# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_VNU-11
_database_code_depnum_ccdc_archive 'CCDC 1560539'
# end Validation Reply Form

#Added by publCIF (Thu Jul 6 08:20:32 2017)


_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT242_VNU-11              
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of         O3 Check 
RESPONSE: This problem is due to the high thermal vibration of O atom as well as
 the low resolution of data collection.
;
_vrf_PLAT213_VNU-11              
;
PROBLEM: Atom C4 has ADP max/min Ratio ..... 4.1 prolat
RESPONSE: This may come from the disorder of Hf-oxo cluster and high vibration
 of formate terminals.
;
_vrf_PLAT220_VNU-11              
;
PROBLEM: Non-Solvent Resd 1 C Ueq(max)/Ueq(min) Range 10.0 Ratio
RESPONSE: This problem is due to the high thermal vibration of the atoms in the
 structure or the low resolution of data set.
;
_vrf_PLAT250_VNU-11              
; 
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.4 Note
RESPONSE: This problem is due to the low resolution of data set and the large
 void space of the structure.
;
_vrf_PLAT975_VNU-11              
;
PROBLEM: Check Calcd Residual Density 0.55A From O4 1.91 eA-3
RESPONSE: This problem is due to disorder u3 Oxo atom.
;
_vrf_PLAT990_VNU-11              
;
PROBLEM: Deprecated RES file style based SQUEEZE job
RESPONSE: This is a result of the high porosity and void space of this material,
which was removed by SQUEEZE job.
;
_publcif_datablock.id            {17100e3f-be27-45db-b501-788e0e1adfcc}

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H6 Hf3 O16'
_chemical_formula_weight         941.64

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'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   34.9801(12)
_cell_length_b                   34.9801(12)
_cell_length_c                   34.9801(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     42802(4)
_cell_formula_units_Z            32
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2453
_cell_measurement_theta_min      2.763
_cell_measurement_theta_max      30.642

_exptl_crystal_description       octahedral
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.169
_exptl_crystal_F_000             13504
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    5.836
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.944
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.916
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   SADABS
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  graphite
_diffrn_measurement_method       Bruker
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2453
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.647
_diffrn_reflns_theta_max         27.917
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             2453
_reflns_number_gt                1996
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.003 -0.007 -0.003 30424 2670 ' '
2 0.625 0.125 0.125 102 7 ' '
3 0.125 0.125 0.625 102 7 ' '
4 0.375 0.375 0.375 102 7 ' '
5 0.875 0.375 0.875 102 7 ' '
6 0.125 0.625 0.125 102 7 ' '
7 0.625 0.625 0.625 102 7 ' '
8 0.875 0.875 0.375 102 7 ' '
9 0.375 0.875 0.875 102 7 ' '
_platon_squeeze_details          
;
;
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0750P)²+353.8835P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2453
_refine_ls_number_parameters     57
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_ref         0.1230
_refine_ls_wR_factor_gt          0.1180
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.003
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.54699(2) 0.77298(2) 0.70301(2) 0.02886(14) Uani 1 2 d S T P . .
O1 O 0.54839(9) 0.74696(10) 0.64608(9) 0.0304(7) Uani 1 1 d . . . . .
O2 O 0.5601(2) 0.76260(12) 0.76260(12) 0.0586(18) Uani 1 2 d S T P . .
C1 C 0.54534(14) 0.70466(14) 0.5943(2) 0.0337(15) Uani 1 2 d S T P . .
C2 C 0.5296(2) 0.67187(14) 0.57813(14) 0.0315(14) Uani 1 2 d S T P . .
H2 H 0.507882 0.660369 0.589632 0.038 Uiso 1 2 calc R U P . .
C3 C 0.53059(13) 0.71941(13) 0.63119(19) 0.0267(13) Uani 1 2 d S T P . .
O3 O 0.58832(16) 0.81959(16) 0.7132(2) 0.0854(19) Uani 1 1 d . . . . .
O4 O 0.5327(3) 0.7173(3) 0.7173(3) 0.073(4) Uani 1 6 d S T P . .
C4 C 0.5919(5) 0.8419(5) 0.750000 0.46(4) Uani 1 2 d S T P . .
H4 H 0.611105 0.861103 0.750001 0.549 Uiso 1 2 calc R U P . .


