# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2020

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

data_KSS13
_database_code_depnum_ccdc_archive 'CCDC 1968227'
loop_
_audit_author_name
_audit_author_address
'Waldemar Maniukiewicz'
'Institute of General and Ecological Chemistry , Lodz University of Technology'
_audit_update_record             
;
2019-11-26 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H40 N4 O6 Sn'
_chemical_formula_sum            'C42 H40 N4 O6 Sn'
_chemical_formula_weight         815.47

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+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                   34.4256(14)
_cell_length_b                   7.6022(3)
_cell_length_c                   14.6569(6)
_cell_angle_alpha                90
_cell_angle_beta                 99.167(6)
_cell_angle_gamma                90
_cell_volume                     3786.9(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)

_cell_measurement_reflns_used    3065
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      19.64
_exptl_crystal_description       BLOCK
_exptl_crystal_colour            red


_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.430
_exptl_crystal_F_000             1672
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.728
_shelx_estimated_absorpt_T_min   0.899
_shelx_estimated_absorpt_T_max   0.931
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6252
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       'ω and φ scan'


_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16800
_diffrn_reflns_av_unetI/netI     0.0527
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.198
_diffrn_reflns_theta_max         23.982
_diffrn_reflns_theta_full        23.982
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2962
_reflns_number_gt                1941
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2018/3 (Sheldrick, 2018)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0392P)²+5.5976P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2962
_refine_ls_number_parameters     244
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0861
_refine_ls_R_factor_gt           0.0432
_refine_ls_wR_factor_ref         0.1096
_refine_ls_wR_factor_gt          0.0894
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.51941(18) 1.0196(9) 0.3796(4) 0.101(2) Uani 1 1 d . . . . .
H1A H 0.498181 1.015223 0.415799 0.122 Uiso 1 1 calc R U . . .
H1B H 0.540987 0.949672 0.411353 0.122 Uiso 1 1 calc R U . . .
C2 C 0.5330(3) 1.2088(12) 0.3746(5) 0.153(3) Uani 1 1 d . . . . .
H2A H 0.554610 1.210763 0.339449 0.184 Uiso 1 1 calc R U . . .
H2B H 0.511619 1.275830 0.340014 0.184 Uiso 1 1 calc R U . . .
C3 C 0.5454(3) 1.2969(13) 0.4591(5) 0.166(3) Uani 1 1 d . . . . .
H3A H 0.566612 1.229807 0.494595 0.199 Uiso 1 1 calc R U . . .
H3B H 0.523739 1.298697 0.493970 0.199 Uiso 1 1 calc R U . . .
C4 C 0.5586(4) 1.4719(13) 0.4504(6) 0.222(6) Uani 1 1 d . . . . .
H4A H 0.566435 1.521568 0.510780 0.333 Uiso 1 1 calc R U . . .
H4B H 0.580619 1.471819 0.417636 0.333 Uiso 1 1 calc R U . . .
H4C H 0.537665 1.540840 0.417010 0.333 Uiso 1 1 calc R U . . .
C5 C 0.42982(16) 0.7766(9) 0.2832(3) 0.0684(14) Uani 1 1 d . . . . .
C6 C 0.39744(15) 0.6564(7) 0.2959(3) 0.0604(13) Uani 1 1 d . . . . .
C7 C 0.36167(14) 0.7205(7) 0.3118(3) 0.0626(13) Uani 1 1 d . . . . .
H7 H 0.357946 0.841376 0.315209 0.075 Uiso 1 1 calc R U . . .
C8 C 0.33142(14) 0.6085(7) 0.3227(3) 0.0611(13) Uani 1 1 d . . . . .
H8 H 0.307454 0.653195 0.333769 0.073 Uiso 1 1 calc R U . . .
C9 C 0.33683(14) 0.4288(7) 0.3171(3) 0.0588(13) Uani 1 1 d . . . . .
C10 C 0.37303(16) 0.3629(7) 0.3019(3) 0.0735(15) Uani 1 1 d . . . . .
H10 H 0.376970 0.242154 0.299122 0.088 Uiso 1 1 calc R U . . .
C11 C 0.40275(15) 0.4767(8) 0.2911(3) 0.0703(15) Uani 1 1 d . . . . .
H11 H 0.426813 0.432523 0.280367 0.084 Uiso 1 1 calc R U . . .
C12 C 0.24784(15) 0.2421(6) 0.3681(3) 0.0580(12) Uani 1 1 d . . . . .
C13 C 0.25734(18) 0.0555(7) 0.3789(3) 0.0689(15) Uani 1 1 d . . . . .
C14 C 0.2292(2) -0.0524(7) 0.4175(4) 0.0823(17) Uani 1 1 d . . . . .
H14 H 0.234316 -0.171783 0.426780 0.099 Uiso 1 1 calc R U . . .
C15 C 0.1966(2) 0.0147(9) 0.4396(4) 0.0841(18) Uani 1 1 d . . . . .
H15 H 0.179864 -0.059746 0.465490 0.101 Uiso 1 1 calc R U . . .
C16 C 0.18561(17) 0.1943(8) 0.4262(3) 0.0676(14) Uani 1 1 d . . . . .
C17 C 0.15049(18) 0.2578(10) 0.4488(4) 0.0886(18) Uani 1 1 d . . . . .
H17 H 0.133874 0.182072 0.474156 0.106 Uiso 1 1 calc R U . . .
C18 C 0.14012(18) 0.4292(11) 0.4343(5) 0.099(2) Uani 1 1 d . . . . .
H18 H 0.116763 0.471045 0.450544 0.119 Uiso 1 1 calc R U . . .
C19 C 0.16443(19) 0.5404(9) 0.3954(4) 0.0895(18) Uani 1 1 d . . . . .
H19 H 0.156947 0.656881 0.384094 0.107 Uiso 1 1 calc R U . . .
C20 C 0.19951(17) 0.4829(7) 0.3731(3) 0.0704(14) Uani 1 1 d . . . . .
H20 H 0.215752 0.560625 0.347815 0.085 Uiso 1 1 calc R U . . .
C21 C 0.21072(15) 0.3089(7) 0.3881(3) 0.0612(13) Uani 1 1 d . . . . .
N1 N 0.30737(14) 0.3070(6) 0.3279(3) 0.0671(11) Uani 1 1 d D . . . .
N2 N 0.27284(12) 0.3605(5) 0.3455(2) 0.0602(11) Uani 1 1 d . . . . .
O1 O 0.42740(10) 0.9378(5) 0.2864(3) 0.0854(11) Uani 1 1 d . . . . .
O2 O 0.46264(10) 0.7041(5) 0.2684(2) 0.0813(11) Uani 1 1 d . . . . .
O3 O 0.28845(13) -0.0087(5) 0.3595(3) 0.0886(12) Uani 1 1 d . . . . .
Sn1 Sn 0.500000 0.90817(7) 0.250000 0.0704(2) Uani 1 2 d S T P . .
H1 H 0.314(2) 0.192(4) 0.336(5) 0.16(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.518(9) . ?
C1 Sn1 2.090(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.412(8) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.418(10) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C5 O1 1.230(6) . ?
C5 O2 1.306(6) . ?
C5 C6 1.476(7) . ?
C6 C7 1.378(6) . ?
C6 C11 1.382(7) . ?
C7 C8 1.374(6) . ?
C7 H7 0.9300 . ?
C8 C9 1.383(6) . ?
C8 H8 0.9300 . ?
C9 C10 1.394(7) . ?
C9 N1 1.401(6) . ?
C10 C11 1.368(7) . ?
C10 H10 0.9300 . ?
C11 H11 0.9300 . ?
C12 N2 1.323(5) . ?
C12 C21 1.448(6) . ?
C12 C13 1.459(7) . ?
C13 O3 1.250(6) . ?
C13 C14 1.450(7) . ?
C14 C15 1.321(7) . ?
C14 H14 0.9300 . ?
C15 C16 1.422(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.390(7) . ?
C16 C21 1.405(7) . ?
C17 C18 1.359(8) . ?
C17 H17 0.9300 . ?
C18 C19 1.375(8) . ?
C18 H18 0.9300 . ?
C19 C20 1.372(7) . ?
C19 H19 0.9300 . ?
C20 C21 1.385(7) . ?
C20 H20 0.9300 . ?
N1 N2 1.320(5) . ?
N1 H1 0.91(2) . ?
O2 Sn1 2.060(3) . ?

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
C2 C1 Sn1 113.4(4) . . ?
C2 C1 H1A 108.9 . . ?
Sn1 C1 H1A 108.9 . . ?
C2 C1 H1B 108.9 . . ?
Sn1 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C3 C2 C1 117.4(7) . . ?
C3 C2 H2A 108.0 . . ?
C1 C2 H2A 108.0 . . ?
C3 C2 H2B 108.0 . . ?
C1 C2 H2B 108.0 . . ?
H2A C2 H2B 107.2 . . ?
C2 C3 C4 115.0(8) . . ?
C2 C3 H3A 108.5 . . ?
C4 C3 H3A 108.5 . . ?
C2 C3 H3B 108.5 . . ?
C4 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O1 C5 O2 119.5(5) . . ?
O1 C5 C6 123.7(5) . . ?
O2 C5 C6 116.8(5) . . ?
C7 C6 C11 119.2(5) . . ?
C7 C6 C5 121.0(5) . . ?
C11 C6 C5 119.8(5) . . ?
C8 C7 C6 121.0(5) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C7 C8 C9 119.6(5) . . ?
C7 C8 H8 120.2 . . ?
C9 C8 H8 120.2 . . ?
C8 C9 C10 119.8(5) . . ?
C8 C9 N1 122.6(5) . . ?
C10 C9 N1 117.6(5) . . ?
C11 C10 C9 119.7(5) . . ?
C11 C10 H10 120.1 . . ?
C9 C10 H10 120.1 . . ?
C10 C11 C6 120.8(5) . . ?
C10 C11 H11 119.6 . . ?
C6 C11 H11 119.6 . . ?
N2 C12 C21 116.2(5) . . ?
N2 C12 C13 123.1(5) . . ?
C21 C12 C13 120.6(5) . . ?
O3 C13 C14 121.1(5) . . ?
O3 C13 C12 122.7(5) . . ?
C14 C13 C12 116.2(5) . . ?
C15 C14 C13 121.6(6) . . ?
C15 C14 H14 119.2 . . ?
C13 C14 H14 119.2 . . ?
C14 C15 C16 123.7(6) . . ?
C14 C15 H15 118.2 . . ?
C16 C15 H15 118.2 . . ?
C17 C16 C21 119.5(6) . . ?
C17 C16 C15 121.5(6) . . ?
C21 C16 C15 118.9(6) . . ?
C18 C17 C16 120.9(6) . . ?
C18 C17 H17 119.6 . . ?
C16 C17 H17 119.6 . . ?
C17 C18 C19 119.5(6) . . ?
C17 C18 H18 120.3 . . ?
C19 C18 H18 120.3 . . ?
C20 C19 C18 121.3(6) . . ?
C20 C19 H19 119.3 . . ?
C18 C19 H19 119.3 . . ?
C19 C20 C21 120.0(5) . . ?
C19 C20 H20 120.0 . . ?
C21 C20 H20 120.0 . . ?
C20 C21 C16 118.8(5) . . ?
C20 C21 C12 122.3(5) . . ?
C16 C21 C12 118.8(5) . . ?
N2 N1 C9 120.6(5) . . ?
N2 N1 H1 119(5) . . ?
C9 N1 H1 119(5) . . ?
N1 N2 C12 118.7(4) . . ?
C5 O2 Sn1 106.2(3) . . ?
O2 Sn1 O2 82.3(2) . 2_655 ?
O2 Sn1 C1 107.6(2) . . ?
O2 Sn1 C1 108.0(2) 2_655 . ?
O2 Sn1 C1 108.0(2) . 2_655 ?
O2 Sn1 C1 107.6(2) 2_655 2_655 ?
C1 Sn1 C1 132.2(4) . 2_655 ?

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
Sn1 C1 C2 C3 177.9(7) . . . . ?
C1 C2 C3 C4 178.7(9) . . . . ?
O1 C5 C6 C7 0.5(8) . . . . ?
O2 C5 C6 C7 -179.9(4) . . . . ?
O1 C5 C6 C11 179.9(5) . . . . ?
O2 C5 C6 C11 -0.5(7) . . . . ?
C11 C6 C7 C8 -0.1(7) . . . . ?
C5 C6 C7 C8 179.3(4) . . . . ?
C6 C7 C8 C9 -0.4(7) . . . . ?
C7 C8 C9 C10 0.9(7) . . . . ?
C7 C8 C9 N1 179.8(4) . . . . ?
C8 C9 C10 C11 -1.1(7) . . . . ?
N1 C9 C10 C11 -179.9(4) . . . . ?
C9 C10 C11 C6 0.6(8) . . . . ?
C7 C6 C11 C10 0.0(7) . . . . ?
C5 C6 C11 C10 -179.4(4) . . . . ?
N2 C12 C13 O3 -6.7(8) . . . . ?
C21 C12 C13 O3 177.6(4) . . . . ?
N2 C12 C13 C14 170.9(4) . . . . ?
C21 C12 C13 C14 -4.8(7) . . . . ?
O3 C13 C14 C15 178.9(5) . . . . ?
C12 C13 C14 C15 1.3(8) . . . . ?
C13 C14 C15 C16 1.5(9) . . . . ?
C14 C15 C16 C17 178.5(5) . . . . ?
C14 C15 C16 C21 -0.7(8) . . . . ?
C21 C16 C17 C18 0.2(8) . . . . ?
C15 C16 C17 C18 -179.0(5) . . . . ?
C16 C17 C18 C19 1.0(9) . . . . ?
C17 C18 C19 C20 -1.7(9) . . . . ?
C18 C19 C20 C21 1.1(8) . . . . ?
C19 C20 C21 C16 0.1(7) . . . . ?
C19 C20 C21 C12 -178.4(5) . . . . ?
C17 C16 C21 C20 -0.7(7) . . . . ?
C15 C16 C21 C20 178.5(5) . . . . ?
C17 C16 C21 C12 177.8(4) . . . . ?
C15 C16 C21 C12 -3.0(7) . . . . ?
N2 C12 C21 C20 8.3(7) . . . . ?
C13 C12 C21 C20 -175.8(4) . . . . ?
N2 C12 C21 C16 -170.2(4) . . . . ?
C13 C12 C21 C16 5.7(7) . . . . ?
C8 C9 N1 N2 -1.0(7) . . . . ?
C10 C9 N1 N2 177.8(4) . . . . ?
C9 N1 N2 C12 -170.6(4) . . . . ?
C21 C12 N2 N1 179.0(4) . . . . ?
C13 C12 N2 N1 3.1(7) . . . . ?
O1 C5 O2 Sn1 -2.2(6) . . . . ?
C6 C5 O2 Sn1 178.3(3) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1 H1 O3 0.91(2) 1.82(5) 2.549(6) 135(6) . yes

