# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_MIL53_101_3
_database_code_depnum_ccdc_archive 'CCDC 1578119'
_audit_update_record             
;
2018-04-18 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT077_MIL53_101_3         
;
PROBLEM: Unitcell contains non-integer number of atoms ..     Please Check
RESPONSE: Due to the partial occupancy of the Iodine atoms within 
          the structure.
;
_vrf_PLAT082_MIL53_101_3         
;
PROBLEM: High R1 Value ..................................       0.13 Report
RESPONSE: What was considered electron density from a disordered solvent 
          molecule was not treated by PLATON/SQUEEZE due to its location 
          near the I2 site.  Due to the chemical uncertainty of the sites,
          they were not modeled.
;
_vrf_PLAT084_MIL53_101_3         
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.35 Report
RESPONSE: What was considered electron density from a disordered solvent 
          molecule was not treated by PLATON/SQUEEZE due to its location 
          near the I2 site.  Due to the chemical uncertainty of the sites,
          they were not modeled.
;
_vrf_PLAT088_MIL53_101_3         
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.43 Note  
RESPONSE: The diffraction qualtiy, as is the case for many MOF materials,
          was poor.
;
_vrf_PLAT094_MIL53_101_3         
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       2.53 Report
RESPONSE: What was considered electron density from a disordered solvent 
          molecule was not treated by PLATON/SQUEEZE due to its location 
          near the I2 site.  Due to the chemical uncertainty of the sites,
          they were not modeled.
;
_vrf_PLAT250_MIL53_101_3         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.3 Note  
RESPONSE: The diffraction qualtiy, as is the case for many MOF materials,
          was poor.  All attempts to improve this were made during the 
          refinement process.
;
_vrf_PLAT342_MIL53_101_3         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.014 Ang.  
RESPONSE: The diffraction qualtiy, as is the case for many MOF materials,
          was poor.
;
_vrf_PLAT906_MIL53_101_3         
;
PROBLEM: Large K value in the Analysis of Variance ......      3.883 Check 
RESPONSE: The diffraction qualtiy, as is the case for many MOF materials,
          was poor and resulted in a poor absorption correction.
;
_vrf_PLAT976_MIL53_101_3         
;
PROBLEM: Check Calcd Residual Density  1.05A From      O1      -0.74 eA-3  
RESPONSE: Most likely due to the poor absoprtion correction that was 
          applied to the experimental data.  There was no resonable
          chemical answer given this sites location within the structure.  
      
;
_vrf_PLAT977_MIL53_101_3         
;
PROBLEM: Check the Negative Difference Density on      H1      -0.74 eA-3  
RESPONSE: Most likely due to the poor absoprtion correction that was 
          applied to the experimental data.
;
# end Validation Reply Form

_audit_creation_date             2017-10-03T13:19:50-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C8 H4.19 Al I0.82 O5'
_chemical_formula_weight         310.83

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_Int_Tables_number      74
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   16.501(4)
_cell_length_b                   6.6194(18)
_cell_length_c                   13.210(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1442.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1575
_cell_measurement_theta_min      2.47
_cell_measurement_theta_max      24.95

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.19
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_F_000             594

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.883
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_correction_T_max  0.2590
_exptl_absorpt_correction_T_min  0.2013
_shelx_estimated_absorpt_T_min   0.650
_shelx_estimated_absorpt_T_max   0.716

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(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 APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_av_R_equivalents  0.0558
_diffrn_reflns_number            6080
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.975
_diffrn_reflns_theta_max         25.367
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_reflns_number_total             754
_reflns_number_gt                666
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

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  0.000  0.022  0.500        50        21 ' '
   2  0.500  0.022  1.000        50        21 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                            ?

  The unit cell contains a mixture of most likely water and 
  2-iodoterephthalic molecules which have been treated as a 
  diffuse contribution to the overall scattering without specific
  atoms positions by PLATON/SQUEEZE. Due to the unknown specific 
  amount of void filling molecules, the squeezed atoms were not 
  added to the UNIT card and so the F000, Mr, Mu, and Dx values 
  do not reflect these values.
  
