# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_comp6xH2OxH2O
_database_code_depnum_ccdc_archive 'CCDC 1588509'
_audit_update_record             
;
2017-11-30 deposited with the CCDC.
2018-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H29 Br3 O7 Sn, H2 O'
_chemical_formula_sum            'C14 H31 Br3 O8 Sn'
_chemical_formula_weight         685.81

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'
Br Br -0.2901 2.4595 '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                   7.1137(3)
_cell_length_b                   10.3359(4)
_cell_length_c                   16.6178(7)
_cell_angle_alpha                107.749(4)
_cell_angle_beta                 93.455(3)
_cell_angle_gamma                100.269(4)
_cell_volume                     1136.45(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6880
_cell_measurement_theta_min      2.8150
_cell_measurement_theta_max      29.9770

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.004
_exptl_crystal_F_000             668
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.031
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.018
_exptl_absorpt_coefficient_mu    6.432
_shelx_estimated_absorpt_T_min   0.826
_shelx_estimated_absorpt_T_max   0.893
_exptl_absorpt_correction_T_min  0.75537
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_probe          x-ray
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Sapphire3
_diffrn_measurement_method       'ω und ψ scan'
_diffrn_detector_area_resol_mean 16.0560
_diffrn_reflns_number            16632
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.095
_diffrn_reflns_theta_max         29.455
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.929
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.929
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.929
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             5861
_reflns_number_gt                5004
_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       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'ORTEP-III (1.0.3) (Farrugia, 2012)'
_computing_publication_material  'enCIFer Version 1.5.2'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0180P)²+1.5030P] 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         5861
_refine_ls_number_parameters     260
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0438
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0616
_refine_ls_wR_factor_gt          0.0589
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.13404(3) 0.91536(2) 0.30642(2) 0.01195(6) Uani 1 1 d . . . . .
Br1 Br 0.38129(5) 1.13281(4) 0.30905(2) 0.02195(8) Uani 1 1 d . . . . .
Br2 Br -0.09700(5) 1.05465(4) 0.38563(2) 0.02004(8) Uani 1 1 d . . . . .
Br3 Br -0.01635(5) 0.88432(4) 0.15800(2) 0.01849(8) Uani 1 1 d . . . . .
O1 O -0.0754(4) 0.7183(3) 0.28520(17) 0.0232(6) Uani 1 1 d D . . . .
O4 O 0.5802(5) 0.6007(4) 0.3987(2) 0.0192(7) Uani 0.8 1 d . . P A 1
O7 O 0.9195(3) 0.4913(2) 0.34327(16) 0.0212(5) Uani 1 1 d . . . . .
O10 O 0.8557(3) 0.2877(2) 0.16109(15) 0.0188(5) Uani 1 1 d . . . . .
O13 O 0.4726(3) 0.2550(2) 0.06757(15) 0.0184(5) Uani 1 1 d . . . . .
O16 O 0.3468(3) 0.5089(2) 0.10480(14) 0.0175(5) Uani 1 1 d . . . . .
O19 O 0.3293(3) 0.7686(2) 0.23170(14) 0.0155(5) Uani 1 1 d . . . . .
C1 C 0.2905(5) 0.8697(4) 0.4050(2) 0.0174(7) Uani 1 1 d . . . . .
H1C H 0.393669 0.951063 0.435845 0.021 Uiso 1 1 calc R U . . .
H1D H 0.202619 0.851987 0.446198 0.021 Uiso 1 1 calc R U . . .
C2 C 0.3778(7) 0.7459(5) 0.3699(3) 0.0380(11) Uani 1 1 d . . . . .
H2 H 0.268330 0.664214 0.356928 0.046 Uiso 1 1 calc R U . . .
C3 C 0.5183(5) 0.7265(4) 0.4350(2) 0.0174(7) Uani 1 1 d . . . . .
H3AA H 0.630355 0.805352 0.452418 0.021 Uiso 0.75 1 calc R U P A 1
H3AB H 0.455494 0.723417 0.486123 0.021 Uiso 0.75 1 calc R U P A 1
H3BC H 0.579509 0.818791 0.475680 0.021 Uiso 0.25 1 calc R U P A 2
H3BD H 0.445913 0.672518 0.467371 0.021 Uiso 0.25 1 calc R U P A 2
C5 C 0.7295(5) 0.5815(4) 0.4524(2) 0.0206(7) Uani 1 1 d . . . . .
H5AA H 0.679208 0.567076 0.503995 0.025 Uiso 0.75 1 calc R U P A 1
H5AB H 0.835639 0.664446 0.470368 0.025 Uiso 0.75 1 calc R U P A 1
H5BC H 0.619655 0.551852 0.481116 0.025 Uiso 0.25 1 calc R U P A 2
H5BD H 0.833195 0.643828 0.496921 0.025 Uiso 0.25 1 calc R U P A 2
C6 C 0.8006(5) 0.4568(4) 0.4026(2) 0.0208(7) Uani 1 1 d . . . . .
H6A H 0.875006 0.423618 0.441799 0.025 Uiso 1 1 calc R U . . .
H6B H 0.689929 0.381149 0.371960 0.025 Uiso 1 1 calc R U . . .
C8 C 1.0208(5) 0.3858(4) 0.3034(2) 0.0228(8) Uani 1 1 d . . . . .
H8A H 1.082670 0.357014 0.348304 0.027 Uiso 1 1 calc R U . . .
H8B H 1.124710 0.426762 0.276010 0.027 Uiso 1 1 calc R U . . .
C9 C 0.9020(5) 0.2587(4) 0.2381(2) 0.0200(7) Uani 1 1 d . . . . .
H9A H 0.974233 0.182841 0.226159 0.024 Uiso 1 1 calc R U . . .
H9B H 0.781874 0.227877 0.260273 0.024 Uiso 1 1 calc R U . . .
C11 C 0.7464(5) 0.1674(4) 0.0960(2) 0.0213(7) Uani 1 1 d . . . . .
H11A H 0.785215 0.083398 0.102570 0.026 Uiso 1 1 calc R U . . .
H11B H 0.775836 0.172984 0.039566 0.026 Uiso 1 1 calc R U . . .
C12 C 0.5335(5) 0.1541(4) 0.0998(2) 0.0214(7) Uani 1 1 d . . . . .
H12A H 0.464209 0.059605 0.064997 0.026 Uiso 1 1 calc R U . . .
H12B H 0.505277 0.170207 0.159268 0.026 Uiso 1 1 calc R U . . .
C14 C 0.2795(5) 0.2652(4) 0.0811(2) 0.0212(7) Uani 1 1 d . . . . .
H14A H 0.265108 0.285133 0.142294 0.025 Uiso 1 1 calc R U . . .
H14B H 0.190724 0.176513 0.048849 0.025 Uiso 1 1 calc R U . . .
C15 C 0.2317(5) 0.3810(4) 0.0513(2) 0.0200(7) Uani 1 1 d . . . . .
H15A H 0.257931 0.365569 -0.008428 0.024 Uiso 1 1 calc R U . . .
H15B H 0.093644 0.383283 0.053855 0.024 Uiso 1 1 calc R U . . .
C17 C 0.2947(5) 0.6240(4) 0.0850(2) 0.0188(7) Uani 1 1 d . . . . .
H17A H 0.153884 0.616933 0.083779 0.023 Uiso 1 1 calc R U . . .
H17B H 0.329785 0.622989 0.028100 0.023 Uiso 1 1 calc R U . . .
C18 C 0.3970(5) 0.7563(4) 0.1505(2) 0.0173(7) Uani 1 1 d . . . . .
H18A H 0.537066 0.758770 0.155561 0.021 Uiso 1 1 calc R U . . .
H18B H 0.375303 0.835899 0.132429 0.021 Uiso 1 1 calc R U . . .
C20 C 0.4550(6) 0.7336(5) 0.2888(2) 0.0327(10) Uani 1 1 d . . . . .
H20A H 0.583029 0.796120 0.299307 0.039 Uiso 1 1 calc R U . . .
H20B H 0.471488 0.637188 0.262402 0.039 Uiso 1 1 calc R U . . .
O2 O -0.2447(4) 0.5303(3) 0.14501(17) 0.0217(5) Uani 1 1 d D . . . .
H2A H -0.363(3) 0.508(4) 0.131(3) 0.032(12) Uiso 1 1 d D . . . .
H2B H -0.228(5) 0.457(3) 0.153(3) 0.027(11) Uiso 1 1 d D . . . .
O4' O 0.6700(18) 0.6556(14) 0.3990(8) 0.014(3) Uani 0.2 1 d . . P A 2
H1A H -0.138(5) 0.669(4) 0.2386(17) 0.039(13) Uiso 1 1 d D . . . .
H1B H -0.078(8) 0.669(6) 0.316(3) 0.09(2) 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
Sn1 C1 2.141(3) . ?
Sn1 O1 2.215(3) . ?
Sn1 O19 2.363(2) . ?
Sn1 Br3 2.5313(4) . ?
Sn1 Br2 2.5408(4) . ?
Sn1 Br1 2.5824(4) . ?
O1 H1A 0.833(19) . ?
O1 H1B 0.824(19) . ?
O4 C3 1.417(5) . ?
O4 C5 1.426(4) . ?
O7 C6 1.422(4) . ?
O7 C8 1.430(4) . ?
O10 C9 1.433(4) . ?
O10 C11 1.434(4) . ?
O13 C14 1.422(4) . ?
O13 C12 1.427(4) . ?
O16 C15 1.420(4) . ?
O16 C17 1.429(4) . ?
O19 C20 1.433(4) . ?
O19 C18 1.437(4) . ?
C1 C2 1.495(5) . ?
C1 H1C 0.9900 . ?
C1 H1D 0.9900 . ?
C2 C20 1.463(5) . ?
C2 C3 1.512(5) . ?
C2 H2 1.0000 . ?
C3 O4' 1.467(13) . ?
C3 H3AA 0.9900 . ?
C3 H3AB 0.9900 . ?
C3 H3BC 0.9900 . ?
C3 H3BD 0.9900 . ?
C5 O4' 1.428(12) . ?
C5 C6 1.495(5) . ?
C5 H5AA 0.9900 . ?
C5 H5AB 0.9900 . ?
C5 H5BC 0.9900 . ?
C5 H5BD 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C8 C9 1.498(5) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C11 C12 1.504(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C14 C15 1.510(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C17 C18 1.492(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
O2 H2A 0.831(18) . ?
O2 H2B 0.838(18) . ?

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
C1 Sn1 O1 88.30(12) . . ?
C1 Sn1 O19 76.62(10) . . ?
O1 Sn1 O19 84.05(9) . . ?
C1 Sn1 Br3 158.13(9) . . ?
O1 Sn1 Br3 81.45(7) . . ?
O19 Sn1 Br3 83.11(5) . . ?
C1 Sn1 Br2 103.09(9) . . ?
O1 Sn1 Br2 91.09(7) . . ?
O19 Sn1 Br2 175.13(6) . . ?
Br3 Sn1 Br2 96.407(13) . . ?
C1 Sn1 Br1 96.46(10) . . ?
O1 Sn1 Br1 172.15(7) . . ?
O19 Sn1 Br1 90.96(6) . . ?
Br3 Sn1 Br1 91.952(14) . . ?
Br2 Sn1 Br1 93.902(14) . . ?
Sn1 O1 H1A 125(3) . . ?
Sn1 O1 H1B 125(4) . . ?
H1A O1 H1B 107(5) . . ?
C3 O4 C5 112.7(3) . . ?
C6 O7 C8 113.5(3) . . ?
C9 O10 C11 111.9(3) . . ?
C14 O13 C12 111.9(3) . . ?
C15 O16 C17 111.3(2) . . ?
C20 O19 C18 113.5(2) . . ?
C20 O19 Sn1 111.35(19) . . ?
C18 O19 Sn1 129.84(19) . . ?
C2 C1 Sn1 111.6(2) . . ?
C2 C1 H1C 109.3 . . ?
Sn1 C1 H1C 109.3 . . ?
C2 C1 H1D 109.3 . . ?
Sn1 C1 H1D 109.3 . . ?
H1C C1 H1D 108.0 . . ?
C20 C2 C1 115.8(3) . . ?
C20 C2 C3 112.2(3) . . ?
C1 C2 C3 112.8(3) . . ?
C20 C2 H2 104.9 . . ?
C1 C2 H2 104.9 . . ?
C3 C2 H2 104.9 . . ?
O4 C3 C2 109.0(3) . . ?
O4' C3 C2 114.5(5) . . ?
O4 C3 H3AA 109.9 . . ?
C2 C3 H3AA 109.9 . . ?
O4 C3 H3AB 109.9 . . ?
C2 C3 H3AB 109.9 . . ?
H3AA C3 H3AB 108.3 . . ?
O4' C3 H3BC 108.6 . . ?
C2 C3 H3BC 108.6 . . ?
O4' C3 H3BD 108.6 . . ?
C2 C3 H3BD 108.6 . . ?
H3BC C3 H3BD 107.6 . . ?
O4 C5 C6 107.5(3) . . ?
O4' C5 C6 111.5(6) . . ?
O4 C5 H5AA 110.2 . . ?
C6 C5 H5AA 110.2 . . ?
O4 C5 H5AB 110.2 . . ?
C6 C5 H5AB 110.2 . . ?
H5AA C5 H5AB 108.5 . . ?
O4' C5 H5BC 109.3 . . ?
C6 C5 H5BC 109.3 . . ?
O4' C5 H5BD 109.3 . . ?
C6 C5 H5BD 109.3 . . ?
H5BC C5 H5BD 108.0 . . ?
O7 C6 C5 109.8(3) . . ?
O7 C6 H6A 109.7 . . ?
C5 C6 H6A 109.7 . . ?
O7 C6 H6B 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?
O7 C8 C9 115.8(3) . . ?
O7 C8 H8A 108.3 . . ?
C9 C8 H8A 108.3 . . ?
O7 C8 H8B 108.3 . . ?
C9 C8 H8B 108.3 . . ?
H8A C8 H8B 107.4 . . ?
O10 C9 C8 110.2(3) . . ?
O10 C9 H9A 109.6 . . ?
C8 C9 H9A 109.6 . . ?
O10 C9 H9B 109.6 . . ?
C8 C9 H9B 109.6 . . ?
H9A C9 H9B 108.1 . . ?
O10 C11 C12 112.0(3) . . ?
O10 C11 H11A 109.2 . . ?
C12 C11 H11A 109.2 . . ?
O10 C11 H11B 109.2 . . ?
C12 C11 H11B 109.2 . . ?
H11A C11 H11B 107.9 . . ?
O13 C12 C11 107.9(3) . . ?
O13 C12 H12A 110.1 . . ?
C11 C12 H12A 110.1 . . ?
O13 C12 H12B 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O13 C14 C15 108.4(3) . . ?
O13 C14 H14A 110.0 . . ?
C15 C14 H14A 110.0 . . ?
O13 C14 H14B 110.0 . . ?
C15 C14 H14B 110.0 . . ?
H14A C14 H14B 108.4 . . ?
O16 C15 C14 108.6(3) . . ?
O16 C15 H15A 110.0 . . ?
C14 C15 H15A 110.0 . . ?
O16 C15 H15B 110.0 . . ?
C14 C15 H15B 110.0 . . ?
H15A C15 H15B 108.3 . . ?
O16 C17 C18 109.7(3) . . ?
O16 C17 H17A 109.7 . . ?
C18 C17 H17A 109.7 . . ?
O16 C17 H17B 109.7 . . ?
C18 C17 H17B 109.7 . . ?
H17A C17 H17B 108.2 . . ?
O19 C18 C17 110.8(3) . . ?
O19 C18 H18A 109.5 . . ?
C17 C18 H18A 109.5 . . ?
O19 C18 H18B 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 108.1 . . ?
O19 C20 C2 111.1(3) . . ?
O19 C20 H20A 109.4 . . ?
C2 C20 H20A 109.4 . . ?
O19 C20 H20B 109.4 . . ?
C2 C20 H20B 109.4 . . ?
H20A C20 H20B 108.0 . . ?
H2A O2 H2B 99(4) . . ?
C5 O4' C3 109.6(8) . . ?

