0.056 0.3897 0.046 Uiso 1 1 calc R . .
H13C H 1.1911 -0.1962 0.4035 0.046 Uiso 1 1 calc R . .
C14 C 0.9437(8) -0.2466(6) 0.3746(6) 0.0257(14) Uani 1 1 d . . .
H14A H 1.0413 -0.3028 0.3589 0.031 Uiso 1 1 calc R . .
H14B H 0.8761 -0.2363 0.3222 0.031 Uiso 1 1 calc R . .
C15 C 0.8551(9) -0.3068(6) 0.5000(7) 0.0273(14) Uani 1 1 d . . .
C16 C 0.9358(9) -0.4045(7) 0.5790(7) 0.0301(15) Uani 1 1 d . . .
H16 H 1.0456 -0.4296 0.5515 0.036 Uiso 1 1 calc R . .
C17 C 0.8593(11) -0.4670(7) 0.6982(7) 0.0362(17) Uani 1 1 d . . .
H17 H 0.9162 -0.5336 0.7508 0.043 Uiso 1 1 calc R . .
C18 C 0.6992(11) -0.4298(7) 0.7376(7) 0.0371(18) Uani 1 1 d . . .
H18 H 0.6455 -0.4715 0.8179 0.045 Uiso 1 1 calc R . .
C19 C 0.6167(10) -0.3320(7) 0.6607(6) 0.0303(15) Uani 1 1 d . . .
H19 H 0.5069 -0.3075 0.689 0.036 Uiso 1 1 calc R . .
C20 C 0.6931(8) -0.2685(6) 0.5412(6) 0.0251(13) Uani 1 1 d . . .
S1 S 0.5799(2) -0.14743(15) 0.44607(16) 0.0249(3) Uani 1 1 d . . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.248(5) . ?
Pb1 N11 2.634(6) . ?
Pb1 S1 2.6476(17) . ?
N1 Si1 1.724(6) . ?
N1 Si2 1.727(6) . ?
Si1 C3 1.868(8) . ?
Si1 C2 1.879(8) . ?
Si1 C4 1.885(8) . ?
Si2 C5 1.862(8) . ?
Si2 C7 1.868(8) . ?
Si2 C6 1.886(8) . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
N11 C13 1.469(9) . ?
N11 C12 1.474(9) . ?
N11 C14 1.476(9) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C15 1.488(10) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.392(10) . ?
C15 C20 1.407(10) . ?
C16 C17 1.404(11) . ?
C16 H16 0.95 . ?
C17 C18 1.385(12) . ?
C17 H17 0.95 . ?
C18 C19 1.388(11) . ?
C18 H18 0.95 . ?
C19 C20 1.409(10) . ?
C19 H19 0.95 . ?
C20 S1 1.773(7) . ?


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 N11 97.08(19) . . ?
N1 Pb1 S1 100.79(15) . . ?
N11 Pb1 S1 83.09(13) . . ?
Si1 N1 Si2 123.9(3) . . ?
Si1 N1 Pb1 122.0(3) . . ?
Si2 N1 Pb1 114.1(3) . . ?
N1 Si1 C3 112.3(3) . . ?
N1 Si1 C2 112.3(3) . . ?
C3 Si1 C2 108.3(4) . . ?
N1 Si1 C4 113.2(3) . . ?
C3 Si1 C4 105.0(4) . . ?
C2 Si1 C4 105.1(4) . . ?
N1 Si2 C5 113.7(3) . . ?
N1 Si2 C7 114.4(3) . . ?
C5 Si2 C7 105.8(4) . . ?
N1 Si2 C6 110.5(3) . . ?
C5 Si2 C6 106.9(4) . . ?
C7 Si2 C6 104.9(4) . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C13 N11 C12 109.5(6) . . ?
C13 N11 C14 110.4(5) . . ?
C12 N11 C14 110.2(6) . . ?
C13 N11 Pb1 103.3(4) . . ?
C12 N11 Pb1 110.7(4) . . ?
C14 N11 Pb1 112.5(4) . . ?
N11 C12 H12A 109.5 . . ?
N11 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N11 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N11 C13 H13A 109.5 . . ?
N11 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N11 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N11 C14 C15 115.0(6) . . ?
N11 C14 H14A 108.5 . . ?
C15 C14 H14A 108.5 . . ?
N11 C14 H14B 108.5 . . ?
C15 C14 H14B 108.5 . . ?
H14A C14 H14B 107.5 . . ?
C16 C15 C20 119.1(7) . . ?
C16 C15 C14 118.7(6) . . ?
C20 C15 C14 122.3(6) . . ?
C15 C16 C17 121.8(7) . . ?
C15 C16 H16 119.1 . . ?
C17 C16 H16 119.1 . . ?
C18 C17 C16 118.7(7) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 120.5(7) . . ?
C17 C18 H18 119.8 . . ?
C19 C18 H18 119.8 . . ?
C18 C19 C20 121.0(7) . . ?
C18 C19 H19 119.5 . . ?
C20 C19 H19 119.5 . . ?
C15 C20 C19 118.9(6) . . ?
C15 C20 S1 122.1(5) . . ?
C19 C20 S1 118.9(5) . . ?
C20 S1 Pb1 96.9(2) . . ?


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
N11 Pb1 N1 Si1 90.5(3) . . . . ?
S1 Pb1 N1 Si1 6.2(3) . . . . ?
N11 Pb1 N1 Si2 -86.4(3) . . . . ?
S1 Pb1 N1 Si2 -170.7(2) . . . . ?
Si2 N1 Si1 C3 -134.8(4) . . . . ?
Pb1 N1 Si1 C3 48.7(5) . . . . ?
Si2 N1 Si1 C2 102.9(4) . . . . ?
Pb1 N1 Si1 C2 -73.7(4) . . . . ?
Si2 N1 Si1 C4 -16.0(6) . . . . ?
Pb1 N1 Si1 C4 167.4(4) . . . . ?
Si1 N1 Si2 C5 -58.5(5) . . . . ?
Pb1 N1 Si2 C5 118.3(4) . . . . ?
Si1 N1 Si2 C7 63.2(5) . . . . ?
Pb1 N1 Si2 C7 -120.0(4) . . . . ?
Si1 N1 Si2 C6 -178.6(4) . . . . ?
Pb1 N1 Si2 C6 -1.8(4) . . . . ?
N1 Pb1 N11 C13 134.6(4) . . . . ?
S1 Pb1 N11 C13 -125.3(4) . . . . ?
N1 Pb1 N11 C12 17.5(5) . . . . ?
S1 Pb1 N11 C12 117.6(5) . . . . ?
N1 Pb1 N11 C14 -106.3(4) . . . . ?
S1 Pb1 N11 C14 -6.2(4) . . . . ?
C13 N11 C14 C15 60.6(8) . . . . ?
C12 N11 C14 C15 -178.3(6) . . . . ?
Pb1 N11 C14 C15 -54.3(7) . . . . ?
N11 C14 C15 C16 -104.0(7) . . . . ?
N11 C14 C15 C20 76.1(9) . . . . ?
C20 C15 C16 C17 0.9(11) . . . . ?
C14 C15 C16 C17 -178.9(7) . . . . ?
C15 C16 C17 C18 -0.1(12) . . . . ?
C16 C17 C18 C19 -0.4(12) . . . . ?
C17 C18 C19 C20 0.1(12) . . . . ?
C16 C15 C20 C19 -1.2(11) . . . . ?
C14 C15 C20 C19 178.6(7) . . . . ?
C16 C15 C20 S1 -178.5(6) . . . . ?
C14 C15 C20 S1 1.4(10) . . . . ?
C18 C19 C20 C15 0.8(11) . . . . ?
C18 C19 C20 S1 178.1(6) . . . . ?
C15 C20 S1 Pb1 -63.6(6) . . . . ?
C19 C20 S1 Pb1 119.1(6) . . . . ?
N1 Pb1 S1 C20 147.1(3) . . . . ?
N11 Pb1 S1 C20 51.2(3) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006880'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_7

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H46 N2 Se2 Si4 Sn2'
_chemical_formula_sum            'C24 H46 N2 Se2 Si4 Sn'
_chemical_formula_weight         751.6
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   8.7208(4)
_cell_length_b                   17.4865(9)
_cell_length_c                   21.7958(9)
_cell_angle_alpha                90
_cell_angle_beta                 98.565(2)
_cell_angle_gamma                90
_cell_volume                     3286.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2299
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      26.9
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.03
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1512
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.154
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.619
_exptl_absorpt_correction_T_max  0.910


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_unetI/netI     0.0517
_diffrn_reflns_number            11413
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_reflns_number_total             3763
_reflns_number_gt                3049
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0246P)²+0.2974P] 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_number_reflns         3763
_refine_ls_number_parameters     156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0331
_refine_ls_wR_factor_ref         0.0708
_refine_ls_wR_factor_gt          0.0668
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.443
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.094

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Si Si 0.0817 0.0704 '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'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0 0.195531(14) 0.75 0.02058(9) Uani 1 2 d S . .
Se2 Se 0.23785(4) 0.109084(19) 0.757349(17) 0.03967(12) Uani 1 1 d . . .
N1 N 0.0041(3) 0.25926(12) 0.82928(11) 0.0206(5) Uani 1 1 d . . .
Si3 Si 0.14620(10) 0.33040(5) 0.84583(4) 0.02390(19) Uani 1 1 d . . .
Si4 Si -0.12098(10) 0.23653(4) 0.88287(4) 0.0237(2) Uani 1 1 d . . .
C1 C 0.2293(4) 0.06458(16) 0.83743(15) 0.0277(7) Uani 1 1 d . . .
C2 C 0.3278(4) 0.09103(17) 0.88857(16) 0.0364(8) Uani 1 1 d . . .
H2 H 0.3943 0.1331 0.8843 0.044 Uiso 1 1 calc R . .
C3 C 0.3305(5) 0.05665(19) 0.94607(17) 0.0461(10) Uani 1 1 d . . .
H3 H 0.3991 0.0748 0.981 0.055 Uiso 1 1 calc R . .
C4 C 0.2335(5) -0.00360(19) 0.95205(17) 0.0441(9) Uani 1 1 d . . .
H4 H 0.2328 -0.0265 0.9915 0.053 Uiso 1 1 calc R . .
C5 C 0.1378(5) -0.03088(18) 0.90156(18) 0.0421(9) Uani 1 1 d . . .
H5 H 0.0726 -0.0734 0.9061 0.051 Uiso 1 1 calc R . .
C6 C 0.1343(4) 0.00249(16) 0.84387(16) 0.0337(8) Uani 1 1 d . . .
H6 H 0.0674 -0.017 0.809 0.04 Uiso 1 1 calc R . .
C11 C -0.3295(4) 0.25121(18) 0.85275(15) 0.0323(8) Uani 1 1 d . . .
H11A H -0.347 0.3047 0.8403 0.048 Uiso 1 1 calc R . .
H11B H -0.3919 0.2387 0.8853 0.048 Uiso 1 1 calc R . .
H11C H -0.3598 0.218 0.8168 0.048 Uiso 1 1 calc R . .
C12 C -0.0833(4) 0.29813(17) 0.95383(14) 0.0319(8) Uani 1 1 d . . .
H12A H 0.018 0.2852 0.9774 0.048 Uiso 1 1 calc R . .
H12B H -0.1643 0.2894 0.9798 0.048 Uiso 1 1 calc R . .
H12C H -0.084 0.352 0.9415 0.048 Uiso 1 1 calc R . .
C13 C -0.0967(4) 0.13640(17) 0.91080(16) 0.0402(9) Uani 1 1 d . . .
H13A H -0.1206 0.1013 0.8756 0.06 Uiso 1 1 calc R . .
H13B H -0.1673 0.1266 0.941 0.06 Uiso 1 1 calc R . .
H13C H 0.0105 0.1284 0.9306 0.06 Uiso 1 1 calc R . .
C14 C 0.2786(4) 0.30917(18) 0.91950(14) 0.0321(7) Uani 1 1 d . . .
H14A H 0.2578 0.345 0.9518 0.048 Uiso 1 1 calc R . .
H14B H 0.3866 0.3146 0.9126 0.048 Uiso 1 1 calc R . .
H14C H 0.2609 0.2567 0.9327 0.048 Uiso 1 1 calc R . .
C15 C 0.0581(4) 0.42786(16) 0.84954(16) 0.0393(9) Uani 1 1 d . . .
H15A H 0.0143 0.4444 0.8076 0.059 Uiso 1 1 calc R . .
H15B H 0.1382 0.4642 0.8673 0.059 Uiso 1 1 calc R . .
H15C H -0.0242 0.4259 0.8756 0.059 Uiso 1 1 calc R . .
C16 C 0.2730(4) 0.33665(18) 0.78418(15) 0.0318(8) Uani 1 1 d . . .
H16A H 0.3277 0.2881 0.7818 0.048 Uiso 1 1 calc R . .
H16B H 0.3486 0.3779 0.7942 0.048 Uiso 1 1 calc R . .
H16C H 0.2092 0.3473 0.7442 0.048 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.052(2) . ?
Sn1 N1 2.052(2) 2_556 ?
Sn1 Se2 2.5523(4) . ?
Sn1 Se2 2.5523(4) 2_556 ?
Se2 C1 1.923(3) . ?
N1 Si3 1.755(2) . ?
N1 Si4 1.758(2) . ?
Si3 C16 1.866(3) . ?
Si3 C14 1.870(3) . ?
Si3 C15 1.876(3) . ?
Si4 C13 1.856(3) . ?
Si4 C11 1.857(3) . ?
Si4 C12 1.873(3) . ?
C1 C2 1.382(5) . ?
C1 C6 1.386(4) . ?
C2 C3 1.387(5) . ?
C2 H2 0.95 . ?
C3 C4 1.370(5) . ?
C3 H3 0.95 . ?
C4 C5 1.364(5) . ?
C4 H4 0.95 . ?
C5 C6 1.382(4) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?


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 114.21(12) . 2_556 ?
N1 Sn1 Se2 110.90(7) . . ?
N1 Sn1 Se2 106.65(6) 2_556 . ?
N1 Sn1 Se2 106.65(6) . 2_556 ?
N1 Sn1 Se2 110.90(7) 2_556 2_556 ?
Se2 Sn1 Se2 107.36(2) . 2_556 ?
C1 Se2 Sn1 98.96(9) . . ?
Si3 N1 Si4 120.84(13) . . ?
Si3 N1 Sn1 118.77(11) . . ?
Si4 N1 Sn1 120.13(12) . . ?
N1 Si3 C16 111.68(13) . . ?
N1 Si3 C14 111.27(13) . . ?
C16 Si3 C14 105.87(14) . . ?
N1 Si3 C15 111.81(14) . . ?
C16 Si3 C15 105.55(15) . . ?
C14 Si3 C15 110.35(15) . . ?
N1 Si4 C13 112.31(13) . . ?
N1 Si4 C11 113.94(13) . . ?
C13 Si4 C11 107.71(16) . . ?
N1 Si4 C12 111.63(13) . . ?
C13 Si4 C12 105.92(15) . . ?
C11 Si4 C12 104.73(15) . . ?
C2 C1 C6 119.3(3) . . ?
C2 C1 Se2 119.6(2) . . ?
C6 C1 Se2 120.9(3) . . ?
C1 C2 C3 120.6(3) . . ?
C1 C2 H2 119.7 . . ?
C3 C2 H2 119.7 . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3 120.3 . . ?
C2 C3 H3 120.3 . . ?
C5 C4 C3 120.3(3) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C4 C5 C6 120.9(3) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.3(3) . . ?
C5 C6 H6 120.3 . . ?
C1 C6 H6 120.3 . . ?
Si4 C11 H11A 109.5 . . ?
Si4 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si4 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si4 C12 H12A 109.5 . . ?
Si4 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si4 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si4 C13 H13A 109.5 . . ?
Si4 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si4 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si3 C14 H14A 109.5 . . ?
Si3 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
Si3 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si3 C15 H15A 109.5 . . ?
Si3 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
Si3 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si3 C16 H16A 109.5 . . ?
Si3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Si3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?


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
N1 Sn1 Se2 C1 49.27(12) . . . . ?
N1 Sn1 Se2 C1 174.19(12) 2_556 . . . ?
Se2 Sn1 Se2 C1 -66.88(10) 2_556 . . . ?
N1 Sn1 N1 Si3 -52.56(10) 2_556 . . . ?
Se2 Sn1 N1 Si3 67.97(13) . . . . ?
Se2 Sn1 N1 Si3 -175.43(11) 2_556 . . . ?
N1 Sn1 N1 Si4 133.36(16) 2_556 . . . ?
Se2 Sn1 N1 Si4 -106.11(13) . . . . ?
Se2 Sn1 N1 Si4 10.49(15) 2_556 . . . ?
Si4 N1 Si3 C16 175.04(16) . . . . ?
Sn1 N1 Si3 C16 1.00(19) . . . . ?
Si4 N1 Si3 C14 56.97(19) . . . . ?
Sn1 N1 Si3 C14 -117.07(15) . . . . ?
Si4 N1 Si3 C15 -66.94(19) . . . . ?
Sn1 N1 Si3 C15 119.03(16) . . . . ?
Si3 N1 Si4 C13 -117.30(19) . . . . ?
Sn1 N1 Si4 C13 56.7(2) . . . . ?
Si3 N1 Si4 C11 119.88(17) . . . . ?
Sn1 N1 Si4 C11 -66.16(18) . . . . ?
Si3 N1 Si4 C12 1.5(2) . . . . ?
Sn1 N1 Si4 C12 175.45(14) . . . . ?
Sn1 Se2 C1 C2 -101.9(2) . . . . ?
Sn1 Se2 C1 C6 83.1(2) . . . . ?
C6 C1 C2 C3 -0.9(5) . . . . ?
Se2 C1 C2 C3 -176.0(2) . . . . ?
C1 C2 C3 C4 -0.6(5) . . . . ?
C2 C3 C4 C5 1.7(5) . . . . ?
C3 C4 C5 C6 -1.4(5) . . . . ?
C4 C5 C6 C1 -0.1(5) . . . . ?
C2 C1 C6 C5 1.2(5) . . . . ?
Se2 C1 C6 C5 176.2(2) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006881'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_8

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C38 H76 N4 O2 Se2 Si4 Sn2'
_chemical_formula_sum            'C38 H76 N4 O2 Se2 Si4 Sn2'
_chemical_formula_weight         1128.73
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.431(5)
_cell_length_b                   10.948(2)
_cell_length_c                   11.369(4)
_cell_angle_alpha                100.052(13)
_cell_angle_beta                 100.25(2)
_cell_angle_gamma                94.638(17)
_cell_volume                     1249.6(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    709
_cell_measurement_theta_min      2.39
_cell_measurement_theta_max      22.93
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.5
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             572
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.517
_exptl_absorpt_correction_T_max  0.772


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0597
_diffrn_reflns_av_unetI/netI     0.0833
_diffrn_reflns_number            12220
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_full        27.52
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_reflns_number_total             5674
_reflns_number_gt                4291
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1083P)²+0.0000P] 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_number_reflns         5674
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0631
_refine_ls_wR_factor_ref         0.1766
_refine_ls_wR_factor_gt          0.1598
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.92
_refine_diff_density_min         -2.284
_refine_diff_density_rms         0.238

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Si Si 0.0817 0.0704 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.04955(4) 0.11004(3) 0.63701(4) 0.02006(15) Uani 1 1 d . . .
Se1 Se -0.35712(6) -0.25648(6) 0.66639(6) 0.02561(18) Uani 1 1 d . . .
O1 O -0.0296(4) -0.0831(4) 0.5592(4) 0.0197(8) Uani 1 1 d . . .
C2 C -0.0909(6) -0.1689(5) 0.6236(5) 0.0211(12) Uani 1 1 d . . .
C3 C -0.0254(6) -0.1449(7) 0.7549(6) 0.0325(15) Uani 1 1 d . . .
H3A H 0.0653 -0.1648 0.7617 0.049 Uiso 1 1 calc R . .
H3B H -0.0729 -0.1975 0.7983 0.049 Uiso 1 1 calc R . .
H3C H -0.0256 -0.0568 0.7908 0.049 Uiso 1 1 calc R . .
C4 C -0.0749(7) -0.3021(5) 0.5617(6) 0.0283(14) Uani 1 1 d . . .
H4A H -0.1192 -0.3174 0.476 0.042 Uiso 1 1 calc R . .
H4B H -0.114 -0.3627 0.6031 0.042 Uiso 1 1 calc R . .
H4C H 0.0185 -0.311 0.5666 0.042 Uiso 1 1 calc R . .
C5 C -0.2371(6) -0.1491(5) 0.6041(6) 0.0235(12) Uani 1 1 d . . .
H5A H -0.2698 -0.1583 0.5154 0.028 Uiso 1 1 calc R . .
H5B H -0.2431 -0.0615 0.6415 0.028 Uiso 1 1 calc R . .
C6 C -0.3468(6) -0.1701(5) 0.8323(5) 0.0230(13) Uani 1 1 d . . .
C7 C -0.2979(7) -0.0448(7) 0.8742(7) 0.0350(16) Uani 1 1 d . . .
H7 H -0.2651 0.0016 0.8205 0.042 Uiso 1 1 calc R . .
C8 C -0.2965(7) 0.0127(7) 0.9921(7) 0.0363(16) Uani 1 1 d . . .
H8 H -0.2627 0.0982 1.0194 0.044 Uiso 1 1 calc R . .
C9 C -0.3447(8) -0.0547(7) 1.0713(7) 0.0389(17) Uani 1 1 d . . .
H9 H -0.3441 -0.0153 1.1527 0.047 Uiso 1 1 calc R . .
C10 C -0.3933(7) -0.1787(7) 1.0310(6) 0.0371(17) Uani 1 1 d . . .
H10 H -0.4271 -0.2239 1.0851 0.044 Uiso 1 1 calc R . .
C11 C -0.3938(6) -0.2386(6) 0.9131(6) 0.0299(14) Uani 1 1 d . . .
C12 C -0.4447(7) -0.3764(6) 0.8702(7) 0.0338(16) Uani 1 1 d . . .
H12A H -0.3729 -0.4225 0.8458 0.041 Uiso 1 1 calc R . .
H12B H -0.4716 -0.4096 0.9388 0.041 Uiso 1 1 calc R . .
N13 N -0.5552(6) -0.3985(5) 0.7685(5) 0.0307(12) Uani 1 1 d . . .
C14 C -0.5868(8) -0.5322(6) 0.7152(8) 0.045(2) Uani 1 1 d . . .
H14A H -0.5146 -0.5619 0.6777 0.068 Uiso 1 1 calc R . .
H14B H -0.6674 -0.545 0.653 0.068 Uiso 1 1 calc R . .
H14C H -0.5995 -0.5788 0.7792 0.068 Uiso 1 1 calc R . .
C15 C -0.6698(7) -0.3456(7) 0.8002(7) 0.0410(18) Uani 1 1 d . . .
H15A H -0.7019 -0.3883 0.8601 0.061 Uiso 1 1 calc R . .
H15B H -0.7384 -0.3562 0.727 0.061 Uiso 1 1 calc R . .
H15C H -0.6468 -0.2565 0.8351 0.061 Uiso 1 1 calc R . .
N1 N -0.1237(5) 0.1901(4) 0.6702(4) 0.0210(10) Uani 1 1 d . . .
Si1 Si -0.08277(18) 0.29396(16) 0.80973(16) 0.0257(4) Uani 1 1 d . . .
Si2 Si -0.26799(16) 0.20272(15) 0.57195(15) 0.0209(4) Uani 1 1 d . . .
C21 C 0.0175(8) 0.2267(7) 0.9305(6) 0.0393(17) Uani 1 1 d . . .
H21A H -0.0286 0.1473 0.9373 0.059 Uiso 1 1 calc R . .
H21B H 0.0309 0.2851 1.0086 0.059 Uiso 1 1 calc R . .
H21C H 0.1026 0.2122 0.909 0.059 Uiso 1 1 calc R . .
C22 C 0.0159(8) 0.4398(6) 0.7952(8) 0.0438(19) Uani 1 1 d . . .
H22A H 0.1056 0.4224 0.79 0.066 Uiso 1 1 calc R . .
H22B H 0.0178 0.5052 0.8665 0.066 Uiso 1 1 calc R . .
H22C H -0.0242 0.468 0.7214 0.066 Uiso 1 1 calc R . .
C23 C -0.2290(7) 0.3410(7) 0.8737(6) 0.0365(16) Uani 1 1 d . . .
H23A H -0.2955 0.3598 0.8089 0.055 Uiso 1 1 calc R . .
H23B H -0.2023 0.4153 0.9383 0.055 Uiso 1 1 calc R . .
H23C H -0.2656 0.2725 0.9073 0.055 Uiso 1 1 calc R . .
C24 C -0.2866(6) 0.1093(6) 0.4153(6) 0.0248(13) Uani 1 1 d . . .
H24A H -0.2115 0.1334 0.3799 0.037 Uiso 1 1 calc R . .
H24B H -0.3676 0.125 0.3647 0.037 Uiso 1 1 calc R . .
H24C H -0.2904 0.0203 0.4187 0.037 Uiso 1 1 calc R . .
C25 C -0.4189(6) 0.1482(6) 0.6263(6) 0.0297(14) Uani 1 1 d . . .
H25A H -0.4188 0.0597 0.6313 0.045 Uiso 1 1 calc R . .
H25B H -0.4972 0.1591 0.5689 0.045 Uiso 1 1 calc R . .
H25C H -0.4193 0.1974 0.7069 0.045 Uiso 1 1 calc R . .
C26 C -0.2792(7) 0.3683(6) 0.5503(6) 0.0285(14) Uani 1 1 d . . .
H26A H -0.2832 0.4214 0.6281 0.043 Uiso 1 1 calc R . .
H26B H -0.3585 0.3714 0.4904 0.043 Uiso 1 1 calc R . .
H26C H -0.2018 0.3983 0.521 0.043 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.136(5) . ?
Sn1 O1 2.168(4) 2_556 ?
Sn1 O1 2.177(4) . ?
Se1 C6 1.937(6) . ?
Se1 C5 1.954(6) . ?
O1 C2 1.463(7) . ?
O1 Sn1 2.168(4) 2_556 ?
C2 C3 1.495(9) . ?
C2 C4 1.540(8) . ?
C2 C5 1.541(8) . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 C7 1.393(9) . ?
C6 C11 1.409(9) . ?
C7 C8 1.374(10) . ?
C7 H7 0.95 . ?
C8 C9 1.393(11) . ?
C8 H8 0.95 . ?
C9 C10 1.378(11) . ?
C9 H9 0.95 . ?
C10 C11 1.385(10) . ?
C10 H10 0.95 . ?
C11 C12 1.523(9) . ?
C12 N13 1.451(9) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
N13 C15 1.444(9) . ?
N13 C14 1.470(9) . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
N1 Si2 1.738(5) . ?
N1 Si1 1.744(5) . ?
Si1 C21 1.868(7) . ?
Si1 C23 1.874(7) . ?
Si1 C22 1.877(8) . ?
Si2 C24 1.862(6) . ?
Si2 C25 1.881(7) . ?
Si2 C26 1.882(6) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?


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 O1 103.68(17) . 2_556 ?
N1 Sn1 O1 101.17(17) . . ?
O1 Sn1 O1 71.65(17) 2_556 . ?
C6 Se1 C5 103.3(3) . . ?
C2 O1 Sn1 124.8(3) . 2_556 ?
C2 O1 Sn1 125.0(3) . . ?
Sn1 O1 Sn1 108.35(16) 2_556 . ?
O1 C2 C3 110.5(5) . . ?
O1 C2 C4 106.9(5) . . ?
C3 C2 C4 110.0(5) . . ?
O1 C2 C5 105.8(4) . . ?
C3 C2 C5 113.3(5) . . ?
C4 C2 C5 110.0(5) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 Se1 118.7(4) . . ?
C2 C5 H5A 107.6 . . ?
Se1 C5 H5A 107.6 . . ?
C2 C5 H5B 107.6 . . ?
Se1 C5 H5B 107.6 . . ?
H5A C5 H5B 107.1 . . ?
C7 C6 C11 119.1(6) . . ?
C7 C6 Se1 123.5(5) . . ?
C11 C6 Se1 117.4(5) . . ?
C8 C7 C6 121.0(7) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C9 119.8(7) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C10 C9 C8 119.8(7) . . ?
C10 C9 H9 120.1 . . ?
C8 C9 H9 120.1 . . ?
C9 C10 C11 121.2(7) . . ?
C9 C10 H10 119.4 . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C6 119.1(6) . . ?
C10 C11 C12 120.8(6) . . ?
C6 C11 C12 120.1(6) . . ?
N13 C12 C11 112.8(5) . . ?
N13 C12 H12A 109 . . ?
C11 C12 H12A 109 . . ?
N13 C12 H12B 109 . . ?
C11 C12 H12B 109 . . ?
H12A C12 H12B 107.8 . . ?
C15 N13 C12 112.8(6) . . ?
C15 N13 C14 110.7(6) . . ?
C12 N13 C14 111.4(5) . . ?
N13 C14 H14A 109.5 . . ?
N13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N13 C15 H15A 109.5 . . ?
N13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si2 N1 Si1 118.2(3) . . ?
Si2 N1 Sn1 131.3(3) . . ?
Si1 N1 Sn1 107.5(2) . . ?
N1 Si1 C21 112.5(3) . . ?
N1 Si1 C23 113.4(3) . . ?
C21 Si1 C23 105.0(3) . . ?
N1 Si1 C22 110.7(3) . . ?
C21 Si1 C22 107.0(4) . . ?
C23 Si1 C22 107.9(4) . . ?
N1 Si2 C24 114.6(3) . . ?
N1 Si2 C25 112.7(3) . . ?
C24 Si2 C25 104.5(3) . . ?
N1 Si2 C26 111.4(3) . . ?
C24 Si2 C26 104.9(3) . . ?
C25 Si2 C26 108.1(3) . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?


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
N1 Sn1 O1 C2 -64.2(4) . . . . ?
O1 Sn1 O1 C2 -165.1(5) 2_556 . . . ?
N1 Sn1 O1 Sn1 100.9(2) . . . 2_556 ?
O1 Sn1 O1 Sn1 0 2_556 . . 2_556 ?
Sn1 O1 C2 C3 162.2(4) 2_556 . . . ?
Sn1 O1 C2 C3 -35.0(6) . . . . ?
Sn1 O1 C2 C4 42.5(6) 2_556 . . . ?
Sn1 O1 C2 C4 -154.8(4) . . . . ?
Sn1 O1 C2 C5 -74.8(5) 2_556 . . . ?
Sn1 O1 C2 C5 87.9(5) . . . . ?
O1 C2 C5 Se1 175.5(4) . . . . ?
C3 C2 C5 Se1 -63.3(6) . . . . ?
C4 C2 C5 Se1 60.3(6) . . . . ?
C6 Se1 C5 C2 87.6(5) . . . . ?
C5 Se1 C6 C7 17.9(6) . . . . ?
C5 Se1 C6 C11 -163.2(5) . . . . ?
C11 C6 C7 C8 -0.8(10) . . . . ?
Se1 C6 C7 C8 178.1(5) . . . . ?
C6 C7 C8 C9 -0.1(10) . . . . ?
C7 C8 C9 C10 0.1(11) . . . . ?
C8 C9 C10 C11 0.8(11) . . . . ?
C9 C10 C11 C6 -1.7(10) . . . . ?
C9 C10 C11 C12 178.6(7) . . . . ?
C7 C6 C11 C10 1.7(9) . . . . ?
Se1 C6 C11 C10 -177.3(5) . . . . ?
C7 C6 C11 C12 -178.6(6) . . . . ?
Se1 C6 C11 C12 2.5(8) . . . . ?
C10 C11 C12 N13 119.8(7) . . . . ?
C6 C11 C12 N13 -60.0(8) . . . . ?
C11 C12 N13 C15 -65.0(8) . . . . ?
C11 C12 N13 C14 169.7(6) . . . . ?
O1 Sn1 N1 Si2 13.4(4) 2_556 . . . ?
O1 Sn1 N1 Si2 -60.3(4) . . . . ?
O1 Sn1 N1 Si1 -146.2(2) 2_556 . . . ?
O1 Sn1 N1 Si1 140.2(2) . . . . ?
Si2 N1 Si1 C21 151.5(4) . . . . ?
Sn1 N1 Si1 C21 -45.8(4) . . . . ?
Si2 N1 Si1 C23 32.6(4) . . . . ?
Sn1 N1 Si1 C23 -164.7(3) . . . . ?
Si2 N1 Si1 C22 -88.8(4) . . . . ?
Sn1 N1 Si1 C22 73.9(4) . . . . ?
Si1 N1 Si2 C24 168.8(3) . . . . ?
Sn1 N1 Si2 C24 11.0(5) . . . . ?
Si1 N1 Si2 C25 -71.8(4) . . . . ?
Sn1 N1 Si2 C25 130.4(4) . . . . ?
Si1 N1 Si2 C26 50.0(4) . . . . ?
Sn1 N1 Si2 C26 -107.8(4) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006882'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_9

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C38 H76 N4 O2 S2 Si4 Sn2'
_chemical_formula_sum            'C38 H76 N4 O2 S2 Si4 Sn2'
_chemical_formula_weight         1034.95
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9518(9)
_cell_length_b                   10.6790(11)
_cell_length_c                   13.8023(15)
_cell_angle_alpha                101.636(5)
_cell_angle_beta                 104.069(5)
_cell_angle_gamma                93.483(5)
_cell_volume                     1245.2(2)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6710
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.42
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.19
_exptl_crystal_density_diffrn    1.38
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             536
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.694
_exptl_absorpt_correction_T_max  0.794


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0391
_diffrn_reflns_number            15449
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.1
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_reflns_number_total             5620
_reflns_number_gt                5289
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0000P)²+16.4656P] 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_number_reflns         5620
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1493
_refine_ls_wR_factor_gt          0.1481
_refine_ls_goodness_of_fit_ref   1.193
_refine_ls_restrained_S_all      1.193
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         2.92
_refine_diff_density_min         -1.557
_refine_diff_density_rms         0.167

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.15785(5) 0.07751(4) 0.10660(3) 0.01452(12) Uani 1 1 d . . .
S1 S 0.17551(18) 0.39266(15) 0.10762(11) 0.0206(3) Uani 1 1 d . . .
O1 O -0.0383(5) 0.1133(4) -0.0078(3) 0.0173(8) Uani 1 1 d . . .
C2 C -0.0756(7) 0.2353(6) -0.0327(5) 0.0203(12) Uani 1 1 d . . .
C3 C -0.2502(8) 0.2272(6) -0.0752(5) 0.0265(14) Uani 1 1 d . . .
H3A H -0.2836 0.1597 -0.1383 0.04 Uiso 1 1 calc R . .
H3B H -0.2774 0.31 -0.0903 0.04 Uiso 1 1 calc R . .
H3C H -0.3021 0.2067 -0.0246 0.04 Uiso 1 1 calc R . .
C4 C 0.0057(8) 0.2643(6) -0.1118(5) 0.0249(13) Uani 1 1 d . . .
H4A H 0.1115 0.2407 -0.0953 0.037 Uiso 1 1 calc R . .
H4B H 0.0092 0.3564 -0.1111 0.037 Uiso 1 1 calc R . .
H4C H -0.0513 0.2145 -0.18 0.037 Uiso 1 1 calc R . .
C5 C -0.0315(7) 0.3424(6) 0.0665(5) 0.0197(12) Uani 1 1 d . . .
H5A H -0.0643 0.3105 0.1215 0.024 Uiso 1 1 calc R . .
H5B H -0.0872 0.4174 0.0544 0.024 Uiso 1 1 calc R . .
C6 C 0.2078(7) 0.4735(6) 0.2376(5) 0.0196(12) Uani 1 1 d . . .
C7 C 0.0888(8) 0.5090(6) 0.2827(5) 0.0239(13) Uani 1 1 d . . .
H7 H -0.0158 0.4898 0.2427 0.029 Uiso 1 1 calc R . .
C8 C 0.1208(9) 0.5724(7) 0.3860(5) 0.0294(15) Uani 1 1 d . . .
H8 H 0.0388 0.5955 0.4162 0.035 Uiso 1 1 calc R . .
C9 C 0.2732(10) 0.6011(7) 0.4435(5) 0.0348(17) Uani 1 1 d . . .
H9 H 0.2965 0.6444 0.5136 0.042 Uiso 1 1 calc R . .
C10 C 0.3921(8) 0.5666(7) 0.3988(6) 0.0310(15) Uani 1 1 d . . .
H10 H 0.4963 0.587 0.4394 0.037 Uiso 1 1 calc R . .
C11 C 0.3639(8) 0.5034(6) 0.2970(5) 0.0236(13) Uani 1 1 d . . .
C12 C 0.4953(8) 0.4653(7) 0.2499(5) 0.0271(14) Uani 1 1 d . . .
H12A H 0.5925 0.4768 0.3051 0.033 Uiso 1 1 calc R . .
H12B H 0.4738 0.3731 0.2151 0.033 Uiso 1 1 calc R . .
N13 N 0.5165(6) 0.5412(6) 0.1762(5) 0.0285(13) Uani 1 1 d . . .
C14A C 0.6148(9) 0.4787(10) 0.1149(7) 0.047(2) Uani 1 1 d . . .
H14A H 0.6291 0.5294 0.0654 0.07 Uiso 1 1 calc R . .
H14B H 0.5653 0.3921 0.0782 0.07 Uiso 1 1 calc R . .
H14C H 0.7159 0.4727 0.16 0.07 Uiso 1 1 calc R . .
C15A C 0.5855(10) 0.6707(8) 0.2276(7) 0.043(2) Uani 1 1 d . . .
H15A H 0.5243 0.709 0.2735 0.064 Uiso 1 1 calc R . .
H15B H 0.5874 0.7223 0.1766 0.064 Uiso 1 1 calc R . .
H15C H 0.6917 0.6686 0.2675 0.064 Uiso 1 1 calc R . .
N1 N 0.0666(6) 0.0802(5) 0.2374(4) 0.0183(10) Uani 1 1 d . . .
Si1 Si -0.1228(2) 0.07385(17) 0.24861(13) 0.0212(4) Uani 1 1 d . . .
Si2 Si 0.2146(2) 0.09447(18) 0.34871(13) 0.0224(4) Uani 1 1 d . . .
C21 C -0.2750(8) 0.0032(8) 0.1262(5) 0.0308(15) Uani 1 1 d . . .
H21A H -0.2691 0.0546 0.0757 0.046 Uiso 1 1 calc R . .
H21B H -0.3777 0.0036 0.1394 0.046 Uiso 1 1 calc R . .
H21C H -0.2576 -0.0854 0.0998 0.046 Uiso 1 1 calc R . .
C22 C -0.1552(9) -0.0266(8) 0.3405(5) 0.0323(16) Uani 1 1 d . . .
H22A H -0.1257 -0.1128 0.3194 0.049 Uiso 1 1 calc R . .
H22B H -0.265 -0.0333 0.3403 0.049 Uiso 1 1 calc R . .
H22C H -0.0919 0.014 0.4096 0.049 Uiso 1 1 calc R . .
C23 C -0.1793(9) 0.2379(7) 0.2973(6) 0.0352(17) Uani 1 1 d . . .
H23A H -0.0973 0.2847 0.3568 0.053 Uiso 1 1 calc R . .
H23B H -0.2765 0.2278 0.3172 0.053 Uiso 1 1 calc R . .
H23C H -0.1934 0.2862 0.2431 0.053 Uiso 1 1 calc R . .
C24 C 0.2409(10) -0.0637(7) 0.3879(6) 0.0365(17) Uani 1 1 d . . .
H24A H 0.1483 -0.0934 0.4066 0.055 Uiso 1 1 calc R . .
H24B H 0.3314 -0.0522 0.4469 0.055 Uiso 1 1 calc R . .
H24C H 0.2569 -0.1277 0.3307 0.055 Uiso 1 1 calc R . .
C25 C 0.1862(10) 0.2151(8) 0.4606(6) 0.0392(18) Uani 1 1 d . . .
H25A H 0.1837 0.3002 0.4443 0.059 Uiso 1 1 calc R . .
H25B H 0.272 0.2184 0.521 0.059 Uiso 1 1 calc R . .
H25C H 0.0881 0.1895 0.4748 0.059 Uiso 1 1 calc R . .
C26 C 0.4099(9) 0.1506(9) 0.3343(6) 0.0383(18) Uani 1 1 d . . .
H26A H 0.4428 0.0829 0.2873 0.057 Uiso 1 1 calc R . .
H26B H 0.4857 0.1699 0.4014 0.057 Uiso 1 1 calc R . .
H26C H 0.4028 0.2284 0.3067 0.057 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.150(5) . ?
Sn1 O1 2.168(4) . ?
Sn1 O1 2.250(4) 2 ?
S1 C6 1.772(6) . ?
S1 C5 1.813(6) . ?
O1 C2 1.450(7) . ?
O1 Sn1 2.250(4) 2 ?
C2 C3 1.521(9) . ?
C2 C4 1.521(9) . ?
C2 C5 1.546(8) . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 C7 1.394(9) . ?
C6 C11 1.417(9) . ?
C7 C8 1.402(9) . ?
C7 H7 0.95 . ?
C8 C9 1.381(11) . ?
C8 H8 0.95 . ?
C9 C10 1.387(11) . ?
C9 H9 0.95 . ?
C10 C11 1.385(10) . ?
C10 H10 0.95 . ?
C11 C12 1.514(9) . ?
C12 N13 1.462(9) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
N13 C15A 1.443(10) . ?
N13 C14A 1.464(10) . ?
C14A H14A 0.98 . ?
C14A H14B 0.98 . ?
C14A H14C 0.98 . ?
C15A H15A 0.98 . ?
C15A H15B 0.98 . ?
C15A H15C 0.98 . ?
N1 Si1 1.738(5) . ?
N1 Si2 1.741(5) . ?
Si1 C21 1.876(7) . ?
Si1 C22 1.879(7) . ?
Si1 C23 1.891(8) . ?
Si2 C25 1.880(8) . ?
Si2 C26 1.883(8) . ?
Si2 C24 1.886(8) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?