  References:
  Spek, A.L. (2009). Acta Cryst. D65, 148-155.
  Spek, A.L. (2015). Acta Cryst. C71, 9-18.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1964P)²+24.6562P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.10(2)
_refine_ls_number_reflns         754
_refine_ls_number_parameters     80
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.127
_refine_ls_wR_factor_ref         0.3533
_refine_ls_wR_factor_gt          0.3491
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.74
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.23

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
I1A I 0.7491(4) 0.6634(9) 0.5801(5) 0.068(2) Uani 0.115(2) d A 1
I1B I 0.7971(18) 0.570(4) 0.5511(19) 0.096(7) Uani 0.035(2) d A 1
I2 I 0.6044(10) 0.628(2) 0.8092(11) 0.090(7) Uani 0.054(3) d A 1
Al1 Al 0.5 0.5 0.5 0.0195(13) Uani 1 d A 1
O1 O 0.5 0.25 0.4388(6) 0.021(2) Uani 1 d A 1
H1 H 0.5 0.25 0.3660(17) 0.025 Uiso 1 d B 1
O2 O 0.5831(3) 0.4193(7) 0.5915(3) 0.0312(16) Uani 1 d A 1
C1 C 0.6109(6) 0.25 0.6165(7) 0.027(2) Uani 1 d A 1
C2 C 0.6835(6) 0.25 0.6862(9) 0.038(2) Uani 1 d A 1
C3A C 0.7373(11) 0.412(2) 0.6869(14) 0.051(4) Uani 0.5 d A 1
H3A H 0.7311 0.5196 0.64 0.061 Uiso 0.35 calc A 1
C3B C 0.6985(10) 0.415(2) 0.7416(14) 0.049(3) Uani 0.5 d A 1
H3B H 0.6664 0.5327 0.7332 0.059 Uiso 0.446(3) calc A 1



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
I1A I1B 1.08(3) . ?
I1A I1A 1.147(12) 11_575 ?
I1A I1B 1.97(3) 11_575 ?
I1A C3A 2.190(16) . ?
I1A I1B 2.45(3) 4_566 ?
I1A I2 2.836(14) 7_646 ?
I1A I1A 3.027(15) 4_566 ?
I1A I2 3.145(16) 13_666 ?
I1B I1B 1.63(6) 4_566 ?
I1B I1A 1.97(3) 11_575 ?
I1B C3A 2.30(2) . ?
I1B I1B 2.39(6) 11_575 ?
I1B I1A 2.45(3) 4_566 ?
I1B I2 2.49(3) 7_646 ?
I2 I2 1.62(3) 11_575 ?
I2 C3B 2.280(18) . ?
I2 I1B 2.49(3) 7_646 ?
I2 I1A 2.835(14) 7_646 ?
I2 I1A 3.145(16) 13_666 ?
Al1 O1 1.842(4) . ?
Al1 O1 1.842(4) 9_666 ?
Al1 O2 1.905(4) 9_666 ?
Al1 O2 1.905(4) 12_655 ?
Al1 O2 1.905(4) 4_566 ?
Al1 O2 1.905(4) . ?
O1 Al1 1.842(4) 2_655 ?
O1 H1 0.96(2) . ?
O2 C1 1.255(6) . ?
C1 O2 1.255(6) 11_565 ?
C1 C2 1.510(13) . ?
C2 C3B 1.335(15) . ?
C2 C3B 1.335(15) 11_565 ?
C2 C3A 1.392(16) 11_565 ?
C2 C3A 1.392(17) . ?
C3A C3B 1.420(19) 7_646 ?
C3A H3A 0.95 . ?
C3B C3A 1.420(19) 7_646 ?
C3B H3B 0.95 . ?

