# Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2003


data_global

_journal_coden_Cambridge         182

loop_
_publ_author_name
'Viktor Zhdankin'
'Michael J. Ferguson'
'Alexey Y. Koposov'
'Dmitry N. Litvinov'
'Thanh Luu'
'Robert McDonald'
'Rik Tykwinski'

_publ_contact_author_name        'Prof Viktor Zhdankin'
_publ_contact_author_address     
;
Department of Chemistry
University of Minnesota Duluth
Duluth
Minnesota
55812
UNITED STATES OF AMERICA
;

_publ_contact_author_email       VZHDANKI@D.UMN.EDU

_publ_requested_journal          'Chemical Communications'

_publ_section_title              
;
Preparation and Structure of 2-Iodoxybenzoate
Esters: Soluble and Stable Periodinane Oxidizing Reagents
;

data_compound(4c)
_database_code_depnum_ccdc_archive 'CCDC 222124'

_audit_creation_method           'manual editing of SHELXL template'

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H11 I O4'
_chemical_formula_weight         322.09

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'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6939(6)
_cell_length_b                   10.5225(7)
_cell_length_c                   11.2574(7)
_cell_angle_alpha                96.6580(10)
_cell_angle_beta                 94.9130(10)
_cell_angle_gamma                105.5850(10)
_cell_volume                     1090.40(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    4153
_cell_measurement_theta_min      2.533
_cell_measurement_theta_max      26.375

_exptl_crystal_description       fragment
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.28
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.962
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             624
_exptl_absorpt_coefficient_mu    2.928
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.3798
_exptl_absorpt_correction_T_max  0.4944
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            8154
_diffrn_reflns_av_R_equivalents  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.83
_diffrn_reflns_theta_max         26.38
_reflns_number_total             4428
_reflns_number_gt                4179
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0277P)^2^+0.4291P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4428
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.0199
_refine_ls_wR_factor_ref         0.0537
_refine_ls_wR_factor_gt          0.0530
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.115
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.400370(14) -0.077783(13) -0.140929(11) 0.01605(5) Uani 1 1 d . . .
O11 O 0.37159(17) -0.09459(17) 0.01455(14) 0.0223(3) Uani 1 1 d . . .
O12 O 0.51874(18) -0.18118(18) -0.16878(16) 0.0285(4) Uani 1 1 d . . .
O13 O 0.31963(19) -0.06495(18) -0.38482(15) 0.0289(4) Uani 1 1 d . . .
O14 O 0.1347(2) -0.18771(18) -0.52186(15) 0.0316(4) Uani 1 1 d . . .
C10 C 0.2077(2) -0.2321(2) -0.2113(2) 0.0170(4) Uani 1 1 d . . .
C11 C 0.1460(3) -0.3141(2) -0.1310(2) 0.0221(5) Uani 1 1 d . . .
H11 H 0.1789 -0.2924 -0.0472 0.026 Uiso 1 1 calc R . .
C12 C 0.0351(3) -0.4288(3) -0.1752(2) 0.0247(5) Uani 1 1 d . . .
H12 H -0.0059 -0.4878 -0.1216 0.030 Uiso 1 1 calc R . .
C13 C -0.0163(3) -0.4578(2) -0.2972(2) 0.0249(5) Uani 1 1 d . . .
H13 H -0.0901 -0.5377 -0.3271 0.030 Uiso 1 1 calc R . .
C14 C 0.0400(3) -0.3704(2) -0.3749(2) 0.0221(5) Uani 1 1 d . . .
H14 H 0.0012 -0.3881 -0.4575 0.026 Uiso 1 1 calc R . .
C15 C 0.1537(2) -0.2561(2) -0.3328(2) 0.0187(4) Uani 1 1 d . . .
C16 C 0.2136(3) -0.1596(2) -0.4147(2) 0.0221(5) Uani 1 1 d . . .
C17 C 0.1645(3) -0.0915(3) -0.6083(2) 0.0294(6) Uani 1 1 d . . .
H17 H 0.2003 0.0010 -0.5631 0.035 Uiso 1 1 calc R . .
C18 C 0.0204(3) -0.1082(4) -0.6793(3) 0.0508(9) Uani 1 1 d . . .
H18A H -0.0469 -0.0882 -0.6247 0.061 Uiso 1 1 calc R . .
H18B H -0.0176 -0.2002 -0.7201 0.061 Uiso 1 1 calc R . .
H18C H 0.0319 -0.0470 -0.7394 0.061 Uiso 1 1 calc R . .
C19 C 0.2770(4) -0.1185(4) -0.6826(3) 0.0526(9) Uani 1 1 d . . .
H19A H 0.3672 -0.1056 -0.6301 0.063 Uiso 1 1 calc R . .
H19B H 0.2933 -0.0571 -0.7424 0.063 Uiso 1 1 calc R . .
H19C H 0.2442 -0.2106 -0.7239 0.063 Uiso 1 1 calc R . .
I2 I 0.177117(15) 0.106438(14) 0.034583(12) 0.01843(6) Uani 1 1 d . . .
O21 O -0.00160(17) 0.12832(17) 0.00486(16) 0.0253(4) Uani 1 1 d . . .
O22 O 0.23066(19) 0.08335(18) -0.11461(14) 0.0248(4) Uani 1 1 d . . .
O23 O 0.19792(19) 0.19933(17) 0.27100(15) 0.0248(4) Uani 1 1 d . . .
O24 O 0.32357(18) 0.38869(17) 0.39026(14) 0.0236(4) Uani 1 1 d . . .
C20 C 0.2695(2) 0.3171(2) 0.0640(2) 0.0196(5) Uani 1 1 d . . .
C21 C 0.2920(3) 0.3792(3) -0.0368(2) 0.0250(5) Uani 1 1 d . . .
H21 H 0.2725 0.3282 -0.1148 0.030 Uiso 1 1 calc R . .
C22 C 0.3434(3) 0.5170(3) -0.0228(2) 0.0283(5) Uani 1 1 d . . .
H22 H 0.3589 0.5609 -0.0917 0.034 Uiso 1 1 calc R . .
C23 C 0.3725(3) 0.5912(2) 0.0915(2) 0.0286(6) Uani 1 1 d . . .
H23 H 0.4066 0.6857 0.1005 0.034 Uiso 1 1 calc R . .
C24 C 0.3519(3) 0.5277(2) 0.1925(2) 0.0247(5) Uani 1 1 d . . .
H24 H 0.3736 0.5786 0.2705 0.030 Uiso 1 1 calc R . .
C25 C 0.2996(2) 0.3893(2) 0.1797(2) 0.0199(5) Uani 1 1 d . . .
C26 C 0.2687(2) 0.3155(2) 0.2839(2) 0.0198(5) Uani 1 1 d . . .
C27 C 0.3053(3) 0.3184(3) 0.4962(2) 0.0260(5) Uani 1 1 d . . .
H27 H 0.2095 0.2495 0.4837 0.031 Uiso 1 1 calc R . .
C28 C 0.4244(3) 0.2513(3) 0.5094(3) 0.0346(6) Uani 1 1 d . . .
H28A H 0.4151 0.1851 0.4381 0.041 Uiso 1 1 calc R . .
H28B H 0.4170 0.2069 0.5814 0.041 Uiso 1 1 calc R . .
H28C H 0.5183 0.3183 0.5172 0.041 Uiso 1 1 calc R . .
C29 C 0.3094(3) 0.4228(3) 0.6016(2) 0.0339(6) Uani 1 1 d . . .
H29A H 0.2300 0.4623 0.5867 0.041 Uiso 1 1 calc R . .
H29B H 0.4016 0.4926 0.6112 0.041 Uiso 1 1 calc R . .
H29C H 0.2995 0.3814 0.6751 0.041 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.01511(8) 0.01750(9) 0.01512(8) 0.00225(6) -0.00086(5) 0.00479(6)
O11 0.0231(8) 0.0263(9) 0.0142(7) 0.0055(6) -0.0020(6) 0.0017(7)
O12 0.0218(9) 0.0290(10) 0.0363(10) -0.0024(8) 0.0004(7) 0.0140(7)
O13 0.0287(9) 0.0282(10) 0.0221(9) 0.0055(7) -0.0036(7) -0.0035(8)
O14 0.0390(10) 0.0272(10) 0.0200(9) 0.0085(7) -0.0090(7) -0.0035(8)
C10 0.0157(10) 0.0154(11) 0.0191(11) 0.0005(8) -0.0007(8) 0.0044(8)
C11 0.0231(12) 0.0229(12) 0.0211(11) 0.0043(9) 0.0024(9) 0.0077(10)
C12 0.0214(12) 0.0247(13) 0.0286(13) 0.0089(10) 0.0041(10) 0.0051(10)
C13 0.0201(12) 0.0206(12) 0.0316(13) 0.0018(10) 0.0028(10) 0.0027(9)
C14 0.0227(12) 0.0214(12) 0.0204(11) -0.0007(9) -0.0030(9) 0.0066(10)
C15 0.0185(11) 0.0188(11) 0.0192(11) 0.0015(9) -0.0001(8) 0.0070(9)
C16 0.0262(12) 0.0234(12) 0.0159(11) 0.0020(9) -0.0004(9) 0.0069(10)
C17 0.0348(14) 0.0261(13) 0.0227(12) 0.0107(10) -0.0036(10) -0.0001(11)
C18 0.0390(17) 0.062(2) 0.0459(18) 0.0309(16) -0.0082(14) -0.0003(15)
C19 0.062(2) 0.062(2) 0.0457(19) 0.0267(17) 0.0196(16) 0.0272(18)
I2 0.01829(9) 0.01901(9) 0.01773(9) 0.00010(6) 0.00033(6) 0.00644(6)
O21 0.0161(8) 0.0223(9) 0.0360(10) -0.0027(7) -0.0024(7) 0.0076(7)
O22 0.0304(9) 0.0300(10) 0.0177(8) 0.0022(7) 0.0028(7) 0.0153(8)
O23 0.0299(9) 0.0199(9) 0.0218(8) 0.0009(7) 0.0042(7) 0.0026(7)
O24 0.0270(9) 0.0211(9) 0.0192(8) 0.0026(7) -0.0015(7) 0.0020(7)
C20 0.0160(11) 0.0197(11) 0.0238(11) 0.0045(9) 0.0005(9) 0.0060(9)
C21 0.0213(11) 0.0309(14) 0.0248(12) 0.0073(10) 0.0016(9) 0.0101(10)
C22 0.0237(12) 0.0317(14) 0.0344(14) 0.0164(11) 0.0050(11) 0.0107(10)
C23 0.0244(13) 0.0214(13) 0.0423(16) 0.0111(12) 0.0035(11) 0.0077(10)
C24 0.0214(12) 0.0208(12) 0.0300(13) 0.0016(10) -0.0016(10) 0.0053(9)
C25 0.0151(10) 0.0221(12) 0.0230(11) 0.0050(9) -0.0008(9) 0.0060(9)
C26 0.0180(11) 0.0187(12) 0.0230(11) 0.0013(9) 0.0012(9) 0.0065(9)
C27 0.0280(13) 0.0259(13) 0.0210(12) 0.0065(10) -0.0005(10) 0.0020(10)
C28 0.0403(16) 0.0286(14) 0.0330(14) 0.0051(11) -0.0060(12) 0.0095(12)
C29 0.0331(14) 0.0413(16) 0.0242(13) -0.0003(11) 0.0009(11) 0.0081(12)