_refine_diff_density_max         0.487
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.062

# start Validation Reply Form
_vrf_THETM01_KSS13               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
RESPONSE: The crystal quality is poor and it is not diffracting at
higher Brag angle.
;
# end Validation Reply Form


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

data_KSS10
_database_code_depnum_ccdc_archive 'CCDC 1968228'
loop_
_audit_author_name
_audit_author_address
'Waldemar Maniukiewicz'
'Institute of General and Ecological Chemistry , Lodz University of Technology'
_audit_update_record             
;
2019-11-26 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '2-(2-hydroxynaphthylazo)benzoic acid'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H12 N2 O3'
_chemical_formula_sum            'C17 H12 N2 O3'
_chemical_formula_weight         292.29

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   16.5566(5)
_cell_length_b                   4.47010(10)
_cell_length_c                   19.8415(6)
_cell_angle_alpha                90
_cell_angle_beta                 111.270(7)
_cell_angle_gamma                90
_cell_volume                     1368.43(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3892
_cell_measurement_theta_min      3.08
_cell_measurement_theta_max      24.42

_exptl_crystal_description       needle
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.099
_shelx_estimated_absorpt_T_min   0.990
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6249
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2016)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker axs kappa apex3 CMOS Diffractometer'
_diffrn_measurement_method       'ω and φ scan'


_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15519
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.707
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             2413
_reflns_number_gt                1501
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX3(Bruker, 2016)'
_computing_cell_refinement       'APEX3/SAINT (Bruker, 2016)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2016)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'


_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0504P)²+0.6838P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_coef       0.011(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2413
_refine_ls_number_parameters     205
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0988
_refine_ls_R_factor_gt           0.0484
_refine_ls_wR_factor_ref         0.1308
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.40812(17) 0.1141(5) 0.74331(14) 0.0430(7) Uani 1 1 d . . . . .
H1 H 0.3530 0.1965 0.7223 0.052 Uiso 1 1 calc R U . . .
C2 C 0.42507(19) -0.0860(6) 0.80002(14) 0.0508(7) Uani 1 1 d . . . . .
H2 H 0.3813 -0.1371 0.8169 0.061 Uiso 1 1 calc R U . . .
C3 C 0.50663(19) -0.2105(6) 0.83172(15) 0.0541(8) Uani 1 1 d . . . . .
H3 H 0.5175 -0.3443 0.8699 0.065 Uiso 1 1 calc R U . . .
C4 C 0.57166(18) -0.1368(6) 0.80696(14) 0.0501(7) Uani 1 1 d . . . . .
H4 H 0.6263 -0.2219 0.8284 0.060 Uiso 1 1 calc R U . . .
C5 C 0.55618(16) 0.0659(5) 0.74950(13) 0.0408(6) Uani 1 1 d . . . . .
C6 C 0.47340(16) 0.1935(5) 0.71734(12) 0.0361(6) Uani 1 1 d . . . . .
C7 C 0.45881(15) 0.4090(5) 0.65852(12) 0.0344(6) Uani 1 1 d . . . . .
C8 C 0.52863(15) 0.4843(6) 0.63322(13) 0.0389(6) Uani 1 1 d . . . . .
C9 C 0.61127(16) 0.3421(6) 0.66842(14) 0.0489(7) Uani 1 1 d . . . . .
H9 H 0.6569 0.3855 0.6532 0.059 Uiso 1 1 calc R U . . .
C10 C 0.62357(17) 0.1469(6) 0.72306(14) 0.0498(7) Uani 1 1 d . . . . .
H10 H 0.6780 0.0607 0.7447 0.060 Uiso 1 1 calc R U . . .
C11 C 0.27747(15) 0.8633(5) 0.55883(13) 0.0348(6) Uani 1 1 d . . . . .
C12 C 0.22315(16) 0.7988(6) 0.59637(14) 0.0448(7) Uani 1 1 d . . . . .
H12 H 0.2419 0.6693 0.6357 0.054 Uiso 1 1 calc R U . . .
C13 C 0.14168(17) 0.9249(6) 0.57585(15) 0.0513(7) Uani 1 1 d . . . . .
H13 H 0.1057 0.8783 0.6011 0.062 Uiso 1 1 calc R U . . .
C14 C 0.11337(16) 1.1196(6) 0.51818(15) 0.0505(7) Uani 1 1 d . . . . .
H14 H 0.0588 1.2069 0.5048 0.061 Uiso 1 1 calc R U . . .
C15 C 0.16651(16) 1.1836(6) 0.48065(15) 0.0494(7) Uani 1 1 d . . . . .
H15 H 0.1467 1.3126 0.4413 0.059 Uiso 1 1 calc R U . . .
C16 C 0.24908(15) 1.0614(6) 0.49967(13) 0.0397(6) Uani 1 1 d . . . . .
C17 C 0.30011(17) 1.1578(7) 0.45534(15) 0.0534(8) Uani 1 1 d . . . . .
N1 N 0.38003(12) 0.5296(4) 0.63304(10) 0.0355(5) Uani 1 1 d . . . . .
N2 N 0.36025(13) 0.7301(5) 0.58055(11) 0.0368(5) Uani 1 1 d . . . . .
O1 O 0.51667(10) 0.6712(4) 0.58254(9) 0.0479(5) Uani 1 1 d . . . . .
O2 O 0.38331(11) 1.1037(5) 0.48321(9) 0.0530(6) Uani 1 1 d . . . . .
H2A H 0.4067 1.1691 0.4562 0.080 Uiso 1 1 calc R U . . .
O3 O 0.26742(15) 1.2810(8) 0.39819(15) 0.1303(14) Uani 1 1 d . . . . .
H2B H 0.4028(18) 0.792(6) 0.5596(15) 0.066(9) Uiso 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.384(3) . ?
C1 C6 1.401(3) . ?
C1 H1 0.9300 . ?
C2 C3 1.383(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.376(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.405(4) . ?
C4 H4 0.9300 . ?
C5 C6 1.406(3) . ?
C5 C10 1.441(4) . ?
C6 C7 1.464(3) . ?
C7 N1 1.330(3) . ?
C7 C8 1.457(3) . ?
C8 O1 1.266(3) . ?
C8 C9 1.439(3) . ?
C9 C10 1.348(4) . ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C11 C12 1.390(3) . ?
C11 C16 1.408(3) . ?
C11 N2 1.411(3) . ?
C12 C13 1.380(4) . ?
C12 H12 0.9300 . ?
C13 C14 1.377(4) . ?
C13 H13 0.9300 . ?
C14 C15 1.373(4) . ?
C14 H14 0.9300 . ?
C15 C16 1.391(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.487(4) . ?
C17 O3 1.199(3) . ?
C17 O2 1.307(3) . ?
N1 N2 1.322(3) . ?
N2 H2B 0.98(3) . ?
O2 H2A 0.8200 . ?

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
C2 C1 C6 120.4(3) . . ?
C2 C1 H1 119.8 . . ?
C6 C1 H1 119.8 . . ?
C3 C2 C1 120.4(3) . . ?
C3 C2 H2 119.8 . . ?
C1 C2 H2 119.8 . . ?
C4 C3 C2 120.2(3) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 120.5(3) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C4 C5 C6 119.4(2) . . ?
C4 C5 C10 121.3(3) . . ?
C6 C5 C10 119.3(2) . . ?
C1 C6 C5 119.0(2) . . ?
C1 C6 C7 122.2(2) . . ?
C5 C6 C7 118.7(2) . . ?
N1 C7 C8 124.5(2) . . ?
N1 C7 C6 115.2(2) . . ?
C8 C7 C6 120.3(2) . . ?
O1 C8 C9 121.6(2) . . ?
O1 C8 C7 120.7(2) . . ?
C9 C8 C7 117.7(2) . . ?
C10 C9 C8 121.1(2) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C5 123.0(3) . . ?
C9 C10 H10 118.5 . . ?
C5 C10 H10 118.5 . . ?
C12 C11 C16 119.5(2) . . ?
C12 C11 N2 119.6(2) . . ?
C16 C11 N2 120.9(2) . . ?
C13 C12 C11 120.7(3) . . ?
C13 C12 H12 119.7 . . ?
C11 C12 H12 119.7 . . ?
C14 C13 C12 120.3(3) . . ?
C14 C13 H13 119.8 . . ?
C12 C13 H13 119.8 . . ?
C15 C14 C13 119.4(2) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C14 C15 C16 122.1(3) . . ?
C14 C15 H15 119.0 . . ?
C16 C15 H15 119.0 . . ?
C15 C16 C11 118.1(2) . . ?
C15 C16 C17 116.0(2) . . ?
C11 C16 C17 125.9(2) . . ?
O3 C17 O2 122.0(3) . . ?
O3 C17 C16 122.3(3) . . ?
O2 C17 C16 115.7(2) . . ?
N2 N1 C7 120.2(2) . . ?
N1 N2 C11 117.5(2) . . ?
N1 N2 H2B 120.9(16) . . ?
C11 N2 H2B 121.4(16) . . ?
C17 O2 H2A 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
C6 C1 C2 C3 -0.1(4) . . . . ?
C1 C2 C3 C4 -0.2(4) . . . . ?
C2 C3 C4 C5 0.2(4) . . . . ?
C3 C4 C5 C6 0.0(4) . . . . ?
C3 C4 C5 C10 179.7(2) . . . . ?
C2 C1 C6 C5 0.3(4) . . . . ?
C2 C1 C6 C7 -178.7(2) . . . . ?
C4 C5 C6 C1 -0.2(3) . . . . ?
C10 C5 C6 C1 -179.9(2) . . . . ?
C4 C5 C6 C7 178.8(2) . . . . ?
C10 C5 C6 C7 -0.9(3) . . . . ?
C1 C6 C7 N1 1.8(3) . . . . ?
C5 C6 C7 N1 -177.2(2) . . . . ?
C1 C6 C7 C8 -179.9(2) . . . . ?
C5 C6 C7 C8 1.1(3) . . . . ?
N1 C7 C8 O1 -1.6(4) . . . . ?
C6 C7 C8 O1 -179.8(2) . . . . ?
N1 C7 C8 C9 177.6(2) . . . . ?
C6 C7 C8 C9 -0.5(3) . . . . ?
O1 C8 C9 C10 179.0(3) . . . . ?
C7 C8 C9 C10 -0.2(4) . . . . ?
C8 C9 C10 C5 0.4(4) . . . . ?
C4 C5 C10 C9 -179.5(3) . . . . ?
C6 C5 C10 C9 0.2(4) . . . . ?
C16 C11 C12 C13 0.5(4) . . . . ?
N2 C11 C12 C13 -179.6(2) . . . . ?
C11 C12 C13 C14 -0.7(4) . . . . ?
C12 C13 C14 C15 0.9(4) . . . . ?
C13 C14 C15 C16 -1.0(4) . . . . ?
C14 C15 C16 C11 0.8(4) . . . . ?
C14 C15 C16 C17 -178.3(3) . . . . ?
C12 C11 C16 C15 -0.6(4) . . . . ?
N2 C11 C16 C15 179.5(2) . . . . ?
C12 C11 C16 C17 178.5(3) . . . . ?
N2 C11 C16 C17 -1.4(4) . . . . ?
C15 C16 C17 O3 -15.1(5) . . . . ?
C11 C16 C17 O3 165.8(3) . . . . ?
C15 C16 C17 O2 163.9(3) . . . . ?
C11 C16 C17 O2 -15.2(4) . . . . ?
C8 C7 N1 N2 0.9(3) . . . . ?
C6 C7 N1 N2 179.1(2) . . . . ?
C7 N1 N2 C11 -176.2(2) . . . . ?
C12 C11 N2 N1 5.0(3) . . . . ?
C16 C11 N2 N1 -175.1(2) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C9 H9 O3 0.93 2.40 3.247(4) 151.4 3_676
O2 H2A O1 0.82 1.85 2.650(2) 165.3 3_676
N2 H2B O1 0.98(3) 1.85(3) 2.589(3) 130(2) .
N2 H2B O2 0.98(3) 2.00(3) 2.683(3) 125(2) .

