# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_publication_text
_database_code_depnum_ccdc_archive 'CCDC 1490700'
_audit_update_record             
;
2016-07-05 deposited with the CCDC.
2016-11-08 downloaded from the CCDC.
;
_cell_length_a                   20.1413(24)
_cell_length_b                   34.892(10)
_cell_length_c                   11.19392(74)
_cell_angle_alpha                90.000
_cell_angle_beta                 90.000
_cell_angle_gamma                90.000
_cell_volume                     7866.8(2)
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   CMMM
_symmetry_int_tables_number      65
_chemical_absolute_configuration ?
_symmetry_space_group_name_Hall  -C22
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 -x,-y,-z
2 -x,-y,z
3 -x,y,-z
4 -x,y,z
5 -x+1/2,-y+1/2,-z
6 -x+1/2,-y+1/2,z
7 -x+1/2,y+1/2,-z
8 -x+1/2,y+1/2,z
9 x,-y,-z
10 x,-y,z
11 x,y,-z
12 x,y,z
13 x+1/2,-y+1/2,-z
14 x+1/2,-y+1/2,z
15 x+1/2,y+1/2,-z
16 x+1/2,y+1/2,z
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_radius_bond
Zr ? 1.200
O ? 1.200
C ? 1.200

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Zr1 Zr 0 -0.91887(67) 0 0.1535(11) 1 8.00(97)
Zr2 Zr 0 -0.5 -0.43432(49) 0 1 8.00(97)
O1 O 0 -0.56547(92) 0.39402(71) 0.1020(16) 1 8.0(19)
O2 O 0 -0.1021(10) -0.05759(55) 0.2195(21) 1 8.0(19)
O3 O 0 -0.81495(97) 0 0.1287(48) 1 8.0(19)
O4 O 0 -0.0593(13) 0 0.3460(21) 1 8.0(19)
O5 O 0 -1 -0.03966(87) 1.1793(22) 1 8.0(19)
O6 O 0 -0.8968(20) -0.03714(93) 0 1 8.0(19)
C3 C 0 -0.2151846 -0.219867 0.4373874 1 8.0(15)
C4 C 0 -0.1899218 -0.1870023 0.3691041 1 8.0(15)
C5 C 0 -0.1327918 -0.1921697 0.3007653 1 8.0(15)
C6 C 0 -0.1047615 -0.1613072 0.2412782 1 8.0(15)
C7 C 0 -0.219785 -0.1506542 0.3747721 1 8.0(15)
C8 C 0 -0.09934975 -0.09314622 0.1870015 1 8.0(15)
C9 C 0 -0.1329249 -0.1246366 0.2493083 1 8.0(15)
C10 C 0 -0.1910847 -0.1193688 0.3157231 1 8.0(15)
C19 C 0 0.75 0.25 0.3769(39) 1 8.0(15)
OG1 O 0 -0.9602(29) 0.1552(15) 1.4175(55) 0.652(37) 8.0(15)
OG2 O 0 0.5 0.5 0.5 1.000(86) 8.0(15)

_chemical_formula_moiety         'C68 O32 Zr6, 2.608(O2), O'
_chemical_formula_sum            'C68 O38.22 Zr6'
_chemical_formula_weight         1468
_diffrn_ambient_temperature      298
_diffrn_ambient_pressure         1013
_cell_measurement_temperature    298
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.826215
_diffrn_source_type              'STOE StadiP Mythen'
_diffrn_measured_fraction_theta_full 30
# start Validation Reply Form
_vrf_EXPT005_ALERT_1_A           
;
PROBLEM: _exptl_crystal_description is missing Crystal habit description.
RESPONSE: No Crystals observed. Rietveld refined structure.
;
_vrf_DIFF003_1_A                 
;
PROBLEM: _diffrn_measurement_device_type is missing
            Diffractometer make and type. Replaces _diffrn_measurement_type.
RESPONSE: No Crystals observed. Rietveld refined structure.
;
_vrf_ATOM007_1_A                 
;
PROBLEM: _atom_site_aniso_label_1 is missing
RESPONSE: Rietveld refined structure. Anisotropy meaningless.
;
_vrf_GEOM001_1_A                 
;
PROBLEM: _geom_bond_atom_site_label_1 is missing
RESPONSE: Geometry not given as model refined by the Rietveld method.
;
_vrf_GEOM003_1_A                 
;
PROBLEM: _geom_bond_distance is missing
RESPONSE: Geometry not given as model refined by the Rietveld method.
;
_vrf_GEOM006_1_A                 
;
PROBLEM: _geom_angle_atom_site_label_2 is missing
RESPONSE: Geometry not given as model refined by the Rietveld method.
;
_vrf_GEOM007_1_A                 
;
PROBLEM: _geom_angle_atom_site_label_3 is missing
RESPONSE: Geometry not given as model refined by the Rietveld method.
;
_vrf_PLAT043_ALERT_1_A           
;
PROBLEM: check reported molecular weight
RESPONSE: reported molecular weight is the calculated molecular weight withouth the hydrogen atoms since these cannot be refined by the Rietveld method.
;
_vrf_PLAT183_ALERT_1_A           
;
PROBLEM:  Missing _cell_measurement_reflns_used value
RESPONSE: No Crystals observed. Rietveld refined structure.
;
_vrf_PLAT184_ALERT_1_A           
;
PROBLEM:  Missing _cell_measurement_reflns_used value
RESPONSE: No Crystals observed. Rietveld refined structure.
;
_vrf_PLAT185_ALERT_1_A           
;
PROBLEM:  Missing _cell_measurement_reflns_used value
RESPONSE: No Crystals observed. Rietveld refined structure.
;
_vrf_PLAT602_ALERT_2_A           
;
PROBLEM:  VERY LARGE Solvent Accessible VOID(S) in Structure
RESPONSE: Structure is a porous structure. Electron densities were searched by fourier analysis and marked as OG.
;
_vrf_PLAT049_ALERT_1_B           
;
PROBLEM:  Calculated Density less than 1.0 gcm-3
RESPONSE: Structure is a porous structure. 
;
_vrf_PLAT306_ALERT_2_B           
;
PROBLEM:  Isolated Oxygen Atom (H-atoms Missing ?)
RESPONSE: Electron densities were searched by fourier analysis and marked as OG. Hydrogen atoms cannot be refined by the Rietveld method.
;
# end Validation Reply Form
#END


_exptl_crystal_recrystallization_method 'solvothermal synthesis'
