#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/12/14/4121466.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_4121466
loop_
_publ_author_name
'Furukawa, Hiroyasu'
'Gándara, Felipe'
'Zhang, Yue-Biao'
'Jiang, Juncong'
'Queen, Wendy L.'
'Hudson, Matthew R.'
'Yaghi, Omar M.'
_publ_section_title
;
 Water adsorption in porous metal-organic frameworks and related
 materials.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4369
_journal_page_last               4381
_journal_paper_doi               10.1021/ja500330a
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         '0.25(C336 H96 O176 Zr24), 5.5(O)'
_chemical_formula_sum            'C84 H24 O49.5 Zr6'
_chemical_formula_weight         2372.35
_chemical_name_systematic        MOF-806
_space_group_crystal_system      cubic
_space_group_IT_number           202
_space_group_name_Hall           '-F 2 2 3'
_space_group_name_H-M_alt        'F m -3'
_symmetry_space_group_name_Hall  '-F 2 2 3'
_symmetry_space_group_name_H-M   'F m -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2013.12.10 svn.r2850 for OlexSys, GUI svn.r4736)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.8514(7)
_cell_length_b                   26.8514(7)
_cell_length_c                   26.8514(7)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100
_cell_measurement_theta_max      59.90
_cell_measurement_theta_min      2.85
_cell_volume                     19359.8(9)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.826
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Photon-100'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0099
_diffrn_reflns_Laue_measured_fraction_full 0.826
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            24557
_diffrn_reflns_point_group_measured_fraction_full 0.826
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         59.895
_diffrn_reflns_theta_min         2.850
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.984
_exptl_absorpt_correction_T_max  0.7517
_exptl_absorpt_correction_T_min  0.6920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.814
_exptl_crystal_description       prism
_exptl_crystal_F_000             4656
_refine_diff_density_max         1.103
_refine_diff_density_min         -0.531
_refine_diff_density_rms         0.179
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.297
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.297
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0631
_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)+(0.1422P)²+194.6438P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2346
_refine_ls_wR_factor_ref         0.2388
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1211
_reflns_number_total             1302
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja500330a_si_006.cif
_cod_data_source_block           mof-806
_cod_original_cell_volume        19359.8(15)
_cod_original_formula_sum        'C84 H24 O49.50 Zr6'
_cod_database_code               4121466
#BEGIN Tags that were not found in dictionaries:
_shelxl_version_number           2013-4
_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. Uiso/Uaniso restraints and constraints
Uanis(O4) = Uanis(O9) = Uanis(O8) = Uanis(O5)
3. Others
 Fixed Sof: O1(0.16667) O4(0.125) O5(0.125) O6(0.16667) O7(0.0625)
 O1B(0.16667) O8(0.125) O9(0.125)
4.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C7(H7)
;
#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'
'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'
'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'
'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'
'-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'
'-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'
'-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'
'-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'
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 0.5000 0.0000 0.09200(3) 0.0220(7) Uani 1 4 d S T P .
O1 O 0.4605(4) 0.0395(4) 0.0395(4) 0.018(4) Uani 0.5 3 d S T P 1
O3 O 0.3664(3) 0.0000 0.0713(3) 0.065(2) Uani 1 2 d S T P .
O2 O 0.4284(3) 0.0000 0.1336(3) 0.066(2) Uani 1 2 d S T P .
C1 C 0.3822(5) 0.0000 0.1175(5) 0.070(3) Uani 1 2 d S T P .
C2 C 0.3431(5) 0.0000 0.1569(5) 0.089(5) Uani 1 2 d S T P .
O4 O 0.4043(15) 0.0000 0.2254(16) 0.09(2) Uani 0.25 2 d S T P 2
O5 O 0.2749(16) 0.0000 0.0961(15) 0.09(2) Uani 0.25 2 d S T P 2
O6 O 0.3874(7) -0.1126(7) 0.1126(7) 0.118(10) Uani 0.5 3 d S T P .
O7 O 0.5000 0.0000 0.207(2) 0.086(15) Uiso 0.25 4 d S T P .
O1B O 0.4476(4) 0.0524(4) 0.0524(4) 0.030(5) Uani 0.5 3 d S T P 2
O8 O 0.280(2) -0.032(3) 0.100(2) 0.09(2) Uani 0.125 1 d . . P 1
O9 O 0.400(2) 0.032(3) 0.220(2) 0.09(2) Uani 0.125 1 d . . P 1
C3 C 0.2930(6) 0.0000 0.1432(6) 0.126(8) Uani 1 2 d S T P .
C4 C 0.3565(7) 0.0000 0.2069(6) 0.126(8) Uani 1 2 d S T P .
C5 C 0.3177(6) 0.0000 0.2422(7) 0.153(10) Uani 1 2 d S T P .
H5 H 0.3262 0.0000 0.2765 0.183 Uiso 1 2 calc RS T P .
C6 C 0.2702(6) 0.0000 0.2299(6) 0.114(6) Uani 1 2 d S T P .
C7 C 0.2576(7) 0.0000 0.1823(6) 0.155(10) Uani 1 2 d S T P .
H7 H 0.2233 0.0000 0.1740 0.186 Uiso 1 2 calc RS 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 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -0.1862 2.2449 '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
O1 Zr1 O1 62.1(5) . 51
O1 Zr1 O1 93.7(9) . 2_655
O1 Zr1 O1 62.1(5) 51 2_655
O1 Zr1 O1 62.1(5) . 52_655
O1 Zr1 O1 93.7(9) 51 52_655
O1 Zr1 O1 62.1(5) 2_655 52_655
O1 Zr1 O3 84.2(4) . 34
O1 Zr1 O3 142.21(13) 51 34
O1 Zr1 O3 142.21(13) 2_655 34
O1 Zr1 O3 84.2(4) 52_655 34
O1 Zr1 O3 142.21(13) . 81
O1 Zr1 O3 84.2(4) 51 81
O1 Zr1 O3 84.2(4) 2_655 81
O1 Zr1 O3 142.21(13) 52_655 81
O1 Zr1 O2 142.16(13) 52_655 .
