# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2008


data_global
_journal_name_full               Chem.Commun.

_journal_coden_Cambridge         0182

_publ_contact_author_name        'M Schroder'
_publ_contact_author_email       M.SCHRODER@NOTTINGHAM.AC.UK

_publ_section_title              
;
Enhancement of H2 Adsorption in Li+-Exchanged
Co-ordination Framework Materials
;
loop_
_publ_author_name
'M Schroder'
'Alexander Blake'
'Neil Champness'
'Peter Hubberstey'
'Xiang Lin.'
;
K.Thomas
;
'Sihai Yang.'

# Attachment 'INHAXD.CIF'

data_INHAXD
_database_code_depnum_ccdc_archive 'CCDC 698649'

#_database_code_depnum_ccdc_archive 'CCDC ??????'
#INHAXD

_refine_special_details          
;

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
1 -0.020 0.000 -0.003 9299.3 1252.2
;

_platon_squeeze_details          
;
Approximately 69% of the unit cell volume comprises a large region of
disordered solvent which could not be modelled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate 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 1252 electrons per unit cell.
The final formula including one dimethylammonium cation, one DMF, one MeCN
and four water molecules per indium complex anion, was calculated from the
SQUEEZE results combined with elemental analysis data.
;

_audit_creation_method           'manual editing of SHELXL97 CIF output'
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'In C16 H6 O8 -, C2 H6 N H2 +, C3 H7 N O, C2 H3 N, 4(H2 O)'
_chemical_formula_sum            'C23 H32 In N3 O13'
_chemical_formula_weight         673.34

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

_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_H-M   'I 41/a c d'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+1/4, x+3/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+1/4, -x+1/4, z+3/4'
'x, -y, -z+1/2'
'y+1/4, x+3/4, -z+3/4'
'-x+1/2, y, -z'
'-y+1/4, -x+1/4, -z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+3/4, x+5/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+3/4, -x+3/4, z+5/4'
'x+1/2, -y+1/2, -z+1'
'y+3/4, x+5/4, -z+5/4'
'-x+1, y+1/2, -z+1/2'
'-y+3/4, -x+3/4, -z+3/4'
'-x, -y, -z'
'y-1/4, -x-3/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-1/4, x-1/4, -z-3/4'
'-x, y, z-1/2'
'-y-1/4, -x-3/4, z-3/4'
'x-1/2, -y, z'
'y-1/4, x-1/4, z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+1/4, -x-1/4, -z+1/4'
'x, y+1/2, -z'
'-y+1/4, x+1/4, -z-1/4'
'-x+1/2, y+1/2, z'
'-y+1/4, -x-1/4, z-1/4'
'x, -y+1/2, z+1/2'
'y+1/4, x+1/4, z+1/4'

_cell_length_a                   19.659(3)
_cell_length_b                   19.659(3)
_cell_length_c                   36.149(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     13971(4)
_cell_formula_units_Z            16
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    989
_cell_measurement_theta_min      2.78
_cell_measurement_theta_max      23.18

_exptl_crystal_description       BLOCK
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3440
_exptl_absorpt_coefficient_mu    0.732
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   'Bruker SADABS'

_exptl_special_details           
;
?
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.6893
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Daresbury SRS station 9.8'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD diffractometer'
_diffrn_measurement_method       'fine-slice \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        5
_diffrn_reflns_number            48568
_diffrn_reflns_av_R_equivalents  0.0666
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_theta_min         2.29
_diffrn_reflns_theta_max         24.22
_reflns_number_total             3088
_reflns_number_gt                2393
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_molecular_graphics    ?
_computing_publication_material  
'enCIFer (Allen et al., 2004); PLATON (Spek, 2003)'