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 C20 38.3(5) . . . . ?
Sn1 C1 C2 C3 169.5(3) . . . . ?
C5 O4 C3 C2 173.4(3) . . . . ?
C20 C2 C3 O4 -52.3(5) . . . . ?
C1 C2 C3 O4 174.7(3) . . . . ?
C20 C2 C3 O4' -19.3(8) . . . . ?
C1 C2 C3 O4' -152.3(7) . . . . ?
C3 O4 C5 C6 -172.2(3) . . . . ?
C8 O7 C6 C5 169.6(3) . . . . ?
O4 C5 C6 O7 76.1(4) . . . . ?
O4' C5 C6 O7 42.9(7) . . . . ?
C6 O7 C8 C9 73.4(4) . . . . ?
C11 O10 C9 C8 178.4(3) . . . . ?
O7 C8 C9 O10 74.9(4) . . . . ?
C9 O10 C11 C12 89.2(3) . . . . ?
C14 O13 C12 C11 -170.7(3) . . . . ?
O10 C11 C12 O13 74.5(3) . . . . ?
C12 O13 C14 C15 175.8(3) . . . . ?
C17 O16 C15 C14 -174.3(3) . . . . ?
O13 C14 C15 O16 -66.0(3) . . . . ?
C15 O16 C17 C18 171.5(3) . . . . ?
C20 O19 C18 C17 100.7(3) . . . . ?
Sn1 O19 C18 C17 -107.7(3) . . . . ?
O16 C17 C18 O19 -67.0(3) . . . . ?
C18 O19 C20 C2 -179.2(3) . . . . ?
Sn1 O19 C20 C2 23.9(4) . . . . ?
C1 C2 C20 O19 -41.6(5) . . . . ?
C3 C2 C20 O19 -173.1(3) . . . . ?
C6 C5 O4' C3 151.1(6) . . . . ?
C2 C3 O4' C5 -150.8(6) . . . . ?

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
O2 H2B O10 0.838(18) 1.98(2) 2.809(3) 169(4) 1_455 yes
O2 H2A O16 0.831(18) 2.09(2) 2.896(3) 165(4) 1_455 yes
O1 H1B O7 0.824(19) 2.02(3) 2.792(4) 155(6) 1_455 yes
O1 H1A O2 0.833(19) 1.78(2) 2.593(4) 165(5) . yes
O1 H1B O4'^b 0.824(19) 2.33(5) 2.831(13) 119(5) 1_455 yes

_refine_diff_density_max         1.461
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.130

####################################################################### 
# 
# 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_comp7
_database_code_depnum_ccdc_archive 'CCDC 780588'
_audit_update_record             
;
2017-07-27 deposited with the CCDC.
2018-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
Trichloro-(1,4,7,10,13,16-hexaoxa-cyclononadec-18-ylmethyl)-stannane
;
_chemical_name_common            ?
_chemical_melting_point          401
_chemical_formula_moiety         'C14 H29 Cl3 O7 Sn, H2 O'
_chemical_formula_sum            'C14 H31 Cl3 O8 Sn'
_chemical_formula_weight         552.43

# start Validation Reply Form
_vrf_GOODF01_comp7               
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: Due to weak reflection data  the least squares goodness 
of fit parameter lies outside the range 0.60 <> 4.00.
;
_vrf_PLAT026_comp7               
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         34 %     
RESPONSE: The low ratio is caused by weak data 
beyond sin(theta)/lambda > 0.5.
;
# end Validation Reply Form

_ccdc_journal_depnumber          CCDC-780588

_ccdc_chemdiag_type              ChemDraw
_ccdc_chemdiag_records           comp7.cdx

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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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                   7.1523(15)
_cell_length_b                   10.2096(18)
_cell_length_c                   16.569(4)
_cell_angle_alpha                72.642(11)
_cell_angle_beta                 80.828(6)
_cell_angle_gamma                79.071(12)
_cell_volume                     1127.0(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    11713
_cell_measurement_theta_min      2.59
_cell_measurement_theta_max      25.86

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.628
_exptl_crystal_F_000             560
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    1.523
_shelx_estimated_absorpt_T_min   0.750
_shelx_estimated_absorpt_T_max   0.771
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.887
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
R.H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_number            3980
_diffrn_reflns_av_unetI/netI     0.3609
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.592
_diffrn_reflns_theta_max         25.058
_diffrn_reflns_theta_full        25.058
_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             3980
_reflns_number_gt                1341
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_reduction        
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-III (1.0.3) (Farrugia, 2012)'
_computing_publication_material  'enCIFer Version 1.5.2'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²] 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       0.0046(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3980
_refine_ls_number_parameters     248
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.1553
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0729
_refine_ls_wR_factor_gt          0.0542
_refine_ls_goodness_of_fit_ref   0.420
_refine_ls_restrained_S_all      0.423
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.12895(6) 0.39135(5) 0.19141(3) 0.0525(2) Uani 1 1 d . . . . .
Cl1 Cl -0.0908(2) 0.33769(16) 0.11626(10) 0.0699(5) Uani 1 1 d . . . . .
Cl2 Cl 0.3580(2) 0.18459(17) 0.18976(11) 0.0786(6) Uani 1 1 d . . . . .
Cl3 Cl -0.0077(2) 0.28423(16) 0.32996(10) 0.0670(5) Uani 1 1 d . . . . .
O1W O 0.7522(7) 0.6225(5) 0.3551(3) 0.0752(13) Uani 1 1 d D . . . .
H1WA H 0.783(8) 0.704(3) 0.340(4) 0.090 Uiso 1 1 d D U . . .
H1WB H 0.634(3) 0.621(6) 0.370(4) 0.090 Uiso 1 1 d D U . . .
O2W O -0.0799(7) 0.5716(5) 0.2131(3) 0.0665(13) Uani 1 1 d D . . . .
H2WA H -0.100(8) 0.554(6) 0.2671(13) 0.080 Uiso 1 1 d D U . . .
H2WB H -0.130(8) 0.653(3) 0.197(4) 0.080 Uiso 1 1 d D U . . .
O1 O 0.3264(5) 0.4625(4) 0.2670(2) 0.0537(11) Uani 1 1 d . . . . .
O2 O 0.3444(6) 0.6005(5) 0.3963(3) 0.0708(13) Uani 1 1 d . . . . .
O3 O 0.4657(7) 0.8260(4) 0.4298(3) 0.0744(13) Uani 1 1 d . . . . .
O4 O 0.8387(6) 0.8892(4) 0.3326(3) 0.0796(14) Uani 1 1 d . . . . .
O5 O 0.9040(6) 0.8597(4) 0.1528(3) 0.0757(13) Uani 1 1 d . . . . .
O6 O 0.5854(7) 0.7877(5) 0.0979(3) 0.1041(17) Uani 1 1 d . U . . .
C21 C 0.2809(8) 0.5325(6) 0.0946(3) 0.0618(18) Uani 1 1 d . . . . .
H21A H 0.3758 0.4800 0.0610 0.074 Uiso 1 1 calc R U . . .
H21B H 0.1899 0.5960 0.0559 0.074 Uiso 1 1 calc R U . . .
C22 C 0.3827(10) 0.6169(7) 0.1283(4) 0.083(2) Uani 1 1 d . . . . .
H22A H 0.2750 0.6892 0.1402 0.099 Uiso 1 1 calc R U . . .
C23 C 0.4461(9) 0.5565(7) 0.2102(4) 0.073(2) Uani 1 1 d . . . . .
H23A H 0.4513 0.6316 0.2359 0.088 Uiso 1 1 calc R U . . .
H23B H 0.5777 0.5060 0.2038 0.088 Uiso 1 1 calc R U . . .
C24 C 0.3927(8) 0.3964(6) 0.3491(4) 0.0608(18) Uani 1 1 d . . . . .
H24A H 0.5318 0.3984 0.3450 0.073 Uiso 1 1 calc R U . . .
H24B H 0.3726 0.2981 0.3674 0.073 Uiso 1 1 calc R U . . .
C25 C 0.2903(9) 0.4666(7) 0.4134(4) 0.071(2) Uani 1 1 d . . . . .
H25A H 0.1503 0.4761 0.4123 0.086 Uiso 1 1 calc R U . . .
H25B H 0.3215 0.4099 0.4708 0.086 Uiso 1 1 calc R U . . .
C26 C 0.2333(9) 0.6799(8) 0.4495(5) 0.085(2) Uani 1 1 d . . . . .
H26A H 0.2644 0.6383 0.5088 0.103 Uiso 1 1 calc R U . . .
H26B H 0.0953 0.6793 0.4487 0.103 Uiso 1 1 calc R U . . .
C27 C 0.2739(10) 0.8243(8) 0.4192(5) 0.088(2) Uani 1 1 d . . . . .
H27A H 0.2536 0.8634 0.3584 0.105 Uiso 1 1 calc R U . . .
H27B H 0.1857 0.8820 0.4520 0.105 Uiso 1 1 calc R U . . .
C28 C 0.5192(10) 0.9586(8) 0.3958(4) 0.085(2) Uani 1 1 d . . . . .
H28A H 0.4487 1.0214 0.4296 0.102 Uiso 1 1 calc R U . . .
H28B H 0.4871 0.9977 0.3365 0.102 Uiso 1 1 calc R U . . .
C29 C 0.7299(11) 0.9471(7) 0.3977(4) 0.086(2) Uani 1 1 d . . . . .
H29A H 0.7626 1.0404 0.3899 0.103 Uiso 1 1 calc R U . . .
H29B H 0.7650 0.8878 0.4540 0.103 Uiso 1 1 calc R U . . .
C30 C 0.8835(10) 0.9930(7) 0.2558(5) 0.084(2) Uani 1 1 d . . . . .
H30A H 0.9528 1.0590 0.2680 0.101 Uiso 1 1 calc R U . . .
H30B H 0.7637 1.0455 0.2324 0.101 Uiso 1 1 calc R U . . .
C31 C 1.0035(9) 0.9276(7) 0.1929(4) 0.085(2) Uani 1 1 d . . . . .
H31A H 1.0651 0.9999 0.1483 0.102 Uiso 1 1 calc R U . . .
H31B H 1.1066 0.8588 0.2217 0.102 Uiso 1 1 calc R U . . .
C32 C 0.7884(10) 0.9485(7) 0.0912(4) 0.078(2) Uani 1 1 d . . . . .
H32A H 0.8622 1.0189 0.0515 0.093 Uiso 1 1 calc R U . . .
H32B H 0.6760 0.9974 0.1193 0.093 Uiso 1 1 calc R U . . .
C33 C 0.7226(9) 0.8664(7) 0.0430(4) 0.075(2) Uani 1 1 d . . . . .
H33A H 0.6645 0.9294 -0.0077 0.090 Uiso 1 1 calc R U . . .
H33B H 0.8326 0.8037 0.0238 0.090 Uiso 1 1 calc R U . . .
C34 C 0.5120(9) 0.7044(6) 0.0637(4) 0.0625(18) Uani 1 1 d . . . . .
H34A H 0.6184 0.6436 0.0407 0.075 Uiso 1 1 calc R U . . .
H34B H 0.4396 0.7628 0.0160 0.075 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C21 2.119(5) . ?
Sn1 O2W 2.220(4) . ?
Sn1 O1 2.363(3) . ?
Sn1 Cl3 2.3694(17) . ?
Sn1 Cl1 2.3828(14) . ?
Sn1 Cl2 2.4186(17) . ?
O1W H1WA 0.859(19) . ?
O1W H1WB 0.844(19) . ?
O2W H2WA 0.852(19) . ?
O2W H2WB 0.817(19) . ?
O1 C23 1.433(6) . ?
O1 C24 1.439(6) . ?
O2 C26 1.423(7) . ?
O2 C25 1.425(6) . ?
O3 C28 1.403(7) . ?
O3 C27 1.414(7) . ?
O4 C30 1.428(7) . ?
O4 C29 1.435(7) . ?
O5 C32 1.407(6) . ?
O5 C31 1.429(6) . ?
O6 C34 1.370(6) . ?
O6 C33 1.419(6) . ?
C21 C22 1.496(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.420(7) . ?
C22 C34 1.492(7) . ?
C22 H22A 1.0000 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.481(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.477(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.494(8) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.478(8) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.493(7) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 Sn1 O2W 88.2(2) . . ?
C21 Sn1 O1 76.63(17) . . ?
O2W Sn1 O1 84.39(16) . . ?
C21 Sn1 Cl3 157.99(15) . . ?
O2W Sn1 Cl3 81.47(13) . . ?
O1 Sn1 Cl3 83.01(11) . . ?
C21 Sn1 Cl1 102.95(15) . . ?
O2W Sn1 Cl1 90.40(14) . . ?
O1 Sn1 Cl1 174.78(11) . . ?
Cl3 Sn1 Cl1 96.57(6) . . ?
C21 Sn1 Cl2 97.08(17) . . ?
O2W Sn1 Cl2 171.74(13) . . ?
O1 Sn1 Cl2 90.68(10) . . ?
Cl3 Sn1 Cl2 91.37(6) . . ?
Cl1 Sn1 Cl2 94.53(6) . . ?
H1WA O1W H1WB 113(6) . . ?
Sn1 O2W H2WA 104(4) . . ?
Sn1 O2W H2WB 151(5) . . ?
H2WA O2W H2WB 103(6) . . ?
C23 O1 C24 114.4(4) . . ?
C23 O1 Sn1 111.1(3) . . ?
C24 O1 Sn1 130.6(3) . . ?
C26 O2 C25 112.8(5) . . ?
C28 O3 C27 112.5(5) . . ?
C30 O4 C29 112.5(5) . . ?
C32 O5 C31 115.3(5) . . ?
C34 O6 C33 115.6(5) . . ?
C22 C21 Sn1 113.3(4) . . ?
C22 C21 H21A 108.9 . . ?
Sn1 C21 H21A 108.9 . . ?
C22 C21 H21B 108.9 . . ?
Sn1 C21 H21B 108.9 . . ?
H21A C21 H21B 107.7 . . ?
C23 C22 C34 116.2(6) . . ?
C23 C22 C21 117.7(6) . . ?
C34 C22 C21 115.2(5) . . ?
C23 C22 H22A 101.1 . . ?
C34 C22 H22A 101.1 . . ?
C21 C22 H22A 101.1 . . ?
C22 C23 O1 113.7(5) . . ?
C22 C23 H23A 108.8 . . ?
O1 C23 H23A 108.8 . . ?
C22 C23 H23B 108.8 . . ?
O1 C23 H23B 108.8 . . ?
H23A C23 H23B 107.7 . . ?
O1 C24 C25 111.3(5) . . ?
O1 C24 H24A 109.4 . . ?
C25 C24 H24A 109.4 . . ?
O1 C24 H24B 109.4 . . ?
C25 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
O2 C25 C24 110.2(5) . . ?
O2 C25 H25A 109.6 . . ?
C24 C25 H25A 109.6 . . ?
O2 C25 H25B 109.6 . . ?
C24 C25 H25B 109.6 . . ?
H25A C25 H25B 108.1 . . ?
O2 C26 C27 109.9(6) . . ?
O2 C26 H26A 109.7 . . ?
C27 C26 H26A 109.7 . . ?
O2 C26 H26B 109.7 . . ?
C27 C26 H26B 109.7 . . ?
H26A C26 H26B 108.2 . . ?
O3 C27 C26 109.4(6) . . ?
O3 C27 H27A 109.8 . . ?
C26 C27 H27A 109.8 . . ?
O3 C27 H27B 109.8 . . ?
C26 C27 H27B 109.8 . . ?
H27A C27 H27B 108.2 . . ?
O3 C28 C29 108.8(6) . . ?
O3 C28 H28A 109.9 . . ?
C29 C28 H28A 109.9 . . ?
O3 C28 H28B 109.9 . . ?
C29 C28 H28B 109.9 . . ?
H28A C28 H28B 108.3 . . ?
O4 C29 C28 111.9(5) . . ?
O4 C29 H29A 109.2 . . ?
C28 C29 H29A 109.2 . . ?
O4 C29 H29B 109.2 . . ?
C28 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
O4 C30 C31 110.0(6) . . ?
O4 C30 H30A 109.7 . . ?
C31 C30 H30A 109.7 . . ?
O4 C30 H30B 109.7 . . ?
C31 C30 H30B 109.7 . . ?
H30A C30 H30B 108.2 . . ?
O5 C31 C30 115.2(5) . . ?
O5 C31 H31A 108.5 . . ?
C30 C31 H31A 108.5 . . ?
O5 C31 H31B 108.5 . . ?
C30 C31 H31B 108.5 . . ?
H31A C31 H31B 107.5 . . ?
O5 C32 C33 109.9(5) . . ?
O5 C32 H32A 109.7 . . ?
C33 C32 H32A 109.7 . . ?
O5 C32 H32B 109.7 . . ?
C33 C32 H32B 109.7 . . ?
H32A C32 H32B 108.2 . . ?
O6 C33 C32 108.0(5) . . ?
O6 C33 H33A 110.1 . . ?
C32 C33 H33A 110.1 . . ?
O6 C33 H33B 110.1 . . ?
C32 C33 H33B 110.1 . . ?
H33A C33 H33B 108.4 . . ?
O6 C34 C22 111.5(5) . . ?
O6 C34 H34A 109.3 . . ?
C22 C34 H34A 109.3 . . ?
O6 C34 H34B 109.3 . . ?
C22 C34 H34B 109.3 . . ?
H34A C34 H34B 108.0 . . ?

