# Electronic Supplementary Material for CrystEngComm
# This journal is (c) The Royal Society of Chemistry 2009

data_global
_journal_name_full               CrystEngComm

_journal_coden_Cambridge         1350

_publ_contact_author_name        'Maochun Hong'
_publ_contact_author_email       HMC@FJIRSM.AC.CN

_publ_section_title              
;
Double-walled tubular metal-organic frameworks constructed
from bistrand helices
;
loop_
_publ_author_name
'Maochun Hong'
'Lian Chen'
'Qiang Gao'
'Yougui Huang'
'Fei-Long Jiang'
;
Wei Wei
;
'Mingyan Wu'
'Qingfu Zhang'

# Attachment '1.cif'

data_d:\9-4-y6\a
_database_code_depnum_ccdc_archive 'CCDC 719130'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C8 H12 In N O8'
_chemical_formula_sum            'C8 H12 In N O8'
_chemical_formula_weight         365.01

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'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Trigonal
_symmetry_space_group_name_H-M   R-3

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   29.411(10)
_cell_length_b                   29.411(10)
_cell_length_c                   8.116(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     6079(4)
_cell_formula_units_Z            18
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4402
_cell_measurement_theta_min      2.3975
_cell_measurement_theta_max      27.4603

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1500
_exptl_crystal_size_min          0.1200
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.795
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3240
_exptl_absorpt_coefficient_mu    1.779
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8417
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Rigaku Mercury CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15451
_diffrn_reflns_av_R_equivalents  0.0694
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         2.98
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3095
_reflns_number_gt                2479
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 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^)+(0.0516P)^2^+16.9073P] 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         3095
_refine_ls_number_parameters     153
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1078
_refine_ls_wR_factor_gt          0.0994
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.088
_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
In1 In 0.054210(13) 0.377113(13) 0.60115(4) 0.01531(12) Uani 1 1 d . . .
O1 O 0.07682(14) 0.31772(14) 0.6286(4) 0.0230(8) Uani 1 1 d . . .
O2 O 0.06319(14) 0.28222(14) 0.8821(4) 0.0226(8) Uani 1 1 d . . .
O3 O 0.24308(13) 0.27994(14) 0.3076(4) 0.0216(8) Uani 1 1 d . . .
O4 O 0.16026(16) 0.2461(2) 0.2295(5) 0.0514(14) Uani 1 1 d . . .
O5 O 0.01642(13) 0.35387(13) 0.8301(4) 0.0189(7) Uani 1 1 d . . .
O6 O 0.1870(3) 0.1331(3) 0.7690(9) 0.089(2) Uani 1 1 d . . .
O7 O 0.1335(11) 0.1085(11) 0.449(3) 0.479(18) Uiso 1 1 d . . .
H1A H 0.1819 0.2267 1.0114 0.575 Uiso 1 1 d R . .
