# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011


data_global

_journal_coden_Cambridge         222
_journal_volume                  ?
_journal_page_first              ?
_journal_year                    ?

loop_
_publ_author_name
'Abrahams, Brendan F'
'Grannas, Martin'
'Hudson, Timothy'
'Hughes, Steven'
'Pranoto, Naomi'
'Robson, Richard'

_publ_contact_author_name        'Dr Brendan F Abrahams'
_publ_contact_author_email       bfa@unimelb.edu.au

_publ_section_title              
;
Synthesis, structure and
host-guest properties of (Et4N)2[SnIVCaII(chloranilate)4],
a new type of robust microporous coordination polymer with
a 2D square grid structure.

;

# Attachment '- bfasn1final.cif'

data_shelxl1
_database_code_depnum_ccdc_archive 'CCDC 826950'
#TrackingRef '- bfasn1final.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H40 Ca Cl8 N2 O16 Sn'
_chemical_formula_weight         1247.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I422

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

_cell_length_a                   11.9264(1)
_cell_length_b                   11.9264(1)
_cell_length_c                   20.0544(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2852.52(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    3331
_cell_measurement_theta_min      3.15
_cell_measurement_theta_max      31.03

_exptl_crystal_description       'square plate'
_exptl_crystal_colour            'deep purple'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.452
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1256
_exptl_absorpt_coefficient_mu    0.972
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.815
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4105
_diffrn_reflns_av_R_equivalents  0.0199
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.16
_diffrn_reflns_theta_max         28.00
_reflns_number_total             1715
_reflns_number_gt                1650
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
(compiled Aug 27 2010,11:50:40)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0185P)^2^+0.8833P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.500(19)
_refine_ls_number_reflns         1715
_refine_ls_number_parameters     99
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0201
_refine_ls_R_factor_gt           0.0182
_refine_ls_wR_factor_ref         0.0441
_refine_ls_wR_factor_gt          0.0432
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_restrained_S_all      1.094
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O2 O -0.41799(10) 0.34245(10) 0.05812(5) 0.0128(3) Uani 1 1 d . . .
C2 C -0.28261(14) 0.19932(14) 0.06317(7) 0.0120(3) Uani 1 1 d . . .
C3 C -0.33655(14) 0.29211(13) 0.03395(7) 0.0107(3) Uani 1 1 d . . .
Sn1 Sn 0.0000 0.0000 0.0000 0.00826(8) Uani 1 8 d S . .
Cl1 Cl -0.33281(4) 0.14872(4) 0.13843(2) 0.01763(10) Uani 1 1 d . . .
N1 N 0.0000 0.0000 0.25408(12) 0.0146(5) Uani 1 4 d S . .
O1 O -0.13983(10) 0.06437(9) 0.05756(5) 0.0107(2) Uani 1 1 d . . .
C1 C -0.19162(13) 0.14852(14) 0.03338(7) 0.0101(3) Uani 1 1 d . . .
Ca1 Ca -0.5000 0.5000 0.0000 0.00763(16) Uani 1 8 d S . .
C4 C -0.0962(3) -0.0332(3) 0.20860(16) 0.0194(8) Uani 0.50 1 d P A 1
H4A H -0.1155 0.0318 0.1801 0.023 Uiso 0.50 1 calc PR A 1
H4B H -0.0704 -0.0943 0.1789 0.023 Uiso 0.50 1 calc PR A 1
C5 C -0.2011(13) -0.0716(17) 0.2442(5) 0.028(2) Uani 0.50 1 d P A 1
H5A H -0.2585 -0.0915 0.2113 0.042 Uiso 0.50 1 calc PR A 1
H5B H -0.2290 -0.0109 0.2727 0.042 Uiso 0.50 1 calc PR A 1
H5C H -0.1837 -0.1372 0.2718 0.042 Uiso 0.50 1 calc PR A 1
C6 C -0.0963(4) -0.0334(3) 0.29946(17) 0.0256(10) Uani 0.50 1 d P A 2
H6A H -0.0709 -0.0958 0.3283 0.031 Uiso 0.50 1 calc PR A 2
H6B H -0.1142 0.0309 0.3288 0.031 Uiso 0.50 1 calc PR A 2
C7 C -0.2023(15) -0.0693(19) 0.2646(5) 0.036(3) Uani 0.50 1 d P A 2
H7A H -0.2592 -0.0892 0.2978 0.054 Uiso 0.50 1 calc PR A 2
H7B H -0.1866 -0.1346 0.2363 0.054 Uiso 0.50 1 calc PR A 2
H7C H -0.2300 -0.0076 0.2368 0.054 Uiso 0.50 1 calc PR A 2

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O2 0.0131(6) 0.0134(6) 0.0120(5) 0.0018(5) 0.0030(5) 0.0031(5)
C2 0.0135(8) 0.0134(8) 0.0090(7) 0.0030(6) 0.0019(6) 0.0012(7)
C3 0.0107(8) 0.0118(7) 0.0098(7) -0.0009(6) 0.0008(6) -0.0011(7)
Sn1 0.00790(10) 0.00790(10) 0.00899(13) 0.000 0.000 0.000
Cl1 0.0188(2) 0.0203(2) 0.01382(19) 0.00713(17) 0.00778(16) 0.00596(17)
N1 0.0178(8) 0.0178(8) 0.0083(11) 0.000 0.000 0.000
O1 0.0109(6) 0.0111(6) 0.0100(5) 0.0021(5) 0.0006(5) 0.0017(5)
C1 0.0098(7) 0.0101(7) 0.0104(7) -0.0008(6) -0.0018(6) -0.0015(7)
Ca1 0.0068(2) 0.0068(2) 0.0092(4) 0.000 0.000 0.000
C4 0.0239(19) 0.0174(18) 0.0169(16) -0.0013(14) -0.0089(15) -0.0005(14)
C5 0.015(4) 0.021(3) 0.048(6) -0.003(6) -0.005(4) -0.002(3)
C6 0.039(2) 0.022(2) 0.0157(16) 0.0066(15) 0.0147(17) 0.0052(16)
C7 0.026(4) 0.029(4) 0.052(6) 0.006(7) 0.018(5) -0.001(3)

_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
O2 C3 1.240(2) . ?
O2 Ca1 2.4179(12) . ?
C2 C1 1.379(2) . ?
C2 C3 1.408(2) . ?
C2 Cl1 1.7322(15) . ?
C3 C3 1.554(3) 8 ?
C3 Ca1 3.2266(17) . ?
Sn1 O1 2.1686(11) 2 ?
Sn1 O1 2.1686(11) 3 ?
Sn1 O1 2.1686(11) 6 ?
Sn1 O1 2.1686(11) 5 ?
Sn1 O1 2.1686(11) 7 ?
Sn1 O1 2.1686(11) 4 ?
Sn1 O1 2.1686(11) . ?
Sn1 O1 2.1686(11) 8 ?
N1 C4 1.518(4) . ?
N1 C4 1.518(4) 7 ?
N1 C4 1.518(4) 6 ?
N1 C4 1.518(4) 3 ?
N1 C6 1.519(4) 3 ?
N1 C6 1.519(4) 6 ?
N1 C6 1.519(4) . ?
N1 C6 1.519(4) 7 ?
O1 C1 1.274(2) . ?
C1 C1 1.524(3) 8 ?
Ca1 O2 2.4179(12) 4_455 ?
Ca1 O2 2.4179(12) 7_565 ?
Ca1 O2 2.4179(12) 3_465 ?
Ca1 O2 2.4179(12) 6_455 ?
Ca1 O2 2.4179(12) 2_565 ?
Ca1 O2 2.4179(12) 8 ?
Ca1 O2 2.4179(12) 5_465 ?
Ca1 C3 3.2266(17) 4_455 ?
Ca1 C3 3.2266(17) 6_455 ?
Ca1 C3 3.2266(17) 2_565 ?
Ca1 C3 3.2266(17) 7_565 ?
C4 C5 1.511(15) . ?
C6 C7 1.507(17) . ?