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 O1 103.09(18) . . ?
N1 Sn1 O1 99.46(17) . 2 ?
O1 Sn1 O1 71.78(17) . 2 ?
C6 S1 C5 103.9(3) . . ?
C2 O1 Sn1 128.1(3) . . ?
C2 O1 Sn1 122.8(3) . 2 ?
Sn1 O1 Sn1 108.22(17) . 2 ?
O1 C2 C3 108.6(5) . . ?
O1 C2 C4 110.3(5) . . ?
C3 C2 C4 109.8(5) . . ?
O1 C2 C5 109.4(5) . . ?
C3 C2 C5 106.6(5) . . ?
C4 C2 C5 112.0(5) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 S1 111.6(4) . . ?
C2 C5 H5A 109.3 . . ?
S1 C5 H5A 109.3 . . ?
C2 C5 H5B 109.3 . . ?
S1 C5 H5B 109.3 . . ?
H5A C5 H5B 108 . . ?
C7 C6 C11 119.4(6) . . ?
C7 C6 S1 123.4(5) . . ?
C11 C6 S1 117.2(5) . . ?
C6 C7 C8 121.1(6) . . ?
C6 C7 H7 119.5 . . ?
C8 C7 H7 119.5 . . ?
C9 C8 C7 119.2(7) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C10 120.0(7) . . ?
C8 C9 H9 120 . . ?
C10 C9 H9 120 . . ?
C11 C10 C9 122.1(7) . . ?
C11 C10 H10 119 . . ?
C9 C10 H10 119 . . ?
C10 C11 C6 118.3(6) . . ?
C10 C11 C12 121.3(6) . . ?
C6 C11 C12 120.4(6) . . ?
N13 C12 C11 112.5(6) . . ?
N13 C12 H12A 109.1 . . ?
C11 C12 H12A 109.1 . . ?
N13 C12 H12B 109.1 . . ?
C11 C12 H12B 109.1 . . ?
H12A C12 H12B 107.8 . . ?
C15A N13 C12 111.0(6) . . ?
C15A N13 C14A 110.0(7) . . ?
C12 N13 C14A 109.4(6) . . ?
N13 C14A H14A 109.5 . . ?
N13 C14A H14B 109.5 . . ?
H14A C14A H14B 109.5 . . ?
N13 C14A H14C 109.5 . . ?
H14A C14A H14C 109.5 . . ?
H14B C14A H14C 109.5 . . ?
N13 C15A H15A 109.5 . . ?
N13 C15A H15B 109.5 . . ?
H15A C15A H15B 109.5 . . ?
N13 C15A H15C 109.5 . . ?
H15A C15A H15C 109.5 . . ?
H15B C15A H15C 109.5 . . ?
Si1 N1 Si2 117.5(3) . . ?
Si1 N1 Sn1 131.2(3) . . ?
Si2 N1 Sn1 111.3(3) . . ?
N1 Si1 C21 114.9(3) . . ?
N1 Si1 C22 112.2(3) . . ?
C21 Si1 C22 105.0(3) . . ?
N1 Si1 C23 112.7(3) . . ?
C21 Si1 C23 105.2(4) . . ?
C22 Si1 C23 106.0(4) . . ?
N1 Si2 C25 113.1(3) . . ?
N1 Si2 C26 112.8(3) . . ?
C25 Si2 C26 104.9(4) . . ?
N1 Si2 C24 112.7(3) . . ?
C25 Si2 C24 108.3(4) . . ?
C26 Si2 C24 104.5(4) . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?


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
N1 Sn1 O1 C2 94.8(5) . . . . ?
O1 Sn1 O1 C2 -169.4(5) 2 . . . ?
N1 Sn1 O1 Sn1 -95.8(2) . . . 2 ?
O1 Sn1 O1 Sn1 0 2 . . 2 ?
Sn1 O1 C2 C3 -152.6(4) . . . . ?
Sn1 O1 C2 C3 39.4(6) 2 . . . ?
Sn1 O1 C2 C4 87.0(6) . . . . ?
Sn1 O1 C2 C4 -81.0(6) 2 . . . ?
Sn1 O1 C2 C5 -36.6(7) . . . . ?
Sn1 O1 C2 C5 155.4(4) 2 . . . ?
O1 C2 C5 S1 77.9(5) . . . . ?
C3 C2 C5 S1 -164.8(4) . . . . ?
C4 C2 C5 S1 -44.7(6) . . . . ?
C6 S1 C5 C2 -162.2(4) . . . . ?
C5 S1 C6 C7 -12.0(6) . . . . ?
C5 S1 C6 C11 168.4(5) . . . . ?
C11 C6 C7 C8 -0.7(10) . . . . ?
S1 C6 C7 C8 179.8(5) . . . . ?
C6 C7 C8 C9 0.6(11) . . . . ?
C7 C8 C9 C10 -0.2(11) . . . . ?
C8 C9 C10 C11 0.0(12) . . . . ?
C9 C10 C11 C6 -0.1(11) . . . . ?
C9 C10 C11 C12 -179.4(7) . . . . ?
C7 C6 C11 C10 0.4(9) . . . . ?
S1 C6 C11 C10 180.0(5) . . . . ?
C7 C6 C11 C12 179.7(6) . . . . ?
S1 C6 C11 C12 -0.7(8) . . . . ?
C10 C11 C12 N13 -110.0(7) . . . . ?
C6 C11 C12 N13 70.7(8) . . . . ?
C11 C12 N13 C15A 73.2(7) . . . . ?
C11 C12 N13 C14A -165.2(6) . . . . ?
O1 Sn1 N1 Si1 13.9(4) . . . . ?
O1 Sn1 N1 Si1 -59.5(4) 2 . . . ?
O1 Sn1 N1 Si2 -164.7(2) . . . . ?
O1 Sn1 N1 Si2 121.9(3) 2 . . . ?
Si2 N1 Si1 C21 -159.9(3) . . . . ?
Sn1 N1 Si1 C21 21.5(5) . . . . ?
Si2 N1 Si1 C22 -40.1(4) . . . . ?
Sn1 N1 Si1 C22 141.3(4) . . . . ?
Si2 N1 Si1 C23 79.5(4) . . . . ?
Sn1 N1 Si1 C23 -99.0(4) . . . . ?
Si1 N1 Si2 C25 -43.6(5) . . . . ?
Sn1 N1 Si2 C25 135.2(3) . . . . ?
Si1 N1 Si2 C26 -162.4(4) . . . . ?
Sn1 N1 Si2 C26 16.5(4) . . . . ?
Si1 N1 Si2 C24 79.6(4) . . . . ?
Sn1 N1 Si2 C24 -101.5(4) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006883'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_10

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C19 H38 N2 O1 Pb1 Se1 Si2'
_chemical_formula_sum            'C19 H38 N2 O Pb Se Si2'
_chemical_formula_weight         652.84
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9533(3)
_cell_length_b                   10.7807(4)
_cell_length_c                   13.9822(5)
_cell_angle_alpha                101.8840(10)
_cell_angle_beta                 103.3150(10)
_cell_angle_gamma                93.6150(10)
_cell_volume                     1276.49(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8187
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      27.35
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    8.139
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_T_max  0.850


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_number            17730
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.952
_reflns_number_total             5554
_reflns_number_gt                4938
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0159P)²+0.0000P] 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_number_reflns         5554
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0237
_refine_ls_wR_factor_ref         0.0454
_refine_ls_wR_factor_gt          0.0433
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.862
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.123

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.665777(13) 0.081804(12) 0.108549(8) 0.01578(4) Uani 1 1 d . . .
Se2 Se 0.69079(4) 0.39740(3) 0.10303(2) 0.02001(8) Uani 1 1 d . . .
Si3 Si 0.38141(10) 0.07753(9) 0.25376(7) 0.0213(2) Uani 1 1 d . . .
Si4 Si 0.71822(11) 0.09660(10) 0.35240(7) 0.0235(2) Uani 1 1 d . . .
C1 C 1.1219(5) 0.4840(5) 0.1217(3) 0.0486(12) Uani 1 1 d . . .
H1A H 1.1298 0.5307 0.0696 0.073 Uiso 1 1 calc R . .
H1B H 1.0778 0.3956 0.0897 0.073 Uiso 1 1 calc R . .
H1C H 1.225 0.4849 0.1653 0.073 Uiso 1 1 calc R . .
N2 N 1.0229(3) 0.5443(3) 0.1819(2) 0.0277(7) Uani 1 1 d . . .
C3 C 1.0836(4) 0.6773(4) 0.2281(3) 0.0431(11) Uani 1 1 d . . .
H3A H 1.0134 0.7173 0.2664 0.065 Uiso 1 1 calc R . .
H3B H 1.0922 0.7227 0.1753 0.065 Uiso 1 1 calc R . .
H3C H 1.1858 0.6813 0.2737 0.065 Uiso 1 1 calc R . .
C4 C 1.0061(4) 0.4745(3) 0.2584(3) 0.0255(8) Uani 1 1 d . . .
H4A H 1.1022 0.493 0.3132 0.031 Uiso 1 1 calc R . .
H4B H 0.9914 0.3818 0.2279 0.031 Uiso 1 1 calc R . .
C5 C 0.8710(4) 0.5092(3) 0.3025(2) 0.0230(8) Uani 1 1 d . . .
C6 C 0.8946(4) 0.5700(3) 0.4030(3) 0.0288(9) Uani 1 1 d . . .
H6 H 0.9971 0.5914 0.4442 0.035 Uiso 1 1 calc R . .
C7 C 0.7722(4) 0.6005(4) 0.4449(3) 0.0355(10) Uani 1 1 d . . .
H7 H 0.7908 0.641 0.5144 0.043 Uiso 1 1 calc R . .
C8 C 0.6230(4) 0.5717(4) 0.3855(3) 0.0307(9) Uani 1 1 d . . .
H8 H 0.5386 0.5931 0.4137 0.037 Uiso 1 1 calc R . .
C9 C 0.5966(4) 0.5119(3) 0.2849(2) 0.0229(8) Uani 1 1 d . . .
H9 H 0.4937 0.4925 0.244 0.027 Uiso 1 1 calc R . .
C10 C 0.7190(4) 0.4797(3) 0.2430(2) 0.0194(7) Uani 1 1 d . . .
C11 C 0.4674(3) 0.3432(3) 0.0636(2) 0.0204(7) Uani 1 1 d . . .
H11A H 0.4367 0.3131 0.1194 0.024 Uiso 1 1 calc R . .
H11B H 0.4114 0.4172 0.0522 0.024 Uiso 1 1 calc R . .
C12 C 0.4200(4) 0.2354(3) -0.0330(2) 0.0180(7) Uani 1 1 d . . .
C13 C 0.4967(4) 0.2627(3) -0.1148(2) 0.0261(8) Uani 1 1 d . . .
H13A H 0.6092 0.268 -0.0903 0.039 Uiso 1 1 calc R . .
H13B H 0.4689 0.3439 -0.1308 0.039 Uiso 1 1 calc R . .
H13C H 0.4612 0.1939 -0.1755 0.039 Uiso 1 1 calc R . .
C14 C 0.2436(4) 0.2282(3) -0.0714(3) 0.0297(9) Uani 1 1 d . . .
H14A H 0.2081 0.162 -0.1339 0.045 Uiso 1 1 calc R . .
H14B H 0.2162 0.3108 -0.0845 0.045 Uiso 1 1 calc R . .
H14C H 0.194 0.2073 -0.0202 0.045 Uiso 1 1 calc R . .
O15 O 0.4606(2) 0.1169(2) -0.00840(15) 0.0176(5) Uani 1 1 d . . .
N16 N 0.5710(3) 0.0839(3) 0.24514(18) 0.0188(6) Uani 1 1 d . . .
C17 C 0.3235(4) 0.2396(4) 0.2982(3) 0.0349(9) Uani 1 1 d . . .
H17A H 0.3983 0.2844 0.3606 0.052 Uiso 1 1 calc R . .
H17B H 0.2206 0.2303 0.3109 0.052 Uiso 1 1 calc R . .
H17C H 0.3213 0.2887 0.2463 0.052 Uiso 1 1 calc R . .
C18 C 0.3440(4) -0.0217(4) 0.3438(3) 0.0330(9) Uani 1 1 d . . .
H18A H 0.373 -0.1074 0.3232 0.05 Uiso 1 1 calc R . .
H18B H 0.234 -0.0276 0.343 0.05 Uiso 1 1 calc R . .
H18C H 0.4056 0.0184 0.4122 0.05 Uiso 1 1 calc R . .
C19 C 0.2373(4) 0.0058(4) 0.1318(2) 0.0273(8) Uani 1 1 d . . .
H19A H 0.2453 0.0571 0.0826 0.041 Uiso 1 1 calc R . .
H19B H 0.133 0.0039 0.1427 0.041 Uiso 1 1 calc R . .
H19C H 0.2581 -0.0814 0.1062 0.041 Uiso 1 1 calc R . .
C20 C 0.6931(4) 0.2170(4) 0.4639(2) 0.0333(9) Uani 1 1 d . . .
H20A H 0.6889 0.301 0.4475 0.05 Uiso 1 1 calc R . .
H20B H 0.7805 0.2212 0.5219 0.05 Uiso 1 1 calc R . .
H20C H 0.5968 0.1915 0.4805 0.05 Uiso 1 1 calc R . .
C21 C 0.7466(5) -0.0588(4) 0.3895(3) 0.0372(10) Uani 1 1 d . . .
H21A H 0.6515 -0.093 0.403 0.056 Uiso 1 1 calc R . .
H21B H 0.8314 -0.0456 0.4504 0.056 Uiso 1 1 calc R . .
H21C H 0.7719 -0.1194 0.3345 0.056 Uiso 1 1 calc R . .
C22 C 0.9104(4) 0.1524(4) 0.3335(3) 0.0381(10) Uani 1 1 d . . .
H22A H 0.9367 0.0889 0.2808 0.057 Uiso 1 1 calc R . .
H22B H 0.99 0.1633 0.3968 0.057 Uiso 1 1 calc R . .
H22C H 0.9046 0.234 0.3132 0.057 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N16 2.258(2) . ?
Pb1 O15 2.269(2) . ?
Pb1 O15 2.357(2) 2_655 ?
Se2 C10 1.926(3) . ?
Se2 C11 1.964(3) . ?
Si3 N16 1.727(3) . ?
Si3 C19 1.868(3) . ?
Si3 C17 1.877(4) . ?
Si3 C18 1.883(4) . ?
Si4 N16 1.728(3) . ?
Si4 C21 1.869(4) . ?
Si4 C20 1.879(3) . ?
Si4 C22 1.880(4) . ?
C1 N2 1.452(5) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
N2 C4 1.457(4) . ?
N2 C3 1.458(5) . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 C5 1.513(5) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C5 C6 1.384(5) . ?
C5 C10 1.401(4) . ?
C6 C7 1.383(5) . ?
C6 H6 0.95 . ?
C7 C8 1.379(5) . ?
C7 H7 0.95 . ?
C8 C9 1.380(4) . ?
C8 H8 0.95 . ?
C9 C10 1.387(4) . ?
C9 H9 0.95 . ?
C11 C12 1.544(4) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C12 O15 1.437(4) . ?
C12 C13 1.529(4) . ?
C12 C14 1.539(4) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
O15 Pb1 2.357(2) 2_655 ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?


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
N16 Pb1 O15 103.37(8) . . ?
N16 Pb1 O15 98.66(8) . 2_655 ?
O15 Pb1 O15 71.39(9) . 2_655 ?
C10 Se2 C11 100.83(13) . . ?
N16 Si3 C19 114.02(14) . . ?
N16 Si3 C17 112.55(15) . . ?
C19 Si3 C17 105.41(18) . . ?
N16 Si3 C18 112.09(16) . . ?
C19 Si3 C18 105.23(16) . . ?
C17 Si3 C18 106.91(18) . . ?
N16 Si4 C21 113.29(15) . . ?
N16 Si4 C20 113.09(16) . . ?
C21 Si4 C20 108.80(17) . . ?
N16 Si4 C22 111.64(15) . . ?
C21 Si4 C22 104.50(19) . . ?
C20 Si4 C22 104.83(17) . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C1 N2 C4 110.5(3) . . ?
C1 N2 C3 110.6(3) . . ?
C4 N2 C3 110.9(3) . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C4 C5 112.4(3) . . ?
N2 C4 H4A 109.1 . . ?
C5 C4 H4A 109.1 . . ?
N2 C4 H4B 109.1 . . ?
C5 C4 H4B 109.1 . . ?
H4A C4 H4B 107.9 . . ?
C6 C5 C10 118.3(3) . . ?
C6 C5 C4 120.8(3) . . ?
C10 C5 C4 120.9(3) . . ?
C7 C6 C5 121.5(3) . . ?
C7 C6 H6 119.2 . . ?
C5 C6 H6 119.2 . . ?
C8 C7 C6 119.7(3) . . ?
C8 C7 H7 120.2 . . ?
C6 C7 H7 120.2 . . ?
C7 C8 C9 119.9(3) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 H8 120.1 . . ?
C8 C9 C10 120.6(3) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C9 C10 C5 120.0(3) . . ?
C9 C10 Se2 122.8(2) . . ?
C5 C10 Se2 117.2(2) . . ?
C12 C11 Se2 112.0(2) . . ?
C12 C11 H11A 109.2 . . ?
Se2 C11 H11A 109.2 . . ?
C12 C11 H11B 109.2 . . ?
Se2 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
O15 C12 C13 110.0(3) . . ?
O15 C12 C14 109.8(2) . . ?
C13 C12 C14 109.3(3) . . ?
O15 C12 C11 109.2(2) . . ?
C13 C12 C11 111.9(2) . . ?
C14 C12 C11 106.4(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 O15 Pb1 128.82(16) . . ?
C12 O15 Pb1 121.93(16) . 2_655 ?
Pb1 O15 Pb1 108.61(9) . 2_655 ?
Si3 N16 Si4 119.69(15) . . ?
Si3 N16 Pb1 129.18(13) . . ?
Si4 N16 Pb1 111.11(12) . . ?
Si3 C17 H17A 109.5 . . ?
Si3 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Si3 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si3 C18 H18A 109.5 . . ?
Si3 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
Si3 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si3 C19 H19A 109.5 . . ?
Si3 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
Si3 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si4 C20 H20A 109.5 . . ?
Si4 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
Si4 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si4 C21 H21A 109.5 . . ?
Si4 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si4 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si4 C22 H22A 109.5 . . ?
Si4 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si4 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?


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
C1 N2 C4 C5 -163.6(3) . . . . ?
C3 N2 C4 C5 73.4(4) . . . . ?
N2 C4 C5 C6 -114.7(4) . . . . ?
N2 C4 C5 C10 65.8(4) . . . . ?
C10 C5 C6 C7 0.6(6) . . . . ?
C4 C5 C6 C7 -178.9(4) . . . . ?
C5 C6 C7 C8 -1.0(6) . . . . ?
C6 C7 C8 C9 0.6(6) . . . . ?
C7 C8 C9 C10 0.3(6) . . . . ?
C8 C9 C10 C5 -0.7(5) . . . . ?
C8 C9 C10 Se2 -179.5(3) . . . . ?
C6 C5 C10 C9 0.3(5) . . . . ?
C4 C5 C10 C9 179.8(3) . . . . ?
C6 C5 C10 Se2 179.1(3) . . . . ?
C4 C5 C10 Se2 -1.4(4) . . . . ?
C11 Se2 C10 C9 -13.6(3) . . . . ?
C11 Se2 C10 C5 167.7(3) . . . . ?
C10 Se2 C11 C12 -160.1(2) . . . . ?
Se2 C11 C12 O15 76.8(3) . . . . ?
Se2 C11 C12 C13 -45.3(3) . . . . ?
Se2 C11 C12 C14 -164.7(2) . . . . ?
C13 C12 O15 Pb1 89.0(3) . . . . ?
C14 C12 O15 Pb1 -150.6(2) . . . . ?
C11 C12 O15 Pb1 -34.2(3) . . . . ?
C13 C12 O15 Pb1 -80.7(3) . . . 2_655 ?
C14 C12 O15 Pb1 39.7(3) . . . 2_655 ?
C11 C12 O15 Pb1 156.09(17) . . . 2_655 ?
N16 Pb1 O15 C12 94.4(2) . . . . ?
O15 Pb1 O15 C12 -170.8(3) 2_655 . . . ?
N16 Pb1 O15 Pb1 -94.78(10) . . . 2_655 ?
O15 Pb1 O15 Pb1 0 2_655 . . 2_655 ?
C19 Si3 N16 Si4 -158.76(19) . . . . ?
C17 Si3 N16 Si4 81.2(2) . . . . ?
C18 Si3 N16 Si4 -39.3(2) . . . . ?
C19 Si3 N16 Pb1 22.6(3) . . . . ?
C17 Si3 N16 Pb1 -97.4(2) . . . . ?
C18 Si3 N16 Pb1 142.01(19) . . . . ?
C21 Si4 N16 Si3 80.1(2) . . . . ?
C20 Si4 N16 Si3 -44.3(2) . . . . ?
C22 Si4 N16 Si3 -162.3(2) . . . . ?
C21 Si4 N16 Pb1 -101.04(18) . . . . ?
C20 Si4 N16 Pb1 134.55(15) . . . . ?
C22 Si4 N16 Pb1 16.6(2) . . . . ?
O15 Pb1 N16 Si3 13.0(2) . . . . ?
O15 Pb1 N16 Si3 -59.81(19) 2_655 . . . ?
O15 Pb1 N16 Si4 -165.75(13) . . . . ?
O15 Pb1 N16 Si4 121.44(14) 2_655 . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006884'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_11

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C38 H76 N4 O2 Pb2 S2 Si4'
_chemical_formula_sum            'C38 H76 N4 O2 Pb2 S2 Si4'
_chemical_formula_weight         1211.89
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9509(3)
_cell_length_b                   10.6875(4)
_cell_length_c                   13.9731(5)
_cell_angle_alpha                102.1710(10)
_cell_angle_beta                 103.790(2)
_cell_angle_gamma                93.8130(10)
_cell_volume                     1259.36(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9942
_cell_measurement_theta_min      2.36
_cell_measurement_theta_max      27.46
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             600
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    6.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_T_max  0.709


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_unetI/netI     0.0313
_diffrn_reflns_number            20184
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.09
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_full        27.46
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_reflns_number_total             5741
_reflns_number_gt                5408
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0204P)²+0.0000P] 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_number_reflns         5741
_refine_ls_number_parameters     245
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0206
_refine_ls_R_factor_gt           0.0185
_refine_ls_wR_factor_ref         0.0432
_refine_ls_wR_factor_gt          0.0424
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.966
_refine_diff_density_min         -0.481
_refine_diff_density_rms         0.097

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.165903(9) 0.084110(8) 0.609931(6) 0.01594(4) Uani 1 1 d . . .
Si1 Si -0.11877(8) 0.07580(7) 0.75372(5) 0.02180(15) Uani 1 1 d . . .
Si2 Si 0.21910(8) 0.09458(7) 0.85357(5) 0.02350(16) Uani 1 1 d . . .
N1 N 0.0709(2) 0.0827(2) 0.74558(15) 0.0189(4) Uani 1 1 d . . .
C2 C -0.2648(3) 0.0062(3) 0.6298(2) 0.0311(7) Uani 1 1 d . . .
H2A H -0.2539 0.0581 0.5813 0.047 Uiso 1 1 calc R . .
H2B H -0.3695 0.0066 0.6399 0.047 Uiso 1 1 calc R . .
H2C H -0.2475 -0.0826 0.6034 0.047 Uiso 1 1 calc R . .
C3 C -0.1752(3) 0.2386(3) 0.8018(2) 0.0356(7) Uani 1 1 d . . .
H3A H -0.1002 0.282 0.8656 0.053 Uiso 1 1 calc R . .
H3B H -0.2787 0.2284 0.8133 0.053 Uiso 1 1 calc R . .
H3C H -0.1761 0.2905 0.7516 0.053 Uiso 1 1 calc R . .
C4 C -0.1567(3) -0.0271(3) 0.8409(2) 0.0339(7) Uani 1 1 d . . .
H4A H -0.1337 -0.1147 0.8165 0.051 Uiso 1 1 calc R . .
H4B H -0.2657 -0.0297 0.8424 0.051 Uiso 1 1 calc R . .
H4C H -0.0904 0.0094 0.9093 0.051 Uiso 1 1 calc R . .
C5 C 0.1965(4) 0.2176(3) 0.9652(2) 0.0356(7) Uani 1 1 d . . .
H5A H 0.1956 0.3025 0.9491 0.053 Uiso 1 1 calc R . .
H5B H 0.2833 0.2207 1.024 0.053 Uiso 1 1 calc R . .
H5C H 0.0988 0.1938 0.9808 0.053 Uiso 1 1 calc R . .
C6 C 0.2439(4) -0.0628(3) 0.8909(2) 0.0362(7) Uani 1 1 d . . .
H6A H 0.149 -0.0948 0.9059 0.054 Uiso 1 1 calc R . .
H6B H 0.331 -0.0502 0.9512 0.054 Uiso 1 1 calc R . .
H6C H 0.2648 -0.1258 0.8351 0.054 Uiso 1 1 calc R . .
C7 C 0.4131(3) 0.1486(3) 0.8360(2) 0.0369(7) Uani 1 1 d . . .
H7A H 0.4385 0.0834 0.7836 0.055 Uiso 1 1 calc R . .
H7B H 0.4926 0.1599 0.9 0.055 Uiso 1 1 calc R . .
H7C H 0.4092 0.2307 0.8154 0.055 Uiso 1 1 calc R . .
O11 O -0.04112(18) 0.11782(15) 0.49189(12) 0.0178(3) Uani 1 1 d . . .
C12 C -0.0795(3) 0.2369(2) 0.46651(18) 0.0187(5) Uani 1 1 d . . .
C13 C -0.2564(3) 0.2274(3) 0.4240(2) 0.0286(6) Uani 1 1 d . . .
H13A H -0.2898 0.1587 0.3619 0.043 Uiso 1 1 calc R . .
H13B H -0.2835 0.3097 0.4088 0.043 Uiso 1 1 calc R . .
H13C H -0.3084 0.2078 0.4743 0.043 Uiso 1 1 calc R . .
C14 C 0.0018(3) 0.2650(3) 0.38740(19) 0.0275(6) Uani 1 1 d . . .
H14A H 0.1144 0.2735 0.4153 0.041 Uiso 1 1 calc R . .
H14B H -0.0273 0.3456 0.3695 0.041 Uiso 1 1 calc R . .
H14C H -0.0294 0.1941 0.3267 0.041 Uiso 1 1 calc R . .
C15 C -0.0360(3) 0.3458(2) 0.56405(19) 0.0217(5) Uani 1 1 d . . .
H15A H -0.0727 0.3163 0.618 0.026 Uiso 1 1 calc R . .
H15B H -0.0882 0.4216 0.551 0.026 Uiso 1 1 calc R . .
S1 S 0.17279(7) 0.39237(6) 0.60675(5) 0.02198(13) Uani 1 1 d . . .
C16 C 0.2064(3) 0.4730(2) 0.73633(19) 0.0199(5) Uani 1 1 d . . .
C17 C 0.0874(3) 0.5099(2) 0.7809(2) 0.0244(6) Uani 1 1 d . . .
H17 H -0.0171 0.4926 0.7411 0.029 Uiso 1 1 calc R . .
C18 C 0.1202(3) 0.5718(3) 0.8830(2) 0.0311(6) Uani 1 1 d . . .
H18 H 0.0387 0.5962 0.9131 0.037 Uiso 1 1 calc R . .
C19 C 0.2732(4) 0.5978(3) 0.9408(2) 0.0357(7) Uani 1 1 d . . .
H19 H 0.2967 0.6398 1.0106 0.043 Uiso 1 1 calc R . .
C20 C 0.3907(3) 0.5625(3) 0.8963(2) 0.0309(6) Uani 1 1 d . . .
H20 H 0.4949 0.5815 0.9362 0.037 Uiso 1 1 calc R . .
C21 C 0.3611(3) 0.4999(3) 0.7946(2) 0.0240(6) Uani 1 1 d . . .
C22 C 0.4915(3) 0.4616(3) 0.7482(2) 0.0271(6) Uani 1 1 d . . .
H22A H 0.5882 0.4728 0.8029 0.033 Uiso 1 1 calc R . .
H22B H 0.4689 0.369 0.7133 0.033 Uiso 1 1 calc R . .
N23 N 0.5159(2) 0.5366(2) 0.67567(18) 0.0297(5) Uani 1 1 d . . .
C24 C 0.5860(4) 0.6680(3) 0.7286(3) 0.0450(8) Uani 1 1 d . . .
H24A H 0.5154 0.711 0.7649 0.068 Uiso 1 1 calc R . .
H24B H 0.6054 0.7158 0.6793 0.068 Uiso 1 1 calc R . .
H24C H 0.6841 0.6652 0.7771 0.068 Uiso 1 1 calc R . .
C25 C 0.6131(4) 0.4740(4) 0.6151(3) 0.0499(9) Uani 1 1 d . . .
H25A H 0.7145 0.4694 0.6595 0.075 Uiso 1 1 calc R . .
H25B H 0.6268 0.5238 0.5658 0.075 Uiso 1 1 calc R . .
H25C H 0.5637 0.3867 0.5793 0.075 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.2571(19) . ?
Pb1 O11 2.2729(16) . ?
Pb1 O11 2.3572(16) 2_556 ?
Si1 N1 1.726(2) . ?
Si1 C2 1.873(3) . ?
Si1 C3 1.876(3) . ?
Si1 C4 1.876(3) . ?
Si2 N1 1.731(2) . ?
Si2 C6 1.875(3) . ?
Si2 C5 1.877(3) . ?
Si2 C7 1.881(3) . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
O11 C12 1.433(3) . ?
O11 Pb1 2.3572(16) 2_556 ?
C12 C14 1.529(3) . ?
C12 C13 1.541(3) . ?
C12 C15 1.543(3) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 S1 1.821(2) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
S1 C16 1.778(3) . ?
C16 C17 1.395(4) . ?
C16 C21 1.405(3) . ?
C17 C18 1.392(4) . ?
C17 H17 0.95 . ?
C18 C19 1.389(4) . ?
C18 H18 0.95 . ?
C19 C20 1.379(4) . ?
C19 H19 0.95 . ?
C20 C21 1.390(4) . ?
C20 H20 0.95 . ?
C21 C22 1.505(4) . ?
C22 N23 1.463(3) . ?
C22 H22A 0.99 . ?
C22 H22B 0.99 . ?
N23 C25 1.453(4) . ?
N23 C24 1.461(4) . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?


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 O11 103.35(6) . . ?
N1 Pb1 O11 98.24(6) . 2_556 ?
O11 Pb1 O11 71.62(7) . 2_556 ?
N1 Si1 C2 113.94(11) . . ?
N1 Si1 C3 112.78(12) . . ?
C2 Si1 C3 105.35(14) . . ?
N1 Si1 C4 112.07(12) . . ?
C2 Si1 C4 105.36(13) . . ?
C3 Si1 C4 106.70(14) . . ?
N1 Si2 C6 113.44(12) . . ?
N1 Si2 C5 112.78(13) . . ?
C6 Si2 C5 108.78(14) . . ?
N1 Si2 C7 111.96(11) . . ?
C6 Si2 C7 104.47(15) . . ?
C5 Si2 C7 104.72(14) . . ?
Si1 N1 Si2 119.56(11) . . ?
Si1 N1 Pb1 129.42(11) . . ?
Si2 N1 Pb1 111.00(10) . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C12 O11 Pb1 128.40(14) . . ?
C12 O11 Pb1 122.26(13) . 2_556 ?
Pb1 O11 Pb1 108.38(7) . 2_556 ?
O11 C12 C14 110.3(2) . . ?
O11 C12 C13 109.23(19) . . ?
C14 C12 C13 109.6(2) . . ?
O11 C12 C15 109.1(2) . . ?
C14 C12 C15 112.0(2) . . ?
C13 C12 C15 106.5(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 S1 111.09(17) . . ?
C12 C15 H15A 109.4 . . ?
S1 C15 H15A 109.4 . . ?
C12 C15 H15B 109.4 . . ?
S1 C15 H15B 109.4 . . ?
H15A C15 H15B 108 . . ?
C16 S1 C15 104.44(12) . . ?
C17 C16 C21 119.8(2) . . ?
C17 C16 S1 123.0(2) . . ?
C21 C16 S1 117.18(19) . . ?
C18 C17 C16 120.6(3) . . ?
C18 C17 H17 119.7 . . ?
C16 C17 H17 119.7 . . ?
C19 C18 C17 119.6(3) . . ?
C19 C18 H18 120.2 . . ?
C17 C18 H18 120.2 . . ?
C20 C19 C18 119.7(3) . . ?
C20 C19 H19 120.1 . . ?
C18 C19 H19 120.1 . . ?
C19 C20 C21 121.9(3) . . ?
C19 C20 H20 119 . . ?
C21 C20 H20 119 . . ?
C20 C21 C16 118.4(2) . . ?
C20 C21 C22 120.8(2) . . ?
C16 C21 C22 120.8(2) . . ?
N23 C22 C21 113.1(2) . . ?
N23 C22 H22A 109 . . ?
C21 C22 H22A 109 . . ?
N23 C22 H22B 109 . . ?
C21 C22 H22B 109 . . ?
H22A C22 H22B 107.8 . . ?
C25 N23 C24 110.5(2) . . ?
C25 N23 C22 110.0(2) . . ?
C24 N23 C22 110.5(2) . . ?
N23 C24 H24A 109.5 . . ?
N23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
N23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
N23 C25 H25A 109.5 . . ?
N23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?