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 C21 C22 C23 29.4(8) . . . . ?
Sn1 C21 C22 C34 172.4(5) . . . . ?
C34 C22 C23 O1 -174.0(5) . . . . ?
C21 C22 C23 O1 -31.4(9) . . . . ?
C24 O1 C23 C22 177.7(6) . . . . ?
Sn1 O1 C23 C22 17.7(7) . . . . ?
C23 O1 C24 C25 99.0(6) . . . . ?
Sn1 O1 C24 C25 -105.8(5) . . . . ?
C26 O2 C25 C24 172.6(5) . . . . ?
O1 C24 C25 O2 -69.3(6) . . . . ?
C25 O2 C26 C27 -170.6(5) . . . . ?
C28 O3 C27 C26 175.0(6) . . . . ?
O2 C26 C27 O3 -66.1(7) . . . . ?
C27 O3 C28 C29 -171.5(5) . . . . ?
C30 O4 C29 C28 91.9(7) . . . . ?
O3 C28 C29 O4 75.2(7) . . . . ?
C29 O4 C30 C31 177.2(5) . . . . ?
C32 O5 C31 C30 74.4(8) . . . . ?
O4 C30 C31 O5 75.4(7) . . . . ?
C31 O5 C32 C33 169.4(5) . . . . ?
C34 O6 C33 C32 -179.1(6) . . . . ?
O5 C32 C33 O6 71.5(7) . . . . ?
C33 O6 C34 C22 174.9(5) . . . . ?
C23 C22 C34 O6 -42.1(9) . . . . ?
C21 C22 C34 O6 174.3(6) . . . . ?

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
O1W H1WA O4 0.859(19) 1.96(2) 2.809(6) 168(6) .
O1W H1WB O2 0.844(19) 2.09(2) 2.923(6) 172(6) .
O1W H1WB O3 0.844(19) 2.58(6) 3.027(6) 114(5) .
O2W H2WA O1W 0.852(19) 1.89(4) 2.615(7) 142(6) 1_455
O2W H2WB O5 0.817(19) 2.07(4) 2.795(6) 148(6) 1_455

_refine_diff_density_max         0.476
_refine_diff_density_min         -0.362
_refine_diff_density_rms         0.061

####################################################################### 
# 
# 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_comp3
_database_code_depnum_ccdc_archive 'CCDC 780589'
_audit_update_record             
;
2017-07-27 deposited with the CCDC.
2018-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
Dibromo-(1,4,7,10,13,16-hexaoxa-cyclononadec-18-ylmethyl)-phenylstannane
;
_chemical_name_common            ?
_chemical_melting_point          365
_chemical_formula_moiety         'C20 H32 Br2 O6 Sn'
_chemical_formula_sum            'C20 H32 Br2 O6 Sn'
_chemical_formula_weight         646.96

_ccdc_journal_depnumber          CCDC-780589

_ccdc_chemdiag_type              ChemDraw
_ccdc_chemdiag_records           comp3.cdx

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'
Br Br -0.2901 2.4595 '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           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                   9.4436(4)
_cell_length_b                   14.3024(7)
_cell_length_c                   18.0530(8)
_cell_angle_alpha                90
_cell_angle_beta                 98.649(2)
_cell_angle_gamma                90
_cell_volume                     2410.62(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9959
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      27.4