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
I1B I1A I1A 125.2(13) . 11_575 ?
I1B I1A I1B 98.7(18) . 11_575 ?
I1B I1A C3A 81.8(11) . . ?
I1A I1A C3A 139.5(5) 11_575 . ?
I1B I1A C3A 147.2(9) 11_575 . ?
I1A I1A I1B 129.0(6) 11_575 4_566 ?
I1B I1A I1B 107.2(9) 11_575 4_566 ?
C3A I1A I1B 90.3(8) . 4_566 ?
I1B I1A I2 60.5(16) . 7_646 ?
I1A I1A I2 94.8(3) 11_575 7_646 ?
I1B I1A I2 80.3(9) 11_575 7_646 ?
C3A I1A I2 71.4(5) . 7_646 ?
I1B I1A I2 92.1(7) 4_566 7_646 ?
I1B I1A I1A 48.7(16) . 4_566 ?
I1A I1A I1A 135.62(18) 11_575 4_566 ?
I1B I1A I1A 120.3(7) 11_575 4_566 ?
C3A I1A I1A 84.7(5) . 4_566 ?
I2 I1A I1A 107.5(5) 7_646 4_566 ?
I1B I1A I2 81.5(16) . 13_666 ?
I1A I1A I2 63.9(3) 11_575 13_666 ?
I1B I1A I2 52.3(9) 11_575 13_666 ?
C3A I1A I2 95.9(5) . 13_666 ?
I1B I1A I2 110.9(7) 4_566 13_666 ?
I1A I1A I2 129.7(3) 4_566 13_666 ?
I1A I1B I1B 128.2(17) . 4_566 ?
I1B I1B I1A 131.7(17) 4_566 11_575 ?
I1A I1B C3A 70.6(11) . . ?
I1B I1B C3A 112.9(19) 4_566 . ?
I1A I1B C3A 94.7(12) 11_575 . ?
I1A I1B I1B 54.8(13) . 11_575 ?
I1B I1B I1B 124.3(15) 4_566 11_575 ?
C3A I1B I1B 117.0(9) . 11_575 ?
I1A I1B I1A 112.1(19) . 4_566 ?
I1A I1B I1A 124.8(13) 11_575 4_566 ?
C3A I1B I1A 97.3(10) . 4_566 ?
I1B I1B I1A 129.0(6) 11_575 4_566 ?
I1A I1B I2 97.3(19) . 7_646 ?
I1B I1B I2 134.4(13) 4_566 7_646 ?
I1A I1B I2 88.8(12) 11_575 7_646 ?
C3A I1B I2 76.8(9) . 7_646 ?
I1B I1B I2 81.1(7) 11_575 7_646 ?
I1A I1B I2 146.4(14) 4_566 7_646 ?
I2 I2 C3B 128.3(7) 11_575 . ?
I2 I2 I1B 98.9(7) 11_575 7_646 ?
C3B I2 I1B 75.5(7) . 7_646 ?
I2 I2 I1A 85.2(3) 11_575 7_646 ?
C3B I2 I1A 70.9(5) . 7_646 ?
I2 I2 I1A 63.9(3) 11_575 13_666 ?
C3B I2 I1A 86.0(6) . 13_666 ?
O1 Al1 O1 180 . 9_666 ?
O1 Al1 O2 88.5(2) . 9_666 ?
O1 Al1 O2 91.5(2) 9_666 9_666 ?
O1 Al1 O2 91.5(2) . 12_655 ?
O1 Al1 O2 88.5(2) 9_666 12_655 ?
O2 Al1 O2 87.9(3) 9_666 12_655 ?
O1 Al1 O2 88.5(2) . 4_566 ?
O1 Al1 O2 91.5(2) 9_666 4_566 ?
O2 Al1 O2 92.1(3) 9_666 4_566 ?
O2 Al1 O2 180 12_655 4_566 ?
O1 Al1 O2 91.5(2) . . ?
O1 Al1 O2 88.5(2) 9_666 . ?
O2 Al1 O2 180 9_666 . ?
O2 Al1 O2 92.1(3) 12_655 . ?
O2 Al1 O2 87.9(3) 4_566 . ?
Al1 O1 Al1 127.9(4) . 2_655 ?
Al1 O1 H1 116.0(2) . . ?
Al1 O1 H1 116.0(2) 2_655 . ?
C1 O2 Al1 132.9(5) . . ?
O2 C1 O2 126.5(8) . 11_565 ?
O2 C1 C2 116.8(4) . . ?
O2 C1 C2 116.8(4) 11_565 . ?
C3B C2 C3B 109.4(15) . 11_565 ?
C3B C2 C3A 120.4(11) . 11_565 ?
C3B C2 C3A 120.4(11) 11_565 . ?
C3A C2 C3A 100.7(16) 11_565 . ?
C3B C2 C1 118.8(8) . . ?
C3B C2 C1 118.7(8) 11_565 . ?
C3A C2 C1 120.6(8) 11_565 . ?
C3A C2 C1 120.6(8) . . ?
C2 C3A C3B 119.3(12) . 7_646 ?
C2 C3A I1A 129.6(10) . . ?
C3B C3A I1A 110.6(11) 7_646 . ?
C2 C3A I1B 128.2(14) . . ?
C3B C3A I1B 101.1(14) 7_646 . ?
C2 C3A H3A 120.3 . . ?
C3B C3A H3A 120.3 7_646 . ?
C2 C3B C3A 119.5(12) . 7_646 ?
C2 C3B I2 126.4(12) . . ?
C3A C3B I2 104.8(12) 7_646 . ?
C2 C3B H3B 120.2 . . ?
C3A C3B H3B 120.2 7_646 . ?