_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 O12 1.8033(17) . ?
I1 O11 1.8170(15) . ?
I1 C10 2.138(2) . ?
I1 O11 2.6285(16) 2_655 ?
I1 O22 2.6711(17) . ?
I1 O13 2.8185(17) . ?
O11 I1 2.6285(16) 2_655 ?
O12 I2 3.0510(17) 2_655 ?
O13 C16 1.214(3) . ?
O14 C16 1.329(3) . ?
O14 C17 1.475(3) . ?
C10 C11 1.383(3) . ?
C10 C15 1.391(3) . ?
C11 C12 1.390(3) . ?
C12 C13 1.389(3) . ?
C13 C14 1.382(3) . ?
C14 C15 1.397(3) . ?
C15 C16 1.487(3) . ?
C17 C19 1.496(4) . ?
C17 C18 1.505(4) . ?
I2 O22 1.8088(16) . ?
I2 O21 1.8164(16) . ?
I2 C20 2.130(2) . ?
I2 O21 2.5597(17) 2 ?
I2 O23 2.6979(16) . ?
I2 O12 3.0510(17) 2_655 ?
O21 I2 2.5597(17) 2 ?
O23 C26 1.215(3) . ?
O24 C26 1.329(3) . ?
O24 C27 1.473(3) . ?
C20 C21 1.378(3) . ?
C20 C25 1.394(3) . ?
C21 C22 1.386(4) . ?
C22 C23 1.390(4) . ?
C23 C24 1.386(3) . ?
C24 C25 1.394(3) . ?
C25 C26 1.488(3) . ?
C27 C29 1.511(4) . ?
C27 C28 1.512(4) . ?