O1 Zr1 O2 84.2(4) . .
O1 Zr1 O2 84.2(4) 51 .
O1 Zr1 O2 142.16(13) 2_655 .
O1 Zr1 O2 142.16(13) . 2_655
O1 Zr1 O2 142.16(13) 51 2_655
O1 Zr1 O2 84.2(4) 2_655 2_655
O1 Zr1 O2 84.2(4) 52_655 2_655
O3 Zr1 O3 119.4(5) 34 81
O3 Zr1 O2 75.32(16) 34 .
O3 Zr1 O2 75.32(16) 81 .
O3 Zr1 O2 75.32(16) 34 2_655
O3 Zr1 O2 75.32(16) 81 2_655
O3 Zr1 O1B 72.5(4) 81 2_655
O3 Zr1 O1B 140.92(11) 34 51
O3 Zr1 O1B 140.92(11) 81 .
O3 Zr1 O1B 72.5(4) 34 .
O3 Zr1 O1B 72.5(4) 81 51
O3 Zr1 O1B 72.5(4) 34 52_655
O3 Zr1 O1B 140.92(11) 81 52_655
O3 Zr1 O1B 140.92(11) 34 2_655
O2 Zr1 O2 119.6(5) . 2_655
O2 Zr1 O1B 140.90(11) 2_655 51
O2 Zr1 O1B 72.4(4) . 51
O2 Zr1 O1B 72.4(4) . .
O2 Zr1 O1B 140.91(11) 2_655 .
O2 Zr1 O1B 72.4(4) 2_655 2_655
O2 Zr1 O1B 72.4(4) 2_655 52_655
O2 Zr1 O1B 140.90(11) . 2_655
O2 Zr1 O1B 140.90(11) . 52_655
O1B Zr1 O1B 77.1(3) . 52_655
O1B Zr1 O1B 123.7(8) 51 52_655
O1B Zr1 O1B 77.1(3) . 51
O1B Zr1 O1B 77.1(3) 52_655 2_655
O1B Zr1 O1B 77.1(3) 51 2_655
O1B Zr1 O1B 123.7(8) . 2_655
Zr1 O1 Zr1 116.1(3) . 89
Zr1 O1 Zr1 116.1(3) . 33_554
Zr1 O1 Zr1 116.1(3) 89 33_554
C1 O3 Zr1 130.8(7) . 89
C1 O2 Zr1 130.6(7) . .
O3 C1 O2 128.1(10) . .
O3 C1 C2 116.4(12) . .
O2 C1 C2 115.5(12) . .
C3 C2 C1 119.4(14) . .
C4 C2 C1 120.3(14) . .
C4 C2 C3 120.3(13) . .
Zr1 O1B Zr1 101.5(5) . 89
Zr1 O1B Zr1 101.5(5) . 33_554
Zr1 O1B Zr1 101.5(5) 89 33_554
C3 O8 O8 54(3) . 51
C4 O9 O9 55(3) . 51
C2 C3 O8 115(2) . 51
C2 C3 O8 115(2) . .
C2 C3 C7 116.8(16) . .
O5 C3 C2 126(2) . .
O5 C3 C7 117(2) . .
O8 C3 O8 71(5) . 51
C7 C3 O8 115(2) . 51
C7 C3 O8 115(2) . .
C2 C4 O9 116(2) . .
C2 C4 O9 116(2) . 51
C2 C4 C5 117.2(16) . .
O4 C4 C2 126(2) . .
O4 C4 C5 117(2) . .
O9 C4 O9 70(5) 51 .
C5 C4 O9 115(2) . .
C5 C4 O9 115(2) . 51
C6 C5 C4 123.3(18) . .
C5 C6 C6 121(2) . 73
C5 C6 C7 119.3(16) . .
C7 C6 C6 120(2) . 73
C6 C7 C3 123.2(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Zr1 O1 2.059(3) .
Zr1 O1 2.059(3) 51
Zr1 O1 2.059(3) 2_655
Zr1 O1 2.059(3) 52_655
Zr1 O3 2.217(7) 34
Zr1 O3 2.217(7) 81
Zr1 O2 2.223(7) .
Zr1 O2 2.223(7) 2_655
Zr1 O1B 2.256(8) .
Zr1 O1B 2.256(8) 51
Zr1 O1B 2.256(8) 52_655
Zr1 O1B 2.256(8) 2_655
O1 Zr1 2.059(3) 89
O1 Zr1 2.059(3) 33_554
O3 Zr1 2.217(7) 89
O3 C1 1.310(16) .
O2 C1 1.316(15) .
C1 C2 1.490(17) .
C2 C3 1.40(2) .
C2 C4 1.39(2) .
O4 C4 1.38(5) .
O5 C3 1.35(5) .
O1B Zr1 2.256(8) 89
O1B Zr1 2.256(8) 33_554
O8 O8 1.75(16) 51
O8 C3 1.50(7) .
O9 O9 1.73(16) 51
O9 C4 1.50(8) .
C3 O8 1.50(7) 51
C3 C7 1.42(2) .
C4 O9 1.50(8) 51
C4 C5 1.41(2) .
C5 C6 1.32(2) .
C6 C6 1.53(3) 73
C6 C7 1.32(2) .