####################################################################### 
# 
# 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_MIL53_124_9
_database_code_depnum_ccdc_archive 'CCDC 1578120'
_audit_update_record             
;
2018-04-18 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT420_MIL53_124_9         
;
PROBLEM: D-H Without Acceptor       O1     --  H1     ...     Please Check 
RESPONSE: Due to the activation of the MOF crystal, there are no solvent
          molecules for the hydrogen atom to interact with.
;
_vrf_PLAT077_MIL53_124_9         
;
PROBLEM: Unitcell contains non-integer number of atoms ..     Please Check
RESPONSE: Due to the partial occupancy of the Iodine atoms within 
          the structure.
;
_vrf_PLAT082_MIL53_124_9         
;
PROBLEM: High R1 Value ..................................       0.14 Report
RESPONSE: After the activation process, the poor diffraction quality of the
          crystal was reduced even further.
;
_vrf_PLAT084_MIL53_124_9         
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.33 Report
RESPONSE: After the activation process, the poor diffraction quality of the
          crystal was reduced even further.
;
_vrf_PLAT088_MIL53_124_9         
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.38 Note  
RESPONSE: After the activation process, the poor diffraction quality of the
          crystal was reduced even further.
;
_vrf_PLAT213_MIL53_124_9         
;
PROBLEM: Atom Al1             has ADP max/min Ratio .....        3.6 prolat
RESPONSE: Due to the poor diffraction qualtiy of the crystal, even though
          multiple attempts with various absorption parameters were tested.
;
_vrf_PLAT250_MIL53_124_9         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        3.8 Note  
RESPONSE: Due to the poor diffraction qualtiy of the crystal, even though
          multiple attempts with various absorption parameters were tested.
;
_vrf_PLAT342_MIL53_124_9         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............       0.02 Ang.  
RESPONSE: Due to the poor diffraction quality of the crystal.
;
_vrf_PLAT906_MIL53_124_9         
;
PROBLEM: Large K value in the Analysis of Variance ......     15.969 Check 
RESPONSE: Due to the poor diffraction qualtiy of the crystal, even though
          multiple attempts with various absorption parameters were tested.
;
_vrf_PLAT973_MIL53_124_9         
;
PROBLEM: Check Calcd Positive Residual Density on     Al1       1.32 eA-3  
RESPONSE: Most likely due to the poor absoprtion correction that was 
          applied to the experimental data.  There was no resonable
          chemical answer, given this site's location within the structure.
;
_vrf_PLAT975_MIL53_124_9         
;
PROBLEM: Check Calcd Residual Density  1.04A From      O2       0.45 eA-3  
RESPONSE: Most likely due to the poor absoprtion correction that was 
          applied to the experimental data.  There was no resonable
          chemical answer, given this site's location within the structure.
;
_vrf_PLAT977_MIL53_124_9         
;
PROBLEM: Check the Negative Difference Density on      H1      -0.49 eA-3  
RESPONSE: This appeared to potentially be a partially occupied water 
          molecule, but when placed in the model the refinement became
          unstable.
;
_vrf_PLAT978_MIL53_124_9         
;
PROBLEM: Number C-C Bonds with Positive Residual Density.          0 Info  
RESPONSE: Due to the poor diffraction quality of the crystal.
;
# end Validation Reply Form

_audit_creation_date             2017-10-03T16:29:11-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C8 H4.36 Al I0.64 O5'
_chemical_formula_weight         288.67

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_Int_Tables_number      74
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   18.466(17)
_cell_length_b                   6.635(5)
_cell_length_c                   9.627(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1179.5(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1828
_cell_measurement_theta_min      2.21
_cell_measurement_theta_max      25.22

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_F_000             557

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.843
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_correction_T_max  0.5619
_exptl_absorpt_correction_T_min  0.1958
_shelx_estimated_absorpt_T_min   0.656
_shelx_estimated_absorpt_T_max   0.733

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(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 APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_unetI/netI     0.0739
_diffrn_reflns_av_R_equivalents  0.0974
_diffrn_reflns_number            5570
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.206
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_number_total             619
_reflns_number_gt                543
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

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  0.500  0.250  0.104        16         0 ' '
   2  0.000  0.250  0.396        15         0 ' '
   3  0.000  0.750  0.604        16         0 ' '
   4  0.500  0.750  0.896        15         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details    

  To demonstrate that the crystal had been activated the 
  PLATON/SQUEEZE program was applied to the data. Due to 
  the lack of electron density within the pore space, no 
  crystallogrpahic values were changed.
  
