# Electronic Supplementary Material (ESI) for Inorganic Chemistry Frontiers.
# This journal is © The Royal Society of Chemistry 2014


data_UiO67

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C84 H48 O32 Zr6'
_chemical_formula_weight         2116.54

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'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           cubic
_symmetry_space_group_name_H-M   Fm-3m

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

_cell_length_a                   26.896(3)
_cell_length_b                   26.896(3)
_cell_length_c                   26.896(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     19458(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    357
_cell_measurement_theta_min      3.54
_cell_measurement_theta_max      19.85

_exptl_crystal_description       octahedral
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    0.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4192
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9897
_exptl_absorpt_correction_T_max  0.9897
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(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  'STOE IPDS II'
_diffrn_measurement_method       'omega scan'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            4307
_diffrn_reflns_av_R_equivalents  0.1445
_diffrn_reflns_av_sigmaI/netI    0.1439
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         1.51
_diffrn_reflns_theta_max         25.67
_reflns_number_total             977
_reflns_number_gt                537
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       X-Area
_computing_cell_refinement       X-Area
_computing_data_reduction        X-Area
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    Diamond
_computing_publication_material  publCIF

_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)+(0.0866P)²+0.0000P] 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_number_reflns         977
_refine_ls_number_parameters     37
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1268
_refine_ls_R_factor_gt           0.0768
_refine_ls_wR_factor_ref         0.1887
_refine_ls_wR_factor_gt          0.1755
_refine_ls_goodness_of_fit_ref   0.893
_refine_ls_restrained_S_all      0.893
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.09204(6) 0.0000 0.0000 0.0224(5) Uani 1 8 d S . .
O1 O 0.0454(4) 0.0454(4) 0.0454(4) 0.060(4) Uani 1 6 d S . .
O2 O 0.1326(2) 0.0000 0.0719(2) 0.0421(18) Uani 1 2 d S . .
C1 C 0.1172(4) 0.0000 0.1172(4) 0.039(3) Uani 1 4 d S . .
C2 C 0.1565(4) 0.0000 0.1565(4) 0.056(4) Uani 1 4 d S . .
C3 C 0.2058(5) 0.0000 0.1447(5) 0.127(9) Uani 1 2 d S . .
H3 H 0.2149 0.0000 0.1114 0.152 Uiso 1 2 calc SR . .
C4 C 0.2420(5) 0.0000 0.1795(5) 0.146(10) Uani 1 2 d S . .
H4 H 0.2751 0.0000 0.1695 0.175 Uiso 1 2 calc SR . .
C5 C 0.2307(3) 0.0000 0.2307(3) 0.080(7) Uani 1 4 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
Zr1 O1 2.135(5) . ?
Zr1 O1 2.135(5) 4 ?
Zr1 O1 2.135(5) 99 ?
Zr1 O1 2.135(5) 98 ?
Zr1 O2 2.219(6) 17 ?
Zr1 O2 2.219(6) 114 ?
Zr1 O2 2.219(6) 98 ?
Zr1 O2 2.219(6) . ?
Zr1 Zr1 3.501(2) 105 ?
Zr1 Zr1 3.501(2) 101 ?
Zr1 Zr1 3.501(2) 5 ?
Zr1 Zr1 3.501(2) 9 ?
O1 Zr1 2.135(5) 5 ?
O1 Zr1 2.135(5) 9 ?
O2 C1 1.287(8) . ?
C1 O2 1.287(8) 22 ?
C1 C2 1.496(19) . ?
C2 C3 1.363(14) . ?
C2 C3 1.363(14) 22 ?
C3 C4 1.351(17) . ?
C3 H3 0.9300 . ?
C4 C5 1.410(16) . ?
C4 H4 0.9300 . ?
C5 C4 1.410(16) 22 ?
C5 C5 1.47(3) 145 ?