H1B H 0.2009 0.1998 0.9020 0.575 Uiso 1 1 d R . .
H5 H 0.0016 0.3699 0.8802 0.575 Uiso 1 1 d R . .
H7B H 0.1553 0.1290 0.3732 0.575 Uiso 1 1 d R . .
H7A H 0.1233 0.1282 0.4974 0.575 Uiso 1 1 d R . .
H6A H 0.2112 0.1221 0.7686 0.575 Uiso 1 1 d R . .
H8A H 0.0921 0.0734 0.0001 0.575 Uiso 1 1 d R . .
H8B H 0.1195 0.0675 0.1247 0.575 Uiso 1 1 d R . .
H6B H 0.1786 0.1325 0.6597 0.575 Uiso 1 1 d R . .
O8 O 0.1219(12) 0.0906(13) 0.057(4) 0.478(17) Uiso 1 1 d . . .
N1 N 0.20400(16) 0.22966(17) 0.9328(5) 0.0198(9) Uani 1 1 d . . .
C1 C 0.08590(19) 0.29388(19) 0.7418(6) 0.0172(10) Uani 1 1 d . . .
C2 C 0.12560(18) 0.27746(18) 0.7062(6) 0.0158(10) Uani 1 1 d . . .
C3 C 0.14205(19) 0.2785(2) 0.5467(6) 0.0211(11) Uani 1 1 d . . .
H3 H 0.1279 0.2887 0.4617 0.025 Uiso 1 1 calc R . .
C4 C 0.17943(19) 0.2646(2) 0.5120(6) 0.0187(10) Uani 1 1 d . . .
C5 C 0.1946(2) 0.2630(2) 0.3359(6) 0.0224(11) Uani 1 1 d . . .
C6 C 0.20133(19) 0.2497(2) 0.6407(6) 0.0194(10) Uani 1 1 d . . .
H6 H 0.2277 0.2419 0.6193 0.023 Uiso 1 1 calc R . .
C7 C 0.18309(18) 0.24689(19) 0.7994(6) 0.0165(10) Uani 1 1 d . . .
C8 C 0.14536(19) 0.2604(2) 0.8338(6) 0.0192(10) Uani 1 1 d . . .
H8 H 0.1332 0.2581 0.9409 0.023 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
In1 0.01683(19) 0.0184(2) 0.01183(19) 0.00147(13) 0.00028(13) 0.00970(15)
O1 0.027(2) 0.029(2) 0.020(2) 0.0058(15) 0.0022(15) 0.0196(17)
O2 0.0236(19) 0.032(2) 0.0172(19) 0.0032(15) 0.0039(15) 0.0173(17)
O3 0.0211(18) 0.032(2) 0.0136(18) -0.0006(15) 0.0044(14) 0.0150(16)
O4 0.028(2) 0.108(4) 0.015(2) -0.008(2) -0.0040(17) 0.032(3)
O5 0.0259(19) 0.0185(18) 0.0124(17) 0.0034(13) 0.0026(14) 0.0113(15)
O6 0.102(5) 0.074(4) 0.124(6) -0.030(4) -0.025(4) 0.068(4)
N1 0.020(2) 0.023(2) 0.017(2) 0.0022(17) -0.0043(17) 0.0115(19)
C1 0.017(2) 0.018(2) 0.014(3) -0.0006(19) 0.0034(18) 0.006(2)
C2 0.013(2) 0.017(2) 0.017(3) 0.0027(18) 0.0009(18) 0.0077(19)
C3 0.020(3) 0.028(3) 0.019(3) 0.001(2) -0.002(2) 0.014(2)
C4 0.018(2) 0.028(3) 0.011(2) -0.0001(19) 0.0012(18) 0.012(2)
C5 0.022(3) 0.040(3) 0.012(2) 0.001(2) 0.004(2) 0.021(2)
C6 0.017(2) 0.026(3) 0.016(3) -0.002(2) 0.0015(19) 0.012(2)
C7 0.012(2) 0.018(2) 0.017(3) -0.0020(19) -0.0009(18) 0.006(2)
C8 0.020(3) 0.025(3) 0.012(2) 0.0041(19) 0.0038(19) 0.011(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
In1 O5 2.096(3) . ?
In1 O5 2.107(3) 8_554 ?
In1 O2 2.163(3) 8_554 ?
In1 O1 2.169(3) . ?
In1 O3 2.183(3) 16 ?
In1 N1 2.292(4) 16_556 ?
O1 C1 1.263(6) . ?
O2 C1 1.277(6) . ?
O2 In1 2.164(3) 6_455 ?
O3 C5 1.273(6) . ?
O3 In1 2.183(3) 16 ?
O4 C5 1.230(6) . ?
O5 In1 2.107(3) 6_455 ?
O5 H5 0.8856 . ?
O6 H6A 0.9140 . ?
O6 H6B 0.9186 . ?
O7 H7B 0.8730 . ?
O7 H7A 0.8693 . ?
O8 H8A 0.8908 . ?
O8 H8B 0.8488 . ?
N1 C7 1.456(6) . ?
N1 In1 2.292(4) 16_556 ?
N1 H1A 0.8836 . ?
N1 H1B 0.8717 . ?
C1 C2 1.498(7) . ?
C2 C3 1.376(7) . ?
C2 C8 1.398(7) . ?
C3 C4 1.381(7) . ?
C3 H3 0.9300 . ?
C4 C6 1.407(7) . ?
C4 C5 1.505(7) . ?
C6 C7 1.381(7) . ?
C6 H6 0.9300 . ?
C7 C8 1.381(7) . ?
C8 H8 0.9300 . ?