  References:
  Spek, A.L. (2009). Acta Cryst. D65, 148-155.
  Spek, A.L. (2015). Acta Cryst. C71, 9-18
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+85.7685P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         619
_refine_ls_number_parameters     66
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.1448
_refine_ls_R_factor_gt           0.1352
_refine_ls_wR_factor_ref         0.3346
_refine_ls_wR_factor_gt          0.3299
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_restrained_S_all      1.149
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.964
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.215

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
I1A I 0.6374(3) 1.1446(9) 0.8803(6) 0.0498(18) Uani 0.1548(17) d . .
I1B I 0.675(6) 1.25 0.773(18) 0.063(18) Uani 0.010(3) d . .
Al1 Al 0.5 0.5 0.5 0.0202(14) Uani 1 d . .
O1 O 0.5 0.25 0.5857(16) 0.024(3) Uani 1 d . .
H1 H 0.5 0.25 0.685(3) 0.029 Uiso 1 d . .
O2 O 0.5753(4) 0.5817(11) 0.6240(8) 0.032(2) Uani 1 d . .
C1 C 0.6042(8) 0.75 0.6458(18) 0.029(3) Uani 1 d . .
C2 C 0.6785(9) 0.75 0.703(2) 0.037(4) Uani 1 d . .
C3A C 0.7046(12) 0.914(4) 0.769(3) 0.047(5) Uani 0.5 d . .
H3A H 0.6751 1.0305 0.7804 0.056 Uiso 0.34 calc . .
C3B C 0.7236(12) 0.912(4) 0.679(3) 0.045(5) Uani 0.5 d . .
H3B H 0.7062 1.0237 0.6267 0.054 Uiso 0.5 calc . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
I1A I1A 1.399(12) 11_585 ?
I1A I1B 1.43(14) . ?
I1A C3A 2.24(3) . ?
I1A I1A 2.999(14) 4_577 ?
I1B I1A 1.43(14) 11_585 ?
I1B C3A 2.29(4) 11_585 ?
I1B C3A 2.29(4) . ?
I1B C3B 2.58(8) . ?
I1B C3B 2.58(8) 11_585 ?
I1B I1B 2.8(2) 13_676 ?
Al1 O1 1.853(7) . ?
Al1 O1 1.853(7) 9_666 ?
Al1 O2 1.911(7) 9_666 ?
Al1 O2 1.911(7) 12_655 ?
Al1 O2 1.911(7) 4_566 ?
Al1 O2 1.911(7) . ?
O1 Al1 1.853(7) 2_655 ?
O1 H1 0.96(2) . ?
O2 C1 1.256(10) . ?
C1 O2 1.256(10) 11_575 ?
C1 C2 1.48(2) . ?
C2 C3A 1.35(3) . ?
C2 C3A 1.35(3) 11_575 ?
C2 C3B 1.38(3) . ?
C2 C3B 1.38(3) 11_575 ?
C3A C3B 1.42(3) 7_646 ?
C3A H3A 0.95 . ?
C3B C3A 1.42(3) 7_646 ?
C3B H3B 0.95 . ?