_refine_diff_density_max         0.296
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.040


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

data_SS7NEW1
_database_code_depnum_ccdc_archive 'CCDC 1968229'
loop_
_audit_author_name
_audit_author_address
'Waldemar Maniukiewicz'
'Institute of General and Ecological Chemistry , Lodz University of Technology'
_audit_update_record             
;
2019-11-26 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C50 H58 N4 O8 Sn2'

_chemical_formula_sum            'C50 H58 N4 O8 Sn2'
_chemical_formula_weight         1080.38

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   8.5110(3)
_cell_length_b                   14.2959(5)
_cell_length_c                   21.9517(8)
_cell_angle_alpha                76.859(2)
_cell_angle_beta                 83.682(2)
_cell_angle_gamma                73.089(2)
_cell_volume                     2485.74(16)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9121
_cell_measurement_theta_min      2.18
_cell_measurement_theta_max      20.42

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    1.060
_shelx_estimated_absorpt_T_min   0.857
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6679
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a

_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker axs kappa apex2 CCD Diffractometer'
_diffrn_measurement_method       'ω and φ scan'



_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            48989
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_av_R_equivalents  0.0659
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.182
_diffrn_reflns_theta_max         24.764
_diffrn_reflns_theta_full        24.764
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             8478
_reflns_number_gt                4052
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SHELXT-2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    
'ORTEP3 (Farrugia, 1997) and Mercury (Bruno et al., 2002)'
_computing_publication_material  'SHELXL-2014/7 (Sheldrick, 2014)'



_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0285P)²+7.7375P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8478
_refine_ls_number_parameters     659
_refine_ls_number_restraints     255
_refine_ls_R_factor_all          0.1436
_refine_ls_R_factor_gt           0.0561
_refine_ls_wR_factor_ref         0.1510
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.071
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.7203(9) -0.5869(5) 0.5824(4) 0.081(2) Uani 1 1 d . . . . .
H1 H 0.7660 -0.5716 0.5422 0.097 Uiso 1 1 calc R U . . .
C2 C 0.7865(11) -0.6775(6) 0.6205(5) 0.099(3) Uani 1 1 d . . . . .
H2 H 0.8779 -0.7227 0.6064 0.119 Uiso 1 1 calc R U . . .
C3 C 0.7176(13) -0.7014(7) 0.6795(5) 0.105(3) Uani 1 1 d . . . . .
H3 H 0.7618 -0.7634 0.7049 0.126 Uiso 1 1 calc R U . . .
C4 C 0.5860(12) -0.6357(7) 0.7010(5) 0.100(3) Uani 1 1 d . . . . .
H4 H 0.5412 -0.6528 0.7412 0.119 Uiso 1 1 calc R U . . .
C5 C 0.5167(10) -0.5423(6) 0.6633(4) 0.076(2) Uani 1 1 d . . . . .
C6 C 0.3785(11) -0.4721(6) 0.6851(4) 0.090(3) Uani 1 1 d . . . . .
H6 H 0.3349 -0.4887 0.7255 0.108 Uiso 1 1 calc R U . . .
C7 C 0.3089(10) -0.3831(6) 0.6494(4) 0.082(2) Uani 1 1 d . . . . .
H7 H 0.2173 -0.3406 0.6656 0.098 Uiso 1 1 calc R U . . .
C8 C 0.3707(9) -0.3513(6) 0.5874(4) 0.068(2) Uani 1 1 d . . . . .
C9 C 0.5133(8) -0.4207(5) 0.5643(4) 0.0613(19) Uani 1 1 d . . . . .
C10 C 0.5863(9) -0.5178(5) 0.6031(4) 0.067(2) Uani 1 1 d . . . . .
C11 C 0.6241(9) -0.2955(5) 0.4126(4) 0.0622(19) Uani 1 1 d . . . . .
C12 C 0.7628(9) -0.3683(6) 0.3983(4) 0.080(2) Uani 1 1 d . . . . .
H12 H 0.7976 -0.4283 0.4268 0.096 Uiso 1 1 calc R U . . .
C13 C 0.8483(10) -0.3515(7) 0.3423(5) 0.092(3) Uani 1 1 d . . . . .
H13 H 0.9412 -0.4005 0.3329 0.110 Uiso 1 1 calc R U . . .
C14 C 0.7985(10) -0.2625(7) 0.2993(4) 0.092(3) Uani 1 1 d . . . . .
H14 H 0.8568 -0.2513 0.2612 0.110 Uiso 1 1 calc R U . . .
C15 C 0.6629(10) -0.1919(6) 0.3139(4) 0.084(2) Uani 1 1 d . . . . .
H15 H 0.6296 -0.1320 0.2852 0.101 Uiso 1 1 calc R U . . .
C16 C 0.5719(9) -0.2058(5) 0.3700(4) 0.067(2) Uani 1 1 d . . . . .
C17 C 0.4250(10) -0.1226(6) 0.3808(5) 0.081(2) Uani 1 1 d . . . . .
C18 C 0.298(2) 0.0846(9) 0.4477(11) 0.124(5) Uani 0.704(12) 1 d D U P A 1
H18A H 0.3641 0.0457 0.4829 0.149 Uiso 0.704(12) 1 calc R U P A 1
H18B H 0.3726 0.0877 0.4111 0.149 Uiso 0.704(12) 1 calc R U P A 1
C19 C 0.2330(19) 0.1875(8) 0.4587(7) 0.134(5) Uani 0.704(12) 1 d D U P A 1
H19A H 0.1570 0.1869 0.4950 0.161 Uiso 0.704(12) 1 calc R U P A 1
H19B H 0.3234 0.2095 0.4683 0.161 Uiso 0.704(12) 1 calc R U P A 1
C20 C 0.148(2) 0.2604(9) 0.4051(8) 0.135(5) Uani 0.704(12) 1 d D U P A 1
H20A H 0.0636 0.2368 0.3919 0.162 Uiso 0.704(12) 1 calc R U P A 1
H20B H 0.2253 0.2702 0.3700 0.162 Uiso 0.704(12) 1 calc R U P A 1
C21 C 0.068(2) 0.3610(10) 0.4285(9) 0.140(5) Uani 0.704(12) 1 d D U P A 1
H21A H 0.0110 0.4109 0.3951 0.210 Uiso 0.704(12) 1 calc R U P A 1
H21B H -0.0081 0.3501 0.4633 0.210 Uiso 0.704(12) 1 calc R U P A 1
H21C H 0.1527 0.3833 0.4415 0.210 Uiso 0.704(12) 1 calc R U P A 1
C18' C 0.228(6) 0.0966(18) 0.434(3) 0.129(8) Uani 0.296(12) 1 d D U P A 2
H18C H 0.2524 0.0926 0.4771 0.155 Uiso 0.296(12) 1 calc R U P A 2
H18D H 0.3312 0.0844 0.4100 0.155 Uiso 0.296(12) 1 calc R U P A 2
C19' C 0.127(4) 0.2009(17) 0.4092(19) 0.126(6) Uani 0.296(12) 1 d D U P A 2
H19C H 0.1287 0.2122 0.3639 0.152 Uiso 0.296(12) 1 calc R U P A 2
H19D H 0.0144 0.2088 0.4251 0.152 Uiso 0.296(12) 1 calc R U P A 2
C20' C 0.193(5) 0.2765(18) 0.428(2) 0.134(7) Uani 0.296(12) 1 d D U P A 2
H20C H 0.3112 0.2603 0.4203 0.161 Uiso 0.296(12) 1 calc R U P A 2
H20D H 0.1673 0.2770 0.4717 0.161 Uiso 0.296(12) 1 calc R U P A 2
C21' C 0.112(5) 0.3786(18) 0.388(2) 0.142(8) Uani 0.296(12) 1 d D U P A 2
H21D H 0.1513 0.4287 0.3986 0.213 Uiso 0.296(12) 1 calc R U P A 2
H21E H 0.1378 0.3773 0.3442 0.213 Uiso 0.296(12) 1 calc R U P A 2
H21F H -0.0055 0.3939 0.3954 0.213 Uiso 0.296(12) 1 calc R U P A 2
C22 C -0.0051(12) -0.0295(9) 0.3687(6) 0.167(5) Uani 1 1 d D U . . .
H22A H 0.0582 -0.0213 0.3292 0.201 Uiso 1 1 calc R U . . .
H22B H 0.0026 -0.1002 0.3809 0.201 Uiso 1 1 calc R U . . .
C23 C -0.1855(15) 0.0208(10) 0.3513(7) 0.192(5) Uani 1 1 d D U . . .
H23A H -0.2177 -0.0175 0.3260 0.230 Uiso 1 1 calc R U . . .
H23B H -0.2554 0.0198 0.3893 0.230 Uiso 1 1 calc R U . . .
C24 C -0.2101(15) 0.1157(9) 0.3196(7) 0.184(5) Uani 1 1 d D U . . .
H24A H -0.1397 0.1157 0.2817 0.221 Uiso 1 1 calc R U . . .
H24B H -0.1748 0.1527 0.3449 0.221 Uiso 1 1 calc R U . . .
C25 C -0.3842(13) 0.1712(9) 0.3014(6) 0.166(5) Uani 1 1 d D U . . .
H25A H -0.3877 0.2378 0.2791 0.248 Uiso 1 1 calc R U . . .
H25B H -0.4201 0.1369 0.2750 0.248 Uiso 1 1 calc R U . . .
H25C H -0.4554 0.1741 0.3384 0.248 Uiso 1 1 calc R U . . .
C26 C 0.1088(14) 0.0407(8) -0.1243(6) 0.100(3) Uani 1 1 d . . . . .
C27 C 0.1965(16) -0.0335(9) -0.1560(6) 0.129(4) Uani 1 1 d . . . . .
H27 H 0.1676 -0.0321 -0.1959 0.155 Uiso 1 1 calc R U . . .
C28 C 0.3247(18) -0.1084(9) -0.1290(7) 0.141(5) Uani 1 1 d . . . . .
H28 H 0.3819 -0.1580 -0.1506 0.169 Uiso 1 1 calc R U . . .
C29 C 0.3698(15) -0.1114(8) -0.0710(7) 0.138(5) Uani 1 1 d . . . . .
H29 H 0.4570 -0.1630 -0.0530 0.166 Uiso 1 1 calc R U . . .
C30 C 0.2855(12) -0.0373(7) -0.0383(5) 0.114(3) Uani 1 1 d . . . . .
H30 H 0.3170 -0.0393 0.0013 0.137 Uiso 1 1 calc R U . . .
C31 C 0.1538(11) 0.0400(6) -0.0650(5) 0.090(3) Uani 1 1 d . . . . .
C32 C 0.0636(10) 0.1184(6) -0.0325(4) 0.080(2) Uani 1 1 d . . . . .
C33 C -0.0721(11) 0.1977(7) -0.0620(4) 0.084(2) Uani 1 1 d . . . . .
C34 C -0.1092(12) 0.1925(7) -0.1232(5) 0.097(3) Uani 1 1 d . . . . .
H34 H -0.1946 0.2425 -0.1438 0.117 Uiso 1 1 calc R U . . .
C35 C -0.0263(14) 0.1194(9) -0.1513(5) 0.113(3) Uani 1 1 d . . . . .
H35 H -0.0574 0.1191 -0.1906 0.136 Uiso 1 1 calc R U . . .
C36 C 0.0947(9) 0.1695(6) 0.1166(4) 0.076(2) Uani 1 1 d . . . . .
C37 C 0.2261(10) 0.0889(7) 0.1393(5) 0.101(3) Uani 1 1 d . . . . .
H37 H 0.2772 0.0424 0.1147 0.121 Uiso 1 1 calc R U . . .
C38 C 0.2808(12) 0.0777(8) 0.1978(5) 0.116(4) Uani 1 1 d . . . . .
H38 H 0.3679 0.0232 0.2126 0.140 Uiso 1 1 calc R U . . .
C39 C 0.2089(12) 0.1456(8) 0.2343(5) 0.112(3) Uani 1 1 d . . . . .
H39 H 0.2479 0.1382 0.2736 0.135 Uiso 1 1 calc R U . . .
C40 C 0.0784(11) 0.2247(7) 0.2126(4) 0.095(3) Uani 1 1 d . . . . .
H40 H 0.0285 0.2704 0.2379 0.114 Uiso 1 1 calc R U . . .
C41 C 0.0190(10) 0.2385(6) 0.1540(4) 0.080(2) Uani 1 1 d . . . . .
C42 C -0.1248(11) 0.3264(7) 0.1361(5) 0.095(3) Uani 1 1 d . . . . .
C43 C -0.5540(17) 0.4069(10) 0.1332(7) 0.206(6) Uani 1 1 d D U . . .
H43A H -0.6188 0.3785 0.1126 0.247 Uiso 1 1 calc R U . . .
H43B H -0.4929 0.3545 0.1653 0.247 Uiso 1 1 calc R U . . .
C44 C -0.666(2) 0.4919(13) 0.1623(9) 0.274(8) Uani 1 1 d D U . . .
H44A H -0.6017 0.5221 0.1819 0.329 Uiso 1 1 calc R U . . .
H44B H -0.7317 0.5429 0.1309 0.329 Uiso 1 1 calc R U . . .
C45 C -0.765(3) 0.4457(15) 0.2068(10) 0.308(9) Uani 1 1 d D U . . .
H45A H -0.7108 0.4174 0.2462 0.370 Uiso 1 1 calc R U . . .
H45B H -0.7912 0.3932 0.1922 0.370 Uiso 1 1 calc R U . . .
C46 C -0.912(2) 0.5266(13) 0.2138(9) 0.283(9) Uani 1 1 d D U . . .
H46A H -0.9878 0.5013 0.2440 0.424 Uiso 1 1 calc R U . . .
H46B H -0.8822 0.5779 0.2278 0.424 Uiso 1 1 calc R U . . .
H46C H -0.9621 0.5539 0.1742 0.424 Uiso 1 1 calc R U . . .
C47 C -0.228(3) 0.5741(15) 0.0440(12) 0.131(7) Uani 0.516(14) 1 d D U P B 3
H47A H -0.1269 0.5412 0.0656 0.157 Uiso 0.516(14) 1 calc R U P B 3
H47B H -0.1996 0.5823 -0.0005 0.157 Uiso 0.516(14) 1 calc R U P B 3
C48 C -0.291(3) 0.6741(15) 0.0583(10) 0.147(6) Uani 0.516(14) 1 d D U P B 3
H48A H -0.1991 0.7031 0.0523 0.176 Uiso 0.516(14) 1 calc R U P B 3
H48B H -0.3684 0.7138 0.0268 0.176 Uiso 0.516(14) 1 calc R U P B 3
C49 C -0.370(4) 0.688(2) 0.1187(11) 0.154(7) Uani 0.516(14) 1 d D U P B 3
H49A H -0.2921 0.6521 0.1506 0.184 Uiso 0.516(14) 1 calc R U P B 3
H49B H -0.4606 0.6578 0.1260 0.184 Uiso 0.516(14) 1 calc R U P B 3
C50 C -0.437(7) 0.794(3) 0.128(2) 0.160(11) Uani 0.516(14) 1 d D U P B 3
H50A H -0.4865 0.7938 0.1696 0.241 Uiso 0.516(14) 1 calc R U P B 3
H50B H -0.3492 0.8251 0.1227 0.241 Uiso 0.516(14) 1 calc R U P B 3
H50C H -0.5183 0.8308 0.0980 0.241 Uiso 0.516(14) 1 calc R U P B 3
C48' C -0.408(3) 0.6564(18) 0.1020(13) 0.142(7) Uani 0.484(14) 1 d D U P B 4
H48C H -0.5142 0.6826 0.0831 0.171 Uiso 0.484(14) 1 calc R U P B 4
H48D H -0.4271 0.6260 0.1454 0.171 Uiso 0.484(14) 1 calc R U P B 4
C47' C -0.303(4) 0.5760(17) 0.0692(14) 0.138(7) Uani 0.484(14) 1 d D U P B 4
H47C H -0.1987 0.5484 0.0890 0.166 Uiso 0.484(14) 1 calc R U P B 4
H47D H -0.2813 0.6069 0.0262 0.166 Uiso 0.484(14) 1 calc R U P B 4
C49' C -0.340(4) 0.7408(19) 0.1005(13) 0.149(7) Uani 0.484(14) 1 d D U P B 4
H49C H -0.3376 0.7779 0.0577 0.178 Uiso 0.484(14) 1 calc R U P B 4
H49D H -0.2272 0.7142 0.1132 0.178 Uiso 0.484(14) 1 calc R U P B 4
C50' C -0.433(7) 0.813(3) 0.142(2) 0.146(9) Uani 0.484(14) 1 d D U P B 4
H50D H -0.3809 0.8648 0.1381 0.220 Uiso 0.484(14) 1 calc R U P B 4
H50E H -0.5443 0.8411 0.1289 0.220 Uiso 0.484(14) 1 calc R U P B 4
H50F H -0.4337 0.7772 0.1846 0.220 Uiso 0.484(14) 1 calc R U P B 4
N1 N 0.5893(6) -0.4007(4) 0.5091(3) 0.0619(16) Uani 1 1 d . . . . .
N2 N 0.5386(7) -0.3153(4) 0.4698(3) 0.0619(16) Uani 1 1 d D . . . .
N3 N 0.0408(9) 0.1785(6) 0.0570(4) 0.0820(19) Uani 1 1 d D . . . .
N4 N 0.1129(8) 0.1120(5) 0.0233(4) 0.0796(19) Uani 1 1 d . . . . .
O1 O 0.3058(6) -0.2689(4) 0.5537(3) 0.0873(16) Uani 1 1 d . . . . .
O2 O 0.3406(6) -0.1342(3) 0.4328(3) 0.0850(16) Uani 1 1 d . . . . .
O3 O 0.3875(7) -0.0467(4) 0.3391(3) 0.120(2) Uani 1 1 d . . . . .
O4 O 0.0892(7) -0.0850(4) 0.5193(3) 0.129(3) Uani 1 1 d . . . . .
O5 O -0.1498(7) 0.2665(5) -0.0357(3) 0.1003(19) Uani 1 1 d . . . . .
O6 O -0.1839(7) 0.3392(4) 0.0821(3) 0.1015(19) Uani 1 1 d . . . . .
O7 O -0.1877(9) 0.3825(5) 0.1726(3) 0.141(3) Uani 1 1 d . . . . .
O8 O -0.3988(8) 0.4232(5) -0.0122(3) 0.132(3) Uani 1 1 d . . . . .
Sn1 Sn 0.13461(8) -0.00311(4) 0.43396(3) 0.1090(3) Uani 1 1 d . . . . .
Sn2 Sn -0.39283(10) 0.46779(5) 0.06816(3) 0.1176(3) Uani 1 1 d . . . . .
H2A H 0.454(5) -0.276(4) 0.483(3) 0.06(2) Uiso 1 1 d D . . . .
H3A H -0.044(6) 0.224(4) 0.043(4) 0.10(3) Uiso 1 1 d D . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.372(10) . ?
C1 C10 1.384(9) . ?
C1 H1 0.9300 . ?
C2 C3 1.373(12) . ?
C2 H2 0.9300 . ?
C3 C4 1.354(12) . ?
C3 H3 0.9300 . ?
C4 C5 1.401(10) . ?
C4 H4 0.9300 . ?
C5 C10 1.399(10) . ?
C5 C6 1.424(11) . ?
C6 C7 1.339(10) . ?
C6 H6 0.9300 . ?
C7 C8 1.427(10) . ?
C7 H7 0.9300 . ?
C8 O1 1.247(8) . ?
C8 C9 1.452(9) . ?
C9 N1 1.321(8) . ?
C9 C10 1.455(9) . ?
C11 C12 1.388(9) . ?
C11 C16 1.390(9) . ?
C11 N2 1.395(9) . ?
C12 C13 1.368(10) . ?
C12 H12 0.9300 . ?
C13 C14 1.384(11) . ?
C13 H13 0.9300 . ?
C14 C15 1.357(10) . ?
C14 H14 0.9300 . ?
C15 C16 1.386(10) . ?
C15 H15 0.9300 . ?
C16 C17 1.494(10) . ?
C17 O3 1.236(8) . ?
C17 O2 1.284(9) . ?
C18 C19 1.479(14) . ?
C18 Sn1 2.207(17) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.479(15) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.578(15) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C18' C19' 1.497(19) . ?
C18' Sn1 1.82(4) . ?
C18' H18C 0.9700 . ?
C18' H18D 0.9700 . ?
C19' C20' 1.496(19) . ?
C19' H19C 0.9700 . ?
C19' H19D 0.9700 . ?
C20' C21' 1.530(19) . ?
C20' H20C 0.9700 . ?
C20' H20D 0.9700 . ?
C21' H21D 0.9600 . ?
C21' H21E 0.9600 . ?
C21' H21F 0.9600 . ?
C22 C23 1.544(12) . ?
C22 Sn1 2.119(12) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C23 C24 1.344(12) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C24 C25 1.513(12) . ?
C24 H24A 0.9700 . ?
C24 H24B 0.9700 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.388(13) . ?
C26 C31 1.393(12) . ?
C26 C35 1.426(13) . ?
C27 C28 1.365(15) . ?
C27 H27 0.9300 . ?
C28 C29 1.359(15) . ?
C28 H28 0.9300 . ?
C29 C30 1.393(13) . ?
C29 H29 0.9300 . ?
C30 C31 1.397(12) . ?
C30 H30 0.9300 . ?
C31 C32 1.449(11) . ?
C32 N4 1.314(10) . ?
C32 C33 1.451(11) . ?
C33 O5 1.238(9) . ?
C33 C34 1.437(11) . ?
C34 C35 1.319(12) . ?
C34 H34 0.9300 . ?
C35 H35 0.9300 . ?
C36 C37 1.392(10) . ?
C36 C41 1.394(11) . ?
C36 N3 1.400(10) . ?
C37 C38 1.373(12) . ?
C37 H37 0.9300 . ?
C38 C39 1.364(13) . ?
C38 H38 0.9300 . ?
C39 C40 1.372(11) . ?
C39 H39 0.9300 . ?
C40 C41 1.386(10) . ?
C40 H40 0.9300 . ?
C41 C42 1.489(11) . ?
C42 O7 1.232(10) . ?
C42 O6 1.293(10) . ?
C43 C44 1.528(14) . ?
C43 Sn2 2.092(15) . ?
C43 H43A 0.9700 . ?
C43 H43B 0.9700 . ?
C44 C45 1.396(15) . ?
C44 H44A 0.9700 . ?
C44 H44B 0.9700 . ?
C45 C46 1.457(15) . ?
C45 H45A 0.9700 . ?
C45 H45B 0.9700 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 C48 1.466(16) . ?
C47 Sn2 2.29(2) . ?
C47 H47A 0.9700 . ?
C47 H47B 0.9700 . ?
C48 C49 1.451(17) . ?
C48 H48A 0.9700 . ?
C48 H48B 0.9700 . ?
C49 C50 1.505(18) . ?
C49 H49A 0.9700 . ?
C49 H49B 0.9700 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C48' C49' 1.478(18) . ?
C48' C47' 1.508(17) . ?
C48' H48C 0.9700 . ?
C48' H48D 0.9700 . ?
C47' Sn2 1.92(2) . ?
C47' H47C 0.9700 . ?
C47' H47D 0.9700 . ?
C49' C50' 1.516(18) . ?
C49' H49C 0.9700 . ?
C49' H49D 0.9700 . ?
C50' H50D 0.9600 . ?
C50' H50E 0.9600 . ?
C50' H50F 0.9600 . ?
N1 N2 1.310(7) . ?
N2 H2A 0.85(2) . ?
N3 N4 1.307(9) . ?
N3 H3A 0.85(2) . ?
O2 Sn1 2.165(4) . ?
O4 Sn1 2.034(6) . ?
O4 Sn1 2.243(5) 2_556 ?
O6 Sn2 2.144(5) . ?
O8 Sn2 2.018(6) . ?
O8 Sn2 2.254(5) 2_465 ?
Sn1 O4 2.243(5) 2_556 ?
Sn2 O8 2.254(5) 2_465 ?