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
O12 I1 O11 101.77(8) . . ?
O12 I1 C10 94.54(8) . . ?
O11 I1 C10 93.15(8) . . ?
O12 I1 O11 85.53(7) . 2_655 ?
O11 I1 O11 75.98(7) . 2_655 ?
C10 I1 O11 168.87(7) . 2_655 ?
O12 I1 O22 175.67(7) . . ?
O11 I1 O22 82.40(6) . . ?
C10 I1 O22 86.33(7) . . ?
O11 I1 O22 94.43(5) 2_655 . ?
O12 I1 O13 96.18(7) . . ?
O11 I1 O13 155.77(6) . . ?
C10 I1 O13 69.14(7) . . ?
O11 I1 O13 121.95(5) 2_655 . ?
O22 I1 O13 80.15(5) . . ?
I1 O11 I1 104.02(7) . 2_655 ?
I1 O12 I2 120.87(8) . 2_655 ?
C16 O13 I1 104.31(14) . . ?
C16 O14 C17 119.30(19) . . ?
C11 C10 C15 121.6(2) . . ?
C11 C10 I1 116.14(16) . . ?
C15 C10 I1 122.08(16) . . ?
C10 C11 C12 118.8(2) . . ?
C13 C12 C11 120.5(2) . . ?
C14 C13 C12 120.0(2) . . ?
C13 C14 C15 120.4(2) . . ?
C10 C15 C14 118.6(2) . . ?
C10 C15 C16 120.3(2) . . ?
C14 C15 C16 121.1(2) . . ?
O13 C16 O14 124.8(2) . . ?
O13 C16 C15 123.4(2) . . ?
O14 C16 C15 111.8(2) . . ?
O14 C17 C19 109.7(2) . . ?
O14 C17 C18 104.8(2) . . ?
C19 C17 C18 114.4(3) . . ?
O22 I2 O21 102.97(8) . . ?
O22 I2 C20 94.85(8) . . ?
O21 I2 C20 90.35(8) . . ?
O22 I2 O21 90.28(7) . 2 ?
O21 I2 O21 73.96(7) . 2 ?
C20 I2 O21 164.24(7) . 2 ?
O22 I2 O23 158.81(7) . . ?
O21 I2 O23 92.40(7) . . ?
C20 I2 O23 70.24(7) . . ?
O21 I2 O23 108.14(5) 2 . ?
O22 I2 O12 95.85(6) . 2_655 ?
O21 I2 O12 153.27(6) . 2_655 ?
C20 I2 O12 69.07(7) . 2_655 ?
O21 I2 O12 125.26(5) 2 2_655 ?
O23 I2 O12 65.18(5) . 2_655 ?
I2 O21 I2 106.04(7) . 2 ?
I2 O22 I1 114.69(8) . . ?
C26 O23 I2 106.31(14) . . ?
C26 O24 C27 116.25(18) . . ?
C21 C20 C25 121.7(2) . . ?
C21 C20 I2 116.87(17) . . ?
C25 C20 I2 121.39(17) . . ?
C20 C21 C22 119.1(2) . . ?
C21 C22 C23 120.3(2) . . ?
C24 C23 C22 120.1(2) . . ?
C23 C24 C25 120.2(2) . . ?
C24 C25 C20 118.6(2) . . ?
C24 C25 C26 122.8(2) . . ?
C20 C25 C26 118.5(2) . . ?
O23 C26 O24 124.0(2) . . ?
O23 C26 C25 122.1(2) . . ?
O24 C26 C25 113.9(2) . . ?
O24 C27 C29 106.1(2) . . ?
O24 C27 C28 107.9(2) . . ?
C29 C27 C28 113.9(2) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12 I1 O11 I1 82.30(8) . . . 2_655 ?
C10 I1 O11 I1 177.60(8) . . . 2_655 ?
O11 I1 O11 I1 0.0 2_655 . . 2_655 ?
O22 I1 O11 I1 -96.53(7) . . . 2_655 ?
O13 I1 O11 I1 -140.71(12) . . . 2_655 ?
O11 I1 O12 I2 -65.56(10) . . . 2_655 ?
C10 I1 O12 I2 -159.74(9) . . . 2_655 ?
O11 I1 O12 I2 9.10(8) 2_655 . . 2_655 ?
O22 I1 O12 I2 98.8(9) . . . 2_655 ?
O13 I1 O12 I2 130.79(8) . . . 2_655 ?
O12 I1 O13 C16 89.96(17) . . . . ?
O11 I1 O13 C16 -47.8(3) . . . . ?
C10 I1 O13 C16 -2.55(16) . . . . ?
O11 I1 O13 C16 178.54(15) 2_655 . . . ?
O22 I1 O13 C16 -92.36(17) . . . . ?
O12 I1 C10 C11 86.76(18) . . . . ?
O11 I1 C10 C11 -15.33(18) . . . . ?
O11 I1 C10 C11 -3.2(5) 2_655 . . . ?
O22 I1 C10 C11 -97.49(17) . . . . ?
O13 I1 C10 C11 -178.35(19) . . . . ?
O12 I1 C10 C15 -88.02(19) . . . . ?
O11 I1 C10 C15 169.90(18) . . . . ?
O11 I1 C10 C15 -178.0(3) 2_655 . . . ?
O22 I1 C10 C15 87.73(18) . . . . ?
O13 I1 C10 C15 6.88(17) . . . . ?
C15 C10 C11 C12 5.2(4) . . . . ?
I1 C10 C11 C12 -169.60(18) . . . . ?
C10 C11 C12 C13 -2.3(4) . . . . ?
C11 C12 C13 C14 -1.9(4) . . . . ?
C12 C13 C14 C15 3.3(4) . . . . ?
C11 C10 C15 C14 -3.8(3) . . . . ?
I1 C10 C15 C14 170.70(17) . . . . ?
C11 C10 C15 C16 174.4(2) . . . . ?
I1 C10 C15 C16 -11.1(3) . . . . ?
C13 C14 C15 C10 -0.5(3) . . . . ?
C13 C14 C15 C16 -178.7(2) . . . . ?
I1 O13 C16 O14 176.1(2) . . . . ?
I1 O13 C16 C15 -1.8(3) . . . . ?
C17 O14 C16 O13 -7.4(4) . . . . ?
C17 O14 C16 C15 170.7(2) . . . . ?
C10 C15 C16 O13 8.1(4) . . . . ?
C14 C15 C16 O13 -173.8(2) . . . . ?
C10 C15 C16 O14 -170.1(2) . . . . ?
C14 C15 C16 O14 8.1(3) . . . . ?
C16 O14 C17 C19 88.2(3) . . . . ?
C16 O14 C17 C18 -148.6(3) . . . . ?
O22 I2 O21 I2 86.50(8) . . . 2 ?
C20 I2 O21 I2 -178.43(8) . . . 2 ?
O21 I2 O21 I2 0.0 2 . . 2 ?
O23 I2 O21 I2 -108.20(7) . . . 2 ?
O12 I2 O21 I2 -139.88(11) 2_655 . . 2 ?
O21 I2 O22 I1 -147.73(8) . . . . ?
C20 I2 O22 I1 120.79(9) . . . . ?
O21 I2 O22 I1 -74.13(8) 2 . . . ?
O23 I2 O22 I1 76.8(2) . . . . ?
O12 I2 O22 I1 51.38(8) 2_655 . . . ?
O12 I1 O22 I2 -161.9(9) . . . . ?
O11 I1 O22 I2 2.72(9) . . . . ?
C10 I1 O22 I2 96.40(10) . . . . ?
O11 I1 O22 I2 -72.48(9) 2_655 . . . ?
O13 I1 O22 I2 165.84(9) . . . . ?
O22 I2 O23 C26 38.2(3) . . . . ?
O21 I2 O23 C26 -98.67(16) . . . . ?
C20 I2 O23 C26 -9.15(16) . . . . ?
O21 I2 O23 C26 -172.57(15) 2 . . . ?
O12 I2 O23 C26 66.25(15) 2_655 . . . ?
O22 I2 C20 C21 21.89(18) . . . . ?
O21 I2 C20 C21 -81.16(18) . . . . ?
O21 I2 C20 C21 -86.7(3) 2 . . . ?
O23 I2 C20 C21 -173.58(19) . . . . ?
O12 I2 C20 C21 116.31(18) 2_655 . . . ?
O22 I2 C20 C25 -160.96(18) . . . . ?
O21 I2 C20 C25 95.99(19) . . . . ?
O21 I2 C20 C25 90.4(3) 2 . . . ?
O23 I2 C20 C25 3.57(17) . . . . ?
O12 I2 C20 C25 -66.54(18) 2_655 . . . ?
C25 C20 C21 C22 -1.1(4) . . . . ?
I2 C20 C21 C22 176.00(18) . . . . ?
C20 C21 C22 C23 0.3(4) . . . . ?
C21 C22 C23 C24 0.8(4) . . . . ?
C22 C23 C24 C25 -1.2(4) . . . . ?
C23 C24 C25 C20 0.4(3) . . . . ?
C23 C24 C25 C26 -177.1(2) . . . . ?
C21 C20 C25 C24 0.8(3) . . . . ?
I2 C20 C25 C24 -176.22(17) . . . . ?
C21 C20 C25 C26 178.4(2) . . . . ?
I2 C20 C25 C26 1.4(3) . . . . ?
I2 O23 C26 O24 -167.69(18) . . . . ?
I2 O23 C26 C25 13.3(3) . . . . ?
C27 O24 C26 O23 5.1(3) . . . . ?
C27 O24 C26 C25 -175.79(19) . . . . ?
C24 C25 C26 O23 165.5(2) . . . . ?
C20 C25 C26 O23 -12.0(3) . . . . ?
C24 C25 C26 O24 -13.6(3) . . . . ?
C20 C25 C26 O24 168.9(2) . . . . ?
C26 O24 C27 C29 -154.3(2) . . . . ?
C26 O24 C27 C28 83.1(2) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        26.38
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.960
_refine_diff_density_rms         0.133