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
O5 In1 O5 86.13(9) . 8_554 ?
O5 In1 O2 102.55(13) . 8_554 ?
O5 In1 O2 91.83(13) 8_554 8_554 ?
O5 In1 O1 88.42(13) . . ?
O5 In1 O1 98.07(14) 8_554 . ?
O2 In1 O1 165.73(14) 8_554 . ?
O5 In1 O3 169.73(13) . 16 ?
O5 In1 O3 90.07(13) 8_554 16 ?
O2 In1 O3 87.09(13) 8_554 16 ?
O1 In1 O3 82.66(13) . 16 ?
O5 In1 N1 89.11(14) . 16_556 ?
O5 In1 N1 170.27(14) 8_554 16_556 ?
O2 In1 N1 80.91(14) 8_554 16_556 ?
O1 In1 N1 90.27(14) . 16_556 ?
O3 In1 N1 95.99(14) 16 16_556 ?
C1 O1 In1 139.2(3) . . ?
C1 O2 In1 124.4(3) . 6_455 ?
C5 O3 In1 126.1(3) . 16 ?
In1 O5 In1 123.90(16) . 6_455 ?
In1 O5 H5 123.7 . . ?
In1 O5 H5 110.1 6_455 . ?
H6A O6 H6B 104.0 . . ?
H7B O7 H7A 103.8 . . ?
H8A O8 H8B 102.4 . . ?
C7 N1 In1 119.6(3) . 16_556 ?
C7 N1 H1A 98.7 . . ?
In1 N1 H1A 96.6 16_556 . ?
C7 N1 H1B 106.7 . . ?
In1 N1 H1B 118.9 16_556 . ?
H1A N1 H1B 114.1 . . ?
O1 C1 O2 124.8(4) . . ?
O1 C1 C2 117.0(4) . . ?
O2 C1 C2 118.2(4) . . ?
C3 C2 C8 120.0(4) . . ?
C3 C2 C1 119.7(4) . . ?
C8 C2 C1 120.2(4) . . ?
C2 C3 C4 120.5(5) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C3 C4 C6 119.8(4) . . ?
C3 C4 C5 119.8(4) . . ?
C6 C4 C5 120.4(4) . . ?
O4 C5 O3 124.4(5) . . ?
O4 C5 C4 118.8(4) . . ?
O3 C5 C4 116.8(4) . . ?
C7 C6 C4 119.1(5) . . ?
C7 C6 H6 120.4 . . ?
C4 C6 H6 120.4 . . ?
C8 C7 C6 121.0(5) . . ?
C8 C7 N1 119.3(4) . . ?
C6 C7 N1 119.7(4) . . ?
C7 C8 C2 119.4(4) . . ?
C7 C8 H8 120.3 . . ?
C2 C8 H8 120.3 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1A O4 0.88 2.06 2.882(6) 155.4 1_556
O5 H5 O3 0.89 2.01 2.820(5) 152.3 14_456
N1 H1B O6 0.87 2.10 2.945(7) 164.7 .
O6 H6B O7 0.92 2.06 2.94(3) 158.3 .
O6 H6A O4 0.91 1.81 2.713(7) 167.1 11_556

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         2.618
_refine_diff_density_min         -0.762
_refine_diff_density_rms         0.156

# Attachment '2.CIF'

data_d:\data\10-20-f\10-20-f\1a
_database_code_depnum_ccdc_archive 'CCDC 719131'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C16 H16 In2 O19 S2'
_chemical_formula_sum            'C16 H16 In2 O19 S2'
_chemical_formula_weight         806.05

