# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_InOF-12
_database_code_depnum_ccdc_archive 'CCDC 1039033'
_audit_update_record             
;
2015-09-09 deposited with the CCDC.
2015-10-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C21.6 H26 In O13'
_chemical_formula_sum            'C16 H6 In O8'
_chemical_formula_weight         441.03

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   P42/mmc

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

_cell_length_a                   9.9843(6)
_cell_length_b                   9.9843(6)
_cell_length_c                   18.2816(18)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     1822.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       prism
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.804
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             430
_exptl_absorpt_coefficient_mu    0.667
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9674
_exptl_absorpt_correction_T_max  0.9738
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(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  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13298
_diffrn_reflns_av_R_equivalents  0.1238
_diffrn_reflns_av_sigmaI/netI    0.0675
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.32
_diffrn_reflns_theta_max         27.50
_reflns_number_total             1200
_reflns_number_gt                912
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1500P)²+0.1967P] where P=(Fo²+2Fc²)/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       0.037(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         1200
_refine_ls_number_parameters     42
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0805
_refine_ls_R_factor_gt           0.0682
_refine_ls_wR_factor_ref         0.2219
_refine_ls_wR_factor_gt          0.2076
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
# SQUEEZE RESULTS (APPEND TO CIF)
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 -0.013 -0.007 -0.008 1225.0 195.7
_platon_squeeze_details          
;
SQUEEZE removed disordered DMA, isolated water molecules and EtOH per formula unit.  This value is calculated based upon volume/count_electrons analysis and TG analyses. 

Specifically, the above reported formulation is fully in accord with the SQUEEZE data where we see that some 190 electrons were removed from the unit-cell contents; equivalent to some 195.7/2 ?Ö 98 electrons per formula unit in this P42/mmc  system with Z = 2. The electron count from the reported disordered 2/3DMA, 3H2O, 4/3EtOH material is 32 + 30 + 36 = 98 electrons.  

See ref: a) CrystEngComm, 2015, 17, 1750-1753
;
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 0.5000 0.5000 0.2500 0.0516(5) Uani 1 8 d S . .
O1 O 0.3578(3) 0.5000 0.15746(19) 0.0794(12) Uani 1 2 d S . .
C4 C 0.0000 0.5000 0.1934(3) 0.0668(18) Uani 1 4 d S . .
H4 H 0.0000 0.5000 0.2454 0.080 Uiso 1 4 calc SR . .
C3 C 0.1200(4) 0.5000 0.1571(2) 0.0631(13) Uani 1 2 d S . .
C1 C 0.0000 0.5000 0.0408(3) 0.0667(18) Uani 1 4 d S . .
C5 C 0.2511(6) 0.5000 0.1965(4) 0.0686(14) Uani 1 2 d S . .
C2 C 0.1203(4) 0.5000 0.0794(3) 0.0673(14) Uani 1 2 d S . .
H2 H 0.2030 0.5000 0.0536 0.081 Uiso 1 2 calc SR . .
O2 O 0.2597(7) 0.5000 0.2631(3) 0.0874(17) Uani 1 2 d S . .