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
C3 O2 Ca1 120.30(10) . . ?
C1 C2 C3 121.65(14) . . ?
C1 C2 Cl1 119.76(13) . . ?
C3 C2 Cl1 118.59(13) . . ?
O2 C3 C2 125.14(14) . . ?
O2 C3 C3 116.38(9) . 8 ?
C2 C3 C3 118.48(9) . 8 ?
O2 C3 Ca1 40.32(8) . . ?
C2 C3 Ca1 165.46(11) . . ?
C3 C3 Ca1 76.06(3) 8 . ?
O1 Sn1 O1 138.54(6) 2 3 ?
O1 Sn1 O1 145.87(6) 2 6 ?
O1 Sn1 O1 73.54(3) 3 6 ?
O1 Sn1 O1 73.54(3) 2 5 ?
O1 Sn1 O1 74.86(6) 3 5 ?
O1 Sn1 O1 138.54(6) 6 5 ?
O1 Sn1 O1 74.86(6) 2 7 ?
O1 Sn1 O1 73.54(3) 3 7 ?
O1 Sn1 O1 115.68(6) 6 7 ?
O1 Sn1 O1 79.47(6) 5 7 ?
O1 Sn1 O1 115.68(6) 2 4 ?
O1 Sn1 O1 79.47(6) 3 4 ?
O1 Sn1 O1 74.86(6) 6 4 ?
O1 Sn1 O1 73.54(3) 5 4 ?
O1 Sn1 O1 145.87(6) 7 4 ?
O1 Sn1 O1 79.47(6) 2 . ?
O1 Sn1 O1 115.68(6) 3 . ?
O1 Sn1 O1 73.54(3) 6 . ?
O1 Sn1 O1 145.87(6) 5 . ?
O1 Sn1 O1 73.54(3) 7 . ?
O1 Sn1 O1 138.54(6) 4 . ?
O1 Sn1 O1 73.54(3) 2 8 ?
O1 Sn1 O1 145.87(6) 3 8 ?
O1 Sn1 O1 79.47(6) 6 8 ?
O1 Sn1 O1 115.68(6) 5 8 ?
O1 Sn1 O1 138.54(6) 7 8 ?
O1 Sn1 O1 73.54(3) 4 8 ?
O1 Sn1 O1 74.86(6) . 8 ?
C4 N1 C4 68.85(16) . 7 ?
C4 N1 C4 68.85(16) . 6 ?
C4 N1 C4 106.2(3) 7 6 ?
C4 N1 C4 106.2(3) . 3 ?
C4 N1 C4 68.85(16) 7 3 ?
C4 N1 C4 68.85(16) 6 3 ?
C4 N1 C6 179.9(3) . 3 ?
C4 N1 C6 111.2(2) 7 3 ?
C4 N1 C6 111.0(2) 6 3 ?
C4 N1 C6 73.72(18) 3 3 ?
C4 N1 C6 111.0(2) . 6 ?
C4 N1 C6 179.9(3) 7 6 ?
C4 N1 C6 73.72(18) 6 6 ?
C4 N1 C6 111.2(2) 3 6 ?
C6 N1 C6 68.96(17) 3 6 ?
C4 N1 C6 73.72(18) . . ?
C4 N1 C6 111.0(2) 7 . ?
C4 N1 C6 111.2(2) 6 . ?
C4 N1 C6 179.9(3) 3 . ?
C6 N1 C6 106.4(3) 3 . ?
C6 N1 C6 68.96(17) 6 . ?
C4 N1 C6 111.2(2) . 7 ?
C4 N1 C6 73.72(18) 7 7 ?
C4 N1 C6 179.9(3) 6 7 ?
C4 N1 C6 111.0(2) 3 7 ?
C6 N1 C6 68.96(17) 3 7 ?
C6 N1 C6 106.4(3) 6 7 ?
C6 N1 C6 68.96(17) . 7 ?
C1 O1 Sn1 116.68(9) . . ?
O1 C1 C2 124.24(14) . . ?
O1 C1 C1 115.88(8) . 8 ?
C2 C1 C1 119.87(9) . 8 ?
O2 Ca1 O2 149.44(6) 4_455 7_565 ?
O2 Ca1 O2 132.28(6) 4_455 3_465 ?
O2 Ca1 O2 76.56(2) 7_565 3_465 ?
O2 Ca1 O2 66.65(5) 4_455 6_455 ?
O2 Ca1 O2 122.36(5) 7_565 6_455 ?
O2 Ca1 O2 76.56(2) 3_465 6_455 ?
O2 Ca1 O2 78.00(6) 4_455 . ?
O2 Ca1 O2 76.56(2) 7_565 . ?
O2 Ca1 O2 122.36(5) 3_465 . ?
O2 Ca1 O2 76.56(2) 6_455 . ?
O2 Ca1 O2 122.36(5) 4_455 2_565 ?
O2 Ca1 O2 66.65(5) 7_565 2_565 ?
O2 Ca1 O2 78.00(6) 3_465 2_565 ?
O2 Ca1 O2 149.44(6) 6_455 2_565 ?
O2 Ca1 O2 132.28(6) . 2_565 ?
O2 Ca1 O2 76.56(2) 4_455 8 ?
O2 Ca1 O2 78.00(6) 7_565 8 ?
O2 Ca1 O2 149.44(6) 3_465 8 ?
O2 Ca1 O2 132.28(6) 6_455 8 ?
O2 Ca1 O2 66.65(5) . 8 ?
O2 Ca1 O2 76.56(2) 2_565 8 ?
O2 Ca1 O2 76.56(2) 4_455 5_465 ?
O2 Ca1 O2 132.28(6) 7_565 5_465 ?
O2 Ca1 O2 66.65(5) 3_465 5_465 ?
O2 Ca1 O2 78.00(6) 6_455 5_465 ?
O2 Ca1 O2 149.44(6) . 5_465 ?
O2 Ca1 O2 76.56(2) 2_565 5_465 ?
O2 Ca1 O2 122.36(5) 8 5_465 ?
O2 Ca1 C3 19.39(4) 4_455 4_455 ?
O2 Ca1 C3 151.89(4) 7_565 4_455 ?
O2 Ca1 C3 117.03(4) 3_465 4_455 ?
O2 Ca1 C3 47.26(4) 6_455 4_455 ?
O2 Ca1 C3 75.46(4) . 4_455 ?
O2 Ca1 C3 137.72(4) 2_565 4_455 ?
O2 Ca1 C3 93.26(4) 8 4_455 ?
O2 Ca1 C3 74.91(4) 5_465 4_455 ?
O2 Ca1 C3 47.26(4) 4_455 6_455 ?
O2 Ca1 C3 137.72(4) 7_565 6_455 ?
O2 Ca1 C3 93.26(4) 3_465 6_455 ?
O2 Ca1 C3 19.39(4) 6_455 6_455 ?
O2 Ca1 C3 74.91(4) . 6_455 ?
O2 Ca1 C3 151.89(4) 2_565 6_455 ?
O2 Ca1 C3 117.03(4) 8 6_455 ?
O2 Ca1 C3 75.46(4) 5_465 6_455 ?
C3 Ca1 C3 27.88(5) 4_455 6_455 ?
O2 Ca1 C3 137.72(4) 4_455 2_565 ?
O2 Ca1 C3 47.26(4) 7_565 2_565 ?
O2 Ca1 C3 75.46(4) 3_465 2_565 ?
O2 Ca1 C3 151.89(4) 6_455 2_565 ?
O2 Ca1 C3 117.03(4) . 2_565 ?
O2 Ca1 C3 19.39(4) 2_565 2_565 ?
O2 Ca1 C3 74.91(4) 8 2_565 ?
O2 Ca1 C3 93.26(4) 5_465 2_565 ?
C3 Ca1 C3 155.63(5) 4_455 2_565 ?
C3 Ca1 C3 166.66(5) 6_455 2_565 ?
O2 Ca1 C3 151.89(4) 4_455 7_565 ?
O2 Ca1 C3 19.39(4) 7_565 7_565 ?
O2 Ca1 C3 74.91(4) 3_465 7_565 ?
O2 Ca1 C3 137.72(4) 6_455 7_565 ?
O2 Ca1 C3 93.26(4) . 7_565 ?
O2 Ca1 C3 47.26(4) 2_565 7_565 ?
O2 Ca1 C3 75.46(4) 8 7_565 ?
O2 Ca1 C3 117.03(4) 5_465 7_565 ?
C3 Ca1 C3 166.66(5) 4_455 7_565 ?
C3 Ca1 C3 155.63(5) 6_455 7_565 ?
C3 Ca1 C3 27.88(5) 2_565 7_565 ?
C5 C4 N1 114.9(5) . . ?
C7 C6 N1 115.5(5) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.432
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.050

