#------------------------------------------------------------------------------
#$Date: 2016-03-24 14:32:51 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179667 $
#$URL: svn://www.crystallography.net/cod/cif/4/51/20/4512072.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4512072
loop_
_publ_author_name
'Øien, Sigurd'
'Wragg, David'
'Reinsch, Helge'
'Svelle, Stian'
'Bordiga, Silvia'
'Lamberti, Carlo'
'Lillerud, Karl Petter'
_publ_section_title
;
 Detailed Structure Analysis of Atomic Positions and Defects in Zirconium
 Metal--Organic Frameworks
;
_journal_issue                   11
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              5370
_journal_paper_doi               10.1021/cg501386j
_journal_volume                  14
_journal_year                    2014
_chemical_formula_moiety         'n[(C34.94 H17.47 O32 Zr6), 29.74(O)]'
_chemical_formula_sum            'C34.94 H17.47 O61.74 Zr6'
_chemical_formula_weight         1972.51
_chemical_name_common            UiO-66
_chemical_name_systematic
;
Zr(IV) terephthalate metal-organic framework
;
_space_group_crystal_system      cubic
_space_group_IT_number           225
_space_group_name_Hall           '-F 4 2 3'
_space_group_name_H-M_alt        'F m -3 m'
_symmetry_space_group_name_Hall  '-F 4 2 3'
_symmetry_space_group_name_H-M   'F m -3 m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2014-04-30
_audit_creation_method
;
Olex2 1.2
(compiled 2014.03.20 svn.r2914 for OlexSys, GUI svn.r4816)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7465(2)
_cell_length_b                   20.7465(2)
_cell_length_c                   20.7465(2)
_cell_measurement_reflns_used    6384
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.645
_cell_measurement_theta_min      2.970
_cell_volume                     8929.65(15)
_computing_cell_refinement       'APEX2 v2013.6--2 (Bruker AXS)'
_computing_data_collection       'APEX2 v2013.6--2 (Bruker AXS)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Diamond v3.2i (Brandenburg, 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'APEX2 v2013.6--2 (Bruker AXS)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 13.6986
_diffrn_detector_type            'Marmosaic 225'
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'κ-geometry diffractometer'
_diffrn_measurement_device_type  'MD2 microdiffractometer with MK3 mini-kappa'
_diffrn_measurement_method       'φ scans'
_diffrn_radiation_collimation    'Rh-coated Si focusing mirrors'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.760
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0168
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            12999
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        27.129
_diffrn_reflns_theta_max         32.828
_diffrn_reflns_theta_min         2.970
_diffrn_source                   synchrotron
_diffrn_source_type              'Wiggler, Station I911-3, MAX II, MAXLAB'
_exptl_absorpt_coefficient_mu    0.928
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6050
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.0651 before and 0.0499 after correction.
The Ratio of minimum to maximum transmission is 0.8102.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             3779
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.395
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     53
_refine_ls_number_reflns         739
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0233
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0456P)²+20.2522P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0710
_refine_ls_wR_factor_ref         0.0714
_reflns_Friedel_coverage         0.000
_reflns_number_gt                701
_reflns_number_total             739
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cg501386j_si_001.cif
_cod_data_source_block           66cpub_a
_cod_depositor_comments
'Adding full bibliography for 4512072--4512074.cif.'
_cod_original_cell_volume        8929.7(3)
_cod_database_code               4512072
#BEGIN Tags that were not found in dictionaries:
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Others
 Sof(O1A)=0.16667*(1-FVAR(2))
 Sof(O1B)=0.16667*FVAR(2)
 Sof(O2B)=0.5*(1-FVAR(3))
 Sof(C2)=Sof(C1)=0.25*FVAR(3)
 Sof(O2A)=Sof(C3)=Sof(H3)=0.5*FVAR(3)
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3)
;
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_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'
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_group
Zr1 Zr 0.0000 0.0000 0.11975(2) 0.00837(13) Uani 1 8 d S T P .
O1B O -0.0674(5) -0.0674(5) 0.0674(5) 0.015(2) Uani 0.54(4) 6 d S T P 2
O2A O 0.0940(2) 0.0000 0.17023(19) 0.0202(7) Uani 0.727(7) 2 d S T P 1
O3 O -0.1511(7) -0.1511(7) 0.1511(7) 0.26(2) Uani 0.56(4) 6 d S T P .
O4 O -0.2108(7) -0.2108(7) 0.2108(7) 0.78(4) Uani 1 6 d S T P .