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.783
_exptl_crystal_F_000             1280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    4.406
_shelx_estimated_absorpt_T_min   0.308
_shelx_estimated_absorpt_T_max   0.693
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.526
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   
;
R.H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            36293
_diffrn_reflns_av_unetI/netI     0.0167
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.825
_diffrn_reflns_theta_max         26.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4989
_reflns_number_gt                4036
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_reduction        
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-III (1.0.3) (Farrugia, 2012)'
_computing_publication_material  'enCIFer Version 1.5.2'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0736P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4989
_refine_ls_number_parameters     250
_refine_ls_number_restraints     35
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1532
_refine_ls_wR_factor_gt          0.1461
_refine_ls_goodness_of_fit_ref   1.573
_refine_ls_restrained_S_all      1.627
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.40111(3) 0.01428(3) 0.30071(2) 0.04541(15) Uani 1 1 d . . . . .
Br1 Br 0.35094(7) 0.15065(5) 0.38579(3) 0.0736(2) Uani 1 1 d . . . . .
Br2 Br 0.30028(7) -0.11930(5) 0.37340(3) 0.0714(2) Uani 1 1 d . . . . .
C1 C 0.6226(5) -0.0052(3) 0.3403(3) 0.0431(10) Uani 1 1 d . . . . .
C2 C 0.6635(6) -0.0224(4) 0.4163(3) 0.0537(12) Uani 1 1 d . . . . .
H2A H 0.5931 -0.0242 0.4488 0.064 Uiso 1 1 calc R U . . .
C3 C 0.8068(6) -0.0369(4) 0.4451(3) 0.0655(15) Uani 1 1 d . . . . .
H3A H 0.8345 -0.0488 0.4970 0.079 Uiso 1 1 calc R U . . .
C4 C 0.9085(6) -0.0339(4) 0.3978(4) 0.0687(16) Uani 1 1 d . . . . .
H4A H 1.0063 -0.0446 0.4172 0.082 Uiso 1 1 calc R U . . .
C5 C 0.8689(6) -0.0155(4) 0.3223(4) 0.0624(15) Uani 1 1 d . . . . .
H5A H 0.9399 -0.0116 0.2903 0.075 Uiso 1 1 calc R U . . .
C6 C 0.7248(5) -0.0027(3) 0.2931(3) 0.0464(11) Uani 1 1 d . . . . .
H6A H 0.6972 0.0076 0.2409 0.056 Uiso 1 1 calc R U . . .
C21 C 0.2256(6) 0.0310(5) 0.2123(3) 0.0635(15) Uani 1 1 d . . . . .
H21A H 0.1536 -0.0188 0.2148 0.076 Uiso 1 1 calc R U . . .
H21B H 0.1790 0.0924 0.2164 0.076 Uiso 1 1 calc R U . . .
C22 C 0.2859(6) 0.0246(4) 0.1387(3) 0.0565(13) Uani 1 1 d . . . . .
H22A H 0.2035 0.0321 0.0973 0.068 Uiso 1 1 calc R U . . .
C23 C 0.3497(6) -0.0689(4) 0.1293(3) 0.0597(14) Uani 1 1 d . . . . .
H23A H 0.2731 -0.1166 0.1207 0.072 Uiso 1 1 calc R U . . .
H23B H 0.4008 -0.0683 0.0852 0.072 Uiso 1 1 calc R U . . .
O1 O 0.4486(4) -0.0918(2) 0.19597(18) 0.0512(8) Uani 1 1 d . . . . .
C24 C 0.4660(7) -0.1920(4) 0.2107(3) 0.0674(16) Uani 1 1 d . . . . .
H24A H 0.5365 -0.2003 0.2566 0.081 Uiso 1 1 calc R U . . .
H24B H 0.3734 -0.2172 0.2212 0.081 Uiso 1 1 calc R U . . .
C25 C 0.5121(8) -0.2478(5) 0.1515(4) 0.085(2) Uani 1 1 d D . . . .
H25A H 0.5167 -0.3141 0.1673 0.102 Uiso 1 1 calc R U . . .
H25B H 0.4392 -0.2427 0.1062 0.102 Uiso 1 1 calc R U . . .
O2 O 0.6417(5) -0.2227(3) 0.1333(2) 0.0742(12) Uani 1 1 d D . . . .
C26 C 0.6680(9) -0.2648(5) 0.0642(4) 0.0919(12) Uani 1 1 d D . . . .
H26A H 0.6704 -0.3338 0.0693 0.110 Uiso 1 1 calc R U . . .
H26B H 0.5902 -0.2481 0.0232 0.110 Uiso 1 1 calc R U . . .
C27 C 0.8007(10) -0.2321(5) 0.0473(4) 0.0919(12) Uani 1 1 d . . . . .
H27A H 0.8764 -0.2462 0.0900 0.110 Uiso 1 1 calc R U . . .
H27B H 0.8242 -0.2662 0.0030 0.110 Uiso 1 1 calc R U . . .
O3 O 0.8010(6) -0.1372(3) 0.0329(2) 0.0926(15) Uani 1 1 d D . . . .
C28 C 0.871(4) -0.0894(9) 0.0930(11) 0.0919(12) Uani 0.67 1 d D . P A 1
H28A H 0.9749 -0.0972 0.0927 0.110 Uiso 0.67 1 calc R U P A 1
H28B H 0.8484 -0.1205 0.1388 0.110 Uiso 0.67 1 calc R U P A 1
C29 C 0.8447(18) 0.0072(7) 0.1002(7) 0.0919(12) Uani 0.67 1 d D . P A 1
H29A H 0.7410 0.0154 0.1013 0.110 Uiso 0.67 1 calc R U P A 1
H29B H 0.8957 0.0278 0.1495 0.110 Uiso 0.67 1 calc R U P A 1
O4 O 0.8825(9) 0.0657(5) 0.0471(3) 0.0845(18) Uani 0.67 1 d D . P A 1
O4' O 0.9054(17) 0.0645(9) 0.1256(7) 0.0845(18) Uani 0.33 1 d D . P A 2
C28' C 0.861(8) -0.0828(16) 0.094(2) 0.0919(12) Uani 0.33 1 d D . P A 2
H28C H 0.9620 -0.0999 0.1104 0.110 Uiso 0.33 1 calc R U P A 2
H28D H 0.8064 -0.0894 0.1361 0.110 Uiso 0.33 1 calc R U P A 2
C29' C 0.849(3) 0.0080(15) 0.0641(12) 0.0919(12) Uani 0.33 1 d D . P A 2
H29C H 0.7480 0.0242 0.0457 0.110 Uiso 0.33 1 calc R U P A 2
H29D H 0.9056 0.0148 0.0224 0.110 Uiso 0.33 1 calc R U P A 2
C30 C 0.9139(11) 0.1625(6) 0.0791(6) 0.125(3) Uani 1 1 d . U . . .
H30A H 0.9635 0.1571 0.1313 0.150 Uiso 1 1 calc R U . A 1
H30B H 0.9790 0.1953 0.0496 0.150 Uiso 1 1 calc R U . A 1
C31 C 0.7920(7) 0.2143(5) 0.0784(4) 0.0811(19) Uani 1 1 d D . . . .
H31A H 0.7234 0.2015 0.0324 0.097 Uiso 1 1 calc R U . B 1
H31B H 0.8145 0.2819 0.0805 0.097 Uiso 1 1 calc R U . B 1
O5 O 0.7309(7) 0.1848(4) 0.1465(3) 0.0620(14) Uani 0.67 1 d D . P C 1
O5' O 0.6672(12) 0.1974(9) 0.1056(7) 0.0620(14) Uani 0.33 1 d D . P C 2
C32 C 0.6411(10) 0.2357(5) 0.1669(4) 0.0919(12) Uani 1 1 d . . . . .
H32A H 0.5788 0.2575 0.1212 0.110 Uiso 1 1 calc R U . C 1
H32B H 0.6924 0.2914 0.1898 0.110 Uiso 1 1 calc R U . C 1
C33 C 0.5506(6) 0.2057(4) 0.2166(3) 0.0610(14) Uani 1 1 d . . . . .
H33A H 0.4733 0.2525 0.2164 0.073 Uiso 1 1 calc R U . . .
H33B H 0.6060 0.2048 0.2677 0.073 Uiso 1 1 calc R U . . .
O6 O 0.4850(4) 0.1146(2) 0.20169(18) 0.0502(8) Uani 1 1 d . . . . .
C34 C 0.3872(6) 0.1070(4) 0.1333(3) 0.0562(13) Uani 1 1 d . . . . .
H34A H 0.4410 0.0972 0.0909 0.067 Uiso 1 1 calc R U . . .
H34B H 0.3313 0.1655 0.1241 0.067 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C1 2.125(5) . ?
Sn1 C21 2.135(5) . ?
Sn1 O6 2.511(3) . ?
Sn1 O1 2.516(3) . ?
Sn1 Br1 2.5703(7) . ?
Sn1 Br2 2.5797(7) . ?
C1 C6 1.381(7) . ?
C1 C2 1.391(7) . ?
C2 C3 1.390(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.377(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.384(9) . ?
C4 H4A 0.9500 . ?
C5 C6 1.395(7) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C21 C22 1.524(7) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.487(8) . ?
C22 C34 1.530(7) . ?
C22 H22A 1.0000 . ?
C23 O1 1.446(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
O1 C24 1.462(7) . ?
C24 C25 1.451(9) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 O2 1.362(7) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
O2 C26 1.441(6) . ?
C26 C27 1.413(10) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 O3 1.383(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
O3 C28 1.366(10) . ?
O3 C28' 1.391(14) . ?
C28 C29 1.412(14) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 O4 1.360(10) . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
O4 C30 1.512(11) . ?
O4' C29' 1.411(14) . ?
O4' C30 1.641(16) . ?
C28' C29' 1.40(2) . ?
C28' H28C 0.9900 . ?
C28' H28D 0.9900 . ?
C29' H29C 0.9900 . ?
C29' H29D 0.9900 . ?
C30 C31 1.367(11) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 O5' 1.364(10) . ?
C31 O5 1.494(7) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
O5 C32 1.217(9) . ?
O5' C32 1.292(14) . ?
C32 C33 1.395(9) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 O6 1.450(6) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O6 C34 1.431(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Sn1 C21 151.7(2) . . ?
C1 Sn1 O6 85.09(16) . . ?
C21 Sn1 O6 72.32(18) . . ?
C1 Sn1 O1 84.04(15) . . ?
C21 Sn1 O1 73.24(18) . . ?
O6 Sn1 O1 72.47(11) . . ?
C1 Sn1 Br1 99.14(12) . . ?
C21 Sn1 Br1 99.79(17) . . ?
O6 Sn1 Br1 95.62(8) . . ?
O1 Sn1 Br1 167.46(8) . . ?
C1 Sn1 Br2 98.74(14) . . ?
C21 Sn1 Br2 99.13(17) . . ?
O6 Sn1 Br2 164.86(8) . . ?
O1 Sn1 Br2 93.26(8) . . ?
Br1 Sn1 Br2 98.20(3) . . ?
C6 C1 C2 119.8(5) . . ?
C6 C1 Sn1 122.2(4) . . ?
C2 C1 Sn1 117.9(4) . . ?
C1 C2 C3 120.3(5) . . ?
C1 C2 H2A 119.8 . . ?
C3 C2 H2A 119.8 . . ?
C4 C3 C2 119.6(6) . . ?
C4 C3 H3A 120.2 . . ?
C2 C3 H3A 120.2 . . ?
C3 C4 C5 120.4(5) . . ?
C3 C4 H4A 119.8 . . ?
C5 C4 H4A 119.8 . . ?
C4 C5 C6 120.0(6) . . ?
C4 C5 H5A 120.0 . . ?
C6 C5 H5A 120.0 . . ?
C1 C6 C5 119.8(5) . . ?
C1 C6 H6A 120.1 . . ?
C5 C6 H6A 120.1 . . ?
C22 C21 Sn1 107.1(3) . . ?
C22 C21 H21A 110.3 . . ?
Sn1 C21 H21A 110.3 . . ?
C22 C21 H21B 110.3 . . ?
Sn1 C21 H21B 110.3 . . ?
H21A C21 H21B 108.5 . . ?
C23 C22 C21 111.4(5) . . ?
C23 C22 C34 114.6(5) . . ?
C21 C22 C34 109.2(5) . . ?
C23 C22 H22A 107.1 . . ?
C21 C22 H22A 107.1 . . ?
C34 C22 H22A 107.1 . . ?
O1 C23 C22 109.3(4) . . ?
O1 C23 H23A 109.8 . . ?
C22 C23 H23A 109.8 . . ?
O1 C23 H23B 109.8 . . ?
C22 C23 H23B 109.8 . . ?
H23A C23 H23B 108.3 . . ?
C23 O1 C24 114.5(4) . . ?
C23 O1 Sn1 108.8(3) . . ?
C24 O1 Sn1 118.8(3) . . ?
C25 C24 O1 116.3(5) . . ?
C25 C24 H24A 108.2 . . ?
O1 C24 H24A 108.2 . . ?
C25 C24 H24B 108.2 . . ?
O1 C24 H24B 108.2 . . ?
H24A C24 H24B 107.4 . . ?
O2 C25 C24 114.4(6) . . ?
O2 C25 H25A 108.7 . . ?
C24 C25 H25A 108.7 . . ?
O2 C25 H25B 108.7 . . ?
C24 C25 H25B 108.7 . . ?
H25A C25 H25B 107.6 . . ?
C25 O2 C26 112.1(5) . . ?
C27 C26 O2 108.8(6) . . ?
C27 C26 H26A 109.9 . . ?
O2 C26 H26A 109.9 . . ?
C27 C26 H26B 109.9 . . ?
O2 C26 H26B 109.9 . . ?
H26A C26 H26B 108.3 . . ?
O3 C27 C26 113.2(7) . . ?
O3 C27 H27A 108.9 . . ?
C26 C27 H27A 108.9 . . ?
O3 C27 H27B 108.9 . . ?
C26 C27 H27B 108.9 . . ?
H27A C27 H27B 107.8 . . ?
C28 O3 C27 110.9(8) . . ?
C27 O3 C28' 114.3(13) . . ?
O3 C28 C29 119.5(13) . . ?
O3 C28 H28A 107.4 . . ?
C29 C28 H28A 107.4 . . ?
O3 C28 H28B 107.4 . . ?
C29 C28 H28B 107.4 . . ?
H28A C28 H28B 107.0 . . ?
O4 C29 C28 117.9(19) . . ?
O4 C29 H29A 107.8 . . ?
C28 C29 H29A 107.8 . . ?
O4 C29 H29B 107.8 . . ?
C28 C29 H29B 107.8 . . ?
H29A C29 H29B 107.2 . . ?
C29 O4 C30 110.6(7) . . ?
C29' O4' C30 97.4(13) . . ?
O3 C28' C29' 102.7(17) . . ?
O3 C28' H28C 111.2 . . ?
C29' C28' H28C 111.2 . . ?
O3 C28' H28D 111.2 . . ?
C29' C28' H28D 111.2 . . ?
H28C C28' H28D 109.1 . . ?
C28' C29' O4' 103.5(17) . . ?
C28' C29' H29C 111.1 . . ?
O4' C29' H29C 111.1 . . ?
C28' C29' H29D 111.1 . . ?
O4' C29' H29D 111.1 . . ?
H29C C29' H29D 109.0 . . ?
C31 C30 O4 112.0(8) . . ?
C31 C30 O4' 111.2(8) . . ?
C31 C30 H30A 109.2 . . ?
O4 C30 H30A 109.2 . . ?
C31 C30 H30B 109.2 . . ?
O4 C30 H30B 109.2 . . ?
H30A C30 H30B 107.9 . . ?
O5' C31 C30 132.3(8) . . ?
C30 C31 O5 105.6(7) . . ?
C30 C31 H31A 110.6 . . ?
O5 C31 H31A 110.6 . . ?
C30 C31 H31B 110.6 . . ?
O5 C31 H31B 110.6 . . ?
H31A C31 H31B 108.8 . . ?
C32 O5 C31 117.0(6) . . ?
C32 O5' C31 121.3(11) . . ?
O5 C32 C33 122.2(7) . . ?
O5' C32 C33 129.4(8) . . ?
O5 C32 H32A 106.8 . . ?
C33 C32 H32A 106.8 . . ?
O5 C32 H32B 106.8 . . ?
C33 C32 H32B 106.8 . . ?
H32A C32 H32B 106.6 . . ?
C32 C33 O6 116.3(5) . . ?
C32 C33 H33A 108.2 . . ?
O6 C33 H33A 108.2 . . ?
C32 C33 H33B 108.2 . . ?
O6 C33 H33B 108.2 . . ?
H33A C33 H33B 107.4 . . ?
C34 O6 C33 115.5(4) . . ?
C34 O6 Sn1 109.9(3) . . ?
C33 O6 Sn1 123.6(3) . . ?
O6 C34 C22 109.3(4) . . ?
O6 C34 H34A 109.8 . . ?
C22 C34 H34A 109.8 . . ?
O6 C34 H34B 109.8 . . ?
C22 C34 H34B 109.8 . . ?
H34A C34 H34B 108.3 . . ?

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(8) . . . . ?
Sn1 C1 C2 C3 179.1(4) . . . . ?
C1 C2 C3 C4 0.2(9) . . . . ?
C2 C3 C4 C5 0.8(9) . . . . ?
C3 C4 C5 C6 -2.0(9) . . . . ?
C2 C1 C6 C5 -1.4(7) . . . . ?
Sn1 C1 C6 C5 179.7(4) . . . . ?
C4 C5 C6 C1 2.3(8) . . . . ?
Sn1 C21 C22 C23 63.0(5) . . . . ?
Sn1 C21 C22 C34 -64.7(5) . . . . ?
C21 C22 C23 O1 -51.0(6) . . . . ?
C34 C22 C23 O1 73.6(5) . . . . ?
C22 C23 O1 C24 152.2(4) . . . . ?
C22 C23 O1 Sn1 16.6(5) . . . . ?
C23 O1 C24 C25 57.0(7) . . . . ?
Sn1 O1 C24 C25 -172.0(5) . . . . ?
O1 C24 C25 O2 60.3(8) . . . . ?
C24 C25 O2 C26 -166.9(6) . . . . ?
C25 O2 C26 C27 177.2(6) . . . . ?
O2 C26 C27 O3 -64.9(8) . . . . ?
C26 C27 O3 C28 103(2) . . . . ?
C26 C27 O3 C28' 98(4) . . . . ?
C27 O3 C28 C29 -160(2) . . . . ?
O3 C28 C29 O4 -64(4) . . . . ?
C28 C29 O4 C30 -153.3(16) . . . . ?
C27 O3 C28' C29' 179(3) . . . . ?
O3 C28' C29' O4' 178(4) . . . . ?
C30 O4' C29' C28' 169(4) . . . . ?
C29 O4 C30 C31 -83.2(12) . . . . ?
C29' O4' C30 C31 92.4(17) . . . . ?
O4' C30 C31 O5' -3.2(17) . . . . ?
O4 C30 C31 O5 82.1(9) . . . . ?
C30 C31 O5 C32 163.7(8) . . . . ?
C30 C31 O5' C32 102.9(15) . . . . ?
C31 O5 C32 C33 163.3(7) . . . . ?
C31 O5' C32 C33 -155.5(10) . . . . ?
O5 C32 C33 O6 -45.4(11) . . . . ?
O5' C32 C33 O6 6.0(14) . . . . ?
C32 C33 O6 C34 -64.9(7) . . . . ?
C32 C33 O6 Sn1 154.9(5) . . . . ?
C33 O6 C34 C22 -158.2(4) . . . . ?
Sn1 O6 C34 C22 -12.8(5) . . . . ?
C23 C22 C34 O6 -77.1(5) . . . . ?
C21 C22 C34 O6 48.6(6) . . . . ?