data_compound(4a)
_database_code_depnum_ccdc_archive 'CCDC 222125'

_audit_creation_method           'manual editing of SHELXL template'

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H13 I O5 S'
_chemical_formula_weight         372.16

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'
S S 0.1246 0.1234 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.0364(4)
_cell_length_b                   9.0124(5)
_cell_length_c                   10.0969(6)
_cell_angle_alpha                81.2810(10)
_cell_angle_beta                 76.5950(10)
_cell_angle_gamma                67.4220(10)
_cell_volume                     655.25(6)
_cell_formula_units_Z            2
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    5405
_cell_measurement_theta_min      2.796
_cell_measurement_theta_max      26.396

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.23
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             364
_exptl_absorpt_coefficient_mu    2.609
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.3735
_exptl_absorpt_correction_T_max  0.5852
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            4571
_diffrn_reflns_av_R_equivalents  0.0140
_diffrn_reflns_av_sigmaI/netI    0.0271
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.08
_diffrn_reflns_theta_max         26.40
_reflns_number_total             2632
_reflns_number_gt                2617
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0096P)^2^+0.4186P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0853(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         2632
_refine_ls_number_parameters     158
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0162
_refine_ls_R_factor_gt           0.0160
_refine_ls_wR_factor_ref         0.0424
_refine_ls_wR_factor_gt          0.0423
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_restrained_S_all      1.113
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I I 0.349304(14) 0.049397(13) 0.163169(11) 0.01886(7) Uani 1 1 d . . .
O1 O 0.2989(2) 0.1897(2) 0.39440(16) 0.0312(3) Uani 1 1 d . . .
O2 O 0.0592(2) 0.31119(19) 0.55443(15) 0.0283(3) Uani 1 1 d . . .
O3 O 0.3121(2) -0.0008(2) 0.00865(15) 0.0299(3) Uani 1 1 d . . .
O4 O 0.4423(2) -0.14454(19) 0.25000(17) 0.0355(4) Uani 1 1 d . . .
C1 C 0.0724(3) 0.1046(2) 0.26814(19) 0.0191(4) Uani 1 1 d . . .
C2 C 0.0097(3) 0.1787(2) 0.3916(2) 0.0200(4) Uani 1 1 d . . .
C3 C -0.1693(3) 0.2020(2) 0.4608(2) 0.0244(4) Uani 1 1 d . . .
H3 H -0.2144 0.2522 0.5447 0.029 Uiso 1 1 calc R . .
C4 C -0.2810(3) 0.1518(3) 0.4072(2) 0.0281(4) Uani 1 1 d . . .
H4 H -0.4023 0.1668 0.4551 0.034 Uiso 1 1 calc R . .
C5 C -0.2173(3) 0.0799(3) 0.2841(2) 0.0284(4) Uani 1 1 d . . .
H5 H -0.2952 0.0463 0.2480 0.034 Uiso 1 1 calc R . .
C6 C -0.0393(3) 0.0567(2) 0.2129(2) 0.0241(4) Uani 1 1 d . . .
H6 H 0.0042 0.0089 0.1279 0.029 Uiso 1 1 calc R . .
C7 C 0.1376(3) 0.2256(2) 0.4454(2) 0.0220(4) Uani 1 1 d . . .
C8 C 0.1803(3) 0.3587(3) 0.6108(2) 0.0345(5) Uani 1 1 d . . .
H8A H 0.1078 0.4323 0.6828 0.041 Uiso 1 1 calc R . .
H8B H 0.2456 0.4131 0.5385 0.041 Uiso 1 1 calc R . .
H8C H 0.2693 0.2629 0.6492 0.041 Uiso 1 1 calc R . .
S S 0.29549(7) 0.46323(6) 0.04701(6) 0.02832(12) Uani 1 1 d . . .
O1S O 0.1669(2) 0.37390(19) 0.1090(2) 0.0412(4) Uani 1 1 d . . .
C1S C 0.2914(3) 0.4962(3) -0.1302(2) 0.0351(5) Uani 1 1 d . . .
H1SA H 0.3525 0.3933 -0.1729 0.042 Uiso 1 1 calc R . .
H1SB H 0.3556 0.5697 -0.1722 0.042 Uiso 1 1 calc R . .
H1SC H 0.1638 0.5438 -0.1433 0.042 Uiso 1 1 calc R . .
C2S C 0.1726(4) 0.6662(3) 0.0919(3) 0.0401(6) Uani 1 1 d . . .
H2SA H 0.1554 0.6704 0.1908 0.048 Uiso 1 1 calc R . .
H2SB H 0.0526 0.7061 0.0649 0.048 Uiso 1 1 calc R . .
H2SC H 0.2424 0.7336 0.0447 0.048 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I 0.01616(9) 0.02190(9) 0.01722(9) -0.00318(5) -0.00154(5) -0.00576(6)
O1 0.0194(7) 0.0487(9) 0.0292(8) -0.0142(7) -0.0017(6) -0.0139(7)
O2 0.0241(7) 0.0373(8) 0.0265(8) -0.0134(6) -0.0050(6) -0.0100(6)
O3 0.0290(8) 0.0446(9) 0.0203(7) -0.0116(6) 0.0012(6) -0.0177(7)
O4 0.0290(8) 0.0271(8) 0.0339(8) 0.0054(6) -0.0012(7) 0.0021(6)
C1 0.0172(8) 0.0195(8) 0.0196(9) -0.0003(7) -0.0033(7) -0.0061(7)
C2 0.0192(9) 0.0210(8) 0.0201(9) -0.0007(7) -0.0039(7) -0.0077(7)
C3 0.0193(9) 0.0280(10) 0.0227(10) -0.0019(8) -0.0012(8) -0.0067(8)
C4 0.0182(9) 0.0334(11) 0.0315(11) 0.0012(9) -0.0021(8) -0.0107(8)
C5 0.0233(10) 0.0325(10) 0.0357(11) -0.0010(9) -0.0107(9) -0.0145(8)
C6 0.0249(10) 0.0246(9) 0.0252(10) -0.0021(7) -0.0070(8) -0.0102(8)
C7 0.0226(9) 0.0238(9) 0.0192(9) -0.0026(7) -0.0047(8) -0.0070(7)
C8 0.0343(12) 0.0406(12) 0.0356(12) -0.0139(10) -0.0132(10) -0.0134(10)
S 0.0247(3) 0.0257(2) 0.0372(3) 0.0028(2) -0.0088(2) -0.0122(2)
O1S 0.0274(8) 0.0277(8) 0.0669(12) 0.0114(8) -0.0085(8) -0.0140(7)
C1S 0.0333(12) 0.0346(11) 0.0375(12) -0.0089(9) -0.0109(10) -0.0078(9)
C2S 0.0515(15) 0.0318(12) 0.0382(13) -0.0085(10) 0.0013(11) -0.0197(11)