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
C2 Si1 N1 Si2 -159.56(14) . . . . ?
C3 Si1 N1 Si2 80.40(17) . . . . ?
C4 Si1 N1 Si2 -40.04(18) . . . . ?
C2 Si1 N1 Pb1 22.35(19) . . . . ?
C3 Si1 N1 Pb1 -97.69(17) . . . . ?
C4 Si1 N1 Pb1 141.87(14) . . . . ?
C6 Si2 N1 Si1 78.72(18) . . . . ?
C5 Si2 N1 Si1 -45.54(17) . . . . ?
C7 Si2 N1 Si1 -163.35(15) . . . . ?
C6 Si2 N1 Pb1 -102.87(14) . . . . ?
C5 Si2 N1 Pb1 132.88(12) . . . . ?
C7 Si2 N1 Pb1 15.07(17) . . . . ?
O11 Pb1 N1 Si1 11.75(15) . . . . ?
O11 Pb1 N1 Si1 -61.20(15) 2_556 . . . ?
O11 Pb1 N1 Si2 -166.47(9) . . . . ?
O11 Pb1 N1 Si2 120.58(10) 2_556 . . . ?
N1 Pb1 O11 C12 96.76(18) . . . . ?
O11 Pb1 O11 C12 -168.9(2) 2_556 . . . ?
N1 Pb1 O11 Pb1 -94.39(8) . . . 2_556 ?
O11 Pb1 O11 Pb1 0 2_556 . . 2_556 ?
Pb1 O11 C12 C14 86.4(2) . . . . ?
Pb1 O11 C12 C14 -81.1(2) 2_556 . . . ?
Pb1 O11 C12 C13 -153.08(16) . . . . ?
Pb1 O11 C12 C13 39.5(2) 2_556 . . . ?
Pb1 O11 C12 C15 -37.1(2) . . . . ?
Pb1 O11 C12 C15 155.47(14) 2_556 . . . ?
O11 C12 C15 S1 75.1(2) . . . . ?
C14 C12 C15 S1 -47.3(3) . . . . ?
C13 C12 C15 S1 -167.13(17) . . . . ?
C12 C15 S1 C16 -160.64(18) . . . . ?
C15 S1 C16 C17 -11.3(3) . . . . ?
C15 S1 C16 C21 168.9(2) . . . . ?
C21 C16 C17 C18 -0.8(4) . . . . ?
S1 C16 C17 C18 179.4(2) . . . . ?
C16 C17 C18 C19 0.5(4) . . . . ?
C17 C18 C19 C20 0.2(4) . . . . ?
C18 C19 C20 C21 -0.6(5) . . . . ?
C19 C20 C21 C16 0.3(4) . . . . ?
C19 C20 C21 C22 -179.5(3) . . . . ?
C17 C16 C21 C20 0.4(4) . . . . ?
S1 C16 C21 C20 -179.8(2) . . . . ?
C17 C16 C21 C22 -179.8(2) . . . . ?
S1 C16 C21 C22 0.0(3) . . . . ?
C20 C21 C22 N23 -110.7(3) . . . . ?
C16 C21 C22 N23 69.5(3) . . . . ?
C21 C22 N23 C25 -165.2(2) . . . . ?
C21 C22 N23 C24 72.5(3) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006885'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_12

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C44 H76 N4 O2 S2 Si4 Sn2'
_chemical_formula_sum            'C44 H76 N4 O2 S2 Si4 Sn2'
_chemical_formula_weight         1107.01
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.6263(11)
_cell_length_b                   8.4904(4)
_cell_length_c                   21.1602(11)
_cell_angle_alpha                90
_cell_angle_beta                 107.158(3)
_cell_angle_gamma                90
_cell_volume                     2682.5(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1601
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      24.41
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       stick
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.37
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1144
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.135
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.781
_exptl_absorpt_correction_T_max  0.934


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_number            23307
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.07
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_reflns_number_total             6117
_reflns_number_gt                4714
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0175P)²+0.0000P] 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_number_reflns         6117
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0394
_refine_ls_wR_factor_ref         0.0754
_refine_ls_wR_factor_gt          0.0693
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_restrained_S_all      1.028
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.106

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.093973(15) -0.12927(2) 0.533052(10) 0.01738(7) Uani 1 1 d . . .
Si1 Si 0.12077(7) 0.08901(11) 0.68009(4) 0.0241(2) Uani 1 1 d . . .
Si2 Si 0.20350(6) -0.22583(11) 0.68251(4) 0.0201(2) Uani 1 1 d . . .
S1 S 0.26299(6) 0.02489(10) 0.50083(4) 0.0242(2) Uani 1 1 d . . .
O1 O 0.05701(14) 0.0994(2) 0.48796(10) 0.0203(5) Uani 1 1 d . . .
C2 C 0.1112(2) 0.2077(4) 0.46392(16) 0.0254(8) Uani 1 1 d . . .
C3 C 0.0745(2) 0.3737(4) 0.4641(2) 0.0405(10) Uani 1 1 d . . .
H3A H 0.0125 0.3774 0.4356 0.061 Uiso 1 1 calc R . .
H3B H 0.1111 0.4477 0.4476 0.061 Uiso 1 1 calc R . .
H3C H 0.0764 0.4028 0.5093 0.061 Uiso 1 1 calc R . .
C4 C 0.1090(2) 0.1623(4) 0.39354(16) 0.0371(10) Uani 1 1 d . . .
H4A H 0.1282 0.0526 0.3929 0.056 Uiso 1 1 calc R . .
H4B H 0.1494 0.2312 0.3786 0.056 Uiso 1 1 calc R . .
H4C H 0.0479 0.1741 0.364 0.056 Uiso 1 1 calc R . .
C5 C 0.2072(2) 0.2065(4) 0.51151(17) 0.0260(8) Uani 1 1 d . . .
H5A H 0.2053 0.2148 0.5577 0.031 Uiso 1 1 calc R . .
H5B H 0.2409 0.298 0.5023 0.031 Uiso 1 1 calc R . .
C6 C 0.3632(2) 0.0262(4) 0.56815(15) 0.0249(8) Uani 1 1 d . . .
C7 C 0.3864(2) 0.1560(4) 0.60836(16) 0.0320(9) Uani 1 1 d . . .
H7 H 0.3523 0.25 0.5972 0.038 Uiso 1 1 calc R . .
C8 C 0.4607(2) 0.1514(5) 0.66642(18) 0.0392(10) Uani 1 1 d . . .
H8 H 0.4771 0.243 0.693 0.047 Uiso 1 1 calc R . .
C9 C 0.5081(3) 0.0175(5) 0.68393(18) 0.0437(11) Uani 1 1 d . . .
H9 H 0.5556 0.0146 0.7241 0.052 Uiso 1 1 calc R . .
C10 C 0.4889(2) -0.1181(5) 0.64409(17) 0.0353(9) Uani 1 1 d . . .
C11 C 0.5362(3) -0.2614(6) 0.6629(2) 0.0508(12) Uani 1 1 d . . .
H11 H 0.583 -0.2658 0.7035 0.061 Uiso 1 1 calc R . .
C12 C 0.5165(3) -0.3919(6) 0.6248(2) 0.0564(13) Uani 1 1 d . . .
H12 H 0.5465 -0.4881 0.6401 0.068 Uiso 1 1 calc R . .
C13 C 0.4520(3) -0.3859(5) 0.56284(19) 0.0445(11) Uani 1 1 d . . .
H13 H 0.4404 -0.4772 0.5357 0.053 Uiso 1 1 calc R . .
C14 C 0.4052(2) -0.2501(4) 0.54072(17) 0.0301(9) Uani 1 1 d . . .
C15 C 0.4181(2) -0.1133(4) 0.58265(15) 0.0249(8) Uani 1 1 d . . .
N16 N 0.34424(19) -0.2358(3) 0.47669(13) 0.0286(7) Uani 1 1 d . . .
C17 C 0.2930(3) -0.3760(4) 0.4492(2) 0.0486(11) Uani 1 1 d . . .
H17A H 0.3326 -0.4534 0.4378 0.073 Uiso 1 1 calc R . .
H17B H 0.245 -0.3474 0.4093 0.073 Uiso 1 1 calc R . .
H17C H 0.2669 -0.4214 0.4819 0.073 Uiso 1 1 calc R . .
C18 C 0.3831(3) -0.1602(5) 0.42965(17) 0.0427(11) Uani 1 1 d . . .
H18A H 0.4125 -0.0619 0.4487 0.064 Uiso 1 1 calc R . .
H18B H 0.3356 -0.137 0.3887 0.064 Uiso 1 1 calc R . .
H18C H 0.4272 -0.2308 0.42 0.064 Uiso 1 1 calc R . .
N20 N 0.13822(17) -0.0749(3) 0.63675(12) 0.0181(6) Uani 1 1 d . . .
C21 C 0.0271(2) 0.2196(4) 0.63373(17) 0.0367(10) Uani 1 1 d . . .
H21A H 0.0402 0.2616 0.5945 0.055 Uiso 1 1 calc R . .
H21B H 0.0205 0.3068 0.6623 0.055 Uiso 1 1 calc R . .
H21C H -0.0287 0.1588 0.6201 0.055 Uiso 1 1 calc R . .
C22 C 0.2221(2) 0.2197(4) 0.70607(18) 0.0379(10) Uani 1 1 d . . .
H22A H 0.2754 0.1592 0.7059 0.057 Uiso 1 1 calc R . .
H22B H 0.2291 0.26 0.7507 0.057 Uiso 1 1 calc R . .
H22C H 0.2146 0.3082 0.6752 0.057 Uiso 1 1 calc R . .
C23 C 0.0919(3) 0.0329(4) 0.75721(16) 0.0371(10) Uani 1 1 d . . .
H23A H 0.0423 -0.0427 0.7461 0.056 Uiso 1 1 calc R . .
H23B H 0.0741 0.1272 0.7769 0.056 Uiso 1 1 calc R . .
H23C H 0.1443 -0.015 0.7889 0.056 Uiso 1 1 calc R . .
C24 C 0.1413(2) -0.3520(4) 0.72668(17) 0.0344(9) Uani 1 1 d . . .
H24A H 0.1181 -0.2862 0.756 0.052 Uiso 1 1 calc R . .
H24B H 0.1819 -0.4316 0.7529 0.052 Uiso 1 1 calc R . .
H24C H 0.0913 -0.4042 0.6943 0.052 Uiso 1 1 calc R . .
C25 C 0.3067(2) -0.1530(4) 0.74593(16) 0.0326(9) Uani 1 1 d . . .
H25A H 0.3436 -0.0936 0.724 0.049 Uiso 1 1 calc R . .
H25B H 0.3409 -0.2428 0.7696 0.049 Uiso 1 1 calc R . .
H25C H 0.2896 -0.0843 0.7774 0.049 Uiso 1 1 calc R . .
C26 C 0.2457(2) -0.3643(4) 0.62916(16) 0.0284(8) Uani 1 1 d . . .
H26A H 0.1952 -0.4234 0.6004 0.043 Uiso 1 1 calc R . .
H26B H 0.2887 -0.4379 0.6573 0.043 Uiso 1 1 calc R . .
H26C H 0.2751 -0.304 0.602 0.043 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 N20 2.147(2) . ?
Sn1 O1 2.165(2) . ?
Sn1 O1 2.282(2) 3_556 ?
Si1 N20 1.732(3) . ?
Si1 C21 1.868(3) . ?
Si1 C23 1.878(3) . ?
Si1 C22 1.878(4) . ?
Si2 N20 1.743(3) . ?
Si2 C24 1.871(3) . ?
Si2 C25 1.873(3) . ?
Si2 C26 1.879(3) . ?
S1 C6 1.780(3) . ?
S1 C5 1.818(3) . ?
O1 C2 1.441(4) . ?
O1 Sn1 2.282(2) 3_556 ?
C2 C3 1.522(4) . ?
C2 C4 1.529(5) . ?
C2 C5 1.540(4) . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 C7 1.374(4) . ?
C6 C15 1.442(5) . ?
C7 C8 1.420(5) . ?
C7 H7 0.95 . ?
C8 C9 1.348(5) . ?
C8 H8 0.95 . ?
C9 C10 1.406(5) . ?
C9 H9 0.95 . ?
C10 C11 1.418(5) . ?
C10 C15 1.438(5) . ?
C11 C12 1.352(6) . ?
C11 H11 0.95 . ?
C12 C13 1.399(5) . ?
C12 H12 0.95 . ?
C13 C14 1.371(5) . ?
C13 H13 0.95 . ?
C14 N16 1.413(4) . ?
C14 C15 1.439(5) . ?
N16 C17 1.457(4) . ?
N16 C18 1.459(4) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?


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
N20 Sn1 O1 102.77(8) . . ?
N20 Sn1 O1 100.25(9) . 3_556 ?
O1 Sn1 O1 71.86(9) . 3_556 ?
N20 Si1 C21 114.85(14) . . ?
N20 Si1 C23 111.85(14) . . ?
C21 Si1 C23 104.76(17) . . ?
N20 Si1 C22 112.27(15) . . ?
C21 Si1 C22 105.41(17) . . ?
C23 Si1 C22 107.06(17) . . ?
N20 Si2 C24 113.16(15) . . ?
N20 Si2 C25 113.22(14) . . ?
C24 Si2 C25 107.19(16) . . ?
N20 Si2 C26 112.20(13) . . ?
C24 Si2 C26 105.53(16) . . ?
C25 Si2 C26 104.88(16) . . ?
C6 S1 C5 103.66(16) . . ?
C2 O1 Sn1 128.27(19) . . ?
C2 O1 Sn1 122.83(18) . 3_556 ?
Sn1 O1 Sn1 108.14(9) . 3_556 ?
O1 C2 C3 109.2(3) . . ?
O1 C2 C4 109.6(3) . . ?
C3 C2 C4 109.6(3) . . ?
O1 C2 C5 109.0(3) . . ?
C3 C2 C5 107.4(3) . . ?
C4 C2 C5 111.9(3) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 S1 109.5(2) . . ?
C2 C5 H5A 109.8 . . ?
S1 C5 H5A 109.8 . . ?
C2 C5 H5B 109.8 . . ?
S1 C5 H5B 109.8 . . ?
H5A C5 H5B 108.2 . . ?
C7 C6 C15 119.7(3) . . ?
C7 C6 S1 120.7(3) . . ?
C15 C6 S1 119.5(3) . . ?
C6 C7 C8 120.8(4) . . ?
C6 C7 H7 119.6 . . ?
C8 C7 H7 119.6 . . ?
C9 C8 C7 120.2(4) . . ?
C9 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
C8 C9 C10 121.5(4) . . ?
C8 C9 H9 119.2 . . ?
C10 C9 H9 119.2 . . ?
C9 C10 C11 122.2(4) . . ?
C9 C10 C15 119.4(4) . . ?
C11 C10 C15 118.5(4) . . ?
C12 C11 C10 121.8(4) . . ?
C12 C11 H11 119.1 . . ?
C10 C11 H11 119.1 . . ?
C11 C12 C13 120.2(4) . . ?
C11 C12 H12 119.9 . . ?
C13 C12 H12 119.9 . . ?
C14 C13 C12 121.0(4) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 N16 122.7(4) . . ?
C13 C14 C15 120.3(3) . . ?
N16 C14 C15 117.0(3) . . ?
C10 C15 C14 117.7(3) . . ?
C10 C15 C6 117.8(3) . . ?
C14 C15 C6 124.5(3) . . ?
C14 N16 C17 116.7(3) . . ?
C14 N16 C18 113.2(3) . . ?
C17 N16 C18 112.1(3) . . ?
N16 C17 H17A 109.5 . . ?
N16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N16 C18 H18A 109.5 . . ?
N16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 N20 Si2 117.02(14) . . ?
Si1 N20 Sn1 131.33(13) . . ?
Si2 N20 Sn1 111.64(12) . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?


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
N20 Sn1 O1 C2 93.1(2) . . . . ?
O1 Sn1 O1 C2 -170.2(3) 3_556 . . . ?
N20 Sn1 O1 Sn1 -96.76(10) . . . 3_556 ?
O1 Sn1 O1 Sn1 0 3_556 . . 3_556 ?
Sn1 O1 C2 C3 -156.0(2) . . . . ?
Sn1 O1 C2 C3 35.1(3) 3_556 . . . ?
Sn1 O1 C2 C4 83.9(3) . . . . ?
Sn1 O1 C2 C4 -85.0(3) 3_556 . . . ?
Sn1 O1 C2 C5 -39.0(4) . . . . ?
Sn1 O1 C2 C5 152.2(2) 3_556 . . . ?
O1 C2 C5 S1 73.5(3) . . . . ?
C3 C2 C5 S1 -168.3(2) . . . . ?
C4 C2 C5 S1 -47.9(3) . . . . ?
C6 S1 C5 C2 -170.0(2) . . . . ?
C5 S1 C6 C7 -7.2(3) . . . . ?
C5 S1 C6 C15 169.5(3) . . . . ?
C15 C6 C7 C8 -3.9(5) . . . . ?
S1 C6 C7 C8 172.8(3) . . . . ?
C6 C7 C8 C9 -2.0(6) . . . . ?
C7 C8 C9 C10 3.4(6) . . . . ?
C8 C9 C10 C11 -177.8(4) . . . . ?
C8 C9 C10 C15 1.1(6) . . . . ?
C9 C10 C11 C12 179.1(4) . . . . ?
C15 C10 C11 C12 0.1(6) . . . . ?
C10 C11 C12 C13 4.3(7) . . . . ?
C11 C12 C13 C14 -2.5(7) . . . . ?
C12 C13 C14 N16 175.4(4) . . . . ?
C12 C13 C14 C15 -3.6(6) . . . . ?
C9 C10 C15 C14 175.1(3) . . . . ?
C11 C10 C15 C14 -6.0(5) . . . . ?
C9 C10 C15 C6 -6.8(5) . . . . ?
C11 C10 C15 C6 172.2(3) . . . . ?
C13 C14 C15 C10 7.7(5) . . . . ?
N16 C14 C15 C10 -171.3(3) . . . . ?
C13 C14 C15 C6 -170.3(3) . . . . ?
N16 C14 C15 C6 10.7(5) . . . . ?
C7 C6 C15 C10 8.1(5) . . . . ?
S1 C6 C15 C10 -168.6(2) . . . . ?
C7 C6 C15 C14 -173.8(3) . . . . ?
S1 C6 C15 C14 9.4(5) . . . . ?
C13 C14 N16 C17 34.7(5) . . . . ?
C15 C14 N16 C17 -146.3(3) . . . . ?
C13 C14 N16 C18 -97.7(4) . . . . ?
C15 C14 N16 C18 81.3(4) . . . . ?
C21 Si1 N20 Si2 -163.99(18) . . . . ?
C23 Si1 N20 Si2 -44.8(2) . . . . ?
C22 Si1 N20 Si2 75.6(2) . . . . ?
C21 Si1 N20 Sn1 16.6(3) . . . . ?
C23 Si1 N20 Sn1 135.9(2) . . . . ?
C22 Si1 N20 Sn1 -103.8(2) . . . . ?
C24 Si2 N20 Si1 78.1(2) . . . . ?
C25 Si2 N20 Si1 -44.2(2) . . . . ?
C26 Si2 N20 Si1 -162.66(17) . . . . ?
C24 Si2 N20 Sn1 -102.45(17) . . . . ?
C25 Si2 N20 Sn1 135.32(16) . . . . ?
C26 Si2 N20 Sn1 16.84(19) . . . . ?
O1 Sn1 N20 Si1 18.0(2) . . . . ?
O1 Sn1 N20 Si1 -55.5(2) 3_556 . . . ?
O1 Sn1 N20 Si2 -161.35(13) . . . . ?
O1 Sn1 N20 Si2 125.12(13) 3_556 . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006886'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_13

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C22 H38 N2 O1 Pb1 S1 Si2'
_chemical_formula_sum            'C22 H38 N2 O Pb S Si2'
_chemical_formula_weight         641.97
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   13.0728(5)
_cell_length_b                   11.7745(4)
_cell_length_c                   17.6806(5)
_cell_angle_alpha                90
_cell_angle_beta                 99.5030(10)
_cell_angle_gamma                90
_cell_volume                     2684.15(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9930
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      27.5
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.43
_exptl_crystal_density_diffrn    1.589
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1272
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    6.468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.029
_exptl_absorpt_correction_T_max  0.062


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_number            22836
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.12
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_reflns_number_total             6080
_reflns_number_gt                5153
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0123P)²+3.4828P] 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_number_reflns         6080
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0233
_refine_ls_wR_factor_ref         0.0515
_refine_ls_wR_factor_gt          0.0493
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_restrained_S_all      1.044
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.002
_refine_diff_density_min         -1.14
_refine_diff_density_rms         0.113

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.574574(9) 0.126486(10) 0.472608(6) 0.01250(4) Uani 1 1 d . . .
N1 N 0.6393(2) 0.2109(2) 0.58507(15) 0.0160(6) Uani 1 1 d . . .
O1 O 0.58932(16) -0.06183(17) 0.50143(12) 0.0136(4) Uani 1 1 d . . .
Si1 Si 0.65503(7) 0.15581(8) 0.67664(5) 0.01705(19) Uani 1 1 d . . .
Si2 Si 0.66864(7) 0.35078(7) 0.57133(5) 0.01672(19) Uani 1 1 d . . .
S1 S 0.78559(6) 0.02838(7) 0.43695(5) 0.01768(17) Uani 1 1 d . . .
C2 C 0.6754(2) -0.1353(3) 0.49926(18) 0.0151(7) Uani 1 1 d . . .
C3 C 0.6632(3) -0.1953(3) 0.4221(2) 0.0231(8) Uani 1 1 d . . .
H3A H 0.5978 -0.2378 0.4137 0.035 Uiso 1 1 calc R . .
H3B H 0.7212 -0.2479 0.4217 0.035 Uiso 1 1 calc R . .
H3C H 0.6626 -0.139 0.3812 0.035 Uiso 1 1 calc R . .
C4 C 0.6802(3) -0.2246(3) 0.5630(2) 0.0254(8) Uani 1 1 d . . .
H4A H 0.6836 -0.1864 0.6126 0.038 Uiso 1 1 calc R . .
H4B H 0.742 -0.272 0.5638 0.038 Uiso 1 1 calc R . .
H4C H 0.6181 -0.2724 0.5534 0.038 Uiso 1 1 calc R . .
C5 C 0.7767(2) -0.0665(3) 0.51674(18) 0.0163(7) Uani 1 1 d . . .
H5A H 0.8369 -0.1187 0.5246 0.02 Uiso 1 1 calc R . .
H5B H 0.7776 -0.0218 0.5643 0.02 Uiso 1 1 calc R . .
C6 C 0.8879(2) 0.1228(3) 0.47452(19) 0.0173(7) Uani 1 1 d . . .
C7 C 0.9436(3) 0.1054(3) 0.5468(2) 0.0212(7) Uani 1 1 d . . .
H7 H 0.9302 0.0395 0.5746 0.025 Uiso 1 1 calc R . .
C8 C 1.0200(3) 0.1830(3) 0.5807(2) 0.0247(8) Uani 1 1 d . . .
H8 H 1.058 0.1684 0.6304 0.03 Uiso 1 1 calc R . .
C9 C 1.0392(3) 0.2783(3) 0.5424(2) 0.0244(8) Uani 1 1 d . . .
H9 H 1.0887 0.3318 0.5662 0.029 Uiso 1 1 calc R . .
C10 C 0.9865(3) 0.2985(3) 0.4676(2) 0.0210(7) Uani 1 1 d . . .
C11 C 1.0054(3) 0.4003(3) 0.4289(2) 0.0303(9) Uani 1 1 d . . .
H11 H 1.0558 0.4525 0.4531 0.036 Uiso 1 1 calc R . .
C12 C 0.9530(3) 0.4240(3) 0.3582(2) 0.0324(10) Uani 1 1 d . . .
H12 H 0.9642 0.4941 0.3342 0.039 Uiso 1 1 calc R . .
C13 C 0.8816(3) 0.3446(3) 0.3201(2) 0.0296(9) Uani 1 1 d . . .
H13 H 0.8466 0.3612 0.2699 0.036 Uiso 1 1 calc R . .
C14 C 0.8617(3) 0.2444(3) 0.3538(2) 0.0211(7) Uani 1 1 d . . .
C15 C 0.9110(3) 0.2191(3) 0.43076(19) 0.0173(7) Uani 1 1 d . . .
N16 N 0.7943(2) 0.1616(3) 0.31481(17) 0.0259(7) Uani 1 1 d . . .
C17 C 0.8469(4) 0.0801(3) 0.2726(2) 0.0381(10) Uani 1 1 d . . .
H17A H 0.8637 0.1163 0.2263 0.057 Uiso 1 1 calc R . .
H17B H 0.8014 0.0148 0.2582 0.057 Uiso 1 1 calc R . .
H17C H 0.9109 0.0546 0.305 0.057 Uiso 1 1 calc R . .
C18 C 0.6993(3) 0.2045(4) 0.2691(2) 0.0452(11) Uani 1 1 d . . .
H18A H 0.6688 0.2626 0.2982 0.068 Uiso 1 1 calc R . .
H18B H 0.65 0.1419 0.2566 0.068 Uiso 1 1 calc R . .
H18C H 0.7152 0.2378 0.2215 0.068 Uiso 1 1 calc R . .
C21 C 0.5734(3) 0.0271(3) 0.68171(19) 0.0217(8) Uani 1 1 d . . .
H21A H 0.5004 0.0462 0.6641 0.033 Uiso 1 1 calc R . .
H21B H 0.5823 0 0.7348 0.033 Uiso 1 1 calc R . .
H21C H 0.5947 -0.0325 0.6489 0.033 Uiso 1 1 calc R . .
C22 C 0.7925(3) 0.1142(3) 0.7150(2) 0.0293(8) Uani 1 1 d . . .
H22A H 0.8105 0.0457 0.6886 0.044 Uiso 1 1 calc R . .
H22B H 0.7995 0.099 0.7701 0.044 Uiso 1 1 calc R . .
H22C H 0.8393 0.1761 0.7063 0.044 Uiso 1 1 calc R . .
C23 C 0.6167(3) 0.2580(3) 0.74845(19) 0.0258(8) Uani 1 1 d . . .
H23A H 0.6615 0.3252 0.7517 0.039 Uiso 1 1 calc R . .
H23B H 0.6242 0.2213 0.7988 0.039 Uiso 1 1 calc R . .
H23C H 0.5443 0.281 0.7324 0.039 Uiso 1 1 calc R . .
C24 C 0.5672(3) 0.4495(3) 0.5962(2) 0.0252(8) Uani 1 1 d . . .
H24A H 0.4992 0.4276 0.5678 0.038 Uiso 1 1 calc R . .
H24B H 0.5833 0.5274 0.5826 0.038 Uiso 1 1 calc R . .
H24C H 0.5658 0.4453 0.6514 0.038 Uiso 1 1 calc R . .
C25 C 0.7963(3) 0.3948(3) 0.6278(2) 0.0292(9) Uani 1 1 d . . .
H25A H 0.7968 0.3791 0.6823 0.044 Uiso 1 1 calc R . .
H25B H 0.8068 0.4762 0.6206 0.044 Uiso 1 1 calc R . .
H25C H 0.8522 0.3521 0.6101 0.044 Uiso 1 1 calc R . .
C26 C 0.6784(3) 0.3824(3) 0.4685(2) 0.0262(8) Uani 1 1 d . . .
H26A H 0.7287 0.3308 0.4513 0.039 Uiso 1 1 calc R . .
H26B H 0.7012 0.4611 0.4642 0.039 Uiso 1 1 calc R . .
H26C H 0.6104 0.3718 0.4365 0.039 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.259(3) . ?
Pb1 O1 2.276(2) . ?
Pb1 O1 2.389(2) 3_656 ?
N1 Si2 1.718(3) . ?
N1 Si1 1.724(3) . ?
O1 C2 1.425(4) . ?
O1 Pb1 2.389(2) 3_656 ?
Si1 C21 1.864(3) . ?
Si1 C23 1.877(3) . ?
Si1 C22 1.879(4) . ?
Si2 C24 1.871(4) . ?
Si2 C25 1.871(4) . ?
Si2 C26 1.880(3) . ?
S1 C6 1.781(3) . ?
S1 C5 1.818(3) . ?
C2 C3 1.521(4) . ?
C2 C4 1.535(4) . ?
C2 C5 1.540(4) . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C6 C7 1.378(5) . ?
C6 C15 1.433(4) . ?
C7 C8 1.412(5) . ?
C7 H7 0.95 . ?
C8 C9 1.355(5) . ?
C8 H8 0.95 . ?
C9 C10 1.406(5) . ?
C9 H9 0.95 . ?
C10 C11 1.422(5) . ?
C10 C15 1.435(5) . ?
C11 C12 1.351(6) . ?
C11 H11 0.95 . ?
C12 C13 1.411(6) . ?
C12 H12 0.95 . ?
C13 C14 1.366(5) . ?
C13 H13 0.95 . ?
C14 N16 1.416(5) . ?
C14 C15 1.437(5) . ?
N16 C18 1.455(5) . ?
N16 C17 1.456(5) . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?


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 O1 103.05(9) . . ?
N1 Pb1 O1 100.88(8) . 3_656 ?
O1 Pb1 O1 72.06(8) . 3_656 ?
Si2 N1 Si1 119.91(15) . . ?
Si2 N1 Pb1 110.93(13) . . ?
Si1 N1 Pb1 129.08(14) . . ?
C2 O1 Pb1 128.57(17) . . ?
C2 O1 Pb1 123.31(17) . 3_656 ?
Pb1 O1 Pb1 107.94(8) . 3_656 ?
N1 Si1 C21 111.74(14) . . ?
N1 Si1 C23 112.99(15) . . ?
C21 Si1 C23 105.66(16) . . ?
N1 Si1 C22 113.31(15) . . ?
C21 Si1 C22 106.95(17) . . ?
C23 Si1 C22 105.63(17) . . ?
N1 Si2 C24 112.30(15) . . ?
N1 Si2 C25 112.97(16) . . ?
C24 Si2 C25 107.87(17) . . ?
N1 Si2 C26 112.27(14) . . ?
C24 Si2 C26 105.57(17) . . ?
C25 Si2 C26 105.32(18) . . ?
C6 S1 C5 103.54(15) . . ?
O1 C2 C3 109.8(3) . . ?
O1 C2 C4 109.4(2) . . ?
C3 C2 C4 109.0(3) . . ?
O1 C2 C5 109.4(2) . . ?
C3 C2 C5 112.6(3) . . ?
C4 C2 C5 106.5(3) . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 S1 109.3(2) . . ?
C2 C5 H5A 109.8 . . ?
S1 C5 H5A 109.8 . . ?
C2 C5 H5B 109.8 . . ?
S1 C5 H5B 109.8 . . ?
H5A C5 H5B 108.3 . . ?
C7 C6 C15 119.5(3) . . ?
C7 C6 S1 120.2(3) . . ?
C15 C6 S1 120.3(3) . . ?
C6 C7 C8 121.8(3) . . ?
C6 C7 H7 119.1 . . ?
C8 C7 H7 119.1 . . ?
C9 C8 C7 120.0(4) . . ?
C9 C8 H8 120 . . ?
C7 C8 H8 120 . . ?
C8 C9 C10 120.5(3) . . ?
C8 C9 H9 119.8 . . ?
C10 C9 H9 119.8 . . ?
C9 C10 C11 119.9(3) . . ?
C9 C10 C15 120.7(3) . . ?
C11 C10 C15 119.4(3) . . ?
C12 C11 C10 121.2(4) . . ?
C12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 C12 C13 119.9(3) . . ?
C11 C12 H12 120 . . ?
C13 C12 H12 120 . . ?
C14 C13 C12 121.5(4) . . ?
C14 C13 H13 119.3 . . ?
C12 C13 H13 119.3 . . ?
C13 C14 N16 122.1(3) . . ?
C13 C14 C15 120.3(3) . . ?
N16 C14 C15 117.7(3) . . ?
C6 C15 C10 117.4(3) . . ?
C6 C15 C14 125.0(3) . . ?
C10 C15 C14 117.6(3) . . ?
C14 N16 C18 115.9(3) . . ?
C14 N16 C17 113.2(3) . . ?
C18 N16 C17 112.0(3) . . ?
N16 C17 H17A 109.5 . . ?
N16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N16 C18 H18A 109.5 . . ?
N16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?


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
O1 Pb1 N1 Si2 163.56(12) . . . . ?
O1 Pb1 N1 Si2 -122.55(13) 3_656 . . . ?
O1 Pb1 N1 Si1 -19.9(2) . . . . ?
O1 Pb1 N1 Si1 54.03(19) 3_656 . . . ?
N1 Pb1 O1 C2 -87.5(2) . . . . ?
O1 Pb1 O1 C2 175.1(3) 3_656 . . . ?
N1 Pb1 O1 Pb1 97.39(10) . . . 3_656 ?
O1 Pb1 O1 Pb1 0 3_656 . . 3_656 ?
Si2 N1 Si1 C21 157.64(18) . . . . ?
Pb1 N1 Si1 C21 -18.7(2) . . . . ?
Si2 N1 Si1 C23 38.6(2) . . . . ?
Pb1 N1 Si1 C23 -137.68(19) . . . . ?
Si2 N1 Si1 C22 -81.5(2) . . . . ?
Pb1 N1 Si1 C22 102.2(2) . . . . ?
Si1 N1 Si2 C24 -75.7(2) . . . . ?
Pb1 N1 Si2 C24 101.20(17) . . . . ?
Si1 N1 Si2 C25 46.6(2) . . . . ?
Pb1 N1 Si2 C25 -136.50(16) . . . . ?
Si1 N1 Si2 C26 165.48(19) . . . . ?
Pb1 N1 Si2 C26 -17.6(2) . . . . ?
Pb1 O1 C2 C3 -93.7(3) . . . . ?
Pb1 O1 C2 C3 80.7(3) 3_656 . . . ?
Pb1 O1 C2 C4 146.6(2) . . . . ?
Pb1 O1 C2 C4 -39.0(3) 3_656 . . . ?
Pb1 O1 C2 C5 30.4(3) . . . . ?
Pb1 O1 C2 C5 -155.25(18) 3_656 . . . ?
O1 C2 C5 S1 -69.6(3) . . . . ?
C3 C2 C5 S1 52.8(3) . . . . ?
C4 C2 C5 S1 172.2(2) . . . . ?
C6 S1 C5 C2 167.0(2) . . . . ?
C5 S1 C6 C7 5.1(3) . . . . ?
C5 S1 C6 C15 -173.1(2) . . . . ?
C15 C6 C7 C8 3.0(5) . . . . ?
S1 C6 C7 C8 -175.2(3) . . . . ?
C6 C7 C8 C9 0.9(5) . . . . ?
C7 C8 C9 C10 -2.6(5) . . . . ?
C8 C9 C10 C11 178.3(3) . . . . ?
C8 C9 C10 C15 0.4(5) . . . . ?
C9 C10 C11 C12 -177.4(3) . . . . ?
C15 C10 C11 C12 0.5(5) . . . . ?
C10 C11 C12 C13 -3.0(6) . . . . ?
C11 C12 C13 C14 1.7(6) . . . . ?
C12 C13 C14 N16 -176.7(3) . . . . ?
C12 C13 C14 C15 2.2(5) . . . . ?
C7 C6 C15 C10 -4.9(4) . . . . ?
S1 C6 C15 C10 173.3(2) . . . . ?
C7 C6 C15 C14 177.4(3) . . . . ?
S1 C6 C15 C14 -4.4(4) . . . . ?
C9 C10 C15 C6 3.3(4) . . . . ?
C11 C10 C15 C6 -174.6(3) . . . . ?
C9 C10 C15 C14 -178.9(3) . . . . ?
C11 C10 C15 C14 3.2(4) . . . . ?
C13 C14 C15 C6 173.1(3) . . . . ?
N16 C14 C15 C6 -7.9(5) . . . . ?
C13 C14 C15 C10 -4.5(5) . . . . ?
N16 C14 C15 C10 174.4(3) . . . . ?
C13 C14 N16 C18 -41.8(5) . . . . ?
C15 C14 N16 C18 139.2(3) . . . . ?
C13 C14 N16 C17 89.7(4) . . . . ?
C15 C14 N16 C17 -89.2(4) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006887'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_14

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C26 H28 F12 N2 O2 Se2 Sn'
_chemical_formula_sum            'C26 H28 F12 N2 O2 Se2 Sn'
_chemical_formula_weight         905.11
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.9934(2)
_cell_length_b                   11.6181(2)
_cell_length_c                   15.2377(3)
_cell_angle_alpha                72.2840(6)
_cell_angle_beta                 82.4962(7)
_cell_angle_gamma                67.4339(7)
_cell_volume                     1556.04(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9883
_cell_measurement_theta_min      2.6
_cell_measurement_theta_max      27.48
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.932
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             880
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.261
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_T_max  0.770


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0303
_diffrn_reflns_number            23659
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_reflns_number_total             7026
_reflns_number_gt                6195
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0175P)²+0.5688P] 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_number_reflns         7026
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0212
_refine_ls_wR_factor_ref         0.0477
_refine_ls_wR_factor_gt          0.0455
_refine_ls_goodness_of_fit_ref   1.02
_refine_ls_restrained_S_all      1.02
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.46
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.068

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.145998(14) 0.162596(12) 0.823947(8) 0.01933(4) Uani 1 1 d . . .
O1 O 0.08629(15) 0.36194(13) 0.80065(11) 0.0298(3) Uani 1 1 d . . .
C2 C -0.0388(2) 0.46374(19) 0.76942(14) 0.0219(4) Uani 1 1 d . . .
C3 C 0.0045(2) 0.5758(2) 0.70638(16) 0.0316(5) Uani 1 1 d . . .
F4 F 0.07898(17) 0.54211(15) 0.63285(10) 0.0501(4) Uani 1 1 d . . .
F5 F 0.08958(15) 0.60750(13) 0.74788(10) 0.0455(4) Uani 1 1 d . . .
F6 F -0.10896(15) 0.68370(12) 0.67490(10) 0.0462(4) Uani 1 1 d . . .
C7 C -0.1264(2) 0.5042(2) 0.85283(16) 0.0332(5) Uani 1 1 d . . .
F8 F -0.05566(16) 0.53817(15) 0.90209(10) 0.0520(4) Uani 1 1 d . . .
F9 F -0.25173(15) 0.60443(15) 0.82951(11) 0.0531(4) Uani 1 1 d . . .
F10 F -0.16085(18) 0.40608(15) 0.91008(9) 0.0526(4) Uani 1 1 d . . .
C11 C -0.1322(2) 0.43624(19) 0.71047(14) 0.0235(4) Uani 1 1 d . . .
H11A H -0.084 0.4319 0.6499 0.028 Uiso 1 1 calc R . .
H11B H -0.2278 0.5079 0.6997 0.028 Uiso 1 1 calc R . .
C70 C 0.5856(2) 0.2097(2) 0.99955(16) 0.0351(5) Uani 1 1 d . . .
H70A H 0.6275 0.2621 0.9493 0.053 Uiso 1 1 calc R . .
H70B H 0.6552 0.1203 1.0179 0.053 Uiso 1 1 calc R . .
H70C H 0.5632 0.246 1.0523 0.053 Uiso 1 1 calc R . .
Se1 Se -0.15900(2) 0.27322(2) 0.772755(13) 0.02224(5) Uani 1 1 d . . .
C21 C -0.1635(2) 0.21279(19) 0.66904(13) 0.0207(4) Uani 1 1 d . . .
C22 C -0.1867(2) 0.2941(2) 0.57976(14) 0.0265(5) Uani 1 1 d . . .
H22 H -0.1959 0.382 0.5675 0.032 Uiso 1 1 calc R . .
C23 C -0.1965(2) 0.2465(2) 0.50864(14) 0.0306(5) Uani 1 1 d . . .
H23 H -0.2126 0.3021 0.4476 0.037 Uiso 1 1 calc R . .
C24 C -0.1831(2) 0.1192(2) 0.52617(15) 0.0331(5) Uani 1 1 d . . .
H24 H -0.189 0.0865 0.4773 0.04 Uiso 1 1 calc R . .
C25 C -0.1610(2) 0.0392(2) 0.61528(15) 0.0305(5) Uani 1 1 d . . .
H25 H -0.1518 -0.0486 0.6269 0.037 Uiso 1 1 calc R . .
C26 C -0.1519(2) 0.0840(2) 0.68836(14) 0.0232(4) Uani 1 1 d . . .
C27 C -0.1343(2) -0.0042(2) 0.78557(14) 0.0260(4) Uani 1 1 d . . .
H27A H -0.212 0.0387 0.8252 0.031 Uiso 1 1 calc R . .
H27B H -0.146 -0.0852 0.7859 0.031 Uiso 1 1 calc R . .
N28 N 0.00690(18) -0.03716(16) 0.82456(12) 0.0244(4) Uani 1 1 d . . .
C29 C 0.0058(3) -0.1058(3) 0.92211(16) 0.0432(6) Uani 1 1 d . . .
H29A H -0.0119 -0.1855 0.929 0.065 Uiso 1 1 calc R . .
H29B H -0.071 -0.0502 0.9542 0.065 Uiso 1 1 calc R . .
H29C H 0.0997 -0.1279 0.9486 0.065 Uiso 1 1 calc R . .
C30 C 0.1236(2) -0.1169(2) 0.77625(18) 0.0364(6) Uani 1 1 d . . .
H30A H 0.1093 -0.1979 0.7826 0.055 Uiso 1 1 calc R . .
H30B H 0.2167 -0.1366 0.8028 0.055 Uiso 1 1 calc R . .
H30C H 0.1233 -0.0698 0.7108 0.055 Uiso 1 1 calc R . .
O41 O 0.18815(14) 0.16468(15) 0.68814(9) 0.0264(3) Uani 1 1 d . . .
C42 C 0.3082(2) 0.16476(19) 0.63210(13) 0.0206(4) Uani 1 1 d . . .
C43 C 0.2504(2) 0.2228(2) 0.53291(14) 0.0270(5) Uani 1 1 d . . .
F44 F 0.15958(15) 0.34570(13) 0.52034(9) 0.0414(3) Uani 1 1 d . . .
F45 F 0.17909(14) 0.15899(13) 0.51243(8) 0.0349(3) Uani 1 1 d . . .
F46 F 0.35683(15) 0.22510(14) 0.46919(8) 0.0407(3) Uani 1 1 d . . .
C47 C 0.4158(2) 0.0245(2) 0.64465(14) 0.0256(4) Uani 1 1 d . . .
F48 F 0.36265(13) -0.05138(12) 0.62130(9) 0.0331(3) Uani 1 1 d . . .
F49 F 0.53832(13) 0.01723(13) 0.59619(10) 0.0404(3) Uani 1 1 d . . .
F50 F 0.45179(15) -0.03161(12) 0.73383(9) 0.0385(3) Uani 1 1 d . . .
C51 C 0.3861(2) 0.2492(2) 0.64609(13) 0.0236(4) Uani 1 1 d . . .
H51A H 0.3215 0.3415 0.6264 0.028 Uiso 1 1 calc R . .
H51B H 0.474 0.2383 0.6061 0.028 Uiso 1 1 calc R . .
Se2 Se 0.442650(19) 0.206361(18) 0.774643(13) 0.01837(5) Uani 1 1 d . . .
C61 C 0.4341(2) 0.37709(19) 0.76899(13) 0.0194(4) Uani 1 1 d . . .
C62 C 0.4716(2) 0.4537(2) 0.68751(14) 0.0251(4) Uani 1 1 d . . .
H62 H 0.4963 0.4237 0.634 0.03 Uiso 1 1 calc R . .
C63 C 0.4731(2) 0.5742(2) 0.68415(16) 0.0305(5) Uani 1 1 d . . .
H63 H 0.4959 0.6274 0.6279 0.037 Uiso 1 1 calc R . .
C64 C 0.4417(2) 0.6161(2) 0.76220(17) 0.0333(5) Uani 1 1 d . . .
H64 H 0.4453 0.6973 0.7605 0.04 Uiso 1 1 calc R . .
C65 C 0.4047(2) 0.5397(2) 0.84329(16) 0.0299(5) Uani 1 1 d . . .
H65 H 0.3829 0.5695 0.8969 0.036 Uiso 1 1 calc R . .
C66 C 0.3985(2) 0.42002(19) 0.84815(14) 0.0216(4) Uani 1 1 d . . .
C67 C 0.3493(2) 0.34340(19) 0.93585(13) 0.0234(4) Uani 1 1 d . . .
H67A H 0.3343 0.3882 0.9842 0.028 Uiso 1 1 calc R . .
H67B H 0.255 0.3404 0.9255 0.028 Uiso 1 1 calc R . .
N68 N 0.45293(18) 0.21083(16) 0.96849(11) 0.0225(4) Uani 1 1 d . . .
C69 C 0.3881(3) 0.1347(2) 1.04335(14) 0.0327(5) Uani 1 1 d . . .
H69A H 0.3603 0.1747 1.0943 0.049 Uiso 1 1 calc R . .
H69B H 0.4585 0.0461 1.0649 0.049 Uiso 1 1 calc R . .
H69C H 0.3019 0.1321 1.021 0.049 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O41 2.0519(13) . ?
Sn1 O1 2.0833(14) . ?
Sn1 Se1 2.9248(2) . ?
O1 C2 1.366(2) . ?
C2 C7 1.536(3) . ?
C2 C3 1.539(3) . ?
C2 C11 1.550(2) . ?
C3 F6 1.331(2) . ?
C3 F5 1.334(2) . ?
C3 F4 1.337(3) . ?
C7 F8 1.324(2) . ?
C7 F9 1.340(3) . ?
C7 F10 1.340(3) . ?
C11 Se1 1.946(2) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C70 N68 1.460(3) . ?
C70 H70A 0.98 . ?
C70 H70B 0.98 . ?
C70 H70C 0.98 . ?
Se1 C21 1.9264(19) . ?
C21 C22 1.389(3) . ?
C21 C26 1.395(3) . ?
C22 C23 1.387(3) . ?
C22 H22 0.95 . ?
C23 C24 1.377(3) . ?
C23 H23 0.95 . ?
C24 C25 1.381(3) . ?
C24 H24 0.95 . ?
C25 C26 1.391(3) . ?
C25 H25 0.95 . ?
C26 C27 1.511(3) . ?
C27 N28 1.469(2) . ?
C27 H27A 0.99 . ?
C27 H27B 0.99 . ?
N28 C30 1.456(3) . ?
N28 C29 1.458(3) . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C30 H30A 0.98 . ?
C30 H30B 0.98 . ?
C30 H30C 0.98 . ?
O41 C42 1.379(2) . ?
C42 C47 1.538(3) . ?
C42 C51 1.540(3) . ?
C42 C43 1.543(3) . ?
C43 F45 1.326(2) . ?
C43 F44 1.335(2) . ?
C43 F46 1.346(2) . ?
C47 F49 1.332(2) . ?
C47 F48 1.337(2) . ?
C47 F50 1.345(2) . ?
C51 Se2 1.9708(19) . ?
C51 H51A 0.99 . ?
C51 H51B 0.99 . ?
Se2 C61 1.9280(19) . ?
C61 C62 1.392(3) . ?
C61 C66 1.396(3) . ?
C62 C63 1.390(3) . ?
C62 H62 0.95 . ?
C63 C64 1.374(3) . ?
C63 H63 0.95 . ?
C64 C65 1.385(3) . ?
C64 H64 0.95 . ?
C65 C66 1.394(3) . ?
C65 H65 0.95 . ?
C66 C67 1.504(3) . ?
C67 N68 1.462(3) . ?
C67 H67A 0.99 . ?
C67 H67B 0.99 . ?
N68 C69 1.462(3) . ?
C69 H69A 0.98 . ?
C69 H69B 0.98 . ?
C69 H69C 0.98 . ?