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
I1A I1A I1B 61(3) 11_585 . ?
I1A I1A C3A 133.0(7) 11_585 . ?
I1B I1A C3A 74(3) . . ?
I1A I1A I1A 129.8(2) 11_585 4_577 ?
I1B I1A I1A 150(4) . 4_577 ?
C3A I1A I1A 86.0(8) . 4_577 ?
I1A I1B I1A 59(6) 11_585 . ?
I1A I1B C3A 69.7(17) 11_585 11_585 ?
I1A I1B C3A 127(8) . 11_585 ?
I1A I1B C3A 127(8) 11_585 . ?
I1A I1B C3A 69.7(16) . . ?
C3A I1B C3A 152(6) 11_585 . ?
I1A I1B C3B 148(7) 11_585 . ?
I1A I1B C3B 89.9(8) . . ?
C3A I1B C3B 139(6) 11_585 . ?
I1A I1B C3B 89.9(8) 11_585 11_585 ?
I1A I1B C3B 148(7) . 11_585 ?
C3A I1B C3B 139(6) . 11_585 ?
C3B I1B C3B 121(6) . 11_585 ?
I1A I1B I1B 126(9) 11_585 13_676 ?
I1A I1B I1B 126(9) . 13_676 ?
C3A I1B I1B 76(3) 11_585 13_676 ?
C3A I1B I1B 76(3) . 13_676 ?
C3B I1B I1B 66(3) . 13_676 ?
C3B I1B I1B 66(3) 11_585 13_676 ?
O1 Al1 O1 180 . 9_666 ?
O1 Al1 O2 91.4(4) . 9_666 ?
O1 Al1 O2 88.6(4) 9_666 9_666 ?
O1 Al1 O2 88.6(4) . 12_655 ?
O1 Al1 O2 91.4(4) 9_666 12_655 ?
O2 Al1 O2 86.7(5) 9_666 12_655 ?
O1 Al1 O2 91.4(4) . 4_566 ?
O1 Al1 O2 88.6(4) 9_666 4_566 ?
O2 Al1 O2 93.3(5) 9_666 4_566 ?
O2 Al1 O2 180 12_655 4_566 ?
O1 Al1 O2 88.6(4) . . ?
O1 Al1 O2 91.4(4) 9_666 . ?
O2 Al1 O2 180 9_666 . ?
O2 Al1 O2 93.3(5) 12_655 . ?
O2 Al1 O2 86.7(5) 4_566 . ?
Al1 O1 Al1 127.1(9) 2_655 . ?
Al1 O1 H1 116.4(4) 2_655 . ?
Al1 O1 H1 116.4(4) . . ?
C1 O2 Al1 131.8(8) . . ?
O2 C1 O2 125.6(13) . 11_575 ?
O2 C1 C2 117.2(7) . . ?
O2 C1 C2 117.2(7) 11_575 . ?
C3A C2 C3A 108(3) . 11_575 ?
C3A C2 C3B 119.7(16) 11_575 . ?
C3A C2 C3B 119.7(16) . 11_575 ?
C3B C2 C3B 102(2) . 11_575 ?
C3A C2 C1 120.4(13) . . ?
C3A C2 C1 120.4(13) 11_575 . ?
C3B C2 C1 119.6(14) . . ?
C3B C2 C1 119.6(14) 11_575 . ?
C2 C3A C3B 119(3) . 7_646 ?
C2 C3A I1A 125.2(16) . . ?
C3B C3A I1A 111(2) 7_646 . ?
C2 C3A I1B 135(4) . . ?
C3B C3A I1B 103(4) 7_646 . ?
C2 C3A H3A 120.3 . . ?
C3B C3A H3A 120.3 7_646 . ?
C2 C3B C3A 121(3) . 7_646 ?
C2 C3B I1B 114(3) . . ?
C3A C3B I1B 101(3) 7_646 . ?
C2 C3B H3B 119.6 . . ?
C3A C3B H3B 119.6 7_646 . ?