_refine_diff_density_max         1.360
_refine_diff_density_min         -0.948
_refine_diff_density_rms         0.109

####################################################################### 
# 
# 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_comp4x(Ph3P)2NCl
_database_code_depnum_ccdc_archive 'CCDC 780583'
_audit_update_record             
;
2017-07-27 deposited with the CCDC.
2018-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;Dichloro-(1,4,7,10,13,16-hexaoxa-cyclononadec-18-ylmethyl)-phenylstannane 
bis(triphenylphosphine)iminium chloride complex
;
_chemical_name_common            ?
_chemical_melting_point          422-432
_chemical_formula_moiety         
;C36 H30 N P2, C20 H32 Cl3 O6 Sn, 0.5(C H2 Cl2)
;
_chemical_formula_sum            'C56.50 H63 Cl4 N O6 P2 Sn'
_chemical_formula_weight         1174.51

# start Validation Reply Form
_vrf_PLAT026_comp4x(Ph3P)2NCl    
;
PROBLEM: Ratio Observed / Unique Reflections (too) Low ..         32 %     
RESPONSE: The low ratio is caused by weak data 
beyond sin(theta)/lambda > 0.5.
;
# end Validation Reply Form

_ccdc_journal_depnumber          CCDC-780583

_ccdc_chemdiag_type              ChemDraw
_ccdc_chemdiag_records           comp4.cdx

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   10.8696(8)
_cell_length_b                   32.808(3)
_cell_length_c                   16.1991(13)
_cell_angle_alpha                90
_cell_angle_beta                 95.866(4)
_cell_angle_gamma                90
_cell_volume                     5746.5(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    43956
_cell_measurement_theta_min      2.82
_cell_measurement_theta_max      25.03