_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 O1 2.208(3) . ?
In1 O1 2.208(3) 10_566 ?
In1 O1 2.208(3) 3_665 ?
In1 O1 2.208(3) 12_656 ?
In1 O2 2.412(7) 12_656 ?
In1 O2 2.412(7) 10_566 ?
In1 O2 2.412(7) . ?
In1 O2 2.412(7) 3_665 ?
In1 C5 2.671(5) 10_566 ?
In1 C5 2.671(5) . ?
In1 C5 2.671(5) 12_656 ?
In1 C5 2.671(5) 3_665 ?
O1 C5 1.283(7) . ?
C4 C3 1.369(5) 3_565 ?
C4 C3 1.369(5) . ?
C4 H4 0.9500 . ?
C3 C2 1.421(6) . ?
C3 C5 1.494(7) . ?
C1 C2 1.393(5) . ?
C1 C2 1.393(5) 3_565 ?
C1 C1 1.491(12) 9_565 ?
C5 O2 1.221(6) . ?
C2 H2 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
O1 In1 O1 125.94(11) . 10_566 ?
O1 In1 O1 79.99(18) . 3_665 ?
O1 In1 O1 125.94(11) 10_566 3_665 ?
O1 In1 O1 125.94(11) . 12_656 ?
O1 In1 O1 79.99(18) 10_566 12_656 ?
O1 In1 O1 125.94(11) 3_665 12_656 ?
O1 In1 O2 85.63(9) . 12_656 ?
O1 In1 O2 135.71(15) 10_566 12_656 ?
O1 In1 O2 85.63(9) 3_665 12_656 ?
O1 In1 O2 55.72(14) 12_656 12_656 ?
O1 In1 O2 85.63(9) . 10_566 ?
O1 In1 O2 55.72(14) 10_566 10_566 ?
O1 In1 O2 85.63(9) 3_665 10_566 ?
O1 In1 O2 135.71(15) 12_656 10_566 ?
O2 In1 O2 168.6(2) 12_656 10_566 ?
O1 In1 O2 55.72(14) . . ?
O1 In1 O2 85.63(9) 10_566 . ?
O1 In1 O2 135.71(15) 3_665 . ?
O1 In1 O2 85.63(9) 12_656 . ?
O2 In1 O2 90.57(2) 12_656 . ?
O2 In1 O2 90.57(2) 10_566 . ?
O1 In1 O2 135.71(15) . 3_665 ?
O1 In1 O2 85.63(9) 10_566 3_665 ?
O1 In1 O2 55.72(14) 3_665 3_665 ?
O1 In1 O2 85.63(9) 12_656 3_665 ?
O2 In1 O2 90.57(2) 12_656 3_665 ?
O2 In1 O2 90.57(2) 10_566 3_665 ?
O2 In1 O2 168.6(2) . 3_665 ?
O1 In1 C5 106.29(11) . 10_566 ?
O1 In1 C5 28.52(16) 10_566 10_566 ?
O1 In1 C5 106.29(11) 3_665 10_566 ?
O1 In1 C5 108.51(18) 12_656 10_566 ?
O2 In1 C5 164.2(2) 12_656 10_566 ?
O2 In1 C5 27.20(14) 10_566 10_566 ?
O2 In1 C5 87.91(4) . 10_566 ?
O2 In1 C5 87.91(4) 3_665 10_566 ?
O1 In1 C5 28.52(16) . . ?
O1 In1 C5 106.29(11) 10_566 . ?
O1 In1 C5 108.51(18) 3_665 . ?
O1 In1 C5 106.29(11) 12_656 . ?
O2 In1 C5 87.91(4) 12_656 . ?
O2 In1 C5 87.91(4) 10_566 . ?
O2 In1 C5 27.20(14) . . ?
O2 In1 C5 164.2(2) 3_665 . ?
C5 In1 C5 97.71(10) 10_566 . ?
O1 In1 C5 106.29(11) . 12_656 ?
O1 In1 C5 108.51(18) 10_566 12_656 ?
O1 In1 C5 106.29(11) 3_665 12_656 ?
O1 In1 C5 28.52(16) 12_656 12_656 ?
O2 In1 C5 27.20(14) 12_656 12_656 ?
O2 In1 C5 164.2(2) 10_566 12_656 ?
O2 In1 C5 87.91(4) . 12_656 ?
O2 In1 C5 87.91(4) 3_665 12_656 ?
C5 In1 C5 137.0(3) 10_566 12_656 ?
C5 In1 C5 97.71(10) . 12_656 ?
O1 In1 C5 108.51(18) . 3_665 ?
O1 In1 C5 106.29(11) 10_566 3_665 ?
O1 In1 C5 28.52(16) 3_665 3_665 ?
O1 In1 C5 106.29(11) 12_656 3_665 ?
O2 In1 C5 87.91(4) 12_656 3_665 ?
O2 In1 C5 87.91(4) 10_566 3_665 ?
O2 In1 C5 164.2(2) . 3_665 ?
O2 In1 C5 27.20(14) 3_665 3_665 ?
C5 In1 C5 97.71(10) 10_566 3_665 ?
C5 In1 C5 137.0(3) . 3_665 ?
C5 In1 C5 97.71(10) 12_656 3_665 ?
C5 O1 In1 96.2(3) . . ?
C3 C4 C3 122.1(6) 3_565 . ?
C3 C4 H4 119.0 3_565 . ?
C3 C4 H4 119.0 . . ?
C4 C3 C2 119.1(4) . . ?
C4 C3 C5 122.2(5) . . ?
C2 C3 C5 118.7(4) . . ?
C2 C1 C2 119.1(6) . 3_565 ?
C2 C1 C1 120.4(3) . 9_565 ?
C2 C1 C1 120.4(3) 3_565 9_565 ?
O2 C5 O1 119.8(6) . . ?
O2 C5 C3 122.8(6) . . ?
O1 C5 C3 117.4(5) . . ?
O2 C5 In1 64.5(4) . . ?
O1 C5 In1 55.3(3) . . ?
C3 C5 In1 172.7(4) . . ?
C1 C2 C3 120.3(4) . . ?
C1 C2 H2 119.9 . . ?
C3 C2 H2 119.9 . . ?
C5 O2 In1 88.3(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.178
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_InOF-13
_database_code_depnum_ccdc_archive 'CCDC 1039034'
_audit_update_record             
;
2015-09-18 deposited with the CCDC.
2015-10-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        InOF-13
_chemical_name_common            InOF-13
_chemical_melting_point          ?
_chemical_formula_moiety         'C23.7 H28.7 In N2.3 O11.3'
_chemical_formula_sum            'C22 H19 In N2 O8'
_chemical_formula_weight         554.22