####################################################################### 
# 
# 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_MIL53_108_9
_database_code_depnum_ccdc_archive 'CCDC 1578569'
_audit_update_record             
;
2018-04-18 deposited with the CCDC.
2018-08-03 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT250_MIL53_108_9         
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor ....        7.2 Note  
RESPONSE: This is due to the large thermal motion of the I2 site. 
;
_vrf_PLAT076_MIL53_108_9         
;
PROBLEM: Occupancy      0.250 less than 1.0 for Sp.pos  .         O3       
RESPONSE: This is most likely a partial occupied oxygen site and was 
          modeled as such.
;
_vrf_PLAT077_MIL53_108_9         
;
PROBLEM: Unitcell contains non-integer number of atoms ..     Please Check
RESPONSE: Due to the partial occupancy of the Iodine atoms within 
          the structure.
;
_vrf_PLAT082_MIL53_108_9         
;
PROBLEM: High R1 Value ..................................       0.11 Report
RESPONSE: The crystal diffraction quality of these crystals was poor at
          best.
;
_vrf_PLAT084_MIL53_108_9         
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.29 Report
RESPONSE: The crystal diffraction quality of these crystals was poor at
          best.
;
_vrf_PLAT088_MIL53_108_9         
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.73 Note  
RESPONSE: The crystal diffraction quality of these crystals was poor at
          best.
;
_vrf_PLAT215_MIL53_108_9         
;
PROBLEM: Disordered C3A       has ADP max/min Ratio .....        3.2 Note  
RESPONSE: The structure appears to have more thermal motion about the 
          linker ligand, leading to a slightly larger pore space and more
          elongated thermal ellipsoids.
;
_vrf_PLAT342_MIL53_108_9         
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............      0.012 Ang.  
RESPONSE: The crystal diffraction quality of these crystals was poor at
          best.
;
_vrf_PLAT906_MIL53_108_9         
;
PROBLEM: Large K value in the Analysis of Variance ......      6.776 Check 
RESPONSE: The crystal diffraction quality of these crystals was poor at
          best.  This led to a less than ideal absorption correction.
;
_vrf_PLAT911_MIL53_108_9         
;
PROBLEM: Missing # FCF Refl Between THmin & STh/L=  0.600          2 Report
RESPONSE: These reflections were not collected during the omega only scans.
;
# end Validation Reply Form

_audit_creation_date             2017-10-06T10:05:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_sum            'C8 H4.30 Al I0.70 O5.25'
_chemical_formula_weight         300.1

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'I m m a'
_symmetry_space_group_name_Hall  '-I 2b 2'
_symmetry_Int_Tables_number      74
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'-x, y+1/2, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'-x+1/2, y+1, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'x, -y-1/2, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y+1/2, z+1/2'

_cell_length_a                   17.107(11)
_cell_length_b                   6.622(4)
_cell_length_c                   12.229(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1385.2(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1645
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      24.87

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       blocky
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.165
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_F_000             577

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.703
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5049
_shelx_estimated_absorpt_T_min   0.564
_shelx_estimated_absorpt_T_max   0.766

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_ambient_temperature      100(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 APEX-II CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_unetI/netI     0.0494
_diffrn_reflns_av_R_equivalents  0.0878
_diffrn_reflns_number            6789
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.047
_diffrn_reflns_theta_max         25.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_reflns_number_total             730
_reflns_number_gt                596
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2014)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.

 For this structure the PLATON/SQUEEZE routine was not used.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1560P)²+10.1819P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.059(16)
_refine_ls_number_reflns         730
_refine_ls_number_parameters     75
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.1215
_refine_ls_R_factor_gt           0.1067
_refine_ls_wR_factor_ref         0.2903
_refine_ls_wR_factor_gt          0.2786
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.141

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
I1 I 0.6157(3) 0.6389(8) 0.8241(5) 0.078(3) Uani 0.098(2) d . .
I2 I 0.7435(9) 0.653(2) 0.5669(17) 0.222(12) Uani 0.077(3) d . .
Al1 Al 0.5 0.5 0.5 0.0219(11) Uani 1 d . .
O1 O 0.5 0.25 0.4345(6) 0.0249(16) Uani 1 d . .
H1 H 0.5 0.25 0.3567(18) 0.03 Uiso 1 d . .
O2 O 0.5801(2) 0.4187(5) 0.5982(3) 0.0397(14) Uani 1 d . .
C1 C 0.6070(4) 0.25 0.6229(7) 0.036(2) Uani 1 d . .
C2 C 0.6804(5) 0.25 0.6901(9) 0.050(2) Uani 1 d . .
C3A C 0.6998(9) 0.4146(18) 0.7558(16) 0.065(4) Uani 0.5 d . .
H3A H 0.6663 0.5288 0.76 0.079 Uiso 0.402(2) calc . .
C3B C 0.7329(9) 0.4085(19) 0.6865(15) 0.066(4) Uani 0.5 d . .
H3B H 0.7209 0.52 0.6407 0.079 Uiso 0.423(3) calc . .
O3 O 0.5 0.25 0.876(4) 0.15(3) Uani 0.25 d . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 I1 1.471(11) 11_575 ?
I1 C3A 2.230(15) . ?
I1 I2 2.754(13) 7_646 ?
I1 I2 3.077(13) 13_666 ?
I2 I2 1.28(3) 11_575 ?
I2 C3B 2.191(18) . ?
I2 I2 2.61(4) 4_566 ?
I2 I1 2.754(13) 7_646 ?
I2 I1 3.077(13) 13_666 ?
Al1 O1 1.839(3) . ?
Al1 O1 1.839(3) 9_666 ?
Al1 O2 1.900(4) . ?
Al1 O2 1.900(4) 9_666 ?
Al1 O2 1.900(4) 12_655 ?
Al1 O2 1.900(4) 4_566 ?
O1 Al1 1.839(3) 2_655 ?
O1 H1 0.95(2) . ?
O2 C1 1.246(5) . ?
C1 O2 1.246(5) 11_565 ?
C1 C2 1.501(11) . ?
C2 C3B 1.382(15) . ?
C2 C3B 1.382(15) 11_565 ?
C2 C3A 1.394(14) 11_565 ?
C2 C3A 1.394(14) . ?
C3A C3B 1.351(18) 7_646 ?
C3A H3A 0.95 . ?
C3B C3A 1.351(18) 7_646 ?
C3B H3B 0.95 . ?