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
C2 C1 C10 120.9(8) . . ?
C2 C1 H1 119.6 . . ?
C10 C1 H1 119.6 . . ?
C1 C2 C3 119.9(9) . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C4 C3 C2 120.7(9) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C3 C4 C5 120.6(10) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
C10 C5 C4 118.9(8) . . ?
C10 C5 C6 119.6(7) . . ?
C4 C5 C6 121.5(9) . . ?
C7 C6 C5 122.4(8) . . ?
C7 C6 H6 118.8 . . ?
C5 C6 H6 118.8 . . ?
C6 C7 C8 122.2(8) . . ?
C6 C7 H7 118.9 . . ?
C8 C7 H7 118.9 . . ?
O1 C8 C7 122.6(7) . . ?
O1 C8 C9 120.7(7) . . ?
C7 C8 C9 116.7(7) . . ?
N1 C9 C8 124.0(6) . . ?
N1 C9 C10 115.3(6) . . ?
C8 C9 C10 120.6(7) . . ?
C1 C10 C5 119.1(7) . . ?
C1 C10 C9 122.4(8) . . ?
C5 C10 C9 118.5(7) . . ?
C12 C11 C16 120.1(8) . . ?
C12 C11 N2 118.5(7) . . ?
C16 C11 N2 121.4(6) . . ?
C13 C12 C11 119.9(8) . . ?
C13 C12 H12 120.0 . . ?
C11 C12 H12 120.0 . . ?
C12 C13 C14 120.9(8) . . ?
C12 C13 H13 119.6 . . ?
C14 C13 H13 119.6 . . ?
C15 C14 C13 118.6(8) . . ?
C15 C14 H14 120.7 . . ?
C13 C14 H14 120.7 . . ?
C14 C15 C16 122.6(8) . . ?
C14 C15 H15 118.7 . . ?
C16 C15 H15 118.7 . . ?
C15 C16 C11 118.0(7) . . ?
C15 C16 C17 117.7(7) . . ?
C11 C16 C17 124.3(7) . . ?
O3 C17 O2 122.7(7) . . ?
O3 C17 C16 119.0(8) . . ?
O2 C17 C16 118.3(7) . . ?
C19 C18 Sn1 122.0(11) . . ?
C19 C18 H18A 106.8 . . ?
Sn1 C18 H18A 106.8 . . ?
C19 C18 H18B 106.8 . . ?
Sn1 C18 H18B 106.8 . . ?
H18A C18 H18B 106.7 . . ?
C20 C19 C18 113.9(13) . . ?
C20 C19 H19A 108.8 . . ?
C18 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C18 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C19 C20 C21 106.4(13) . . ?
C19 C20 H20A 110.4 . . ?
C21 C20 H20A 110.4 . . ?
C19 C20 H20B 110.4 . . ?
C21 C20 H20B 110.4 . . ?
H20A C20 H20B 108.6 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19' C18' Sn1 116(2) . . ?
C19' C18' H18C 108.2 . . ?
Sn1 C18' H18C 108.2 . . ?
C19' C18' H18D 108.2 . . ?
Sn1 C18' H18D 108.2 . . ?
H18C C18' H18D 107.4 . . ?
C20' C19' C18' 111.4(19) . . ?
C20' C19' H19C 109.3 . . ?
C18' C19' H19C 109.3 . . ?
C20' C19' H19D 109.3 . . ?
C18' C19' H19D 109.3 . . ?
H19C C19' H19D 108.0 . . ?
C19' C20' C21' 107.7(18) . . ?
C19' C20' H20C 110.2 . . ?
C21' C20' H20C 110.2 . . ?
C19' C20' H20D 110.2 . . ?
C21' C20' H20D 110.2 . . ?
H20C C20' H20D 108.5 . . ?
C20' C21' H21D 109.5 . . ?
C20' C21' H21E 109.5 . . ?
H21D C21' H21E 109.5 . . ?
C20' C21' H21F 109.5 . . ?
H21D C21' H21F 109.5 . . ?
H21E C21' H21F 109.5 . . ?
C23 C22 Sn1 130.2(10) . . ?
C23 C22 H22A 104.7 . . ?
Sn1 C22 H22A 104.7 . . ?
C23 C22 H22B 104.7 . . ?
Sn1 C22 H22B 104.7 . . ?
H22A C22 H22B 105.7 . . ?
C24 C23 C22 112.9(12) . . ?
C24 C23 H23A 109.0 . . ?
C22 C23 H23A 109.0 . . ?
C24 C23 H23B 109.0 . . ?
C22 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
C23 C24 C25 116.5(12) . . ?
C23 C24 H24A 108.2 . . ?
C25 C24 H24A 108.2 . . ?
C23 C24 H24B 108.2 . . ?
C25 C24 H24B 108.2 . . ?
H24A C24 H24B 107.3 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C31 119.9(11) . . ?
C27 C26 C35 121.5(12) . . ?
C31 C26 C35 118.6(10) . . ?
C28 C27 C26 120.5(13) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C29 C28 C27 120.7(12) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C28 C29 C30 120.1(12) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C29 C30 C31 120.0(11) . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C26 C31 C30 118.7(10) . . ?
C26 C31 C32 119.7(9) . . ?
C30 C31 C32 121.6(11) . . ?
N4 C32 C31 116.0(9) . . ?
N4 C32 C33 124.1(8) . . ?
C31 C32 C33 119.9(9) . . ?
O5 C33 C34 122.2(9) . . ?
O5 C33 C32 121.3(9) . . ?
C34 C33 C32 116.5(9) . . ?
C35 C34 C33 122.2(10) . . ?
C35 C34 H34 118.9 . . ?
C33 C34 H34 118.9 . . ?
C34 C35 C26 123.0(11) . . ?
C34 C35 H35 118.5 . . ?
C26 C35 H35 118.5 . . ?
C37 C36 C41 119.3(8) . . ?
C37 C36 N3 119.0(9) . . ?
C41 C36 N3 121.6(7) . . ?
C38 C37 C36 120.3(10) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C39 C38 C37 120.8(9) . . ?
C39 C38 H38 119.6 . . ?
C37 C38 H38 119.6 . . ?
C38 C39 C40 119.3(10) . . ?
C38 C39 H39 120.4 . . ?
C40 C39 H39 120.4 . . ?
C39 C40 C41 121.7(10) . . ?
C39 C40 H40 119.1 . . ?
C41 C40 H40 119.1 . . ?
C40 C41 C36 118.5(8) . . ?
C40 C41 C42 116.6(9) . . ?
C36 C41 C42 124.8(8) . . ?
O7 C42 O6 121.7(8) . . ?
O7 C42 C41 120.8(9) . . ?
O6 C42 C41 117.5(9) . . ?
C44 C43 Sn2 107.0(10) . . ?
C44 C43 H43A 110.3 . . ?
Sn2 C43 H43A 110.3 . . ?
C44 C43 H43B 110.3 . . ?
Sn2 C43 H43B 110.3 . . ?
H43A C43 H43B 108.6 . . ?
C45 C44 C43 104.1(16) . . ?
C45 C44 H44A 110.9 . . ?
C43 C44 H44A 110.9 . . ?
C45 C44 H44B 110.9 . . ?
C43 C44 H44B 110.9 . . ?
H44A C44 H44B 109.0 . . ?
C44 C45 C46 103.7(16) . . ?
C44 C45 H45A 111.0 . . ?
C46 C45 H45A 111.0 . . ?
C44 C45 H45B 111.0 . . ?
C46 C45 H45B 111.0 . . ?
H45A C45 H45B 109.0 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 Sn2 118.8(15) . . ?
C48 C47 H47A 107.6 . . ?
Sn2 C47 H47A 107.6 . . ?
C48 C47 H47B 107.6 . . ?
Sn2 C47 H47B 107.6 . . ?
H47A C47 H47B 107.0 . . ?
C49 C48 C47 121.2(18) . . ?
C49 C48 H48A 107.0 . . ?
C47 C48 H48A 107.0 . . ?
C49 C48 H48B 107.0 . . ?
C47 C48 H48B 107.0 . . ?
H48A C48 H48B 106.8 . . ?
C48 C49 C50 117(2) . . ?
C48 C49 H49A 108.0 . . ?
C50 C49 H49A 108.0 . . ?
C48 C49 H49B 108.0 . . ?
C50 C49 H49B 108.0 . . ?
H49A C49 H49B 107.2 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49' C48' C47' 115.6(18) . . ?
C49' C48' H48C 108.4 . . ?
C47' C48' H48C 108.4 . . ?
C49' C48' H48D 108.4 . . ?
C47' C48' H48D 108.4 . . ?
H48C C48' H48D 107.4 . . ?
C48' C47' Sn2 116.3(17) . . ?
C48' C47' H47C 108.2 . . ?
Sn2 C47' H47C 108.2 . . ?
C48' C47' H47D 108.2 . . ?
Sn2 C47' H47D 108.2 . . ?
H47C C47' H47D 107.4 . . ?
C48' C49' C50' 115(2) . . ?
C48' C49' H49C 108.5 . . ?
C50' C49' H49C 108.5 . . ?
C48' C49' H49D 108.5 . . ?
C50' C49' H49D 108.5 . . ?
H49C C49' H49D 107.5 . . ?
C49' C50' H50D 109.5 . . ?
C49' C50' H50E 109.5 . . ?
H50D C50' H50E 109.5 . . ?
C49' C50' H50F 109.5 . . ?
H50D C50' H50F 109.5 . . ?
H50E C50' H50F 109.5 . . ?
N2 N1 C9 121.8(6) . . ?
N1 N2 C11 120.4(6) . . ?
N1 N2 H2A 114(4) . . ?
C11 N2 H2A 126(4) . . ?
N4 N3 C36 120.3(8) . . ?
N4 N3 H3A 117(6) . . ?
C36 N3 H3A 122(6) . . ?
N3 N4 C32 121.4(7) . . ?
C17 O2 Sn1 109.6(4) . . ?
Sn1 O4 Sn1 109.4(2) . 2_556 ?
C42 O6 Sn2 110.5(5) . . ?
Sn2 O8 Sn2 108.9(2) . 2_465 ?
C18' Sn1 O4 115.9(18) . . ?
C18' Sn1 C22 133.5(16) . . ?
O4 Sn1 C22 107.6(4) . . ?
C18' Sn1 O2 104.7(12) . . ?
O4 Sn1 O2 81.5(2) . . ?
C22 Sn1 O2 96.8(3) . . ?
O4 Sn1 C18 107.2(6) . . ?
C22 Sn1 C18 145.1(7) . . ?
O2 Sn1 C18 91.4(4) . . ?
C18' Sn1 O4 86.9(16) . 2_556 ?
O4 Sn1 O4 70.6(2) . 2_556 ?
C22 Sn1 O4 92.9(4) . 2_556 ?
O2 Sn1 O4 152.0(2) . 2_556 ?
C18 Sn1 O4 95.5(5) . 2_556 ?
C47' Sn2 O8 121.1(9) . . ?
C47' Sn2 C43 129.6(9) . . ?
O8 Sn2 C43 106.9(5) . . ?
C47' Sn2 O6 103.5(9) . . ?
O8 Sn2 O6 82.2(2) . . ?
C43 Sn2 O6 96.9(4) . . ?
C47' Sn2 O8 89.4(10) . 2_465 ?
O8 Sn2 O8 71.1(2) . 2_465 ?
C43 Sn2 O8 92.4(4) . 2_465 ?
O6 Sn2 O8 153.3(2) . 2_465 ?
O8 Sn2 C47 104.9(6) . . ?
C43 Sn2 C47 147.9(7) . . ?
O6 Sn2 C47 91.8(7) . . ?
O8 Sn2 C47 93.5(8) 2_465 . ?