_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
Hf1 O4 2.072(5) . ?
Hf1 O2 2.140(6) 175_557 ?
Hf1 O2 2.165(4) . ?
Hf1 O2 2.165(4) 34_645 ?
Hf1 O1 2.190(3) 190_657 ?
Hf1 O1 2.190(3) . ?
Hf1 O3 2.208(5) . ?
Hf1 O3 2.208(5) 190_657 ?
Hf1 Hf1 3.4610(5) 34_645 ?
Hf1 Hf1 3.4610(5) 55_564 ?
Hf1 Hf1 3.4954(5) 106_576 ?
Hf1 Hf1 3.4954(5) 175_557 ?
O1 C3 1.260(4) . ?
C1 C2 1.392(5) . ?
C1 C2 1.392(5) 78_456 ?
C1 C3 1.482(10) . ?
C2 H2 0.9500 . ?
O3 C4 1.511(11) . ?
C4 H4 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
O4 Hf1 O2 107.4(5) . 175_557 ?
O4 Hf1 O2 70.2(3) . . ?
O2 Hf1 O2 71.3(2) 175_557 . ?
O4 Hf1 O2 70.2(3) . 34_645 ?
O2 Hf1 O2 71.3(2) 175_557 34_645 ?
O2 Hf1 O2 112.3(4) . 34_645 ?
O4 Hf1 O1 80.4(4) . 190_657 ?
O2 Hf1 O1 140.88(9) 175_557 190_657 ?
O2 Hf1 O1 76.1(2) . 190_657 ?
O2 Hf1 O1 143.24(17) 34_645 190_657 ?
O4 Hf1 O1 80.4(4) . . ?
O2 Hf1 O1 140.88(9) 175_557 . ?
O2 Hf1 O1 143.24(17) . . ?
O2 Hf1 O1 76.1(2) 34_645 . ?
O1 Hf1 O1 77.68(17) 190_657 . ?
O4 Hf1 O3 144.40(18) . . ?
O2 Hf1 O3 80.2(2) 175_557 . ?
O2 Hf1 O3 80.2(3) . . ?
O2 Hf1 O3 142.0(2) 34_645 . ?
O1 Hf1 O3 73.45(18) 190_657 . ?
O1 Hf1 O3 116.0(2) . . ?
O4 Hf1 O3 144.40(18) . 190_657 ?
O2 Hf1 O3 80.2(2) 175_557 190_657 ?
O2 Hf1 O3 142.0(2) . 190_657 ?
O2 Hf1 O3 80.2(3) 34_645 190_657 ?
O1 Hf1 O3 116.0(2) 190_657 190_657 ?
O1 Hf1 O3 73.45(18) . 190_657 ?
O3 Hf1 O3 70.5(4) . 190_657 ?
O4 Hf1 Hf1 33.37(19) . 34_645 ?
O2 Hf1 Hf1 91.81(18) 175_557 34_645 ?
O2 Hf1 Hf1 91.79(18) . 34_645 ?
O2 Hf1 Hf1 36.93(14) 34_645 34_645 ?
O1 Hf1 Hf1 110.43(9) 190_657 34_645 ?
O1 Hf1 Hf1 73.86(8) . 34_645 ?
O3 Hf1 Hf1 170.1(2) . 34_645 ?
O3 Hf1 Hf1 114.09(19) 190_657 34_645 ?
O4 Hf1 Hf1 33.37(19) . 55_564 ?
O2 Hf1 Hf1 91.81(18) 175_557 55_564 ?
O2 Hf1 Hf1 36.93(14) . 55_564 ?
O2 Hf1 Hf1 91.79(18) 34_645 55_564 ?
O1 Hf1 Hf1 73.86(8) 190_657 55_564 ?
O1 Hf1 Hf1 110.43(9) . 55_564 ?
O3 Hf1 Hf1 114.09(19) . 55_564 ?
O3 Hf1 Hf1 170.1(2) 190_657 55_564 ?
Hf1 Hf1 Hf1 60.0 34_645 55_564 ?
O4 Hf1 Hf1 86.6(4) . 106_576 ?
O2 Hf1 Hf1 35.95(11) 175_557 106_576 ?
O2 Hf1 Hf1 35.47(16) . 106_576 ?
O2 Hf1 Hf1 90.45(19) 34_645 106_576 ?
O1 Hf1 Hf1 109.85(8) 190_657 106_576 ?
O1 Hf1 Hf1 163.82(8) . 106_576 ?
O3 Hf1 Hf1 80.1(2) . 106_576 ?
O3 Hf1 Hf1 113.55(16) 190_657 106_576 ?
Hf1 Hf1 Hf1 90.001(1) 34_645 106_576 ?
Hf1 Hf1 Hf1 60.327(5) 55_564 106_576 ?
O4 Hf1 Hf1 86.6(4) . 175_557 ?
O2 Hf1 Hf1 35.95(11) 175_557 175_557 ?
O2 Hf1 Hf1 90.45(19) . 175_557 ?
O2 Hf1 Hf1 35.47(16) 34_645 175_557 ?
O1 Hf1 Hf1 163.83(8) 190_657 175_557 ?
O1 Hf1 Hf1 109.84(8) . 175_557 ?
O3 Hf1 Hf1 113.55(16) . 175_557 ?
O3 Hf1 Hf1 80.1(2) 190_657 175_557 ?
Hf1 Hf1 Hf1 60.327(5) 34_645 175_557 ?
Hf1 Hf1 Hf1 90.001(1) 55_564 175_557 ?
Hf1 Hf1 Hf1 59.349(11) 106_576 175_557 ?
C3 O1 Hf1 133.1(3) . . ?
Hf1 O2 Hf1 108.6(2) 106_576 . ?
Hf1 O2 Hf1 108.6(2) 106_576 55_564 ?
Hf1 O2 Hf1 106.1(3) . 55_564 ?
C2 C1 C2 119.0(7) . 78_456 ?
C2 C1 C3 120.2(4) . . ?
C2 C1 C3 120.2(4) 78_456 . ?
C1 C2 C1 121.0(7) . 60_564 ?
C1 C2 H2 119.5 . . ?
C1 C2 H2 119.5 60_564 . ?
O1 C3 O1 125.8(6) . 133_765 ?
O1 C3 C1 117.0(3) . . ?
O1 C3 C1 117.0(3) 133_765 . ?
C4 O3 Hf1 125.0(11) . . ?
Hf1 O4 Hf1 113.3(4) 34_645 55_564 ?
Hf1 O4 Hf1 113.3(4) 34_645 . ?
Hf1 O4 Hf1 113.3(4) 55_564 . ?
O3 C4 O3 129.9(19) 13_456 . ?
O3 C4 H4 115.1 13_456 . ?
O3 C4 H4 115.1 . . ?