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_F_000             2420
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_exptl_absorpt_coefficient_mu    0.734
_shelx_estimated_absorpt_T_min   0.930
_shelx_estimated_absorpt_T_max   0.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.867
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
R.H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            9996
_diffrn_reflns_av_unetI/netI     0.4112
_diffrn_reflns_av_R_equivalents  0.075
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.603
_diffrn_reflns_theta_max         25.033
_diffrn_reflns_theta_full        25.033
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.985
_reflns_number_total             9996
_reflns_number_gt                3198
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_reduction        
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-III (1.0.3) (Farrugia, 2012)'
_computing_publication_material  'enCIFer Version 1.5.2'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0825P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9996
_refine_ls_number_parameters     397
_refine_ls_number_restraints     96
_refine_ls_R_factor_all          0.1794
_refine_ls_R_factor_gt           0.0545
_refine_ls_wR_factor_ref         0.1971
_refine_ls_wR_factor_gt          0.1434
_refine_ls_goodness_of_fit_ref   0.831
_refine_ls_restrained_S_all      0.830
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn -0.06555(7) 0.13607(2) 0.74864(4) 0.0336(2) Uani 1 1 d . . . . .
Cl1 Cl -0.2819(2) 0.11736(7) 0.70561(16) 0.0403(7) Uani 1 1 d . . . . .
Cl2 Cl -0.0523(2) 0.18163(7) 0.62127(16) 0.0407(7) Uani 1 1 d . . . . .
Cl3 Cl -0.0491(2) 0.09227(7) 0.88232(15) 0.0357(7) Uani 1 1 d . . . . .
P1 P 0.6874(2) 0.39440(7) 0.71565(16) 0.0316(7) Uani 1 1 d . . . . .
P2 P 0.4422(2) 0.37956(7) 0.62566(16) 0.0301(7) Uani 1 1 d . . . . .
N1 N 0.5442(6) 0.3831(2) 0.7060(4) 0.027(2) Uani 1 1 d . . . . .
O1 O 0.1465(6) 0.16077(18) 0.8027(4) 0.0355(18) Uani 1 1 d . . . . .
O2 O 0.4068(6) 0.1875(2) 0.8333(4) 0.0393(19) Uani 1 1 d . . . . .
O3 O 0.6278(6) 0.22886(19) 0.9218(4) 0.046(2) Uani 1 1 d . . . . .
O4 O 0.5242(6) 0.30585(19) 0.9893(4) 0.0436(19) Uani 1 1 d . . . . .
O5 O 0.2662(7) 0.32815(19) 0.9775(5) 0.056(2) Uani 1 1 d . . . . .
O6 O 0.0917(6) 0.28097(19) 0.8739(4) 0.0424(19) Uani 1 1 d . . . . .
C21 C -0.0966(9) 0.1898(3) 0.8205(6) 0.043(3) Uani 1 1 d . . . . .
H21A H -0.1700 0.2045 0.7945 0.052 Uiso 1 1 calc R U . . .
H21B H -0.1132 0.1816 0.8771 0.052 Uiso 1 1 calc R U . . .
C22 C 0.0154(9) 0.2178(3) 0.8256(7) 0.041(3) Uani 1 1 d . . . . .
H22A H 0.0274 0.2274 0.7684 0.049 Uiso 1 1 calc R U . . .
C23 C 0.1296(9) 0.1944(3) 0.8599(6) 0.041(3) Uani 1 1 d . . . . .
H23A H 0.2029 0.2125 0.8643 0.049 Uiso 1 1 calc R U . . .
H23B H 0.1187 0.1837 0.9158 0.049 Uiso 1 1 calc R U . . .
C24 C 0.2551(9) 0.1363(3) 0.8222(6) 0.036(3) Uani 1 1 d . . . . .
H24A H 0.2391 0.1085 0.8004 0.043 Uiso 1 1 calc R U . . .
H24B H 0.2728 0.1344 0.8833 0.043 Uiso 1 1 calc R U . . .
C25 C 0.3638(9) 0.1530(3) 0.7874(6) 0.040(3) Uani 1 1 d . . . . .
H25A H 0.4298 0.1322 0.7894 0.048 Uiso 1 1 calc R U . . .
H25B H 0.3416 0.1607 0.7286 0.048 Uiso 1 1 calc R U . . .
C26 C 0.5029(10) 0.2069(3) 0.7995(6) 0.048(3) Uani 1 1 d . . . . .
H26A H 0.4738 0.2157 0.7424 0.057 Uiso 1 1 calc R U . . .
H26B H 0.5708 0.1870 0.7957 0.057 Uiso 1 1 calc R U . . .
C27 C 0.5547(10) 0.2442(3) 0.8492(6) 0.046(3) Uani 1 1 d . . . . .
H27A H 0.6065 0.2609 0.8154 0.055 Uiso 1 1 calc R U . . .
H27B H 0.4863 0.2614 0.8655 0.055 Uiso 1 1 calc R U . . .
C28 C 0.6938(9) 0.2609(3) 0.9673(6) 0.040(3) Uani 1 1 d . U . . .
H28A H 0.7181 0.2817 0.9277 0.048 Uiso 1 1 calc R U . . .
H28B H 0.7705 0.2495 0.9967 0.048 Uiso 1 1 calc R U . . .
C29 C 0.6212(10) 0.2810(3) 1.0287(6) 0.051(3) Uani 1 1 d . U . . .
H29A H 0.5851 0.2600 1.0627 0.061 Uiso 1 1 calc R U . . .
H29B H 0.6771 0.2982 1.0663 0.061 Uiso 1 1 calc R U . . .
C30 C 0.4662(10) 0.3297(3) 1.0458(7) 0.058(3) Uani 1 1 d . U . . .
H30A H 0.5274 0.3478 1.0768 0.070 Uiso 1 1 calc R U . . .
H30B H 0.4292 0.3119 1.0861 0.070 Uiso 1 1 calc R U . . .
C31 C 0.3700(10) 0.3540(3) 0.9994(7) 0.060(4) Uani 1 1 d . U . . .
H31A H 0.3458 0.3770 1.0338 0.073 Uiso 1 1 calc R U . . .
H31B H 0.4011 0.3652 0.9487 0.073 Uiso 1 1 calc R U . . .
C32 C 0.1790(10) 0.3461(3) 0.9173(7) 0.053(3) Uani 1 1 d . U . . .
H32A H 0.2139 0.3480 0.8633 0.064 Uiso 1 1 calc R U . . .
H32B H 0.1583 0.3740 0.9348 0.064 Uiso 1 1 calc R U . . .
C33 C 0.0620(10) 0.3194(3) 0.9087(7) 0.056(3) Uani 1 1 d . U . . .
H33A H 0.0322 0.3152 0.9638 0.067 Uiso 1 1 calc R U . . .
H33B H -0.0043 0.3330 0.8722 0.067 Uiso 1 1 calc R U . . .
C34 C -0.0112(10) 0.2541(3) 0.8771(7) 0.048(3) Uani 1 1 d . U . . .
H34A H -0.0888 0.2676 0.8542 0.057 Uiso 1 1 calc R U . . .
H34B H -0.0195 0.2458 0.9351 0.057 Uiso 1 1 calc R U . . .
C41 C 0.0193(9) 0.0874(3) 0.6847(6) 0.032(3) Uani 1 1 d . . . . .
C42 C -0.0276(9) 0.0482(3) 0.6898(6) 0.037(3) Uani 1 1 d . . . . .
H42A H -0.0899 0.0432 0.7257 0.045 Uiso 1 1 calc R U . . .
C43 C 0.0132(10) 0.0166(3) 0.6448(6) 0.038(3) Uani 1 1 d . . . . .
H43A H -0.0240 -0.0096 0.6464 0.045 Uiso 1 1 calc R U . . .
C44 C 0.1072(10) 0.0231(3) 0.5978(6) 0.039(3) Uani 1 1 d . . . . .
H44A H 0.1384 0.0013 0.5675 0.047 Uiso 1 1 calc R U . . .
C45 C 0.1582(10) 0.0618(3) 0.5940(6) 0.046(3) Uani 1 1 d . . . . .
H45A H 0.2248 0.0661 0.5613 0.055 Uiso 1 1 calc R U . . .
C46 C 0.1152(9) 0.0934(3) 0.6356(6) 0.037(3) Uani 1 1 d . . . . .
H46A H 0.1504 0.1197 0.6314 0.044 Uiso 1 1 calc R U . . .
C51 C 0.7860(5) 0.35422(15) 0.6828(4) 0.0385(12) Uani 1 1 d DG . . . .
C52 C 0.7409(4) 0.31456(18) 0.6819(4) 0.0385(12) Uani 1 1 d DG . . . .
H52A H 0.6588 0.3095 0.6946 0.046 Uiso 1 1 calc R U . . .
C53 C 0.8158(5) 0.28234(13) 0.6625(4) 0.0385(12) Uani 1 1 d DG . . . .
H53A H 0.7850 0.2552 0.6619 0.046 Uiso 1 1 calc R U . . .
C54 C 0.9359(5) 0.28977(15) 0.6440(4) 0.0385(12) Uani 1 1 d DG . . . .
H54A H 0.9871 0.2677 0.6308 0.046 Uiso 1 1 calc R U . . .
C55 C 0.9810(4) 0.32943(18) 0.6449(4) 0.0385(12) Uani 1 1 d DG . . . .
H55A H 1.0630 0.3345 0.6322 0.046 Uiso 1 1 calc R U . . .
C56 C 0.9060(5) 0.36166(13) 0.6643(4) 0.0385(12) Uani 1 1 d DG . . . .
H56A H 0.9368 0.3888 0.6648 0.046 Uiso 1 1 calc R U . . .
C61 C 0.7314(6) 0.44228(14) 0.6682(4) 0.0391(12) Uani 1 1 d DG . . . .
C62 C 0.7665(6) 0.44353(14) 0.5881(4) 0.0391(12) Uani 1 1 d DG . . . .
H62A H 0.7691 0.4191 0.5568 0.047 Uiso 1 1 calc R U . . .
C63 C 0.7979(6) 0.48048(18) 0.5539(3) 0.0391(12) Uani 1 1 d DG . . . .
H63A H 0.8219 0.4813 0.4992 0.047 Uiso 1 1 calc R U . . .
C64 C 0.7940(6) 0.51619(14) 0.5998(4) 0.0391(12) Uani 1 1 d DG . . . .
H64A H 0.8154 0.5414 0.5764 0.047 Uiso 1 1 calc R U . . .
C65 C 0.7589(6) 0.51494(14) 0.6799(4) 0.0391(12) Uani 1 1 d DG . . . .
H65A H 0.7562 0.5393 0.7112 0.047 Uiso 1 1 calc R U . . .
C66 C 0.7275(6) 0.47798(18) 0.7141(3) 0.0391(12) Uani 1 1 d DG . . . .
H66A H 0.7035 0.4771 0.7688 0.047 Uiso 1 1 calc R U . . .
C71 C 0.7356(7) 0.3984(2) 0.8235(3) 0.0660(16) Uani 1 1 d DG . . . .
C72 C 0.8539(6) 0.4123(2) 0.8501(4) 0.0660(16) Uani 1 1 d DG . . . .
H72A H 0.9079 0.4205 0.8107 0.079 Uiso 1 1 calc R U . . .
C73 C 0.8932(5) 0.4140(2) 0.9344(4) 0.0660(16) Uani 1 1 d DG . . . .
H73A H 0.9741 0.4234 0.9526 0.079 Uiso 1 1 calc R U . . .
C74 C 0.8143(7) 0.4019(2) 0.9921(3) 0.0660(16) Uani 1 1 d DG . . . .
H74A H 0.8412 0.4030 1.0497 0.079 Uiso 1 1 calc R U . . .
C75 C 0.6960(6) 0.3880(2) 0.9655(4) 0.0660(16) Uani 1 1 d DG . . . .
H75A H 0.6420 0.3797 1.0049 0.079 Uiso 1 1 calc R U . . .
C76 C 0.6567(5) 0.3863(2) 0.8812(5) 0.0660(16) Uani 1 1 d DG . . . .
H76A H 0.5758 0.3768 0.8630 0.079 Uiso 1 1 calc R U . . .
C81 C 0.3151(5) 0.41411(16) 0.6374(4) 0.0409(12) Uani 1 1 d DG . . . .
C82 C 0.2050(6) 0.41065(15) 0.5862(3) 0.0409(12) Uani 1 1 d DG . . . .
H82A H 0.1933 0.3886 0.5481 0.049 Uiso 1 1 calc R U . . .
C83 C 0.1119(4) 0.43940(18) 0.5906(3) 0.0409(12) Uani 1 1 d DG . . . .
H83A H 0.0367 0.4370 0.5555 0.049 Uiso 1 1 calc R U . . .
C84 C 0.1290(5) 0.47162(16) 0.6463(4) 0.0409(12) Uani 1 1 d DG . . . .
H84A H 0.0655 0.4913 0.6493 0.049 Uiso 1 1 calc R U . . .
C85 C 0.2391(6) 0.47508(15) 0.6976(3) 0.0409(12) Uani 1 1 d DG . . . .
H85A H 0.2508 0.4971 0.7357 0.049 Uiso 1 1 calc R U . . .
C86 C 0.3321(4) 0.44633(19) 0.6932(3) 0.0409(12) Uani 1 1 d DG . . . .
H86A H 0.4074 0.4487 0.7282 0.049 Uiso 1 1 calc R U . . .
C91 C 0.4962(5) 0.39182(18) 0.5260(3) 0.0338(11) Uani 1 1 d DG . . . .
C92 C 0.4723(5) 0.43042(16) 0.4928(4) 0.0338(11) Uani 1 1 d DG . . . .
H92A H 0.4171 0.4482 0.5171 0.041 Uiso 1 1 calc R U . . .
C93 C 0.5292(5) 0.44301(13) 0.4241(3) 0.0338(11) Uani 1 1 d DG . . . .
H93A H 0.5129 0.4694 0.4014 0.041 Uiso 1 1 calc R U . . .
C94 C 0.6100(5) 0.41702(18) 0.3886(3) 0.0338(11) Uani 1 1 d DG . . . .
H94A H 0.6489 0.4256 0.3417 0.041 Uiso 1 1 calc R U . . .
C95 C 0.6339(5) 0.37842(16) 0.4219(3) 0.0338(11) Uani 1 1 d DG . . . .
H95A H 0.6891 0.3606 0.3976 0.041 Uiso 1 1 calc R U . . .
C96 C 0.5770(5) 0.36582(14) 0.4906(3) 0.0338(11) Uani 1 1 d DG . . . .
H96A H 0.5934 0.3394 0.5133 0.041 Uiso 1 1 calc R U . . .
C101 C 0.3770(5) 0.32905(13) 0.6247(4) 0.0375(12) Uani 1 1 d DG . . . .
C102 C 0.3419(6) 0.31455(16) 0.6994(3) 0.0375(12) Uani 1 1 d DG . . . .
H10A H 0.3606 0.3299 0.7489 0.045 Uiso 1 1 calc R U . . .
C103 C 0.2796(5) 0.27764(17) 0.7018(3) 0.0375(12) Uani 1 1 d DG . . . .
H10B H 0.2557 0.2677 0.7529 0.045 Uiso 1 1 calc R U . . .
C104 C 0.2523(5) 0.25524(13) 0.6294(4) 0.0375(12) Uani 1 1 d DG . . . .
H10C H 0.2097 0.2300 0.6310 0.045 Uiso 1 1 calc R U . . .
C105 C 0.2873(5) 0.26975(16) 0.5546(3) 0.0375(12) Uani 1 1 d DG . . . .
H10D H 0.2687 0.2544 0.5052 0.045 Uiso 1 1 calc R U . . .
C106 C 0.3497(5) 0.30665(17) 0.5523(3) 0.0375(12) Uani 1 1 d DG . . . .
H10E H 0.3736 0.3166 0.5012 0.045 Uiso 1 1 calc R U . . .
C1L C 0.599(2) 0.0219(7) 0.5982(15) 0.083(8) Uani 0.5 1 d . U P . .
H1LA H 0.6675 0.0398 0.6214 0.099 Uiso 0.5 1 calc R U P . .
H2LB H 0.5704 0.0331 0.5429 0.099 Uiso 0.5 1 calc R U P . .
Cl1L Cl 0.6647(7) -0.0224(2) 0.5803(4) 0.099(3) Uani 0.5 1 d . U P . .
Cl2L Cl 0.4912(5) 0.02922(18) 0.6531(4) 0.0645(19) Uani 0.5 1 d . U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 C21 2.157(9) . ?
Sn1 C41 2.161(9) . ?
Sn1 Cl1 2.461(3) . ?
Sn1 O1 2.515(6) . ?
Sn1 Cl2 2.564(2) . ?
Sn1 Cl3 2.590(2) . ?
P1 N1 1.593(7) . ?
P1 C71 1.776(5) . ?
P1 C51 1.813(5) . ?
P1 C61 1.833(5) . ?
P2 N1 1.626(7) . ?
P2 C101 1.802(5) . ?
P2 C81 1.812(5) . ?
P2 C91 1.818(5) . ?
O1 C24 1.435(9) . ?
O1 C23 1.465(10) . ?
O2 C26 1.382(11) . ?
O2 C25 1.407(10) . ?
O3 C28 1.434(10) . ?
O3 C27 1.440(11) . ?
O4 C30 1.400(11) . ?
O4 C29 1.430(11) . ?
O5 C32 1.418(11) . ?
O5 C31 1.426(11) . ?
O6 C34 1.429(10) . ?
O6 C33 1.431(10) . ?
C21 C22 1.521(12) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C34 1.499(11) . ?
C22 C23 1.515(12) . ?
C22 H22A 1.0000 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.466(12) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.541(12) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.487(12) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.461(13) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.540(13) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C41 C46 1.389(12) . ?
C41 C42 1.389(11) . ?
C42 C43 1.368(12) . ?
C42 H42A 0.9500 . ?
C43 C44 1.352(12) . ?
C43 H43A 0.9500 . ?
C44 C45 1.390(12) . ?
C44 H44A 0.9500 . ?
C45 C46 1.346(12) . ?
C45 H45A 0.9500 . ?
C46 H46A 0.9500 . ?
C51 C52 1.3900 . ?
C51 C56 1.3900 . ?
C52 C53 1.3900 . ?
C52 H52A 0.9500 . ?
C53 C54 1.3900 . ?
C53 H53A 0.9500 . ?
C54 C55 1.3900 . ?
C54 H54A 0.9500 . ?
C55 C56 1.3900 . ?
C55 H55A 0.9500 . ?
C56 H56A 0.9500 . ?
C61 C62 1.3900 . ?
C61 C66 1.3900 . ?
C62 C63 1.3900 . ?
C62 H62A 0.9500 . ?
C63 C64 1.3900 . ?
C63 H63A 0.9500 . ?
C64 C65 1.3900 . ?
C64 H64A 0.9500 . ?
C65 C66 1.3900 . ?
C65 H65A 0.9500 . ?
C66 H66A 0.9500 . ?
C71 C72 1.3900 . ?
C71 C76 1.3900 . ?
C72 C73 1.3900 . ?
C72 H72A 0.9500 . ?
C73 C74 1.3900 . ?
C73 H73A 0.9500 . ?
C74 C75 1.3900 . ?
C74 H74A 0.9500 . ?
C75 C76 1.3900 . ?
C75 H75A 0.9500 . ?
C76 H76A 0.9500 . ?
C81 C82 1.3900 . ?
C81 C86 1.3900 . ?
C82 C83 1.3900 . ?
C82 H82A 0.9500 . ?
C83 C84 1.3900 . ?
C83 H83A 0.9500 . ?
C84 C85 1.3900 . ?
C84 H84A 0.9500 . ?
C85 C86 1.3900 . ?
C85 H85A 0.9500 . ?
C86 H86A 0.9500 . ?
C91 C92 1.3900 . ?
C91 C96 1.3900 . ?
C92 C93 1.3900 . ?
C92 H92A 0.9500 . ?
C93 C94 1.3900 . ?
C93 H93A 0.9500 . ?
C94 C95 1.3900 . ?
C94 H94A 0.9500 . ?
C95 C96 1.3900 . ?
C95 H95A 0.9500 . ?
C96 H96A 0.9500 . ?
C101 C102 1.3900 . ?
C101 C106 1.3900 . ?
C102 C103 1.3900 . ?
C102 H10A 0.9500 . ?
C103 C104 1.3900 . ?
C103 H10B 0.9500 . ?
C104 C105 1.3900 . ?
C104 H10C 0.9500 . ?
C105 C106 1.3900 . ?
C105 H10D 0.9500 . ?
C106 H10E 0.9500 . ?
C1L Cl2L 1.56(3) . ?
C1L Cl1L 1.66(2) . ?
C1L H1LA 0.9900 . ?
C1L H2LB 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C21 Sn1 C41 163.8(4) . . ?
C21 Sn1 Cl1 99.2(3) . . ?
C41 Sn1 Cl1 97.0(3) . . ?
C21 Sn1 O1 74.8(3) . . ?
C41 Sn1 O1 89.1(3) . . ?
Cl1 Sn1 O1 173.84(16) . . ?
C21 Sn1 Cl2 89.0(3) . . ?
C41 Sn1 Cl2 89.1(3) . . ?
Cl1 Sn1 Cl2 92.75(9) . . ?
O1 Sn1 Cl2 88.14(15) . . ?
C21 Sn1 Cl3 90.2(3) . . ?
C41 Sn1 Cl3 89.7(3) . . ?
Cl1 Sn1 Cl3 94.62(8) . . ?
O1 Sn1 Cl3 84.56(15) . . ?
Cl2 Sn1 Cl3 172.62(9) . . ?
N1 P1 C71 107.5(4) . . ?
N1 P1 C51 113.7(3) . . ?
C71 P1 C51 102.6(3) . . ?
N1 P1 C61 116.9(4) . . ?
C71 P1 C61 106.6(3) . . ?
C51 P1 C61 108.2(3) . . ?
N1 P2 C101 107.9(3) . . ?
N1 P2 C81 109.7(3) . . ?
C101 P2 C81 105.8(3) . . ?
N1 P2 C91 116.1(3) . . ?
C101 P2 C91 111.0(3) . . ?
C81 P2 C91 105.9(3) . . ?
P1 N1 P2 132.5(5) . . ?
C24 O1 C23 115.8(7) . . ?
C24 O1 Sn1 126.9(5) . . ?
C23 O1 Sn1 107.0(5) . . ?
C26 O2 C25 112.6(8) . . ?
C28 O3 C27 111.6(7) . . ?
C30 O4 C29 112.7(8) . . ?
C32 O5 C31 112.3(8) . . ?
C34 O6 C33 108.7(7) . . ?
C22 C21 Sn1 110.8(6) . . ?
C22 C21 H21A 109.5 . . ?
Sn1 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
Sn1 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
C34 C22 C23 113.3(8) . . ?
C34 C22 C21 108.2(8) . . ?
C23 C22 C21 109.5(8) . . ?
C34 C22 H22A 108.6 . . ?
C23 C22 H22A 108.6 . . ?
C21 C22 H22A 108.6 . . ?
O1 C23 C22 107.5(8) . . ?
O1 C23 H23A 110.2 . . ?
C22 C23 H23A 110.2 . . ?
O1 C23 H23B 110.2 . . ?
C22 C23 H23B 110.2 . . ?
H23A C23 H23B 108.5 . . ?
O1 C24 C25 112.6(8) . . ?
O1 C24 H24A 109.1 . . ?
C25 C24 H24A 109.1 . . ?
O1 C24 H24B 109.1 . . ?
C25 C24 H24B 109.1 . . ?
H24A C24 H24B 107.8 . . ?
O2 C25 C24 109.5(8) . . ?
O2 C25 H25A 109.8 . . ?
C24 C25 H25A 109.8 . . ?
O2 C25 H25B 109.8 . . ?
C24 C25 H25B 109.8 . . ?
H25A C25 H25B 108.2 . . ?
O2 C26 C27 114.1(9) . . ?
O2 C26 H26A 108.7 . . ?
C27 C26 H26A 108.7 . . ?
O2 C26 H26B 108.7 . . ?
C27 C26 H26B 108.7 . . ?
H26A C26 H26B 107.6 . . ?
O3 C27 C26 106.8(8) . . ?
O3 C27 H27A 110.4 . . ?
C26 C27 H27A 110.4 . . ?
O3 C27 H27B 110.4 . . ?
C26 C27 H27B 110.4 . . ?
H27A C27 H27B 108.6 . . ?
O3 C28 C29 113.5(8) . . ?
O3 C28 H28A 108.9 . . ?
C29 C28 H28A 108.9 . . ?
O3 C28 H28B 108.9 . . ?
C29 C28 H28B 108.9 . . ?
H28A C28 H28B 107.7 . . ?
O4 C29 C28 111.8(9) . . ?
O4 C29 H29A 109.2 . . ?
C28 C29 H29A 109.2 . . ?
O4 C29 H29B 109.2 . . ?
C28 C29 H29B 109.2 . . ?
H29A C29 H29B 107.9 . . ?
O4 C30 C31 108.3(9) . . ?
O4 C30 H30A 110.0 . . ?
C31 C30 H30A 110.0 . . ?
O4 C30 H30B 110.0 . . ?
C31 C30 H30B 110.0 . . ?
H30A C30 H30B 108.4 . . ?
O5 C31 C30 108.1(9) . . ?
O5 C31 H31A 110.1 . . ?
C30 C31 H31A 110.1 . . ?
O5 C31 H31B 110.1 . . ?
C30 C31 H31B 110.1 . . ?
H31A C31 H31B 108.4 . . ?
O5 C32 C33 108.2(9) . . ?
O5 C32 H32A 110.1 . . ?
C33 C32 H32A 110.1 . . ?
O5 C32 H32B 110.1 . . ?
C33 C32 H32B 110.1 . . ?
H32A C32 H32B 108.4 . . ?
O6 C33 C32 108.7(9) . . ?
O6 C33 H33A 110.0 . . ?
C32 C33 H33A 110.0 . . ?
O6 C33 H33B 110.0 . . ?
C32 C33 H33B 110.0 . . ?
H33A C33 H33B 108.3 . . ?
O6 C34 C22 105.9(8) . . ?
O6 C34 H34A 110.6 . . ?
C22 C34 H34A 110.6 . . ?
O6 C34 H34B 110.6 . . ?
C22 C34 H34B 110.6 . . ?
H34A C34 H34B 108.7 . . ?
C46 C41 C42 117.9(9) . . ?
C46 C41 Sn1 123.5(7) . . ?
C42 C41 Sn1 118.6(8) . . ?
C43 C42 C41 121.9(10) . . ?
C43 C42 H42A 119.0 . . ?
C41 C42 H42A 119.0 . . ?
C44 C43 C42 119.1(10) . . ?
C44 C43 H43A 120.5 . . ?
C42 C43 H43A 120.5 . . ?
C43 C44 C45 119.8(9) . . ?
C43 C44 H44A 120.1 . . ?
C45 C44 H44A 120.1 . . ?
C46 C45 C44 121.4(10) . . ?
C46 C45 H45A 119.3 . . ?
C44 C45 H45A 119.3 . . ?
C45 C46 C41 119.8(9) . . ?
C45 C46 H46A 120.1 . . ?
C41 C46 H46A 120.1 . . ?
C52 C51 C56 120.0 . . ?
C52 C51 P1 117.7(4) . . ?
C56 C51 P1 122.1(4) . . ?
C53 C52 C51 120.0 . . ?
C53 C52 H52A 120.0 . . ?
C51 C52 H52A 120.0 . . ?
C54 C53 C52 120.0 . . ?
C54 C53 H53A 120.0 . . ?
C52 C53 H53A 120.0 . . ?
C53 C54 C55 120.0 . . ?
C53 C54 H54A 120.0 . . ?
C55 C54 H54A 120.0 . . ?
C56 C55 C54 120.0 . . ?
C56 C55 H55A 120.0 . . ?
C54 C55 H55A 120.0 . . ?
C55 C56 C51 120.0 . . ?
C55 C56 H56A 120.0 . . ?
C51 C56 H56A 120.0 . . ?
C62 C61 C66 120.0 . . ?
C62 C61 P1 121.7(4) . . ?
C66 C61 P1 118.3(4) . . ?
C61 C62 C63 120.0 . . ?
C61 C62 H62A 120.0 . . ?
C63 C62 H62A 120.0 . . ?
C64 C63 C62 120.0 . . ?
C64 C63 H63A 120.0 . . ?
C62 C63 H63A 120.0 . . ?
C65 C64 C63 120.0 . . ?
C65 C64 H64A 120.0 . . ?
C63 C64 H64A 120.0 . . ?
C66 C65 C64 120.0 . . ?
C66 C65 H65A 120.0 . . ?
C64 C65 H65A 120.0 . . ?
C65 C66 C61 120.0 . . ?
C65 C66 H66A 120.0 . . ?
C61 C66 H66A 120.0 . . ?
C72 C71 C76 120.0 . . ?
C72 C71 P1 120.0(5) . . ?
C76 C71 P1 120.0(5) . . ?
C73 C72 C71 120.0 . . ?
C73 C72 H72A 120.0 . . ?
C71 C72 H72A 120.0 . . ?
C72 C73 C74 120.0 . . ?
C72 C73 H73A 120.0 . . ?
C74 C73 H73A 120.0 . . ?
C75 C74 C73 120.0 . . ?
C75 C74 H74A 120.0 . . ?
C73 C74 H74A 120.0 . . ?
C74 C75 C76 120.0 . . ?
C74 C75 H75A 120.0 . . ?
C76 C75 H75A 120.0 . . ?
C75 C76 C71 120.0 . . ?
C75 C76 H76A 120.0 . . ?
C71 C76 H76A 120.0 . . ?
C82 C81 C86 120.0 . . ?
C82 C81 P2 120.3(4) . . ?
C86 C81 P2 119.4(4) . . ?
C83 C82 C81 120.0 . . ?
C83 C82 H82A 120.0 . . ?
C81 C82 H82A 120.0 . . ?
C84 C83 C82 120.0 . . ?
C84 C83 H83A 120.0 . . ?
C82 C83 H83A 120.0 . . ?
C83 C84 C85 120.0 . . ?
C83 C84 H84A 120.0 . . ?
C85 C84 H84A 120.0 . . ?
C84 C85 C86 120.0 . . ?
C84 C85 H85A 120.0 . . ?
C86 C85 H85A 120.0 . . ?
C85 C86 C81 120.0 . . ?
C85 C86 H86A 120.0 . . ?
C81 C86 H86A 120.0 . . ?
C92 C91 C96 120.0 . . ?
C92 C91 P2 118.7(4) . . ?
C96 C91 P2 120.4(4) . . ?
C93 C92 C91 120.0 . . ?
C93 C92 H92A 120.0 . . ?
C91 C92 H92A 120.0 . . ?
C94 C93 C92 120.0 . . ?
C94 C93 H93A 120.0 . . ?
C92 C93 H93A 120.0 . . ?
C93 C94 C95 120.0 . . ?
C93 C94 H94A 120.0 . . ?
C95 C94 H94A 120.0 . . ?
C96 C95 C94 120.0 . . ?
C96 C95 H95A 120.0 . . ?
C94 C95 H95A 120.0 . . ?
C95 C96 C91 120.0 . . ?
C95 C96 H96A 120.0 . . ?
C91 C96 H96A 120.0 . . ?
C102 C101 C106 120.0 . . ?
C102 C101 P2 116.7(4) . . ?
C106 C101 P2 122.9(4) . . ?
C103 C102 C101 120.0 . . ?
C103 C102 H10A 120.0 . . ?
C101 C102 H10A 120.0 . . ?
C102 C103 C104 120.0 . . ?
C102 C103 H10B 120.0 . . ?
C104 C103 H10B 120.0 . . ?
C103 C104 C105 120.0 . . ?
C103 C104 H10C 120.0 . . ?
C105 C104 H10C 120.0 . . ?
C106 C105 C104 120.0 . . ?
C106 C105 H10D 120.0 . . ?
C104 C105 H10D 120.0 . . ?
C105 C106 C101 120.0 . . ?
C105 C106 H10E 120.0 . . ?
C101 C106 H10E 120.0 . . ?
Cl2L C1L Cl1L 126.6(16) . . ?
Cl2L C1L H1LA 105.7 . . ?
Cl1L C1L H1LA 105.7 . . ?
Cl2L C1L H2LB 105.7 . . ?
Cl1L C1L H2LB 105.7 . . ?
H1LA C1L H2LB 106.1 . . ?