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
C10 C1 C2 C3 1.3(13) . . . . ?
C1 C2 C3 C4 -1.0(15) . . . . ?
C2 C3 C4 C5 0.5(14) . . . . ?
C3 C4 C5 C10 -0.3(13) . . . . ?
C3 C4 C5 C6 -179.9(8) . . . . ?
C10 C5 C6 C7 1.5(12) . . . . ?
C4 C5 C6 C7 -179.0(8) . . . . ?
C5 C6 C7 C8 -1.4(13) . . . . ?
C6 C7 C8 O1 179.3(8) . . . . ?
C6 C7 C8 C9 0.4(12) . . . . ?
O1 C8 C9 N1 4.2(11) . . . . ?
C7 C8 C9 N1 -176.9(7) . . . . ?
O1 C8 C9 C10 -178.4(7) . . . . ?
C7 C8 C9 C10 0.5(10) . . . . ?
C2 C1 C10 C5 -1.2(12) . . . . ?
C2 C1 C10 C9 179.6(7) . . . . ?
C4 C5 C10 C1 0.7(11) . . . . ?
C6 C5 C10 C1 -179.8(7) . . . . ?
C4 C5 C10 C9 179.9(7) . . . . ?
C6 C5 C10 C9 -0.5(11) . . . . ?
N1 C9 C10 C1 -3.6(10) . . . . ?
C8 C9 C10 C1 178.8(7) . . . . ?
N1 C9 C10 C5 177.2(7) . . . . ?
C8 C9 C10 C5 -0.4(10) . . . . ?
C16 C11 C12 C13 0.1(12) . . . . ?
N2 C11 C12 C13 179.4(7) . . . . ?
C11 C12 C13 C14 0.1(13) . . . . ?
C12 C13 C14 C15 0.1(13) . . . . ?
C13 C14 C15 C16 -0.4(13) . . . . ?
C14 C15 C16 C11 0.5(12) . . . . ?
C14 C15 C16 C17 180.0(8) . . . . ?
C12 C11 C16 C15 -0.3(11) . . . . ?
N2 C11 C16 C15 -179.6(7) . . . . ?
C12 C11 C16 C17 -179.7(7) . . . . ?
N2 C11 C16 C17 1.0(11) . . . . ?
C15 C16 C17 O3 2.1(12) . . . . ?
C11 C16 C17 O3 -178.4(8) . . . . ?
C15 C16 C17 O2 -179.4(7) . . . . ?
C11 C16 C17 O2 0.0(12) . . . . ?
Sn1 C18 C19 C20 -65(2) . . . . ?
C18 C19 C20 C21 172.7(15) . . . . ?
Sn1 C18' C19' C20' 164(4) . . . . ?
C18' C19' C20' C21' 167(4) . . . . ?
Sn1 C22 C23 C24 70.0(18) . . . . ?
C22 C23 C24 C25 -179.2(12) . . . . ?
C31 C26 C27 C28 1.2(16) . . . . ?
C35 C26 C27 C28 -179.5(10) . . . . ?
C26 C27 C28 C29 -0.5(19) . . . . ?
C27 C28 C29 C30 0(2) . . . . ?
C28 C29 C30 C31 0.4(17) . . . . ?
C27 C26 C31 C30 -1.1(13) . . . . ?
C35 C26 C31 C30 179.6(8) . . . . ?
C27 C26 C31 C32 179.0(8) . . . . ?
C35 C26 C31 C32 -0.2(13) . . . . ?
C29 C30 C31 C26 0.3(14) . . . . ?
C29 C30 C31 C32 -179.8(9) . . . . ?
C26 C31 C32 N4 179.6(8) . . . . ?
C30 C31 C32 N4 -0.3(12) . . . . ?
C26 C31 C32 C33 -0.4(12) . . . . ?
C30 C31 C32 C33 179.7(8) . . . . ?
N4 C32 C33 O5 1.0(13) . . . . ?
C31 C32 C33 O5 -179.0(8) . . . . ?
N4 C32 C33 C34 -179.8(8) . . . . ?
C31 C32 C33 C34 0.2(11) . . . . ?
O5 C33 C34 C35 179.9(9) . . . . ?
C32 C33 C34 C35 0.7(13) . . . . ?
C33 C34 C35 C26 -1.4(15) . . . . ?
C27 C26 C35 C34 -178.0(10) . . . . ?
C31 C26 C35 C34 1.2(15) . . . . ?
C41 C36 C37 C38 -0.1(13) . . . . ?
N3 C36 C37 C38 -179.5(8) . . . . ?
C36 C37 C38 C39 -0.7(15) . . . . ?
C37 C38 C39 C40 1.3(16) . . . . ?
C38 C39 C40 C41 -1.0(15) . . . . ?
C39 C40 C41 C36 0.1(13) . . . . ?
C39 C40 C41 C42 179.1(8) . . . . ?
C37 C36 C41 C40 0.4(12) . . . . ?
N3 C36 C41 C40 179.7(7) . . . . ?
C37 C36 C41 C42 -178.5(8) . . . . ?
N3 C36 C41 C42 0.8(13) . . . . ?
C40 C41 C42 O7 -1.0(14) . . . . ?
C36 C41 C42 O7 177.9(9) . . . . ?
C40 C41 C42 O6 -178.6(8) . . . . ?
C36 C41 C42 O6 0.3(13) . . . . ?
Sn2 C43 C44 C45 -177.6(16) . . . . ?
C43 C44 C45 C46 -155.4(18) . . . . ?
Sn2 C47 C48 C49 47(3) . . . . ?
C47 C48 C49 C50 -178(4) . . . . ?
C49' C48' C47' Sn2 -178(2) . . . . ?
C47' C48' C49' C50' -171(4) . . . . ?
C8 C9 N1 N2 -1.2(11) . . . . ?
C10 C9 N1 N2 -178.7(6) . . . . ?
C9 N1 N2 C11 178.4(6) . . . . ?
C12 C11 N2 N1 0.2(10) . . . . ?
C16 C11 N2 N1 179.5(6) . . . . ?
C37 C36 N3 N4 0.1(11) . . . . ?
C41 C36 N3 N4 -179.2(7) . . . . ?
C36 N3 N4 C32 179.4(7) . . . . ?
C31 C32 N4 N3 -180.0(7) . . . . ?
C33 C32 N4 N3 0.0(12) . . . . ?
O3 C17 O2 Sn1 -0.6(11) . . . . ?
C16 C17 O2 Sn1 -179.0(5) . . . . ?
O7 C42 O6 Sn2 1.0(12) . . . . ?
C41 C42 O6 Sn2 178.5(6) . . . . ?
C19' C18' Sn1 O4 -117(4) . . . . ?
C19' C18' Sn1 C22 41(5) . . . . ?
C19' C18' Sn1 O2 156(4) . . . . ?
C19' C18' Sn1 O4 -50(4) . . . 2_556 ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2 H2A O1 0.85(2) 1.89(4) 2.597(8) 140(6) .
N2 H2A O2 0.85(2) 2.08(5) 2.648(7) 124(5) .
N3 H3A O5 0.85(2) 1.92(6) 2.594(9) 135(8) .
N3 H3A O6 0.85(2) 2.04(7) 2.651(10) 128(7) .