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In 0.0822 5.0449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   P21212

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

_cell_length_a                   19.72440(10)
_cell_length_b                   17.08140(10)
_cell_length_c                   9.95540(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3354.18(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    6539
_cell_measurement_theta_min      4.4550
_cell_measurement_theta_max      72.5460

_exptl_crystal_description       bulk
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_absorpt_coefficient_mu    5.935
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6482
_exptl_absorpt_correction_T_max  0.8420
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            69475
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0172
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.42
_diffrn_reflns_theta_max         73.54
_reflns_number_total             6764
_reflns_number_gt                6576
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0800P)²+1.3813P] where P=(Fo²+2Fc²)/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   0.005(8)
_refine_ls_number_reflns         6764
_refine_ls_number_parameters     247
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0424
_refine_ls_R_factor_gt           0.0417
_refine_ls_wR_factor_ref         0.1164
_refine_ls_wR_factor_gt          0.1155
_refine_ls_goodness_of_fit_ref   1.134
_refine_ls_restrained_S_all      1.135
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
# SQUEEZE RESULTS (APPEND TO CIF)
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 0.953 0.344 0.500 1557 200.4
_platon_squeeze_details          
;
SQUEEZE removed disordered DEF and isolated water molecules per formula unit.  This value is calculated based upon volume/count_electrons analysis and TG analyses. 

Specifically, the above reported formulation is fully in accord with the SQUEEZE data where we see that some 200.4 electrons were removed from the unit-cell contents; equivalent to some 200.4/4 ?Ö 50 electrons per formula unit in this P21212 system with Z = 4. The electron count from the reported disordered 1/3DEF and 3H2O material is 19 + 30 = 49 electrons.   