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'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           trigonal
_symmetry_space_group_name_H-M   R-3m

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x-y, -y, -z'
'-x, -x+y, -z'
'y, x, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'y+1/3, x+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+y, y, z'
'x, x-y, z'
'-y, -x, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
'-y+1/3, -x+2/3, z+2/3'

_cell_length_a                   27.652(5)
_cell_length_b                   27.652(5)
_cell_length_c                   20.028(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_volume                     13262(7)
_cell_formula_units_Z            18
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9073
_cell_measurement_theta_min      2.2040
_cell_measurement_theta_max      27.4835

_exptl_crystal_description       Prism
_exptl_crystal_colour            White
_exptl_crystal_size_max          0.2000
_exptl_crystal_size_mid          0.1000
_exptl_crystal_size_min          0.0800
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.817
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7092
_exptl_absorpt_coefficient_mu    1.783
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8750
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      293(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  'Rigaku Mercury CCD area-detector'
_diffrn_measurement_method       \w
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            28198
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.20
_diffrn_reflns_theta_max         24.99
_reflns_number_total             2760
_reflns_number_gt                2479
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku, 2000)'
_computing_cell_refinement       CrystalClear
_computing_data_reduction        CrystalClear
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 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^)+(0.1173P)^2^+165.6475P] 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         2760
_refine_ls_number_parameters     216
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0600
_refine_ls_wR_factor_ref         0.1820
_refine_ls_wR_factor_gt          0.1757
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.68892(3) 0.68892(3) 0.5000 0.0301(3) Uani 1 2 d S . .
In2 In 0.63099(3) 0.6667 0.6667 0.0286(3) Uani 1 2 d S . .
S1 S 0.87472(9) 0.74944(19) 0.83776(16) 0.0629(11) Uani 1 2 d S . .
S2 S 0.58633(8) 0.41367(8) 0.41313(18) 0.0389(13) Uani 0.783(12) 2 d SP A 1
S21 S 0.6031(3) 0.3969(3) 0.4517(7) 0.0389(13) Uani 0.22 2 d SP A 2
OW1 O 0.73637(17) 0.26363(17) 0.4137(4) 0.050(2) Uani 1 2 d S . .
O1 O 0.5522(3) 0.6667 0.6667 0.061(2) Uani 1 2 d S . .
O2 O 0.7654(2) 0.7158(2) 0.5533(3) 0.0466(13) Uani 1 1 d . . .
O3 O 0.5867(2) 0.58799(19) 0.6167(2) 0.0346(11) Uani 1 1 d . . .
O4 O 0.6543(2) 0.7122(2) 0.5777(2) 0.0374(12) Uani 1 1 d . . .
O5 O 0.65299(18) 0.60344(19) 0.5422(2) 0.0310(11) Uani 1 1 d . . .
O6 O 0.7173(4) 0.6818(4) 0.6571(5) 0.026(3) Uani 0.462(14) 1 d PD . 1
O7 O 0.7825(6) 0.7645(7) 0.6099(8) 0.225(18) Uani 0.538(14) 1 d PD . 2