_refine_diff_density_max         0.590
_refine_diff_density_min         -0.929
_refine_diff_density_rms         0.074


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

data_KSP16
_database_code_depnum_ccdc_archive 'CCDC 1968230'
loop_
_audit_author_name
_audit_author_address
'Waldemar Maniukiewicz'
'Institute of General and Ecological Chemistry , Lodz University of Technology'
_audit_update_record             
;
2019-11-26 deposited with the CCDC.	2020-03-09 downloaded from the CCDC.
;

#===============================================================================

# CHEMICAL DATA

_chemical_name_systematic        
;
;
_chemical_melting_point          ?
_chemical_formula_moiety         'C100 H116 N8 O14 Sn4, C7 H8'

_chemical_formula_structural     ?
_chemical_formula_sum            'C107 H124 N8 O14 Sn4'
_chemical_formula_iupac          ?
_chemical_formula_weight         2220.99

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

#===============================================================================

# CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   12.1753(1)
_cell_length_b                   13.8987(1)
_cell_length_c                   15.6416(1)
_cell_angle_alpha                103.640(1)
_cell_angle_beta                 90.895(1)
_cell_angle_gamma                103.259(1)
_cell_volume                     2496.86(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100
_cell_measurement_reflns_used    76002
_cell_measurement_theta_min      2.739
_cell_measurement_theta_max      32.911
_exptl_crystal_description       Needle
_exptl_crystal_colour            Orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.13
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.477
_exptl_crystal_F_000             1134
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_min  0.204
_exptl_absorpt_correction_T_max  1.000
_shelx_estimated_absorpt_T_min   0.570
_shelx_estimated_absorpt_T_max   0.875
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_empirical_full_min 0.732
_exptl_absorpt_empirical_full_max 1.394
_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
#===============================================================================

# EXPERIMENTAL DATA

_diffrn_ambient_temperature      100
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'Pilatus 300K'
_diffrn_detector_area_resol_mean 5.8140

# number of measured reflections (redundant set)
_diffrn_reflns_number            76306
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.58
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_reduction_process 
;
;

# number of unique reflections
_reflns_number_total             8830
# number of observed reflections (> n sig(I))
_reflns_number_gt                8393
_reflns_threshold_expression     I>2σ(I)

_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'

#===============================================================================

# REFINEMENT DATA

_refine_special_details          
;Refinement on F² for ALL reflections except those
 flagged by the user for potential systematic errors.
 Weighted R-factors wR and all goodnesses of fit S
 are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The
 observed criterion of F² > 2sigma(F²) is used only
 for calculating -R-factor-obs 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.,disordered one n-butyl ligand and toluene solvent
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'W=1/[Σ²(FO²)+(0.0485P)²+3.6343P] WHERE P=(FO²+2FC²)/3'
_atom_sites_solution_primary     diffmap
_atom_sites_solution_secondary   diffmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         8830
_refine_ls_number_parameters     710
_refine_ls_number_restraints     117
_refine_ls_number_constraints    ?
_refine_ls_R_factor_all          0.0319
_refine_ls_R_factor_gt           0.0306
_refine_ls_wR_factor_ref         0.0821
_refine_ls_wR_factor_gt          0.0811
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         1.594
_refine_diff_density_min         -0.962
_refine_diff_density_rms         0.089

#===============================================================================

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn Uani 0.54075(2) 0.28373(2) 0.53409(2) 1.000 0.0231(1) d . . .
Sn2 Sn Uani 0.57206(2) 0.56987(2) 0.59310(2) 1.000 0.0175(1) d . . .
O1 O Uani 1.2325(2) 0.71635(17) 1.04314(17) 1.000 0.0495(8) d . . .
O2 O Uani 0.67886(17) 0.36245(14) 0.64419(13) 1.000 0.0301(6) d . . .
O3 O Uani 0.63826(18) 0.51182(16) 0.70133(13) 1.000 0.0330(6) d . . .
O4 O Uani 0.51849(15) 0.42095(13) 0.52270(11) 1.000 0.0219(5) d . . .
O5 O Uani 0.13416(17) -0.19219(15) -0.09081(13) 1.000 0.0312(6) d . . .
O6 O Uani 0.42229(16) 0.23753(15) 0.41727(12) 1.000 0.0278(6) d . . .
O7 O Uani 0.4395(2) 0.08546(16) 0.42728(14) 1.000 0.0416(7) d . . .
N1 N Uani 1.15259(19) 0.50934(17) 0.94619(14) 1.000 0.0251(7) d . . .
N2 N Uani 1.0936(2) 0.57318(19) 0.93294(15) 1.000 0.0268(7) d . . .
N3 N Uani 0.2024(2) -0.03367(18) 0.03771(15) 1.000 0.0247(7) d . . .
N4 N Uani 0.15642(18) 0.01809(17) -0.00617(14) 1.000 0.0211(6) d . . .
C1 C Uani 1.2716(2) 0.3650(2) 0.9694(2) 1.000 0.0318(9) d . . .
C2 C Uani 1.3255(3) 0.2947(3) 0.9882(2) 1.000 0.0371(10) d . . .
C3 C Uani 1.4167(3) 0.3256(3) 1.0528(2) 1.000 0.0387(10) d . . .
C4 C Uani 1.4524(2) 0.4264(3) 1.09539(19) 1.000 0.0344(10) d . . .
C5 C Uani 1.3982(2) 0.4992(2) 1.07841(18) 1.000 0.0291(8) d . . .
C6 C Uani 1.4335(2) 0.6043(3) 1.12648(19) 1.000 0.0343(9) d . . .
C7 C Uani 1.3804(3) 0.6752(2) 1.1154(2) 1.000 0.0399(10) d . . .
C8 C Uani 1.2821(3) 0.6502(2) 1.0528(2) 1.000 0.0360(9) d . . .
C9 C Uani 1.2442(2) 0.5436(2) 1.00218(18) 1.000 0.0276(8) d . . .
C10 C Uani 1.3048(2) 0.4682(2) 1.01506(18) 1.000 0.0268(8) d . . .
C11 C Uani 0.9963(2) 0.5391(2) 0.87436(17) 1.000 0.0235(7) d . . .
C12 C Uani 0.9666(2) 0.4405(2) 0.81983(18) 1.000 0.0258(8) d . . .
C13 C Uani 0.8697(2) 0.4116(2) 0.76310(18) 1.000 0.0256(8) d . . .
C14 C Uani 0.8023(2) 0.47953(19) 0.75982(16) 1.000 0.0216(7) d . . .
C15 C Uani 0.8333(2) 0.5776(2) 0.81481(17) 1.000 0.0250(8) d . . .
C16 C Uani 0.9300(2) 0.6072(2) 0.87169(17) 1.000 0.0263(8) d . . .
C17 C Uani 0.6982(2) 0.4485(2) 0.69796(17) 1.000 0.0236(8) d . . .
C18 C Uani 0.6759(2) 0.2371(2) 0.46555(19) 1.000 0.0282(8) d . . .
C19 C Uani 0.7215(3) 0.1610(3) 0.5050(2) 1.000 0.0365(10) d . . .
C20 C Uani 0.8125(3) 0.1227(3) 0.4520(2) 1.000 0.0470(11) d . . .
C21 C Uani 0.8385(7) 0.0254(7) 0.4870(6) 0.500 0.047(3) d P . 1
C21A C Uani 0.8870(8) 0.0803(7) 0.5009(6) 0.500 0.049(3) d P . 2
C22 C Uani 0.4296(3) 0.2331(3) 0.6263(2) 1.000 0.0463(8) d U . .
C23 C Uani 0.3192(6) 0.1939(6) 0.6009(4) 0.500 0.0459(8) d UP . 1
C23A C Uani 0.4365(6) 0.1612(5) 0.6713(4) 0.500 0.0439(8) d UP . 2
C24 C Uani 0.2491(6) 0.1508(6) 0.6697(4) 0.500 0.0454(8) d UP . 1
C24A C Uani 0.3452(6) 0.1355(5) 0.7339(4) 0.500 0.0434(8) d UP . 2
C25 C Uani 0.2558(7) 0.2232(6) 0.7561(5) 0.500 0.0489(10) d UP . 1
C25A C Uani 0.3640(6) 0.0570(5) 0.7811(4) 0.500 0.0403(12) d UP . 2
C26 C Uani 0.0505(2) 0.1348(2) -0.0881(2) 1.000 0.0307(9) d . . .
C27 C Uani 0.0015(3) 0.1916(3) -0.1316(3) 1.000 0.0444(11) d . . .
C28 C Uani -0.0415(4) 0.1516(3) -0.2192(3) 1.000 0.0557(12) d . . .
C29 C Uani -0.0378(3) 0.0541(3) -0.2618(2) 1.000 0.0477(11) d . . .
C30 C Uani 0.0095(3) -0.0060(2) -0.21825(19) 1.000 0.0325(9) d . . .
C31 C Uani 0.0076(3) -0.1105(3) -0.26026(19) 1.000 0.0360(9) d . . .
C32 C Uani 0.0472(2) -0.1718(2) -0.21939(19) 1.000 0.0328(9) d . . .
C33 C Uani 0.0981(2) -0.1351(2) -0.12930(18) 1.000 0.0255(8) d . . .
C34 C Uani 0.1058(2) -0.0280(2) -0.08589(17) 1.000 0.0216(7) d . . .
C35 C Uani 0.0558(2) 0.0352(2) -0.13031(18) 1.000 0.0250(8) d . . .
C36 C Uani 0.2541(2) 0.0134(2) 0.12282(18) 1.000 0.0259(8) d . . .
C37 C Uani 0.2605(2) 0.1157(2) 0.16224(18) 1.000 0.0259(8) d . . .
C38 C Uani 0.3095(2) 0.1563(2) 0.24742(18) 1.000 0.0277(8) d . . .
C39 C Uani 0.3519(2) 0.0968(2) 0.29412(18) 1.000 0.0276(8) d . . .
C40 C Uani 0.3450(3) -0.0051(2) 0.2531(2) 1.000 0.0347(9) d . . .
C41 C Uani 0.2966(3) -0.0467(2) 0.1679(2) 1.000 0.0344(9) d . . .
C42 C Uani 0.4077(2) 0.1396(2) 0.38543(19) 1.000 0.0293(8) d . . .
C43 C Uani 0.4526(2) 0.6117(2) 0.68374(17) 1.000 0.0252(8) d . . .
C44 C Uani 0.3599(2) 0.5216(2) 0.69308(19) 1.000 0.0310(9) d . . .
C45 C Uani 0.2736(3) 0.5535(3) 0.7578(2) 1.000 0.0362(9) d . . .
C46 C Uani 0.2075(3) 0.6216(3) 0.7297(2) 1.000 0.0443(11) d . . .
C47 C Uani 0.7424(3) 0.6200(3) 0.5639(2) 1.000 0.0478(8) d U . .
C48 C Uani 0.7833(6) 0.6738(6) 0.5117(5) 0.500 0.0467(8) d UP . 1
C48A C Uani 0.8211(5) 0.5641(6) 0.5367(5) 0.500 0.0465(8) d UP . 2
C49 C Uani 0.9007(6) 0.6683(6) 0.4743(5) 0.500 0.0483(8) d UP . 1
C49A C Uani 0.9280(6) 0.6135(6) 0.5000(5) 0.500 0.0499(8) d UP . 2
C50 C Uani 0.9332(6) 0.7334(6) 0.4128(5) 0.500 0.0502(12) d UP . 1
C50A C Uani 1.0114(6) 0.5596(6) 0.4734(5) 0.500 0.0523(10) d UP . 2
C60 C Uani 0.4311(15) -0.1094(15) 0.9220(11) 0.500 0.041(4) d UP . -1
C61 C Uani 0.4953(13) -0.0477(12) 1.0088(7) 0.500 0.043(3) d UP . -1
C62 C Uani 0.5349(7) -0.0889(6) 1.0706(5) 0.500 0.048(2) d UP . -1
C63 C Uani 0.5974(7) -0.0321(7) 1.1468(6) 0.500 0.057(3) d UP . -1
C64 C Uani 0.6191(7) 0.0719(7) 1.1651(6) 0.500 0.053(2) d UP . -1
C65 C Uani 0.583(2) 0.116(2) 1.1050(13) 0.500 0.062(5) d UP . -1
C66 C Uani 0.5204(12) 0.0582(11) 1.0265(8) 0.500 0.043(4) d UP . -1
H1 H Uiso 1.21107 0.34340 0.92487 1.000 0.0380 c RU . .
H2 H Uiso 1.30104 0.22496 0.95747 1.000 0.0450 c RU . .
H2N H Uiso 1.121(3) 0.634(3) 0.954(3) 1.000 0.042(10) d . . .
H3 H Uiso 1.45299 0.27695 1.06658 1.000 0.0470 c RU . .
H3N H Uiso 0.194(3) -0.095(3) 0.016(3) 1.000 0.042(10) d . . .
H4 H Uiso 1.51561 0.44758 1.13756 1.000 0.0410 c RU . .
H6 H Uiso 1.49733 0.62424 1.16796 1.000 0.0410 c RU . .
H7 H Uiso 1.40748 0.74348 1.14908 1.000 0.0480 c RU . .
H12 H Uiso 1.01215 0.39380 0.82154 1.000 0.0310 c RU . .
H13 H Uiso 0.84886 0.34453 0.72593 1.000 0.0310 c RU . .
H15 H Uiso 0.78780 0.62441 0.81330 1.000 0.0300 c RU . .
H16 H Uiso 0.95079 0.67426 0.90887 1.000 0.0320 c RU . .
H18A H Uiso 0.64952 0.20499 0.40293 1.000 0.0340 c RU . .
H18B H Uiso 0.73806 0.29783 0.46755 1.000 0.0340 c RU . .
H19A H Uiso 0.75287 0.19466 0.56632 1.000 0.0440 c RU . .
H19B H Uiso 0.65837 0.10238 0.50675 1.000 0.0440 c RU . .
H20A H Uiso 0.88231 0.17796 0.45985 0.500 0.0560 c RUP A 1
H20B H Uiso 0.78692 0.10018 0.38849 0.500 0.0560 c RUP A 1
H20C H Uiso 0.77588 0.06922 0.39917 0.500 0.0560 c RUP B 2
H20D H Uiso 0.85983 0.17963 0.43133 0.500 0.0560 c RUP B 2
H21A H Uiso 0.87026 0.04955 0.54838 0.500 0.0700 c RUP . 1
H21B H Uiso 0.89276 -0.00399 0.45006 0.500 0.0700 c RUP . 1
H21C H Uiso 0.76792 -0.02678 0.48322 0.500 0.0700 c RUP . 1
H21D H Uiso 0.93300 0.13514 0.54779 0.500 0.0730 c RUP . 2
H21E H Uiso 0.93668 0.04893 0.46038 0.500 0.0730 c RUP . 2
H21F H Uiso 0.84059 0.02862 0.52704 0.500 0.0730 c RUP . 2
H22A H Uiso 0.42804 0.29546 0.67214 0.500 0.0560 c RUP . 2
H22B H Uiso 0.35354 0.20973 0.59464 0.500 0.0560 c RUP . 2
H22C H Uiso 0.45842 0.18087 0.64699 0.500 0.0560 c RUP . 1
H22D H Uiso 0.43536 0.29164 0.67788 0.500 0.0560 c RUP . 1
H23A H Uiso 0.31211 0.13884 0.54632 0.500 0.0550 c RUP . 1
H23B H Uiso 0.28689 0.24781 0.58636 0.500 0.0550 c RUP . 1
H23C H Uiso 0.51048 0.18384 0.70605 0.500 0.0530 c RUP . 2
H23D H Uiso 0.43730 0.09726 0.62727 0.500 0.0530 c RUP . 2
H24A H Uiso 0.16892 0.12683 0.64623 0.500 0.0540 c RUP . 1
H24B H Uiso 0.27466 0.09074 0.67809 0.500 0.0540 c RUP . 1
H24C H Uiso 0.34274 0.19875 0.77826 0.500 0.0520 c RUP . 2
H24D H Uiso 0.27079 0.10983 0.69976 0.500 0.0520 c RUP . 2
H25A H Uiso 0.33164 0.23727 0.78518 0.500 0.0730 c RUP . 1
H25B H Uiso 0.19954 0.19362 0.79273 0.500 0.0730 c RUP . 1
H25C H Uiso 0.24061 0.28680 0.74791 0.500 0.0730 c RUP . 1
H25D H Uiso 0.36977 -0.00494 0.73774 0.500 0.0600 c RUP . 2
H25E H Uiso 0.30032 0.04066 0.81699 0.500 0.0600 c RUP . 2
H25F H Uiso 0.43422 0.08432 0.81939 0.500 0.0600 c RUP . 2
H26 H Uiso 0.08102 0.16339 -0.02880 1.000 0.0370 c RU . .
H27 H Uiso -0.00297 0.25844 -0.10179 1.000 0.0540 c RU . .
H28 H Uiso -0.07340 0.19180 -0.24936 1.000 0.0670 c RU . .
H29 H Uiso -0.06763 0.02698 -0.32131 1.000 0.0570 c RU . .
H31 H Uiso -0.02308 -0.13726 -0.31962 1.000 0.0430 c RU . .
H32 H Uiso 0.04188 -0.24059 -0.24994 1.000 0.0390 c RU . .
H37 H Uiso 0.23165 0.15680 0.13122 1.000 0.0310 c RU . .
H38 H Uiso 0.31447 0.22604 0.27468 1.000 0.0330 c RU . .
H40 H Uiso 0.37375 -0.04637 0.28390 1.000 0.0420 c RU . .
H41 H Uiso 0.29250 -0.11625 0.14028 1.000 0.0410 c RU . .
H43A H Uiso 0.49293 0.64624 0.74227 1.000 0.0300 c RU . .
H43B H Uiso 0.41755 0.66109 0.66394 1.000 0.0300 c RU . .
H44A H Uiso 0.39471 0.47266 0.71384 1.000 0.0370 c RU . .
H44B H Uiso 0.32005 0.48649 0.63451 1.000 0.0370 c RU . .
H45A H Uiso 0.21981 0.49127 0.76518 1.000 0.0430 c RU . .
H45B H Uiso 0.31418 0.58936 0.81603 1.000 0.0430 c RU . .
H46A H Uiso 0.25946 0.68566 0.72628 1.000 0.0660 c RU . .
H46B H Uiso 0.15230 0.63611 0.77284 1.000 0.0660 c RU . .
H46C H Uiso 0.16786 0.58734 0.67169 1.000 0.0660 c RU . .
H47A H Uiso 0.78344 0.65646 0.62185 0.500 0.0570 c RUP . 1
H47B H Uiso 0.76937 0.55676 0.54505 0.500 0.0570 c RUP . 1
H47C H Uiso 0.73824 0.65824 0.51849 0.500 0.0570 c RUP . 2
H47D H Uiso 0.77901 0.67155 0.61786 0.500 0.0570 c RUP . 2
H48A H Uiso 0.78837 0.74585 0.54220 0.500 0.0560 c RUP . 1
H48B H Uiso 0.72722 0.65641 0.46054 0.500 0.0560 c RUP . 1
H48C H Uiso 0.78229 0.50260 0.49096 0.500 0.0560 c RUP . 2
H48D H Uiso 0.84411 0.54031 0.58754 0.500 0.0560 c RUP . 2
H49A H Uiso 0.95928 0.68910 0.52401 0.500 0.0580 c RUP . 1
H49B H Uiso 0.89812 0.59678 0.44347 0.500 0.0580 c RUP . 1
H49C H Uiso 0.90440 0.63575 0.44839 0.500 0.0600 c RUP . 2
H49D H Uiso 0.96504 0.67610 0.54519 0.500 0.0600 c RUP . 2
H50A H Uiso 0.87792 0.71071 0.36162 0.500 0.0750 c RUP . 1
H50B H Uiso 1.00828 0.72874 0.39321 0.500 0.0750 c RUP . 1
H50C H Uiso 0.93512 0.80429 0.44260 0.500 0.0750 c RUP . 1
H50D H Uiso 1.05411 0.58725 0.42841 0.500 0.0780 c RUP . 2
H50E H Uiso 0.97523 0.48731 0.44886 0.500 0.0780 c RUP . 2
H50F H Uiso 1.06302 0.56666 0.52443 0.500 0.0780 c RUP . 2
H60A H Uiso 0.38061 -0.07138 0.90315 0.500 0.0610 c RUP . -1
H60B H Uiso 0.38638 -0.17464 0.92961 0.500 0.0610 c RUP . -1
H60C H Uiso 0.48492 -0.12188 0.87715 0.500 0.0610 c RUP . -1
H62 H Uiso 0.51808 -0.16105 1.06015 0.500 0.0580 c RUP . -1
H63 H Uiso 0.62543 -0.06461 1.18653 0.500 0.0690 c RUP . -1
H64 H Uiso 0.65865 0.11248 1.21914 0.500 0.0640 c RUP . -1
H65 H Uiso 0.60136 0.18861 1.11644 0.500 0.0740 c RUP . -1
H66 H Uiso 0.49507 0.09093 0.98569 0.500 0.0520 c RUP . -1


