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_4121461
_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
'C28 H9 N10.5 O34 Zr6, C3 H7 N O, C2 N, 1.5(O), C3 N O, C N, 0.5(C), C O0.75, 0.33(C2 O2)'
_chemical_formula_sum            'C39.17 H16 N14.5 O38.92 Zr6'
_chemical_formula_weight         1859.65
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           43
_space_group_name_Hall           'F 2 -2d'
_space_group_name_H-M_alt        'F d d 2'
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_atom_sites_solution_hydrogens   geom
_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            16
_cell_length_a                   39.222(3)
_cell_length_b                   26.018(2)
_cell_length_c                   27.887(2)
_cell_measurement_reflns_used    9705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      58.99
_cell_measurement_theta_min      3.92
_cell_volume                     28458(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker Photon-100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Goebel mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0142
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            27657
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.802
_diffrn_reflns_theta_min         2.253
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.853
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5875
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABAS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.736
_exptl_crystal_F_000             14461
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.555
_refine_diff_density_min         -0.826
_refine_diff_density_rms         0.163
_refine_ls_abs_structure_details
;
 Flack x determined using 4157 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.021(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     797
_refine_ls_number_reflns         10910
_refine_ls_number_restraints     145
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0725P)^2^+533.1031P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1157
_reflns_Friedel_coverage         0.957
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                10764
_reflns_number_total             10910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja500330a_si_005.cif
_cod_data_source_block           mof-802
_cod_original_cell_volume        28459(4)
_cod_original_formula_sum        'C39.17 H16 N14.50 O38.92 Zr6'
_cod_database_code               4121461
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.332
_shelx_estimated_absorpt_t_min   0.244
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O30-C1A = O1A-C1A
 1.25 with sigma of 0.02
 O29-C1B = O1B-C1B
 1.25 with sigma of 0.02
 O31-C33
 1.25 with sigma of 0.02
 O29-C35
 1.25 with sigma of 0.02
 N29-C35
 1.32 with sigma of 0.02
 N29-C43
 1.45 with sigma of 0.02
 O32-C1C = O1C-C1C
 1.25 with sigma of 0.02
 O31-C33
 1.25 with sigma of 0.02
 O31-C33 = O40-C33
 1.25 with sigma of 0.02
 C1J-N1I
 1.32 with sigma of 0.02
 O33-C27
 2.8 with sigma of 0.02
 O33-C26
 1.25 with sigma of 0.02
 N11-C26
 1.32 with sigma of 0.02
 C28-C27
 2.5 with sigma of 0.02
 N11-C27 = N11-C28
 1.45 with sigma of 0.02
 O9-C4 \\sim O10-C4
 with sigma of 0.02
 O12-C5 \\sim O11-C5
 with sigma of 0.02
 O14-C9 \\sim O13-C9
 with sigma of 0.02
 O16-C10 \\sim O15-C10
 with sigma of 0.02
 O17-C14 \\sim O18-C14
 with sigma of 0.02
 O19-C15 \\sim O20-C15
 with sigma of 0.02
 O22-C19 \\sim O21-C19
 with sigma of 0.02
 O24-C20 \\sim O23-C20
 with sigma of 0.02
 O26-C24 \\sim O25-C24
 with sigma of 0.02
 O27-C25 \\sim O28-C25
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N10 \\sim N9 \\sim C23 \\sim C22 \\sim C21: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C35) \\sim Ueq, Uanis(N29) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C1C) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1C) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1C) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1L) \\sim Ueq, Uanis(C1J) \\sim Ueq, Uanis(N1I) \\sim Ueq, Uanis(C1K)
\\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C1L) \\sim Ueq, Uanis(N1I) \\sim Ueq, Uanis(C1J) \\sim Ueq, Uanis(C1K)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq, Uanis(N11) \\sim Ueq: with sigma of 0.1 and sigma for
terminal atoms of 0.2
Uanis(C26) \\sim Ueq, Uanis(N11) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C28) \\sim Ueq, Uanis(C27) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O4) = Uanis(O2) = Uanis(O3) = Uanis(O1)
Uanis(O8) = Uanis(O5) = Uanis(O6) = Uanis(O7)
Uanis(O17) = Uanis(O18)
Uanis(O10) = Uanis(O9)
Uanis(O23) = Uanis(O24)
Uanis(O12) = Uanis(O11)
Uanis(C25) = Uanis(C24)
Uanis(O1B) = Uanis(O1A)
Uanis(C1A) = Uanis(C1B)
Uanis(C5) = Uanis(C4)
Uanis(C33) = Uanis(C1C)
Uanis(O40) = Uanis(O1C)
Uanis(C27) = Uanis(C28)
4. Others
 Fixed Sof: O1A(0.5) C1A(0.5) O1B(0.5) C1B(0.5) O1C(0.5) N29(0.5) C33(0.5)
 C35(0.5) C43(0.5) C1C(0.5) O40(0.5) O1D(0.5) O1H(0.25) O1I(0.33333)
 O1G(0.33333) C1G(0.33333) C1I(0.33333) O1J(0.5) C1M(0.5) C1N(0.5)
5.a Ternary CH refined with riding coordinates:
 O8(H8), O5(H5), O7(H7A), O6(H6)
5.b Me refined with riding coordinates:
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C7(H7), C17(H17), C12(H12), C22(H22), C26(H26)
5.d Fitted pentagon refined as free rotating group:
 N3(N4,C6,C7,C8)
;