O8 O 0.725(2) 0.823(2) 0.5867(10) 0.26(3) Uani 0.50 1 d P . .
O11 O 0.6437(6) 0.4551(7) 0.4038(9) 0.069(4) Uani 0.50 1 d P . .
O12 O 0.5735(7) 0.3571(8) 0.4320(12) 0.101(7) Uani 0.50 1 d P . .
O13 O 0.5557(6) 0.4077(9) 0.3544(8) 0.119(8) Uani 0.50 1 d P . .
O21 O 0.8447(4) 0.6894(7) 0.8623(7) 0.180(10) Uani 1 2 d S . .
O22 O 0.9284(3) 0.7676(4) 0.8589(4) 0.098(3) Uani 1 1 d . . .
C1 C 0.8290(5) 0.7426(6) 0.7135(5) 0.088(4) Uani 1 1 d . . .
H1 H 0.8024 0.7474 0.7361 0.106 Uiso 1 1 calc R . .
C2 C 0.8728(2) 0.7457(5) 0.7480(6) 0.040(3) Uani 1 2 d S . .
C3 C 0.5957(3) 0.4921(3) 0.5025(4) 0.0418(19) Uani 1 1 d . A .
H3 H 0.6323 0.5136 0.4879 0.050 Uiso 1 1 calc R . .
C4 C 0.6072(3) 0.5725(3) 0.5711(3) 0.0267(14) Uani 1 1 d . . .
C5 C 0.5737(3) 0.5130(3) 0.5491(3) 0.0273(14) Uani 1 1 d . . .
C6 C 0.51979(18) 0.48021(18) 0.5724(4) 0.0237(18) Uani 1 2 d S . .
H6 H 0.5055 0.4945 0.6038 0.028 Uiso 1 2 calc SR . .
C7 C 0.8232(5) 0.7324(6) 0.6458(5) 0.086(4) Uani 1 1 d D . .
C8 C 0.5616(3) 0.4384(3) 0.4782(6) 0.046(3) Uani 1 2 d S . .
C9 C 0.8645(2) 0.7291(5) 0.6124(6) 0.044(3) Uani 1 2 d S . .
H9 H 0.8623 0.7245 0.5663 0.053 Uiso 1 2 calc SR . .
C11 C 0.7618(5) 0.7073(6) 0.6196(6) 0.094(4) Uiso 1 1 d D . .
H1A H 0.5478 0.6788 0.6315 0.113 Uiso 1 1 d R . .
H1B H 0.5187 0.6288 0.6684 0.113 Uiso 1 1 d R . .
H4 H 0.6353 0.7244 0.5616 0.113 Uiso 1 1 d 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
In1 0.0306(4) 0.0306(4) 0.0254(4) -0.00248(13) 0.00248(13) 0.0125(3)
In2 0.0281(3) 0.0289(4) 0.0291(4) -0.0086(3) -0.00430(13) 0.0145(2)
S1 0.0557(13) 0.107(3) 0.0429(17) -0.0398(18) -0.0199(9) 0.0537(15)
S2 0.0294(15) 0.0294(15) 0.048(2) -0.0115(7) 0.0115(7) 0.0070(14)
S21 0.0294(15) 0.0294(15) 0.048(2) -0.0115(7) 0.0115(7) 0.0070(14)
OW1 0.023(2) 0.023(2) 0.078(6) -0.023(2) 0.023(2) -0.009(3)
O1 0.047(3) 0.080(7) 0.066(6) -0.010(5) -0.005(2) 0.040(3)
O2 0.052(3) 0.048(3) 0.037(3) -0.013(2) -0.018(3) 0.023(3)
O3 0.033(3) 0.026(2) 0.035(3) -0.008(2) 0.002(2) 0.008(2)
O4 0.044(3) 0.033(3) 0.035(3) -0.003(2) 0.009(2) 0.019(2)
O5 0.022(2) 0.023(2) 0.041(3) -0.001(2) 0.001(2) 0.0055(19)
O6 0.017(5) 0.036(8) 0.021(6) 0.000(5) 0.000(4) 0.010(5)
O7 0.073(11) 0.24(2) 0.103(13) 0.120(15) -0.075(10) -0.120(14)
O8 0.52(6) 0.50(6) 0.091(15) 0.03(2) 0.02(2) 0.50(6)
O11 0.030(7) 0.055(9) 0.097(12) -0.016(9) 0.012(7) 0.002(7)
O12 0.047(9) 0.084(13) 0.17(2) -0.058(13) 0.026(11) 0.033(10)
O13 0.061(9) 0.146(17) 0.082(11) -0.071(11) 0.008(8) 0.001(10)
O21 0.30(2) 0.104(12) 0.068(9) 0.008(8) 0.004(4) 0.052(6)
O22 0.068(5) 0.160(9) 0.058(4) -0.023(5) -0.017(4) 0.053(6)
C1 0.082(8) 0.180(13) 0.054(6) -0.061(7) -0.036(5) 0.104(9)
C2 0.031(4) 0.050(6) 0.047(6) -0.023(5) -0.011(3) 0.025(3)
C3 0.030(4) 0.033(4) 0.040(4) -0.012(3) 0.011(3) -0.002(3)
C4 0.030(4) 0.027(3) 0.022(3) -0.004(3) -0.006(3) 0.013(3)
C5 0.030(3) 0.026(3) 0.019(3) -0.002(3) -0.004(3) 0.009(3)
C6 0.027(3) 0.027(3) 0.019(4) -0.0008(17) 0.0008(17) 0.016(4)
C7 0.093(8) 0.168(12) 0.051(6) -0.050(7) -0.034(6) 0.106(9)
C8 0.034(4) 0.034(4) 0.049(6) -0.016(3) 0.016(3) 0.002(5)
C9 0.049(5) 0.047(6) 0.036(6) -0.010(5) -0.005(2) 0.023(3)