See Ref: a) CrystEngComm, 2015, 17, 1750-1753
;

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 0.181279(11) 0.840141(13) 0.91388(3) 0.03748(9) Uani 1 1 d . . .
O1 O 0.29948(14) 0.85524(16) 0.9265(4) 0.0499(7) Uani 1 1 d . . .
O2 O 0.22936(14) 0.95496(16) 0.9302(4) 0.0519(7) Uani 1 1 d . . .
O3 O 0.29863(15) 1.21519(16) 1.0695(4) 0.0488(7) Uani 1 1 d . . .
O4 O 0.40554(17) 1.24392(19) 1.1003(6) 0.0803(13) Uani 1 1 d . . .
O5 O 0.19374(16) 0.8345(2) 0.6838(3) 0.0526(7) Uani 1 1 d . . .
O6 O 0.11067(15) 0.90145(19) 0.7740(3) 0.0465(6) Uani 1 1 d . . .
O7 O 0.1971(2) 0.8341(3) 0.1587(3) 0.0736(7) Uani 1 1 d . . .
O8 O 0.1104(2) 0.8881(3) 0.0619(3) 0.0736(7) Uani 1 1 d . . .
N1 N 0.1100(4) 1.1775(4) 0.8342(7) 0.110(2) Uiso 1 1 d D . .
N2 N 0.0780(6) 1.1294(7) 1.0546(13) 0.213(6) Uiso 1 1 d D . .
H1 H 0.1238 1.1957 0.7505 0.132 Uiso 1 1 calc R . .
H2 H 0.4235 0.9068 0.9517 0.066 Uiso 1 1 calc R . .
H4 H 0.2821 1.0761 1.0078 0.063 Uiso 1 1 calc R . .
H6 H 0.4799 1.1259 1.0654 0.073 Uiso 1 1 calc R . .
H10 H 0.0395 0.9669 0.6140 0.087 Uiso 1 1 calc R . .
H12 H 0.1833 0.8401 0.4175 0.071 Uiso 1 1 calc R . .
H14 H 0.0418 0.9598 0.2082 0.103 Uiso 1 1 calc R . .
C1 C 0.4639(2) 1.0119(3) 1.0096(6) 0.0551(11) Uani 1 1 d . . .
C2 C 0.4124(2) 0.9591(3) 0.9752(6) 0.0551(11) Uani 1 1 d . . .
C3 C 0.3459(2) 0.9828(3) 0.9754(5) 0.0498(10) Uani 1 1 d . . .
C4 C 0.3281(2) 1.0599(3) 1.0083(5) 0.0529(10) Uani 1 1 d . . .
C5 C 0.3796(2) 1.1121(3) 1.0416(5) 0.0554(11) Uani 1 1 d . . .
C6 C 0.4456(2) 1.0892(2) 1.0423(6) 0.0608(13) Uani 1 1 d . . .
C7 C 0.2892(2) 0.9273(2) 0.9391(5) 0.0485(10) Uani 1 1 d . . .
C8 C 0.3603(2) 1.1955(2) 1.0741(6) 0.0535(10) Uani 1 1 d . . .
C9 C 0.0296(3) 0.9736(4) 0.4137(5) 0.0797(17) Uani 1 1 d . . .
C10 C 0.0589(3) 0.9494(4) 0.5320(5) 0.0724(16) Uani 1 1 d . . .
C11 C 0.1161(3) 0.9003(3) 0.5384(5) 0.0576(12) Uani 1 1 d . . .
C12 C 0.1447(3) 0.8734(3) 0.4174(5) 0.0588(11) Uani 1 1 d . . .
C13 C 0.1152(3) 0.8969(4) 0.2994(5) 0.0670(14) Uani 1 1 d . . .
C14 C 0.0599(3) 0.9452(5) 0.2930(5) 0.085(2) Uani 1 1 d . . .
C15 C 0.1422(2) 0.8766(3) 0.6725(4) 0.0490(10) Uani 1 1 d . . .
C16 C 0.1429(4) 0.8703(4) 0.1664(5) 0.0736(7) Uani 1 1 d . . .
H18A H 0.2030 1.2000 0.9134 0.137 Uiso 1 1 calc R . .
H18B H 0.1954 1.1123 0.8579 0.137 Uiso 1 1 calc R . .
C18 C 0.1719(4) 1.1546(5) 0.9073(9) 0.114(3) Uiso 1 1 d D . .
H17A H 0.0338 1.2596 0.8503 0.176 Uiso 1 1 calc R . .
H17B H 0.1050 1.2897 0.9100 0.176 Uiso 1 1 calc R . .
C17 C 0.0745(5) 1.2439(6) 0.9019(12) 0.147(4) Uiso 1 1 d D . .
H19A H 0.0851 1.0710 0.7520 0.209 Uiso 1 1 calc R . .
H19B H 0.0212 1.1294 0.7649 0.209 Uiso 1 1 calc R . .
C19 C 0.0633(6) 1.1112(6) 0.8092(13) 0.174(6) Uiso 1 1 d D . .
H20A H 0.0759 1.2462 1.1106 0.189 Uiso 1 1 calc R . .
H20B H 0.0048 1.2164 1.0513 0.189 Uiso 1 1 calc R . .
C20 C 0.0546(7) 1.2135(6) 1.0402(12) 0.158(5) Uiso 1 1 d D . .
H21A H 0.1743 1.1616 1.1146 0.282 Uiso 1 1 calc R . .
H21B H 0.1706 1.0729 1.0606 0.282 Uiso 1 1 calc R . .
C21 C 0.1539(6) 1.1269(9) 1.0460(13) 0.235(8) Uiso 1 1 d D . .
H22A H -0.0012 1.0759 0.9588 0.234 Uiso 1 1 calc R . .
H22B H 0.0674 1.0258 0.9536 0.234 Uiso 1 1 calc R . .
C22 C 0.0485(7) 1.0794(7) 0.9463(14) 0.195(7) Uiso 1 1 d D . .

