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#$Date: 2016-02-14 05:40:26 +0100 (dom 14 de feb de 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/92/4109209.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_4109209
loop_
_publ_author_name
'Jasmina Hafizovic'
'Morten Bjørgen'
'Unni Olsbye'
'Pascal D. C. Dietzel'
'Silvia Bordiga'
'Carmelo Prestipino'
'Carlo Lamberti'
'Karl Petter Lillerud'
_publ_contact_author_address
;
Department of Chemistry
University of Oslo
P.O. Box 1033 Blindern
N-0315 Oslo
Norway
;
_publ_contact_author_email       k.p.lillerud@kjemi.uio.no
_publ_contact_author_name        'Prof. Karl Petter Lillerud'
_publ_section_title
;
 The Inconsistency in Adsorption Properties and Powder XRD Data of MOF-5
 Is Rationalized by Framework Interpenetration and the Presence of Organic
 and Inorganic Species in the Nanocavities
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3612
_journal_page_last               3620
_journal_paper_doi               10.1021/ja0675447
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C24 H12 O13 Zn4'
_chemical_formula_sum            'C24 H12 O13 Zn4'
_chemical_formula_weight         769.82
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           166
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"'
_symmetry_space_group_name_H-M   'R -3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   18.406(3)
_cell_length_b                   18.406(3)
_cell_length_c                   44.750(9)
_cell_measurement_reflns_used    799
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.05
_cell_measurement_theta_min      2.21
_cell_volume                     13129(4)
_computing_cell_refinement       'Smart (Bruker, 1998)'
_computing_data_collection       'Smart (Bruker, 1998)'
_computing_data_reduction        'SAINT (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker Apex II CCD'
_diffrn_measurement_method       'ω scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1506
_diffrn_reflns_av_sigmaI/netI    0.0765
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            16367
_diffrn_reflns_theta_full        19.05
_diffrn_reflns_theta_max         19.05
_diffrn_reflns_theta_min         2.21
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    1.103
_exptl_absorpt_correction_T_max  0.9169
_exptl_absorpt_correction_T_min  0.9169
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1997)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    0.584
_exptl_crystal_description       Cube
_exptl_crystal_F_000             2280
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     79
_refine_ls_number_reflns         1344
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1100
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1583P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2240
_refine_ls_wR_factor_ref         0.2401
_reflns_number_gt                1021
_reflns_number_total             1344
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0675447si20070105_035922.cif
_cod_data_source_block           mof-5_m_zn
_cod_original_sg_symbol_Hall     '-R 3 2'
_cod_original_sg_symbol_H-M      'R -3 m'
_cod_database_code               4109209
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z'
'x-y, -y, -z'
'-x, -x+y, -z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'y+2/3, x+1/3, -z+1/3'
'x-y+2/3, -y+1/3, -z+1/3'
'-x+2/3, -x+y+1/3, -z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'y+1/3, x+2/3, -z+2/3'
'x-y+1/3, -y+2/3, -z+2/3'
'-x+1/3, -x+y+2/3, -z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z'
'-x+y, y, z'
'x, x-y, z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-y+2/3, -x+1/3, z+1/3'
'-x+y+2/3, y+1/3, z+1/3'
'x+2/3, x-y+1/3, z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'-y+1/3, -x+2/3, z+2/3'
'-x+y+1/3, y+2/3, z+2/3'
'x+1/3, x-y+2/3, z+2/3'
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
O1 O 0.6667 0.3333 0.0818(3) 0.026(3) Uani 1 6 d S
Zn1 Zn 0.72425(5) 0.27575(5) 0.06898(3) 0.0543(9) Uani 1 2 d S
Zn2 Zn 0.6667 0.3333 0.12724(6) 0.0539(11) Uani 1 6 d S
O2 O 0.7227(4) 0.2773(4) 0.1432(2) 0.087(4) Uani 1 2 d S
O3 O 0.7648(3) 0.2352(3) 0.1014(3) 0.080(3) Uani 1 2 d S
O4 O 0.8194(5) 0.3465(5) 0.04531(19) 0.094(3) Uani 1 1 d .
C11 C 0.7596(5) 0.2404(5) 0.1291(4) 0.069(5) Uani 1 2 d S
C12 C 0.7967(5) 0.2033(5) 0.1494(4) 0.078(5) Uani 1 2 d S
C13 C 0.8353(6) 0.1647(6) 0.1353(4) 0.090(6) Uani 1 2 d S
H13 H 0.8366 0.1634 0.1146 0.108 Uiso 1 2 calc SR
C14 C 0.7936(6) 0.2064(6) 0.1812(5) 0.101(6) Uani 1 2 d S
H14 H 0.7676 0.2324 0.1907 0.121 Uiso 1 2 calc SR
C21 C 0.8518(11) 0.4259(5) 0.0365(4) 0.090(6) Uani 1 2 d S
C22 C 0.9217(11) 0.4609(6) 0.0184(4) 0.077(5) Uani 1 2 d S
C23 C 0.9628(7) 0.5482(8) 0.0095(3) 0.105(4) Uani 1 1 d .