O2B O 0.0825(8) 0.0000 0.1882(6) 0.035(3) Uani 0.273(7) 2 d S T P 2
C2 C 0.20279(12) 0.0000 0.20279(12) 0.0277(10) Uani 0.727(7) 4 d S T P 1
C3 C 0.26712(15) 0.0000 0.18534(15) 0.0541(14) Uani 0.727(7) 2 d S T P 1
H3 H 0.2789 0.0000 0.1411 0.065 Uiso 0.727(7) 2 calc RS T P 1
O1A O -0.0505(5) -0.0505(5) 0.0505(5) 0.006(2) Uani 0.46(4) 6 d S T P 1
C1 C 0.15179(11) 0.0000 0.15179(11) 0.0180(8) Uani 0.727(7) 4 d S T P 1
O6 O 0.396(3) 0.104(3) 0.104(3) 0.72(9) Uani 0.80(11) 6 d S T P .
O5 O 0.373(2) 0.0000 0.0000 1.16(13) Uani 1.8(3) 8 d S T P .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 '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 0.0140 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -1.9670 0.6570 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O2A Zr1 O2A 123.50(17) 110 109
O2A Zr1 O2A 123.50(17) 2 .
O2A Zr1 O2A 77.05(7) 109 .
O2A Zr1 O2A 77.05(7) 109 2
O2A Zr1 O2A 77.05(7) 110 .
O2A Zr1 O2A 77.05(7) 110 2
O2B Zr1 O2B 65.9(4) . 109
O2B Zr1 O2B 65.9(4) 110 2
O2B Zr1 O2B 100.6(8) 110 109
O2B Zr1 O2B 100.6(8) . 2
O2B Zr1 O2B 65.9(4) . 110
O2B Zr1 O2B 65.9(4) 109 2
O1A Zr1 O2A 83.3(4) . 2
O1A Zr1 O2A 83.3(4) 100 109
O1A Zr1 O2A 83.3(4) 2 110
O1A Zr1 O2A 140.95(9) 100 110
O1A Zr1 O2A 83.3(4) 2 .
O1A Zr1 O2A 140.95(9) 100 2
O1A Zr1 O2A 140.95(9) . 110
O1A Zr1 O2A 140.95(9) 2 109
O1A Zr1 O2A 83.3(4) . 109
O1A Zr1 O2A 140.95(9) 99 109
O1A Zr1 O2A 83.3(4) 99 2
O1A Zr1 O2A 83.3(4) 99 110
O1A Zr1 O2A 140.95(9) 2 2
O1A Zr1 O2A 83.3(4) 100 .
O1A Zr1 O2A 140.95(9) 99 .
O1A Zr1 O2A 140.95(9) . .
O1A Zr1 O1A 61.0(6) 100 .
O1A Zr1 O1A 61.0(6) 99 2
O1A Zr1 O1A 91.7(10) 100 99
O1A Zr1 O1A 61.0(6) 99 .
O1A Zr1 O1A 91.7(10) 2 .
O1A Zr1 O1A 61.0(6) 100 2
Zr1 O1B Zr1 102.3(5) . 101
Zr1 O1B Zr1 102.3(5) . 105
Zr1 O1B Zr1 102.3(5) 105 101
C1 O2A Zr1 134.1(3) . .
C3 C2 C3 120.3(3) . 22
C3 C2 C1 119.82(17) . .
C3 C2 C1 119.83(17) 22 .
C2 C3 C3 119.83(17) . 166
C2 C3 H3 120.1 . .
C3 C3 H3 120.1 166 .
Zr1 O1A Zr1 116.7(3) 105 101
Zr1 O1A Zr1 116.7(3) . 101
Zr1 O1A Zr1 116.7(3) . 105
O2A C1 O2A 125.4(5) . 22
O2A C1 C2 117.3(2) 22 .
O2A C1 C2 117.3(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O2A 2.213(5) 110
Zr1 O2A 2.213(5) 2
Zr1 O2A 2.213(5) 109
Zr1 O2A 2.213(5) .
Zr1 O2B 2.225(15) .
Zr1 O2B 2.225(15) 109
Zr1 O2B 2.225(15) 110
Zr1 O2B 2.225(15) 2
Zr1 O1A 2.064(3) 100
Zr1 O1A 2.064(3) .
Zr1 O1A 2.064(3) 99
Zr1 O1A 2.064(3) 2
O1B Zr1 2.256(8) 101
O1B Zr1 2.256(8) 105
O2A C1 1.259(4) .
C2 C3 1.383(4) 22
C2 C3 1.383(4) .
C2 C1 1.496(5) .
C3 C3 1.395(6) 166
C3 H3 0.9500 .
O1A Zr1 2.064(3) 105
O1A Zr1 2.064(3) 101
C1 O2A 1.260(4) 22
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_4
Zr1 O2A C1 O2A 0.000(0) . 22
Zr1 O2A C1 C2 180.000(0) . .
C3 C2 C3 C3 0.000(0) 22 166
C3 C2 C1 O2A 0.000(0) 22 .
C3 C2 C1 O2A 0.000(0) . 22
C3 C2 C1 O2A 180.000(0) 22 22
C3 C2 C1 O2A 180.000(0) . .
C1 C2 C3 C3 180.000(0) . 166