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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
In1 O3 2.177(3) 4_547 ?
In1 O2 2.185(3) . ?
In1 O8 2.191(4) 1_556 ?
In1 O6 2.231(3) . ?
In1 O5 2.305(3) . ?
In1 O1 2.349(3) . ?
In1 O4 2.378(3) 4_547 ?
In1 O7 2.459(3) 1_556 ?
In1 C15 2.599(5) . ?
In1 C8 2.605(4) 4_547 ?
In1 C7 2.610(4) . ?
In1 C16 2.675(5) 1_556 ?
O5 C15 1.251(6) . ?
O6 C15 1.260(5) . ?
O2 C7 1.275(5) . ?
O1 C7 1.254(5) . ?
C6 C5 1.360(7) . ?
C6 C1 1.407(6) . ?
C12 C13 1.371(8) . ?
C12 C11 1.407(6) . ?
C2 C3 1.373(6) . ?
C2 C1 1.401(6) . ?
C1 C1 1.480(8) 2_675 ?
C11 C10 1.407(8) . ?
C11 C15 1.487(7) . ?
C3 C4 1.401(6) . ?
C3 C7 1.510(6) . ?
C10 C9 1.376(7) . ?
C13 C14 1.369(9) . ?
C13 C16 1.503(7) . ?
C4 C5 1.392(6) . ?
C5 C8 1.509(6) . ?
C9 C14 1.427(8) . ?
C9 C9 1.475(12) 2_575 ?
O4 C8 1.244(6) . ?
O4 In1 2.378(3) 4_557 ?
C8 O3 1.263(5) . ?
C8 In1 2.605(4) 4_557 ?
O3 In1 2.177(3) 4_557 ?
O8 C16 1.259(8) . ?
O8 In1 2.191(4) 1_554 ?
O7 C16 1.237(8) . ?
O7 In1 2.459(3) 1_554 ?
C16 In1 2.675(5) 1_554 ?
N1 C18 1.474(7) . ?
N1 C19 1.481(8) . ?
N1 C17 1.494(7) . ?
C18 C21 1.502(9) . ?
C17 C20 1.523(9) . ?
N2 C22 1.494(9) . ?
N2 C21 1.500(9) . ?
N2 C20 1.516(9) . ?
C22 C19 1.497(9) . ?