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
O41 Sn1 O1 95.52(6) . . ?
O41 Sn1 Se1 85.16(4) . . ?
O1 Sn1 Se1 74.95(4) . . ?
C2 O1 Sn1 132.00(11) . . ?
O1 C2 C7 108.30(17) . . ?
O1 C2 C3 107.26(16) . . ?
C7 C2 C3 109.77(17) . . ?
O1 C2 C11 114.37(16) . . ?
C7 C2 C11 110.63(16) . . ?
C3 C2 C11 106.39(16) . . ?
F6 C3 F5 106.92(17) . . ?
F6 C3 F4 106.97(19) . . ?
F5 C3 F4 106.50(18) . . ?
F6 C3 C2 113.05(18) . . ?
F5 C3 C2 112.87(18) . . ?
F4 C3 C2 110.15(17) . . ?
F8 C7 F9 106.32(18) . . ?
F8 C7 F10 106.67(19) . . ?
F9 C7 F10 106.38(19) . . ?
F8 C7 C2 113.37(19) . . ?
F9 C7 C2 113.09(18) . . ?
F10 C7 C2 110.54(18) . . ?
C2 C11 Se1 110.46(13) . . ?
C2 C11 H11A 109.6 . . ?
Se1 C11 H11A 109.6 . . ?
C2 C11 H11B 109.6 . . ?
Se1 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N68 C70 H70A 109.5 . . ?
N68 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
N68 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
C21 Se1 C11 100.83(8) . . ?
C21 Se1 Sn1 104.90(6) . . ?
C11 Se1 Sn1 88.04(6) . . ?
C22 C21 C26 120.78(18) . . ?
C22 C21 Se1 122.44(15) . . ?
C26 C21 Se1 116.65(14) . . ?
C23 C22 C21 119.7(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C24 C23 C22 120.3(2) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.6(2) . . ?
C23 C24 H24 120.2 . . ?
C25 C24 H24 120.2 . . ?
C24 C25 C26 121.7(2) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C25 C26 C21 117.94(19) . . ?
C25 C26 C27 120.35(19) . . ?
C21 C26 C27 121.69(18) . . ?
N28 C27 C26 113.04(16) . . ?
N28 C27 H27A 109 . . ?
C26 C27 H27A 109 . . ?
N28 C27 H27B 109 . . ?
C26 C27 H27B 109 . . ?
H27A C27 H27B 107.8 . . ?
C30 N28 C29 110.20(19) . . ?
C30 N28 C27 110.89(17) . . ?
C29 N28 C27 109.05(16) . . ?
N28 C29 H29A 109.5 . . ?
N28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N28 C30 H30A 109.5 . . ?
N28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C42 O41 Sn1 132.34(11) . . ?
O41 C42 C47 109.53(16) . . ?
O41 C42 C51 114.98(16) . . ?
C47 C42 C51 109.79(16) . . ?
O41 C42 C43 105.26(15) . . ?
C47 C42 C43 109.88(16) . . ?
C51 C42 C43 107.22(16) . . ?
F45 C43 F44 107.13(17) . . ?
F45 C43 F46 106.97(16) . . ?
F44 C43 F46 106.24(17) . . ?
F45 C43 C42 113.15(17) . . ?
F44 C43 C42 110.53(16) . . ?
F46 C43 C42 112.43(17) . . ?
F49 C47 F48 106.58(16) . . ?
F49 C47 F50 107.28(16) . . ?
F48 C47 F50 105.91(16) . . ?
F49 C47 C42 113.02(17) . . ?
F48 C47 C42 113.73(16) . . ?
F50 C47 C42 109.87(16) . . ?
C42 C51 Se2 113.29(13) . . ?
C42 C51 H51A 108.9 . . ?
Se2 C51 H51A 108.9 . . ?
C42 C51 H51B 108.9 . . ?
Se2 C51 H51B 108.9 . . ?
H51A C51 H51B 107.7 . . ?
C61 Se2 C51 96.17(8) . . ?
C62 C61 C66 120.35(18) . . ?
C62 C61 Se2 119.83(15) . . ?
C66 C61 Se2 119.72(15) . . ?
C63 C62 C61 120.2(2) . . ?
C63 C62 H62 119.9 . . ?
C61 C62 H62 119.9 . . ?
C64 C63 C62 119.9(2) . . ?
C64 C63 H63 120 . . ?
C62 C63 H63 120 . . ?
C63 C64 C65 119.8(2) . . ?
C63 C64 H64 120.1 . . ?
C65 C64 H64 120.1 . . ?
C64 C65 C66 121.6(2) . . ?
C64 C65 H65 119.2 . . ?
C66 C65 H65 119.2 . . ?
C65 C66 C61 118.09(19) . . ?
C65 C66 C67 120.04(18) . . ?
C61 C66 C67 121.84(17) . . ?
N68 C67 C66 112.78(16) . . ?
N68 C67 H67A 109 . . ?
C66 C67 H67A 109 . . ?
N68 C67 H67B 109 . . ?
C66 C67 H67B 109 . . ?
H67A C67 H67B 107.8 . . ?
C70 N68 C67 111.05(16) . . ?
C70 N68 C69 110.00(16) . . ?
C67 N68 C69 110.08(16) . . ?
N68 C69 H69A 109.5 . . ?
N68 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
N68 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?


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
O41 Sn1 O1 C2 78.59(18) . . . . ?
Se1 Sn1 O1 C2 -4.88(17) . . . . ?
Sn1 O1 C2 C7 99.89(18) . . . . ?
Sn1 O1 C2 C3 -141.70(15) . . . . ?
Sn1 O1 C2 C11 -24.0(3) . . . . ?
O1 C2 C3 F6 -176.91(17) . . . . ?
C7 C2 C3 F6 -59.4(2) . . . . ?
C11 C2 C3 F6 60.3(2) . . . . ?
O1 C2 C3 F5 -55.4(2) . . . . ?
C7 C2 C3 F5 62.1(2) . . . . ?
C11 C2 C3 F5 -178.21(17) . . . . ?
O1 C2 C3 F4 63.5(2) . . . . ?
C7 C2 C3 F4 -179.05(17) . . . . ?
C11 C2 C3 F4 -59.3(2) . . . . ?
O1 C2 C7 F8 58.6(2) . . . . ?
C3 C2 C7 F8 -58.2(2) . . . . ?
C11 C2 C7 F8 -175.32(18) . . . . ?
O1 C2 C7 F9 179.73(17) . . . . ?
C3 C2 C7 F9 62.9(2) . . . . ?
C11 C2 C7 F9 -54.2(2) . . . . ?
O1 C2 C7 F10 -61.1(2) . . . . ?
C3 C2 C7 F10 -177.92(17) . . . . ?
C11 C2 C7 F10 65.0(2) . . . . ?
O1 C2 C11 Se1 49.4(2) . . . . ?
C7 C2 C11 Se1 -73.21(18) . . . . ?
C3 C2 C11 Se1 167.62(14) . . . . ?
C2 C11 Se1 C21 -146.46(14) . . . . ?
C2 C11 Se1 Sn1 -41.65(13) . . . . ?
O41 Sn1 Se1 C21 27.03(7) . . . . ?
O1 Sn1 Se1 C21 124.07(8) . . . . ?
O41 Sn1 Se1 C11 -73.66(7) . . . . ?
O1 Sn1 Se1 C11 23.39(8) . . . . ?
C11 Se1 C21 C22 -16.92(18) . . . . ?
Sn1 Se1 C21 C22 -107.78(16) . . . . ?
C11 Se1 C21 C26 167.25(15) . . . . ?
Sn1 Se1 C21 C26 76.39(15) . . . . ?
C26 C21 C22 C23 -0.9(3) . . . . ?
Se1 C21 C22 C23 -176.56(15) . . . . ?
C21 C22 C23 C24 -0.1(3) . . . . ?
C22 C23 C24 C25 0.5(3) . . . . ?
C23 C24 C25 C26 0.0(3) . . . . ?
C24 C25 C26 C21 -1.0(3) . . . . ?
C24 C25 C26 C27 177.28(19) . . . . ?
C22 C21 C26 C25 1.4(3) . . . . ?
Se1 C21 C26 C25 177.33(15) . . . . ?
C22 C21 C26 C27 -176.82(18) . . . . ?
Se1 C21 C26 C27 -0.9(2) . . . . ?
C25 C26 C27 N28 112.9(2) . . . . ?
C21 C26 C27 N28 -68.9(2) . . . . ?
C26 C27 N28 C30 -66.9(2) . . . . ?
C26 C27 N28 C29 171.61(19) . . . . ?
O1 Sn1 O41 C42 83.19(17) . . . . ?
Se1 Sn1 O41 C42 157.53(17) . . . . ?
Sn1 O41 C42 C47 84.81(19) . . . . ?
Sn1 O41 C42 C51 -39.4(2) . . . . ?
Sn1 O41 C42 C43 -157.10(13) . . . . ?
O41 C42 C43 F45 -56.4(2) . . . . ?
C47 C42 C43 F45 61.4(2) . . . . ?
C51 C42 C43 F45 -179.31(17) . . . . ?
O41 C42 C43 F44 63.7(2) . . . . ?
C47 C42 C43 F44 -178.44(16) . . . . ?
C51 C42 C43 F44 -59.2(2) . . . . ?
O41 C42 C43 F46 -177.75(16) . . . . ?
C47 C42 C43 F46 -59.9(2) . . . . ?
C51 C42 C43 F46 59.4(2) . . . . ?
O41 C42 C47 F49 -176.69(15) . . . . ?
C51 C42 C47 F49 -49.5(2) . . . . ?
C43 C42 C47 F49 68.1(2) . . . . ?
O41 C42 C47 F48 61.6(2) . . . . ?
C51 C42 C47 F48 -171.25(16) . . . . ?
C43 C42 C47 F48 -53.6(2) . . . . ?
O41 C42 C47 F50 -56.90(19) . . . . ?
C51 C42 C47 F50 70.2(2) . . . . ?
C43 C42 C47 F50 -172.07(15) . . . . ?
O41 C42 C51 Se2 54.8(2) . . . . ?
C47 C42 C51 Se2 -69.22(18) . . . . ?
C43 C42 C51 Se2 171.45(13) . . . . ?
C42 C51 Se2 C61 -151.73(15) . . . . ?
C51 Se2 C61 C62 -33.81(16) . . . . ?
C51 Se2 C61 C66 149.92(15) . . . . ?
C66 C61 C62 C63 -0.4(3) . . . . ?
Se2 C61 C62 C63 -176.62(14) . . . . ?
C61 C62 C63 C64 1.9(3) . . . . ?
C62 C63 C64 C65 -1.8(3) . . . . ?
C63 C64 C65 C66 0.1(3) . . . . ?
C64 C65 C66 C61 1.4(3) . . . . ?
C64 C65 C66 C67 -176.35(19) . . . . ?
C62 C61 C66 C65 -1.3(3) . . . . ?
Se2 C61 C66 C65 174.97(14) . . . . ?
C62 C61 C66 C67 176.47(17) . . . . ?
Se2 C61 C66 C67 -7.3(2) . . . . ?
C65 C66 C67 N68 -126.35(19) . . . . ?
C61 C66 C67 N68 55.9(2) . . . . ?
C66 C67 N68 C70 68.4(2) . . . . ?
C66 C67 N68 C69 -169.58(16) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006888'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_15

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C26 H28 F12 N2 O2 Pb Se2'
_chemical_formula_sum            'C26 H28 F12 N2 O2 Pb Se2'
_chemical_formula_weight         993.61
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.0061(3)
_cell_length_b                   11.5976(3)
_cell_length_c                   15.2067(4)
_cell_angle_alpha                72.1480(10)
_cell_angle_beta                 83.0470(10)
_cell_angle_gamma                67.7890(10)
_cell_volume                     1555.06(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9977
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      27.49
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.17
_exptl_crystal_density_diffrn    2.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             944
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    7.866
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.107
_exptl_absorpt_correction_T_max  0.263


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_number            25256
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.95
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total             7109
_reflns_number_gt                6344
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0182P)²+0.1157P] 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_number_reflns         7109
_refine_ls_number_parameters     410
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0265
_refine_ls_wR_factor_ref         0.0546
_refine_ls_wR_factor_gt          0.053
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.01
_refine_diff_density_rms         0.127

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.145252(13) 0.152576(11) 0.827928(8) 0.01535(4) Uani 1 1 d . . .
O1 O 0.0797(3) 0.3620(2) 0.81210(19) 0.0305(6) Uani 1 1 d . . .
C2 C -0.0410(4) 0.4644(3) 0.7759(2) 0.0203(8) Uani 1 1 d . . .
C3 C 0.0080(4) 0.5739(4) 0.7138(3) 0.0318(9) Uani 1 1 d . . .
F4 F 0.0843(3) 0.5392(3) 0.64218(19) 0.0539(7) Uani 1 1 d . . .
F5 F 0.0900(3) 0.6057(2) 0.75798(19) 0.0479(7) Uani 1 1 d . . .
F6 F -0.1027(3) 0.6837(2) 0.67834(17) 0.0456(6) Uani 1 1 d . . .
C7 C -0.1347(4) 0.5093(4) 0.8556(3) 0.0322(9) Uani 1 1 d . . .
F8 F -0.0671(3) 0.5447(3) 0.90661(18) 0.0526(7) Uani 1 1 d . . .
F9 F -0.2569(2) 0.6096(2) 0.82831(18) 0.0506(7) Uani 1 1 d . . .
F10 F -0.1736(3) 0.4134(3) 0.91227(17) 0.0550(7) Uani 1 1 d . . .
C11 C -0.1298(4) 0.4368(3) 0.7139(2) 0.0191(7) Uani 1 1 d . . .
H11A H -0.0766 0.429 0.6554 0.023 Uiso 1 1 calc R . .
H11B H -0.2229 0.5104 0.6986 0.023 Uiso 1 1 calc R . .
Se2 Se 0.43984(3) 0.20675(3) 0.77351(2) 0.01516(8) Uani 1 1 d . . .
C21 C -0.1669(3) 0.2157(3) 0.6719(2) 0.0175(7) Uani 1 1 d . . .
C22 C -0.1904(4) 0.2982(4) 0.5820(2) 0.0235(8) Uani 1 1 d . . .
H22 H -0.2017 0.3867 0.5698 0.028 Uiso 1 1 calc R . .
C23 C -0.1972(4) 0.2493(4) 0.5104(3) 0.0289(9) Uani 1 1 d . . .
H23 H -0.213 0.3049 0.449 0.035 Uiso 1 1 calc R . .
C24 C -0.1813(4) 0.1214(4) 0.5275(3) 0.0316(9) Uani 1 1 d . . .
H24 H -0.1854 0.0885 0.4783 0.038 Uiso 1 1 calc R . .
C25 C -0.1591(4) 0.0408(4) 0.6174(3) 0.0286(9) Uani 1 1 d . . .
H25 H -0.1487 -0.0475 0.6291 0.034 Uiso 1 1 calc R . .
C26 C -0.1518(3) 0.0859(3) 0.6905(2) 0.0198(7) Uani 1 1 d . . .
C27 C -0.1315(4) -0.0039(3) 0.7878(2) 0.0232(8) Uani 1 1 d . . .
H27A H -0.2064 0.0389 0.8283 0.028 Uiso 1 1 calc R . .
H27B H -0.1458 -0.084 0.7883 0.028 Uiso 1 1 calc R . .
N28 N 0.0113(3) -0.0396(3) 0.8260(2) 0.0227(7) Uani 1 1 d . . .
C29 C 0.0135(4) -0.1138(4) 0.9236(3) 0.0423(12) Uani 1 1 d . . .
H29A H -0.0074 -0.1916 0.9287 0.063 Uiso 1 1 calc R . .
H29B H -0.0597 -0.0598 0.9578 0.063 Uiso 1 1 calc R . .
H29C H 0.109 -0.1394 0.9494 0.063 Uiso 1 1 calc R . .
C30 C 0.1247(4) -0.1174(4) 0.7754(3) 0.0360(10) Uani 1 1 d . . .
H30A H 0.1063 -0.1956 0.7782 0.054 Uiso 1 1 calc R . .
H30B H 0.2185 -0.1425 0.8034 0.054 Uiso 1 1 calc R . .
H30C H 0.1254 -0.0664 0.7108 0.054 Uiso 1 1 calc R . .
O51 O 0.1827(2) 0.1680(2) 0.68252(15) 0.0222(5) Uani 1 1 d . . .
C52 C 0.3045(4) 0.1663(3) 0.6295(2) 0.0186(7) Uani 1 1 d . . .
C53 C 0.2513(4) 0.2231(4) 0.5284(2) 0.0249(8) Uani 1 1 d . . .
F54 F 0.1632(3) 0.3474(2) 0.51323(15) 0.0399(6) Uani 1 1 d . . .
F55 F 0.1792(2) 0.1604(2) 0.50726(14) 0.0340(5) Uani 1 1 d . . .
F56 F 0.3608(3) 0.2220(2) 0.46700(14) 0.0406(6) Uani 1 1 d . . .
C57 C 0.4115(4) 0.0246(4) 0.6445(2) 0.0241(8) Uani 1 1 d . . .
F58 F 0.3609(2) -0.0504(2) 0.61823(15) 0.0311(5) Uani 1 1 d . . .
F59 F 0.5370(2) 0.0174(2) 0.60105(17) 0.0387(6) Uani 1 1 d . . .
F60 F 0.4409(2) -0.0306(2) 0.73507(15) 0.0350(5) Uani 1 1 d . . .
C61 C 0.3823(4) 0.2503(3) 0.6444(2) 0.0197(7) Uani 1 1 d . . .
H61A H 0.3179 0.3427 0.6246 0.024 Uiso 1 1 calc R . .
H61B H 0.4696 0.2401 0.6047 0.024 Uiso 1 1 calc R . .
Se1 Se -0.16628(3) 0.27738(3) 0.77548(2) 0.01814(8) Uani 1 1 d . . .
C71 C 0.4322(3) 0.3775(3) 0.7685(2) 0.0166(7) Uani 1 1 d . . .
C72 C 0.4698(3) 0.4543(3) 0.6863(2) 0.0201(8) Uani 1 1 d . . .
H72 H 0.4931 0.4245 0.6328 0.024 Uiso 1 1 calc R . .
C73 C 0.4728(4) 0.5741(3) 0.6832(3) 0.0284(9) Uani 1 1 d . . .
H73 H 0.4948 0.6277 0.6267 0.034 Uiso 1 1 calc R . .
C74 C 0.4443(4) 0.6156(3) 0.7612(3) 0.0288(9) Uani 1 1 d . . .
H74 H 0.4492 0.6964 0.7594 0.035 Uiso 1 1 calc R . .
C75 C 0.4081(4) 0.5380(3) 0.8427(3) 0.0270(8) Uani 1 1 d . . .
H75 H 0.3884 0.567 0.8965 0.032 Uiso 1 1 calc R . .
C76 C 0.3999(3) 0.4192(3) 0.8475(2) 0.0185(7) Uani 1 1 d . . .
C77 C 0.3503(4) 0.3432(3) 0.9355(2) 0.0203(8) Uani 1 1 d . . .
H77A H 0.3382 0.3872 0.9839 0.024 Uiso 1 1 calc R . .
H77B H 0.255 0.3422 0.9251 0.024 Uiso 1 1 calc R . .
N78 N 0.4514(3) 0.2089(3) 0.96841(19) 0.0193(6) Uani 1 1 d . . .
C79 C 0.5843(4) 0.2060(4) 0.9996(3) 0.0316(9) Uani 1 1 d . . .
H79A H 0.6257 0.2594 0.9497 0.047 Uiso 1 1 calc R . .
H79B H 0.6532 0.1163 1.0172 0.047 Uiso 1 1 calc R . .
H79C H 0.564 0.2404 1.0532 0.047 Uiso 1 1 calc R . .
C80 C 0.3853(4) 0.1346(4) 1.0433(2) 0.0297(9) Uani 1 1 d . . .
H80A H 0.4531 0.0449 1.0648 0.045 Uiso 1 1 calc R . .
H80B H 0.2972 0.135 1.0211 0.045 Uiso 1 1 calc R . .
H80C H 0.3611 0.1739 1.0945 0.045 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O51 2.161(2) . ?
Pb1 O1 2.205(2) . ?
Pb1 Se1 2.9885(4) . ?
Pb1 Se2 3.2030(3) . ?
O1 C2 1.359(4) . ?
C2 C3 1.539(5) . ?
C2 C7 1.537(5) . ?
C2 C11 1.544(5) . ?
C3 F4 1.329(4) . ?
C3 F5 1.333(5) . ?
C3 F6 1.340(4) . ?
C7 F8 1.326(4) . ?
C7 F9 1.331(4) . ?
C7 F10 1.338(5) . ?
C11 Se1 1.948(3) . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
Se2 C71 1.930(3) . ?
Se2 C61 1.971(3) . ?
C21 C22 1.395(5) . ?
C21 C26 1.395(5) . ?
C21 Se1 1.920(3) . ?
C22 C23 1.392(5) . ?
C22 H22 0.95 . ?
C23 C24 1.374(5) . ?
C23 H23 0.95 . ?
C24 C25 1.387(5) . ?
C24 H24 0.95 . ?
C25 C26 1.385(5) . ?
C25 H25 0.95 . ?
C26 C27 1.512(5) . ?
C27 N28 1.468(4) . ?
C27 H27A 0.99 . ?
C27 H27B 0.99 . ?
N28 C30 1.461(5) . ?
N28 C29 1.467(5) . ?
C29 H29A 0.98 . ?
C29 H29B 0.98 . ?
C29 H29C 0.98 . ?
C30 H30A 0.98 . ?
C30 H30B 0.98 . ?
C30 H30C 0.98 . ?
O51 C52 1.375(4) . ?
C52 C61 1.536(5) . ?
C52 C53 1.546(5) . ?
C52 C57 1.548(5) . ?
C53 F55 1.323(4) . ?
C53 F54 1.339(4) . ?
C53 F56 1.349(4) . ?
C57 F58 1.330(4) . ?
C57 F59 1.332(4) . ?
C57 F60 1.344(4) . ?
C61 H61A 0.99 . ?
C61 H61B 0.99 . ?
C71 C76 1.389(5) . ?
C71 C72 1.397(4) . ?
C72 C73 1.388(5) . ?
C72 H72 0.95 . ?
C73 C74 1.372(5) . ?
C73 H73 0.95 . ?
C74 C75 1.389(5) . ?
C74 H74 0.95 . ?
C75 C76 1.390(5) . ?
C75 H75 0.95 . ?
C76 C77 1.503(5) . ?
C77 N78 1.467(4) . ?
C77 H77A 0.99 . ?
C77 H77B 0.99 . ?
N78 C79 1.451(5) . ?
N78 C80 1.458(4) . ?
C79 H79A 0.98 . ?
C79 H79B 0.98 . ?
C79 H79C 0.98 . ?
C80 H80A 0.98 . ?
C80 H80B 0.98 . ?
C80 H80C 0.98 . ?


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
O51 Pb1 O1 95.71(10) . . ?
O51 Pb1 Se1 84.46(6) . . ?
O1 Pb1 Se1 72.47(6) . . ?
O51 Pb1 Se2 72.89(6) . . ?
O1 Pb1 Se2 76.41(7) . . ?
Se1 Pb1 Se2 139.142(9) . . ?
C2 O1 Pb1 131.5(2) . . ?
O1 C2 C3 107.3(3) . . ?
O1 C2 C7 108.5(3) . . ?
C3 C2 C7 109.7(3) . . ?
O1 C2 C11 114.4(3) . . ?
C3 C2 C11 106.2(3) . . ?
C7 C2 C11 110.5(3) . . ?
F4 C3 F5 107.2(3) . . ?
F4 C3 F6 106.2(3) . . ?
F5 C3 F6 106.3(3) . . ?
F4 C3 C2 110.7(3) . . ?
F5 C3 C2 112.9(3) . . ?
F6 C3 C2 113.0(3) . . ?
F8 C7 F9 106.1(3) . . ?
F8 C7 F10 107.0(3) . . ?
F9 C7 F10 106.0(3) . . ?
F8 C7 C2 112.9(3) . . ?
F9 C7 C2 113.9(3) . . ?
F10 C7 C2 110.4(3) . . ?
C2 C11 Se1 111.0(2) . . ?
C2 C11 H11A 109.4 . . ?
Se1 C11 H11A 109.4 . . ?
C2 C11 H11B 109.4 . . ?
Se1 C11 H11B 109.4 . . ?
H11A C11 H11B 108 . . ?
C71 Se2 C61 96.49(14) . . ?
C71 Se2 Pb1 116.25(9) . . ?
C61 Se2 Pb1 85.66(10) . . ?
C22 C21 C26 120.7(3) . . ?
C22 C21 Se1 121.9(3) . . ?
C26 C21 Se1 117.3(2) . . ?
C21 C22 C23 119.2(4) . . ?
C21 C22 H22 120.4 . . ?
C23 C22 H22 120.4 . . ?
C24 C23 C22 120.7(3) . . ?
C24 C23 H23 119.6 . . ?
C22 C23 H23 119.6 . . ?
C23 C24 C25 119.4(4) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C24 C25 C26 121.6(4) . . ?
C24 C25 H25 119.2 . . ?
C26 C25 H25 119.2 . . ?
C25 C26 C21 118.4(3) . . ?
C25 C26 C27 120.1(3) . . ?
C21 C26 C27 121.5(3) . . ?
N28 C27 C26 113.5(3) . . ?
N28 C27 H27A 108.9 . . ?
C26 C27 H27A 108.9 . . ?
N28 C27 H27B 108.9 . . ?
C26 C27 H27B 108.9 . . ?
H27A C27 H27B 107.7 . . ?
C30 N28 C29 109.7(3) . . ?
C30 N28 C27 111.0(3) . . ?
C29 N28 C27 108.9(3) . . ?
N28 C29 H29A 109.5 . . ?
N28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
N28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
N28 C30 H30A 109.5 . . ?
N28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
N28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C52 O51 Pb1 130.3(2) . . ?
O51 C52 C61 115.3(3) . . ?
O51 C52 C53 105.2(3) . . ?
C61 C52 C53 107.0(3) . . ?
O51 C52 C57 109.8(3) . . ?
C61 C52 C57 109.7(3) . . ?
C53 C52 C57 109.6(3) . . ?
F55 C53 F54 107.2(3) . . ?
F55 C53 F56 107.2(3) . . ?
F54 C53 F56 106.4(3) . . ?
F55 C53 C52 113.0(3) . . ?
F54 C53 C52 110.3(3) . . ?
F56 C53 C52 112.4(3) . . ?
F58 C57 F59 107.4(3) . . ?
F58 C57 F60 106.4(3) . . ?
F59 C57 F60 106.9(3) . . ?
F58 C57 C52 113.9(3) . . ?
F59 C57 C52 112.6(3) . . ?
F60 C57 C52 109.3(3) . . ?
C52 C61 Se2 113.7(2) . . ?
C52 C61 H61A 108.8 . . ?
Se2 C61 H61A 108.8 . . ?
C52 C61 H61B 108.8 . . ?
Se2 C61 H61B 108.8 . . ?
H61A C61 H61B 107.7 . . ?
C21 Se1 C11 100.94(15) . . ?
C21 Se1 Pb1 101.57(9) . . ?
C11 Se1 Pb1 87.62(10) . . ?
C76 C71 C72 120.5(3) . . ?
C76 C71 Se2 120.1(2) . . ?
C72 C71 Se2 119.2(3) . . ?
C73 C72 C71 119.9(3) . . ?
C73 C72 H72 120.1 . . ?
C71 C72 H72 120.1 . . ?
C74 C73 C72 120.3(3) . . ?
C74 C73 H73 119.8 . . ?
C72 C73 H73 119.8 . . ?
C73 C74 C75 119.3(4) . . ?
C73 C74 H74 120.3 . . ?
C75 C74 H74 120.3 . . ?
C74 C75 C76 121.8(4) . . ?
C74 C75 H75 119.1 . . ?
C76 C75 H75 119.1 . . ?
C71 C76 C75 118.1(3) . . ?
C71 C76 C77 122.0(3) . . ?
C75 C76 C77 119.8(3) . . ?
N78 C77 C76 112.9(3) . . ?
N78 C77 H77A 109 . . ?
C76 C77 H77A 109 . . ?
N78 C77 H77B 109 . . ?
C76 C77 H77B 109 . . ?
H77A C77 H77B 107.8 . . ?
C79 N78 C80 110.1(3) . . ?
C79 N78 C77 110.6(3) . . ?
C80 N78 C77 109.9(3) . . ?
N78 C79 H79A 109.5 . . ?
N78 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
N78 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
N78 C80 H80A 109.5 . . ?
N78 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
N78 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?


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
O51 Pb1 O1 C2 70.8(3) . . . . ?
Se1 Pb1 O1 C2 -11.6(3) . . . . ?
Se2 Pb1 O1 C2 141.6(3) . . . . ?
Pb1 O1 C2 C3 -135.1(3) . . . . ?
Pb1 O1 C2 C7 106.4(3) . . . . ?
Pb1 O1 C2 C11 -17.5(4) . . . . ?
O1 C2 C3 F4 64.8(4) . . . . ?
C7 C2 C3 F4 -177.4(3) . . . . ?
C11 C2 C3 F4 -58.0(4) . . . . ?
O1 C2 C3 F5 -55.4(4) . . . . ?
C7 C2 C3 F5 62.3(4) . . . . ?
C11 C2 C3 F5 -178.3(3) . . . . ?
O1 C2 C3 F6 -176.1(3) . . . . ?
C7 C2 C3 F6 -58.4(4) . . . . ?
C11 C2 C3 F6 61.0(4) . . . . ?
O1 C2 C7 F8 59.1(4) . . . . ?
C3 C2 C7 F8 -57.9(4) . . . . ?
C11 C2 C7 F8 -174.7(3) . . . . ?
O1 C2 C7 F9 -179.8(3) . . . . ?
C3 C2 C7 F9 63.2(4) . . . . ?
C11 C2 C7 F9 -53.6(4) . . . . ?
O1 C2 C7 F10 -60.7(4) . . . . ?
C3 C2 C7 F10 -177.6(3) . . . . ?
C11 C2 C7 F10 65.6(4) . . . . ?
O1 C2 C11 Se1 50.1(4) . . . . ?
C3 C2 C11 Se1 168.4(2) . . . . ?
C7 C2 C11 Se1 -72.8(3) . . . . ?
O51 Pb1 Se2 C71 107.95(13) . . . . ?
O1 Pb1 Se2 C71 7.49(13) . . . . ?
Se1 Pb1 Se2 C71 48.63(11) . . . . ?
O51 Pb1 Se2 C61 12.84(12) . . . . ?
O1 Pb1 Se2 C61 -87.62(12) . . . . ?
Se1 Pb1 Se2 C61 -46.48(10) . . . . ?
C26 C21 C22 C23 -0.7(5) . . . . ?
Se1 C21 C22 C23 -176.7(3) . . . . ?
C21 C22 C23 C24 0.1(5) . . . . ?
C22 C23 C24 C25 0.4(6) . . . . ?
C23 C24 C25 C26 -0.4(6) . . . . ?
C24 C25 C26 C21 -0.1(5) . . . . ?
C24 C25 C26 C27 178.4(3) . . . . ?
C22 C21 C26 C25 0.7(5) . . . . ?
Se1 C21 C26 C25 176.8(3) . . . . ?
C22 C21 C26 C27 -177.8(3) . . . . ?
Se1 C21 C26 C27 -1.7(4) . . . . ?
C25 C26 C27 N28 109.8(4) . . . . ?
C21 C26 C27 N28 -71.7(4) . . . . ?
C26 C27 N28 C30 -65.7(4) . . . . ?
C26 C27 N28 C29 173.5(3) . . . . ?
O1 Pb1 O51 C52 87.6(3) . . . . ?
Se1 Pb1 O51 C52 159.3(3) . . . . ?
Se2 Pb1 O51 C52 13.8(3) . . . . ?
Pb1 O51 C52 C61 -45.2(4) . . . . ?
Pb1 O51 C52 C53 -162.8(2) . . . . ?
Pb1 O51 C52 C57 79.3(3) . . . . ?
O51 C52 C53 F55 -55.4(4) . . . . ?
C61 C52 C53 F55 -178.6(3) . . . . ?
C57 C52 C53 F55 62.6(4) . . . . ?
O51 C52 C53 F54 64.5(4) . . . . ?
C61 C52 C53 F54 -58.7(4) . . . . ?
C57 C52 C53 F54 -177.5(3) . . . . ?
O51 C52 C53 F56 -176.9(3) . . . . ?
C61 C52 C53 F56 59.9(4) . . . . ?
C57 C52 C53 F56 -58.9(4) . . . . ?
O51 C52 C57 F58 62.9(4) . . . . ?
C61 C52 C57 F58 -169.4(3) . . . . ?
C53 C52 C57 F58 -52.2(4) . . . . ?
O51 C52 C57 F59 -174.6(3) . . . . ?
C61 C52 C57 F59 -46.8(4) . . . . ?
C53 C52 C57 F59 70.3(4) . . . . ?
O51 C52 C57 F60 -55.9(4) . . . . ?
C61 C52 C57 F60 71.8(3) . . . . ?
C53 C52 C57 F60 -171.0(3) . . . . ?
O51 C52 C61 Se2 56.8(3) . . . . ?
C53 C52 C61 Se2 173.4(2) . . . . ?
C57 C52 C61 Se2 -67.8(3) . . . . ?
C71 Se2 C61 C52 -151.9(2) . . . . ?
Pb1 Se2 C61 C52 -35.9(2) . . . . ?
C22 C21 Se1 C11 -20.6(3) . . . . ?
C26 C21 Se1 C11 163.3(2) . . . . ?
C22 C21 Se1 Pb1 -110.4(3) . . . . ?
C26 C21 Se1 Pb1 73.5(2) . . . . ?
C2 C11 Se1 C21 -147.4(2) . . . . ?
C2 C11 Se1 Pb1 -46.1(2) . . . . ?
O51 Pb1 Se1 C21 30.17(13) . . . . ?
O1 Pb1 Se1 C21 127.96(13) . . . . ?
Se2 Pb1 Se1 C21 85.85(10) . . . . ?
O51 Pb1 Se1 C11 -70.51(12) . . . . ?
O1 Pb1 Se1 C11 27.28(13) . . . . ?
Se2 Pb1 Se1 C11 -14.83(11) . . . . ?
C61 Se2 C71 C76 150.8(3) . . . . ?
Pb1 Se2 C71 C76 62.4(3) . . . . ?
C61 Se2 C71 C72 -33.8(3) . . . . ?
Pb1 Se2 C71 C72 -122.2(2) . . . . ?
C76 C71 C72 C73 -0.9(5) . . . . ?
Se2 C71 C72 C73 -176.3(2) . . . . ?
C71 C72 C73 C74 2.4(5) . . . . ?
C72 C73 C74 C75 -1.9(5) . . . . ?
C73 C74 C75 C76 0.0(5) . . . . ?
C72 C71 C76 C75 -0.9(5) . . . . ?
Se2 C71 C76 C75 174.4(2) . . . . ?
C72 C71 C76 C77 176.2(3) . . . . ?
Se2 C71 C76 C77 -8.5(4) . . . . ?
C74 C75 C76 C71 1.4(5) . . . . ?
C74 C75 C76 C77 -175.8(3) . . . . ?
C71 C76 C77 N78 55.8(4) . . . . ?
C75 C76 C77 N78 -127.1(3) . . . . ?
C76 C77 N78 C79 68.6(4) . . . . ?
C76 C77 N78 C80 -169.7(3) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006889'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_WLF033

_audit_creation_date             2014-08-21T17:11:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         
'2(C36 H2 B2 F30 N),C26 H40 N2 O2 Pb2 Se2,7(C H2 Cl2)'
_chemical_formula_sum            'C105 H58 B4 Cl14 F60 N4 O2 Pb2 Se2'
_chemical_formula_weight         3659.39
_chemical_compound_source        'synthesis as described'
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_Int_Tables_number      4
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   11.9038(6)
_cell_length_b                   14.3044(7)
_cell_length_c                   32.5897(18)
_cell_angle_alpha                90
_cell_angle_beta                 90.138(2)
_cell_angle_gamma                90
_cell_volume                     5549.3(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9945
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      24.97
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.834
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3524
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.181
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.334
_exptl_absorpt_correction_T_max  0.471


#----------------------------------------------------------------------------#
#                   SQUEEZE RESULTS                                          #
#----------------------------------------------------------------------------#

# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.113 0.110 -0.024 112 59 '2(CH2Cl2) '
2 0.112 0.610 0.024 113 59 '2(CH2Cl2) '
3 0.005 -0.065 0.249 181 91 '3(CH2Cl2) '
4 0.097 0.266 0.463 118 56 '2(CH2Cl2) '
5 -0.097 0.766 0.537 117 57 '2(CH2Cl2) '
6 -0.005 0.435 0.751 181 94 '3(CH2Cl2) '
7 0.395 0.838 0.811 10 5 ' '
8 0.605 0.338 0.189 10 4 ' '
_platon_squeeze_details          
;
;

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0512
_diffrn_reflns_av_unetI/netI     0.0973
_diffrn_reflns_number            49272
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total             25119
_reflns_number_gt                22512
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0986P)²+0.0000P] 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_number_reflns         25119
_refine_ls_number_parameters     722
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0604
_refine_ls_wR_factor_ref         0.1612
_refine_ls_wR_factor_gt          0.1561
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.039(6)
_refine_diff_density_max         1.541
_refine_diff_density_min         -2.065
_refine_diff_density_rms         0.195

