Detailed Structure Analysis of Atomic Positions and Defects in Zirconium Metal‒Organic Frameworks
Øien, Sigurd; Wragg, David; Reinsch, Helge; Svelle, Stian; Bordiga, Silvia; Lamberti, Carlo; Lillerud, Karl Petter; Crystal Growth & Design 14 (2014) 5370–; doi:10.1021/cg501386j

data_4512072
_publ_section_title
;
 Detailed Structure Analysis of Atomic Positions and Defects in Zirconium
 Metal--Organic Frameworks
;
_journal_issue                   11
_journal_name_full               'Crystal Growth &amp; 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       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'MD2 microdiffractometer with MK3 mini-kappa'
_diffrn_measurement_method       '\f 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 \l/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/[\s^2^(Fo^2^)+(0.0456P)^2^+20.2522P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;