A Fine-Tuned Metal-Organic Framework for Autonomous Indoor Moisture Control.
AbdulHalim, Rasha G.; Bhatt, Prashant M.; Belmabkhout, Youssef; Shkurenko, Aleksander; Adil, Karim; Barbour, Leonard J.; Eddaoudi, Mohamed; Journal of the American Chemical Society 139 (2017) 10715–10722; doi:10.1021/jacs.7b04132

data_4131316
_publ_section_title
;
 A Fine-Tuned Metal-Organic Framework for Autonomous Indoor Moisture
 Control.
;
_journal_issue                   31
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10715
_journal_page_last               10722
_journal_paper_doi               10.1021/jacs.7b04132
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C2 H8 N1 1+, C102 H54 O47 Y9 1-, 74(H2 O1)'
_chemical_formula_sum            'C104 H240 N O121 Y9'
_chemical_formula_weight         4241.15
_space_group_crystal_system      hexagonal
_space_group_IT_number           194
_space_group_name_Hall           '-P 6c 2c'
_space_group_name_H-M_alt        'P 63/m m c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2015-11-08
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   22.098(1)
_cell_length_b                   22.098(1)
_cell_length_c                   24.706(2)
_cell_measurement_reflns_used    10806
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.82
_cell_measurement_theta_min      1.82
_cell_volume                     10448.1(11)
_computing_cell_refinement       'SAINT v7.68A (Bruker AXS Inc., 2009)'
_computing_data_collection
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker AXS Inc., 2009)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXS (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX II Duo'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1604
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            38850
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        24.701
_diffrn_reflns_theta_max         24.701
_diffrn_reflns_theta_min         2.693
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.565
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0914 before and 0.0655 after correction.
The Ratio of minimum to maximum transmission is 0.7876.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.348
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_F_000             4380
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.433
_refine_diff_density_min         -1.070
_refine_diff_density_rms         0.151
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     159
_refine_ls_number_reflns         3288
_refine_ls_number_restraints     42
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1399
_refine_ls_R_factor_gt           0.0824
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1803P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2357
_refine_ls_wR_factor_ref         0.2731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1953
_reflns_number_total             3288
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04132_si_005.cif
_cod_data_source_block           100rh
_cod_original_cell_volume        10448(2)
_cod_database_code               4131316
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C2-C3A = C3A-C4A = C4A-C5 = C5-C6A = C6A-C7A = C7A-C2
 1.39 with sigma of 0.01
 C2-C3B = C3B-C4B = C4B-C5 = C5-C6B = C6B-C7B = C7B-C2
 1.39 with sigma of 0.01
 N1-C10 = N1-C11
 1.47 with sigma of 0.02
 C11-O1WA = C11-O1WB
 -3.3 with sigma of 0.01
 C1-O1A = C1-O2A = C1-O1B = C1-O2B
 1.22 with sigma of 0.01
 O1WA-N1
 2.76 with sigma of 0.02
 O1WB_$1-C10
 -3.3 with sigma of 0.01
 C11-O1WB_$2
 -3.2 with sigma of 0.02
 O2WB-O7WB
 -2.76 with sigma of 0.01
 O7WA-O7WA_$3
 -2.76 with sigma of 0.01
 O4W-O3W
 -2.76 with sigma of 0.01
 C10-C11
 2.5 with sigma of 0.02
 Y1A-Y2A \\sim Y1B-Y2B
 with sigma of 0.01
 Y1A-O1A \\sim Y1B-O1B
 with sigma of 0.01
 Y1A-O3A \\sim Y1B-O3B
 with sigma of 0.01
 Y1A-O4 \\sim Y1B-O4
 with sigma of 0.01
 Y2A-O2A \\sim Y2B-O2B
 with sigma of 0.01
 Y2A-O3A \\sim Y2B-O3B
 with sigma of 0.01
 Y2A-O4 \\sim Y2B-O4
 with sigma of 0.01
 Y2A-O5 \\sim Y2B-O5
 with sigma of 0.01
 Y2A-O1WA \\sim Y2B-O1WB
 with sigma of 0.01
3. Restrained planarity
 C2, C3B, C4B, C5, C6B, C7B
 with sigma of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(O2WB) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(O1A) = Uanis(O2A) = Uanis(O1B) = Uanis(O2B)
Uanis(C3A) = Uanis(C4A) = Uanis(C6A) = Uanis(C7A)
Uanis(C3B) = Uanis(C4B) = Uanis(C6B) = Uanis(C7B)
Uanis(O1WA) = Uanis(O1WB)
Uanis(Y1A) = Uanis(Y1B)
Uanis(Y2A) = Uanis(Y2B) = Uanis(O3A) = Uanis(O3B) = Uanis(O4) = Uanis(O5)
Uiso(C10) = Uiso(N1) = Uiso(C11)
Uanis(O2WA) = Uanis(O2WB)
5. Others
 Sof(O1B)=Sof(O2B)=Sof(C3B)=Sof(H3B)=Sof(C4B)=Sof(H4B)=Sof(C6B)=Sof(H6B)=
 Sof(C7B)=Sof(H7B)=1-FVAR(1)
 Sof(Y2B)=Sof(O3B)=Sof(O1WB)=0.5*(1-FVAR(2))
 Sof(Y1B)=Sof(O2WB)=0.25*(1-FVAR(2))
 Sof(Y1A)=Sof(O2WA)=0.25*FVAR(2)
 Sof(Y2A)=Sof(O3A)=Sof(O1WA)=0.5*FVAR(2)
 Sof(O1A)=Sof(O2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C6A)=Sof(H6A)=
 Sof(C7A)=Sof(H7A)=FVAR(1)
 Fixed Sof: C10(0.08333) C11(0.08333) N1(0.08333) O3W(0.125) O4W(0.125)
 O5W(0.0625) O6W(0.08333) O7WA(0.125) O7WB(0.0625) O8W(0.04167) O9W(0.08333)
6.a Aromatic/amide H refined with riding coordinates:
 C3A(H3A), C4A(H4A), C3B(H3B), C4B(H4B), C6A(H6A), C7A(H7A), C6B(H6B),
 C7B(H7B), C9(H9)
;
_shelx_res_checksum              53480
_shelx_hkl_checksum              73028
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'