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
I1 I1 C3A 131.8(5) 11_575 . ?
I1 I1 I2 88.0(4) 11_575 7_646 ?
C3A I1 I2 68.9(5) . 7_646 ?
I1 I1 I2 63.4(3) 11_575 13_666 ?
C3A I1 I2 87.4(6) . 13_666 ?
I2 I2 C3B 137.7(8) 11_575 . ?
I2 I2 I2 141.1(6) 11_575 4_566 ?
C3B I2 I2 81.0(7) . 4_566 ?
I2 I2 I1 92.0(3) 11_575 7_646 ?
C3B I2 I1 74.0(5) . 7_646 ?
I2 I2 I1 106.1(5) 4_566 7_646 ?
I2 I2 I1 63.4(3) 11_575 13_666 ?
C3B I2 I1 96.1(6) . 13_666 ?
I2 I2 I1 128.3(4) 4_566 13_666 ?
O1 Al1 O1 180 . 9_666 ?
O1 Al1 O2 91.18(18) . . ?
O1 Al1 O2 88.82(18) 9_666 . ?
O1 Al1 O2 88.82(18) . 9_666 ?
O1 Al1 O2 91.18(18) 9_666 9_666 ?
O2 Al1 O2 180.00(18) . 9_666 ?
O1 Al1 O2 91.18(18) . 12_655 ?
O1 Al1 O2 88.82(18) 9_666 12_655 ?
O2 Al1 O2 92.3(3) . 12_655 ?
O2 Al1 O2 87.7(3) 9_666 12_655 ?
O1 Al1 O2 88.82(18) . 4_566 ?
O1 Al1 O2 91.18(18) 9_666 4_566 ?
O2 Al1 O2 87.7(3) . 4_566 ?
O2 Al1 O2 92.3(3) 9_666 4_566 ?
O2 Al1 O2 180 12_655 4_566 ?
Al1 O1 Al1 128.3(4) . 2_655 ?
Al1 O1 H1 115.8(2) . . ?
Al1 O1 H1 115.8(2) 2_655 . ?
C1 O2 Al1 132.4(4) . . ?
O2 C1 O2 127.5(7) 11_565 . ?
O2 C1 C2 116.3(3) 11_565 . ?
O2 C1 C2 116.3(3) . . ?
C3B C2 C3B 98.8(14) . 11_565 ?
C3B C2 C3A 117.3(9) . 11_565 ?
C3B C2 C3A 117.3(9) 11_565 . ?
C3A C2 C3A 102.9(15) 11_565 . ?
C3B C2 C1 121.7(8) . . ?
C3B C2 C1 121.7(8) 11_565 . ?
C3A C2 C1 121.0(7) 11_565 . ?
C3A C2 C1 121.0(7) . . ?
C3B C3A C2 118.7(11) 7_646 . ?
C3B C3A I1 112.0(12) 7_646 . ?
C2 C3A I1 125.7(9) . . ?
C3B C3A H3A 120.7 7_646 . ?
C2 C3A H3A 120.7 . . ?
C3A C3B C2 124.1(12) 7_646 . ?
C3A C3B I2 104.8(11) 7_646 . ?
C2 C3B I2 129.6(11) . . ?
C3A C3B H3B 118 7_646 . ?
C2 C3B H3B 118 . . ?



# END of CIF