_refine_diff_density_max         1.136
_refine_diff_density_min         -1.346
_refine_diff_density_rms         0.159

loop_
_publcif_info_exptl_table_extra_item

sin_theta_over_lambda_max
loop_
_publcif_info_exptl_table_header_item

?



_publcif_funding_html            
;
;
####################################################################### 
# 
# 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_VNU-11-SO4
_database_code_depnum_ccdc_archive 'CCDC 1560540'
# end Validation Reply Form

#Added by publCIF (Thu Jul 6 08:55:18 2017)


_audit_update_record             
;
2017-07-06 deposited with the CCDC.
2017-08-24 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT241_VNU-11-SO4          
;
PROBLEM: High   'MainMol' Ueq as Compared to Neighbors of         S1 
RESPONSE: This problem is due to the high thermal vibration of SO4 groups binding to Hf-oxo clusters and
 the low resolution of data collection.
;
_vrf_PLAT242_VNU-11-SO4          
;
PROBLEM: Low    'MainMol' Ueq as Compared to Neighbors of        Hf1 
RESPONSE: This problem is due to the low resolution of data collection.
;
_vrf_PLAT250_VNU-11-SO4          
;
PROBLEM: Large U3/U1 Ratio for Average U(i,j) Tensor .... 4.7 
RESPONSE: This problem is due to the low resolution of data set and the large
 void space of the structure.
;
_vrf_PLAT990_VNU-11-SO4          
;
PROBLEM: Deprecated RES file style based SQUEEZE job
RESPONSE: This is a result of the high porosity and void space of this material,
which was removed by SQUEEZE job.
;
_publcif_datablock.id            {ee9f9a5f-1f14-4564-b32c-863685b24cee}

# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C9 H3 Hf3 O13 S6'
_chemical_formula_weight         1046.94

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      cubic
_space_group_IT_number           227
_space_group_name_H-M_alt        'F d -3 m'
_space_group_name_Hall           '-F 4vw 2vw 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   34.901(3)
_cell_length_b                   34.901(3)
_cell_length_c                   34.901(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     42512(9)
_cell_formula_units_Z            32
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    1962
_cell_measurement_theta_min      1.935
_cell_measurement_theta_max      25.74

_exptl_crystal_description       octahedral
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_F_000             15008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.015
_exptl_crystal_size_mid          0.012
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    5.931
_shelx_estimated_absorpt_T_min   0.918
_shelx_estimated_absorpt_T_max   0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   SADABS
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            1962
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_min       ?
_diffrn_reflns_limit_h_max       ?
_diffrn_reflns_limit_k_min       ?
_diffrn_reflns_limit_k_max       ?
_diffrn_reflns_limit_l_min       ?
_diffrn_reflns_limit_l_max       ?
_diffrn_reflns_theta_min         1.935
_diffrn_reflns_theta_max         25.739
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             1962
_reflns_number_gt                1567
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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.
;
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
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 -0.005 -0.009 -0.006 26962 1194 ' '
2 0.625 0.125 0.125 81 2 ' '
3 0.125 0.125 0.625 81 2 ' '
4 0.375 0.375 0.375 81 2 ' '
5 0.875 0.375 0.875 81 2 ' '
6 0.125 0.625 0.125 81 2 ' '
7 0.625 0.625 0.625 81 2 ' '
8 0.875 0.875 0.375 81 2 ' '
9 0.375 0.875 0.875 81 2 ' '
_platon_squeeze_details          
;
;
_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0707P)²+359.8019P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1962
_refine_ls_number_parameters     64
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1518
_refine_ls_wR_factor_gt          0.1461
_refine_ls_goodness_of_fit_ref   1.383
_refine_ls_restrained_S_all      1.383
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Hf1 Hf 0.47661(2) 0.54725(2) 0.54725(2) 0.0495(2) Uani 1 2 d S T P . .
S1 S 0.3974(15) 0.565(2) 0.565(2) 1.51(8) Uani 1 2 d S TU P . .
O1 O 0.50326(17) 0.60371(16) 0.54967(16) 0.0610(14) Uani 1 1 d . . . . .
S2 S 0.4119(5) 0.5881(5) 0.500000 0.84(4) Uani 1 2 d S TU P . .
O2 O 0.5310(5) 0.5310(5) 0.5310(5) 0.119(9) Uani 1 6 d S T P . .
O4 O 0.4310(2) 0.5885(2) 0.5398(3) 0.037(2) Uani 0.5 1 d . . P . .
C2 C 0.5474(2) 0.6538(4) 0.5474(2) 0.060(3) Uani 1 2 d S T P . .
C1 C 0.5321(4) 0.6700(3) 0.5800(3) 0.077(4) Uani 1 2 d S T P . .
H1 H 0.510888 0.658579 0.591423 0.092 Uiso 1 2 calc R U P . .
C3 C 0.5332(3) 0.6168(4) 0.5332(3) 0.064(3) Uani 1 2 d S T P . .
O3 O 0.4419(3) 0.51184(19) 0.51184(19) 0.082(3) Uani 1 2 d S T P . .