_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
I O4 1.7940(15) . ?
I O3 1.8061(14) . ?
I C1 2.1307(19) . ?
I O1 2.6979(15) . ?
I O1S 2.7560(16) . ?
I O3 2.7805(15) 2_655 ?
O1 C7 1.212(2) . ?
O2 C7 1.329(2) . ?
O2 C8 1.451(2) . ?
C1 C6 1.381(3) . ?
C1 C2 1.399(3) . ?
C2 C3 1.396(3) . ?
C2 C7 1.480(3) . ?
C3 C4 1.384(3) . ?
C4 C5 1.386(3) . ?
C5 C6 1.395(3) . ?
S O1S 1.5145(15) . ?
S C1S 1.775(2) . ?
S C2S 1.784(2) . ?

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
O4 I O3 102.62(8) . . ?
O4 I C1 96.79(7) . . ?
O3 I C1 95.12(7) . . ?
O4 I O1 89.52(7) . . ?
O3 I O1 162.35(6) . . ?
C1 I O1 70.46(6) . . ?
O4 I O1S 162.79(7) . . ?
O3 I O1S 92.29(7) . . ?
C1 I O1S 73.07(6) . . ?
O1 I O1S 74.10(6) . . ?
O4 I O3 90.22(6) . 2_655 ?
O3 I O3 78.19(6) . 2_655 ?
C1 I O3 171.26(6) . 2_655 ?
O1 I O3 114.98(4) . 2_655 ?
O1S I O3 101.34(5) . 2_655 ?
C7 O1 I 106.31(12) . . ?
C7 O2 C8 115.55(16) . . ?
C6 C1 C2 121.57(18) . . ?
C6 C1 I 117.20(14) . . ?
C2 C1 I 121.15(13) . . ?
C3 C2 C1 118.72(18) . . ?
C3 C2 C7 122.63(18) . . ?
C1 C2 C7 118.63(17) . . ?
C4 C3 C2 120.03(19) . . ?
C3 C4 C5 120.48(19) . . ?
C4 C5 C6 120.38(19) . . ?
C1 C6 C5 118.80(19) . . ?
O1 C7 O2 123.05(18) . . ?
O1 C7 C2 123.12(18) . . ?
O2 C7 C2 113.84(17) . . ?
O1S S C1S 106.47(12) . . ?
O1S S C2S 105.52(11) . . ?
C1S S C2S 98.00(12) . . ?
S O1S I 112.94(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
O4 I O1 C7 -100.83(14) . . . . ?
O3 I O1 C7 33.1(3) . . . . ?
C1 I O1 C7 -3.45(13) . . . . ?
O1S I O1 C7 73.83(14) . . . . ?
O3 I O1 C7 169.15(13) 2_655 . . . ?
O4 I C1 C6 -89.54(16) . . . . ?
O3 I C1 C6 13.85(16) . . . . ?
O1 I C1 C6 -176.61(16) . . . . ?
O1S I C1 C6 104.69(15) . . . . ?
O3 I C1 C6 53.5(4) 2_655 . . . ?
O4 I C1 C2 87.19(16) . . . . ?
O3 I C1 C2 -169.43(15) . . . . ?
O1 I C1 C2 0.12(14) . . . . ?
O1S I C1 C2 -78.59(15) . . . . ?
O3 I C1 C2 -129.7(3) 2_655 . . . ?
C6 C1 C2 C3 1.0(3) . . . . ?
I C1 C2 C3 -175.58(14) . . . . ?
C6 C1 C2 C7 179.45(18) . . . . ?
I C1 C2 C7 2.9(2) . . . . ?
C1 C2 C3 C4 0.1(3) . . . . ?
C7 C2 C3 C4 -178.27(19) . . . . ?
C2 C3 C4 C5 -0.7(3) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
C2 C1 C6 C5 -1.5(3) . . . . ?
I C1 C6 C5 175.23(15) . . . . ?
C4 C5 C6 C1 0.9(3) . . . . ?
I O1 C7 O2 -173.38(16) . . . . ?
I O1 C7 C2 6.3(2) . . . . ?
C8 O2 C7 O1 -0.7(3) . . . . ?
C8 O2 C7 C2 179.66(17) . . . . ?
C3 C2 C7 O1 171.4(2) . . . . ?
C1 C2 C7 O1 -7.0(3) . . . . ?
C3 C2 C7 O2 -8.9(3) . . . . ?
C1 C2 C7 O2 172.69(17) . . . . ?
C1S S O1S I 102.64(11) . . . . ?
C2S S O1S I -153.91(12) . . . . ?
O4 I O1S S 110.5(2) . . . . ?
O3 I O1S S -99.23(12) . . . . ?
C1 I O1S S 166.12(13) . . . . ?
O1 I O1S S 92.19(11) . . . . ?
O3 I O1S S -20.82(12) 2_655 . . . ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        26.40
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.070

data_compound(4d)
_database_code_depnum_ccdc_archive 'CCDC 222126'

_audit_creation_method           'manual editing of SHELXL template'

_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C11 H13 I O4'
_chemical_formula_weight         336.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.8981(9)
_cell_length_b                   11.3827(10)
_cell_length_c                   11.5247(10)
_cell_angle_alpha                83.3624(17)
_cell_angle_beta                 62.3591(16)
_cell_angle_gamma                89.6303(17)
_cell_volume                     1256.18(19)
_cell_formula_units_Z            4
_cell_measurement_temperature    193(2)
_cell_measurement_reflns_used    5212
_cell_measurement_theta_min      2.526
_cell_measurement_theta_max      26.351

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      0
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             656
_exptl_absorpt_coefficient_mu    2.546
_exptl_absorpt_correction_type   integration
_exptl_absorpt_correction_T_min  0.3872
_exptl_absorpt_correction_T_max  0.8419
_exptl_absorpt_process_details   'Bruker SHELXTL (Bruker, 1997)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      193(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  
'Bruker PLATFORM diffractometer/SMART 1000 CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number         0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        0
_diffrn_reflns_number            7149
_diffrn_reflns_av_R_equivalents  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         1.80
_diffrn_reflns_theta_max         26.37
_reflns_number_total             5063
_reflns_number_gt                4375
_reflns_threshold_expression     I>2\s(I)

