Water adsorption in porous metal-organic frameworks and related materials.
Furukawa, Hiroyasu; Gándara, Felipe; Zhang, Yue-Biao; Jiang, Juncong; Queen, Wendy L.; Hudson, Matthew R.; Yaghi, Omar M.; Journal of the American Chemical Society 136 (2014) 4369–4381; doi:10.1021/ja500330a

data_4121460
_publ_section_title
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 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         'C48 H24 O64 Zr12, 17.17(O)'
_chemical_formula_sum            'C48 H24 O81.17 Zr12'
_chemical_formula_weight         2993.98
_chemical_name_systematic        MOF-801(SC)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2013-11-20
_audit_creation_method
;
Olex2 1.2
(compiled 2013.11.15 svn.r2834 for OlexSys, GUI svn.r4715)
;
_cell_angle_alpha                90.031(6)
_cell_angle_beta                 90.182(6)
_cell_angle_gamma                89.999(6)
_cell_formula_units_Z            2
_cell_length_a                   17.809(6)
_cell_length_b                   17.831(6)
_cell_length_c                   17.812(6)
_cell_measurement_reflns_used    2067
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.25
_cell_measurement_theta_min      2.82
_cell_volume                     5656(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_wavelength     0.6199
_diffrn_reflns_av_R_equivalents  0.1395
_diffrn_reflns_av_unetI/netI     0.2001
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56059
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        21.835
_diffrn_reflns_theta_max         22.900
_diffrn_reflns_theta_min         2.817
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.733
_exptl_absorpt_correction_T_max  0.7448
_exptl_absorpt_correction_T_min  0.5642
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.758
_exptl_crystal_description       octahedral
_exptl_crystal_F_000             2883
_exptl_crystal_size_max          0.02
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         3.882
_refine_diff_density_min         -6.895
_refine_diff_density_rms         0.390
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1280
_refine_ls_number_reflns         23306
_refine_ls_number_restraints     192
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.2137
_refine_ls_R_factor_gt           0.1763
_refine_ls_shift/su_max          0.050
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+809.4526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3982
_refine_ls_wR_factor_ref         0.4263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15415
_reflns_number_total             23306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja500330a_si_002.cif
_cod_data_source_block           MOF-801-filled
_cod_database_code               4121460
_shelxl_version_number           2013-4
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C30 \\sim C26 \\sim C7 \\sim C34 \\sim C3 \\sim C1 \\sim C47 \\sim C50 \\sim
C2F \\sim C1E \\sim C43 \\sim C9 \\sim C1F \\sim C24 \\sim C14 \\sim C15 \\sim
C13 \\sim C2 \\sim C11 \\sim C38 \\sim C44 \\sim C40 \\sim C36 \\sim C32 \\sim
C18 \\sim C1G \\sim C12 \\sim C16 \\sim C19 \\sim C42 \\sim C8 \\sim C6 \\sim
C4 \\sim C1D \\sim C1B \\sim C17 \\sim C33 \\sim C45 \\sim C1C \\sim C1I \\sim
C35 \\sim C48 \\sim C46: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uiso(O25) = Uiso(O84)
3. Others
 Fixed Sof: O20(0.5) O23(0.5) O25(0.5) O27(0.5) O28(0.5) O30(0.5) O32(0.5)
 O34(0.5) O35(0.5) O36(0.5) O39(0.5) O5(0.5) O9(0.5) O1(0.5) O1J(0.5) O1K(0.5)
 O1L(0.5) O1O(0.5) O1P(0.5) O1Q(0.5) O1R(0.33333) O1S(0.5) O1T(0.5) O1U(0.5)
 O1V(0.5) O1W(0.5) O1X(0.5) O1Y(0.5) O1Z(0.5) O24(0.5) O2A(0.5) O2B(0.5)
 O2C(0.5) O46(0.5) O2D(0.5) O41(0.5) O2E(0.5) O2G(0.5) O2H(0.5) O2P(0.5)
 O2I(0.33333) O77(0.5) O2J(0.33333) O2K(0.5) O2L(0.5) O67(0.25) O2M(0.5)
 O74(0.33333) O99(0.25) O73(0.25) O2N(0.25) O2O(0.5) O86(0.33333) O97(0.33333)
 O2Q(0.5) O2R(0.33333) O2S(0.33333) O2T(0.5) O2U(0.25) O2V(0.5) O2W(0.5)
 O92(0.25) O95(0.25) O100(0.33333) O58(0.5) O93(0.33333) O2Y(0.33333) O84(0.5)
 O83(0.25) O102(0.25) O2F(0.25) O196(0.25) O276(0.5) O65(0.5) O150(0.25)
 O176(0.25) O162(0.25)
4.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C48(H48), C49(H49), C44(H44), C35(H35), C2(H2), C43(H43), C4(H4),
 C5(H5), C47(H47), C7(H7), C33(H33), C42(H42), C11(H11), C40(H40), C14(H14),
 C18(H18), C19(H19), C26(H26), C1D(H1D), C45(H45), C1E(H1E), C1G(H1G), C24(H24)
;