# Attachment '- sncacs2bfinal.cif'

data_shelxl2
_database_code_depnum_ccdc_archive 'CCDC 826951'
#TrackingRef '- sncacs2bfinal.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C42 H40 Ca Cl8 N2 O16 S4 Sn'
_chemical_formula_weight         1399.37

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I422

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

_cell_length_a                   11.9699(3)
_cell_length_b                   11.9699(3)
_cell_length_c                   20.3410(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2914.43(17)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    1934
_cell_measurement_theta_min      3.12
_cell_measurement_theta_max      29.09

_exptl_crystal_description       'square plate'
_exptl_crystal_colour            'deep purple'
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.595
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_absorpt_coefficient_mu    1.099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.89878
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4255
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         28.00
_reflns_number_total             1685
_reflns_number_gt                1560
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;

_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;

_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0424P)^2^+6.6887P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.36(4)
_refine_ls_number_reflns         1685
_refine_ls_number_parameters     118
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.5000 0.5000 0.2461(3) 0.0140(11) Uani 1 4 d S . .
C4 C 0.5985(7) 0.5276(7) 0.2008(4) 0.023(2) Uani 0.50 1 d PD A 1
H4A H 0.6150 0.4611 0.1736 0.028 Uiso 0.50 1 calc PR A 1
H4B H 0.5755 0.5884 0.1707 0.028 Uiso 0.50 1 calc PR A 1
C5 C 0.7040(13) 0.562(2) 0.2350(10) 0.037(5) Uani 0.50 1 d PD A 1
H5A H 0.7609 0.5812 0.2022 0.056 Uiso 0.50 1 calc PR A 1
H5B H 0.7309 0.5010 0.2626 0.056 Uiso 0.50 1 calc PR A 1
H5C H 0.6890 0.6280 0.2625 0.056 Uiso 0.50 1 calc PR A 1
C6 C 0.5977(6) 0.5276(6) 0.2910(4) 0.0170(18) Uani 0.50 1 d PD A 2
H6A H 0.5770 0.5922 0.3189 0.020 Uiso 0.50 1 calc PR A 2
H6B H 0.6113 0.4632 0.3205 0.020 Uiso 0.50 1 calc PR A 2
C7 C 0.7051(12) 0.555(2) 0.2549(8) 0.022(4) Uani 0.50 1 d PD A 2
H7A H 0.7639 0.5724 0.2868 0.033 Uiso 0.50 1 calc PR A 2
H7B H 0.6930 0.6194 0.2261 0.033 Uiso 0.50 1 calc PR A 2
H7C H 0.7279 0.4904 0.2284 0.033 Uiso 0.50 1 calc PR A 2
S1 S 0.9063(5) 0.5842(5) 0.0879(4) 0.050(2) Uani 0.259(5) 1 d PD . .
S2 S 0.9670(10) 0.5286(9) 0.0323(6) 0.116(6) Uani 0.241(5) 1 d PD . .
Sn1 Sn 1.0000 1.0000 0.0000 0.00980(18) Uani 1 8 d S . .
Cl1 Cl 0.68489(9) 0.83365(9) 0.14333(4) 0.0222(2) Uani 1 1 d . . .
O2 O 0.5877(2) 0.6528(2) 0.05911(12) 0.0132(6) Uani 1 1 d . . .
O1 O 0.8630(2) 0.9322(2) 0.05782(11) 0.0115(6) Uani 1 1 d . . .
C3 C 0.6669(3) 0.7041(3) 0.03488(15) 0.0121(8) Uani 1 1 d . . .
C2 C 0.7251(3) 0.7934(3) 0.06498(16) 0.0136(7) Uani 1 1 d . . .
C1 C 0.8107(3) 0.8488(3) 0.03398(15) 0.0123(8) Uani 1 1 d . . .
Ca1 Ca 0.5000 0.5000 0.0000 0.0079(3) Uani 1 8 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0160(16) 0.0160(16) 0.010(2) 0.000 0.000 0.000
C4 0.033(5) 0.018(5) 0.018(3) 0.005(3) 0.017(3) 0.005(3)
C5 0.022(8) 0.035(7) 0.055(12) 0.029(10) 0.014(7) 0.013(6)
C6 0.021(4) 0.012(4) 0.018(3) 0.003(3) -0.007(3) 0.001(3)
C7 0.007(6) 0.025(7) 0.035(9) 0.007(7) -0.008(5) -0.007(4)
S1 0.028(3) 0.027(3) 0.095(5) 0.028(3) -0.029(3) -0.007(2)
S2 0.085(10) 0.083(11) 0.179(12) 0.047(8) -0.047(7) -0.010(5)
Sn1 0.0084(2) 0.0084(2) 0.0125(3) 0.000 0.000 0.000
Cl1 0.0241(5) 0.0264(6) 0.0161(4) -0.0092(4) 0.0092(4) -0.0122(4)
O2 0.0108(13) 0.0124(13) 0.0164(12) -0.0021(10) 0.0022(10) -0.0038(10)
O1 0.0116(13) 0.0117(13) 0.0114(11) -0.0021(10) -0.0011(10) -0.0017(9)
C3 0.0147(18) 0.0082(17) 0.0133(15) -0.0010(13) 0.0041(13) 0.0017(15)
C2 0.014(2) 0.0139(19) 0.0125(14) -0.0039(14) 0.0028(14) -0.0016(14)
C1 0.0102(17) 0.0130(19) 0.0138(15) 0.0012(14) -0.0019(13) -0.0008(15)
Ca1 0.0061(5) 0.0061(5) 0.0114(7) 0.000 0.000 0.000