_computing_data_collection       'Bruker SMART (Bruker, 1997)'
_computing_cell_refinement       'Bruker SAINT (Bruker, 1997)'
_computing_data_reduction        'Bruker SAINT (Bruker, 1997)'
_computing_structure_solution    'DIRDIF-96 (Beurskens et al., 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker, 1997)'
_computing_publication_material  'Bruker SHELXTL (Bruker, 1997)'

_refine_special_details          
;
Refinement of F^2^ against ALL reflections.  The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement.  R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0603P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5063
_refine_ls_number_parameters     289
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0324
_refine_ls_wR_factor_ref         0.0880
_refine_ls_wR_factor_gt          0.0843
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.17368(2) 0.458645(18) 0.40297(2) 0.02079(8) Uani 1 1 d . . .
I2 I -0.07062(2) 0.280638(19) 0.76031(2) 0.02585(9) Uani 1 1 d . . .
O11 O 0.1420(3) 0.3127(2) 0.4944(3) 0.0300(6) Uani 1 1 d . . .
O12 O 0.0235(2) 0.4676(2) 0.3740(3) 0.0267(5) Uani 1 1 d . . .
O13 O 0.4351(3) 0.4508(3) 0.3679(3) 0.0334(6) Uani 1 1 d . . .
O14 O 0.6383(2) 0.3941(2) 0.2106(3) 0.0324(6) Uani 1 1 d . . .
O21 O -0.2085(3) 0.3164(2) 0.7182(3) 0.0362(7) Uani 1 1 d . . .
O22 O -0.1632(3) 0.2496(3) 0.9356(3) 0.0429(7) Uani 1 1 d . . .
O23 O 0.1428(3) 0.1831(2) 0.7820(3) 0.0373(7) Uani 1 1 d . . .
O24 O 0.2448(3) 0.0078(2) 0.7465(3) 0.0418(7) Uani 1 1 d . . .
C10 C 0.3057(3) 0.4075(3) 0.2135(3) 0.0222(7) Uani 1 1 d . . .
C11 C 0.2456(3) 0.3888(3) 0.1339(4) 0.0269(8) Uani 1 1 d . . .
H11 H 0.1509 0.4037 0.1610 0.032 Uiso 1 1 calc R . .
C12 C 0.3266(4) 0.3480(3) 0.0141(4) 0.0306(8) Uani 1 1 d . . .
H12 H 0.2870 0.3342 -0.0416 0.037 Uiso 1 1 calc R . .
C13 C 0.4648(4) 0.3273(3) -0.0253(4) 0.0295(8) Uani 1 1 d . . .
H13 H 0.5190 0.2986 -0.1075 0.035 Uiso 1 1 calc R . .
C14 C 0.5247(3) 0.3476(3) 0.0528(4) 0.0253(7) Uani 1 1 d . . .
H14 H 0.6200 0.3343 0.0241 0.030 Uiso 1 1 calc R . .
C15 C 0.4442(3) 0.3882(3) 0.1752(3) 0.0216(7) Uani 1 1 d . . .
C16 C 0.5041(3) 0.4138(3) 0.2630(4) 0.0272(8) Uani 1 1 d . . .
C17 C 0.7216(4) 0.4106(4) 0.2799(4) 0.0355(9) Uani 1 1 d . . .
C1A C 0.7260(5) 0.5378(4) 0.3016(5) 0.0471(11) Uani 1 1 d . . .
H1AA H 0.6335 0.5580 0.3658 0.057 Uiso 1 1 calc R . .
H1AB H 0.7552 0.5889 0.2178 0.057 Uiso 1 1 calc R . .
H1AC H 0.7921 0.5494 0.3353 0.057 Uiso 1 1 calc R . .
C1B C 0.6651(5) 0.3271(4) 0.4057(5) 0.0442(11) Uani 1 1 d . . .
H1BA H 0.5737 0.3512 0.4679 0.053 Uiso 1 1 calc R . .
H1BB H 0.7283 0.3290 0.4445 0.053 Uiso 1 1 calc R . .
H1BC H 0.6565 0.2466 0.3871 0.053 Uiso 1 1 calc R . .
C1C C 0.8655(4) 0.3790(6) 0.1792(5) 0.0571(14) Uani 1 1 d . . .
H1CA H 0.8625 0.2958 0.1656 0.069 Uiso 1 1 calc R . .
H1CB H 0.9321 0.3910 0.2122 0.069 Uiso 1 1 calc R . .
H1CC H 0.8941 0.4297 0.0953 0.069 Uiso 1 1 calc R . .
C20 C -0.0547(4) 0.1052(3) 0.7099(4) 0.0291(8) Uani 1 1 d . . .
C21 C -0.1537(4) 0.0634(4) 0.6803(4) 0.0391(10) Uani 1 1 d . . .
H21 H -0.2240 0.1125 0.6789 0.047 Uiso 1 1 calc R . .
C22 C -0.1481(5) -0.0541(4) 0.6522(5) 0.0476(11) Uani 1 1 d . . .
H22 H -0.2163 -0.0851 0.6327 0.057 Uiso 1 1 calc R . .
C23 C -0.0460(5) -0.1242(4) 0.6525(5) 0.0458(11) Uani 1 1 d . . .
H23 H -0.0429 -0.2030 0.6321 0.055 Uiso 1 1 calc R . .
C24 C 0.0531(5) -0.0809(4) 0.6823(5) 0.0409(10) Uani 1 1 d . . .
H24 H 0.1243 -0.1300 0.6815 0.049 Uiso 1 1 calc R . .
C25 C 0.0489(4) 0.0340(3) 0.7134(4) 0.0330(8) Uani 1 1 d . . .
C26 C 0.1507(4) 0.0834(3) 0.7506(4) 0.0331(9) Uani 1 1 d . . .
C27 C 0.3476(5) 0.0346(4) 0.7926(5) 0.0438(10) Uani 1 1 d . . .
C2A C 0.4395(5) 0.1410(4) 0.7068(6) 0.0579(14) Uani 1 1 d . . .
H2AA H 0.3847 0.2115 0.7216 0.069 Uiso 1 1 calc R . .
H2AB H 0.4787 0.1286 0.6138 0.069 Uiso 1 1 calc R . .
H2AC H 0.5148 0.1521 0.7291 0.069 Uiso 1 1 calc R . .
C2B C 0.2706(6) 0.0496(5) 0.9372(6) 0.0600(14) Uani 1 1 d . . .
H2BA H 0.2188 0.1217 0.9481 0.072 Uiso 1 1 calc R . .
H2BB H 0.3371 0.0559 0.9716 0.072 Uiso 1 1 calc R . .
H2BC H 0.2060 -0.0191 0.9858 0.072 Uiso 1 1 calc R . .
C2C C 0.4301(6) -0.0761(5) 0.7716(7) 0.0641(16) Uani 1 1 d . . .
H2CA H 0.3689 -0.1444 0.8281 0.077 Uiso 1 1 calc R . .
H2CB H 0.5053 -0.0658 0.7942 0.077 Uiso 1 1 calc R . .
H2CC H 0.4694 -0.0894 0.6789 0.077 Uiso 1 1 calc R . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
I1 0.01577(12) 0.02756(13) 0.01741(14) -0.00573(9) -0.00574(10) 0.00086(8)
I2 0.02162(13) 0.02858(14) 0.02239(15) -0.00415(10) -0.00593(11) 0.00300(9)
O11 0.0329(13) 0.0274(13) 0.0230(14) 0.0009(11) -0.0083(11) 0.0006(10)
O12 0.0166(11) 0.0393(14) 0.0254(14) -0.0101(11) -0.0097(10) 0.0031(10)
O13 0.0226(12) 0.0555(17) 0.0270(15) -0.0194(13) -0.0126(12) 0.0099(12)
O14 0.0208(12) 0.0491(16) 0.0352(16) -0.0182(13) -0.0167(12) 0.0110(11)
O21 0.0227(13) 0.0392(15) 0.0432(18) 0.0009(13) -0.0139(13) 0.0015(11)
O22 0.0422(16) 0.0511(17) 0.0195(15) -0.0070(13) -0.0007(13) 0.0106(13)
O23 0.0382(15) 0.0305(14) 0.0485(19) -0.0099(13) -0.0238(14) 0.0068(11)
O24 0.0422(16) 0.0335(15) 0.058(2) -0.0115(14) -0.0293(16) 0.0089(12)
C10 0.0164(15) 0.0276(17) 0.0179(17) -0.0060(14) -0.0033(14) 0.0006(13)
C11 0.0171(16) 0.041(2) 0.0224(19) -0.0049(16) -0.0087(14) -0.0002(14)
C12 0.0268(18) 0.043(2) 0.025(2) -0.0068(17) -0.0138(16) -0.0014(16)
C13 0.0286(18) 0.0335(19) 0.0196(19) -0.0079(15) -0.0045(16) 0.0026(15)
C14 0.0190(15) 0.0286(17) 0.0248(19) -0.0077(15) -0.0063(15) 0.0037(13)
C15 0.0187(15) 0.0234(16) 0.0196(18) -0.0029(13) -0.0063(14) -0.0003(12)
C16 0.0213(17) 0.0301(18) 0.031(2) -0.0075(16) -0.0120(16) 0.0033(14)
C17 0.031(2) 0.048(2) 0.035(2) -0.0081(19) -0.0202(18) 0.0023(17)
C1A 0.050(3) 0.055(3) 0.044(3) -0.002(2) -0.029(2) -0.013(2)
C1B 0.041(2) 0.048(2) 0.048(3) -0.006(2) -0.025(2) 0.0049(19)
C1C 0.027(2) 0.101(4) 0.051(3) -0.019(3) -0.023(2) 0.013(2)
C20 0.0283(18) 0.0306(19) 0.025(2) -0.0038(15) -0.0089(16) -0.0023(15)
C21 0.031(2) 0.047(2) 0.035(2) -0.0061(19) -0.0112(18) -0.0025(17)
C22 0.046(2) 0.053(3) 0.043(3) -0.004(2) -0.020(2) -0.017(2)
C23 0.059(3) 0.031(2) 0.046(3) -0.0069(19) -0.024(2) -0.009(2)
C24 0.046(2) 0.032(2) 0.042(3) -0.0086(18) -0.018(2) 0.0035(17)
C25 0.0332(19) 0.0319(19) 0.031(2) -0.0033(16) -0.0128(17) -0.0012(15)
C26 0.037(2) 0.030(2) 0.032(2) -0.0041(17) -0.0155(18) 0.0018(16)
C27 0.047(2) 0.037(2) 0.055(3) -0.002(2) -0.031(2) 0.0011(18)
C2A 0.042(3) 0.053(3) 0.075(4) 0.001(3) -0.026(3) -0.003(2)
C2B 0.080(4) 0.052(3) 0.059(4) 0.004(3) -0.043(3) -0.004(3)
C2C 0.066(3) 0.048(3) 0.102(5) -0.011(3) -0.059(4) 0.015(2)