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pb1 Pb 0.79410(3) 0.08597(3) 0.720867(12) 0.01820(9) Uani 1 1 d . . .
Pb2 Pb 0.95150(3) 0.00953(3) 0.815696(12) 0.01879(9) Uani 1 1 d . . .
Se1 Se 0.57415(9) -0.03118(8) 0.72693(3) 0.0202(2) Uani 1 1 d . . .
Se2 Se 1.19102(9) -0.04065(8) 0.78119(4) 0.0214(2) Uani 1 1 d . . .
C201 C 0.6861(10) 0.0182(10) 0.8501(4) 0.0276(10) Uani 1 1 d . . .
H20A H 0.7077 -0.0474 0.8537 0.041 Uiso 1 1 calc R . .
H20B H 0.6159 0.0303 0.8648 0.041 Uiso 1 1 calc R . .
H20C H 0.7455 0.0586 0.861 0.041 Uiso 1 1 calc R . .
C202 C 0.6694(10) 0.0386(9) 0.8047(4) 0.0276(10) Uani 1 1 d D . .
C203 C 0.6351(10) 0.1397(9) 0.7998(4) 0.0276(10) Uani 1 1 d D . .
H20D H 0.6226 0.1534 0.7706 0.041 Uiso 1 1 calc R . .
H20E H 0.6947 0.1803 0.8104 0.041 Uiso 1 1 calc R . .
H20F H 0.5656 0.1511 0.815 0.041 Uiso 1 1 calc R . .
C204 C 0.5846(10) -0.0282(10) 0.7868(4) 0.0276(10) Uani 1 1 d . . .
H20G H 0.5097 -0.0119 0.7978 0.033 Uiso 1 1 calc R . .
H20H H 0.603 -0.0919 0.7965 0.033 Uiso 1 1 calc R . .
C205 C 0.6405(11) -0.1539(9) 0.7176(4) 0.0276(11) Uani 1 1 d . . .
C206 C 0.6052(11) -0.2272(9) 0.7415(4) 0.0276(11) Uani 1 1 d . . .
H206 H 0.551 -0.2172 0.7624 0.033 Uiso 1 1 calc R . .
C207 C 0.6496(11) -0.3177(9) 0.7349(4) 0.0276(11) Uani 1 1 d . . .
H207 H 0.6345 -0.3676 0.7534 0.033 Uiso 1 1 calc R . .
C208 C 0.7148(11) -0.3303(9) 0.7013(4) 0.0276(11) Uani 1 1 d . . .
H208 H 0.7388 -0.3919 0.6949 0.033 Uiso 1 1 calc R . .
C209 C 0.7487(11) -0.2573(9) 0.6756(4) 0.0276(11) Uani 1 1 d . . .
H209 H 0.8004 -0.2684 0.654 0.033 Uiso 1 1 calc R . .
C210 C 0.7053(11) -0.1681(8) 0.6822(4) 0.0276(11) Uani 1 1 d D . .
C211 C 0.7426(10) -0.0913(8) 0.6529(4) 0.0251(9) Uani 1 1 d D . .
H21A H 0.6765 -0.0515 0.6469 0.03 Uiso 1 1 calc R . .
H21B H 0.7652 -0.1212 0.6268 0.03 Uiso 1 1 calc R . .
C212 C 0.8580(11) 0.0314(9) 0.6307(4) 0.0251(9) Uani 1 1 d . . .
H21C H 0.794 0.0735 0.6267 0.038 Uiso 1 1 calc R . .
H21D H 0.8669 -0.0082 0.6063 0.038 Uiso 1 1 calc R . .
H21E H 0.9264 0.0683 0.6349 0.038 Uiso 1 1 calc R . .
C213 C 0.9352(11) -0.0864(9) 0.6749(4) 0.0251(9) Uani 1 1 d . . .
H21F H 0.9971 -0.0477 0.6853 0.038 Uiso 1 1 calc R . .
H21G H 0.9585 -0.1174 0.6495 0.038 Uiso 1 1 calc R . .
H21H H 0.9157 -0.1336 0.6955 0.038 Uiso 1 1 calc R . .
C251 C 1.0562(11) 0.1729(10) 0.7030(4) 0.0276(10) Uani 1 1 d . . .
H25A H 1.0454 0.1272 0.6809 0.041 Uiso 1 1 calc R . .
H25B H 1.1238 0.2099 0.6976 0.041 Uiso 1 1 calc R . .
H25C H 0.9908 0.2143 0.7044 0.041 Uiso 1 1 calc R . .
C252 C 1.0702(10) 0.1198(10) 0.7452(4) 0.0276(10) Uani 1 1 d . . .
C253 C 1.0806(10) 0.1889(10) 0.7789(4) 0.0276(10) Uani 1 1 d . . .
H25D H 1.0784 0.1565 0.8053 0.041 Uiso 1 1 calc R . .
H25E H 1.0182 0.2335 0.7773 0.041 Uiso 1 1 calc R . .
H25F H 1.152 0.2225 0.7763 0.041 Uiso 1 1 calc R . .
C254 C 1.1738(10) 0.0579(9) 0.7394(4) 0.0276(10) Uani 1 1 d . . .
H25G H 1.2417 0.0979 0.7398 0.033 Uiso 1 1 calc R . .
H25H H 1.1695 0.0281 0.712 0.033 Uiso 1 1 calc R . .
C255 C 1.1498(11) -0.1465(9) 0.7483(4) 0.0295(11) Uani 1 1 d . . .
C256 C 1.1839(11) -0.1539(9) 0.7093(4) 0.0295(11) Uani 1 1 d . . .
H256 H 1.2311 -0.1069 0.6981 0.035 Uiso 1 1 calc R . .
C257 C 1.1510(11) -0.2301(9) 0.6844(5) 0.0295(11) Uani 1 1 d . . .
H257 H 1.1755 -0.2333 0.6568 0.035 Uiso 1 1 calc R . .
C258 C 1.0854(11) -0.2978(9) 0.6996(4) 0.0295(11) Uani 1 1 d . . .
H258 H 1.0612 -0.3475 0.6824 0.035 Uiso 1 1 calc R . .
C259 C 1.0535(11) -0.2955(9) 0.7397(4) 0.0295(11) Uani 1 1 d . . .
H259 H 1.0118 -0.346 0.7508 0.035 Uiso 1 1 calc R . .
C260 C 1.0825(11) -0.2171(9) 0.7651(4) 0.0295(11) Uani 1 1 d . . .
C261 C 1.0475(11) -0.2185(9) 0.8114(4) 0.0251(9) Uani 1 1 d . . .
H26A H 1.0335 -0.2841 0.8197 0.03 Uiso 1 1 calc R . .
H26B H 1.1109 -0.1947 0.8281 0.03 Uiso 1 1 calc R . .
C262 C 0.8448(11) -0.2071(9) 0.7978(4) 0.0251(9) Uani 1 1 d . . .
H26C H 0.778 -0.1686 0.8025 0.038 Uiso 1 1 calc R . .
H26D H 0.8316 -0.2704 0.8083 0.038 Uiso 1 1 calc R . .
H26E H 0.8602 -0.2101 0.7683 0.038 Uiso 1 1 calc R . .
C263 C 0.9306(4) -0.1767(3) 0.86608(13) 0.0251(9) Uani 1 1 d . . .
H26F H 0.8651 -0.1407 0.875 0.038 Uiso 1 1 calc R . .
H26G H 0.9975 -0.155 0.8809 0.038 Uiso 1 1 calc R . .
H26H H 0.9184 -0.2432 0.8718 0.038 Uiso 1 1 calc R . .
N201 N 0.8381(4) -0.0277(3) 0.66678(13) 0.0251(9) Uani 1 1 d RD . .
N202 N 0.9477(4) -0.1631(3) 0.82047(13) 0.0251(9) Uani 1 1 d R . .
O1 O 0.7772(4) 0.0218(3) 0.78435(13) 0.0239(12) Uani 1 1 d R . .
O2 O 0.9639(4) 0.0519(3) 0.74907(13) 0.0239(12) Uani 1 1 d R . .
C1 C 0.4748(10) 0.5814(10) 0.6117(4) 0.0245(10) Uani 1 1 d . . .
C2 C 0.4323(11) 0.6087(8) 0.6498(4) 0.0245(10) Uani 1 1 d . . .
C3 C 0.4280(11) 0.6992(9) 0.6642(4) 0.0245(10) Uani 1 1 d . . .
C4 C 0.4576(11) 0.7733(9) 0.6391(4) 0.0245(10) Uani 1 1 d . . .
C5 C 0.5033(11) 0.7540(9) 0.6013(4) 0.0245(10) Uani 1 1 d . . .
C6 C 0.5060(11) 0.6595(9) 0.5883(4) 0.0245(10) Uani 1 1 d . . .
C11 C 0.3693(12) 0.4904(9) 0.5553(4) 0.0298(11) Uani 1 1 d . . .
C12 C 0.2635(11) 0.5077(10) 0.5688(4) 0.0298(11) Uani 1 1 d . . .
C13 C 0.1693(11) 0.5267(9) 0.5434(4) 0.0298(11) Uani 1 1 d . . .
C14 C 0.1854(11) 0.5222(9) 0.4994(4) 0.0298(11) Uani 1 1 d . . .
C15 C 0.2960(11) 0.5077(10) 0.4837(4) 0.0298(11) Uani 1 1 d . . .
C16 C 0.3817(11) 0.4952(9) 0.5118(4) 0.0298(11) Uani 1 1 d . . .
C21 C 0.4449(11) 0.3967(9) 0.6234(4) 0.0248(10) Uani 1 1 d . . .
C22 C 0.5111(10) 0.3842(9) 0.6569(4) 0.0248(10) Uani 1 1 d . . .
C23 C 0.4975(10) 0.3173(9) 0.6856(4) 0.0248(10) Uani 1 1 d . . .
C24 C 0.4140(10) 0.2497(9) 0.6804(4) 0.0248(10) Uani 1 1 d . . .
C25 C 0.3424(11) 0.2546(9) 0.6475(4) 0.0248(10) Uani 1 1 d . . .
C26 C 0.3587(10) 0.3258(9) 0.6194(4) 0.0248(10) Uani 1 1 d . . .
C31 C 0.7161(10) 0.3757(9) 0.5137(4) 0.0231(10) Uani 1 1 d . . .
C32 C 0.7184(10) 0.3073(9) 0.4840(4) 0.0231(10) Uani 1 1 d . . .
C33 C 0.7665(10) 0.3174(9) 0.4459(4) 0.0231(10) Uani 1 1 d . . .
C34 C 0.8063(10) 0.3979(9) 0.4343(4) 0.0231(10) Uani 1 1 d . . .
C35 C 0.8140(10) 0.4747(9) 0.4632(4) 0.0231(10) Uani 1 1 d . . .
C36 C 0.7677(10) 0.4587(9) 0.5016(4) 0.0231(10) Uani 1 1 d . . .
C41 C 0.5942(10) 0.2740(8) 0.5709(4) 0.0218(10) Uani 1 1 d . . .
C42 C 0.6087(10) 0.2166(8) 0.6037(4) 0.0218(10) Uani 1 1 d . . .
C43 C 0.5398(10) 0.1358(8) 0.6104(4) 0.0218(10) Uani 1 1 d . . .
C44 C 0.4555(10) 0.1128(8) 0.5831(4) 0.0218(10) Uani 1 1 d . . .
C45 C 0.4392(10) 0.1717(8) 0.5499(4) 0.0218(10) Uani 1 1 d . . .
C46 C 0.5060(10) 0.2493(8) 0.5437(4) 0.0218(10) Uani 1 1 d . . .
C51 C 0.7881(10) 0.3725(8) 0.5892(4) 0.0223(10) Uani 1 1 d . . .
C52 C 0.8297(10) 0.4436(8) 0.6129(4) 0.0223(10) Uani 1 1 d . . .
C53 C 0.9330(10) 0.4417(8) 0.6322(4) 0.0223(10) Uani 1 1 d . . .
C54 C 1.0027(10) 0.3650(8) 0.6273(4) 0.0223(10) Uani 1 1 d . . .
C55 C 0.9635(10) 0.2908(8) 0.6040(4) 0.0223(10) Uani 1 1 d . . .
C56 C 0.8603(10) 0.2969(8) 0.5865(4) 0.0223(10) Uani 1 1 d . . .
N1 N 0.5922(7) 0.4620(6) 0.5701(3) 0.0138(17) Uani 1 1 d . . .
H1A H 0.588 0.4902 0.5448 0.017 Uiso 1 1 calc R . .
H1B H 0.6394 0.4993 0.5854 0.017 Uiso 1 1 calc R . .
F2 F 0.3981(7) 0.5457(5) 0.6766(2) 0.0342(8) Uani 1 1 d . . .
F3 F 0.3881(7) 0.7186(5) 0.7014(2) 0.0342(8) Uani 1 1 d . . .
F4 F 0.4502(8) 0.8623(5) 0.6518(2) 0.0342(8) Uani 1 1 d . . .
F5 F 0.5342(8) 0.8224(5) 0.5769(2) 0.0342(8) Uani 1 1 d . . .
F6 F 0.5439(8) 0.6473(5) 0.5496(2) 0.0342(8) Uani 1 1 d . . .
F12 F 0.2378(6) 0.5123(7) 0.6092(2) 0.0385(8) Uani 1 1 d . . .
F13 F 0.0659(7) 0.5417(6) 0.5581(3) 0.0385(8) Uani 1 1 d . . .
F14 F 0.1000(7) 0.5419(6) 0.4751(3) 0.0385(8) Uani 1 1 d . . .
F15 F 0.3112(7) 0.5088(7) 0.4449(2) 0.0385(8) Uani 1 1 d . . .
F16 F 0.4831(7) 0.4835(6) 0.4952(3) 0.0385(8) Uani 1 1 d . . .
F22 F 0.5971(7) 0.4445(6) 0.6637(3) 0.0376(8) Uani 1 1 d . . .
F23 F 0.5668(7) 0.3079(6) 0.7197(3) 0.0376(8) Uani 1 1 d . . .
F24 F 0.4012(7) 0.1818(6) 0.7094(3) 0.0376(8) Uani 1 1 d . . .
F25 F 0.2664(7) 0.1916(6) 0.6413(3) 0.0376(8) Uani 1 1 d . . .
F26 F 0.2917(8) 0.3232(6) 0.5877(3) 0.0376(8) Uani 1 1 d . . .
F32 F 0.6777(7) 0.2188(5) 0.4923(2) 0.0297(7) Uani 1 1 d . . .
F33 F 0.7672(7) 0.2445(5) 0.4191(2) 0.0297(7) Uani 1 1 d . . .
F34 F 0.8561(7) 0.4127(5) 0.3969(2) 0.0297(7) Uani 1 1 d . . .
F35 F 0.8601(7) 0.5543(5) 0.4538(2) 0.0297(7) Uani 1 1 d . . .
F36 F 0.7776(6) 0.5294(5) 0.5276(2) 0.0297(7) Uani 1 1 d . . .
F42 F 0.6861(6) 0.2315(5) 0.6330(2) 0.0289(7) Uani 1 1 d . . .
F43 F 0.5602(6) 0.0810(6) 0.6437(2) 0.0289(7) Uani 1 1 d . . .
F44 F 0.3938(6) 0.0383(5) 0.5891(2) 0.0289(7) Uani 1 1 d . . .
F45 F 0.3523(6) 0.1511(5) 0.5238(2) 0.0289(7) Uani 1 1 d . . .
F46 F 0.4798(6) 0.3034(5) 0.5125(2) 0.0289(7) Uani 1 1 d . . .
F52 F 0.7702(7) 0.5236(6) 0.6184(3) 0.0375(8) Uani 1 1 d . . .
F53 F 0.9693(7) 0.5179(6) 0.6541(2) 0.0375(8) Uani 1 1 d . . .
F54 F 1.1008(7) 0.3611(6) 0.6460(3) 0.0375(8) Uani 1 1 d . . .
F55 F 1.0290(7) 0.2167(6) 0.6003(3) 0.0375(8) Uani 1 1 d . . .
F56 F 0.8280(7) 0.2205(6) 0.5641(3) 0.0375(8) Uani 1 1 d . . .
B1 B 0.4670(11) 0.4821(8) 0.5903(4) 0.0174(17) Uani 1 1 d . . .
B2 B 0.6665(11) 0.3698(8) 0.5616(4) 0.0174(17) Uani 1 1 d . . .
C61 C 0.4253(9) 0.2764(8) 0.9012(3) 0.0174(9) Uani 1 1 d . . .
C62 C 0.4621(10) 0.2020(8) 0.9232(3) 0.0174(9) Uani 1 1 d . . .
C63 C 0.4525(10) 0.1100(7) 0.9133(3) 0.0174(9) Uani 1 1 d . . .
C64 C 0.3954(9) 0.0852(9) 0.8762(3) 0.0174(9) Uani 1 1 d . . .
C65 C 0.3591(10) 0.1589(8) 0.8522(3) 0.0174(9) Uani 1 1 d . . .
C66 C 0.3731(10) 0.2513(8) 0.8651(3) 0.0174(9) Uani 1 1 d . . .
C71 C 0.3370(10) 0.3841(9) 0.9563(4) 0.0234(10) Uani 1 1 d . . .
C72 C 0.3505(10) 0.3807(9) 0.9983(4) 0.0234(10) Uani 1 1 d . . .
C73 C 0.2649(10) 0.3707(9) 1.0274(4) 0.0234(10) Uani 1 1 d . . .
C74 C 0.1547(10) 0.3578(9) 1.0126(4) 0.0234(10) Uani 1 1 d . . .
C75 C 0.1336(10) 0.3591(9) 0.9725(4) 0.0234(10) Uani 1 1 d . . .
C76 C 0.2250(10) 0.3736(9) 0.9453(4) 0.0234(10) Uani 1 1 d . . .
C81 C 0.4101(10) 0.4644(9) 0.8837(4) 0.0239(10) Uani 1 1 d . . .
C82 C 0.4701(10) 0.4607(8) 0.8478(4) 0.0239(10) Uani 1 1 d . . .
C83 C 0.4581(10) 0.5184(9) 0.8151(4) 0.0239(10) Uani 1 1 d . . .
C84 C 0.3746(10) 0.5923(9) 0.8174(4) 0.0239(10) Uani 1 1 d . . .
C85 C 0.3198(10) 0.5993(8) 0.8524(4) 0.0239(10) Uani 1 1 d . . .
C86 C 0.3337(11) 0.5384(8) 0.8859(4) 0.0239(10) Uani 1 1 d . . .
C91 C 0.7590(10) 0.4427(9) 0.9034(4) 0.0235(10) Uani 1 1 d . . .
C92 C 0.8496(9) 0.4999(10) 0.8981(3) 0.0235(10) Uani 1 1 d . . .
C93 C 0.9493(10) 0.4778(9) 0.8773(3) 0.0235(10) Uani 1 1 d . . .
C94 C 0.9584(10) 0.3884(9) 0.8605(3) 0.0235(10) Uani 1 1 d . . .
C95 C 0.8675(10) 0.3296(9) 0.8662(4) 0.0235(10) Uani 1 1 d . . .
C96 C 0.7691(10) 0.3550(9) 0.8868(4) 0.0235(10) Uani 1 1 d . . .
C101 C 0.5945(9) 0.5804(9) 0.9210(3) 0.0214(9) Uani 1 1 d . . .
C102 C 0.6144(10) 0.6331(9) 0.8852(4) 0.0214(9) Uani 1 1 d . . .
C103 C 0.5660(10) 0.7185(8) 0.8791(4) 0.0214(9) Uani 1 1 d . . .
C104 C 0.4854(10) 0.7531(8) 0.9054(4) 0.0214(9) Uani 1 1 d . . .
C105 C 0.4575(10) 0.6981(8) 0.9407(4) 0.0214(9) Uani 1 1 d . . .
C106 C 0.5149(10) 0.6182(9) 0.9472(4) 0.0214(9) Uani 1 1 d . . .
C111 C 0.7175(10) 0.4896(8) 0.9803(4) 0.0228(10) Uani 1 1 d . . .
C112 C 0.7570(10) 0.4082(9) 0.9989(4) 0.0228(10) Uani 1 1 d . . .
C113 C 0.8088(10) 0.4046(8) 1.0374(4) 0.0228(10) Uani 1 1 d . . .
C114 C 0.8246(10) 0.4875(8) 1.0575(4) 0.0228(10) Uani 1 1 d . . .
C115 C 0.7920(10) 0.5712(8) 1.0409(4) 0.0228(10) Uani 1 1 d . . .
C116 C 0.7412(9) 0.5715(9) 1.0021(4) 0.0228(10) Uani 1 1 d . . .
N2 N 0.5572(8) 0.4014(6) 0.9394(3) 0.0153(12) Uani 1 1 d . . .
H2A H 0.5441 0.4009 0.9672 0.018 Uiso 1 1 calc R . .
H2B H 0.5942 0.3463 0.9341 0.018 Uiso 1 1 calc R . .
F62 F 0.5127(7) 0.2179(5) 0.9604(2) 0.0295(7) Uani 1 1 d . . .
F63 F 0.4897(7) 0.0402(5) 0.9366(2) 0.0295(7) Uani 1 1 d . . .
F64 F 0.3845(7) -0.0022(5) 0.8648(2) 0.0295(7) Uani 1 1 d . . .
F65 F 0.3097(7) 0.1375(5) 0.8154(2) 0.0295(7) Uani 1 1 d . . .
F66 F 0.3284(7) 0.3146(5) 0.8381(2) 0.0295(7) Uani 1 1 d . . .
F72 F 0.4567(7) 0.3876(6) 1.0159(2) 0.0338(8) Uani 1 1 d . . .
F73 F 0.2900(7) 0.3676(6) 1.0672(2) 0.0338(8) Uani 1 1 d . . .
F74 F 0.0736(6) 0.3458(6) 1.0417(2) 0.0338(8) Uani 1 1 d . . .
F75 F 0.0307(7) 0.3465(6) 0.9592(2) 0.0338(8) Uani 1 1 d . . .
F76 F 0.1969(7) 0.3693(6) 0.9052(2) 0.0338(8) Uani 1 1 d . . .
F82 F 0.5469(7) 0.3927(6) 0.8414(2) 0.0328(8) Uani 1 1 d . . .
F83 F 0.5145(6) 0.5108(6) 0.7805(2) 0.0328(8) Uani 1 1 d . . .
F84 F 0.3629(7) 0.6509(6) 0.7869(2) 0.0328(8) Uani 1 1 d . . .
F85 F 0.2442(7) 0.6693(6) 0.8567(2) 0.0328(8) Uani 1 1 d . . .
F86 F 0.2746(7) 0.5539(5) 0.9200(2) 0.0328(8) Uani 1 1 d . . .
F92 F 0.8492(6) 0.5892(7) 0.9134(2) 0.0343(8) Uani 1 1 d . . .
F93 F 1.0298(7) 0.5388(6) 0.8713(2) 0.0343(8) Uani 1 1 d . . .
F94 F 1.0449(7) 0.3619(6) 0.8399(2) 0.0343(8) Uani 1 1 d . . .
F95 F 0.8720(7) 0.2413(6) 0.8512(2) 0.0343(8) Uani 1 1 d . . .
F96 F 0.6909(7) 0.2912(6) 0.8908(3) 0.0343(8) Uani 1 1 d . . .
F102 F 0.6875(7) 0.6043(5) 0.8570(2) 0.0303(8) Uani 1 1 d . . .
F103 F 0.5858(7) 0.7654(5) 0.8446(2) 0.0303(8) Uani 1 1 d . . .
F104 F 0.4324(7) 0.8327(5) 0.8988(2) 0.0303(8) Uani 1 1 d . . .
F105 F 0.3789(7) 0.7298(5) 0.9662(2) 0.0303(8) Uani 1 1 d . . .
F106 F 0.4864(7) 0.5694(5) 0.9809(2) 0.0303(8) Uani 1 1 d . . .
F112 F 0.7452(7) 0.3236(5) 0.9792(2) 0.0289(8) Uani 1 1 d . . .
F113 F 0.8382(7) 0.3225(5) 1.0543(2) 0.0289(8) Uani 1 1 d . . .
F114 F 0.8716(6) 0.4848(5) 1.0967(2) 0.0289(8) Uani 1 1 d . . .
F115 F 0.8133(6) 0.6494(5) 1.0600(2) 0.0289(8) Uani 1 1 d . . .
F116 F 0.7139(7) 0.6534(5) 0.9880(2) 0.0289(8) Uani 1 1 d . . .
B11 B 0.4330(10) 0.3839(9) 0.9198(4) 0.0153(12) Uani 1 1 d . . .
B12 B 0.6550(10) 0.4797(8) 0.9345(4) 0.0153(12) Uani 1 1 d . . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O2 2.272(5) . ?
Pb1 O1 2.273(4) . ?
Pb1 N201 2.455(5) . ?
Pb1 Se1 3.1153(12) . ?
Pb2 O2 2.260(4) . ?
Pb2 O1 2.318(5) . ?
Pb2 N202 2.475(5) . ?
Pb2 Se2 3.1504(12) . ?
Se1 C205 1.949(13) . ?
Se1 C204 1.955(13) . ?
Se2 C255 1.917(13) . ?
Se2 C254 1.970(13) . ?
C201 C202 1.521(17) . ?
C201 H20A 0.98 . ?
C201 H20B 0.98 . ?
C201 H20C 0.98 . ?
C202 O1 1.465(13) . ?
C202 C204 1.506(18) . ?
C202 C203 1.511(14) . ?
C203 H20D 0.98 . ?
C203 H20E 0.98 . ?
C203 H20F 0.98 . ?
C204 H20G 0.99 . ?
C204 H20H 0.99 . ?
C205 C206 1.373(18) . ?
C205 C210 1.405(18) . ?
C206 C207 1.415(19) . ?
C206 H206 0.95 . ?
C207 C208 1.357(18) . ?
C207 H207 0.95 . ?
C208 C209 1.399(17) . ?
C208 H208 0.95 . ?
C209 C210 1.393(19) . ?
C209 H209 0.95 . ?
C210 C211 1.521(13) . ?
C211 N201 1.524(12) . ?
C211 H21A 0.99 . ?
C211 H21B 0.99 . ?
C212 N201 1.469(12) . ?
C212 H21C 0.98 . ?
C212 H21D 0.98 . ?
C212 H21E 0.98 . ?
C213 N201 1.453(13) . ?
C213 H21F 0.98 . ?
C213 H21G 0.98 . ?
C213 H21H 0.98 . ?
C251 C252 1.580(18) . ?
C251 H25A 0.98 . ?
C251 H25B 0.98 . ?
C251 H25C 0.98 . ?
C252 C253 1.481(19) . ?
C252 C254 1.531(18) . ?
C252 O2 1.600(13) . ?
C253 H25D 0.98 . ?
C253 H25E 0.98 . ?
C253 H25F 0.98 . ?
C254 H25G 0.99 . ?
C254 H25H 0.99 . ?
C255 C256 1.34(2) . ?
C255 C260 1.40(2) . ?
C256 C257 1.412(17) . ?
C256 H256 0.95 . ?
C257 C258 1.34(2) . ?
C257 H257 0.95 . ?
C258 C259 1.36(2) . ?
C258 H258 0.95 . ?
C259 C260 1.437(17) . ?
C259 H259 0.95 . ?
C260 C261 1.564(18) . ?
C261 N202 1.459(13) . ?
C261 H26A 0.99 . ?
C261 H26B 0.99 . ?
C262 N202 1.561(14) . ?
C262 H26C 0.98 . ?
C262 H26D 0.98 . ?
C262 H26E 0.98 . ?
C263 N202 1.5132 . ?
C263 H26F 0.98 . ?
C263 H26G 0.98 . ?
C263 H26H 0.98 . ?
C1 C2 1.398(17) . ?
C1 C6 1.402(19) . ?
C1 B1 1.584(18) . ?
C2 F2 1.320(15) . ?
C2 C3 1.378(17) . ?
C3 F3 1.330(15) . ?
C3 C4 1.385(18) . ?
C4 F4 1.340(15) . ?
C4 C5 1.376(18) . ?
C5 F5 1.314(15) . ?
C5 C6 1.417(18) . ?
C6 F6 1.353(15) . ?
C11 C12 1.36(2) . ?
C11 C16 1.429(19) . ?
C11 B1 1.631(18) . ?
C12 F12 1.354(15) . ?
C12 C13 1.417(18) . ?
C13 F13 1.340(17) . ?
C13 C14 1.450(19) . ?
C14 F14 1.317(15) . ?
C14 C15 1.43(2) . ?
C15 F15 1.278(15) . ?
C15 C16 1.380(18) . ?
C16 F16 1.334(16) . ?
C21 C22 1.357(18) . ?
C21 C26 1.448(19) . ?
C21 B1 1.651(17) . ?
C22 C23 1.348(18) . ?
C22 F22 1.357(16) . ?
C23 F23 1.388(15) . ?
C23 C24 1.398(18) . ?
C24 F24 1.362(15) . ?
C24 C25 1.372(18) . ?
C25 F25 1.291(16) . ?
C25 C26 1.383(18) . ?
C26 F26 1.303(16) . ?
C31 C32 1.376(18) . ?
C31 C36 1.395(18) . ?
C31 B2 1.671(17) . ?
C32 C33 1.376(17) . ?
C32 F32 1.382(15) . ?
C33 C34 1.301(18) . ?
C33 F33 1.360(15) . ?
C34 F34 1.373(14) . ?
C34 C35 1.451(18) . ?
C35 F35 1.300(15) . ?
C35 C36 1.387(17) . ?
C36 F36 1.325(15) . ?
C41 C42 1.359(17) . ?
C41 C46 1.416(17) . ?
C41 B2 1.647(17) . ?
C42 F42 1.341(14) . ?
C42 C43 1.435(17) . ?
C43 F43 1.360(14) . ?
C43 C44 1.379(17) . ?
C44 F44 1.308(13) . ?
C44 C45 1.386(17) . ?
C45 F45 1.368(14) . ?
C45 C46 1.381(17) . ?
C46 F46 1.317(14) . ?
C51 C52 1.370(17) . ?
C51 C56 1.384(18) . ?
C51 B2 1.702(18) . ?
C52 F52 1.359(15) . ?
C52 C53 1.380(17) . ?
C53 F53 1.372(15) . ?
C53 C54 1.384(18) . ?
C54 F54 1.318(15) . ?
C54 C55 1.385(17) . ?
C55 F55 1.321(15) . ?
C55 C56 1.356(17) . ?
C56 F56 1.368(15) . ?
N1 B2 1.613(15) . ?
N1 B1 1.656(15) . ?
N1 H1A 0.92 . ?
N1 H1B 0.92 . ?
C61 C62 1.356(15) . ?
C61 C66 1.377(16) . ?
C61 B11 1.656(16) . ?
C62 C63 1.361(15) . ?
C62 F62 1.371(13) . ?
C63 F63 1.330(13) . ?
C63 C64 1.430(15) . ?
C64 F64 1.311(15) . ?
C64 C65 1.383(16) . ?
C65 F65 1.370(13) . ?
C65 C66 1.395(16) . ?
C66 F66 1.370(13) . ?
C71 C72 1.378(18) . ?
C71 C76 1.388(18) . ?
C71 B11 1.651(16) . ?
C72 F72 1.391(15) . ?
C72 C73 1.401(16) . ?
C73 F73 1.333(15) . ?
C73 C74 1.408(18) . ?
C74 C75 1.328(18) . ?
C74 F74 1.366(14) . ?
C75 F75 1.312(15) . ?
C75 C76 1.420(16) . ?
C76 F76 1.351(15) . ?
C81 C82 1.374(18) . ?
C81 C86 1.397(18) . ?
C81 B11 1.670(17) . ?
C82 F82 1.351(15) . ?
C82 C83 1.355(17) . ?
C83 F83 1.318(15) . ?
C83 C84 1.453(18) . ?
C84 F84 1.309(14) . ?
C84 C85 1.318(18) . ?
C85 F85 1.353(15) . ?
C85 C86 1.406(17) . ?
C86 F86 1.335(15) . ?
C91 C92 1.365(18) . ?
C91 C96 1.371(18) . ?
C91 B12 1.686(17) . ?
C92 F92 1.371(16) . ?
C92 C93 1.405(16) . ?
C93 F93 1.310(15) . ?
C93 C94 1.395(18) . ?
C94 F94 1.288(14) . ?
C94 C95 1.383(18) . ?
C95 F95 1.356(15) . ?
C95 C96 1.399(17) . ?
C96 F96 1.312(15) . ?
C101 C106 1.386(16) . ?
C101 C102 1.408(17) . ?
C101 B12 1.670(17) . ?
C102 F102 1.334(14) . ?
C102 C103 1.364(17) . ?
C103 F103 1.331(14) . ?
C103 C104 1.382(17) . ?
C104 F104 1.319(14) . ?
C104 C105 1.433(17) . ?
C105 F105 1.333(14) . ?
C105 C106 1.348(18) . ?
C106 F106 1.346(14) . ?
C111 C112 1.393(17) . ?
C111 C116 1.399(17) . ?
C111 B12 1.673(17) . ?
C112 F112 1.378(15) . ?
C112 C113 1.398(17) . ?
C113 F113 1.341(14) . ?
C113 C114 1.368(17) . ?
C114 C115 1.370(16) . ?
C114 F114 1.393(14) . ?
C115 F115 1.305(14) . ?
C115 C116 1.398(17) . ?
C116 F116 1.300(14) . ?
N2 B12 1.623(15) . ?
N2 B11 1.628(15) . ?
N2 H2A 0.92 . ?
N2 H2B 0.92 . ?