_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
N1 C6 1.521(8) . ?
N1 C6 1.521(8) 7_655 ?
N1 C6 1.521(8) 6_565 ?
N1 C6 1.521(8) 3_665 ?
N1 C4 1.531(8) 3_665 ?
N1 C4 1.531(8) 6_565 ?
N1 C4 1.531(8) . ?
N1 C4 1.531(8) 7_655 ?
C4 C5 1.500(15) . ?
C6 C7 1.517(14) . ?
S1 S2 1.500(12) . ?
S1 S2 2.324(12) 3_765 ?
S2 S2 1.04(2) 3_765 ?
S2 S2 1.48(3) 2_565 ?
S2 S2 1.53(3) 4_755 ?
S2 S1 2.324(12) 3_765 ?
Sn1 O1 2.175(2) 5 ?
Sn1 O1 2.175(2) 3_775 ?
Sn1 O1 2.175(2) 6_575 ?
Sn1 O1 2.175(2) 2_575 ?
Sn1 O1 2.175(2) 8_775 ?
Sn1 O1 2.175(2) 7_755 ?
Sn1 O1 2.175(2) 4_755 ?
Sn1 O1 2.175(2) . ?
Cl1 C2 1.733(3) . ?
O2 C3 1.232(4) . ?
O2 Ca1 2.427(2) . ?
O1 C1 1.274(4) . ?
C3 C2 1.415(5) . ?
C3 C3 1.553(6) 5 ?
C3 Ca1 3.235(4) . ?
C2 C1 1.375(5) . ?
C1 C1 1.525(6) 5 ?
Ca1 O2 2.427(2) 8_665 ?
Ca1 O2 2.427(2) 6_565 ?
Ca1 O2 2.427(2) 3_665 ?
Ca1 O2 2.427(2) 7_655 ?
Ca1 O2 2.427(2) 2_565 ?
Ca1 O2 2.427(2) 5 ?
Ca1 O2 2.427(2) 4_655 ?
Ca1 C3 3.235(4) 8_665 ?
Ca1 C3 3.235(4) 3_665 ?
Ca1 C3 3.235(4) 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
C6 N1 C6 68.8(3) . 7_655 ?
C6 N1 C6 68.8(3) . 6_565 ?
C6 N1 C6 106.0(6) 7_655 6_565 ?
C6 N1 C6 106.0(6) . 3_665 ?
C6 N1 C6 68.8(3) 7_655 3_665 ?
C6 N1 C6 68.8(3) 6_565 3_665 ?
C6 N1 C4 179.9(6) . 3_665 ?
C6 N1 C4 111.1(4) 7_655 3_665 ?
C6 N1 C4 111.3(5) 6_565 3_665 ?
C6 N1 C4 73.9(4) 3_665 3_665 ?
C6 N1 C4 111.3(5) . 6_565 ?
C6 N1 C4 179.9(6) 7_655 6_565 ?
C6 N1 C4 73.9(4) 6_565 6_565 ?
C6 N1 C4 111.1(4) 3_665 6_565 ?
C4 N1 C4 68.9(4) 3_665 6_565 ?
C6 N1 C4 73.9(4) . . ?
C6 N1 C4 111.3(5) 7_655 . ?
C6 N1 C4 111.1(4) 6_565 . ?
C6 N1 C4 179.9(6) 3_665 . ?
C4 N1 C4 106.2(7) 3_665 . ?
C4 N1 C4 68.9(4) 6_565 . ?
C6 N1 C4 111.1(4) . 7_655 ?
C6 N1 C4 73.9(4) 7_655 7_655 ?
C6 N1 C4 179.9(6) 6_565 7_655 ?
C6 N1 C4 111.3(5) 3_665 7_655 ?
C4 N1 C4 68.9(4) 3_665 7_655 ?
C4 N1 C4 106.2(7) 6_565 7_655 ?
C4 N1 C4 68.9(4) . 7_655 ?
C5 C4 N1 115.5(9) . . ?
C7 C6 N1 114.0(8) . . ?
S2 S1 S2 19.8(4) . 3_765 ?
S2 S2 S2 72.4(9) 3_765 2_565 ?
S2 S2 S1 131.0(4) 3_765 . ?
S2 S2 S1 150.9(4) 2_565 . ?
S2 S2 S2 67.1(9) 3_765 4_755 ?
S2 S2 S2 40.5(7) 2_565 4_755 ?
S1 S2 S2 153.6(4) . 4_755 ?
S2 S2 S1 29.1(3) 3_765 3_765 ?
S2 S2 S1 99.4(7) 2_565 3_765 ?
S1 S2 S1 101.9(6) . 3_765 ?
S2 S2 S1 94.7(7) 4_755 3_765 ?
O1 Sn1 O1 148.77(14) 5 3_775 ?
O1 Sn1 O1 136.18(14) 5 6_575 ?
O1 Sn1 O1 72.99(6) 3_775 6_575 ?
O1 Sn1 O1 72.99(6) 5 2_575 ?
O1 Sn1 O1 136.18(14) 3_775 2_575 ?
O1 Sn1 O1 74.33(13) 6_575 2_575 ?
O1 Sn1 O1 114.52(12) 5 8_775 ?
O1 Sn1 O1 74.33(13) 3_775 8_775 ?
O1 Sn1 O1 82.15(13) 6_575 8_775 ?
O1 Sn1 O1 72.99(6) 2_575 8_775 ?
O1 Sn1 O1 82.15(13) 5 7_755 ?
O1 Sn1 O1 72.99(6) 3_775 7_755 ?
O1 Sn1 O1 114.52(12) 6_575 7_755 ?
O1 Sn1 O1 148.77(14) 2_575 7_755 ?
O1 Sn1 O1 136.18(14) 8_775 7_755 ?
O1 Sn1 O1 72.99(6) 5 4_755 ?
O1 Sn1 O1 82.15(13) 3_775 4_755 ?
O1 Sn1 O1 148.77(14) 6_575 4_755 ?
O1 Sn1 O1 114.52(12) 2_575 4_755 ?
O1 Sn1 O1 72.99(6) 8_775 4_755 ?
O1 Sn1 O1 74.33(13) 7_755 4_755 ?
O1 Sn1 O1 74.33(13) 5 . ?
O1 Sn1 O1 114.52(12) 3_775 . ?
O1 Sn1 O1 72.99(6) 6_575 . ?
O1 Sn1 O1 82.15(13) 2_575 . ?
O1 Sn1 O1 148.77(14) 8_775 . ?
O1 Sn1 O1 72.99(6) 7_755 . ?
O1 Sn1 O1 136.18(14) 4_755 . ?
C3 O2 Ca1 120.7(2) . . ?
C1 O1 Sn1 117.2(2) . . ?
O2 C3 C2 125.6(3) . . ?
O2 C3 C3 116.30(19) . 5 ?
C2 C3 C3 118.09(19) . 5 ?
O2 C3 Ca1 40.20(16) . . ?
C2 C3 Ca1 165.8(2) . . ?
C3 C3 Ca1 76.11(5) 5 . ?
C1 C2 C3 122.2(3) . . ?
C1 C2 Cl1 119.6(3) . . ?
C3 C2 Cl1 118.1(3) . . ?
O1 C1 C2 124.8(3) . . ?
O1 C1 C1 115.61(18) . 5 ?
C2 C1 C1 119.6(2) . 5 ?
O2 Ca1 O2 153.75(12) . 8_665 ?
O2 Ca1 O2 75.80(5) . 6_565 ?
O2 Ca1 O2 128.77(12) 8_665 6_565 ?
O2 Ca1 O2 120.62(11) . 3_665 ?
O2 Ca1 O2 66.03(11) 8_665 3_665 ?
O2 Ca1 O2 75.80(5) 6_565 3_665 ?
O2 Ca1 O2 75.80(5) . 7_655 ?
O2 Ca1 O2 82.21(12) 8_665 7_655 ?
O2 Ca1 O2 120.62(11) 6_565 7_655 ?
O2 Ca1 O2 75.80(5) 3_665 7_655 ?
O2 Ca1 O2 128.77(12) . 2_565 ?
O2 Ca1 O2 75.80(5) 8_665 2_565 ?
O2 Ca1 O2 66.03(11) 6_565 2_565 ?
O2 Ca1 O2 82.21(12) 3_665 2_565 ?
O2 Ca1 O2 153.75(12) 7_655 2_565 ?
O2 Ca1 O2 66.03(11) . 5 ?
O2 Ca1 O2 120.62(11) 8_665 5 ?
O2 Ca1 O2 82.21(12) 6_565 5 ?
O2 Ca1 O2 153.75(12) 3_665 5 ?
O2 Ca1 O2 128.77(12) 7_655 5 ?
O2 Ca1 O2 75.80(5) 2_565 5 ?
O2 Ca1 O2 82.21(12) . 4_655 ?
O2 Ca1 O2 75.80(5) 8_665 4_655 ?
O2 Ca1 O2 153.75(12) 6_565 4_655 ?
O2 Ca1 O2 128.77(12) 3_665 4_655 ?
O2 Ca1 O2 66.03(11) 7_655 4_655 ?
O2 Ca1 O2 120.62(11) 2_565 4_655 ?
O2 Ca1 O2 75.80(5) 5 4_655 ?
O2 Ca1 C3 19.13(8) . . ?
O2 Ca1 C3 154.22(8) 8_665 . ?
O2 Ca1 C3 75.68(9) 6_565 . ?
O2 Ca1 C3 136.68(8) 3_665 . ?
O2 Ca1 C3 91.72(8) 7_655 . ?
O2 Ca1 C3 114.26(9) 2_565 . ?
O2 Ca1 C3 46.91(8) 5 . ?
O2 Ca1 C3 78.84(9) 4_655 . ?
O2 Ca1 C3 154.22(8) . 8_665 ?
O2 Ca1 C3 19.13(8) 8_665 8_665 ?
O2 Ca1 C3 114.26(9) 6_565 8_665 ?
O2 Ca1 C3 46.91(8) 3_665 8_665 ?
O2 Ca1 C3 78.84(9) 7_655 8_665 ?
O2 Ca1 C3 75.68(9) 2_565 8_665 ?
O2 Ca1 C3 136.68(8) 5 8_665 ?
O2 Ca1 C3 91.72(8) 4_655 8_665 ?
C3 Ca1 C3 168.81(12) . 8_665 ?
O2 Ca1 C3 136.68(8) . 3_665 ?
O2 Ca1 C3 46.91(8) 8_665 3_665 ?
O2 Ca1 C3 91.72(8) 6_565 3_665 ?
O2 Ca1 C3 19.13(8) 3_665 3_665 ?
O2 Ca1 C3 75.68(9) 7_655 3_665 ?
O2 Ca1 C3 78.84(9) 2_565 3_665 ?
O2 Ca1 C3 154.22(8) 5 3_665 ?
O2 Ca1 C3 114.26(9) 4_655 3_665 ?
C3 Ca1 C3 154.66(11) . 3_665 ?
C3 Ca1 C3 27.78(11) 8_665 3_665 ?
O2 Ca1 C3 46.91(8) . 5 ?
O2 Ca1 C3 136.68(8) 8_665 5 ?
O2 Ca1 C3 78.84(9) 6_565 5 ?
O2 Ca1 C3 154.22(8) 3_665 5 ?
O2 Ca1 C3 114.26(9) 7_655 5 ?
O2 Ca1 C3 91.72(8) 2_565 5 ?
O2 Ca1 C3 19.13(8) 5 5 ?
O2 Ca1 C3 75.68(9) 4_655 5 ?
C3 Ca1 C3 27.78(11) . 5 ?
C3 Ca1 C3 154.66(11) 8_665 5 ?
C3 Ca1 C3 168.81(12) 3_665 5 ?