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In1 O4 2.090(5) . ?
In1 O4 2.090(5) 6_556 ?
In1 O2 2.144(5) . ?
In1 O2 2.144(5) 6_556 ?
In1 O5 2.222(5) 6_556 ?
In1 O5 2.222(5) . ?
In2 O4 2.090(5) 10_566 ?
In2 O4 2.090(5) . ?
In2 O3 2.138(4) 10_566 ?
In2 O3 2.138(4) . ?
In2 O1 2.179(8) . ?
In2 O6 2.215(9) 10_566 ?
In2 O6 2.215(9) . ?
S1 O22 1.374(8) . ?
S1 O22 1.374(8) 22_655 ?
S1 O21 1.520(17) . ?
S1 C2 1.800(12) . ?
S2 O13 1.410(19) . ?
S2 O13 1.410(19) 24_665 ?
S2 O11 1.430(13) 24_665 ?
S2 O11 1.430(13) . ?
S2 O12 1.47(2) 24_665 ?
S2 O12 1.47(2) . ?
S2 C8 1.761(11) . ?
S21 O12 1.066(18) 24_665 ?
S21 O12 1.066(18) . ?
S21 O11 1.721(19) . ?
S21 O11 1.721(19) 24_665 ?
S21 C8 2.056(18) . ?
O1 H1A 0.8152 . ?
O1 H1B 0.9918 . ?
O2 C11 1.342(13) . ?
O2 O7 1.64(2) . ?
O3 C4 1.259(8) . ?
O4 H4 0.8197 . ?
O5 C4 1.259(8) . ?
O6 O6 0.821(17) 10_566 ?
O6 C11 1.308(13) . ?
O7 C11 1.402(17) . ?
O7 C7 1.89(2) . ?
O11 O12 0.96(2) 24_665 ?
O11 O13 1.63(3) 24_665 ?
O12 O11 0.96(2) 24_665 ?
O13 O13 1.01(3) 24_665 ?
O13 O11 1.63(3) 24_665 ?
C1 C2 1.360(11) . ?
C1 C7 1.377(13) . ?
C1 H1 0.9300 . ?
C2 C1 1.360(11) 22_655 ?
C3 C5 1.386(10) . ?
C3 C8 1.390(9) . ?
C3 H3 0.9300 . ?
C4 C5 1.495(9) . ?
C5 C6 1.383(8) . ?
C6 C5 1.383(8) 24_665 ?
C6 H6 0.9300 . ?
C7 C9 1.367(11) . ?
C7 C11 1.568(13) . ?
C8 C3 1.390(9) 24_665 ?
C9 C7 1.367(11) 22_655 ?
C9 H9 0.9300 . ?