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 O2 142.70(11) 4_547 . ?
O3 In1 O8 115.57(15) 4_547 1_556 ?
O2 In1 O8 83.77(15) . 1_556 ?
O3 In1 O6 128.41(12) 4_547 . ?
O2 In1 O6 84.03(12) . . ?
O8 In1 O6 81.13(13) 1_556 . ?
O3 In1 O5 90.85(13) 4_547 . ?
O2 In1 O5 93.75(13) . . ?
O8 In1 O5 138.77(15) 1_556 . ?
O6 In1 O5 57.73(11) . . ?
O3 In1 O1 85.58(10) 4_547 . ?
O2 In1 O1 57.77(10) . . ?
O8 In1 O1 123.83(14) 1_556 . ?
O6 In1 O1 126.99(11) . . ?
O5 In1 O1 87.25(12) . . ?
O3 In1 O4 57.18(11) 4_547 4_547 ?
O2 In1 O4 159.66(11) . 4_547 ?
O8 In1 O4 80.69(17) 1_556 4_547 ?
O6 In1 O4 80.67(13) . 4_547 ?
O5 In1 O4 89.37(17) . 4_547 ?
O1 In1 O4 142.55(10) . 4_547 ?
O3 In1 O7 81.99(15) 4_547 1_556 ?
O2 In1 O7 84.76(15) . 1_556 ?
O8 In1 O7 55.25(16) 1_556 1_556 ?
O6 In1 O7 135.85(13) . 1_556 ?
O5 In1 O7 165.75(13) . 1_556 ?
O1 In1 O7 79.96(13) . 1_556 ?
O4 In1 O7 96.96(17) 4_547 1_556 ?
O3 In1 C15 111.03(15) 4_547 . ?
O2 In1 C15 89.02(15) . . ?
O8 In1 C15 110.05(16) 1_556 . ?
O6 In1 C15 28.97(13) . . ?
O5 In1 C15 28.76(13) . . ?
O1 In1 C15 108.53(14) . . ?
O4 In1 C15 84.08(17) 4_547 . ?
O7 In1 C15 164.54(15) 1_556 . ?
O3 In1 C8 28.88(13) 4_547 4_547 ?
O2 In1 C8 169.85(15) . 4_547 ?
O8 In1 C8 97.03(17) 1_556 4_547 ?
O6 In1 C8 106.10(15) . 4_547 ?
O5 In1 C8 92.26(16) . 4_547 ?
O1 In1 C8 114.46(12) . 4_547 ?
O4 In1 C8 28.44(13) 4_547 4_547 ?
O7 In1 C8 87.40(18) 1_556 4_547 ?
C15 In1 C8 100.14(17) . 4_547 ?
O3 In1 C7 113.79(12) 4_547 . ?
O2 In1 C7 29.15(12) . . ?
O8 In1 C7 104.07(15) 1_556 . ?
O6 In1 C7 107.55(13) . . ?
O5 In1 C7 91.86(14) . . ?
O1 In1 C7 28.67(12) . . ?
O4 In1 C7 170.91(12) 4_547 . ?
O7 In1 C7 79.93(15) 1_556 . ?
C15 In1 C7 101.22(15) . . ?
C8 In1 C7 142.48(14) 4_547 . ?
O3 In1 C16 99.74(19) 4_547 1_556 ?
O2 In1 C16 83.08(18) . 1_556 ?
O8 In1 C16 27.8(2) 1_556 1_556 ?
O6 In1 C16 108.63(18) . 1_556 ?
O5 In1 C16 166.33(18) . 1_556 ?
O1 In1 C16 102.07(18) . 1_556 ?
O4 In1 C16 89.2(2) 4_547 1_556 ?
O7 In1 C16 27.47(18) 1_556 1_556 ?
C15 In1 C16 137.60(18) . 1_556 ?