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
O2 Pb1 O1 68.03(13) . . ?
O2 Pb1 N201 87.55(15) . . ?
O1 Pb1 N201 113.94(19) . . ?
O2 Pb1 Se1 127.32(12) . . ?
O1 Pb1 Se1 69.43(12) . . ?
N201 Pb1 Se1 82.53(11) . . ?
O2 Pb2 O1 67.46(13) . . ?
O2 Pb2 N202 109.22(18) . . ?
O1 Pb2 N202 94.98(17) . . ?
O2 Pb2 Se2 69.92(12) . . ?
O1 Pb2 Se2 132.08(11) . . ?
N202 Pb2 Se2 79.16(10) . . ?
C205 Se1 C204 98.7(6) . . ?
C205 Se1 Pb1 97.7(4) . . ?
C204 Se1 Pb1 90.0(4) . . ?
C255 Se2 C254 98.8(6) . . ?
C255 Se2 Pb2 98.6(4) . . ?
C254 Se2 Pb2 89.5(4) . . ?
C202 C201 H20A 109.5 . . ?
C202 C201 H20B 109.5 . . ?
H20A C201 H20B 109.5 . . ?
C202 C201 H20C 109.5 . . ?
H20A C201 H20C 109.5 . . ?
H20B C201 H20C 109.5 . . ?
O1 C202 C204 107.9(10) . . ?
O1 C202 C203 110.2(9) . . ?
C204 C202 C203 112.6(11) . . ?
O1 C202 C201 107.2(9) . . ?
C204 C202 C201 109.9(10) . . ?
C203 C202 C201 108.8(11) . . ?
C202 C203 H20D 109.5 . . ?
C202 C203 H20E 109.5 . . ?
H20D C203 H20E 109.5 . . ?
C202 C203 H20F 109.5 . . ?
H20D C203 H20F 109.5 . . ?
H20E C203 H20F 109.5 . . ?
C202 C204 Se1 116.2(9) . . ?
C202 C204 H20G 108.2 . . ?
Se1 C204 H20G 108.2 . . ?
C202 C204 H20H 108.2 . . ?
Se1 C204 H20H 108.2 . . ?
H20G C204 H20H 107.4 . . ?
C206 C205 C210 121.7(12) . . ?
C206 C205 Se1 118.3(10) . . ?
C210 C205 Se1 118.8(9) . . ?
C205 C206 C207 119.8(12) . . ?
C205 C206 H206 120.1 . . ?
C207 C206 H206 120.1 . . ?
C208 C207 C206 117.3(12) . . ?
C208 C207 H207 121.3 . . ?
C206 C207 H207 121.3 . . ?
C207 C208 C209 123.5(13) . . ?
C207 C208 H208 118.3 . . ?
C209 C208 H208 118.3 . . ?
C210 C209 C208 118.9(12) . . ?
C210 C209 H209 120.5 . . ?
C208 C209 H209 120.5 . . ?
C209 C210 C205 117.6(11) . . ?
C209 C210 C211 117.2(11) . . ?
C205 C210 C211 124.9(11) . . ?
C210 C211 N201 117.7(9) . . ?
C210 C211 H21A 107.9 . . ?
N201 C211 H21A 107.9 . . ?
C210 C211 H21B 107.9 . . ?
N201 C211 H21B 107.9 . . ?
H21A C211 H21B 107.2 . . ?
N201 C212 H21C 109.5 . . ?
N201 C212 H21D 109.5 . . ?
H21C C212 H21D 109.5 . . ?
N201 C212 H21E 109.5 . . ?
H21C C212 H21E 109.5 . . ?
H21D C212 H21E 109.5 . . ?
N201 C213 H21F 109.5 . . ?
N201 C213 H21G 109.5 . . ?
H21F C213 H21G 109.5 . . ?
N201 C213 H21H 109.5 . . ?
H21F C213 H21H 109.5 . . ?
H21G C213 H21H 109.5 . . ?
C252 C251 H25A 109.5 . . ?
C252 C251 H25B 109.5 . . ?
H25A C251 H25B 109.5 . . ?
C252 C251 H25C 109.5 . . ?
H25A C251 H25C 109.5 . . ?
H25B C251 H25C 109.5 . . ?
C253 C252 C254 114.4(11) . . ?
C253 C252 C251 109.4(11) . . ?
C254 C252 C251 104.7(10) . . ?
C253 C252 O2 114.3(9) . . ?
C254 C252 O2 107.2(10) . . ?
C251 C252 O2 106.1(9) . . ?
C252 C253 H25D 109.5 . . ?
C252 C253 H25E 109.5 . . ?
H25D C253 H25E 109.5 . . ?
C252 C253 H25F 109.5 . . ?
H25D C253 H25F 109.5 . . ?
H25E C253 H25F 109.5 . . ?
C252 C254 Se2 114.2(8) . . ?
C252 C254 H25G 108.7 . . ?
Se2 C254 H25G 108.7 . . ?
C252 C254 H25H 108.7 . . ?
Se2 C254 H25H 108.7 . . ?
H25G C254 H25H 107.6 . . ?
C256 C255 C260 119.2(12) . . ?
C256 C255 Se2 121.0(11) . . ?
C260 C255 Se2 119.8(10) . . ?
C255 C256 C257 121.4(14) . . ?
C255 C256 H256 119.3 . . ?
C257 C256 H256 119.3 . . ?
C258 C257 C256 120.5(14) . . ?
C258 C257 H257 119.7 . . ?
C256 C257 H257 119.7 . . ?
C257 C258 C259 120.0(13) . . ?
C257 C258 H258 120 . . ?
C259 C258 H258 120 . . ?
C258 C259 C260 120.4(13) . . ?
C258 C259 H259 119.8 . . ?
C260 C259 H259 119.8 . . ?
C255 C260 C259 118.3(13) . . ?
C255 C260 C261 122.7(11) . . ?
C259 C260 C261 118.8(12) . . ?
N202 C261 C260 114.0(9) . . ?
N202 C261 H26A 108.7 . . ?
C260 C261 H26A 108.7 . . ?
N202 C261 H26B 108.7 . . ?
C260 C261 H26B 108.7 . . ?
H26A C261 H26B 107.6 . . ?
N202 C262 H26C 109.5 . . ?
N202 C262 H26D 109.5 . . ?
H26C C262 H26D 109.5 . . ?
N202 C262 H26E 109.5 . . ?
H26C C262 H26E 109.5 . . ?
H26D C262 H26E 109.5 . . ?
N202 C263 H26F 109.5 . . ?
N202 C263 H26G 109.5 . . ?
H26F C263 H26G 109.5 . . ?
N202 C263 H26H 109.5 . . ?
H26F C263 H26H 109.5 . . ?
H26G C263 H26H 109.5 . . ?
C213 N201 C212 110.4(7) . . ?
C213 N201 C211 107.6(8) . . ?
C212 N201 C211 103.2(7) . . ?
C213 N201 Pb1 115.0(6) . . ?
C212 N201 Pb1 103.2(5) . . ?
C211 N201 Pb1 116.6(5) . . ?
C261 N202 C263 103.9(5) . . ?
C261 N202 C262 108.8(8) . . ?
C263 N202 C262 107.9(5) . . ?
C261 N202 Pb2 120.9(6) . . ?
C263 N202 Pb2 101.1(3) . . ?
C262 N202 Pb2 112.8(5) . . ?
C202 O1 Pb1 115.2(5) . . ?
C202 O1 Pb2 126.7(6) . . ?
Pb1 O1 Pb2 110.52(18) . . ?
C252 O2 Pb2 106.9(5) . . ?
C252 O2 Pb1 122.8(5) . . ?
Pb2 O2 Pb1 112.71(18) . . ?
C2 C1 C6 110.9(12) . . ?
C2 C1 B1 128.3(12) . . ?
C6 C1 B1 119.3(10) . . ?
F2 C2 C3 113.9(11) . . ?
F2 C2 C1 120.6(11) . . ?
C3 C2 C1 125.4(12) . . ?
F3 C3 C2 121.3(12) . . ?
F3 C3 C4 118.0(11) . . ?
C2 C3 C4 120.6(12) . . ?
F4 C4 C5 119.6(11) . . ?
F4 C4 C3 121.9(11) . . ?
C5 C4 C3 118.4(12) . . ?
F5 C5 C4 120.3(11) . . ?
F5 C5 C6 121.5(11) . . ?
C4 C5 C6 118.0(12) . . ?
F6 C6 C1 119.6(11) . . ?
F6 C6 C5 114.2(11) . . ?
C1 C6 C5 126.2(12) . . ?
C12 C11 C16 114.2(12) . . ?
C12 C11 B1 116.6(12) . . ?
C16 C11 B1 128.5(12) . . ?
F12 C12 C11 122.3(11) . . ?
F12 C12 C13 112.2(12) . . ?
C11 C12 C13 125.4(13) . . ?
F13 C13 C12 123.3(12) . . ?
F13 C13 C14 118.9(11) . . ?
C12 C13 C14 117.6(13) . . ?
F14 C14 C15 121.8(12) . . ?
F14 C14 C13 118.9(12) . . ?
C15 C14 C13 118.9(11) . . ?
F15 C15 C16 123.4(12) . . ?
F15 C15 C14 118.9(11) . . ?
C16 C15 C14 117.6(12) . . ?
F16 C16 C15 114.6(12) . . ?
F16 C16 C11 119.5(11) . . ?
C15 C16 C11 125.9(13) . . ?
C22 C21 C26 112.9(11) . . ?
C22 C21 B1 122.0(12) . . ?
C26 C21 B1 125.0(11) . . ?
C23 C22 F22 115.4(12) . . ?
C23 C22 C21 125.6(13) . . ?
F22 C22 C21 119.0(11) . . ?
C22 C23 F23 123.5(12) . . ?
C22 C23 C24 119.6(12) . . ?
F23 C23 C24 116.8(11) . . ?
F24 C24 C25 120.6(11) . . ?
F24 C24 C23 119.3(11) . . ?
C25 C24 C23 120.0(12) . . ?
F25 C25 C24 121.3(11) . . ?
F25 C25 C26 120.7(12) . . ?
C24 C25 C26 117.9(12) . . ?
F26 C26 C25 114.6(12) . . ?
F26 C26 C21 121.6(11) . . ?
C25 C26 C21 123.9(12) . . ?
C32 C31 C36 113.4(11) . . ?
C32 C31 B2 128.9(11) . . ?
C36 C31 B2 117.6(10) . . ?
C31 C32 C33 124.7(12) . . ?
C31 C32 F32 120.4(10) . . ?
C33 C32 F32 114.8(11) . . ?
C34 C33 F33 119.2(11) . . ?
C34 C33 C32 120.5(12) . . ?
F33 C33 C32 120.1(11) . . ?
C33 C34 F34 123.6(11) . . ?
C33 C34 C35 120.2(11) . . ?
F34 C34 C35 115.6(11) . . ?
F35 C35 C36 121.8(11) . . ?
F35 C35 C34 122.4(10) . . ?
C36 C35 C34 115.8(11) . . ?
F36 C36 C35 114.6(11) . . ?
F36 C36 C31 120.5(10) . . ?
C35 C36 C31 124.9(12) . . ?
C42 C41 C46 115.7(11) . . ?
C42 C41 B2 125.6(11) . . ?
C46 C41 B2 118.7(11) . . ?
F42 C42 C41 123.3(11) . . ?
F42 C42 C43 114.3(10) . . ?
C41 C42 C43 122.3(12) . . ?
F43 C43 C44 120.4(10) . . ?
F43 C43 C42 119.0(11) . . ?
C44 C43 C42 120.6(11) . . ?
F44 C44 C43 120.4(10) . . ?
F44 C44 C45 122.2(11) . . ?
C43 C44 C45 117.4(11) . . ?
F45 C45 C46 121.2(11) . . ?
F45 C45 C44 117.3(10) . . ?
C46 C45 C44 121.5(11) . . ?
F46 C46 C45 116.7(11) . . ?
F46 C46 C41 120.7(11) . . ?
C45 C46 C41 122.4(11) . . ?
C52 C51 C56 113.0(11) . . ?
C52 C51 B2 128.3(11) . . ?
C56 C51 B2 118.5(10) . . ?
F52 C52 C51 120.8(11) . . ?
F52 C52 C53 114.9(10) . . ?
C51 C52 C53 124.3(12) . . ?
F53 C53 C52 120.0(11) . . ?
F53 C53 C54 120.1(11) . . ?
C52 C53 C54 119.8(11) . . ?
F54 C54 C53 120.7(11) . . ?
F54 C54 C55 121.2(11) . . ?
C53 C54 C55 118.0(11) . . ?
F55 C55 C56 123.2(11) . . ?
F55 C55 C54 117.9(11) . . ?
C56 C55 C54 119.0(12) . . ?
C55 C56 F56 115.2(11) . . ?
C55 C56 C51 125.9(12) . . ?
F56 C56 C51 118.9(11) . . ?
B2 N1 B1 134.8(8) . . ?
B2 N1 H1A 103.5 . . ?
B1 N1 H1A 103.5 . . ?
B2 N1 H1B 103.5 . . ?
B1 N1 H1B 103.5 . . ?
H1A N1 H1B 105.3 . . ?
C1 B1 C11 106.5(9) . . ?
C1 B1 C21 112.7(10) . . ?
C11 B1 C21 113.3(10) . . ?
C1 B1 N1 106.2(9) . . ?
C11 B1 N1 112.0(10) . . ?
C21 B1 N1 106.0(9) . . ?
N1 B2 C41 111.2(9) . . ?
N1 B2 C31 108.3(9) . . ?
C41 B2 C31 113.5(10) . . ?
N1 B2 C51 110.9(9) . . ?
C41 B2 C51 111.5(9) . . ?
C31 B2 C51 101.0(9) . . ?
C62 C61 C66 113.1(10) . . ?
C62 C61 B11 121.1(10) . . ?
C66 C61 B11 125.5(10) . . ?
C61 C62 C63 127.3(11) . . ?
C61 C62 F62 118.7(10) . . ?
C63 C62 F62 114.0(9) . . ?
F63 C63 C62 124.2(10) . . ?
F63 C63 C64 117.0(10) . . ?
C62 C63 C64 118.7(10) . . ?
F64 C64 C65 122.4(10) . . ?
F64 C64 C63 121.6(10) . . ?
C65 C64 C63 115.9(11) . . ?
F65 C65 C64 117.3(10) . . ?
F65 C65 C66 121.8(10) . . ?
C64 C65 C66 121.0(11) . . ?
F66 C66 C61 123.4(10) . . ?
F66 C66 C65 112.7(10) . . ?
C61 C66 C65 123.9(10) . . ?
C72 C71 C76 111.2(11) . . ?
C72 C71 B11 129.5(11) . . ?
C76 C71 B11 118.7(11) . . ?
C71 C72 F72 120.7(10) . . ?
C71 C72 C73 126.3(12) . . ?
F72 C72 C73 113.0(11) . . ?
F73 C73 C72 120.1(11) . . ?
F73 C73 C74 122.4(10) . . ?
C72 C73 C74 117.4(12) . . ?
C75 C74 F74 123.4(11) . . ?
C75 C74 C73 120.5(11) . . ?
F74 C74 C73 116.0(11) . . ?
F75 C75 C74 119.9(11) . . ?
F75 C75 C76 122.0(11) . . ?
C74 C75 C76 118.2(12) . . ?
F76 C76 C71 119.3(10) . . ?
F76 C76 C75 114.2(11) . . ?
C71 C76 C75 126.3(12) . . ?
C82 C81 C86 114.4(11) . . ?
C82 C81 B11 119.3(11) . . ?
C86 C81 B11 126.3(11) . . ?
F82 C82 C83 112.9(11) . . ?
F82 C82 C81 120.8(11) . . ?
C83 C82 C81 126.3(12) . . ?
F83 C83 C82 124.7(12) . . ?
F83 C83 C84 117.0(10) . . ?
C82 C83 C84 118.3(11) . . ?
F84 C84 C85 123.8(11) . . ?
F84 C84 C83 119.8(11) . . ?
C85 C84 C83 116.1(11) . . ?
C84 C85 F85 118.5(11) . . ?
C84 C85 C86 124.5(12) . . ?
F85 C85 C86 117.0(11) . . ?
F86 C86 C81 120.8(11) . . ?
F86 C86 C85 118.8(11) . . ?
C81 C86 C85 120.3(12) . . ?
C92 C91 C96 115.3(11) . . ?
C92 C91 B12 117.9(10) . . ?
C96 C91 B12 126.2(11) . . ?
C91 C92 F92 120.6(10) . . ?
C91 C92 C93 126.5(12) . . ?
F92 C92 C93 112.9(11) . . ?
F93 C93 C94 119.7(11) . . ?
F93 C93 C92 122.7(11) . . ?
C94 C93 C92 117.5(12) . . ?
F94 C94 C95 121.2(11) . . ?
F94 C94 C93 122.5(12) . . ?
C95 C94 C93 116.4(11) . . ?
F95 C95 C94 119.1(11) . . ?
F95 C95 C96 116.7(11) . . ?
C94 C95 C96 124.2(12) . . ?
F96 C96 C91 122.2(11) . . ?
F96 C96 C95 117.6(11) . . ?
C91 C96 C95 120.1(12) . . ?
C106 C101 C102 114.7(11) . . ?
C106 C101 B12 118.0(10) . . ?
C102 C101 B12 127.3(10) . . ?
F102 C102 C103 116.8(11) . . ?
F102 C102 C101 121.1(11) . . ?
C103 C102 C101 121.9(11) . . ?
F103 C103 C102 120.0(10) . . ?
F103 C103 C104 118.0(11) . . ?
C102 C103 C104 121.5(11) . . ?
F104 C104 C103 122.6(11) . . ?
F104 C104 C105 119.6(10) . . ?
C103 C104 C105 117.7(11) . . ?
F105 C105 C106 123.3(11) . . ?
F105 C105 C104 118.5(11) . . ?
C106 C105 C104 118.2(11) . . ?
F106 C106 C105 116.0(10) . . ?
F106 C106 C101 118.3(11) . . ?
C105 C106 C101 125.6(12) . . ?
C112 C111 C116 114.2(11) . . ?
C112 C111 B12 117.8(10) . . ?
C116 C111 B12 127.9(10) . . ?
F112 C112 C111 119.8(11) . . ?
F112 C112 C113 115.5(10) . . ?
C111 C112 C113 124.7(11) . . ?
F113 C113 C114 121.9(11) . . ?
F113 C113 C112 120.9(11) . . ?
C114 C113 C112 117.2(11) . . ?
C113 C114 C115 122.1(11) . . ?
C113 C114 F114 117.9(10) . . ?
C115 C114 F114 120.0(10) . . ?
F115 C115 C114 120.3(10) . . ?
F115 C115 C116 120.9(10) . . ?
C114 C115 C116 118.8(11) . . ?
F116 C116 C115 115.4(11) . . ?
F116 C116 C111 121.7(11) . . ?
C115 C116 C111 122.9(11) . . ?
B12 N2 B11 135.9(8) . . ?
B12 N2 H2A 103.2 . . ?
B11 N2 H2A 103.2 . . ?
B12 N2 H2B 103.2 . . ?
B11 N2 H2B 103.2 . . ?
H2A N2 H2B 105.2 . . ?
N2 B11 C71 110.3(9) . . ?
N2 B11 C61 109.7(8) . . ?
C71 B11 C61 103.2(9) . . ?
N2 B11 C81 108.5(9) . . ?
C71 B11 C81 113.2(9) . . ?
C61 B11 C81 111.9(9) . . ?
N2 B12 C101 108.2(9) . . ?
N2 B12 C111 106.7(9) . . ?
C101 B12 C111 110.6(9) . . ?
N2 B12 C91 111.8(9) . . ?
C101 B12 C91 115.5(9) . . ?
C111 B12 C91 103.7(9) . . ?


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
O2 Pb1 Se1 C205 -43.5(4) . . . . ?
O1 Pb1 Se1 C205 -81.5(4) . . . . ?
N201 Pb1 Se1 C205 37.6(4) . . . . ?
O2 Pb1 Se1 C204 55.2(4) . . . . ?
O1 Pb1 Se1 C204 17.3(4) . . . . ?
N201 Pb1 Se1 C204 136.4(4) . . . . ?
O2 Pb2 Se2 C255 -74.0(5) . . . . ?
O1 Pb2 Se2 C255 -45.6(5) . . . . ?
N202 Pb2 Se2 C255 41.3(5) . . . . ?
O2 Pb2 Se2 C254 24.8(4) . . . . ?
O1 Pb2 Se2 C254 53.2(4) . . . . ?
N202 Pb2 Se2 C254 140.1(4) . . . . ?
O1 C202 C204 Se1 -51.0(12) . . . . ?
C203 C202 C204 Se1 70.9(13) . . . . ?
C201 C202 C204 Se1 -167.7(9) . . . . ?
C205 Se1 C204 C202 109.3(10) . . . . ?
Pb1 Se1 C204 C202 11.6(9) . . . . ?
C204 Se1 C205 C206 46.2(12) . . . . ?
Pb1 Se1 C205 C206 137.3(11) . . . . ?
C204 Se1 C205 C210 -145.8(11) . . . . ?
Pb1 Se1 C205 C210 -54.6(11) . . . . ?
C210 C205 C206 C207 11(2) . . . . ?
Se1 C205 C206 C207 178.6(10) . . . . ?
C205 C206 C207 C208 -9(2) . . . . ?
C206 C207 C208 C209 7(2) . . . . ?
C207 C208 C209 C210 -6(2) . . . . ?
C208 C209 C210 C205 8(2) . . . . ?
C208 C209 C210 C211 -178.8(12) . . . . ?
C206 C205 C210 C209 -10(2) . . . . ?
Se1 C205 C210 C209 -178.0(10) . . . . ?
C206 C205 C210 C211 176.7(13) . . . . ?
Se1 C205 C210 C211 9.1(18) . . . . ?
C209 C210 C211 N201 -97.6(14) . . . . ?
C205 C210 C211 N201 75.3(16) . . . . ?
C253 C252 C254 Se2 75.2(13) . . . . ?
C251 C252 C254 Se2 -165.1(9) . . . . ?
O2 C252 C254 Se2 -52.6(11) . . . . ?
C255 Se2 C254 C252 106.7(10) . . . . ?
Pb2 Se2 C254 C252 8.1(9) . . . . ?
C254 Se2 C255 C256 40.2(12) . . . . ?
Pb2 Se2 C255 C256 131.0(11) . . . . ?
C254 Se2 C255 C260 -139.4(11) . . . . ?
Pb2 Se2 C255 C260 -48.6(11) . . . . ?
C260 C255 C256 C257 2(2) . . . . ?
Se2 C255 C256 C257 -178.0(10) . . . . ?
C255 C256 C257 C258 -1(2) . . . . ?
C256 C257 C258 C259 -3(2) . . . . ?
C257 C258 C259 C260 5(2) . . . . ?
C256 C255 C260 C259 1(2) . . . . ?
Se2 C255 C260 C259 -179.8(10) . . . . ?
C256 C255 C260 C261 174.6(12) . . . . ?
Se2 C255 C260 C261 -5.8(18) . . . . ?
C258 C259 C260 C255 -4(2) . . . . ?
C258 C259 C260 C261 -178.1(12) . . . . ?
C255 C260 C261 N202 85.2(15) . . . . ?
C259 C260 C261 N202 -100.9(13) . . . . ?
C210 C211 N201 C213 58.7(12) . . . . ?
C210 C211 N201 C212 175.4(10) . . . . ?
C210 C211 N201 Pb1 -72.2(11) . . . . ?
O2 Pb1 N201 C213 11.6(7) . . . . ?
O1 Pb1 N201 C213 -53.0(7) . . . . ?
Se1 Pb1 N201 C213 -116.5(6) . . . . ?
O2 Pb1 N201 C212 -108.7(6) . . . . ?
O1 Pb1 N201 C212 -173.3(5) . . . . ?
Se1 Pb1 N201 C212 123.1(6) . . . . ?
O2 Pb1 N201 C211 138.9(5) . . . . ?
O1 Pb1 N201 C211 74.3(6) . . . . ?
Se1 Pb1 N201 C211 10.8(5) . . . . ?
C260 C261 N202 C263 179.3(8) . . . . ?
C260 C261 N202 C262 64.5(12) . . . . ?
C260 C261 N202 Pb2 -68.4(11) . . . . ?
O2 Pb2 N202 C261 70.2(7) . . . . ?
O1 Pb2 N202 C261 138.1(6) . . . . ?
Se2 Pb2 N202 C261 6.1(6) . . . . ?
O2 Pb2 N202 C263 -175.98(14) . . . . ?
O1 Pb2 N202 C263 -108.13(11) . . . . ?
Se2 Pb2 N202 C263 120.0(3) . . . . ?
O2 Pb2 N202 C262 -61.1(6) . . . . ?
O1 Pb2 N202 C262 6.8(6) . . . . ?
Se2 Pb2 N202 C262 -125.2(5) . . . . ?
C204 C202 O1 Pb1 78.9(9) . . . . ?
C203 C202 O1 Pb1 -44.5(11) . . . . ?
C201 C202 O1 Pb1 -162.8(7) . . . . ?
C204 C202 O1 Pb2 -134.8(8) . . . . ?
C203 C202 O1 Pb2 101.9(10) . . . . ?
C201 C202 O1 Pb2 -16.4(12) . . . . ?
O2 Pb1 O1 C202 160.4(6) . . . . ?
N201 Pb1 O1 C202 -122.9(6) . . . . ?
Se1 Pb1 O1 C202 -51.5(6) . . . . ?
O2 Pb1 O1 Pb2 8.7(2) . . . . ?
N201 Pb1 O1 Pb2 85.4(2) . . . . ?
Se1 Pb1 O1 Pb2 156.9(2) . . . . ?
O2 Pb2 O1 C202 -156.4(6) . . . . ?
N202 Pb2 O1 C202 94.8(7) . . . . ?
Se2 Pb2 O1 C202 174.7(6) . . . . ?
O2 Pb2 O1 Pb1 -8.8(2) . . . . ?
N202 Pb2 O1 Pb1 -117.53(15) . . . . ?
Se2 Pb2 O1 Pb1 -37.7(3) . . . . ?
C253 C252 O2 Pb2 -42.1(11) . . . . ?
C254 C252 O2 Pb2 85.8(9) . . . . ?
C251 C252 O2 Pb2 -162.8(7) . . . . ?
C253 C252 O2 Pb1 90.4(10) . . . . ?
C254 C252 O2 Pb1 -141.7(7) . . . . ?
C251 C252 O2 Pb1 -30.3(11) . . . . ?
O1 Pb2 O2 C252 146.7(5) . . . . ?
N202 Pb2 O2 C252 -125.9(5) . . . . ?
Se2 Pb2 O2 C252 -55.7(5) . . . . ?
O1 Pb2 O2 Pb1 8.9(3) . . . . ?
N202 Pb2 O2 Pb1 96.3(2) . . . . ?
Se2 Pb2 O2 Pb1 166.5(2) . . . . ?
O1 Pb1 O2 C252 -139.2(6) . . . . ?
N201 Pb1 O2 C252 103.7(6) . . . . ?
Se1 Pb1 O2 C252 -177.6(6) . . . . ?
O1 Pb1 O2 Pb2 -9.1(3) . . . . ?
N201 Pb1 O2 Pb2 -126.12(14) . . . . ?
Se1 Pb1 O2 Pb2 -47.4(2) . . . . ?
C6 C1 C2 F2 -179.9(11) . . . . ?
B1 C1 C2 F2 13.9(19) . . . . ?
C6 C1 C2 C3 -4.2(18) . . . . ?
B1 C1 C2 C3 -170.4(12) . . . . ?
F2 C2 C3 F3 -2.6(17) . . . . ?
C1 C2 C3 F3 -178.6(11) . . . . ?
F2 C2 C3 C4 -177.8(11) . . . . ?
C1 C2 C3 C4 6(2) . . . . ?
F3 C3 C4 F4 2.2(18) . . . . ?
C2 C3 C4 F4 177.4(12) . . . . ?
F3 C3 C4 C5 177.4(11) . . . . ?
C2 C3 C4 C5 -7.4(19) . . . . ?
F4 C4 C5 F5 -3.5(18) . . . . ?
C3 C4 C5 F5 -178.8(11) . . . . ?
F4 C4 C5 C6 -177.8(11) . . . . ?
C3 C4 C5 C6 6.9(18) . . . . ?
C2 C1 C6 F6 -176.7(11) . . . . ?
B1 C1 C6 F6 -9.1(17) . . . . ?
C2 C1 C6 C5 4.0(18) . . . . ?
B1 C1 C6 C5 171.6(12) . . . . ?
F5 C5 C6 F6 0.8(17) . . . . ?
C4 C5 C6 F6 175.0(11) . . . . ?
F5 C5 C6 C1 -179.9(12) . . . . ?
C4 C5 C6 C1 -5.7(19) . . . . ?
C16 C11 C12 F12 -175.5(12) . . . . ?
B1 C11 C12 F12 -4.0(19) . . . . ?
C16 C11 C12 C13 2(2) . . . . ?
B1 C11 C12 C13 173.2(12) . . . . ?
F12 C12 C13 F13 -3.8(19) . . . . ?
C11 C12 C13 F13 178.7(13) . . . . ?
F12 C12 C13 C14 -178.8(11) . . . . ?
C11 C12 C13 C14 4(2) . . . . ?
F13 C13 C14 F14 6.5(18) . . . . ?
C12 C13 C14 F14 -178.3(11) . . . . ?
F13 C13 C14 C15 179.0(11) . . . . ?
C12 C13 C14 C15 -5.8(18) . . . . ?
F14 C14 C15 F15 -4(2) . . . . ?
C13 C14 C15 F15 -176.2(12) . . . . ?
F14 C14 C15 C16 174.7(12) . . . . ?
C13 C14 C15 C16 2.4(19) . . . . ?
F15 C15 C16 F16 -0.4(19) . . . . ?
C14 C15 C16 F16 -179.0(11) . . . . ?
F15 C15 C16 C11 -177.8(13) . . . . ?
C14 C15 C16 C11 4(2) . . . . ?
C12 C11 C16 F16 177.1(12) . . . . ?
B1 C11 C16 F16 7(2) . . . . ?
C12 C11 C16 C15 -6(2) . . . . ?
B1 C11 C16 C15 -175.9(12) . . . . ?
C26 C21 C22 C23 -3.7(19) . . . . ?
B1 C21 C22 C23 178.8(12) . . . . ?
C26 C21 C22 F22 178.3(11) . . . . ?
B1 C21 C22 F22 0.9(18) . . . . ?
F22 C22 C23 F23 -1.2(18) . . . . ?
C21 C22 C23 F23 -179.2(12) . . . . ?
F22 C22 C23 C24 -177.4(11) . . . . ?
C21 C22 C23 C24 5(2) . . . . ?
C22 C23 C24 F24 179.4(11) . . . . ?
F23 C23 C24 F24 3.0(17) . . . . ?
C22 C23 C24 C25 -3.6(19) . . . . ?
F23 C23 C24 C25 180.0(11) . . . . ?
F24 C24 C25 F25 -4.9(18) . . . . ?
C23 C24 C25 F25 178.1(11) . . . . ?
F24 C24 C25 C26 179.1(11) . . . . ?
C23 C24 C25 C26 2.2(18) . . . . ?
F25 C25 C26 F26 0.5(17) . . . . ?
C24 C25 C26 F26 176.4(11) . . . . ?
F25 C25 C26 C21 -177.6(11) . . . . ?
C24 C25 C26 C21 -1.6(19) . . . . ?
C22 C21 C26 F26 -175.7(11) . . . . ?
B1 C21 C26 F26 1.6(18) . . . . ?
C22 C21 C26 C25 2.2(18) . . . . ?
B1 C21 C26 C25 179.6(11) . . . . ?
C36 C31 C32 C33 0.2(18) . . . . ?
B2 C31 C32 C33 -176.5(12) . . . . ?
C36 C31 C32 F32 175.4(10) . . . . ?
B2 C31 C32 F32 -1.3(19) . . . . ?
C31 C32 C33 C34 -5.6(19) . . . . ?
F32 C32 C33 C34 178.9(11) . . . . ?
C31 C32 C33 F33 178.1(11) . . . . ?
F32 C32 C33 F33 2.6(16) . . . . ?
F33 C33 C34 F34 -4.2(18) . . . . ?
C32 C33 C34 F34 179.5(11) . . . . ?
F33 C33 C34 C35 -175.5(10) . . . . ?
C32 C33 C34 C35 8.2(18) . . . . ?
C33 C34 C35 F35 175.3(11) . . . . ?
F34 C34 C35 F35 3.3(17) . . . . ?
C33 C34 C35 C36 -5.6(17) . . . . ?
F34 C34 C35 C36 -177.6(10) . . . . ?
F35 C35 C36 F36 -1.9(17) . . . . ?
C34 C35 C36 F36 178.9(10) . . . . ?
F35 C35 C36 C31 179.3(11) . . . . ?
C34 C35 C36 C31 0.2(18) . . . . ?
C32 C31 C36 F36 -176.4(10) . . . . ?
B2 C31 C36 F36 0.7(16) . . . . ?
C32 C31 C36 C35 2.3(18) . . . . ?
B2 C31 C36 C35 179.4(11) . . . . ?
C46 C41 C42 F42 -177.9(11) . . . . ?
B2 C41 C42 F42 -0.5(19) . . . . ?
C46 C41 C42 C43 0.4(18) . . . . ?
B2 C41 C42 C43 177.9(11) . . . . ?
F42 C42 C43 F43 -2.3(16) . . . . ?
C41 C42 C43 F43 179.2(11) . . . . ?
F42 C42 C43 C44 178.9(11) . . . . ?
C41 C42 C43 C44 0.5(19) . . . . ?
F43 C43 C44 F44 0.4(17) . . . . ?
C42 C43 C44 F44 179.1(11) . . . . ?
F43 C43 C44 C45 179.9(11) . . . . ?
C42 C43 C44 C45 -1.4(17) . . . . ?
F44 C44 C45 F45 2.4(17) . . . . ?
C43 C44 C45 F45 -177.2(10) . . . . ?
F44 C44 C45 C46 -179.1(11) . . . . ?
C43 C44 C45 C46 1.4(18) . . . . ?
F45 C45 C46 F46 2.0(17) . . . . ?
C44 C45 C46 F46 -176.5(11) . . . . ?
F45 C45 C46 C41 178.0(11) . . . . ?
C44 C45 C46 C41 -0.5(19) . . . . ?
C42 C41 C46 F46 175.4(11) . . . . ?
B2 C41 C46 F46 -2.2(17) . . . . ?
C42 C41 C46 C45 -0.4(18) . . . . ?
B2 C41 C46 C45 -178.0(11) . . . . ?
C56 C51 C52 F52 179.3(10) . . . . ?
B2 C51 C52 F52 3.3(19) . . . . ?
C56 C51 C52 C53 0.2(18) . . . . ?
B2 C51 C52 C53 -175.8(11) . . . . ?
F52 C52 C53 F53 -1.6(16) . . . . ?
C51 C52 C53 F53 177.5(11) . . . . ?
F52 C52 C53 C54 -177.4(10) . . . . ?
C51 C52 C53 C54 1.8(19) . . . . ?
F53 C53 C54 F54 5.3(17) . . . . ?
C52 C53 C54 F54 -178.9(11) . . . . ?
F53 C53 C54 C55 -178.3(11) . . . . ?
C52 C53 C54 C55 -2.5(17) . . . . ?
F54 C54 C55 F55 -1.7(18) . . . . ?
C53 C54 C55 F55 -178.1(11) . . . . ?
F54 C54 C55 C56 177.7(11) . . . . ?
C53 C54 C55 C56 1.3(17) . . . . ?
F55 C55 C56 F56 -0.6(17) . . . . ?
C54 C55 C56 F56 -180.0(11) . . . . ?
F55 C55 C56 C51 -179.8(11) . . . . ?
C54 C55 C56 C51 0.8(19) . . . . ?
C52 C51 C56 C55 -1.5(18) . . . . ?
B2 C51 C56 C55 174.9(11) . . . . ?
C52 C51 C56 F56 179.3(11) . . . . ?
B2 C51 C56 F56 -4.3(16) . . . . ?
C2 C1 B1 C11 102.7(14) . . . . ?
C6 C1 B1 C11 -62.4(14) . . . . ?
C2 C1 B1 C21 -22.0(17) . . . . ?
C6 C1 B1 C21 172.8(11) . . . . ?
C2 C1 B1 N1 -137.7(12) . . . . ?
C6 C1 B1 N1 57.1(13) . . . . ?
C12 C11 B1 C1 -63.8(14) . . . . ?
C16 C11 B1 C1 106.3(14) . . . . ?
C12 C11 B1 C21 60.6(14) . . . . ?
C16 C11 B1 C21 -129.3(13) . . . . ?
C12 C11 B1 N1 -179.5(11) . . . . ?
C16 C11 B1 N1 -9.4(16) . . . . ?
C22 C21 B1 C1 -52.8(16) . . . . ?
C26 C21 B1 C1 130.1(12) . . . . ?
C22 C21 B1 C11 -173.7(12) . . . . ?
C26 C21 B1 C11 9.1(16) . . . . ?
C22 C21 B1 N1 63.0(14) . . . . ?
C26 C21 B1 N1 -114.1(12) . . . . ?
B2 N1 B1 C1 148.5(11) . . . . ?
B2 N1 B1 C11 -95.6(13) . . . . ?
B2 N1 B1 C21 28.4(16) . . . . ?
B1 N1 B2 C41 7.8(17) . . . . ?
B1 N1 B2 C31 133.2(12) . . . . ?
B1 N1 B2 C51 -116.9(12) . . . . ?
C42 C41 B2 N1 -106.6(13) . . . . ?
C46 C41 B2 N1 70.8(13) . . . . ?
C42 C41 B2 C31 131.0(12) . . . . ?
C46 C41 B2 C31 -51.7(14) . . . . ?
C42 C41 B2 C51 17.8(16) . . . . ?
C46 C41 B2 C51 -164.9(10) . . . . ?
C32 C31 B2 N1 -134.4(12) . . . . ?
C36 C31 B2 N1 49.0(14) . . . . ?
C32 C31 B2 C41 -10.3(17) . . . . ?
C36 C31 B2 C41 173.1(10) . . . . ?
C32 C31 B2 C51 109.1(13) . . . . ?
C36 C31 B2 C51 -67.5(12) . . . . ?
C52 C51 B2 N1 -6.3(16) . . . . ?
C56 C51 B2 N1 177.9(10) . . . . ?
C52 C51 B2 C41 -130.8(12) . . . . ?
C56 C51 B2 C41 53.3(14) . . . . ?
C52 C51 B2 C31 108.4(13) . . . . ?
C56 C51 B2 C31 -67.5(12) . . . . ?
C66 C61 C62 C63 0.0(18) . . . . ?
B11 C61 C62 C63 174.1(11) . . . . ?
C66 C61 C62 F62 -178.2(10) . . . . ?
B11 C61 C62 F62 -4.1(16) . . . . ?
C61 C62 C63 F63 -179.3(11) . . . . ?
F62 C62 C63 F63 -1.1(17) . . . . ?
C61 C62 C63 C64 -1.7(19) . . . . ?
F62 C62 C63 C64 176.6(10) . . . . ?
F63 C63 C64 F64 -2.9(16) . . . . ?
C62 C63 C64 F64 179.2(11) . . . . ?
F63 C63 C64 C65 -179.0(10) . . . . ?
C62 C63 C64 C65 3.2(16) . . . . ?
F64 C64 C65 F65 0.4(16) . . . . ?
C63 C64 C65 F65 176.4(10) . . . . ?
F64 C64 C65 C66 -179.3(11) . . . . ?
C63 C64 C65 C66 -3.3(16) . . . . ?
C62 C61 C66 F66 179.4(11) . . . . ?
B11 C61 C66 F66 5.6(18) . . . . ?
C62 C61 C66 C65 0.0(17) . . . . ?
B11 C61 C66 C65 -173.8(11) . . . . ?
F65 C65 C66 F66 2.6(16) . . . . ?
C64 C65 C66 F66 -177.7(10) . . . . ?
F65 C65 C66 C61 -177.9(10) . . . . ?
C64 C65 C66 C61 1.7(18) . . . . ?
C76 C71 C72 F72 178.4(11) . . . . ?
B11 C71 C72 F72 8(2) . . . . ?
C76 C71 C72 C73 -1.7(19) . . . . ?
B11 C71 C72 C73 -172.4(12) . . . . ?
C71 C72 C73 F73 179.4(12) . . . . ?
F72 C72 C73 F73 -0.7(17) . . . . ?
C71 C72 C73 C74 4(2) . . . . ?
F72 C72 C73 C74 -176.5(11) . . . . ?
F73 C73 C74 C75 -178.3(12) . . . . ?
C72 C73 C74 C75 -2.6(19) . . . . ?
F73 C73 C74 F74 2.6(18) . . . . ?
C72 C73 C74 F74 178.3(11) . . . . ?
F74 C74 C75 F75 -1.3(19) . . . . ?
C73 C74 C75 F75 179.7(12) . . . . ?
F74 C74 C75 C76 179.1(11) . . . . ?
C73 C74 C75 C76 0.0(19) . . . . ?
C72 C71 C76 F76 -176.0(11) . . . . ?
B11 C71 C76 F76 -4.1(17) . . . . ?
C72 C71 C76 C75 -1.3(19) . . . . ?
B11 C71 C76 C75 170.6(11) . . . . ?
F75 C75 C76 F76 -2.6(17) . . . . ?
C74 C75 C76 F76 177.0(11) . . . . ?
F75 C75 C76 C71 -177.5(12) . . . . ?
C74 C75 C76 C71 2(2) . . . . ?
C86 C81 C82 F82 -179.9(10) . . . . ?
B11 C81 C82 F82 0.2(17) . . . . ?
C86 C81 C82 C83 -2.7(19) . . . . ?
B11 C81 C82 C83 177.3(11) . . . . ?
F82 C82 C83 F83 -0.2(17) . . . . ?
C81 C82 C83 F83 -177.5(11) . . . . ?
F82 C82 C83 C84 177.5(10) . . . . ?
C81 C82 C83 C84 0.1(19) . . . . ?
F83 C83 C84 F84 -3.9(16) . . . . ?
C82 C83 C84 F84 178.2(11) . . . . ?
F83 C83 C84 C85 -179.4(11) . . . . ?
C82 C83 C84 C85 2.7(17) . . . . ?
F84 C84 C85 F85 2.1(18) . . . . ?
C83 C84 C85 F85 177.4(10) . . . . ?
F84 C84 C85 C86 -178.2(11) . . . . ?
C83 C84 C85 C86 -2.9(18) . . . . ?
C82 C81 C86 F86 -175.9(11) . . . . ?
B11 C81 C86 F86 4.0(18) . . . . ?
C82 C81 C86 C85 2.5(17) . . . . ?
B11 C81 C86 C85 -177.6(11) . . . . ?
C84 C85 C86 F86 178.8(11) . . . . ?
F85 C85 C86 F86 -1.6(16) . . . . ?
C84 C85 C86 C81 0.3(19) . . . . ?
F85 C85 C86 C81 180.0(10) . . . . ?
C96 C91 C92 F92 180.0(10) . . . . ?
B12 C91 C92 F92 -8.2(16) . . . . ?
C96 C91 C92 C93 0.8(18) . . . . ?
B12 C91 C92 C93 172.7(11) . . . . ?
C91 C92 C93 F93 175.6(11) . . . . ?
F92 C92 C93 F93 -3.7(16) . . . . ?
C91 C92 C93 C94 -0.8(18) . . . . ?
F92 C92 C93 C94 180.0(10) . . . . ?
F93 C93 C94 F94 1.6(17) . . . . ?
C92 C93 C94 F94 178.1(11) . . . . ?
F93 C93 C94 C95 -176.5(10) . . . . ?
C92 C93 C94 C95 -0.1(16) . . . . ?
F94 C94 C95 F95 2.8(17) . . . . ?
C93 C94 C95 F95 -179.0(10) . . . . ?
F94 C94 C95 C96 -177.3(11) . . . . ?
C93 C94 C95 C96 0.9(18) . . . . ?
C92 C91 C96 F96 177.1(11) . . . . ?
B12 C91 C96 F96 6.0(19) . . . . ?
C92 C91 C96 C95 0.1(17) . . . . ?
B12 C91 C96 C95 -171.0(11) . . . . ?
F95 C95 C96 F96 1.8(16) . . . . ?
C94 C95 C96 F96 -178.1(11) . . . . ?
F95 C95 C96 C91 178.9(11) . . . . ?
C94 C95 C96 C91 -0.9(19) . . . . ?
C106 C101 C102 F102 -178.9(11) . . . . ?
B12 C101 C102 F102 0.8(19) . . . . ?
C106 C101 C102 C103 5.5(17) . . . . ?
B12 C101 C102 C103 -174.7(11) . . . . ?
F102 C102 C103 F103 5.2(17) . . . . ?
C101 C102 C103 F103 -179.0(11) . . . . ?
F102 C102 C103 C104 177.0(11) . . . . ?
C101 C102 C103 C104 -7.3(19) . . . . ?
F103 C103 C104 F104 -3.7(18) . . . . ?
C102 C103 C104 F104 -175.7(11) . . . . ?
F103 C103 C104 C105 174.6(11) . . . . ?
C102 C103 C104 C105 2.7(18) . . . . ?
F104 C104 C105 F105 -0.8(17) . . . . ?
C103 C104 C105 F105 -179.2(11) . . . . ?
F104 C104 C105 C106 -178.5(11) . . . . ?
C103 C104 C105 C106 3.1(17) . . . . ?
F105 C105 C106 F106 1.9(18) . . . . ?
C104 C105 C106 F106 179.4(10) . . . . ?
F105 C105 C106 C101 177.6(12) . . . . ?
C104 C105 C106 C101 -4.8(19) . . . . ?
C102 C101 C106 F106 176.2(11) . . . . ?
B12 C101 C106 F106 -3.5(16) . . . . ?
C102 C101 C106 C105 0.6(18) . . . . ?
B12 C101 C106 C105 -179.2(12) . . . . ?
C116 C111 C112 F112 -175.9(10) . . . . ?
B12 C111 C112 F112 0.9(16) . . . . ?
C116 C111 C112 C113 4.6(18) . . . . ?
B12 C111 C112 C113 -178.6(11) . . . . ?
F112 C112 C113 F113 -3.7(17) . . . . ?
C111 C112 C113 F113 175.8(11) . . . . ?
F112 C112 C113 C114 178.4(10) . . . . ?
C111 C112 C113 C114 -2.1(19) . . . . ?
F113 C113 C114 C115 -178.2(11) . . . . ?
C112 C113 C114 C115 -0.3(18) . . . . ?
F113 C113 C114 F114 -0.6(17) . . . . ?
C112 C113 C114 F114 177.3(10) . . . . ?
C113 C114 C115 F115 -176.7(11) . . . . ?
F114 C114 C115 F115 5.8(17) . . . . ?
C113 C114 C115 C116 -0.1(18) . . . . ?
F114 C114 C115 C116 -177.7(10) . . . . ?
F115 C115 C116 F116 -2.5(17) . . . . ?
C114 C115 C116 F116 -179.1(11) . . . . ?
F115 C115 C116 C111 179.5(11) . . . . ?
C114 C115 C116 C111 3.0(18) . . . . ?
C112 C111 C116 F116 177.2(11) . . . . ?
B12 C111 C116 F116 0.7(19) . . . . ?
C112 C111 C116 C115 -5.0(17) . . . . ?
B12 C111 C116 C115 178.6(11) . . . . ?
B12 N2 B11 C71 -119.3(12) . . . . ?
B12 N2 B11 C61 127.7(11) . . . . ?
B12 N2 B11 C81 5.2(16) . . . . ?
C72 C71 B11 N2 -12.2(17) . . . . ?
C76 C71 B11 N2 177.7(10) . . . . ?
C72 C71 B11 C61 104.9(14) . . . . ?
C76 C71 B11 C61 -65.2(13) . . . . ?
C72 C71 B11 C81 -134.0(13) . . . . ?
C76 C71 B11 C81 55.9(15) . . . . ?
C62 C61 B11 N2 46.7(14) . . . . ?
C66 C61 B11 N2 -139.9(11) . . . . ?
C62 C61 B11 C71 -70.8(13) . . . . ?
C66 C61 B11 C71 102.5(12) . . . . ?
C62 C61 B11 C81 167.2(11) . . . . ?
C66 C61 B11 C81 -19.5(15) . . . . ?
C82 C81 B11 N2 69.6(13) . . . . ?
C86 C81 B11 N2 -110.4(12) . . . . ?
C82 C81 B11 C71 -167.7(11) . . . . ?
C86 C81 B11 C71 12.4(17) . . . . ?
C82 C81 B11 C61 -51.6(14) . . . . ?
C86 C81 B11 C61 128.5(12) . . . . ?
B11 N2 B12 C101 27.8(15) . . . . ?
B11 N2 B12 C111 146.9(11) . . . . ?
B11 N2 B12 C91 -100.4(13) . . . . ?
C106 C101 B12 N2 59.1(13) . . . . ?
C102 C101 B12 N2 -120.6(12) . . . . ?
C106 C101 B12 C111 -57.4(13) . . . . ?
C102 C101 B12 C111 122.9(13) . . . . ?
C106 C101 B12 C91 -174.8(10) . . . . ?
C102 C101 B12 C91 5.5(17) . . . . ?
C112 C111 B12 N2 52.8(13) . . . . ?
C116 C111 B12 N2 -130.8(12) . . . . ?
C112 C111 B12 C101 170.3(10) . . . . ?
C116 C111 B12 C101 -13.3(16) . . . . ?
C112 C111 B12 C91 -65.3(13) . . . . ?
C116 C111 B12 C91 111.0(13) . . . . ?
C92 C91 B12 N2 -176.8(10) . . . . ?
C96 C91 B12 N2 -5.9(16) . . . . ?
C92 C91 B12 C101 59.0(14) . . . . ?
C96 C91 B12 C101 -130.1(12) . . . . ?
C92 C91 B12 C111 -62.2(13) . . . . ?
C96 C91 B12 C111 108.7(13) . . . . ?