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 In1 O4 171.5(3) . 6_556 ?
O4 In1 O2 92.7(2) . . ?
O4 In1 O2 93.0(2) 6_556 . ?
O4 In1 O2 93.0(2) . 6_556 ?
O4 In1 O2 92.7(2) 6_556 6_556 ?
O2 In1 O2 96.3(3) . 6_556 ?
O4 In1 O5 82.66(19) . 6_556 ?
O4 In1 O5 90.88(19) 6_556 6_556 ?
O2 In1 O5 171.46(19) . 6_556 ?
O2 In1 O5 91.07(19) 6_556 6_556 ?
O4 In1 O5 90.88(19) . . ?
O4 In1 O5 82.66(19) 6_556 . ?
O2 In1 O5 91.07(19) . . ?
O2 In1 O5 171.46(19) 6_556 . ?
O5 In1 O5 81.9(2) 6_556 . ?
O4 In2 O4 179.2(3) 10_566 . ?
O4 In2 O3 93.53(19) 10_566 10_566 ?
O4 In2 O3 86.53(19) . 10_566 ?
O4 In2 O3 86.53(19) 10_566 . ?
O4 In2 O3 93.53(19) . . ?
O3 In2 O3 172.7(3) 10_566 . ?
O4 In2 O1 90.42(15) 10_566 . ?
O4 In2 O1 90.42(15) . . ?
O3 In2 O1 86.33(14) 10_566 . ?
O3 In2 O1 86.33(14) . . ?
O4 In2 O6 80.4(3) 10_566 10_566 ?
O4 In2 O6 98.8(3) . 10_566 ?
O3 In2 O6 99.6(3) 10_566 10_566 ?
O3 In2 O6 87.7(3) . 10_566 ?
O1 In2 O6 169.3(2) . 10_566 ?
O4 In2 O6 98.8(3) 10_566 . ?
O4 In2 O6 80.4(3) . . ?
O3 In2 O6 87.7(3) 10_566 . ?
O3 In2 O6 99.6(3) . . ?
O1 In2 O6 169.3(2) . . ?
O6 In2 O6 21.4(5) 10_566 . ?
O22 S1 O22 127.5(8) . 22_655 ?
O22 S1 O21 101.6(5) . . ?
O22 S1 O21 101.6(5) 22_655 . ?
O22 S1 C2 108.9(4) . . ?
O22 S1 C2 108.9(4) 22_655 . ?
O21 S1 C2 106.0(7) . . ?
O13 S2 O13 42.0(15) . 24_665 ?
O13 S2 O11 70.2(10) . 24_665 ?
O13 S2 O11 110.2(11) 24_665 24_665 ?
O13 S2 O11 110.2(11) . . ?
O13 S2 O11 70.2(10) 24_665 . ?
O11 S2 O11 145.5(15) 24_665 . ?
O13 S2 O12 138.3(11) . 24_665 ?
O13 S2 O12 106.2(12) 24_665 24_665 ?
O11 S2 O12 117.8(13) 24_665 24_665 ?
O11 S2 O12 38.8(8) . 24_665 ?
O13 S2 O12 106.2(12) . . ?
O13 S2 O12 138.3(11) 24_665 . ?
O11 S2 O12 38.8(8) 24_665 . ?
O11 S2 O12 117.8(13) . . ?
O12 S2 O12 81.5(15) 24_665 . ?
O13 S2 C8 109.6(9) . . ?
O13 S2 C8 109.6(9) 24_665 . ?
O11 S2 C8 106.0(7) 24_665 . ?
O11 S2 C8 106.0(7) . . ?
O12 S2 C8 106.8(8) 24_665 . ?
O12 S2 C8 106.8(8) . . ?
O12 S21 O12 128(2) 24_665 . ?
O12 S21 O11 30.2(14) 24_665 . ?
O12 S21 O11 124.3(17) . . ?
O12 S21 O11 124.3(17) 24_665 24_665 ?
O12 S21 O11 30.2(14) . 24_665 ?
O11 S21 O11 105.0(14) . 24_665 ?
O12 S21 C8 108.5(12) 24_665 . ?
O12 S21 C8 108.5(12) . . ?
O11 S21 C8 84.7(8) . . ?