_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 O11 1.804(2) . ?
I1 O12 1.816(2) . ?
I1 C10 2.132(3) . ?
I1 O13 2.688(2) . ?
I1 O12 2.698(2) 2_566 ?
I1 O21 2.710(3) 2_566 ?
I2 O22 1.781(3) . ?
I2 O21 1.811(3) . ?
I2 C20 2.127(4) . ?
I2 O23 2.673(3) . ?
I2 O11 2.838(3) . ?
I2 O12 3.021(3) 2_566 ?
O13 C16 1.215(4) . ?
O14 C16 1.328(4) . ?
O14 C17 1.485(4) . ?
O23 C26 1.221(5) . ?
O24 C26 1.322(5) . ?
O24 C27 1.492(5) . ?
C10 C11 1.385(5) . ?
C10 C15 1.387(5) . ?
C11 C12 1.383(5) . ?
C12 C13 1.385(5) . ?
C13 C14 1.372(5) . ?
C14 C15 1.404(5) . ?
C15 C16 1.488(5) . ?
C17 C1B 1.499(6) . ?
C17 C1A 1.502(6) . ?
C17 C1C 1.528(6) . ?
C20 C21 1.376(5) . ?
C20 C25 1.398(5) . ?
C21 C22 1.406(6) . ?
C22 C23 1.367(7) . ?
C23 C24 1.384(6) . ?
C24 C25 1.390(5) . ?
C25 C26 1.496(5) . ?
C27 C2A 1.506(6) . ?
C27 C2B 1.509(7) . ?
C27 C2C 1.520(6) . ?