#----------------------------------------------------------------------------#
# END OF CIF FILE FOR WLF033                                                 #
#----------------------------------------------------------------------------#
_database_code_depnum_ccdc_archive 'CCDC 1006890'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ge{NR2}2{SePh}2

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H46 Ge N2 Se2 Si4'
_chemical_formula_sum            'C24 H46 Ge N2 Se2 Si4'
_chemical_formula_weight         705.5
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.9113(4)
_cell_length_b                   11.4671(4)
_cell_length_c                   17.4235(6)
_cell_angle_alpha                97.6430(10)
_cell_angle_beta                 94.825(2)
_cell_angle_gamma                112.1520(10)
_cell_volume                     1616.80(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5659
_cell_measurement_theta_min      2.46
_cell_measurement_theta_max      27.4
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             720
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    3.363
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.421
_exptl_absorpt_correction_T_max  0.546


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0406
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_number            18080
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.92
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_reflns_number_total             7359
_reflns_number_gt                5884
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0312P)²+2.4622P] 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_number_reflns         7359
_refine_ls_number_parameters     310
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0404
_refine_ls_wR_factor_ref         0.0961
_refine_ls_wR_factor_gt          0.0913
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.02
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.095

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 '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'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.07739(4) 0.32941(3) 0.75653(2) 0.01576(9) Uani 1 1 d . . .
Si1 Si -0.21183(12) 0.13988(9) 0.62961(6) 0.0254(2) Uani 1 1 d . . .
Si2 Si -0.03797(13) 0.02641(9) 0.73583(7) 0.0304(3) Uani 1 1 d . . .
N1 N -0.0553(3) 0.1634(2) 0.70694(17) 0.0211(6) Uani 1 1 d . . .
C2 C -0.1757(6) 0.0580(5) 0.5374(3) 0.0579(14) Uani 1 1 d . . .
H2A H -0.0777 0.116 0.5197 0.087 Uiso 1 1 calc R . .
H2B H -0.2705 0.0342 0.4969 0.087 Uiso 1 1 calc R . .
H2C H -0.1597 -0.0191 0.5471 0.087 Uiso 1 1 calc R . .
C3 C -0.4224(5) 0.0477(4) 0.6503(3) 0.0438(11) Uani 1 1 d . . .
H3A H -0.4151 0.0112 0.6975 0.066 Uiso 1 1 calc R . .
H3B H -0.4823 -0.0214 0.6059 0.066 Uiso 1 1 calc R . .
H3C H -0.4804 0.105 0.6583 0.066 Uiso 1 1 calc R . .
C4 C -0.2221(5) 0.2916(4) 0.6087(2) 0.0336(9) Uani 1 1 d . . .
H4A H -0.2455 0.3363 0.6552 0.05 Uiso 1 1 calc R . .
H4B H -0.3092 0.2726 0.5649 0.05 Uiso 1 1 calc R . .
H4C H -0.117 0.346 0.595 0.05 Uiso 1 1 calc R . .
C5 C -0.2222(7) -0.1221(4) 0.6938(5) 0.113(3) Uani 1 1 d . . .
H5A H -0.3178 -0.1181 0.7161 0.169 Uiso 1 1 calc R . .
H5B H -0.2036 -0.1968 0.7063 0.169 Uiso 1 1 calc R . .
H5C H -0.2417 -0.1293 0.6368 0.169 Uiso 1 1 calc R . .
C6 C -0.0260(8) 0.0262(5) 0.8424(3) 0.0699(19) Uani 1 1 d . . .
H6A H 0.0864 0.0781 0.868 0.105 Uiso 1 1 calc R . .
H6B H -0.0573 -0.0617 0.8517 0.105 Uiso 1 1 calc R . .
H6C H -0.1006 0.0622 0.8639 0.105 Uiso 1 1 calc R . .
C7 C 0.1430(6) -0.0029(4) 0.7077(3) 0.0476(12) Uani 1 1 d . . .
H7A H 0.1342 -0.0194 0.6505 0.071 Uiso 1 1 calc R . .
H7B H 0.1471 -0.0773 0.7283 0.071 Uiso 1 1 calc R . .
H7C H 0.243 0.0725 0.7295 0.071 Uiso 1 1 calc R . .
Se1 Se -0.07639(6) 0.41490(4) 0.83535(2) 0.03268(11) Uani 1 1 d . . .
C11 C -0.1574(5) 0.2820(4) 0.8957(2) 0.0306(9) Uani 1 1 d . . .
C12 C -0.3048(6) 0.1803(4) 0.8675(3) 0.0476(12) Uani 1 1 d . . .
H12 H -0.3634 0.1756 0.8183 0.057 Uiso 1 1 calc R . .
C13 C -0.3669(7) 0.0849(5) 0.9116(4) 0.0700(18) Uani 1 1 d . . .
H13 H -0.4667 0.0137 0.8918 0.084 Uiso 1 1 calc R . .
C14 C -0.2845(8) 0.0932(5) 0.9836(4) 0.0626(17) Uani 1 1 d . . .
H14 H -0.327 0.0275 1.0134 0.075 Uiso 1 1 calc R . .
C15 C -0.1400(7) 0.1967(5) 1.0126(3) 0.0543(13) Uani 1 1 d . . .
H15 H -0.0845 0.2033 1.063 0.065 Uiso 1 1 calc R . .
C16 C -0.0759(6) 0.2908(4) 0.9685(3) 0.0407(10) Uani 1 1 d . . .
H16 H 0.0243 0.3615 0.9884 0.049 Uiso 1 1 calc R . .
Si11 Si 0.16725(12) 0.60126(9) 0.70414(6) 0.0209(2) Uani 1 1 d . . .
Si12 Si 0.28333(12) 0.41039(9) 0.62139(6) 0.0237(2) Uani 1 1 d . . .
N21 N 0.1661(3) 0.4452(2) 0.69067(16) 0.0174(6) Uani 1 1 d . . .
C21 C -0.0391(5) 0.6087(4) 0.7044(3) 0.0391(10) Uani 1 1 d . . .
H21A H -0.1042 0.5706 0.6525 0.059 Uiso 1 1 calc R . .
H21B H -0.0259 0.6982 0.7173 0.059 Uiso 1 1 calc R . .
H21C H -0.0951 0.5613 0.7435 0.059 Uiso 1 1 calc R . .
C22 C 0.3015(6) 0.7059(4) 0.7940(3) 0.0438(12) Uani 1 1 d . . .
H22A H 0.2616 0.6702 0.8399 0.066 Uiso 1 1 calc R . .
H22B H 0.3004 0.7916 0.7974 0.066 Uiso 1 1 calc R . .
H22C H 0.4135 0.7115 0.7922 0.066 Uiso 1 1 calc R . .
C23 C 0.2418(6) 0.6843(4) 0.6205(3) 0.0409(11) Uani 1 1 d . . .
H23A H 0.3528 0.6894 0.6157 0.061 Uiso 1 1 calc R . .
H23B H 0.243 0.7708 0.6303 0.061 Uiso 1 1 calc R . .
H23C H 0.1685 0.636 0.5719 0.061 Uiso 1 1 calc R . .
C24 C 0.1862(6) 0.3953(5) 0.5186(2) 0.0450(11) Uani 1 1 d . . .
H24A H 0.0702 0.338 0.5118 0.067 Uiso 1 1 calc R . .
H24B H 0.2419 0.3601 0.4816 0.067 Uiso 1 1 calc R . .
H24C H 0.1959 0.4798 0.5087 0.067 Uiso 1 1 calc R . .
C25 C 0.3049(5) 0.2561(4) 0.6248(3) 0.0392(11) Uani 1 1 d . . .
H25A H 0.3659 0.261 0.6754 0.059 Uiso 1 1 calc R . .
H25B H 0.3642 0.2392 0.5826 0.059 Uiso 1 1 calc R . .
H25C H 0.1961 0.1869 0.618 0.059 Uiso 1 1 calc R . .
C26 C 0.4979(5) 0.5339(4) 0.6377(3) 0.0365(10) Uani 1 1 d . . .
H26A H 0.5078 0.5937 0.6013 0.055 Uiso 1 1 calc R . .
H26B H 0.574 0.4918 0.6287 0.055 Uiso 1 1 calc R . .
H26C H 0.5243 0.5807 0.6916 0.055 Uiso 1 1 calc R . .
Se2 Se 0.28354(5) 0.30893(3) 0.84229(2) 0.03420(12) Uani 1 1 d . . .
C31 C 0.4276(5) 0.4845(3) 0.8789(2) 0.0257(8) Uani 1 1 d . . .
C32 C 0.5752(5) 0.5315(4) 0.8499(3) 0.0368(10) Uani 1 1 d . . .
H32 H 0.5988 0.4804 0.809 0.044 Uiso 1 1 calc R . .
C33 C 0.6879(6) 0.6545(4) 0.8813(3) 0.0467(11) Uani 1 1 d . . .
H33 H 0.7881 0.6878 0.8609 0.056 Uiso 1 1 calc R . .
C34 C 0.6566(6) 0.7285(4) 0.9412(3) 0.0452(11) Uani 1 1 d . . .
H34 H 0.735 0.812 0.9628 0.054 Uiso 1 1 calc R . .
C35 C 0.5099(6) 0.6803(4) 0.9700(2) 0.0383(10) Uani 1 1 d . . .
H35 H 0.4874 0.7314 1.0113 0.046 Uiso 1 1 calc R . .
C36 C 0.3952(5) 0.5584(4) 0.9393(2) 0.0321(9) Uani 1 1 d . . .
H36 H 0.2948 0.5257 0.9597 0.039 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Ge1 N1 1.860(3) . ?
Ge1 N21 1.863(3) . ?
Ge1 Se2 2.3706(5) . ?
Ge1 Se1 2.3868(5) . ?
Si1 N1 1.771(3) . ?
Si1 C4 1.858(4) . ?
Si1 C2 1.866(4) . ?
Si1 C3 1.868(4) . ?
Si2 N1 1.768(3) . ?
Si2 C6 1.851(5) . ?
Si2 C7 1.857(4) . ?
Si2 C5 1.868(5) . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
Se1 C11 1.916(4) . ?
C11 C16 1.380(6) . ?
C11 C12 1.382(6) . ?
C12 C13 1.390(7) . ?
C12 H12 0.95 . ?
C13 C14 1.371(8) . ?
C13 H13 0.95 . ?
C14 C15 1.379(8) . ?
C14 H14 0.95 . ?
C15 C16 1.382(6) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?
Si11 N21 1.770(3) . ?
Si11 C22 1.850(4) . ?
Si11 C21 1.873(4) . ?
Si11 C23 1.878(4) . ?
Si12 N21 1.763(3) . ?
Si12 C25 1.858(4) . ?
Si12 C26 1.871(4) . ?
Si12 C24 1.879(4) . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
Se2 C31 1.918(4) . ?
C31 C36 1.381(5) . ?
C31 C32 1.388(6) . ?
C32 C33 1.389(6) . ?
C32 H32 0.95 . ?
C33 C34 1.372(6) . ?
C33 H33 0.95 . ?
C34 C35 1.380(7) . ?
C34 H34 0.95 . ?
C35 C36 1.385(6) . ?
C35 H35 0.95 . ?
C36 H36 0.95 . ?


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 Ge1 N21 115.74(13) . . ?
N1 Ge1 Se2 105.37(9) . . ?
N21 Ge1 Se2 111.88(9) . . ?
N1 Ge1 Se1 109.49(9) . . ?
N21 Ge1 Se1 106.73(8) . . ?
Se2 Ge1 Se1 107.36(2) . . ?
N1 Si1 C4 113.27(16) . . ?
N1 Si1 C2 109.99(19) . . ?
C4 Si1 C2 106.7(2) . . ?
N1 Si1 C3 113.60(18) . . ?
C4 Si1 C3 103.21(19) . . ?
C2 Si1 C3 109.7(2) . . ?
N1 Si2 C6 114.89(18) . . ?
N1 Si2 C7 114.53(17) . . ?
C6 Si2 C7 104.9(2) . . ?
N1 Si2 C5 111.7(2) . . ?
C6 Si2 C5 103.1(3) . . ?
C7 Si2 C5 106.7(3) . . ?
Si2 N1 Si1 117.94(16) . . ?
Si2 N1 Ge1 123.00(16) . . ?
Si1 N1 Ge1 119.02(15) . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C11 Se1 Ge1 99.60(10) . . ?
C16 C11 C12 119.9(4) . . ?
C16 C11 Se1 120.9(3) . . ?
C12 C11 Se1 119.1(3) . . ?
C11 C12 C13 119.6(5) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 120.2(5) . . ?
C14 C13 H13 119.9 . . ?
C12 C13 H13 119.9 . . ?
C13 C14 C15 120.0(5) . . ?
C13 C14 H14 120 . . ?
C15 C14 H14 120 . . ?
C14 C15 C16 120.1(5) . . ?
C14 C15 H15 119.9 . . ?
C16 C15 H15 119.9 . . ?
C11 C16 C15 120.0(5) . . ?
C11 C16 H16 120 . . ?
C15 C16 H16 120 . . ?
N21 Si11 C22 113.04(16) . . ?
N21 Si11 C21 115.14(16) . . ?
C22 Si11 C21 108.0(2) . . ?
N21 Si11 C23 111.57(16) . . ?
C22 Si11 C23 106.4(2) . . ?
C21 Si11 C23 101.79(19) . . ?
N21 Si12 C25 113.30(16) . . ?
N21 Si12 C26 111.92(17) . . ?
C25 Si12 C26 105.10(19) . . ?
N21 Si12 C24 111.47(17) . . ?
C25 Si12 C24 105.2(2) . . ?
C26 Si12 C24 109.4(2) . . ?
Si12 N21 Si11 116.88(15) . . ?
Si12 N21 Ge1 119.37(14) . . ?
Si11 N21 Ge1 122.95(15) . . ?
Si11 C21 H21A 109.5 . . ?
Si11 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si11 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si11 C22 H22A 109.5 . . ?
Si11 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si11 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si11 C23 H23A 109.5 . . ?
Si11 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si11 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si12 C24 H24A 109.5 . . ?
Si12 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si12 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si12 C25 H25A 109.5 . . ?
Si12 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si12 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si12 C26 H26A 109.5 . . ?
Si12 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si12 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C31 Se2 Ge1 101.66(10) . . ?
C36 C31 C32 120.2(4) . . ?
C36 C31 Se2 121.0(3) . . ?
C32 C31 Se2 118.4(3) . . ?
C31 C32 C33 119.1(4) . . ?
C31 C32 H32 120.4 . . ?
C33 C32 H32 120.4 . . ?
C34 C33 C32 121.0(4) . . ?
C34 C33 H33 119.5 . . ?
C32 C33 H33 119.5 . . ?
C33 C34 C35 119.3(4) . . ?
C33 C34 H34 120.3 . . ?
C35 C34 H34 120.3 . . ?
C34 C35 C36 120.7(4) . . ?
C34 C35 H35 119.6 . . ?
C36 C35 H35 119.6 . . ?
C31 C36 C35 119.6(4) . . ?
C31 C36 H36 120.2 . . ?
C35 C36 H36 120.2 . . ?


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
C6 Si2 N1 Si1 -130.2(3) . . . . ?
C7 Si2 N1 Si1 108.1(2) . . . . ?
C5 Si2 N1 Si1 -13.3(4) . . . . ?
C6 Si2 N1 Ge1 47.3(3) . . . . ?
C7 Si2 N1 Ge1 -74.4(3) . . . . ?
C5 Si2 N1 Ge1 164.2(3) . . . . ?
C4 Si1 N1 Si2 177.22(19) . . . . ?
C2 Si1 N1 Si2 -63.5(3) . . . . ?
C3 Si1 N1 Si2 59.9(2) . . . . ?
C4 Si1 N1 Ge1 -0.4(3) . . . . ?
C2 Si1 N1 Ge1 118.9(2) . . . . ?
C3 Si1 N1 Ge1 -117.7(2) . . . . ?
N21 Ge1 N1 Si2 133.69(18) . . . . ?
Se2 Ge1 N1 Si2 9.5(2) . . . . ?
Se1 Ge1 N1 Si2 -105.67(17) . . . . ?
N21 Ge1 N1 Si1 -48.8(2) . . . . ?
Se2 Ge1 N1 Si1 -173.01(14) . . . . ?
Se1 Ge1 N1 Si1 71.81(18) . . . . ?
N1 Ge1 Se1 C11 53.08(17) . . . . ?
N21 Ge1 Se1 C11 179.06(16) . . . . ?
Se2 Ge1 Se1 C11 -60.83(14) . . . . ?
Ge1 Se1 C11 C16 94.7(3) . . . . ?
Ge1 Se1 C11 C12 -89.4(3) . . . . ?
C16 C11 C12 C13 -2.4(6) . . . . ?
Se1 C11 C12 C13 -178.4(4) . . . . ?
C11 C12 C13 C14 1.6(8) . . . . ?
C12 C13 C14 C15 0.4(8) . . . . ?
C13 C14 C15 C16 -1.5(8) . . . . ?
C12 C11 C16 C15 1.3(6) . . . . ?
Se1 C11 C16 C15 177.2(3) . . . . ?
C14 C15 C16 C11 0.7(7) . . . . ?
C25 Si12 N21 Si11 169.4(2) . . . . ?
C26 Si12 N21 Si11 50.8(2) . . . . ?
C24 Si12 N21 Si11 -72.2(2) . . . . ?
C25 Si12 N21 Ge1 -0.7(3) . . . . ?
C26 Si12 N21 Ge1 -119.3(2) . . . . ?
C24 Si12 N21 Ge1 117.8(2) . . . . ?
C22 Si11 N21 Si12 -102.4(2) . . . . ?
C21 Si11 N21 Si12 132.8(2) . . . . ?
C23 Si11 N21 Si12 17.4(3) . . . . ?
C22 Si11 N21 Ge1 67.3(3) . . . . ?
C21 Si11 N21 Ge1 -57.6(3) . . . . ?
C23 Si11 N21 Ge1 -172.9(2) . . . . ?
N1 Ge1 N21 Si12 -55.9(2) . . . . ?
Se2 Ge1 N21 Si12 64.79(18) . . . . ?
Se1 Ge1 N21 Si12 -178.05(13) . . . . ?
N1 Ge1 N21 Si11 134.66(17) . . . . ?
Se2 Ge1 N21 Si11 -104.62(16) . . . . ?
Se1 Ge1 N21 Si11 12.54(19) . . . . ?
N1 Ge1 Se2 C31 172.54(15) . . . . ?
N21 Ge1 Se2 C31 45.97(15) . . . . ?
Se1 Ge1 Se2 C31 -70.81(12) . . . . ?
Ge1 Se2 C31 C36 82.2(3) . . . . ?
Ge1 Se2 C31 C32 -105.3(3) . . . . ?
C36 C31 C32 C33 -1.3(6) . . . . ?
Se2 C31 C32 C33 -173.8(3) . . . . ?
C31 C32 C33 C34 1.3(7) . . . . ?
C32 C33 C34 C35 -0.8(7) . . . . ?
C33 C34 C35 C36 0.4(6) . . . . ?
C32 C31 C36 C35 0.8(6) . . . . ?
Se2 C31 C36 C35 173.2(3) . . . . ?
C34 C35 C36 C31 -0.4(6) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006891'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Ge{NR2}2{TePh}2

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H46 Ge N2 Si4 Te2'
_chemical_formula_sum            'C24 H46 Ge N2 Si4 Te2'
_chemical_formula_weight         802.78
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   8.6866(2)
_cell_length_b                   17.9348(4)
_cell_length_c                   21.2488(5)
_cell_angle_alpha                90
_cell_angle_beta                 98.1587(9)
_cell_angle_gamma                90
_cell_volume                     3276.90(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    6299
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      27.47
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.584
_exptl_absorpt_correction_T_max  0.843


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_number            14204
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.91
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total             3758
_reflns_number_gt                3368
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0269P)²+0.0000P] 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_number_reflns         3758
_refine_ls_number_parameters     156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0269
_refine_ls_R_factor_gt           0.0226
_refine_ls_wR_factor_ref         0.0598
_refine_ls_wR_factor_gt          0.058
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.466
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.081

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ge1 Ge 0.5 0.208994(16) 0.75 0.01430(8) Uani 1 2 d S . .
N1 N 0.4998(2) 0.26651(9) 0.67683(8) 0.0157(4) Uani 1 1 d . . .
Si1 Si 0.35395(7) 0.33476(3) 0.65783(3) 0.01816(13) Uani 1 1 d . . .
Si2 Si 0.61849(7) 0.24469(3) 0.61823(3) 0.01816(13) Uani 1 1 d . . .
C1 C 0.4401(3) 0.42922(12) 0.64901(12) 0.0291(5) Uani 1 1 d . . .
H1A H 0.4812 0.4489 0.6911 0.044 Uiso 1 1 calc R . .
H1B H 0.3597 0.4629 0.6282 0.044 Uiso 1 1 calc R . .
H1C H 0.5245 0.4253 0.6231 0.044 Uiso 1 1 calc R . .
C2 C 0.2258(3) 0.34781(14) 0.72024(12) 0.0263(5) Uani 1 1 d . . .
H2A H 0.1714 0.301 0.7263 0.039 Uiso 1 1 calc R . .
H2B H 0.1495 0.387 0.707 0.039 Uiso 1 1 calc R . .
H2C H 0.289 0.3622 0.7603 0.039 Uiso 1 1 calc R . .
C3 C 0.2205(3) 0.30638(13) 0.58460(11) 0.0265(5) Uani 1 1 d . . .
H3A H 0.2558 0.2589 0.5688 0.04 Uiso 1 1 calc R . .
H3B H 0.2212 0.3448 0.5518 0.04 Uiso 1 1 calc R . .
H3C H 0.1146 0.3006 0.5949 0.04 Uiso 1 1 calc R . .
C4 C 0.5863(3) 0.14918(13) 0.58526(12) 0.0310(6) Uani 1 1 d . . .
H4A H 0.6151 0.1125 0.6191 0.047 Uiso 1 1 calc R . .
H4B H 0.6505 0.1416 0.5514 0.047 Uiso 1 1 calc R . .
H4C H 0.4764 0.143 0.5679 0.047 Uiso 1 1 calc R . .
C5 C 0.8312(3) 0.25674(13) 0.64393(11) 0.0258(5) Uani 1 1 d . . .
H5A H 0.8538 0.3094 0.6534 0.039 Uiso 1 1 calc R . .
H5B H 0.8883 0.2404 0.6098 0.039 Uiso 1 1 calc R . .
H5C H 0.8633 0.2268 0.6821 0.039 Uiso 1 1 calc R . .
C6 C 0.5817(3) 0.30719(14) 0.54712(11) 0.0295(5) Uani 1 1 d . . .
H6A H 0.4727 0.3029 0.5279 0.044 Uiso 1 1 calc R . .
H6B H 0.6493 0.2925 0.516 0.044 Uiso 1 1 calc R . .
H6C H 0.6039 0.3589 0.5602 0.044 Uiso 1 1 calc R . .
Te1 Te 0.253737(17) 0.123128(8) 0.739852(8) 0.02538(6) Uani 1 1 d . . .
C11 C 0.2792(3) 0.06763(12) 0.65378(11) 0.0221(5) Uani 1 1 d . . .
C12 C 0.1801(3) 0.08682(13) 0.59883(12) 0.0271(5) Uani 1 1 d . . .
H12 H 0.1069 0.126 0.5998 0.033 Uiso 1 1 calc R . .
C13 C 0.1886(3) 0.04854(13) 0.54278(12) 0.0336(6) Uani 1 1 d . . .
H13 H 0.1202 0.0612 0.5054 0.04 Uiso 1 1 calc R . .
C14 C 0.2958(3) -0.00771(14) 0.54104(13) 0.0387(7) Uani 1 1 d . . .
H14 H 0.3033 -0.0328 0.5022 0.046 Uiso 1 1 calc R . .
C15 C 0.3918(3) -0.02743(13) 0.59543(13) 0.0369(6) Uani 1 1 d . . .
H15 H 0.4648 -0.0666 0.5942 0.044 Uiso 1 1 calc R . .
C16 C 0.3831(3) 0.00952(13) 0.65239(12) 0.0290(5) Uani 1 1 d . . .
H16 H 0.4481 -0.0051 0.6901 0.035 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Ge1 N1 1.8656(17) 2_656 ?
Ge1 N1 1.8657(17) . ?
Ge1 Te1 2.6197(2) 2_656 ?
Ge1 Te1 2.6198(2) . ?
N1 Si1 1.7669(18) . ?
N1 Si2 1.7693(17) . ?
Si1 C2 1.863(2) . ?
Si1 C1 1.872(2) . ?
Si1 C3 1.874(2) . ?
Si2 C4 1.857(2) . ?
Si2 C5 1.863(2) . ?
Si2 C6 1.872(2) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
Te1 C11 2.121(2) . ?
C11 C16 1.381(3) . ?
C11 C12 1.392(3) . ?
C12 C13 1.386(3) . ?
C12 H12 0.95 . ?
C13 C14 1.377(4) . ?
C13 H13 0.95 . ?
C14 C15 1.372(4) . ?
C14 H14 0.95 . ?
C15 C16 1.391(3) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?


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 Ge1 N1 112.86(10) 2_656 . ?
N1 Ge1 Te1 110.63(5) 2_656 2_656 ?
N1 Ge1 Te1 107.32(5) . 2_656 ?
N1 Ge1 Te1 107.32(5) 2_656 . ?
N1 Ge1 Te1 110.63(5) . . ?
Te1 Ge1 Te1 107.995(12) 2_656 . ?
Si1 N1 Si2 117.58(10) . . ?
Si1 N1 Ge1 119.29(9) . . ?
Si2 N1 Ge1 122.18(9) . . ?
N1 Si1 C2 113.95(10) . . ?
N1 Si1 C1 111.46(10) . . ?
C2 Si1 C1 104.20(12) . . ?
N1 Si1 C3 109.92(10) . . ?
C2 Si1 C3 105.26(11) . . ?
C1 Si1 C3 111.81(11) . . ?
N1 Si2 C4 113.47(10) . . ?
N1 Si2 C5 114.87(10) . . ?
C4 Si2 C5 107.90(12) . . ?
N1 Si2 C6 112.70(10) . . ?
C4 Si2 C6 104.39(12) . . ?
C5 Si2 C6 102.45(11) . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si2 C4 H4A 109.5 . . ?
Si2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C11 Te1 Ge1 99.37(6) . . ?
C16 C11 C12 119.8(2) . . ?
C16 C11 Te1 121.38(18) . . ?
C12 C11 Te1 118.65(17) . . ?
C13 C12 C11 119.8(2) . . ?
C13 C12 H12 120.1 . . ?
C11 C12 H12 120.1 . . ?
C14 C13 C12 120.3(2) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 119.9(2) . . ?
C15 C14 H14 120 . . ?
C13 C14 H14 120 . . ?
C14 C15 C16 120.6(2) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
C11 C16 C15 119.6(2) . . ?
C11 C16 H16 120.2 . . ?
C15 C16 H16 120.2 . . ?


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
N1 Ge1 N1 Si1 -54.47(8) 2_656 . . . ?
Te1 Ge1 N1 Si1 -176.62(8) 2_656 . . . ?
Te1 Ge1 N1 Si1 65.79(11) . . . . ?
N1 Ge1 N1 Si2 136.99(13) 2_656 . . . ?
Te1 Ge1 N1 Si2 14.84(12) 2_656 . . . ?
Te1 Ge1 N1 Si2 -102.75(10) . . . . ?
Si2 N1 Si1 C2 175.29(12) . . . . ?
Ge1 N1 Si1 C2 6.23(15) . . . . ?
Si2 N1 Si1 C1 -67.12(14) . . . . ?
Ge1 N1 Si1 C1 123.82(12) . . . . ?
Si2 N1 Si1 C3 57.43(13) . . . . ?
Ge1 N1 Si1 C3 -111.63(12) . . . . ?
Si1 N1 Si2 C4 -111.95(13) . . . . ?
Ge1 N1 Si2 C4 56.77(16) . . . . ?
Si1 N1 Si2 C5 123.26(12) . . . . ?
Ge1 N1 Si2 C5 -68.01(14) . . . . ?
Si1 N1 Si2 C6 6.42(15) . . . . ?
Ge1 N1 Si2 C6 175.14(12) . . . . ?
N1 Ge1 Te1 C11 178.60(8) 2_656 . . . ?
N1 Ge1 Te1 C11 55.08(8) . . . . ?
Te1 Ge1 Te1 C11 -62.10(6) 2_656 . . . ?
Ge1 Te1 C11 C16 78.53(18) . . . . ?
Ge1 Te1 C11 C12 -106.53(17) . . . . ?
C16 C11 C12 C13 -1.4(3) . . . . ?
Te1 C11 C12 C13 -176.42(17) . . . . ?
C11 C12 C13 C14 -0.8(4) . . . . ?
C12 C13 C14 C15 1.8(4) . . . . ?
C13 C14 C15 C16 -0.7(4) . . . . ?
C12 C11 C16 C15 2.5(3) . . . . ?
Te1 C11 C16 C15 177.39(18) . . . . ?
C14 C15 C16 C11 -1.5(4) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006892'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_{RSeOHH}{H2N{BX3}2}

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C49 H24 B2 F30 N2 O1 Se1'
_chemical_formula_sum            'C49 H24 B2 F30 N2 O Se'
_chemical_formula_weight         1327.28
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   16.5296(6)
_cell_length_b                   15.9662(6)
_cell_length_c                   20.9740(7)
_cell_angle_alpha                90
_cell_angle_beta                 105.7030(10)
_cell_angle_gamma                90
_cell_volume                     5328.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2127
_cell_measurement_theta_min      2.67
_cell_measurement_theta_max      20.02
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_crystal_density_diffrn    1.654
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2616
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.850
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.821
_exptl_absorpt_correction_T_max  0.967


#----------------------------------------------------------------------------#
#                   SQUEEZE RESULTS                                          #
#----------------------------------------------------------------------------#

# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.770 0.163 0.690 136 33 ' '
2 0.770 0.337 0.190 136 33 ' '
3 0.230 0.663 0.810 136 32 ' '
4 0.230 0.837 0.310 136 32 ' '
_platon_squeeze_details          
;
;

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0785
_diffrn_reflns_av_unetI/netI     0.1554
_diffrn_reflns_number            28791
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_full        25
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.939
_reflns_number_total             11484
_reflns_number_gt                4875
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0697P)²+0.0000P] 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_number_reflns         11484
_refine_ls_number_parameters     766
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.1592
_refine_ls_R_factor_gt           0.0646
_refine_ls_wR_factor_ref         0.167
_refine_ls_wR_factor_gt          0.138
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_restrained_S_all      0.886
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.678
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.087

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'


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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C12 C 0.4650(4) 0.2538(4) 0.6863(3) 0.0501(16) Uani 1 1 d . . .
H12A H 0.4339 0.2809 0.715 0.06 Uiso 1 1 calc R A 1
H12B H 0.4234 0.2272 0.6488 0.06 Uiso 1 1 calc R A 1
N13 N 0.5218(3) 0.1883(3) 0.7249(2) 0.0412(11) Uani 1 1 d . B .
H13 H 0.5677 0.2156 0.7527 0.049 Uiso 1 1 calc R . .
C14 C 0.5546(4) 0.1278(4) 0.6848(3) 0.075(2) Uani 1 1 d . . .
H14A H 0.5829 0.1581 0.6564 0.112 Uiso 1 1 calc R B .
H14B H 0.5079 0.0951 0.6573 0.112 Uiso 1 1 calc R . .
H14C H 0.5947 0.0902 0.7142 0.112 Uiso 1 1 calc R . .
C15 C 0.4785(4) 0.1418(3) 0.7678(3) 0.0503(16) Uani 1 1 d . . .
H15A H 0.4665 0.1802 0.8006 0.075 Uiso 1 1 calc R B .
H15B H 0.5148 0.0964 0.7907 0.075 Uiso 1 1 calc R . .
H15C H 0.4257 0.1183 0.7405 0.075 Uiso 1 1 calc R . .
Se1 Se 0.55399(4) 0.39351(3) 0.79144(3) 0.04357(19) Uani 1 1 d . . .
C1 C 0.6733(3) 0.3784(3) 0.8363(3) 0.0387(14) Uani 1 1 d . B .
H1A H 0.7065 0.3966 0.8059 0.046 Uiso 1 1 calc R . .
H1B H 0.6882 0.4156 0.8754 0.046 Uiso 1 1 calc R . .
C2 C 0.6991(3) 0.2897(3) 0.8587(3) 0.0378(13) Uani 1 1 d . . .
O3 O 0.6750(2) 0.2341(2) 0.80154(18) 0.0429(10) Uani 1 1 d . B .
H3 H 0.7162 0.2269 0.786 0.064 Uiso 1 1 calc R . .
C4 C 0.6522(4) 0.2568(3) 0.9068(3) 0.0468(15) Uani 1 1 d . B .
H4A H 0.5918 0.2555 0.8848 0.07 Uiso 1 1 calc R . .
H4B H 0.6628 0.2937 0.9455 0.07 Uiso 1 1 calc R . .
H4C H 0.6718 0.2001 0.9209 0.07 Uiso 1 1 calc R . .
C5 C 0.7938(4) 0.2867(4) 0.8891(3) 0.0631(18) Uani 1 1 d . B .
H5A H 0.8103 0.23 0.9056 0.095 Uiso 1 1 calc R . .
H5B H 0.8097 0.3266 0.9259 0.095 Uiso 1 1 calc R . .
H5C H 0.8225 0.3014 0.8554 0.095 Uiso 1 1 calc R . .
C6A C 0.5571(4) 0.3839(4) 0.7012(3) 0.0505(16) Uani 0.406(13) 1 d PD B 1
C7A C 0.6128(18) 0.4344(15) 0.6792(10) 0.071(3) Uani 0.406(13) 1 d PD B 1
H7A H 0.6407 0.4791 0.7063 0.085 Uiso 0.406(13) 1 calc PR B 1
C8A C 0.6283(14) 0.4200(12) 0.6174(8) 0.071(3) Uani 0.406(13) 1 d PD B 1
H8A H 0.6683 0.4533 0.6039 0.085 Uiso 0.406(13) 1 calc PR B 1
C9A C 0.5852(14) 0.3570(13) 0.5761(8) 0.071(3) Uani 0.406(13) 1 d PD B 1
H9A H 0.5904 0.3516 0.5322 0.085 Uiso 0.406(13) 1 calc PR B 1
C10A C 0.5338(13) 0.3012(12) 0.5995(7) 0.071(3) Uani 0.406(13) 1 d PD B 1
H10A H 0.513 0.2519 0.5751 0.085 Uiso 0.406(13) 1 calc PR B 1
C11A C 0.5127(4) 0.3188(4) 0.6604(3) 0.0619(19) Uani 0.406(13) 1 d PD B 1
C6B C 0.5571(4) 0.3839(4) 0.7012(3) 0.0505(16) Uani 0.594(13) 1 d PD B 2
C7B C 0.5942(13) 0.4492(11) 0.6759(7) 0.071(3) Uani 0.594(13) 1 d PD B 2
H7B H 0.625 0.4911 0.7045 0.085 Uiso 0.594(13) 1 calc PR B 2
C8B C 0.5859(10) 0.4530(9) 0.6082(5) 0.071(3) Uani 0.594(13) 1 d PD B 2
H8B H 0.6129 0.4966 0.591 0.085 Uiso 0.594(13) 1 calc PR B 2
C9B C 0.5401(10) 0.3955(9) 0.5668(5) 0.071(3) Uani 0.594(13) 1 d PD B 2
H9B H 0.5341 0.3992 0.5206 0.085 Uiso 0.594(13) 1 calc PR B 2
C10B C 0.5011(10) 0.3297(9) 0.5925(5) 0.071(3) Uani 0.594(13) 1 d PD B 2
H10B H 0.4659 0.2916 0.5626 0.085 Uiso 0.594(13) 1 calc PR B 2
C11B C 0.5127(4) 0.3188(4) 0.6604(3) 0.0619(19) Uani 0.594(13) 1 d PD B 2
N20 N 0.1340(2) 0.1983(2) 0.88887(17) 0.0253(9) Uani 1 1 d . . .
H20A H 0.0763 0.1939 0.8757 0.03 Uiso 1 1 calc R . .
H20B H 0.1537 0.1445 0.8878 0.03 Uiso 1 1 calc R . .
B21 B 0.1551(4) 0.2199(3) 0.9670(3) 0.0261(13) Uani 1 1 d . . .
C21 C 0.2166(3) 0.1484(3) 1.0127(2) 0.0226(11) Uani 1 1 d . . .
C22 C 0.2452(3) 0.1597(3) 1.0815(2) 0.0283(12) Uani 1 1 d . . .
C23 C 0.2926(3) 0.1030(3) 1.1256(2) 0.0335(12) Uani 1 1 d . . .
C24 C 0.3147(3) 0.0299(3) 1.1022(3) 0.0390(14) Uani 1 1 d . . .
C25 C 0.2892(3) 0.0135(3) 1.0354(3) 0.0362(13) Uani 1 1 d . . .
C26 C 0.2422(3) 0.0711(3) 0.9937(2) 0.0283(12) Uani 1 1 d . . .
F22 F 0.22513(18) 0.23206(16) 1.10854(12) 0.0351(7) Uani 1 1 d . . .
F23 F 0.31914(19) 0.11992(19) 1.19115(14) 0.0479(8) Uani 1 1 d . . .
F24 F 0.3621(2) -0.02715(19) 1.14488(16) 0.0630(10) Uani 1 1 d . . .
F25 F 0.3106(2) -0.05928(18) 1.01183(16) 0.0568(9) Uani 1 1 d . . .
F26 F 0.21805(18) 0.04800(16) 0.92909(13) 0.0369(7) Uani 1 1 d . . .
C31 C 0.1925(3) 0.3161(3) 0.9802(2) 0.0275(12) Uani 1 1 d . . .
C32 C 0.2750(4) 0.3371(3) 1.0101(2) 0.0364(14) Uani 1 1 d . . .
C33 C 0.3039(4) 0.4186(4) 1.0194(3) 0.0452(16) Uani 1 1 d . . .
C34 C 0.2529(5) 0.4835(3) 0.9978(3) 0.0509(18) Uani 1 1 d . . .
C35 C 0.1696(5) 0.4673(3) 0.9683(3) 0.0470(17) Uani 1 1 d . . .
C36 C 0.1418(4) 0.3849(3) 0.9594(2) 0.0362(13) Uani 1 1 d . . .
F32 F 0.33403(18) 0.27737(18) 1.03191(13) 0.0392(7) Uani 1 1 d . . .
F33 F 0.3860(2) 0.4335(2) 1.04872(15) 0.0684(11) Uani 1 1 d . . .
F34 F 0.2804(3) 0.56315(19) 1.00451(16) 0.0807(13) Uani 1 1 d . . .
F35 F 0.1146(3) 0.53121(18) 0.94650(16) 0.0715(12) Uani 1 1 d . . .
F36 F 0.0586(2) 0.37420(17) 0.92914(14) 0.0469(8) Uani 1 1 d . . .
C41 C 0.0659(3) 0.2069(3) 0.9898(2) 0.0247(11) Uani 1 1 d . . .
C42 C 0.0382(3) 0.2589(3) 1.0340(2) 0.0303(12) Uani 1 1 d . . .
C43 C -0.0346(3) 0.2421(3) 1.0534(3) 0.0371(14) Uani 1 1 d . . .
C44 C -0.0817(3) 0.1746(4) 1.0297(3) 0.0402(14) Uani 1 1 d . . .
C45 C -0.0563(3) 0.1202(3) 0.9874(2) 0.0360(13) Uani 1 1 d . . .
C46 C 0.0155(3) 0.1382(3) 0.9699(2) 0.0295(12) Uani 1 1 d . . .
F42 F 0.08091(18) 0.32783(16) 1.06072(13) 0.0382(7) Uani 1 1 d . . .
F43 F -0.0564(2) 0.2938(2) 1.09720(16) 0.0574(10) Uani 1 1 d . . .
F44 F -0.1531(2) 0.1591(2) 1.04727(16) 0.0594(10) Uani 1 1 d . . .
F45 F -0.10245(19) 0.05269(18) 0.96353(15) 0.0492(8) Uani 1 1 d . . .
F46 F 0.03746(18) 0.08156(16) 0.92938(13) 0.0369(7) Uani 1 1 d . . .
B51 B 0.1572(4) 0.2446(3) 0.8264(3) 0.0257(13) Uani 1 1 d . . .
C51 C 0.1606(3) 0.1702(3) 0.7712(2) 0.0276(12) Uani 1 1 d . . .
C52 C 0.2229(3) 0.1568(3) 0.7388(2) 0.0292(12) Uani 1 1 d . . .
C53 C 0.2154(4) 0.0980(3) 0.6890(2) 0.0335(13) Uani 1 1 d . . .
C54 C 0.1459(4) 0.0509(3) 0.6681(2) 0.0375(14) Uani 1 1 d . . .
C55 C 0.0812(4) 0.0619(3) 0.6968(3) 0.0370(13) Uani 1 1 d . . .
C56 C 0.0917(3) 0.1191(3) 0.7477(2) 0.0307(12) Uani 1 1 d . . .
F52 F 0.29350(18) 0.20348(17) 0.75333(13) 0.0381(7) Uani 1 1 d . . .
F53 F 0.2801(2) 0.08969(18) 0.66060(14) 0.0505(9) Uani 1 1 d . . .
F54 F 0.1377(2) -0.00422(18) 0.61804(14) 0.0544(9) Uani 1 1 d . . .
F55 F 0.0096(2) 0.01786(18) 0.67629(14) 0.0497(8) Uani 1 1 d . . .
F56 F 0.02521(17) 0.12571(16) 0.77434(13) 0.0351(7) Uani 1 1 d . . .
C61 C 0.2488(3) 0.2914(3) 0.8546(2) 0.0295(12) Uani 1 1 d . . .
C62 C 0.3192(4) 0.2467(3) 0.8825(2) 0.0321(12) Uani 1 1 d . . .
C63 C 0.3991(4) 0.2791(4) 0.9075(2) 0.0430(15) Uani 1 1 d . . .
C64 C 0.4113(4) 0.3627(4) 0.9038(3) 0.0445(15) Uani 1 1 d . . .
C65 C 0.3442(5) 0.4118(3) 0.8774(3) 0.0497(17) Uani 1 1 d . . .
C66 C 0.2645(4) 0.3768(3) 0.8539(2) 0.0386(14) Uani 1 1 d . . .
F62 F 0.31471(17) 0.16151(18) 0.88771(13) 0.0391(7) Uani 1 1 d . . .
F63 F 0.46557(19) 0.2281(2) 0.93455(15) 0.0551(9) Uani 1 1 d . . .
F64 F 0.4880(2) 0.3973(2) 0.92970(16) 0.0704(11) Uani 1 1 d . . .
F65 F 0.3519(2) 0.4965(2) 0.87601(16) 0.0638(10) Uani 1 1 d . . .
F66 F 0.2004(2) 0.43213(17) 0.83135(14) 0.0457(8) Uani 1 1 d . . .
C71 C 0.0823(3) 0.3050(3) 0.7846(2) 0.0283(12) Uani 1 1 d . . .
C72 C 0.0939(4) 0.3476(3) 0.7289(2) 0.0339(13) Uani 1 1 d . . .
C73 C 0.0344(4) 0.3953(3) 0.6874(3) 0.0415(15) Uani 1 1 d . . .
C74 C -0.0423(4) 0.4055(3) 0.6976(3) 0.0487(16) Uani 1 1 d . . .
C75 C -0.0613(4) 0.3626(3) 0.7487(3) 0.0466(15) Uani 1 1 d . . .
C76 C 0.0018(4) 0.3128(3) 0.7903(2) 0.0348(13) Uani 1 1 d . . .
F72 F 0.1686(2) 0.34157(17) 0.71608(13) 0.0432(8) Uani 1 1 d . . .
F73 F 0.0534(2) 0.43603(19) 0.63689(15) 0.0644(10) Uani 1 1 d . . .
F74 F -0.1019(2) 0.4546(2) 0.65815(17) 0.0750(12) Uani 1 1 d . . .
F75 F -0.1374(2) 0.3693(2) 0.75938(18) 0.0669(10) Uani 1 1 d . . .
F76 F -0.02501(17) 0.27037(17) 0.83805(14) 0.0391(7) Uani 1 1 d . . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C12 N13 1.490(7) . ?
C12 C11A 1.493(7) . ?
C12 H12A 0.99 . ?
C12 H12B 0.99 . ?
N13 C14 1.477(6) . ?
N13 C15 1.491(6) . ?
N13 H13 0.93 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
Se1 C6A 1.913(5) . ?
Se1 C1 1.957(5) . ?
C1 C2 1.517(7) . ?
C1 H1A 0.99 . ?
C1 H1B 0.99 . ?
C2 O3 1.458(6) . ?
C2 C4 1.521(7) . ?
C2 C5 1.523(7) . ?
O3 H3 0.84 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6A C7A 1.393(14) . ?
C6A C11A 1.419(8) . ?
C7A C8A 1.406(15) . ?
C7A H7A 0.95 . ?
C8A C9A 1.392(14) . ?
C8A H8A 0.95 . ?
C9A C10A 1.408(14) . ?
C9A H9A 0.95 . ?
C10A C11A 1.439(13) . ?
C10A H10A 0.95 . ?
C7B C8B 1.389(12) . ?
C7B H7B 0.95 . ?
C8B C9B 1.346(11) . ?
C8B H8B 0.95 . ?
C9B C10B 1.414(11) . ?
C9B H9B 0.95 . ?
C10B H10B 0.95 . ?
N20 B21 1.618(6) . ?
N20 B51 1.638(6) . ?
N20 H20A 0.92 . ?
N20 H20B 0.92 . ?
B21 C21 1.651(7) . ?
B21 C31 1.651(7) . ?
B21 C41 1.681(7) . ?
C21 C26 1.397(6) . ?
C21 C22 1.401(6) . ?
C22 F22 1.368(5) . ?
C22 C23 1.377(7) . ?
C23 F23 1.352(5) . ?
C23 C24 1.353(7) . ?
C24 F24 1.365(6) . ?
C24 C25 1.376(7) . ?
C25 F25 1.347(5) . ?
C25 C26 1.359(7) . ?
C26 F26 1.357(5) . ?
C31 C36 1.378(7) . ?
C31 C32 1.379(7) . ?
C32 F32 1.353(6) . ?
C32 C33 1.382(7) . ?
C33 C34 1.335(8) . ?
C33 F33 1.351(6) . ?
C34 F34 1.345(6) . ?
C34 C35 1.373(8) . ?
C35 F35 1.360(6) . ?
C35 C36 1.390(7) . ?
C36 F36 1.361(6) . ?
C41 C46 1.372(6) . ?
C41 C42 1.410(6) . ?
C42 F42 1.346(5) . ?
C42 C43 1.397(7) . ?
C43 C44 1.343(7) . ?
C43 F43 1.354(5) . ?
C44 F44 1.350(5) . ?
C44 C45 1.387(7) . ?
C45 F45 1.337(6) . ?
C45 C46 1.364(7) . ?
C46 F46 1.356(5) . ?
B51 C71 1.625(7) . ?
B51 C61 1.649(7) . ?
B51 C51 1.671(7) . ?
C51 C56 1.378(7) . ?
C51 C52 1.395(6) . ?
C52 F52 1.348(5) . ?
C52 C53 1.385(7) . ?
C53 C54 1.343(7) . ?
C53 F53 1.363(5) . ?
C54 F54 1.348(5) . ?
C54 C55 1.373(7) . ?
C55 F55 1.342(6) . ?
C55 C56 1.381(7) . ?
C56 F56 1.366(5) . ?
C61 C62 1.355(7) . ?
C61 C66 1.388(6) . ?
C62 F62 1.368(5) . ?
C62 C63 1.383(7) . ?
C63 C64 1.355(8) . ?
C63 F63 1.362(6) . ?
C64 C65 1.349(8) . ?
C64 F64 1.355(6) . ?
C65 F65 1.359(6) . ?
C65 C66 1.393(8) . ?
C66 F66 1.362(6) . ?
C71 C76 1.373(7) . ?
C71 C72 1.409(7) . ?
C72 F72 1.338(6) . ?
C72 C73 1.358(7) . ?
C73 F73 1.350(6) . ?
C73 C74 1.351(8) . ?
C74 F74 1.352(6) . ?
C74 C75 1.377(8) . ?
C75 F75 1.340(6) . ?
C75 C76 1.411(7) . ?
C76 F76 1.378(5) . ?