_diffrn_measured_fraction_theta_max 0.961
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.961
_refine_diff_density_max         1.132
_refine_diff_density_min         -0.384
_refine_diff_density_rms         0.098

# Attachment '- sncamecnfinal.cif'

data_shelxl3
_database_code_depnum_ccdc_archive 'CCDC 826952'
#TrackingRef '- sncamecnfinal.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C44 H47 Ca Cl8 N4 O16.50 Sn'
_chemical_formula_weight         1338.23

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I422

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

_cell_length_a                   11.9523(2)
_cell_length_b                   11.9523(2)
_cell_length_c                   20.2090(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2887.01(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    1920
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      29.21

_exptl_crystal_description       'square plate'
_exptl_crystal_colour            'deep purple'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1354
_exptl_absorpt_coefficient_mu    0.968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.96064
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4061
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         28.00
_reflns_number_total             1705
_reflns_number_gt                1563
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0314P)^2^+3.9277P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.55(3)
_refine_ls_number_reflns         1705
_refine_ls_number_parameters     113
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_ref         0.0787
_refine_ls_wR_factor_gt          0.0744
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.5000 0.5000 0.2460(3) 0.0183(10) Uani 1 4 d S . .
C4 C 0.5971(7) 0.5304(6) 0.2012(4) 0.031(2) Uani 0.50 1 d PD A 1
H4A H 0.6155 0.4644 0.1737 0.037 Uiso 0.50 1 calc PR A 1
H4B H 0.5723 0.5907 0.1710 0.037 Uiso 0.50 1 calc PR A 1
C5 C 0.7018(11) 0.5683(19) 0.2356(11) 0.042(5) Uani 0.50 1 d PD A 1
H5A H 0.7587 0.5872 0.2025 0.063 Uiso 0.50 1 calc PR A 1
H5B H 0.7296 0.5081 0.2641 0.063 Uiso 0.50 1 calc PR A 1
H5C H 0.6853 0.6345 0.2625 0.063 Uiso 0.50 1 calc PR A 1
C6 C 0.5969(6) 0.5307(6) 0.2916(3) 0.0225(17) Uani 0.50 1 d PD A 2
H6A H 0.5743 0.5951 0.3193 0.027 Uiso 0.50 1 calc PR A 2
H6B H 0.6119 0.4669 0.3215 0.027 Uiso 0.50 1 calc PR A 2
C7 C 0.7038(12) 0.5601(16) 0.2555(9) 0.030(4) Uani 0.50 1 d PD A 2
H7A H 0.7625 0.5776 0.2878 0.044 Uiso 0.50 1 calc PR A 2
H7B H 0.6909 0.6253 0.2271 0.044 Uiso 0.50 1 calc PR A 2
H7C H 0.7275 0.4966 0.2283 0.044 Uiso 0.50 1 calc PR A 2
C9 C -0.0334(18) 0.4701(19) -0.0156(13) 0.096(11) Uiso 0.25 1 d PD . .
C8 C 0.0497(17) 0.5440(17) -0.0532(9) 0.053(5) Uiso 0.25 1 d PD . .
N2 N 0.1083(18) 0.5938(19) -0.0871(10) 0.086(6) Uiso 0.25 1 d PD . .
O3 O 1.0000 0.5000 0.2500 0.071(7) Uiso 0.25 4 d SP . .
Sn1 Sn 0.0000 0.0000 0.0000 0.01158(15) Uani 1 8 d S . .
Cl1 Cl -0.15782(8) -0.32359(8) -0.14102(4) 0.0285(2) Uani 1 1 d . . .
O2 O -0.34448(18) -0.41520(18) -0.05835(11) 0.0174(5) Uani 1 1 d . . .
O1 O -0.06581(17) -0.13891(16) -0.05763(10) 0.0121(5) Uani 1 1 d . . .
C3 C -0.2939(2) -0.3343(3) -0.03436(15) 0.0144(7) Uani 1 1 d . . .
C2 C -0.2031(3) -0.2782(3) -0.06428(15) 0.0161(6) Uani 1 1 d . . .
C1 C -0.1502(2) -0.1909(2) -0.03337(14) 0.0124(7) Uani 1 1 d . . .
Ca1 Ca -0.5000 -0.5000 0.0000 0.0096(3) Uani 1 8 d S . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0221(14) 0.0221(14) 0.011(2) 0.000 0.000 0.000
C4 0.048(5) 0.021(4) 0.023(4) 0.011(3) 0.014(4) 0.012(3)
C5 0.022(7) 0.035(7) 0.069(13) 0.033(8) 0.016(6) 0.012(5)
C6 0.031(4) 0.019(4) 0.018(3) -0.001(3) -0.011(3) 0.003(3)
C7 0.025(6) 0.018(6) 0.045(10) 0.007(6) -0.016(5) -0.008(4)
Sn1 0.01029(18) 0.01029(18) 0.0142(3) 0.000 0.000 0.000
Cl1 0.0334(5) 0.0318(5) 0.0204(4) -0.0135(4) 0.0129(4) -0.0167(4)
O2 0.0176(12) 0.0166(11) 0.0180(12) -0.0034(10) 0.0032(10) -0.0056(9)
O1 0.0125(10) 0.0112(11) 0.0127(11) 0.0007(9) 0.0013(9) -0.0030(8)
C3 0.0146(15) 0.0130(15) 0.0157(16) -0.0021(12) -0.0003(12) -0.0011(12)
C2 0.0182(17) 0.0172(16) 0.0129(14) -0.0020(13) 0.0042(13) -0.0033(12)
C1 0.0115(15) 0.0123(14) 0.0134(15) 0.0021(12) -0.0009(12) -0.0012(12)
Ca1 0.0086(4) 0.0086(4) 0.0116(8) 0.000 0.000 0.000