_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
Hf1 O2 2.060(6) . ?
Hf1 O3 2.126(9) . ?
Hf1 O3 2.135(6) 101_666 ?
Hf1 O3 2.135(6) 105_666 ?
Hf1 O4 2.162(8) 115 ?
Hf1 O4 2.162(8) . ?
Hf1 O1 2.181(5) . ?
Hf1 O1 2.181(5) 115 ?
Hf1 S1 2.90(6) . ?
Hf1 Hf1 3.4863(9) 5 ?
Hf1 Hf1 3.4863(9) 9 ?
Hf1 Hf1 3.5015(8) 101_666 ?
S1 O4 1.68(4) 115 ?
S1 O4 1.68(4) . ?
S1 S2 2.46(5) . ?
S1 S2 2.46(5) 105_666 ?
O1 C3 1.277(8) . ?
S2 O4 1.542(11) . ?
S2 O4 1.542(11) 14_666 ?
C2 C1 1.378(8) . ?
C2 C1 1.378(8) 60_564 ?
C2 C3 1.470(17) . ?
C1 H1 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
O2 Hf1 O3 101.8(9) . . ?
O2 Hf1 O3 67.0(5) . 101_666 ?
O3 Hf1 O3 69.5(3) . 101_666 ?
O2 Hf1 O3 67.0(5) . 105_666 ?
O3 Hf1 O3 69.5(3) . 105_666 ?
O3 Hf1 O3 107.9(6) 101_666 105_666 ?
O2 Hf1 O4 146.0(3) . 115 ?
O3 Hf1 O4 84.1(4) . 115 ?
O3 Hf1 O4 143.4(3) 101_666 115 ?
O3 Hf1 O4 84.6(4) 105_666 115 ?
O2 Hf1 O4 146.0(3) . . ?
O3 Hf1 O4 84.1(4) . . ?
O3 Hf1 O4 84.6(4) 101_666 . ?
O3 Hf1 O4 143.4(3) 105_666 . ?
O4 Hf1 O4 67.4(5) 115 . ?
O2 Hf1 O1 82.3(7) . . ?
O3 Hf1 O1 142.25(15) . . ?
O3 Hf1 O1 78.3(3) 101_666 . ?
O3 Hf1 O1 141.8(3) 105_666 . ?
O4 Hf1 O1 113.3(3) 115 . ?
O4 Hf1 O1 73.6(3) . . ?
O2 Hf1 O1 82.3(7) . 115 ?
O3 Hf1 O1 142.25(15) . 115 ?
O3 Hf1 O1 141.8(3) 101_666 115 ?
O3 Hf1 O1 78.3(3) 105_666 115 ?
O4 Hf1 O1 73.6(3) 115 115 ?
O4 Hf1 O1 113.3(3) . 115 ?
O1 Hf1 O1 75.4(3) . 115 ?
O2 Hf1 S1 175(2) . . ?
O3 Hf1 S1 72.8(18) . . ?
O3 Hf1 S1 110.4(9) 101_666 . ?
O3 Hf1 S1 110.4(9) 105_666 . ?
O4 Hf1 S1 35.0(5) 115 . ?
O4 Hf1 S1 35.0(5) . . ?
O1 Hf1 S1 101.9(15) . . ?
O1 Hf1 S1 101.9(15) 115 . ?
O2 Hf1 Hf1 32.2(3) . 5 ?
O3 Hf1 Hf1 89.5(3) . 5 ?
O3 Hf1 Hf1 89.5(3) 101_666 5 ?
O3 Hf1 Hf1 35.3(2) 105_666 5 ?
O4 Hf1 Hf1 115.9(3) 115 5 ?
O4 Hf1 Hf1 172.6(3) . 5 ?
O1 Hf1 Hf1 109.72(16) . 5 ?
O1 Hf1 Hf1 74.09(15) 115 5 ?
S1 Hf1 Hf1 145.6(9) . 5 ?
O2 Hf1 Hf1 32.2(3) . 9 ?
O3 Hf1 Hf1 89.5(3) . 9 ?
O3 Hf1 Hf1 35.3(2) 101_666 9 ?
O3 Hf1 Hf1 89.5(3) 105_666 9 ?
O4 Hf1 Hf1 172.6(3) 115 9 ?
O4 Hf1 Hf1 115.9(3) . 9 ?
O1 Hf1 Hf1 74.09(15) . 9 ?
O1 Hf1 Hf1 109.72(16) 115 9 ?
S1 Hf1 Hf1 145.6(9) . 9 ?
Hf1 Hf1 Hf1 60.0 5 9 ?
O2 Hf1 Hf1 83.9(7) . 101_666 ?
O3 Hf1 Hf1 34.83(16) . 101_666 ?