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
N13 C12 C11A 111.6(5) . . ?
N13 C12 H12A 109.3 . . ?
C11A C12 H12A 109.3 . . ?
N13 C12 H12B 109.3 . . ?
C11A C12 H12B 109.3 . . ?
H12A C12 H12B 108 . . ?
C14 N13 C12 115.1(5) . . ?
C14 N13 C15 109.2(4) . . ?
C12 N13 C15 110.1(4) . . ?
C14 N13 H13 107.4 . . ?
C12 N13 H13 107.4 . . ?
C15 N13 H13 107.4 . . ?
N13 C14 H14A 109.5 . . ?
N13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
N13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N13 C15 H15A 109.5 . . ?
N13 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
N13 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C6A Se1 C1 99.9(2) . . ?
C2 C1 Se1 115.3(3) . . ?
C2 C1 H1A 108.5 . . ?
Se1 C1 H1A 108.5 . . ?
C2 C1 H1B 108.5 . . ?
Se1 C1 H1B 108.5 . . ?
H1A C1 H1B 107.5 . . ?
O3 C2 C1 108.7(4) . . ?
O3 C2 C4 105.1(4) . . ?
C1 C2 C4 112.2(4) . . ?
O3 C2 C5 110.2(4) . . ?
C1 C2 C5 109.3(4) . . ?
C4 C2 C5 111.3(5) . . ?
C2 O3 H3 109.5 . . ?
C2 C4 H4A 109.5 . . ?
C2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C2 C5 H5A 109.5 . . ?
C2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C7A C6A C11A 120.3(9) . . ?
C7A C6A Se1 118.6(9) . . ?
C11A C6A Se1 120.5(4) . . ?
C6A C7A C8A 120.8(13) . . ?
C6A C7A H7A 119.6 . . ?
C8A C7A H7A 119.6 . . ?
C9A C8A C7A 120.2(13) . . ?
C9A C8A H8A 119.9 . . ?
C7A C8A H8A 119.9 . . ?
C8A C9A C10A 119.7(12) . . ?
C8A C9A H9A 120.2 . . ?
C10A C9A H9A 120.2 . . ?
C9A C10A C11A 120.0(12) . . ?
C9A C10A H10A 120 . . ?
C11A C10A H10A 120 . . ?
C6A C11A C10A 118.0(8) . . ?
C6A C11A C12 121.8(5) . . ?
C10A C11A C12 117.8(8) . . ?
C8B C7B H7B 120.2 . . ?
C9B C8B C7B 120.8(9) . . ?
C9B C8B H8B 119.6 . . ?
C7B C8B H8B 119.6 . . ?
C8B C9B C10B 119.7(9) . . ?
C8B C9B H9B 120.1 . . ?
C10B C9B H9B 120.1 . . ?
C9B C10B H10B 119 . . ?
B21 N20 B51 132.9(4) . . ?
B21 N20 H20A 104 . . ?
B51 N20 H20A 104 . . ?
B21 N20 H20B 104 . . ?
B51 N20 H20B 104 . . ?
H20A N20 H20B 105.5 . . ?
N20 B21 C21 111.8(4) . . ?
N20 B21 C31 109.7(4) . . ?
C21 B21 C31 113.7(4) . . ?
N20 B21 C41 107.2(4) . . ?
C21 B21 C41 101.4(4) . . ?
C31 B21 C41 112.6(4) . . ?
C26 C21 C22 111.2(4) . . ?
C26 C21 B21 129.1(4) . . ?
C22 C21 B21 119.5(4) . . ?
F22 C22 C23 115.7(4) . . ?
F22 C22 C21 118.9(4) . . ?
C23 C22 C21 125.4(4) . . ?
F23 C23 C24 119.7(5) . . ?
F23 C23 C22 121.4(5) . . ?
C24 C23 C22 118.9(5) . . ?
C23 C24 F24 120.1(5) . . ?
C23 C24 C25 119.7(5) . . ?
F24 C24 C25 120.2(5) . . ?
F25 C25 C26 120.6(5) . . ?
F25 C25 C24 120.0(5) . . ?
C26 C25 C24 119.3(5) . . ?
F26 C26 C25 114.9(4) . . ?
F26 C26 C21 119.7(4) . . ?
C25 C26 C21 125.4(5) . . ?
C36 C31 C32 113.1(5) . . ?
C36 C31 B21 121.4(5) . . ?
C32 C31 B21 125.5(5) . . ?
F32 C32 C31 121.1(4) . . ?
F32 C32 C33 115.2(5) . . ?
C31 C32 C33 123.7(6) . . ?
C34 C33 F33 118.9(5) . . ?
C34 C33 C32 121.3(6) . . ?
F33 C33 C32 119.8(6) . . ?
C33 C34 F34 122.3(6) . . ?
C33 C34 C35 118.1(5) . . ?
F34 C34 C35 119.6(6) . . ?
F35 C35 C34 120.5(5) . . ?
F35 C35 C36 119.9(6) . . ?
C34 C35 C36 119.5(5) . . ?
F36 C36 C31 119.9(4) . . ?
F36 C36 C35 115.9(5) . . ?
C31 C36 C35 124.2(6) . . ?
C46 C41 C42 113.1(4) . . ?
C46 C41 B21 121.3(4) . . ?
C42 C41 B21 125.5(4) . . ?
F42 C42 C43 115.6(4) . . ?
F42 C42 C41 121.9(4) . . ?
C43 C42 C41 122.5(5) . . ?
C44 C43 F43 120.4(5) . . ?
C44 C43 C42 120.3(5) . . ?
F43 C43 C42 119.2(5) . . ?
C43 C44 F44 120.5(5) . . ?
C43 C44 C45 119.6(5) . . ?
F44 C44 C45 119.9(5) . . ?
F45 C45 C46 121.3(5) . . ?
F45 C45 C44 120.2(5) . . ?
C46 C45 C44 118.5(5) . . ?
F46 C46 C45 115.3(4) . . ?
F46 C46 C41 118.7(4) . . ?
C45 C46 C41 126.0(5) . . ?
C71 B51 N20 113.0(4) . . ?
C71 B51 C61 114.6(4) . . ?
N20 B51 C61 108.0(4) . . ?
C71 B51 C51 102.2(4) . . ?
N20 B51 C51 107.0(4) . . ?
C61 B51 C51 111.7(4) . . ?
C56 C51 C52 112.5(4) . . ?
C56 C51 B51 119.2(4) . . ?
C52 C51 B51 127.9(4) . . ?
F52 C52 C53 116.2(4) . . ?
F52 C52 C51 120.8(4) . . ?
C53 C52 C51 122.9(5) . . ?
C54 C53 F53 120.4(5) . . ?
C54 C53 C52 121.3(5) . . ?
F53 C53 C52 118.3(5) . . ?
C53 C54 F54 121.0(5) . . ?
C53 C54 C55 119.0(5) . . ?
F54 C54 C55 119.9(5) . . ?
F55 C55 C54 121.1(5) . . ?
F55 C55 C56 120.7(5) . . ?
C54 C55 C56 118.2(5) . . ?
F56 C56 C51 119.2(4) . . ?
F56 C56 C55 114.8(5) . . ?
C51 C56 C55 126.0(5) . . ?
C62 C61 C66 112.4(5) . . ?
C62 C61 B51 120.9(4) . . ?
C66 C61 B51 126.7(5) . . ?
C61 C62 F62 120.0(5) . . ?
C61 C62 C63 125.9(5) . . ?
F62 C62 C63 114.1(5) . . ?
C64 C63 F63 119.8(6) . . ?
C64 C63 C62 119.2(6) . . ?
F63 C63 C62 121.0(5) . . ?
C65 C64 C63 118.6(6) . . ?
C65 C64 F64 120.3(6) . . ?
C63 C64 F64 121.0(6) . . ?
C64 C65 F65 121.0(6) . . ?
C64 C65 C66 120.3(5) . . ?
F65 C65 C66 118.5(6) . . ?
F66 C66 C61 120.7(5) . . ?
F66 C66 C65 115.7(5) . . ?
C61 C66 C65 123.5(6) . . ?
C76 C71 C72 112.3(5) . . ?
C76 C71 B51 128.4(4) . . ?
C72 C71 B51 118.6(4) . . ?
F72 C72 C73 117.3(5) . . ?
F72 C72 C71 118.2(5) . . ?
C73 C72 C71 124.5(5) . . ?
F73 C73 C74 119.6(5) . . ?
F73 C73 C72 119.5(6) . . ?
C74 C73 C72 120.9(5) . . ?
C73 C74 F74 122.1(6) . . ?
C73 C74 C75 119.0(5) . . ?
F74 C74 C75 118.8(6) . . ?
F75 C75 C74 120.8(5) . . ?
F75 C75 C76 120.8(5) . . ?
C74 C75 C76 118.4(5) . . ?
C71 C76 F76 121.9(4) . . ?
C71 C76 C75 124.7(5) . . ?
F76 C76 C75 113.4(5) . . ?


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
C11A C12 N13 C14 -74.8(6) . . . . ?
C11A C12 N13 C15 161.4(5) . . . . ?
C6A Se1 C1 C2 -95.1(4) . . . . ?
Se1 C1 C2 O3 56.5(5) . . . . ?
Se1 C1 C2 C4 -59.2(5) . . . . ?
Se1 C1 C2 C5 176.9(4) . . . . ?
C1 Se1 C6A C7A -52.9(16) . . . . ?
C1 Se1 C6A C11A 118.3(6) . . . . ?
C11A C6A C7A C8A -2(3) . . . . ?
Se1 C6A C7A C8A 168.9(19) . . . . ?
C6A C7A C8A C9A 3(4) . . . . ?
C7A C8A C9A C10A -8(3) . . . . ?
C8A C9A C10A C11A 12(3) . . . . ?
C7A C6A C11A C10A 6.7(19) . . . . ?
Se1 C6A C11A C10A -164.4(11) . . . . ?
C7A C6A C11A C12 168.6(17) . . . . ?
Se1 C6A C11A C12 -2.5(9) . . . . ?
C9A C10A C11A C6A -12(2) . . . . ?
C9A C10A C11A C12 -174.2(14) . . . . ?
N13 C12 C11A C6A -78.6(8) . . . . ?
N13 C12 C11A C10A 83.3(12) . . . . ?
C7B C8B C9B C10B -1(2) . . . . ?
B51 N20 B21 C21 -114.6(5) . . . . ?
B51 N20 B21 C31 12.4(7) . . . . ?
B51 N20 B21 C41 135.0(5) . . . . ?
N20 B21 C21 C26 -8.5(7) . . . . ?
C31 B21 C21 C26 -133.3(5) . . . . ?
C41 B21 C21 C26 105.5(5) . . . . ?
N20 B21 C21 C22 176.4(4) . . . . ?
C31 B21 C21 C22 51.5(6) . . . . ?
C41 B21 C21 C22 -69.7(5) . . . . ?
C26 C21 C22 F22 -179.5(4) . . . . ?
B21 C21 C22 F22 -3.6(6) . . . . ?
C26 C21 C22 C23 0.2(7) . . . . ?
B21 C21 C22 C23 176.1(5) . . . . ?
F22 C22 C23 F23 -1.8(7) . . . . ?
C21 C22 C23 F23 178.5(4) . . . . ?
F22 C22 C23 C24 179.9(4) . . . . ?
C21 C22 C23 C24 0.2(8) . . . . ?
F23 C23 C24 F24 1.3(7) . . . . ?
C22 C23 C24 F24 179.7(5) . . . . ?
F23 C23 C24 C25 -178.7(5) . . . . ?
C22 C23 C24 C25 -0.4(8) . . . . ?
C23 C24 C25 F25 -179.8(5) . . . . ?
F24 C24 C25 F25 0.2(8) . . . . ?
C23 C24 C25 C26 0.2(8) . . . . ?
F24 C24 C25 C26 -179.9(4) . . . . ?
F25 C25 C26 F26 1.8(7) . . . . ?
C24 C25 C26 F26 -178.1(4) . . . . ?
F25 C25 C26 C21 -179.8(4) . . . . ?
C24 C25 C26 C21 0.2(8) . . . . ?
C22 C21 C26 F26 177.9(4) . . . . ?
B21 C21 C26 F26 2.4(7) . . . . ?
C22 C21 C26 C25 -0.4(7) . . . . ?
B21 C21 C26 C25 -175.9(5) . . . . ?
N20 B21 C31 C36 70.2(6) . . . . ?
C21 B21 C31 C36 -163.8(4) . . . . ?
C41 B21 C31 C36 -49.1(6) . . . . ?
N20 B21 C31 C32 -107.7(5) . . . . ?
C21 B21 C31 C32 18.3(6) . . . . ?
C41 B21 C31 C32 133.0(5) . . . . ?
C36 C31 C32 F32 -178.1(4) . . . . ?
B21 C31 C32 F32 -0.1(7) . . . . ?
C36 C31 C32 C33 1.0(7) . . . . ?
B21 C31 C32 C33 179.1(4) . . . . ?
F32 C32 C33 C34 177.2(5) . . . . ?
C31 C32 C33 C34 -2.0(8) . . . . ?
F32 C32 C33 F33 -0.2(7) . . . . ?
C31 C32 C33 F33 -179.4(4) . . . . ?
F33 C33 C34 F34 -0.4(8) . . . . ?
C32 C33 C34 F34 -177.9(4) . . . . ?
F33 C33 C34 C35 -179.8(4) . . . . ?
C32 C33 C34 C35 2.7(8) . . . . ?
C33 C34 C35 F35 178.8(5) . . . . ?
F34 C34 C35 F35 -0.7(8) . . . . ?
C33 C34 C35 C36 -2.7(8) . . . . ?
F34 C34 C35 C36 177.9(4) . . . . ?
C32 C31 C36 F36 -179.8(4) . . . . ?
B21 C31 C36 F36 2.0(7) . . . . ?
C32 C31 C36 C35 -1.1(7) . . . . ?
B21 C31 C36 C35 -179.2(4) . . . . ?
F35 C35 C36 F36 -0.7(7) . . . . ?
C34 C35 C36 F36 -179.2(4) . . . . ?
F35 C35 C36 C31 -179.5(4) . . . . ?
C34 C35 C36 C31 2.0(8) . . . . ?
N20 B21 C41 C46 44.8(6) . . . . ?
C21 B21 C41 C46 -72.6(5) . . . . ?
C31 B21 C41 C46 165.5(4) . . . . ?
N20 B21 C41 C42 -140.5(4) . . . . ?
C21 B21 C41 C42 102.2(5) . . . . ?
C31 B21 C41 C42 -19.8(7) . . . . ?
C46 C41 C42 F42 177.8(4) . . . . ?
B21 C41 C42 F42 2.7(7) . . . . ?
C46 C41 C42 C43 -1.6(7) . . . . ?
B21 C41 C42 C43 -176.7(4) . . . . ?
F42 C42 C43 C44 -179.9(5) . . . . ?
C41 C42 C43 C44 -0.4(8) . . . . ?
F42 C42 C43 F43 -1.0(7) . . . . ?
C41 C42 C43 F43 178.5(4) . . . . ?
F43 C43 C44 F44 2.5(8) . . . . ?
C42 C43 C44 F44 -178.6(4) . . . . ?
F43 C43 C44 C45 -176.9(5) . . . . ?
C42 C43 C44 C45 2.0(8) . . . . ?
C43 C44 C45 F45 179.9(5) . . . . ?
F44 C44 C45 F45 0.5(8) . . . . ?
C43 C44 C45 C46 -1.5(8) . . . . ?
F44 C44 C45 C46 179.1(5) . . . . ?
F45 C45 C46 F46 -2.5(7) . . . . ?
C44 C45 C46 F46 178.9(4) . . . . ?
F45 C45 C46 C41 177.9(4) . . . . ?
C44 C45 C46 C41 -0.8(8) . . . . ?
C42 C41 C46 F46 -177.4(4) . . . . ?
B21 C41 C46 F46 -2.1(7) . . . . ?
C42 C41 C46 C45 2.2(7) . . . . ?
B21 C41 C46 C45 177.6(5) . . . . ?
B21 N20 B51 C71 -96.6(6) . . . . ?
B21 N20 B51 C61 31.2(6) . . . . ?
B21 N20 B51 C51 151.6(4) . . . . ?
C71 B51 C51 C56 -63.5(5) . . . . ?
N20 B51 C51 C56 55.4(6) . . . . ?
C61 B51 C51 C56 173.4(4) . . . . ?
C71 B51 C51 C52 109.1(5) . . . . ?
N20 B51 C51 C52 -131.9(5) . . . . ?
C61 B51 C51 C52 -13.9(7) . . . . ?
C56 C51 C52 F52 177.3(4) . . . . ?
B51 C51 C52 F52 4.3(7) . . . . ?
C56 C51 C52 C53 -0.5(7) . . . . ?
B51 C51 C52 C53 -173.5(4) . . . . ?
F52 C52 C53 C54 -176.7(4) . . . . ?
C51 C52 C53 C54 1.2(8) . . . . ?
F52 C52 C53 F53 2.3(6) . . . . ?
C51 C52 C53 F53 -179.8(4) . . . . ?
F53 C53 C54 F54 -1.3(7) . . . . ?
C52 C53 C54 F54 177.6(4) . . . . ?
F53 C53 C54 C55 -178.7(4) . . . . ?
C52 C53 C54 C55 0.2(8) . . . . ?
C53 C54 C55 F55 178.2(4) . . . . ?
F54 C54 C55 F55 0.8(7) . . . . ?
C53 C54 C55 C56 -2.3(8) . . . . ?
F54 C54 C55 C56 -179.7(4) . . . . ?
C52 C51 C56 F56 -179.4(4) . . . . ?
B51 C51 C56 F56 -5.7(7) . . . . ?
C52 C51 C56 C55 -1.8(7) . . . . ?
B51 C51 C56 C55 172.0(5) . . . . ?
F55 C55 C56 F56 0.5(7) . . . . ?
C54 C55 C56 F56 -179.1(4) . . . . ?
F55 C55 C56 C51 -177.2(5) . . . . ?
C54 C55 C56 C51 3.2(8) . . . . ?
C71 B51 C61 C62 -171.2(4) . . . . ?
N20 B51 C61 C62 62.0(5) . . . . ?
C51 B51 C61 C62 -55.5(6) . . . . ?
C71 B51 C61 C66 9.4(7) . . . . ?
N20 B51 C61 C66 -117.4(5) . . . . ?
C51 B51 C61 C66 125.1(5) . . . . ?
C66 C61 C62 F62 179.4(4) . . . . ?
B51 C61 C62 F62 -0.1(6) . . . . ?
C66 C61 C62 C63 -0.8(7) . . . . ?
B51 C61 C62 C63 179.7(4) . . . . ?
C61 C62 C63 C64 -1.0(8) . . . . ?
F62 C62 C63 C64 178.8(4) . . . . ?
C61 C62 C63 F63 -180.0(4) . . . . ?
F62 C62 C63 F63 -0.2(6) . . . . ?
F63 C63 C64 C65 -179.3(4) . . . . ?
C62 C63 C64 C65 1.7(8) . . . . ?
F63 C63 C64 F64 -3.3(7) . . . . ?
C62 C63 C64 F64 177.7(4) . . . . ?
C63 C64 C65 F65 176.2(4) . . . . ?
F64 C64 C65 F65 0.1(8) . . . . ?
C63 C64 C65 C66 -0.6(8) . . . . ?
F64 C64 C65 C66 -176.6(4) . . . . ?
C62 C61 C66 F66 -176.1(4) . . . . ?
B51 C61 C66 F66 3.4(7) . . . . ?
C62 C61 C66 C65 2.0(7) . . . . ?
B51 C61 C66 C65 -178.5(4) . . . . ?
C64 C65 C66 F66 176.7(4) . . . . ?
F65 C65 C66 F66 -0.1(7) . . . . ?
C64 C65 C66 C61 -1.4(8) . . . . ?
F65 C65 C66 C61 -178.2(4) . . . . ?
N20 B51 C71 C76 -8.8(7) . . . . ?
C61 B51 C71 C76 -133.1(5) . . . . ?
C51 B51 C71 C76 105.8(5) . . . . ?
N20 B51 C71 C72 -179.1(4) . . . . ?
C61 B51 C71 C72 56.7(6) . . . . ?
C51 B51 C71 C72 -64.4(5) . . . . ?
C76 C71 C72 F72 -176.9(4) . . . . ?
B51 C71 C72 F72 -5.2(7) . . . . ?
C76 C71 C72 C73 3.6(7) . . . . ?
B51 C71 C72 C73 175.4(5) . . . . ?
F72 C72 C73 F73 -2.0(7) . . . . ?
C71 C72 C73 F73 177.5(4) . . . . ?
F72 C72 C73 C74 -179.0(5) . . . . ?
C71 C72 C73 C74 0.4(8) . . . . ?
F73 C73 C74 F74 1.1(8) . . . . ?
C72 C73 C74 F74 178.1(5) . . . . ?
F73 C73 C74 C75 179.0(5) . . . . ?
C72 C73 C74 C75 -4.0(8) . . . . ?
C73 C74 C75 F75 -178.2(5) . . . . ?
F74 C74 C75 F75 -0.3(8) . . . . ?
C73 C74 C75 C76 3.2(8) . . . . ?
F74 C74 C75 C76 -178.9(5) . . . . ?
C72 C71 C76 F76 174.5(4) . . . . ?
B51 C71 C76 F76 3.8(8) . . . . ?
C72 C71 C76 C75 -4.5(7) . . . . ?
B51 C71 C76 C75 -175.2(5) . . . . ?
F75 C75 C76 C71 -177.3(5) . . . . ?
C74 C75 C76 C71 1.3(8) . . . . ?
F75 C75 C76 F76 3.6(7) . . . . ?
C74 C75 C76 F76 -177.8(4) . . . . ?
_database_code_depnum_ccdc_archive 'CCDC 1006893'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_Sn{NR2}2{TePh}2

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C24 H46 N2 Si4 Sn Te2'
_chemical_formula_sum            'C24 H46 N2 Si4 Sn Te2'
_chemical_formula_weight         848.88
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   8.7218(3)
_cell_length_b                   17.9841(5)
_cell_length_c                   21.6618(6)
_cell_angle_alpha                90
_cell_angle_beta                 98.7190(10)
_cell_angle_gamma                90
_cell_volume                     3358.47(18)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9165
_cell_measurement_theta_min      2.62
_cell_measurement_theta_max      27.44
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.57
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.31
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1656
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    2.622
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_absorpt_correction_T_min  0.317
_exptl_absorpt_correction_T_max  0.444


#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_detector                 'CCD plate'
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_reflns_av_R_equivalents  0.0273
_diffrn_reflns_av_unetI/netI     0.0266
_diffrn_reflns_number            14291
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.96
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_reflns_number_total             3815
_reflns_number_gt                3501
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2 (Bruker, 2006)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2006)'
_computing_data_reduction        'Bruker APEX2 (Bruker, 2006)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  
;
           WinGX publication routines (Farrugia, 2012),
           CRYSCAL (T. Roisnel, local program)
;

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0195P)²+5.3463P] 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_number_reflns         3815
_refine_ls_number_parameters     156
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0273
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0529
_refine_ls_wR_factor_gt          0.0516
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.673
_refine_diff_density_min         -0.601
_refine_diff_density_rms         0.084

# End of res file
#----------------------------------------------------------------------------#

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.5308 1.6751 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'


loop_
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0 0.295709(12) 0.25 0.01366(6) Uani 1 2 d S . .
Te1 Te 0.26097(2) 0.385352(10) 0.262079(8) 0.02702(6) Uani 1 1 d . . .
Si1 Si -0.14740(8) 0.16439(4) 0.15325(3) 0.01730(14) Uani 1 1 d . . .
Si2 Si 0.12032(8) 0.25439(4) 0.11619(3) 0.01788(14) Uani 1 1 d . . .
N1 N -0.0020(2) 0.23172(11) 0.17088(9) 0.0158(4) Uani 1 1 d . . .
C2 C -0.2708(3) 0.15480(16) 0.21574(12) 0.0264(6) Uani 1 1 d . . .
H2A H -0.2057 0.1414 0.2551 0.04 Uiso 1 1 calc R . .
H2B H -0.3484 0.1159 0.2041 0.04 Uiso 1 1 calc R . .
H2C H -0.3232 0.2021 0.2209 0.04 Uiso 1 1 calc R . .
C3 C -0.2823(3) 0.19126(16) 0.08081(11) 0.0259(6) Uani 1 1 d . . .
H3A H -0.3186 0.2423 0.0851 0.039 Uiso 1 1 calc R . .
H3B H -0.3714 0.1574 0.0749 0.039 Uiso 1 1 calc R . .
H3C H -0.2274 0.1881 0.0446 0.039 Uiso 1 1 calc R . .
C4 C -0.0630(3) 0.06976(15) 0.14562(13) 0.0301(6) Uani 1 1 d . . .
H4A H 0.0056 0.0709 0.1138 0.045 Uiso 1 1 calc R . .
H4B H -0.1468 0.034 0.1334 0.045 Uiso 1 1 calc R . .
H4C H -0.0035 0.0548 0.1858 0.045 Uiso 1 1 calc R . .
C5 C 0.0854(3) 0.19431(17) 0.04458(12) 0.0302(6) Uani 1 1 d . . .
H5A H 0.1001 0.142 0.0567 0.045 Uiso 1 1 calc R . .
H5B H 0.1589 0.2078 0.0164 0.045 Uiso 1 1 calc R . .
H5C H -0.0208 0.2018 0.0233 0.045 Uiso 1 1 calc R . .
C6 C 0.0923(4) 0.35155(16) 0.08743(13) 0.0313(6) Uani 1 1 d . . .
H6A H -0.0159 0.3587 0.0683 0.047 Uiso 1 1 calc R . .
H6B H 0.1606 0.3611 0.0563 0.047 Uiso 1 1 calc R . .
H6C H 0.1176 0.3861 0.1225 0.047 Uiso 1 1 calc R . .
C7 C 0.3307(3) 0.24120(16) 0.14619(12) 0.0267(6) Uani 1 1 d . . .
H7A H 0.3604 0.2729 0.1828 0.04 Uiso 1 1 calc R . .
H7B H 0.3921 0.2547 0.1136 0.04 Uiso 1 1 calc R . .
H7C H 0.35 0.189 0.1579 0.04 Uiso 1 1 calc R . .
C11 C 0.2292(3) 0.43659(14) 0.34740(12) 0.0226(5) Uani 1 1 d . . .
C12 C 0.1239(3) 0.49406(15) 0.34850(13) 0.0307(6) Uani 1 1 d . . .
H12 H 0.0617 0.5099 0.311 0.037 Uiso 1 1 calc R . .
C13 C 0.1097(4) 0.52845(16) 0.40501(15) 0.0405(7) Uani 1 1 d . . .
H13 H 0.0355 0.5669 0.4061 0.049 Uiso 1 1 calc R . .
C14 C 0.2025(4) 0.50706(17) 0.45922(14) 0.0426(8) Uani 1 1 d . . .
H14 H 0.1922 0.5307 0.4976 0.051 Uiso 1 1 calc R . .
C15 C 0.3103(4) 0.45124(16) 0.45776(13) 0.0380(7) Uani 1 1 d . . .
H15 H 0.3758 0.4372 0.4951 0.046 Uiso 1 1 calc R . .
C16 C 0.3236(3) 0.41553(15) 0.40219(13) 0.0293(6) Uani 1 1 d . . .
H16 H 0.3971 0.3767 0.4015 0.035 Uiso 1 1 calc R . .





#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 2.0623(19) . ?
Sn1 N1 2.0624(19) 2 ?
Sn1 Te1 2.7690(2) 2 ?
Sn1 Te1 2.7690(2) . ?
Te1 C11 2.121(2) . ?
Si1 N1 1.753(2) . ?
Si1 C2 1.860(3) . ?
Si1 C4 1.872(3) . ?
Si1 C3 1.876(3) . ?
Si2 N1 1.758(2) . ?
Si2 C6 1.859(3) . ?
Si2 C7 1.866(3) . ?
Si2 C5 1.877(3) . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C11 C12 1.385(4) . ?
C11 C16 1.390(4) . ?
C12 C13 1.394(4) . ?
C12 H12 0.95 . ?
C13 C14 1.376(5) . ?
C13 H13 0.95 . ?
C14 C15 1.379(5) . ?
C14 H14 0.95 . ?
C15 C16 1.384(4) . ?
C15 H15 0.95 . ?
C16 H16 0.95 . ?


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 112.17(11) . 2 ?
N1 Sn1 Te1 110.07(5) . 2 ?
N1 Sn1 Te1 107.85(5) 2 2 ?
N1 Sn1 Te1 107.85(5) . . ?
N1 Sn1 Te1 110.07(5) 2 . ?
Te1 Sn1 Te1 108.788(11) 2 . ?
C11 Te1 Sn1 96.97(7) . . ?
N1 Si1 C2 112.63(11) . . ?
N1 Si1 C4 111.46(12) . . ?
C2 Si1 C4 104.99(13) . . ?
N1 Si1 C3 110.21(11) . . ?
C2 Si1 C3 105.89(12) . . ?
C4 Si1 C3 111.44(13) . . ?
N1 Si2 C6 112.43(11) . . ?
N1 Si2 C7 113.62(11) . . ?
C6 Si2 C7 107.97(14) . . ?
N1 Si2 C5 112.61(11) . . ?
C6 Si2 C5 105.52(13) . . ?
C7 Si2 C5 104.02(13) . . ?
Si1 N1 Si2 120.42(11) . . ?
Si1 N1 Sn1 118.74(10) . . ?
Si2 N1 Sn1 120.08(10) . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4A 109.5 . . ?
Si1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
Si1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
Si2 C5 H5A 109.5 . . ?
Si2 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
Si2 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C12 C11 C16 119.8(2) . . ?
C12 C11 Te1 120.91(19) . . ?
C16 C11 Te1 119.2(2) . . ?
C11 C12 C13 119.6(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C14 C13 C12 120.4(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C13 C14 C15 119.9(3) . . ?
C13 C14 H14 120 . . ?
C15 C14 H14 120 . . ?
C14 C15 C16 120.3(3) . . ?
C14 C15 H15 119.8 . . ?
C16 C15 H15 119.8 . . ?
C15 C16 C11 120.0(3) . . ?
C15 C16 H16 120 . . ?
C11 C16 H16 120 . . ?


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
N1 Sn1 Te1 C11 -177.44(9) . . . . ?
N1 Sn1 Te1 C11 -54.77(9) 2 . . . ?
Te1 Sn1 Te1 C11 63.20(7) 2 . . . ?
C2 Si1 N1 Si2 -175.86(13) . . . . ?
C4 Si1 N1 Si2 66.43(16) . . . . ?
C3 Si1 N1 Si2 -57.85(16) . . . . ?
C2 Si1 N1 Sn1 -5.84(16) . . . . ?
C4 Si1 N1 Sn1 -123.56(13) . . . . ?
C3 Si1 N1 Sn1 112.16(13) . . . . ?
C6 Si2 N1 Si1 114.39(15) . . . . ?
C7 Si2 N1 Si1 -122.60(14) . . . . ?
C5 Si2 N1 Si1 -4.66(18) . . . . ?
C6 Si2 N1 Sn1 -55.49(16) . . . . ?
C7 Si2 N1 Sn1 67.52(15) . . . . ?
C5 Si2 N1 Sn1 -174.54(12) . . . . ?
N1 Sn1 N1 Si1 54.52(9) 2 . . . ?
Te1 Sn1 N1 Si1 -65.56(11) 2 . . . ?
Te1 Sn1 N1 Si1 175.89(9) . . . . ?
N1 Sn1 N1 Si2 -135.43(13) 2 . . . ?
Te1 Sn1 N1 Si2 104.49(10) 2 . . . ?
Te1 Sn1 N1 Si2 -14.06(12) . . . . ?
Sn1 Te1 C11 C12 -78.9(2) . . . . ?
Sn1 Te1 C11 C16 105.7(2) . . . . ?
C16 C11 C12 C13 -2.3(4) . . . . ?
Te1 C11 C12 C13 -177.7(2) . . . . ?
C11 C12 C13 C14 1.8(5) . . . . ?
C12 C13 C14 C15 0.0(5) . . . . ?
C13 C14 C15 C16 -1.3(5) . . . . ?
C14 C15 C16 C11 0.8(4) . . . . ?
C12 C11 C16 C15 1.0(4) . . . . ?
Te1 C11 C16 C15 176.4(2) . . . . ?


#----------------------------------------------------------------------------#
# END OF CIF FILE FOR Sn{NR2}2{TePh}2                                        #
#----------------------------------------------------------------------------#

##############################################################################
#         E N D    O F    G L O B A L    C I F    F I L E                    #
##############################################################################
_database_code_depnum_ccdc_archive 'CCDC 1006894'
