# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2012


data_global
_journal_name_full               Chem.Commun.
_journal_coden_cambridge         0182
_journal_year                    ?
_journal_volume                  ?
_journal_page_first              ?
_publ_contact_author_email       hmc@fjirsm.ac.cn
_publ_contact_author_name        'Maochun Hong  '
_publ_author_name                'Maochun Hong'

data_InOF-1
_database_code_depnum_ccdc_archive 'CCDC 890421'
#TrackingRef '- InOF-1.cif'

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H9 In O7.50'
_chemical_formula_weight         339.97

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'
In In -0.7276 1.3100 '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'

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   I4122

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x+1/2, z+1/4'
'-x, -y, z'
'y, -x+1/2, z+1/4'
'x, -y+1/2, -z+1/4'
'-x, y+1/2, -z+1/4'
'y, x, -z'
'-y, -x, -z'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1, z+3/4'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1, z+3/4'
'x+1/2, -y+1, -z+3/4'
'-x+1/2, y+1, -z+3/4'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'

_cell_length_a                   15.5665(6)
_cell_length_b                   15.5665(6)
_cell_length_c                   12.3201(14)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     2985.4(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    4899
_cell_measurement_theta_min      2.1082
_cell_measurement_theta_max      27.4932

_exptl_crystal_description       block
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.513
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1328
_exptl_absorpt_coefficient_mu    1.600
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.6453
_exptl_absorpt_correction_T_max  0.8564
_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            11697
_diffrn_reflns_av_R_equivalents  0.0241
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.70
_diffrn_reflns_theta_max         27.47
_reflns_number_total             1687
_reflns_number_gt                1617
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_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^)+(0.0310P)^2^+0.5689P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.26(4)
_refine_ls_number_reflns         1687
_refine_ls_number_parameters     67
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0164
_refine_ls_R_factor_gt           0.0156
_refine_ls_wR_factor_ref         0.0480
_refine_ls_wR_factor_gt          0.0475
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_restrained_S_all      1.175
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.250 0.250 -0.015 768 157 ' '
2 0.250 0.750 -0.018 768 157 ' '
_platon_squeeze_details          
;
The calculated free volume of InOF-1 with removal of guest solvent molecules is 48.9% by PLATON (1.8 Angstrom probe radius) where a large region of disordered water molecules exist. We employed PLATON SQUEEZE to calculate the contribution to the contribution to the diffraction from the solvent region and thereby produced a set of solvent-free diffraction intensities. SQUEEZE estimated a total count of 314, which was assigned to be 48 H2O per unit. The final formula was calculated from TGA and with elemental analysis data.
;

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 0.312034(9) 0.312034(9) 0.0000 0.01159(7) Uani 1 2 d S . .
O1 O 0.20853(10) 0.40768(11) 0.00497(17) 0.0237(3) Uani 1 1 d . . .
O2 O 0.11708(13) 0.38895(14) -0.13584(13) 0.0248(4) Uani 1 1 d . . .
O3 O 0.2490(2) 0.2500 0.1250 0.0279(5) Uani 1 2 d S . .
H5A H 0.1926 0.2500 0.1250 0.033 Uiso 1 2 d SR . .
C1 C 0.0000 0.5000 0.1887(3) 0.0240(7) Uani 1 2 d S . .
C2 C 0.06782(17) 0.46332(16) 0.1311(2) 0.0250(6) Uani 1 1 d . . .
H2 H 0.1140 0.4398 0.1687 0.030 Uiso 1 1 calc R . .
C3 C 0.06750(16) 0.46143(15) 0.0185(2) 0.0221(6) Uani 1 1 d . . .
C4 C 0.0000 0.5000 -0.0386(2) 0.0245(7) Uani 1 2 d S . .
H4 H 0.0000 0.5000 -0.1141 0.029 Uiso 1 2 calc SR . .
C5 C 0.13719(16) 0.41598(15) -0.04126(19) 0.0177(5) Uani 1 1 d . . .