H23 H 0.9412 0.5815 0.0162 0.126 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.023(5) 0.023(5) 0.032(8) 0.000 0.000 0.012(2)
Zn1 0.0529(11) 0.0529(11) 0.0565(14) -0.0011(4) 0.0011(4) 0.0259(10)
Zn2 0.0548(14) 0.0548(14) 0.052(2) 0.000 0.000 0.0274(7)
O2 0.110(7) 0.110(7) 0.073(8) 0.016(3) -0.016(3) 0.079(8)
O3 0.087(6) 0.087(6) 0.073(8) 0.014(3) -0.014(3) 0.049(7)
O4 0.065(6) 0.076(6) 0.109(6) 0.013(5) 0.040(5) 0.011(5)
C11 0.088(10) 0.088(10) 0.072(14) 0.004(6) -0.004(6) 0.073(11)
C12 0.084(10) 0.084(10) 0.107(19) -0.014(5) 0.014(5) 0.074(11)
C13 0.113(11) 0.113(11) 0.059(11) 0.029(7) -0.029(7) 0.067(13)
C14 0.116(12) 0.116(12) 0.065(13) 0.004(7) -0.004(7) 0.053(14)
C21 0.036(12) 0.137(17) 0.062(12) 0.006(5) 0.012(10) 0.018(6)
C22 0.057(12) 0.091(11) 0.072(12) -0.001(5) -0.003(10) 0.029(6)
C23 0.068(9) 0.101(11) 0.118(12) 0.026(8) 0.028(8) 0.022(8)
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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'
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
Zn1 O1 Zn1 111.5(3) . 3_665
Zn1 O1 Zn1 111.5(3) . 2_655
Zn1 O1 Zn1 111.5(3) 3_665 2_655
Zn1 O1 Zn2 107.3(3) . .
Zn1 O1 Zn2 107.3(3) 3_665 .
Zn1 O1 Zn2 107.3(3) 2_655 .
O4 Zn1 O4 107.1(5) 22_665 .
O4 Zn1 O1 111.2(3) 22_665 .
O4 Zn1 O1 111.2(3) . .
O4 Zn1 O3 106.3(3) 22_665 .
O4 Zn1 O3 106.3(3) . .
O1 Zn1 O3 114.3(5) . .
O2 Zn2 O2 107.1(4) . 2_655
O2 Zn2 O2 107.1(4) . 3_665
O2 Zn2 O2 107.1(4) 2_655 3_665
O2 Zn2 O1 111.8(4) . .
O2 Zn2 O1 111.8(4) 2_655 .
O2 Zn2 O1 111.8(4) 3_665 .
C11 O2 Zn2 130.2(10) . .
C11 O3 Zn1 130.8(11) . .
C21 O4 Zn1 132.1(9) . .
O3 C11 O2 125.6(14) . .
O3 C11 C12 120.0(15) . .
O2 C11 C12 114.4(16) . .
C13 C12 C14 121.0(16) . .
C13 C12 C11 115.4(17) . .
C14 C12 C11 123.6(16) . .
C12 C13 C14 120.9(16) . 25_655
C12 C13 H13 119.5 . .
C14 C13 H13 119.5 25_655 .
C13 C14 C12 118.0(17) 25_655 .
C13 C14 H14 121.0 25_655 .
C12 C14 H14 121.0 . .
O4 C21 O4 121.7(15) . 24
O4 C21 C22 119.1(7) . .
O4 C21 C22 119.1(7) 24 .
C21 C22 C23 121.8(8) . .
C21 C22 C23 121.8(8) . 24
C23 C22 C23 116.2(16) . 24
C22 C23 C23 121.8(8) . 6_765
C22 C23 H23 119.1 . .
C23 C23 H23 119.1 6_765 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 Zn1 1.923(4) .
O1 Zn1 1.923(4) 3_665
O1 Zn1 1.923(4) 2_655
O1 Zn2 2.034(12) .
Zn1 O4 1.899(8) 22_665
Zn1 O4 1.899(8) .
Zn1 O3 1.944(10) .
Zn2 O2 1.923(10) .
Zn2 O2 1.923(10) 2_655
Zn2 O2 1.923(10) 3_665
O2 C11 1.334(17) .
O3 C11 1.251(16) .
O4 C21 1.332(9) .
C11 C12 1.49(2) .
C12 C13 1.38(2) .
C12 C14 1.43(2) .
C13 C14 1.42(2) 25_655
C13 H13 0.9300 .
C14 C13 1.42(2) 25_655
C14 H14 0.9300 .
C21 O4 1.332(9) 24
C21 C22 1.38(2) .
C22 C23 1.449(13) .
C22 C23 1.449(13) 24
C23 C23 1.46(2) 6_765
C23 H23 0.9300 .
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
1 -0.025 -0.015 -0.001 10104.7 384.3