C8 In1 C16 92.9(2) 4_547 1_556 ?
C7 In1 C16 91.73(18) . 1_556 ?
C15 O5 In1 88.8(2) . . ?
C15 O6 In1 92.0(3) . . ?
C7 O2 In1 94.3(2) . . ?
C7 O1 In1 87.3(2) . . ?
C5 C6 C1 121.0(4) . . ?
C13 C12 C11 117.9(5) . . ?
C3 C2 C1 120.2(4) . . ?
C2 C1 C6 118.3(4) . . ?
C2 C1 C1 121.3(5) . 2_675 ?
C6 C1 C1 120.3(5) . 2_675 ?
C12 C11 C10 118.5(5) . . ?
C12 C11 C15 122.8(5) . . ?
C10 C11 C15 118.7(4) . . ?
C2 C3 C4 121.1(4) . . ?
C2 C3 C7 121.5(4) . . ?
C4 C3 C7 117.4(4) . . ?
C9 C10 C11 123.7(5) . . ?
O5 C15 O6 121.5(4) . . ?
O5 C15 C11 121.2(4) . . ?
O6 C15 C11 117.3(4) . . ?
O5 C15 In1 62.5(2) . . ?
O6 C15 In1 59.1(2) . . ?
C11 C15 In1 176.3(3) . . ?
C12 C13 C14 123.7(5) . . ?
C12 C13 C16 120.8(6) . . ?
C14 C13 C16 115.5(5) . . ?
O1 C7 O2 120.4(4) . . ?
O1 C7 C3 121.4(4) . . ?
O2 C7 C3 118.0(4) . . ?
O1 C7 In1 64.0(2) . . ?
O2 C7 In1 56.6(2) . . ?
C3 C7 In1 170.2(3) . . ?
C5 C4 C3 118.4(4) . . ?
C6 C5 C4 121.0(4) . . ?
C6 C5 C8 120.8(4) . . ?
C4 C5 C8 118.2(4) . . ?
C10 C9 C14 116.3(5) . . ?
C10 C9 C9 121.1(4) . 2_575 ?
C14 C9 C9 122.7(3) . 2_575 ?
C13 C14 C9 120.0(5) . . ?
C8 O4 In1 86.0(3) . 4_557 ?
O4 C8 O3 121.5(4) . . ?
O4 C8 C5 119.4(4) . . ?
O3 C8 C5 119.1(4) . . ?
O4 C8 In1 65.6(2) . 4_557 ?
O3 C8 In1 56.38(19) . 4_557 ?
C5 C8 In1 169.7(4) . 4_557 ?
C8 O3 In1 94.7(2) . 4_557 ?
C16 O8 In1 98.0(4) . 1_554 ?
C16 O7 In1 86.0(3) . 1_554 ?
O7 C16 O8 120.7(5) . . ?
O7 C16 C13 121.3(5) . . ?
O8 C16 C13 118.0(6) . . ?
O7 C16 In1 66.5(3) . 1_554 ?
O8 C16 In1 54.2(3) . 1_554 ?
C13 C16 In1 171.5(5) . 1_554 ?
C18 N1 C19 113.3(6) . . ?
C18 N1 C17 111.6(6) . . ?
C19 N1 C17 111.4(6) . . ?
N1 C18 C21 110.0(8) . . ?
N1 C17 C20 105.6(8) . . ?
C22 N2 C21 109.3(8) . . ?
C22 N2 C20 110.8(8) . . ?
C21 N2 C20 109.0(8) . . ?
N2 C20 C17 109.3(9) . . ?
N2 C22 C19 112.0(10) . . ?
N1 C19 C22 104.2(9) . . ?
C18 C21 N2 106.2(9) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        73.54
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.758
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.089