_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
N1 C4 1.515(8) 6_565 ?
N1 C4 1.515(8) . ?
N1 C4 1.515(8) 7_655 ?
N1 C4 1.515(8) 3_665 ?
N1 C6 1.525(7) . ?
N1 C6 1.525(7) 3_665 ?
N1 C6 1.525(7) 7_655 ?
N1 C6 1.525(7) 6_565 ?
C4 C5 1.501(14) . ?
C6 C7 1.512(14) . ?
C9 C8 1.532(8) . ?
C8 N2 1.146(8) . ?
Sn1 O1 2.175(2) 8 ?
Sn1 O1 2.175(2) . ?
Sn1 O1 2.175(2) 2 ?
Sn1 O1 2.175(2) 5 ?
Sn1 O1 2.175(2) 4 ?
Sn1 O1 2.175(2) 6 ?
Sn1 O1 2.175(2) 3 ?
Sn1 O1 2.175(2) 7 ?
Cl1 C2 1.730(3) . ?
O2 C3 1.239(4) . ?
O2 Ca1 2.423(2) . ?
O1 C1 1.282(4) . ?
C3 C2 1.412(4) . ?
C3 C3 1.547(6) 5 ?
C3 Ca1 3.236(3) . ?
C2 C1 1.371(4) . ?
C1 C1 1.514(6) 5 ?
Ca1 O2 2.423(2) 5 ?
Ca1 O2 2.423(2) 2_545 ?
Ca1 O2 2.423(2) 8_445 ?
Ca1 O2 2.423(2) 4_455 ?
Ca1 O2 2.423(2) 3_445 ?
Ca1 O2 2.423(2) 6_545 ?
Ca1 O2 2.423(2) 7_455 ?
Ca1 C3 3.236(3) 5 ?
Ca1 C3 3.236(3) 8_445 ?
Ca1 C3 3.236(3) 3_445 ?

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
C4 N1 C4 69.1(3) 6_565 . ?
C4 N1 C4 106.7(7) 6_565 7_655 ?
C4 N1 C4 69.1(3) . 7_655 ?
C4 N1 C4 69.1(3) 6_565 3_665 ?
C4 N1 C4 106.7(7) . 3_665 ?
C4 N1 C4 69.1(3) 7_655 3_665 ?
C4 N1 C6 111.3(4) 6_565 . ?
C4 N1 C6 73.8(4) . . ?
C4 N1 C6 111.0(4) 7_655 . ?
C4 N1 C6 179.4(5) 3_665 . ?
C4 N1 C6 111.0(4) 6_565 3_665 ?
C4 N1 C6 179.4(5) . 3_665 ?
C4 N1 C6 111.3(4) 7_655 3_665 ?
C4 N1 C6 73.8(4) 3_665 3_665 ?
C6 N1 C6 105.6(6) . 3_665 ?
C4 N1 C6 179.4(5) 6_565 7_655 ?
C4 N1 C6 111.3(4) . 7_655 ?
C4 N1 C6 73.8(4) 7_655 7_655 ?
C4 N1 C6 111.0(4) 3_665 7_655 ?
C6 N1 C6 68.6(3) . 7_655 ?
C6 N1 C6 68.6(3) 3_665 7_655 ?
C4 N1 C6 73.8(4) 6_565 6_565 ?
C4 N1 C6 111.0(4) . 6_565 ?
C4 N1 C6 179.4(5) 7_655 6_565 ?
C4 N1 C6 111.3(4) 3_665 6_565 ?
C6 N1 C6 68.6(3) . 6_565 ?
C6 N1 C6 68.6(3) 3_665 6_565 ?
C6 N1 C6 105.6(6) 7_655 6_565 ?
C5 C4 N1 115.8(9) . . ?
C7 C6 N1 114.0(8) . . ?
N2 C8 C9 173(2) . . ?
O1 Sn1 O1 147.00(11) 8 . ?
O1 Sn1 O1 73.34(5) 8 2 ?
O1 Sn1 O1 137.60(11) . 2 ?
O1 Sn1 O1 115.26(11) 8 5 ?
O1 Sn1 O1 74.61(11) . 5 ?
O1 Sn1 O1 73.34(5) 2 5 ?
O1 Sn1 O1 73.34(5) 8 4 ?
O1 Sn1 O1 80.49(11) . 4 ?
O1 Sn1 O1 115.26(11) 2 4 ?
O1 Sn1 O1 73.34(5) 5 4 ?
O1 Sn1 O1 137.60(11) 8 6 ?
O1 Sn1 O1 73.34(5) . 6 ?
O1 Sn1 O1 74.61(11) 2 6 ?
O1 Sn1 O1 80.49(11) 5 6 ?
O1 Sn1 O1 147.00(11) 4 6 ?
O1 Sn1 O1 74.61(11) 8 3 ?
O1 Sn1 O1 115.26(11) . 3 ?
O1 Sn1 O1 80.49(11) 2 3 ?
O1 Sn1 O1 147.00(11) 5 3 ?
O1 Sn1 O1 137.60(11) 4 3 ?
O1 Sn1 O1 73.34(5) 6 3 ?
O1 Sn1 O1 80.49(11) 8 7 ?
O1 Sn1 O1 73.34(5) . 7 ?
O1 Sn1 O1 147.00(11) 2 7 ?
O1 Sn1 O1 137.60(11) 5 7 ?
O1 Sn1 O1 74.61(11) 4 7 ?
O1 Sn1 O1 115.26(11) 6 7 ?
O1 Sn1 O1 73.34(5) 3 7 ?
C3 O2 Ca1 120.7(2) . . ?
C1 O1 Sn1 116.71(18) . . ?
O2 C3 C2 125.3(3) . . ?
O2 C3 C3 116.27(18) . 5 ?
C2 C3 C3 118.42(18) . 5 ?
O2 C3 Ca1 40.11(15) . . ?
C2 C3 Ca1 165.4(2) . . ?
C3 C3 Ca1 76.17(5) 5 . ?
C1 C2 C3 121.4(3) . . ?
C1 C2 Cl1 120.2(2) . . ?
C3 C2 Cl1 118.4(2) . . ?
O1 C1 C2 123.9(3) . . ?
O1 C1 C1 115.96(16) . 5 ?
C2 C1 C1 120.14(17) . 5 ?
O2 Ca1 O2 66.12(10) 5 . ?
O2 Ca1 O2 76.30(5) 5 2_545 ?
O2 Ca1 O2 79.83(11) . 2_545 ?
O2 Ca1 O2 121.76(10) 5 8_445 ?
O2 Ca1 O2 151.45(10) . 8_445 ?
O2 Ca1 O2 76.30(5) 2_545 8_445 ?
O2 Ca1 O2 76.30(5) 5 4_455 ?
O2 Ca1 O2 130.55(10) . 4_455 ?
O2 Ca1 O2 121.76(10) 2_545 4_455 ?
O2 Ca1 O2 76.30(5) 8_445 4_455 ?
O2 Ca1 O2 151.45(10) 5 3_445 ?
O2 Ca1 O2 121.76(10) . 3_445 ?
O2 Ca1 O2 130.55(10) 2_545 3_445 ?
O2 Ca1 O2 66.12(10) 8_445 3_445 ?
O2 Ca1 O2 79.83(11) 4_455 3_445 ?
O2 Ca1 O2 130.55(10) 5 6_545 ?
O2 Ca1 O2 76.30(5) . 6_545 ?
O2 Ca1 O2 66.12(10) 2_545 6_545 ?
O2 Ca1 O2 79.83(11) 8_445 6_545 ?
O2 Ca1 O2 151.45(10) 4_455 6_545 ?
O2 Ca1 O2 76.30(5) 3_445 6_545 ?
O2 Ca1 O2 79.83(10) 5 7_455 ?
O2 Ca1 O2 76.30(5) . 7_455 ?
O2 Ca1 O2 151.45(10) 2_545 7_455 ?
O2 Ca1 O2 130.55(10) 8_445 7_455 ?
O2 Ca1 O2 66.12(10) 4_455 7_455 ?
O2 Ca1 O2 76.30(5) 3_445 7_455 ?
O2 Ca1 O2 121.76(10) 6_545 7_455 ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        28.00
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.086