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 Zr1 O1 108.1(9) . 4 ?
O1 Zr1 O1 69.8(4) . 99 ?
O1 Zr1 O1 69.8(4) 4 99 ?
O1 Zr1 O1 69.8(4) . 98 ?
O1 Zr1 O1 69.8(4) 4 98 ?
O1 Zr1 O1 108.1(9) 99 98 ?
O1 Zr1 O2 77.9(4) . 17 ?
O1 Zr1 O2 141.90(7) 4 17 ?
O1 Zr1 O2 141.90(7) 99 17 ?
O1 Zr1 O2 77.9(4) 98 17 ?
O1 Zr1 O2 141.90(7) . 114 ?
O1 Zr1 O2 77.9(4) 4 114 ?
O1 Zr1 O2 77.9(4) 99 114 ?
O1 Zr1 O2 141.90(7) 98 114 ?
O2 Zr1 O2 121.2(4) 17 114 ?
O1 Zr1 O2 141.90(7) . 98 ?
O1 Zr1 O2 77.9(4) 4 98 ?
O1 Zr1 O2 141.90(7) 99 98 ?
O1 Zr1 O2 77.9(4) 98 98 ?
O2 Zr1 O2 76.05(16) 17 98 ?
O2 Zr1 O2 76.05(16) 114 98 ?
O1 Zr1 O2 77.9(4) . . ?
O1 Zr1 O2 141.90(7) 4 . ?
O1 Zr1 O2 77.9(4) 99 . ?
O1 Zr1 O2 141.90(7) 98 . ?
O2 Zr1 O2 76.05(16) 17 . ?
O2 Zr1 O2 76.05(16) 114 . ?
O2 Zr1 O2 121.2(4) 98 . ?
O1 Zr1 Zr1 89.4(4) . 105 ?
O1 Zr1 Zr1 34.9(2) 4 105 ?
O1 Zr1 Zr1 89.4(4) 99 105 ?
O1 Zr1 Zr1 34.9(2) 98 105 ?
O2 Zr1 Zr1 110.32(12) 17 105 ?
O2 Zr1 Zr1 110.32(12) 114 105 ?
O2 Zr1 Zr1 74.41(18) 98 105 ?
O2 Zr1 Zr1 164.41(18) . 105 ?
O1 Zr1 Zr1 89.4(4) . 101 ?
O1 Zr1 Zr1 34.9(2) 4 101 ?
O1 Zr1 Zr1 34.9(2) 99 101 ?
O1 Zr1 Zr1 89.4(4) 98 101 ?
O2 Zr1 Zr1 164.41(18) 17 101 ?
O2 Zr1 Zr1 74.41(18) 114 101 ?
O2 Zr1 Zr1 110.32(12) 98 101 ?
O2 Zr1 Zr1 110.32(12) . 101 ?
Zr1 Zr1 Zr1 60.0 105 101 ?
O1 Zr1 Zr1 34.9(2) . 5 ?
O1 Zr1 Zr1 89.4(4) 4 5 ?
O1 Zr1 Zr1 89.4(4) 99 5 ?
O1 Zr1 Zr1 34.9(2) 98 5 ?
O2 Zr1 Zr1 74.41(18) 17 5 ?
O2 Zr1 Zr1 164.41(18) 114 5 ?
O2 Zr1 Zr1 110.32(12) 98 5 ?
O2 Zr1 Zr1 110.32(12) . 5 ?
Zr1 Zr1 Zr1 60.0 105 5 ?
Zr1 Zr1 Zr1 90.0 101 5 ?
O1 Zr1 Zr1 34.9(2) . 9 ?
O1 Zr1 Zr1 89.4(4) 4 9 ?
O1 Zr1 Zr1 34.9(2) 99 9 ?
O1 Zr1 Zr1 89.4(4) 98 9 ?
O2 Zr1 Zr1 110.32(12) 17 9 ?
O2 Zr1 Zr1 110.32(12) 114 9 ?
O2 Zr1 Zr1 164.41(18) 98 9 ?
O2 Zr1 Zr1 74.41(18) . 9 ?
Zr1 Zr1 Zr1 90.0 105 9 ?
Zr1 Zr1 Zr1 60.0 101 9 ?
Zr1 Zr1 Zr1 60.0 5 9 ?
Zr1 O1 Zr1 110.2(4) . 5 ?
Zr1 O1 Zr1 110.2(4) . 9 ?
Zr1 O1 Zr1 110.2(4) 5 9 ?
C1 O2 Zr1 131.9(7) . . ?
O2 C1 O2 127.4(12) . 22 ?
O2 C1 C2 116.3(6) . . ?
O2 C1 C2 116.3(6) 22 . ?
C3 C2 C3 116.9(15) . 22 ?
C3 C2 C1 121.6(7) . . ?
C3 C2 C1 121.6(7) 22 . ?
C4 C3 C2 122.7(13) . . ?
C4 C3 H3 118.6 . . ?
C2 C3 H3 118.6 . . ?
C3 C4 C5 121.4(13) . . ?
C3 C4 H4 119.3 . . ?
C5 C4 H4 119.3 . . ?
C4 C5 C4 114.9(15) . 22 ?
C4 C5 C5 122.6(7) . 145 ?
C4 C5 C5 122.6(7) 22 145 ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.67
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.812
_refine_diff_density_min         -1.101
_refine_diff_density_rms         0.149

# 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 0.321 -0.007 -0.005 13440 3388 ' '
_platon_squeeze_details          
;
;
_database_code_depnum_ccdc_archive 'CCDC 960486'