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
C71 P1 N1 P2 172.8(5) . . . . ?
C51 P1 N1 P2 -74.3(7) . . . . ?
C61 P1 N1 P2 53.1(7) . . . . ?
C101 P2 N1 P1 123.5(6) . . . . ?
C81 P2 N1 P1 -121.6(6) . . . . ?
C91 P2 N1 P1 -1.7(7) . . . . ?
Sn1 C21 C22 C34 -179.2(7) . . . . ?
Sn1 C21 C22 C23 -55.3(10) . . . . ?
C24 O1 C23 C22 176.4(8) . . . . ?
Sn1 O1 C23 C22 -35.8(8) . . . . ?
C34 C22 C23 O1 -178.4(8) . . . . ?
C21 C22 C23 O1 60.7(10) . . . . ?
C23 O1 C24 C25 -86.8(10) . . . . ?
Sn1 O1 C24 C25 132.8(7) . . . . ?
C26 O2 C25 C24 -174.9(8) . . . . ?
O1 C24 C25 O2 74.0(10) . . . . ?
C25 O2 C26 C27 -178.6(8) . . . . ?
C28 O3 C27 C26 172.5(8) . . . . ?
O2 C26 C27 O3 75.0(11) . . . . ?
C27 O3 C28 C29 87.2(10) . . . . ?
C30 O4 C29 C28 -171.3(8) . . . . ?
O3 C28 C29 O4 -71.7(11) . . . . ?
C29 O4 C30 C31 179.5(8) . . . . ?
C32 O5 C31 C30 -167.0(9) . . . . ?
O4 C30 C31 O5 77.6(11) . . . . ?
C31 O5 C32 C33 -170.8(8) . . . . ?
C34 O6 C33 C32 171.7(8) . . . . ?
O5 C32 C33 O6 -66.6(11) . . . . ?
C33 O6 C34 C22 169.3(8) . . . . ?
C23 C22 C34 O6 63.3(11) . . . . ?
C21 C22 C34 O6 -175.1(8) . . . . ?
C46 C41 C42 C43 -3.7(14) . . . . ?
Sn1 C41 C42 C43 173.6(7) . . . . ?
C41 C42 C43 C44 4.2(15) . . . . ?
C42 C43 C44 C45 -1.9(16) . . . . ?
C43 C44 C45 C46 -0.6(16) . . . . ?
C44 C45 C46 C41 1.1(16) . . . . ?
C42 C41 C46 C45 1.0(15) . . . . ?
Sn1 C41 C46 C45 -176.1(7) . . . . ?
N1 P1 C51 C52 -22.8(5) . . . . ?
C71 P1 C51 C52 93.0(4) . . . . ?
C61 P1 C51 C52 -154.5(3) . . . . ?
N1 P1 C51 C56 161.6(4) . . . . ?
C71 P1 C51 C56 -82.6(4) . . . . ?
C61 P1 C51 C56 29.8(5) . . . . ?
C56 C51 C52 C53 0.0 . . . . ?
P1 C51 C52 C53 -175.7(5) . . . . ?
C51 C52 C53 C54 0.0 . . . . ?
C52 C53 C54 C55 0.0 . . . . ?
C53 C54 C55 C56 0.0 . . . . ?
C54 C55 C56 C51 0.0 . . . . ?
C52 C51 C56 C55 0.0 . . . . ?
P1 C51 C56 C55 175.5(5) . . . . ?
N1 P1 C61 C62 -92.8(5) . . . . ?
C71 P1 C61 C62 147.0(4) . . . . ?
C51 P1 C61 C62 37.2(4) . . . . ?
N1 P1 C61 C66 86.5(4) . . . . ?
C71 P1 C61 C66 -33.7(5) . . . . ?
C51 P1 C61 C66 -143.5(3) . . . . ?
C66 C61 C62 C63 0.0 . . . . ?
P1 C61 C62 C63 179.3(5) . . . . ?
C61 C62 C63 C64 0.0 . . . . ?
C62 C63 C64 C65 0.0 . . . . ?
C63 C64 C65 C66 0.0 . . . . ?
C64 C65 C66 C61 0.0 . . . . ?
C62 C61 C66 C65 0.0 . . . . ?
P1 C61 C66 C65 -179.3(5) . . . . ?
N1 P1 C71 C72 -173.2(4) . . . . ?
C51 P1 C71 C72 66.6(4) . . . . ?
C61 P1 C71 C72 -47.1(5) . . . . ?
N1 P1 C71 C76 9.1(5) . . . . ?
C51 P1 C71 C76 -111.1(4) . . . . ?
C61 P1 C71 C76 135.2(4) . . . . ?
C76 C71 C72 C73 0.0 . . . . ?
P1 C71 C72 C73 -177.6(5) . . . . ?
C71 C72 C73 C74 0.0 . . . . ?
C72 C73 C74 C75 0.0 . . . . ?
C73 C74 C75 C76 0.0 . . . . ?
C74 C75 C76 C71 0.0 . . . . ?
C72 C71 C76 C75 0.0 . . . . ?
P1 C71 C76 C75 177.6(5) . . . . ?
N1 P2 C81 C82 -166.3(4) . . . . ?
C101 P2 C81 C82 -50.1(4) . . . . ?
C91 P2 C81 C82 67.7(4) . . . . ?
N1 P2 C81 C86 19.3(5) . . . . ?
C101 P2 C81 C86 135.5(4) . . . . ?
C91 P2 C81 C86 -106.6(4) . . . . ?
C86 C81 C82 C83 0.0 . . . . ?
P2 C81 C82 C83 -174.3(5) . . . . ?
C81 C82 C83 C84 0.0 . . . . ?
C82 C83 C84 C85 0.0 . . . . ?
C83 C84 C85 C86 0.0 . . . . ?
C84 C85 C86 C81 0.0 . . . . ?
C82 C81 C86 C85 0.0 . . . . ?
P2 C81 C86 C85 174.4(5) . . . . ?
N1 P2 C91 C92 -98.7(4) . . . . ?
C101 P2 C91 C92 137.6(3) . . . . ?
C81 P2 C91 C92 23.2(4) . . . . ?
N1 P2 C91 C96 70.7(5) . . . . ?
C101 P2 C91 C96 -53.0(4) . . . . ?
C81 P2 C91 C96 -167.4(3) . . . . ?
C96 C91 C92 C93 0.0 . . . . ?
P2 C91 C92 C93 169.5(4) . . . . ?
C91 C92 C93 C94 0.0 . . . . ?
C92 C93 C94 C95 0.0 . . . . ?
C93 C94 C95 C96 0.0 . . . . ?
C94 C95 C96 C91 0.0 . . . . ?
C92 C91 C96 C95 0.0 . . . . ?
P2 C91 C96 C95 -169.3(4) . . . . ?
N1 P2 C101 C102 46.4(4) . . . . ?
C81 P2 C101 C102 -71.0(4) . . . . ?
C91 P2 C101 C102 174.6(3) . . . . ?
N1 P2 C101 C106 -140.4(4) . . . . ?
C81 P2 C101 C106 102.3(4) . . . . ?
C91 P2 C101 C106 -12.2(4) . . . . ?
C106 C101 C102 C103 0.0 . . . . ?
P2 C101 C102 C103 173.5(4) . . . . ?
C101 C102 C103 C104 0.0 . . . . ?
C102 C103 C104 C105 0.0 . . . . ?
C103 C104 C105 C106 0.0 . . . . ?
C104 C105 C106 C101 0.0 . . . . ?
C102 C101 C106 C105 0.0 . . . . ?
P2 C101 C106 C105 -173.1(5) . . . . ?

_refine_diff_density_max         1.053
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.172

####################################################################### 
# 
# 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_comp2
_database_code_depnum_ccdc_archive 'CCDC 780582'
_audit_update_record             
;
2017-07-27 deposited with the CCDC.
2018-01-02 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        
;
Diiodo-(1,4,7,10,13,16-hexaoxa-cyclononadec-18-ylmethyl)-phenylstannane
;
_chemical_name_common            ?
_chemical_melting_point          445-448
_chemical_formula_moiety         'C20 H32 I2 O6 Sn'
_chemical_formula_sum            'C20 H32 I2 O6 Sn'
_chemical_formula_weight         740.94

# start Validation Reply Form
_vrf_GOODF01_comp2               
;
PROBLEM: The least squares goodness of fit parameter lies
RESPONSE: Due to weak reflection data  the least squares goodness 
of fit parameter lies outside the range 0.60 <> 4.00.
;
# end Validation Reply Form

_ccdc_journal_depnumber          CCDC-780582

_ccdc_chemdiag_type              ChemDraw
_ccdc_chemdiag_records           comp2.cdx


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'
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'
I I -0.4742 1.8119 '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                   13.1138(7)
_cell_length_b                   14.1448(11)
_cell_length_c                   14.5344(11)
_cell_angle_alpha                90
_cell_angle_beta                 107.462(4)
_cell_angle_gamma                90
_cell_volume                     2571.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    27429
_cell_measurement_theta_min      2.94
_cell_measurement_theta_max      27.49