# Attachment '- tincafinal.cif'

data_shelxl4
_database_code_depnum_ccdc_archive 'CCDC 826953'
#TrackingRef '- tincafinal.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H56 Ca Cl8 N2 O20 Sn'
_chemical_formula_weight         1399.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.2262 0.3064 '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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I422

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

_cell_length_a                   11.9869(2)
_cell_length_b                   11.9869(2)
_cell_length_c                   20.7309(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2978.74(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(1)
_cell_measurement_reflns_used    3234
_cell_measurement_theta_min      3.10
_cell_measurement_theta_max      29.07

_exptl_crystal_description       'square plate'
_exptl_crystal_colour            'deep purple'
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1424
_exptl_absorpt_coefficient_mu    0.945
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.60365
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      100(1)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 10.2273
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            4191
_diffrn_reflns_av_R_equivalents  0.0226
_diffrn_reflns_av_sigmaI/netI    0.0294
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         3.10
_diffrn_reflns_theta_max         27.99
_reflns_number_total             1738
_reflns_number_gt                1688
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ 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/[\s^2^(Fo^2^)+(0.0377P)^2^+5.3954P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.48(3)
_refine_ls_number_reflns         1738
_refine_ls_number_parameters     128
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0783
_refine_ls_wR_factor_gt          0.0773
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_restrained_S_all      1.146
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.5000 0.5000 0.2461(2) 0.0139(8) Uani 1 4 d S . .
C4 C 0.5997(6) 0.5231(6) 0.2020(3) 0.0235(17) Uani 0.50 1 d PD A 1
H4A H 0.6137 0.4559 0.1754 0.028 Uiso 0.50 1 calc PR A 1
H4B H 0.5796 0.5846 0.1722 0.028 Uiso 0.50 1 calc PR A 1
C5 C 0.7066(12) 0.554(2) 0.2363(10) 0.035(4) Uani 0.50 1 d PD A 1
H5A H 0.7638 0.5733 0.2045 0.052 Uiso 0.50 1 calc PR A 1
H5B H 0.7322 0.4906 0.2622 0.052 Uiso 0.50 1 calc PR A 1
H5C H 0.6931 0.6182 0.2646 0.052 Uiso 0.50 1 calc PR A 1
C6 C 0.5997(5) 0.5229(5) 0.2900(3) 0.0163(13) Uani 0.50 1 d PD A 2
H6A H 0.5825 0.5885 0.3173 0.020 Uiso 0.50 1 calc PR A 2
H6B H 0.6103 0.4581 0.3190 0.020 Uiso 0.50 1 calc PR A 2
C7 C 0.7077(11) 0.5445(19) 0.2545(9) 0.026(4) Uani 0.50 1 d PD A 2
H7A H 0.7666 0.5621 0.2856 0.039 Uiso 0.50 1 calc PR A 2
H7B H 0.6977 0.6075 0.2249 0.039 Uiso 0.50 1 calc PR A 2
H7C H 0.7286 0.4779 0.2299 0.039 Uiso 0.50 1 calc PR A 2
Sn1 Sn 0.5000 0.5000 0.5000 0.00786(13) Uani 1 8 d S . .
Cl1 Cl 0.67875(7) 0.80309(6) 0.35554(3) 0.01942(18) Uani 1 1 d . . .
O2 O 0.85163(16) 0.90738(17) 0.44045(10) 0.0140(5) Uani 1 1 d . . .
O1 O 0.56943(16) 0.63539(16) 0.44259(9) 0.0105(4) Uani 1 1 d . . .
C3 C 0.7985(2) 0.8293(2) 0.46467(12) 0.0111(6) Uani 1 1 d . . .
C2 C 0.7118(2) 0.7692(2) 0.43454(12) 0.0119(5) Uani 1 1 d . . .
C1 C 0.6535(2) 0.6874(2) 0.46580(12) 0.0097(6) Uani 1 1 d . . .
Ca1 Ca 1.0000 1.0000 0.5000 0.0074(3) Uani 1 8 d S . .
C9 C 0.0768(6) 0.4207(6) 0.3876(6) 0.064(3) Uani 0.50 1 d PD B 3
H9A H 0.0915 0.3545 0.3611 0.097 Uiso 0.50 1 calc PR B 3
H9B H 0.0410 0.3981 0.4280 0.097 Uiso 0.50 1 calc PR B 3
H9C H 0.1474 0.4585 0.3971 0.097 Uiso 0.50 1 calc PR B 3
O3 O 0.0000 0.5000 0.2924(5) 0.059(2) Uani 0.50 2 d SP C 3
C8 C 0.0000 0.5000 0.3509(6) 0.053(3) Uani 0.50 2 d SPD . 3
O4 O 0.0376(13) 0.4387(17) 0.4430(11) 0.116(9) Uani 0.25 1 d P . 4

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0150(13) 0.0150(13) 0.0117(18) 0.000 0.000 0.000
C4 0.026(3) 0.026(4) 0.019(3) 0.003(3) 0.011(3) -0.001(3)
C5 0.020(6) 0.030(7) 0.055(9) 0.024(7) 0.011(5) 0.005(4)
C6 0.014(3) 0.017(4) 0.018(3) 0.001(2) -0.005(2) 0.005(2)
C7 0.012(5) 0.013(4) 0.053(10) 0.017(7) -0.005(5) -0.006(3)
Sn1 0.00626(16) 0.00626(16) 0.0111(2) 0.000 0.000 0.000
Cl1 0.0237(4) 0.0212(4) 0.0134(3) 0.0063(3) -0.0065(3) -0.0104(3)
O2 0.0133(10) 0.0145(10) 0.0143(9) 0.0038(8) -0.0020(8) -0.0056(8)
O1 0.0098(9) 0.0080(9) 0.0135(9) 0.0013(8) -0.0020(8) -0.0001(7)
C3 0.0087(13) 0.0093(13) 0.0153(13) 0.0018(10) 0.0019(10) -0.0003(12)
C2 0.0137(13) 0.0129(13) 0.0091(10) 0.0020(10) -0.0028(11) -0.0007(10)
C1 0.0082(13) 0.0096(13) 0.0114(12) -0.0006(10) 0.0000(10) 0.0013(11)
Ca1 0.0058(4) 0.0058(4) 0.0104(6) 0.000 0.000 0.000
C9 0.032(5) 0.028(5) 0.134(10) 0.028(6) -0.033(6) -0.007(4)
O3 0.053(6) 0.054(6) 0.071(6) 0.000 0.000 -0.017(6)
C8 0.037(6) 0.035(6) 0.088(9) 0.000 0.000 -0.025(6)
O4 0.049(10) 0.131(17) 0.168(17) -0.095(15) -0.072(12) 0.030(10)