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
O11 I1 O12 100.73(12) . . ?
O11 I1 C10 96.63(12) . . ?
O12 I1 C10 93.64(12) . . ?
O11 I1 O13 87.23(10) . . ?
O12 I1 O13 163.10(10) . . ?
C10 I1 O13 70.48(11) . . ?
O11 I1 O12 87.36(10) . 2_566 ?
O12 I1 O12 76.86(11) . 2_566 ?
C10 I1 O12 170.26(11) . 2_566 ?
O13 I1 O12 118.72(8) . 2_566 ?
O11 I1 O21 175.93(10) . 2_566 ?
O12 I1 O21 78.67(10) . 2_566 ?
C10 I1 O21 87.43(11) . 2_566 ?
O13 I1 O21 94.41(8) . 2_566 ?
O12 I1 O21 88.58(8) 2_566 2_566 ?
O22 I2 O21 102.04(13) . . ?
O22 I2 C20 99.69(14) . . ?
O21 I2 C20 94.80(14) . . ?
O22 I2 O23 85.84(12) . . ?
O21 I2 O23 164.87(11) . . ?
C20 I2 O23 70.97(12) . . ?
O22 I2 O11 163.55(11) . . ?
O21 I2 O11 94.40(11) . . ?
C20 I2 O11 78.20(11) . . ?
O23 I2 O11 78.03(8) . . ?
O22 I2 O12 120.62(11) . 2_566 ?
O21 I2 O12 70.23(10) . 2_566 ?
C20 I2 O12 138.79(12) . 2_566 ?
O23 I2 O12 116.98(7) . 2_566 ?
O11 I2 O12 65.55(7) . 2_566 ?
I1 O11 I2 118.01(11) . . ?
C16 O13 I1 107.0(2) . . ?
C16 O14 C17 122.5(3) . . ?
C26 O23 I2 107.6(2) . . ?
C26 O24 C27 121.5(3) . . ?
C11 C10 C15 121.8(3) . . ?
C11 C10 I1 117.3(2) . . ?
C15 C10 I1 120.9(3) . . ?
C12 C11 C10 118.6(3) . . ?
C11 C12 C13 120.5(3) . . ?
C14 C13 C12 120.9(3) . . ?
C13 C14 C15 119.6(3) . . ?
C10 C15 C14 118.7(3) . . ?
C10 C15 C16 119.3(3) . . ?
C14 C15 C16 122.0(3) . . ?
O13 C16 O14 126.0(3) . . ?
O13 C16 C15 122.1(3) . . ?
O14 C16 C15 111.9(3) . . ?
O14 C17 C1B 109.4(3) . . ?
O14 C17 C1A 110.6(3) . . ?
C1B C17 C1A 112.8(4) . . ?
O14 C17 C1C 101.8(3) . . ?
C1B C17 C1C 112.0(4) . . ?
C1A C17 C1C 109.6(4) . . ?
C21 C20 C25 121.7(4) . . ?
C21 C20 I2 117.4(3) . . ?
C25 C20 I2 120.8(3) . . ?
C20 C21 C22 118.2(4) . . ?
C23 C22 C21 120.9(4) . . ?
C22 C23 C24 120.3(4) . . ?
C23 C24 C25 120.3(4) . . ?
C24 C25 C20 118.6(4) . . ?
C24 C25 C26 122.3(4) . . ?
C20 C25 C26 119.1(3) . . ?
O23 C26 O24 125.7(4) . . ?
O23 C26 C25 121.5(4) . . ?
O24 C26 C25 112.7(3) . . ?
O24 C27 C2A 109.5(4) . . ?
O24 C27 C2B 108.8(4) . . ?
C2A C27 C2B 113.7(4) . . ?
O24 C27 C2C 102.7(4) . . ?
C2A C27 C2C 110.5(4) . . ?
C2B C27 C2C 111.0(4) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O12 I1 O11 I2 -73.52(14) . . . . ?
C10 I1 O11 I2 -168.52(13) . . . . ?
O13 I1 O11 I2 121.51(12) . . . . ?
O12 I1 O11 I2 2.57(11) 2_566 . . . ?
O21 I1 O11 I2 7.6(15) 2_566 . . . ?
O22 I2 O11 I1 -118.4(4) . . . . ?
O21 I2 O11 I1 63.43(15) . . . . ?
C20 I2 O11 I1 157.42(17) . . . . ?
O23 I2 O11 I1 -129.81(14) . . . . ?
O12 I2 O11 I1 -2.52(11) 2_566 . . . ?
O11 I1 O13 C16 93.6(3) . . . . ?
O12 I1 O13 C16 -25.2(5) . . . . ?
C10 I1 O13 C16 -4.5(3) . . . . ?
O12 I1 O13 C16 179.1(2) 2_566 . . . ?
O21 I1 O13 C16 -90.1(3) 2_566 . . . ?
O22 I2 O23 C26 102.8(3) . . . . ?
O21 I2 O23 C26 -19.4(6) . . . . ?
C20 I2 O23 C26 1.0(3) . . . . ?
O11 I2 O23 C26 -80.5(3) . . . . ?
O12 I2 O23 C26 -134.8(3) 2_566 . . . ?
O11 I1 C10 C11 97.0(3) . . . . ?
O12 I1 C10 C11 -4.2(3) . . . . ?
O13 I1 C10 C11 -178.3(3) . . . . ?
O12 I1 C10 C11 -16.8(8) 2_566 . . . ?
O21 I1 C10 C11 -82.7(3) 2_566 . . . ?
O11 I1 C10 C15 -79.7(3) . . . . ?
O12 I1 C10 C15 179.0(3) . . . . ?
O13 I1 C10 C15 4.9(3) . . . . ?
O12 I1 C10 C15 166.4(5) 2_566 . . . ?
O21 I1 C10 C15 100.5(3) 2_566 . . . ?
C15 C10 C11 C12 1.0(5) . . . . ?
I1 C10 C11 C12 -175.8(3) . . . . ?
C10 C11 C12 C13 -0.4(6) . . . . ?
C11 C12 C13 C14 -0.6(6) . . . . ?
C12 C13 C14 C15 1.1(6) . . . . ?
C11 C10 C15 C14 -0.5(5) . . . . ?
I1 C10 C15 C14 176.1(2) . . . . ?
C11 C10 C15 C16 177.9(3) . . . . ?
I1 C10 C15 C16 -5.5(4) . . . . ?
C13 C14 C15 C10 -0.5(5) . . . . ?
C13 C14 C15 C16 -178.9(3) . . . . ?
I1 O13 C16 O14 -178.3(3) . . . . ?
I1 O13 C16 C15 3.4(4) . . . . ?
C17 O14 C16 O13 2.9(6) . . . . ?
C17 O14 C16 C15 -178.7(3) . . . . ?
C10 C15 C16 O13 0.4(5) . . . . ?
C14 C15 C16 O13 178.7(4) . . . . ?
C10 C15 C16 O14 -178.1(3) . . . . ?
C14 C15 C16 O14 0.3(5) . . . . ?
C16 O14 C17 C1B 62.1(5) . . . . ?
C16 O14 C17 C1A -62.8(5) . . . . ?
C16 O14 C17 C1C -179.2(4) . . . . ?
O22 I2 C20 C21 94.9(3) . . . . ?
O21 I2 C20 C21 -8.2(3) . . . . ?
O23 I2 C20 C21 177.1(3) . . . . ?
O11 I2 C20 C21 -101.7(3) . . . . ?
O12 I2 C20 C21 -73.4(3) 2_566 . . . ?
O22 I2 C20 C25 -82.0(3) . . . . ?
O21 I2 C20 C25 174.9(3) . . . . ?
O23 I2 C20 C25 0.1(3) . . . . ?
O11 I2 C20 C25 81.4(3) . . . . ?
O12 I2 C20 C25 109.7(3) 2_566 . . . ?
C25 C20 C21 C22 -0.5(6) . . . . ?
I2 C20 C21 C22 -177.4(3) . . . . ?
C20 C21 C22 C23 -0.9(7) . . . . ?
C21 C22 C23 C24 0.8(7) . . . . ?
C22 C23 C24 C25 0.6(7) . . . . ?
C23 C24 C25 C20 -1.9(6) . . . . ?
C23 C24 C25 C26 177.9(4) . . . . ?
C21 C20 C25 C24 1.8(6) . . . . ?
I2 C20 C25 C24 178.6(3) . . . . ?
C21 C20 C25 C26 -178.0(4) . . . . ?
I2 C20 C25 C26 -1.2(5) . . . . ?
I2 O23 C26 O24 178.8(3) . . . . ?
I2 O23 C26 C25 -2.0(5) . . . . ?
C27 O24 C26 O23 5.4(7) . . . . ?
C27 O24 C26 C25 -173.9(4) . . . . ?
C24 C25 C26 O23 -177.5(4) . . . . ?
C20 C25 C26 O23 2.3(6) . . . . ?
C24 C25 C26 O24 1.9(6) . . . . ?
C20 C25 C26 O24 -178.3(4) . . . . ?
C26 O24 C27 C2A -63.5(5) . . . . ?
C26 O24 C27 C2B 61.4(5) . . . . ?
C26 O24 C27 C2C 179.1(4) . . . . ?

_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full        26.37
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max         1.911
_refine_diff_density_min         -1.099
_refine_diff_density_rms         0.149