#===============================================================================

# MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
Sn1 O2 2.273(2) . .
Sn1 O4 2.0343(18) . .
Sn1 O6 2.1842(19) . .
Sn1 C18 2.120(3) . .
Sn1 C22 2.124(4) . .
Sn2 O3 2.251(2) . .
Sn2 O4 2.0507(18) . .
Sn2 C43 2.128(3) . .
Sn2 C47 2.124(4) . .
Sn2 O4 2.1503(18) . 2_666
Sn2 O6 2.705(2) . 2_666
O1 C8 1.245(4) . .
O2 C17 1.258(3) . .
O3 C17 1.259(3) . .
O5 C33 1.250(3) . .
O6 C42 1.303(3) . .
O7 C42 1.226(4) . .
N1 N2 1.312(3) . .
N1 C9 1.329(3) . .
N2 C11 1.404(4) . .
N3 N4 1.307(3) . .
N3 C36 1.404(4) . .
N4 C34 1.328(3) . .
C1 C2 1.377(5) . .
C1 C10 1.405(4) . .
C2 C3 1.407(5) . .
N2 H2N 0.82(4) . .
N3 H3N 0.82(4) . .
C3 C4 1.366(6) . .
C4 C5 1.399(4) . .
C5 C6 1.438(5) . .
C5 C10 1.414(4) . .
C6 C7 1.337(5) . .
C7 C8 1.457(5) . .
C8 C9 1.469(4) . .
C9 C10 1.460(4) . .
C11 C16 1.385(4) . .
C11 C12 1.396(4) . .
C12 C13 1.387(4) . .
C13 C14 1.394(4) . .
C14 C17 1.498(4) . .
C14 C15 1.393(4) . .
C15 C16 1.385(4) . .
C18 C19 1.541(5) . .
C19 C20 1.513(5) . .
C20 C21 1.664(10) . .
C20 C21A 1.480(10) . .
C22 C23A 1.367(8) . .
C22 C23 1.344(8) . .
C23 C24 1.531(10) . .
C23A C24A 1.529(10) . .
C24 C25 1.471(10) . .
C24A C25A 1.509(10) . .
C26 C35 1.403(4) . .
C26 C27 1.378(5) . .
C27 C28 1.395(6) . .
C28 C29 1.373(6) . .
C29 C30 1.404(5) . .
C30 C35 1.412(4) . .
C30 C31 1.441(5) . .
C31 C32 1.343(5) . .
C32 C33 1.456(4) . .
C33 C34 1.464(4) . .
C34 C35 1.465(4) . .
C36 C37 1.394(4) . .
C36 C41 1.388(4) . .
C37 C38 1.384(4) . .
C38 C39 1.398(4) . .
C39 C42 1.496(4) . .
C39 C40 1.393(4) . .
C40 C41 1.383(4) . .
C43 C44 1.519(4) . .
C44 C45 1.536(4) . .
C45 C46 1.507(6) . .
C47 C48A 1.379(8) . .
C47 C48 1.266(9) . .
C48 C49 1.564(11) . .
C48A C49A 1.515(11) . .
C49 C50 1.469(11) . .
C49A C50A 1.407(11) . .
C1 H1 0.9500 . .
C2 H2 0.9500 . .
C3 H3 0.9500 . .
C4 H4 0.9500 . .
C6 H6 0.9500 . .
C7 H7 0.9500 . .
C12 H12 0.9500 . .
C13 H13 0.9500 . .
C15 H15 0.9500 . .
C16 H16 0.9500 . .
C18 H18A 0.9900 . .
C18 H18B 0.9900 . .
C19 H19A 0.9900 . .
C19 H19B 0.9900 . .
C20 H20A 0.9900 . .
C20 H20B 0.9900 . .
C20 H20C 0.9900 . .
C20 H20D 0.9900 . .
C21 H21A 0.9800 . .
C21 H21B 0.9800 . .
C21 H21C 0.9800 . .
C21A H21D 0.9800 . .
C21A H21E 0.9800 . .
C21A H21F 0.9800 . .
C22 H22A 0.9900 . .
C22 H22B 0.9900 . .
C22 H22C 0.9900 . .
C22 H22D 0.9900 . .
C23 H23A 0.9900 . .
C23 H23B 0.9900 . .
C23A H23C 0.9900 . .
C23A H23D 0.9900 . .
C24 H24A 0.9900 . .
C24 H24B 0.9900 . .
C24A H24C 0.9900 . .
C24A H24D 0.9900 . .
C25 H25A 0.9800 . .
C25 H25B 0.9800 . .
C25 H25C 0.9800 . .
C25A H25D 0.9800 . .
C25A H25E 0.9800 . .
C25A H25F 0.9800 . .
C26 H26 0.9500 . .
C27 H27 0.9500 . .
C28 H28 0.9500 . .
C29 H29 0.9500 . .
C31 H31 0.9500 . .
C32 H32 0.9500 . .
C37 H37 0.9500 . .
C38 H38 0.9500 . .
C40 H40 0.9500 . .
C41 H41 0.9500 . .
C43 H43A 0.9900 . .
C43 H43B 0.9900 . .
C44 H44A 0.9900 . .
C44 H44B 0.9900 . .
C45 H45A 0.9900 . .
C45 H45B 0.9900 . .
C46 H46A 0.9800 . .
C46 H46B 0.9800 . .
C46 H46C 0.9800 . .
C47 H47A 0.9900 . .
C47 H47B 0.9900 . .
C47 H47C 0.9900 . .
C47 H47D 0.9900 . .
C48 H48A 0.9900 . .
C48 H48B 0.9900 . .
C48A H48C 0.9900 . .
C48A H48D 0.9900 . .
C49 H49A 0.9900 . .
C49 H49B 0.9900 . .
C49A H49C 0.9900 . .
C49A H49D 0.9900 . .
C50 H50A 0.9800 . .
C50 H50B 0.9800 . .
C50 H50C 0.9800 . .
C50A H50D 0.9800 . .
C50A H50E 0.9800 . .
C50A H50F 0.9800 . .
C60 C61 1.52(2) . .
C61 C62 1.367(16) . .
C61 C66 1.39(2) . .
C62 C63 1.369(12) . .
C63 C64 1.367(14) . .
C64 C65 1.36(3) . .
C65 C66 1.40(3) . .
C60 H60A 0.9800 . .
C60 H60B 0.9800 . .
C60 H60C 0.9800 . .
C62 H62 0.9500 . .
C63 H63 0.9500 . .
C64 H64 0.9500 . .
C65 H65 0.9500 . .
C66 H66 0.9500 . .