_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
N1 C6 1.528(6) . ?
N1 C6 1.528(6) 7_655 ?
N1 C6 1.528(6) 6_565 ?
N1 C6 1.528(6) 3_665 ?
N1 C4 1.530(7) 3_665 ?
N1 C4 1.530(7) 6_565 ?
N1 C4 1.530(7) . ?
N1 C4 1.530(7) 7_655 ?
C4 C5 1.513(15) . ?
C6 C7 1.512(14) . ?
Sn1 O1 2.1778(19) 5_556 ?
Sn1 O1 2.1778(19) 3_665 ?
Sn1 O1 2.1778(19) 4_656 ?
Sn1 O1 2.1778(19) 8_666 ?
Sn1 O1 2.1778(19) 2_566 ?
Sn1 O1 2.1778(19) . ?
Sn1 O1 2.1778(19) 6_565 ?
Sn1 O1 2.1778(19) 7_655 ?
Cl1 C2 1.733(3) . ?
O2 C3 1.238(3) . ?
O2 Ca1 2.433(2) . ?
O1 C1 1.279(3) . ?
C3 C2 1.411(4) . ?
C3 C3 1.555(5) 5_556 ?
C2 C1 1.368(4) . ?
C1 C1 1.530(5) 5_556 ?
Ca1 O2 2.433(2) 8_776 ?
Ca1 O2 2.433(2) 4_756 ?
Ca1 O2 2.433(2) 5_556 ?
Ca1 O2 2.433(2) 2_576 ?
Ca1 O2 2.433(2) 7_755 ?
Ca1 O2 2.433(2) 3_775 ?
Ca1 O2 2.433(2) 6_575 ?
C9 C8 1.526(7) . ?
O3 C8 1.213(14) . ?
O3 O3 1.760(19) 13_455 ?
C8 C9 1.526(7) 3_565 ?
O4 O4 1.72(4) 3_565 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C6 N1 C6 69.2(3) . 7_655 ?
C6 N1 C6 69.2(3) . 6_565 ?
C6 N1 C6 106.8(5) 7_655 6_565 ?
C6 N1 C6 106.8(5) . 3_665 ?
C6 N1 C6 69.2(3) 7_655 3_665 ?
C6 N1 C6 69.2(3) 6_565 3_665 ?
C6 N1 C4 179.8(5) . 3_665 ?
C6 N1 C4 111.0(4) 7_655 3_665 ?
C6 N1 C4 110.8(4) 6_565 3_665 ?
C6 N1 C4 73.3(3) 3_665 3_665 ?
C6 N1 C4 110.8(4) . 6_565 ?
C6 N1 C4 179.8(5) 7_655 6_565 ?
C6 N1 C4 73.3(3) 6_565 6_565 ?
C6 N1 C4 111.0(4) 3_665 6_565 ?
C4 N1 C4 69.0(3) 3_665 6_565 ?
C6 N1 C4 73.3(3) . . ?
C6 N1 C4 110.8(4) 7_655 . ?
C6 N1 C4 111.0(4) 6_565 . ?
C6 N1 C4 179.8(5) 3_665 . ?
C4 N1 C4 106.5(6) 3_665 . ?
C4 N1 C4 69.0(3) 6_565 . ?
C6 N1 C4 111.0(4) . 7_655 ?
C6 N1 C4 73.3(3) 7_655 7_655 ?
C6 N1 C4 179.8(5) 6_565 7_655 ?
C6 N1 C4 110.8(4) 3_665 7_655 ?
C4 N1 C4 69.0(3) 3_665 7_655 ?
C4 N1 C4 106.5(6) 6_565 7_655 ?
C4 N1 C4 69.0(3) . 7_655 ?
C5 C4 N1 115.1(8) . . ?
C7 C6 N1 114.2(7) . . ?
O1 Sn1 O1 150.25(10) 5_556 3_665 ?
O1 Sn1 O1 72.62(5) 5_556 4_656 ?
O1 Sn1 O1 135.06(10) 3_665 4_656 ?
O1 Sn1 O1 113.74(10) 5_556 8_666 ?
O1 Sn1 O1 74.28(10) 3_665 8_666 ?
O1 Sn1 O1 72.62(5) 4_656 8_666 ?
O1 Sn1 O1 72.62(5) 5_556 2_566 ?
O1 Sn1 O1 83.65(10) 3_665 2_566 ?
O1 Sn1 O1 113.74(10) 4_656 2_566 ?
O1 Sn1 O1 72.62(5) 8_666 2_566 ?
O1 Sn1 O1 74.28(10) 5_556 . ?
O1 Sn1 O1 113.74(10) 3_665 . ?
O1 Sn1 O1 83.65(10) 4_656 . ?
O1 Sn1 O1 150.25(10) 8_666 . ?
O1 Sn1 O1 135.06(10) 2_566 . ?
O1 Sn1 O1 83.65(10) 5_556 6_565 ?
O1 Sn1 O1 72.62(5) 3_665 6_565 ?
O1 Sn1 O1 150.25(10) 4_656 6_565 ?
O1 Sn1 O1 135.06(10) 8_666 6_565 ?
O1 Sn1 O1 74.28(10) 2_566 6_565 ?
O1 Sn1 O1 72.62(5) . 6_565 ?
O1 Sn1 O1 135.06(10) 5_556 7_655 ?
O1 Sn1 O1 72.62(5) 3_665 7_655 ?
O1 Sn1 O1 74.28(10) 4_656 7_655 ?
O1 Sn1 O1 83.65(10) 8_666 7_655 ?
O1 Sn1 O1 150.25(10) 2_566 7_655 ?
O1 Sn1 O1 72.62(5) . 7_655 ?
O1 Sn1 O1 113.74(10) 6_565 7_655 ?
C3 O2 Ca1 120.99(17) . . ?
C1 O1 Sn1 117.30(17) . . ?
O2 C3 C2 125.8(2) . . ?
O2 C3 C3 116.06(15) . 5_556 ?
C2 C3 C3 118.09(15) . 5_556 ?
C1 C2 C3 122.2(2) . . ?
C1 C2 Cl1 119.9(2) . . ?
C3 C2 Cl1 117.9(2) . . ?
O1 C1 C2 125.0(2) . . ?
O1 C1 C1 115.38(15) . 5_556 ?
C2 C1 C1 119.58(15) . 5_556 ?
O2 Ca1 O2 157.60(10) 8_776 . ?
O2 Ca1 O2 75.08(4) 8_776 4_756 ?
O2 Ca1 O2 125.70(10) . 4_756 ?
O2 Ca1 O2 119.02(9) 8_776 5_556 ?
O2 Ca1 O2 65.82(9) . 5_556 ?
O2 Ca1 O2 75.08(4) 4_756 5_556 ?
O2 Ca1 O2 75.08(4) 8_776 2_576 ?
O2 Ca1 O2 86.06(10) . 2_576 ?
O2 Ca1 O2 119.02(9) 4_756 2_576 ?
O2 Ca1 O2 75.08(4) 5_556 2_576 ?
O2 Ca1 O2 125.70(10) 8_776 7_755 ?
O2 Ca1 O2 75.08(4) . 7_755 ?
O2 Ca1 O2 65.82(9) 4_756 7_755 ?
O2 Ca1 O2 86.06(10) 5_556 7_755 ?
O2 Ca1 O2 157.60(10) 2_576 7_755 ?
O2 Ca1 O2 65.82(9) 8_776 3_775 ?
O2 Ca1 O2 119.02(9) . 3_775 ?
O2 Ca1 O2 86.06(10) 4_756 3_775 ?
O2 Ca1 O2 157.60(10) 5_556 3_775 ?
O2 Ca1 O2 125.70(10) 2_576 3_775 ?
O2 Ca1 O2 75.08(4) 7_755 3_775 ?
O2 Ca1 O2 86.06(10) 8_776 6_575 ?
O2 Ca1 O2 75.08(4) . 6_575 ?
O2 Ca1 O2 157.60(10) 4_756 6_575 ?
O2 Ca1 O2 125.70(10) 5_556 6_575 ?
O2 Ca1 O2 65.82(9) 2_576 6_575 ?
O2 Ca1 O2 119.02(9) 7_755 6_575 ?
O2 Ca1 O2 75.08(4) 3_775 6_575 ?
C8 O3 O3 180.000(2) . 13_455 ?
O3 C8 C9 119.8(5) . 3_565 ?
O3 C8 C9 119.8(5) . . ?
C9 C8 C9 120.3(11) 3_565 . ?

_diffrn_measured_fraction_theta_max 0.970
_diffrn_reflns_theta_full        27.99
_diffrn_measured_fraction_theta_full 0.970
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.082