O11 S21 C8 84.7(8) 24_665 . ?
In2 O1 H1A 110.8 . . ?
In2 O1 H1B 114.0 . . ?
H1A O1 H1B 102.2 . . ?
C11 O2 O7 55.0(6) . . ?
C11 O2 In1 117.2(6) . . ?
O7 O2 In1 117.3(8) . . ?
C4 O3 In2 124.1(4) . . ?
In2 O4 In1 120.0(3) . . ?
In2 O4 H4 121.0 . . ?
In1 O4 H4 108.7 . . ?
C4 O5 In1 131.4(4) . . ?
O6 O6 C11 133.0(11) 10_566 . ?
O6 O6 In2 79.3(2) 10_566 . ?
C11 O6 In2 141.9(8) . . ?
C11 O7 O2 51.7(10) . . ?
C11 O7 C7 54.5(9) . . ?
O2 O7 C7 82.6(12) . . ?
O12 O11 S2 72.9(16) 24_665 . ?
O12 O11 O13 123(2) 24_665 24_665 ?
S2 O11 O13 54.3(7) . 24_665 ?
O12 O11 S21 33.8(14) 24_665 . ?
S2 O11 S21 40.1(6) . . ?
O13 O11 S21 93.7(9) 24_665 . ?
O11 O12 S21 116(3) 24_665 . ?
O11 O12 S2 68.4(17) 24_665 . ?
S21 O12 S2 49.0(12) . . ?
O13 O13 S2 69.0(8) 24_665 . ?
O13 O13 O11 121.8(8) 24_665 24_665 ?
S2 O13 O11 55.5(10) . 24_665 ?
C2 C1 C7 121.6(9) . . ?
C2 C1 H1 119.2 . . ?
C7 C1 H1 119.2 . . ?
C1 C2 C1 118.4(11) . 22_655 ?
C1 C2 S1 120.7(6) . . ?
C1 C2 S1 120.7(6) 22_655 . ?
C5 C3 C8 118.5(7) . . ?
C5 C3 H3 120.8 . . ?
C8 C3 H3 120.8 . . ?
O3 C4 O5 125.0(6) . . ?
O3 C4 C5 116.9(6) . . ?
O5 C4 C5 118.2(6) . . ?
C6 C5 C3 120.5(6) . . ?
C6 C5 C4 119.6(6) . . ?
C3 C5 C4 119.8(6) . . ?
C5 C6 C5 120.2(8) . 24_665 ?
C5 C6 H6 119.9 . . ?
C5 C6 H6 119.9 24_665 . ?
C9 C7 C1 118.6(9) . . ?
C9 C7 C11 124.3(9) . . ?
C1 C7 C11 114.2(10) . . ?
C9 C7 O7 124.1(11) . . ?
C1 C7 O7 108.4(10) . . ?
C11 C7 O7 46.7(5) . . ?
C3 C8 C3 121.7(10) . 24_665 ?
C3 C8 S2 119.2(5) . . ?
C3 C8 S2 119.2(5) 24_665 . ?
C3 C8 S21 114.7(6) . . ?
C3 C8 S21 114.7(6) 24_665 . ?
S2 C8 S21 32.8(5) . . ?
C7 C9 C7 121.0(11) . 22_655 ?
C7 C9 H9 119.5 . . ?
C7 C9 H9 119.5 22_655 . ?
O6 C11 O2 129.0(11) . . ?
O6 C11 O7 115.5(13) . . ?
O2 C11 O7 73.3(11) . . ?
O6 C11 C7 124.4(11) . . ?
O2 C11 C7 106.5(9) . . ?
O7 C11 C7 78.8(11) . . ?

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
O1 H1A O11 0.82 2.35 2.81(2) 116.5 6_556
O1 H1B O13 0.99 2.74 3.645(19) 152.0 6_556
O4 H4 O22 0.82 2.26 3.063(12) 166.3 36_664

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        24.99
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         2.108
_refine_diff_density_min         -1.612
_refine_diff_density_rms         0.176