O3 Hf1 Hf1 34.7(2) 101_666 101_666 ?
O3 Hf1 Hf1 89.0(3) 105_666 101_666 ?
O4 Hf1 Hf1 115.1(2) 115 101_666 ?
O4 Hf1 Hf1 82.6(3) . 101_666 ?
O1 Hf1 Hf1 110.66(15) . 101_666 ?
O1 Hf1 Hf1 164.08(15) 115 101_666 ?
S1 Hf1 Hf1 91.4(16) . 101_666 ?
Hf1 Hf1 Hf1 90.0 5 101_666 ?
Hf1 Hf1 Hf1 60.141(9) 9 101_666 ?
O4 S1 O4 91(3) 115 . ?
O4 S1 S2 119(4) 115 . ?
O4 S1 S2 38.2(12) . . ?
O4 S1 S2 38.2(12) 115 105_666 ?
O4 S1 S2 119(4) . 105_666 ?
S2 S1 S2 124(4) . 105_666 ?
O4 S1 Hf1 47.7(17) 115 . ?
O4 S1 Hf1 47.7(17) . . ?
S2 S1 Hf1 71.2(17) . . ?
S2 S1 Hf1 71.2(17) 105_666 . ?
C3 O1 Hf1 130.9(6) . . ?
O4 S2 O4 145(2) . 14_666 ?
O4 S2 S1 42.3(14) . . ?
O4 S2 S1 133(2) 14_666 . ?
O4 S2 S1 133(2) . 101_666 ?
O4 S2 S1 42.3(14) 14_666 101_666 ?
S1 S2 S1 170(4) . 101_666 ?
Hf1 O2 Hf1 115.6(6) . 9 ?
Hf1 O2 Hf1 115.6(6) . 5 ?
Hf1 O2 Hf1 115.6(6) 9 5 ?
S2 O4 S1 100(2) . . ?
S2 O4 Hf1 114.9(11) . . ?
S1 O4 Hf1 97(2) . . ?
C1 C2 C1 118.3(12) . 60_564 ?
C1 C2 C3 120.5(6) . . ?
C1 C2 C3 120.5(6) 60_564 . ?
C2 C1 C2 121.7(12) 78_456 . ?
C2 C1 H1 119.2 78_456 . ?
C2 C1 H1 119.2 . . ?
O1 C3 O1 127.4(11) 120 . ?
O1 C3 C2 116.0(6) 120 . ?
O1 C3 C2 116.0(6) . . ?
Hf1 O3 Hf1 110.5(3) . 105_666 ?
Hf1 O3 Hf1 110.5(3) . 101_666 ?
Hf1 O3 Hf1 109.5(5) 105_666 101_666 ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O4 S2 O4 S1 -102(3) 14_666 . . . ?
S1 S2 O4 S1 -167(4) 101_666 . . . ?
O4 S2 O4 Hf1 0.5(3) 14_666 . . . ?
S1 S2 O4 Hf1 103(3) . . . . ?
S1 S2 O4 Hf1 -64(2) 101_666 . . . ?
O4 S1 O4 S2 138(3) 115 . . . ?
S2 S1 O4 S2 110(4) 105_666 . . . ?
Hf1 S1 O4 S2 116.8(14) . . . . ?
O4 S1 O4 Hf1 21(4) 115 . . . ?
S2 S1 O4 Hf1 -116.8(14) . . . . ?
S2 S1 O4 Hf1 -7(4) 105_666 . . . ?
C1 C2 C1 C2 3(3) 60_564 . . 78_456 ?
C3 C2 C1 C2 173.2(11) . . . 78_456 ?
Hf1 O1 C3 O1 21(2) . . . 120 ?
Hf1 O1 C3 C2 -167.9(8) . . . . ?
C1 C2 C3 O1 -178.7(13) . . . 120 ?
C1 C2 C3 O1 -9(2) 60_564 . . 120 ?
C1 C2 C3 O1 9(2) . . . . ?
C1 C2 C3 O1 178.7(13) 60_564 . . . ?

_refine_diff_density_max         2.007
_refine_diff_density_min         -1.498
_refine_diff_density_rms         0.159


loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?



_publcif_funding_html            
;
;
