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_4131313
_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 H82.4 O46.2 Y9 1-, 6.3(O H2)'
_chemical_formula_sum            'C104 H103 N O52.5 Y9'
_chemical_formula_weight         3007.06
_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   constr
_audit_creation_date             2015-11-04
_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                   21.996(2)
_cell_length_b                   21.996(2)
_cell_length_c                   24.912(2)
_cell_measurement_reflns_used    8764
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      1.843
_cell_volume                     10438.2(16)
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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  0.1469
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48234
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        21.260
_diffrn_reflns_theta_max         21.260
_diffrn_reflns_theta_min         2.676
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.523
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0912 before and 0.0705 after correction.
The Ratio of minimum to maximum transmission is 0.72547.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.957
_exptl_crystal_description       'hexagonal bipyramid'
_exptl_crystal_F_000             3010
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.958
_refine_diff_density_min         -1.206
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         2180
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1250
_refine_ls_R_factor_gt           0.0839
_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^)+(0.1955P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2453
_refine_ls_wR_factor_ref         0.2731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1456
_reflns_number_total             2180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b04132_si_004.cif
_cod_data_source_block           22RH
_cod_original_cell_volume        10438(2)
_cod_original_formula_sum        'C104 H103 N O52.50 Y9'
_cod_database_code               4131313
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C1-O1A = C1-O2A = C1-O1B = C1-O2B
 1.22 with sigma of 0.01
 N1-C10 = N1-C11
 1.47 with sigma of 0.02
 O1WA-N1
 2.78 with sigma of 0.02
 O1WA-C10
 -3.3 with sigma of 0.02
 O1WB_$1-C11
 -3.2 with sigma of 0.02
 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
 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
O1A \\sim O2A \\sim O1B \\sim O2B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C3A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7A)
\\sim Ueq, Uanis(C3B) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C6B) \\sim Ueq,
Uanis(C7B) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.14
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C5) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.04
Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.06
Uanis(C9) \\sim Ueq: with sigma of 0.015 and sigma for terminal atoms of 0.06
Uanis(O2WB) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.03
Uanis(O1A) \\sim Ueq, Uanis(O2A) \\sim Ueq, Uanis(O1B) \\sim Ueq, Uanis(O2B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
: with sigma of 0.06 and sigma for terminal atoms of 0.12
Uanis(O1WA) = Uanis(O1WB)
Uanis(Y1A) = Uanis(Y1B)
Uanis(Y2A) = Uanis(Y2B) = Uanis(O3A) = Uanis(O3B) = Uanis(O4) = Uanis(O5)
Uanis(C3A) = Uanis(C4A) = Uanis(C6A) = Uanis(C7A)
Uanis(C3B) = Uanis(C4B) = Uanis(C6B) = Uanis(C7B)
Uiso(C10) = Uiso(N1) = Uiso(C11)
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)=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: N1(0.08333) C10(0.08333) C11(0.08333) O2WA(0.125) O3W(0.125)
 O4W(0.125)
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              8079
_shelx_hkl_checksum              46200
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'