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_2
_geom_angle_site_symmetry_3
O2 Sn1 O4 90.74(7) . . .
O2 Sn1 O6 167.42(7) . . .
O2 Sn1 C18 83.18(9) . . .
O2 Sn1 C22 90.46(11) . . .
O4 Sn1 O6 78.76(7) . . .
O4 Sn1 C18 114.61(9) . . .
O4 Sn1 C22 108.35(12) . . .
O6 Sn1 C18 94.82(9) . . .
O6 Sn1 C22 99.37(11) . . .
C18 Sn1 C22 136.58(13) . . .
O3 Sn2 O4 87.64(7) . . .
O3 Sn2 C43 84.72(9) . . .
O3 Sn2 C47 87.88(11) . . .
O3 Sn2 O4 163.03(7) . . 2_666
O3 Sn2 O6 130.58(7) . . 2_666
O4 Sn2 C43 111.33(9) . . .
O4 Sn2 C47 106.18(11) . . .
O4 Sn2 O4 76.13(7) . . 2_666
O4 Sn2 O6 141.78(6) . . 2_666
C43 Sn2 C47 141.35(12) . . .
O4 Sn2 C43 96.42(9) 2_666 . .
O6 Sn2 C43 77.64(9) 2_666 . .
O4 Sn2 C47 101.27(10) 2_666 . .
O6 Sn2 C47 78.78(12) 2_666 . .
O4 Sn2 O6 65.83(6) 2_666 . 2_666
Sn1 O2 C17 131.66(18) . . .
Sn2 O3 C17 130.23(18) . . .
Sn1 O4 Sn2 136.30(9) . . .
Sn1 O4 Sn2 119.65(8) . . 2_666
Sn2 O4 Sn2 103.87(8) . . 2_666
Sn1 O6 C42 108.12(17) . . .
Sn1 O6 Sn2 94.87(7) . . 2_666
Sn2 O6 C42 154.49(17) 2_666 . .
N2 N1 C9 119.4(2) . . .
N1 N2 C11 120.6(2) . . .
N4 N3 C36 120.0(2) . . .
N3 N4 C34 119.3(2) . . .
C2 C1 C10 121.0(3) . . .
C1 C2 C3 120.3(3) . . .
N1 N2 H2N 117(3) . . .
C11 N2 H2N 122(3) . . .
C2 C3 C4 119.2(3) . . .
N4 N3 H3N 118(3) . . .
C36 N3 H3N 122(3) . . .
C3 C4 C5 121.6(3) . . .
C4 C5 C6 121.1(3) . . .
C4 C5 C10 119.4(3) . . .
C6 C5 C10 119.5(2) . . .
C5 C6 C7 122.9(3) . . .
C6 C7 C8 121.6(3) . . .
O1 C8 C9 121.7(3) . . .
C7 C8 C9 117.0(3) . . .
O1 C8 C7 121.3(3) . . .
N1 C9 C8 123.2(3) . . .
N1 C9 C10 116.6(2) . . .
C8 C9 C10 120.2(2) . . .
C1 C10 C5 118.4(2) . . .
C1 C10 C9 122.7(2) . . .
C5 C10 C9 118.9(2) . . .
N2 C11 C16 117.7(2) . . .
C12 C11 C16 120.4(2) . . .
N2 C11 C12 121.9(2) . . .
C11 C12 C13 119.1(2) . . .
C12 C13 C14 121.0(3) . . .
C13 C14 C17 120.9(2) . . .
C13 C14 C15 119.1(2) . . .
C15 C14 C17 120.0(2) . . .
C14 C15 C16 120.4(2) . . .
C11 C16 C15 120.0(2) . . .
O2 C17 C14 117.8(2) . . .
O3 C17 C14 117.6(2) . . .
O2 C17 O3 124.5(2) . . .
Sn1 C18 C19 112.3(2) . . .
C18 C19 C20 111.9(3) . . .
C19 C20 C21 108.5(4) . . .
C21 C20 C21A 29.9(5) . . .
C19 C20 C21A 114.4(4) . . .
Sn1 C22 C23 119.0(3) . . .
Sn1 C22 C23A 127.8(4) . . .
C23 C22 C23A 94.2(5) . . .
C22 C23 C24 114.5(5) . . .
C22 C23A C24A 118.8(6) . . .
C23 C24 C25 114.7(7) . . .
C23A C24A C25A 113.6(6) . . .
C27 C26 C35 120.7(3) . . .
C26 C27 C28 120.4(4) . . .
C27 C28 C29 120.0(4) . . .
C28 C29 C30 120.7(3) . . .
C29 C30 C31 121.3(3) . . .
C29 C30 C35 119.5(3) . . .
C31 C30 C35 119.2(3) . . .
C30 C31 C32 123.0(3) . . .
C31 C32 C33 121.4(3) . . .
O5 C33 C32 121.6(3) . . .
C32 C33 C34 117.0(2) . . .
O5 C33 C34 121.4(2) . . .
N4 C34 C35 115.9(2) . . .
C33 C34 C35 120.2(2) . . .
N4 C34 C33 123.9(2) . . .
C26 C35 C34 122.3(2) . . .
C30 C35 C34 119.0(2) . . .
C26 C35 C30 118.7(3) . . .
N3 C36 C37 121.9(2) . . .
N3 C36 C41 117.4(3) . . .
C37 C36 C41 120.7(3) . . .
C36 C37 C38 118.8(2) . . .
C37 C38 C39 121.3(3) . . .
C38 C39 C42 122.3(2) . . .
C40 C39 C42 118.9(3) . . .
C38 C39 C40 118.7(3) . . .
C39 C40 C41 120.6(3) . . .
C36 C41 C40 119.8(3) . . .
O7 C42 C39 121.6(3) . . .
O6 C42 O7 122.0(3) . . .
O6 C42 C39 116.4(2) . . .
Sn2 C43 C44 113.34(18) . . .
C43 C44 C45 112.6(3) . . .
C44 C45 C46 114.4(3) . . .
Sn2 C47 C48 130.2(4) . . .
Sn2 C47 C48A 129.5(4) . . .
C48 C47 C48A 86.4(5) . . .
C47 C48 C49 120.6(7) . . .
C47 C48A C49A 119.2(7) . . .
C48 C49 C50 113.1(7) . . .
C48A C49A C50A 120.9(7) . . .
C2 C1 H1 120.00 . . .
C10 C1 H1 119.00 . . .
C1 C2 H2 120.00 . . .
C3 C2 H2 120.00 . . .
C2 C3 H3 120.00 . . .
C4 C3 H3 120.00 . . .
C3 C4 H4 119.00 . . .
C5 C4 H4 119.00 . . .
C5 C6 H6 119.00 . . .
C7 C6 H6 119.00 . . .
C6 C7 H7 119.00 . . .
C8 C7 H7 119.00 . . .
C11 C12 H12 120.00 . . .
C13 C12 H12 120.00 . . .
C12 C13 H13 120.00 . . .
C14 C13 H13 119.00 . . .
C14 C15 H15 120.00 . . .
C16 C15 H15 120.00 . . .
C11 C16 H16 120.00 . . .
C15 C16 H16 120.00 . . .
Sn1 C18 H18A 109.00 . . .
Sn1 C18 H18B 109.00 . . .
C19 C18 H18A 109.00 . . .
C19 C18 H18B 109.00 . . .
H18A C18 H18B 108.00 . . .
C18 C19 H19A 109.00 . . .
C18 C19 H19B 109.00 . . .
C20 C19 H19A 109.00 . . .
C20 C19 H19B 109.00 . . .
H19A C19 H19B 108.00 . . .
C19 C20 H20A 110.00 . . .
C19 C20 H20B 110.00 . . .
C19 C20 H20C 109.00 . . .
C19 C20 H20D 109.00 . . .
C21 C20 H20A 110.00 . . .
C21 C20 H20B 110.00 . . .
C21 C20 H20C 84.00 . . .
C21 C20 H20D 134.00 . . .
C21A C20 H20A 81.00 . . .
C21A C20 H20B 128.00 . . .
C21A C20 H20C 109.00 . . .
C21A C20 H20D 109.00 . . .
H20A C20 H20B 108.00 . . .
H20A C20 H20C 131.00 . . .
H20A C20 H20D 31.00 . . .
H20B C20 H20C 29.00 . . .
H20B C20 H20D 81.00 . . .
H20C C20 H20D 108.00 . . .
C20 C21 H21A 110.00 . . .
C20 C21 H21B 110.00 . . .
C20 C21 H21C 110.00 . . .
H21A C21 H21B 109.00 . . .
H21A C21 H21C 109.00 . . .
H21B C21 H21C 109.00 . . .
C20 C21A H21D 110.00 . . .
C20 C21A H21E 110.00 . . .
C20 C21A H21F 109.00 . . .
H21D C21A H21E 109.00 . . .
H21D C21A H21F 109.00 . . .
H21E C21A H21F 109.00 . . .
Sn1 C22 H22A 105.00 . . .
Sn1 C22 H22B 105.00 . . .
Sn1 C22 H22C 108.00 . . .
Sn1 C22 H22D 108.00 . . .
C23 C22 H22A 102.00 . . .
C23 C22 H22B 14.00 . . .
C23 C22 H22C 108.00 . . .
C23 C22 H22D 108.00 . . .
C23A C22 H22A 105.00 . . .
C23A C22 H22B 105.00 . . .
C23A C22 H22C 20.00 . . .
C23A C22 H22D 98.00 . . .
H22A C22 H22B 106.00 . . .
H22A C22 H22C 116.00 . . .
H22A C22 H22D 9.00 . . .
H22B C22 H22C 116.00 . . .
H22B C22 H22D 113.00 . . .
H22C C22 H22D 107.00 . . .
C22 C23 H23A 109.00 . . .
C22 C23 H23B 109.00 . . .
C24 C23 H23A 109.00 . . .
C24 C23 H23B 109.00 . . .
H23A C23 H23B 108.00 . . .
C22 C23A H23C 108.00 . . .
C22 C23A H23D 108.00 . . .
C24A C23A H23C 108.00 . . .
C24A C23A H23D 108.00 . . .
H23C C23A H23D 107.00 . . .
C23 C24 H24A 109.00 . . .
C23 C24 H24B 109.00 . . .
C25 C24 H24A 109.00 . . .
C25 C24 H24B 109.00 . . .
H24A C24 H24B 108.00 . . .
C23A C24A H24C 109.00 . . .
C23A C24A H24D 109.00 . . .
C25A C24A H24C 109.00 . . .
C25A C24A H24D 109.00 . . .
H24C C24A H24D 108.00 . . .
C24 C25 H25A 109.00 . . .
C24 C25 H25B 109.00 . . .
C24 C25 H25C 109.00 . . .
H25A C25 H25B 109.00 . . .
H25A C25 H25C 110.00 . . .
H25B C25 H25C 109.00 . . .
C24A C25A H25D 110.00 . . .
C24A C25A H25E 109.00 . . .
C24A C25A H25F 109.00 . . .
H25D C25A H25E 109.00 . . .
H25D C25A H25F 109.00 . . .
H25E C25A H25F 109.00 . . .
C27 C26 H26 120.00 . . .
C35 C26 H26 120.00 . . .
C26 C27 H27 120.00 . . .
C28 C27 H27 120.00 . . .
C27 C28 H28 120.00 . . .
C29 C28 H28 120.00 . . .
C28 C29 H29 120.00 . . .
C30 C29 H29 120.00 . . .
C30 C31 H31 118.00 . . .
C32 C31 H31 118.00 . . .
C31 C32 H32 119.00 . . .
C33 C32 H32 119.00 . . .
C36 C37 H37 121.00 . . .
C38 C37 H37 121.00 . . .
C37 C38 H38 119.00 . . .
C39 C38 H38 119.00 . . .
C39 C40 H40 120.00 . . .
C41 C40 H40 120.00 . . .
C36 C41 H41 120.00 . . .
C40 C41 H41 120.00 . . .
Sn2 C43 H43A 109.00 . . .
Sn2 C43 H43B 109.00 . . .
C44 C43 H43A 109.00 . . .
C44 C43 H43B 109.00 . . .
H43A C43 H43B 108.00 . . .
C43 C44 H44A 109.00 . . .
C43 C44 H44B 109.00 . . .
C45 C44 H44A 109.00 . . .
C45 C44 H44B 109.00 . . .
H44A C44 H44B 108.00 . . .
C44 C45 H45A 109.00 . . .
C44 C45 H45B 109.00 . . .
C46 C45 H45A 109.00 . . .
C46 C45 H45B 109.00 . . .
H45A C45 H45B 108.00 . . .
C45 C46 H46A 109.00 . . .
C45 C46 H46B 109.00 . . .
C45 C46 H46C 109.00 . . .
H46A C46 H46B 109.00 . . .
H46A C46 H46C 109.00 . . .
H46B C46 H46C 110.00 . . .
Sn2 C47 H47A 105.00 . . .
Sn2 C47 H47B 105.00 . . .
Sn2 C47 H47C 105.00 . . .
Sn2 C47 H47D 105.00 . . .
C48 C47 H47A 105.00 . . .
C48 C47 H47B 105.00 . . .
C48 C47 H47C 25.00 . . .
C48 C47 H47D 95.00 . . .
C48A C47 H47A 95.00 . . .
C48A C47 H47B 25.00 . . .
C48A C47 H47C 105.00 . . .
C48A C47 H47D 105.00 . . .
H47A C47 H47B 106.00 . . .
H47A C47 H47C 119.00 . . .
H47A C47 H47D 14.00 . . .
H47B C47 H47C 116.00 . . .
H47B C47 H47D 119.00 . . .
H47C C47 H47D 106.00 . . .
C47 C48 H48A 107.00 . . .
C47 C48 H48B 107.00 . . .
C49 C48 H48A 107.00 . . .
C49 C48 H48B 107.00 . . .
H48A C48 H48B 107.00 . . .
C47 C48A H48C 107.00 . . .
C47 C48A H48D 108.00 . . .
C49A C48A H48C 107.00 . . .
C49A C48A H48D 108.00 . . .
H48C C48A H48D 107.00 . . .
C48 C49 H49A 109.00 . . .
C48 C49 H49B 109.00 . . .
C50 C49 H49A 109.00 . . .
C50 C49 H49B 109.00 . . .
H49A C49 H49B 108.00 . . .
C48A C49A H49C 107.00 . . .
C48A C49A H49D 107.00 . . .
C50A C49A H49C 107.00 . . .
C50A C49A H49D 107.00 . . .
H49C C49A H49D 107.00 . . .
C49 C50 H50A 110.00 . . .
C49 C50 H50B 109.00 . . .
C49 C50 H50C 109.00 . . .
H50A C50 H50B 109.00 . . .
H50A C50 H50C 109.00 . . .
H50B C50 H50C 109.00 . . .
C49A C50A H50D 110.00 . . .
C49A C50A H50E 109.00 . . .
C49A C50A H50F 109.00 . . .
H50D C50A H50E 109.00 . . .
H50D C50A H50F 109.00 . . .
H50E C50A H50F 109.00 . . .
C60 C61 C62 124.4(14) . . .
C60 C61 C66 118.8(13) . . .
C62 C61 C66 116.7(11) . . .
C61 C62 C63 123.8(10) . . .
C62 C63 C64 119.3(8) . . .
C63 C64 C65 118.9(13) . . .
C64 C65 C66 122(2) . . .
C61 C66 C65 119.3(16) . . .
C61 C60 H60A 109.00 . . .
C61 C60 H60B 109.00 . . .
C61 C60 H60C 109.00 . . .
H60A C60 H60B 110.00 . . .
H60A C60 H60C 109.00 . . .
H60B C60 H60C 110.00 . . .
C61 C62 H62 118.00 . . .
C63 C62 H62 118.00 . . .
C62 C63 H63 120.00 . . .
C64 C63 H63 120.00 . . .
C63 C64 H64 120.00 . . .
C65 C64 H64 121.00 . . .
C64 C65 H65 119.00 . . .
C66 C65 H65 119.00 . . .
C61 C66 H66 120.00 . . .
C65 C66 H66 120.00 . . .

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
#
#D   H   A   D - H  H...A   D...A    D - H...A  symm(A)
#
N2 H2N O1 0.82(4) 1.89(4) 2.557(4) 138(4) .
N3 H3N O5 0.82(4) 1.90(4) 2.570(3) 139(4) .
C16 H16 O5 0.95 2.55 3.210(3) 126 1_666
C23 H23A O7 0.99 2.53 3.316(7) 136 .
C41 H41 O1 0.95 2.40 3.317(4) 161 1_444



#===END
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: toluene'