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.914
_exptl_crystal_F_000             1424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    3.424
_shelx_estimated_absorpt_T_min   0.548
_shelx_estimated_absorpt_T_max   0.578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.884
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
R.H. Blessing, Acta Crystallogr., Sect A 1995, 51, 33-38
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5327
_diffrn_reflns_av_unetI/netI     0.1430
_diffrn_reflns_av_R_equivalents  0.054
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.938
_diffrn_reflns_theta_max         26.498
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5327
_reflns_number_gt                2723
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker XSCANS'
_computing_cell_refinement       
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_reduction        
;
DENZO and SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-III (1.0.3) (Farrugia, 2012)'
_computing_publication_material  'enCIFer Version 1.5.2'
_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0400P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         5327
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0810
_refine_ls_R_factor_gt           0.0267
_refine_ls_wR_factor_ref         0.0563
_refine_ls_wR_factor_gt          0.0484
_refine_ls_goodness_of_fit_ref   0.480
_refine_ls_restrained_S_all      0.480
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.14345(2) 0.86773(2) 0.16711(2) 0.03392(9) Uani 1 1 d . . . . .
Sn1 Sn -0.00559(2) 0.72132(2) 0.12923(2) 0.02572(9) Uani 1 1 d . . . . .
I2 I 0.13906(2) 0.57177(2) 0.19264(2) 0.03665(10) Uani 1 1 d . . . . .
O1 O -0.1442(2) 0.8411(2) 0.04222(19) 0.0317(8) Uani 1 1 d . . . . .
O2 O -0.3340(2) 0.9502(2) 0.0470(2) 0.0340(8) Uani 1 1 d . . . . .
O3 O -0.4500(2) 0.8622(2) 0.1708(2) 0.0322(8) Uani 1 1 d . . . . .
O4 O -0.5276(2) 0.6713(2) 0.1553(2) 0.0406(8) Uani 1 1 d . . . . .
O5 O -0.3804(2) 0.5102(2) 0.1421(2) 0.0439(9) Uani 1 1 d . . . . .
O6 O -0.1864(2) 0.6398(2) 0.05885(19) 0.0306(7) Uani 1 1 d . . . . .
C1 C -0.0663(3) 0.7366(3) 0.2492(3) 0.0220(10) Uani 1 1 d . . . . .
C2 C -0.1678(3) 0.7722(3) 0.2391(3) 0.0256(10) Uani 1 1 d . . . . .
H2A H -0.2143 0.7867 0.1768 0.031 Uiso 1 1 calc R U . . .
C3 C -0.2015(3) 0.7866(3) 0.3198(3) 0.0311(11) Uani 1 1 d . . . . .
H3A H -0.2713 0.8102 0.3123 0.037 Uiso 1 1 calc R U . . .
C4 C -0.1345(4) 0.7669(3) 0.4111(3) 0.0337(12) Uani 1 1 d . . . . .
H4A H -0.1572 0.7787 0.4662 0.040 Uiso 1 1 calc R U . . .
C5 C -0.0341(4) 0.7297(3) 0.4215(3) 0.0323(11) Uani 1 1 d . . . . .
H5A H 0.0118 0.7147 0.4839 0.039 Uiso 1 1 calc R U . . .
C6 C 0.0000(3) 0.7143(3) 0.3411(3) 0.0279(11) Uani 1 1 d . . . . .
H6A H 0.0689 0.6884 0.3487 0.034 Uiso 1 1 calc R U . . .
C21 C -0.0336(3) 0.6957(4) -0.0214(3) 0.0410(13) Uani 1 1 d . . . . .
H21A H 0.0141 0.7359 -0.0462 0.049 Uiso 1 1 calc R U . . .
H21B H -0.0185 0.6287 -0.0321 0.049 Uiso 1 1 calc R U . . .
C22 C -0.1499(3) 0.7186(3) -0.0738(3) 0.0353(12) Uani 1 1 d . . . . .
H22A H -0.1606 0.7090 -0.1443 0.042 Uiso 1 1 calc R U . . .
C23 C -0.1730(4) 0.8217(3) -0.0599(3) 0.0399(13) Uani 1 1 d . . . . .
H23A H -0.1311 0.8626 -0.0905 0.048 Uiso 1 1 calc R U . . .
H23B H -0.2499 0.8351 -0.0904 0.048 Uiso 1 1 calc R U . . .
C24 C -0.1421(4) 0.9397(3) 0.0653(3) 0.0354(12) Uani 1 1 d . . . . .
H24A H -0.0858 0.9709 0.0434 0.042 Uiso 1 1 calc R U . . .
H24B H -0.1225 0.9467 0.1362 0.042 Uiso 1 1 calc R U . . .
C25 C -0.2475(3) 0.9897(3) 0.0200(3) 0.0393(13) Uani 1 1 d . . . . .
H25A H -0.2397 1.0571 0.0391 0.047 Uiso 1 1 calc R U . . .
H25B H -0.2645 0.9868 -0.0511 0.047 Uiso 1 1 calc R U . . .
C26 C -0.3417(3) 0.9850(3) 0.1366(3) 0.0336(12) Uani 1 1 d . . . . .
H26A H -0.3329 1.0546 0.1391 0.040 Uiso 1 1 calc R U . . .
H26B H -0.2841 0.9572 0.1903 0.040 Uiso 1 1 calc R U . . .
C27 C -0.4483(4) 0.9595(3) 0.1470(3) 0.0344(12) Uani 1 1 d . . . . .
H27A H -0.4627 0.9985 0.1982 0.041 Uiso 1 1 calc R U . . .
H27B H -0.5049 0.9724 0.0858 0.041 Uiso 1 1 calc R U . . .
C28 C -0.5523(4) 0.8353(3) 0.1744(3) 0.0384(12) Uani 1 1 d . . . . .
H28A H -0.6031 0.8359 0.1084 0.046 Uiso 1 1 calc R U . . .
H28B H -0.5778 0.8814 0.2138 0.046 Uiso 1 1 calc R U . . .
C29 C -0.5498(4) 0.7390(3) 0.2168(4) 0.0425(13) Uani 1 1 d . . . . .
H29A H -0.4943 0.7366 0.2803 0.051 Uiso 1 1 calc R U . . .
H29B H -0.6198 0.7250 0.2266 0.051 Uiso 1 1 calc R U . . .
C30 C -0.5223(4) 0.5792(3) 0.1976(4) 0.0535(15) Uani 1 1 d . . . . .
H30A H -0.5931 0.5619 0.2039 0.064 Uiso 1 1 calc R U . . .
H30B H -0.4699 0.5793 0.2628 0.064 Uiso 1 1 calc R U . . .
C31 C -0.4903(4) 0.5102(3) 0.1366(4) 0.0469(14) Uani 1 1 d . . . . .
H31A H -0.5092 0.4463 0.1541 0.056 Uiso 1 1 calc R U . . .
H31B H -0.5328 0.5219 0.0688 0.056 Uiso 1 1 calc R U . . .
C32 C -0.3425(3) 0.5908(3) 0.1036(3) 0.0349(12) Uani 1 1 d . . . . .
H32A H -0.3362 0.6458 0.1470 0.042 Uiso 1 1 calc R U . . .
H32B H -0.3921 0.6073 0.0395 0.042 Uiso 1 1 calc R U . . .
C33 C -0.2346(3) 0.5640(3) 0.0950(3) 0.0356(12) Uani 1 1 d . . . . .
H33A H -0.1873 0.5450 0.1592 0.043 Uiso 1 1 calc R U . . .
H33B H -0.2427 0.5089 0.0513 0.043 Uiso 1 1 calc R U . . .
C34 C -0.2249(3) 0.6506(3) -0.0446(3) 0.0347(12) Uani 1 1 d . . . . .
H34A H -0.2985 0.6762 -0.0642 0.042 Uiso 1 1 calc R U . . .
H34B H -0.2257 0.5887 -0.0765 0.042 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
I1 Sn1 2.7868(4) . ?
Sn1 C1 2.134(4) . ?
Sn1 C21 2.139(4) . ?
Sn1 O1 2.528(3) . ?
Sn1 I2 2.8060(5) . ?
O1 C24 1.433(5) . ?
O1 C23 1.444(5) . ?
O2 C25 1.422(5) . ?
O2 C26 1.423(5) . ?
O3 C28 1.410(5) . ?
O3 C27 1.421(5) . ?
O4 C29 1.398(5) . ?
O4 C30 1.434(5) . ?
O5 C31 1.419(5) . ?
O5 C32 1.424(5) . ?
O6 C33 1.424(5) . ?
O6 C34 1.444(4) . ?
C1 C2 1.390(5) . ?
C1 C6 1.393(6) . ?
C2 C3 1.386(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.382(6) . ?
C3 H3A 0.9500 . ?
C4 C5 1.383(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.388(6) . ?
C5 H5A 0.9500 . ?
C6 H6A 0.9500 . ?
C21 C22 1.522(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 C23 1.516(6) . ?
C22 C34 1.524(6) . ?
C22 H22A 1.0000 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 C25 1.516(6) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.495(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.491(6) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C30 C31 1.462(6) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 C33 1.506(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Sn1 C21 149.54(16) . . ?
C1 Sn1 O1 87.28(13) . . ?
C21 Sn1 O1 74.03(14) . . ?
C1 Sn1 I1 100.05(10) . . ?
C21 Sn1 I1 102.88(13) . . ?
O1 Sn1 I1 87.55(7) . . ?
C1 Sn1 I2 100.90(11) . . ?
C21 Sn1 I2 95.73(13) . . ?
O1 Sn1 I2 169.43(7) . . ?
I1 Sn1 I2 97.494(14) . . ?
C24 O1 C23 113.9(3) . . ?
C24 O1 Sn1 125.1(2) . . ?
C23 O1 Sn1 108.3(2) . . ?
C25 O2 C26 113.5(3) . . ?
C28 O3 C27 110.8(3) . . ?
C29 O4 C30 109.9(4) . . ?
C31 O5 C32 116.5(3) . . ?
C33 O6 C34 114.2(3) . . ?
C2 C1 C6 119.1(4) . . ?
C2 C1 Sn1 122.1(3) . . ?
C6 C1 Sn1 118.8(3) . . ?
C1 C2 C3 120.1(4) . . ?
C1 C2 H2A 119.9 . . ?
C3 C2 H2A 119.9 . . ?
C4 C3 C2 120.7(4) . . ?
C4 C3 H3A 119.7 . . ?
C2 C3 H3A 119.7 . . ?
C5 C4 C3 119.5(4) . . ?
C5 C4 H4A 120.3 . . ?
C3 C4 H4A 120.3 . . ?
C4 C5 C6 120.3(4) . . ?
C4 C5 H5A 119.9 . . ?
C6 C5 H5A 119.9 . . ?
C5 C6 C1 120.4(4) . . ?
C5 C6 H6A 119.8 . . ?
C1 C6 H6A 119.8 . . ?
C22 C21 Sn1 108.4(3) . . ?
C22 C21 H21A 110.0 . . ?
Sn1 C21 H21A 110.0 . . ?
C22 C21 H21B 110.0 . . ?
Sn1 C21 H21B 110.0 . . ?
H21A C21 H21B 108.4 . . ?
C23 C22 C21 110.4(4) . . ?
C23 C22 C34 113.4(4) . . ?
C21 C22 C34 111.1(4) . . ?
C23 C22 H22A 107.2 . . ?
C21 C22 H22A 107.2 . . ?
C34 C22 H22A 107.2 . . ?
O1 C23 C22 108.6(3) . . ?
O1 C23 H23A 110.0 . . ?
C22 C23 H23A 110.0 . . ?
O1 C23 H23B 110.0 . . ?
C22 C23 H23B 110.0 . . ?
H23A C23 H23B 108.4 . . ?
O1 C24 C25 113.7(4) . . ?
O1 C24 H24A 108.8 . . ?
C25 C24 H24A 108.8 . . ?
O1 C24 H24B 108.8 . . ?
C25 C24 H24B 108.8 . . ?
H24A C24 H24B 107.7 . . ?
O2 C25 C24 113.3(4) . . ?
O2 C25 H25A 108.9 . . ?
C24 C25 H25A 108.9 . . ?
O2 C25 H25B 108.9 . . ?
C24 C25 H25B 108.9 . . ?
H25A C25 H25B 107.7 . . ?
O2 C26 C27 109.5(3) . . ?
O2 C26 H26A 109.8 . . ?
C27 C26 H26A 109.8 . . ?
O2 C26 H26B 109.8 . . ?
C27 C26 H26B 109.8 . . ?
H26A C26 H26B 108.2 . . ?
O3 C27 C26 110.1(4) . . ?
O3 C27 H27A 109.6 . . ?
C26 C27 H27A 109.6 . . ?
O3 C27 H27B 109.6 . . ?
C26 C27 H27B 109.6 . . ?
H27A C27 H27B 108.2 . . ?
O3 C28 C29 111.0(4) . . ?
O3 C28 H28A 109.4 . . ?
C29 C28 H28A 109.4 . . ?
O3 C28 H28B 109.4 . . ?
C29 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
O4 C29 C28 110.2(4) . . ?
O4 C29 H29A 109.6 . . ?
C28 C29 H29A 109.6 . . ?
O4 C29 H29B 109.6 . . ?
C28 C29 H29B 109.6 . . ?
H29A C29 H29B 108.1 . . ?
O4 C30 C31 109.4(4) . . ?
O4 C30 H30A 109.8 . . ?
C31 C30 H30A 109.8 . . ?
O4 C30 H30B 109.8 . . ?
C31 C30 H30B 109.8 . . ?
H30A C30 H30B 108.2 . . ?
O5 C31 C30 116.0(4) . . ?
O5 C31 H31A 108.3 . . ?
C30 C31 H31A 108.3 . . ?
O5 C31 H31B 108.3 . . ?
C30 C31 H31B 108.3 . . ?
H31A C31 H31B 107.4 . . ?
O5 C32 C33 106.1(4) . . ?
O5 C32 H32A 110.5 . . ?
C33 C32 H32A 110.5 . . ?
O5 C32 H32B 110.5 . . ?
C33 C32 H32B 110.5 . . ?
H32A C32 H32B 108.7 . . ?
O6 C33 C32 111.9(4) . . ?
O6 C33 H33A 109.2 . . ?
C32 C33 H33A 109.2 . . ?
O6 C33 H33B 109.2 . . ?
C32 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
O6 C34 C22 107.7(3) . . ?
O6 C34 H34A 110.2 . . ?
C22 C34 H34A 110.2 . . ?
O6 C34 H34B 110.2 . . ?
C22 C34 H34B 110.2 . . ?
H34A C34 H34B 108.5 . . ?

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 1.0(6) . . . . ?
Sn1 C1 C2 C3 -175.9(3) . . . . ?
C1 C2 C3 C4 0.8(6) . . . . ?
C2 C3 C4 C5 -2.0(7) . . . . ?
C3 C4 C5 C6 1.4(7) . . . . ?
C4 C5 C6 C1 0.4(6) . . . . ?
C2 C1 C6 C5 -1.6(6) . . . . ?
Sn1 C1 C6 C5 175.4(3) . . . . ?
Sn1 C21 C22 C23 61.1(4) . . . . ?
Sn1 C21 C22 C34 -65.7(4) . . . . ?
C24 O1 C23 C22 168.2(3) . . . . ?
Sn1 O1 C23 C22 24.2(4) . . . . ?
C21 C22 C23 O1 -55.7(5) . . . . ?
C34 C22 C23 O1 69.7(4) . . . . ?
C23 O1 C24 C25 58.0(5) . . . . ?
Sn1 O1 C24 C25 -165.0(2) . . . . ?
C26 O2 C25 C24 84.0(5) . . . . ?
O1 C24 C25 O2 58.6(5) . . . . ?
C25 O2 C26 C27 165.8(3) . . . . ?
C28 O3 C27 C26 -176.0(4) . . . . ?
O2 C26 C27 O3 75.9(4) . . . . ?
C27 O3 C28 C29 -169.5(4) . . . . ?
C30 O4 C29 C28 178.4(4) . . . . ?
O3 C28 C29 O4 -66.8(5) . . . . ?
C29 O4 C30 C31 -175.3(4) . . . . ?
C32 O5 C31 C30 -68.6(5) . . . . ?
O4 C30 C31 O5 76.0(5) . . . . ?
C31 O5 C32 C33 -166.2(4) . . . . ?
C34 O6 C33 C32 -80.7(5) . . . . ?
O5 C32 C33 O6 -178.8(3) . . . . ?
C33 O6 C34 C22 -167.7(4) . . . . ?
C23 C22 C34 O6 -81.0(4) . . . . ?
C21 C22 C34 O6 44.0(5) . . . . ?

_refine_diff_density_max         0.652
_refine_diff_density_min         -0.724
_refine_diff_density_rms         0.109