_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^)+(0.0748P)^2^+140.1189P] 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       0.00029(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_number_reflns         3088
_refine_ls_number_parameters     115
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0792
_refine_ls_R_factor_gt           0.0602
_refine_ls_wR_factor_ref         0.183
_refine_ls_wR_factor_gt          0.173
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_restrained_S_all      1.04
_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 0.22141(2) 0.47141(2) 0.1250 0.0392(3) Uani 1 2 d S . .
O1 O 0.2306(3) 0.3506(3) 0.13284(12) 0.0725(16) Uani 1 1 d . . .
O2 O 0.2172(2) 0.3987(2) 0.07975(12) 0.0510(11) Uani 1 1 d . . .
O3 O 0.2761(3) 0.0410(2) 0.07807(14) 0.0600(13) Uani 1 1 d . . .
O4 O 0.2698(3) 0.0903(3) 0.13276(13) 0.0771(17) Uani 1 1 d . . .
C1 C 0.2490(4) 0.2210(3) 0.02035(19) 0.077(2) Uani 1 1 d DU . .
C2 C 0.2592(4) 0.1614(4) 0.04048(19) 0.074(2) Uani 1 1 d DU . .
H2 H 0.2668 0.1198 0.0277 0.088 Uiso 1 1 calc R . .
C3 C 0.2585(4) 0.1616(4) 0.07858(19) 0.067(2) Uani 1 1 d DU . .
C4 C 0.2481(4) 0.2204(3) 0.09825(19) 0.072(2) Uani 1 1 d DU . .
H4 H 0.2481 0.2197 0.1245 0.086 Uiso 1 1 calc R . .
C5 C 0.2374(4) 0.2809(3) 0.07936(19) 0.071(2) Uani 1 1 d DU . .
C6 C 0.2382(4) 0.2810(4) 0.0405(2) 0.083(3) Uani 1 1 d DU . .
H6 H 0.2312 0.3226 0.0276 0.099 Uiso 1 1 calc R . .
C7 C 0.2296(4) 0.3468(4) 0.0986(2) 0.066(2) Uani 1 1 d . . .
C8 C 0.2701(4) 0.0949(4) 0.09757(19) 0.064(2) 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 0.0451(3) 0.0451(3) 0.0275(4) -0.00118(18) 0.00118(18) 0.0012(3)
O1 0.126(5) 0.052(3) 0.040(3) -0.010(2) 0.009(3) 0.017(3)
O2 0.067(3) 0.035(2) 0.051(3) -0.007(2) -0.010(2) 0.009(2)
O3 0.095(4) 0.040(3) 0.046(3) 0.002(2) 0.008(2) -0.004(2)
O4 0.128(5) 0.062(3) 0.042(3) -0.002(2) 0.009(3) 0.006(3)
C1 0.148(8) 0.040(4) 0.042(4) -0.002(3) 0.008(5) -0.001(4)
C2 0.134(7) 0.041(4) 0.045(3) -0.005(3) 0.010(5) 0.006(4)
C3 0.109(6) 0.044(4) 0.047(3) 0.003(3) 0.015(4) 0.004(4)
C4 0.137(7) 0.041(4) 0.038(3) 0.001(3) 0.009(4) 0.005(4)
C5 0.130(7) 0.040(4) 0.044(3) -0.002(3) 0.002(4) 0.020(4)
C6 0.167(9) 0.039(4) 0.043(3) 0.002(3) 0.005(5) 0.008(5)
C7 0.091(6) 0.052(4) 0.056(4) -0.006(4) -0.010(4) -0.007(4)
C8 0.096(6) 0.053(4) 0.043(4) 0.005(3) 0.004(4) 0.005(4)

_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 O2 2.174(4) . ?
In1 O3 2.180(5) 29 ?
In1 O4 2.360(5) 29 ?
In1 O1 2.400(5) . ?
O1 C7 1.241(9) . ?
O2 C7 1.250(9) . ?
O3 C8 1.277(8) . ?
O4 C8 1.275(8) . ?
C1 C2 1.395(10) . ?
C1 C6 1.403(9) . ?
C1 C1 1.472(13) 7 ?
C2 C3 1.377(9) . ?
C2 H2 0.9500 . ?
C3 C4 1.373(9) . ?
C3 C8 1.498(10) . ?
C4 C5 1.387(9) . ?
C4 H4 0.9500 . ?
C5 C6 1.404(10) . ?
C5 C7 1.478(10) . ?
C6 H6 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 In1 O2 121.1(2) . 14_444 ?
O2 In1 O3 128.63(17) . 26_565 ?
O2 In1 O3 80.11(18) . 29 ?
O3 In1 O3 125.2(3) 26_565 29 ?
O2 In1 O4 138.02(16) . 29 ?
O2 In1 O4 89.78(18) . 26_565 ?
O3 In1 O4 57.94(17) 26_565 26_565 ?
O3 In1 O4 80.75(19) 29 26_565 ?
O4 In1 O4 82.5(3) 29 26_565 ?
O2 In1 O1 55.98(15) . . ?
O2 In1 O1 85.58(17) 14_444 . ?
O3 In1 O1 83.31(19) 26_565 . ?
O3 In1 O1 135.37(16) 29 . ?
O4 In1 O1 163.94(18) 29 . ?
O4 In1 O1 90.7(2) 26_565 . ?
O1 In1 O1 99.4(3) 14_444 . ?
C7 O1 In1 86.6(4) . . ?
C7 O2 In1 96.9(4) . . ?
C8 O3 In1 95.3(4) . 20_656 ?
C8 O4 In1 87.2(4) . 20_656 ?
C2 C1 C6 117.2(6) . . ?
C2 C1 C1 121.2(4) . 7 ?
C6 C1 C1 121.6(4) . 7 ?
C3 C2 C1 121.2(7) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C4 C3 C2 121.5(7) . . ?
C4 C3 C8 121.5(6) . . ?
C2 C3 C8 117.0(6) . . ?
C3 C4 C5 119.3(6) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C4 C5 C6 119.5(6) . . ?
C4 C5 C7 122.4(6) . . ?
C6 C5 C7 118.0(6) . . ?
C1 C6 C5 121.3(6) . . ?
C1 C6 H6 119.3 . . ?
C5 C6 H6 119.3 . . ?
O1 C7 O2 119.8(7) . . ?
O1 C7 C5 121.3(7) . . ?
O2 C7 C5 118.7(6) . . ?
O4 C8 O3 119.5(6) . . ?
O4 C8 C3 121.2(7) . . ?
O3 C8 C3 119.1(6) . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        24.22
_diffrn_measured_fraction_theta_full 0.997

_refine_diff_density_max         0.67
_refine_diff_density_min         -0.48
_refine_diff_density_rms         0.09

#===END of CIF