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 0.01354(8) 0.01354(8) 0.00769(11) 0.00099(6) -0.00099(6) -0.00009(7)
O1 0.0224(8) 0.0288(8) 0.0198(9) -0.0035(9) -0.0024(9) 0.0108(6)
O2 0.0220(10) 0.0382(12) 0.0141(8) -0.0095(9) -0.0009(8) 0.0125(7)
O3 0.027(2) 0.034(2) 0.0222(10) 0.0183(12) 0.000 0.000
C1 0.032(2) 0.026(2) 0.0135(16) 0.000 0.000 0.0111(13)
C2 0.0285(14) 0.0311(14) 0.0154(12) 0.0004(10) -0.0050(11) 0.0130(13)
C3 0.0240(11) 0.0260(12) 0.0163(14) -0.0019(9) 0.0028(10) 0.0076(10)
C4 0.031(2) 0.031(2) 0.0118(15) 0.000 0.000 0.0115(13)
C5 0.0211(12) 0.0207(12) 0.0113(11) 0.0000(8) -0.0001(8) 0.0067(8)

_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 O3 2.0655(15) . ?
In1 O3 2.0655(15) 10_544 ?
In1 O2 2.1515(15) 4 ?
In1 O2 2.1515(15) 14_544 ?
In1 O1 2.1946(16) . ?
In1 O1 2.1946(16) 7 ?
O1 C5 1.255(3) . ?
O2 C5 1.278(3) . ?
O2 In1 2.1516(15) 10_544 ?
O3 In1 2.0654(15) 4 ?
O3 H5A 0.8781 . ?
C1 C2 1.395(3) 3_565 ?
C1 C2 1.395(3) . ?
C1 C1 1.509(6) 15_455 ?
C2 C3 1.388(4) . ?
C2 H2 0.9300 . ?
C3 C4 1.400(3) . ?
C3 C5 1.490(3) . ?
C4 C3 1.400(3) 3_565 ?
C4 H4 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
O3 In1 O3 96.42(9) . 10_544 ?
O3 In1 O2 90.95(7) . 4 ?
O3 In1 O2 172.35(5) 10_544 4 ?
O3 In1 O2 172.35(5) . 14_544 ?
O3 In1 O2 90.95(7) 10_544 14_544 ?
O2 In1 O2 81.75(9) 4 14_544 ?
O3 In1 O1 87.01(8) . . ?
O3 In1 O1 89.99(8) 10_544 . ?
O2 In1 O1 92.43(8) 4 . ?
O2 In1 O1 90.99(8) 14_544 . ?
O3 In1 O1 89.98(8) . 7 ?
O3 In1 O1 87.01(8) 10_544 7 ?
O2 In1 O1 90.98(8) 4 7 ?
O2 In1 O1 92.43(8) 14_544 7 ?
O1 In1 O1 175.49(9) . 7 ?
C5 O1 In1 134.99(16) . . ?
C5 O2 In1 130.83(16) . 10_544 ?
In1 O3 In1 123.30(16) 4 . ?
In1 O3 H5A 118.4 4 . ?
In1 O3 H5A 118.4 . . ?
C2 C1 C2 118.8(3) 3_565 . ?
C2 C1 C1 120.61(15) 3_565 15_455 ?
C2 C1 C1 120.61(15) . 15_455 ?
C3 C2 C1 121.0(2) . . ?
C3 C2 H2 119.5 . . ?
C1 C2 H2 119.5 . . ?
C2 C3 C4 119.8(2) . . ?
C2 C3 C5 120.1(2) . . ?
C4 C3 C5 120.1(2) . . ?
C3 C4 C3 119.6(3) . 3_565 ?
C3 C4 H4 120.2 . . ?
C3 C4 H4 120.2 3_565 . ?
O1 C5 O2 126.6(2) . . ?
O1 C5 C3 118.0(2) . . ?
O2 C5 C3 115.4(2) . . ?

_diffrn_measured_fraction_theta_max 0.976
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.976
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.078

# start Validation Reply Form

_vrf_CHEMW03_InOF-1              
;
PROBLEM: The ratio of given/expected molecular weight as
calculated from the _atom_site* data lies outside
the range 0.90 <> 1.10
From the CIF: _cell_formula_units_Z 8
From the CIF: _chemical_formula_weight 339.97
TEST: Calculate formula weight from _atom_site_*
atom mass num sum
C 12.01 8.00 96.09
H 1.01 4.00 4.03
In 114.82 1.00 114.82
O 16.00 5.00 79.99
Calculated formula weight 294.93
RESPONSE: The contribution of the disordered water molecules removed
by the SQUEEZE process was included in the overall formula.
;