Applying the Power of Reticular Chemistry to Finding the Missing alb-MOF Platform Based on the (6,12)-Coordinated Edge-Transitive Net.
Chen, Zhijie; Weseliński, Łukasz J; Adil, Karim; Belmabkhout, Youssef; Shkurenko, Aleksander; Jiang, Hao; Bhatt, Prashant M.; Guillerm, Vincent; Dauzon, Emilie; Xue, Dong-Xu; O'Keeffe, Michael; Eddaoudi, Mohamed; Journal of the American Chemical Society 139 (2017) 3265–3274; doi:10.1021/jacs.7b00219

data_4125673
_publ_section_title
;
 Applying the Power of Reticular Chemistry to Finding the Missing alb-MOF
 Platform Based on the (6,12)-Coordinated Edge-Transitive Net.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3265
_journal_page_last               3274
_journal_paper_doi               10.1021/jacs.7b00219
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety
'4(C2 H8 N 1+), (Tb6 (O H2)2 (C69 H42 O12)2 (C7 H4 F O2)2 (O H)8)4-'
_chemical_formula_sum            'C160 H136 F2 N4 O38 Tb6'
_chemical_formula_weight         3714.24
_space_group_crystal_system      monoclinic
_space_group_IT_number           10
_space_group_name_Hall           '-P 2y'
_space_group_name_H-M_alt        'P 1 2/m 1'
_symmetry_space_group_name_Hall  '-P 2y'
_symmetry_space_group_name_H-M   'P 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.567(5)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   19.985(2)
_cell_length_b                   17.414(1)
_cell_length_c                   20.090(2)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      54.33
_cell_measurement_theta_min      3.52
_cell_volume                     6307.1(10)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection
'Bruker APEX2 v2009.3-0 (Bruker AXS Inc., 2009)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2009'
_computing_publication_material
'PublCIF. Westrip, S. P. (2010). J. Appl. Cryst. 43, 920-925.'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker X8 PROSPECTOR APEX2 CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  mirrors
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0987
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            48396
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        54.228
_diffrn_reflns_theta_max         54.227
_diffrn_reflns_theta_min         2.438
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    8.497
_exptl_absorpt_correction_T_max  0.0618
_exptl_absorpt_correction_T_min  0.0086
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1224 before and 0.0933 after correction.
The Ratio of minimum to maximum transmission is 0.1392.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.003
_refine_diff_density_max         1.199
_refine_diff_density_min         -2.251
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         7999
_refine_ls_number_restraints     548
_refine_ls_restrained_S_all      1.962
_refine_ls_R_factor_all          0.2106
_refine_ls_R_factor_gt           0.1843
_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/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4757
_refine_ls_wR_factor_ref         0.5045
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5713
_reflns_number_total             7999
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00219_si_007.cif
_cod_data_source_block           kme_935tb_a
_cod_original_cell_volume        6306.9(9)
_cod_database_code               4125673
_shelx_estimated_absorpt_t_max   0.975
_shelx_estimated_absorpt_t_min   0.550
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.871(4) 0.129(4)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C8-C10
 2.41 with sigma of 0.02
 C8-C8_$1
 2.41 with sigma of 0.02
 C8-C7 = C9-C8 = C10-C9
 1.39 with sigma of 0.01
 C7-C9
 2.41 with sigma of 0.02
 C9-C9_$1
 2.41 with sigma of 0.02
 O2-C17 = O1-C17
 1.23 with sigma of 0.02
 O2-O1
 -2.15 with sigma of 0.02
 C4-C3 = C5-C4 = C6-C5 = C1-C6 = C2-C1 = C2-C3
 1.39 with sigma of 0.01
 C1-C3 = C1-C5 = C2-C4 = C2-C6 = C3-C5 = C4-C6
 2.41 with sigma of 0.02
 C9-C11 = C14-C17
 1.5 with sigma of 0.01
 C14-O1 = C14-O2
 -2.3 with sigma of 0.02
 C29-C32
 2.78 with sigma of 0.02
 C30-C31_$1
 2.78 with sigma of 0.02
 C30-C29 = C31-C30 = C32-C31
 1.39 with sigma of 0.01
 C29-C31 = C30-C32 = C30-C30_$1 = C31-C31_$1
 2.41 with sigma of 0.02
 C28-C25
 1.5 with sigma of 0.02
 O3-O4
 2 with sigma of 0.02
 O4-C28 = O3-C28
 1.23 with sigma of 0.02
 C19_$1-C19
 2.41 with sigma of 0.02
 C18-C20
 2.41 with sigma of 0.02
 C20_$1-C20
 2.41 with sigma of 0.02
 C1-C7 = C2-C40 = C3-C18 = C4-C41 = C5-C29 = C6-C42
 1.5 with sigma of 0.02
 C20-C22
 1.5 with sigma of 0.02
 C19-C21
 2.41 with sigma of 0.02
 C19-C18 = C20-C19 = C20-C21
 1.39 with sigma of 0.01
 O6_$2-O6
 -2.9 with sigma of 0.02
 C39-O6
 1.23 with sigma of 0.02
 O5_$2-O5
 -2.9 with sigma of 0.02
 Tb1_$3-O5
 2.45 with sigma of 0.02
 O5_$3-O6_$3
 -2.2 with sigma of 0.02
 C39-O5
 1.23 with sigma of 0.02
 C31-C33
 1.5 with sigma of 0.01
 C36-O6
 -2.3 with sigma of 0.02
 C36-C39
 1.5 with sigma of 0.02
 C36-O5
 -2.3 with sigma of 0.02
 C14-O1 \\sim C14-O2
 with sigma of 0.02
 C40-C1 \\sim C40-C3 \\sim C41-C3 \\sim C41-C5 \\sim C42-C1 \\sim C42-C5
 with sigma of 0.02
 C24-C28 \\sim C26-C28
 with sigma of 0.02
 C25-O4 \\sim C25-O3
 with sigma of 0.02
 C31-C34 \\sim C31-C38
 with sigma of 0.01
 C35-C39 \\sim C37-C39
 with sigma of 0.02
4. Restrained planarity
 C7, C8_$1, C8, C9_$1, C9, C10
 with sigma of 0.02
 O1, O2, C14, C17
 with sigma of 0.09
 O3, O4, C25, C28
 with sigma of 0.09
 C18, C19, C19_$1, C20, C20_$1, C21
 with sigma of 0.02
 C31, C33, C34, C38
 with sigma of 0.09
 C35, C36, C37, C39
 with sigma of 0.09
 C36, C39, O5, O6
 with sigma of 0.09
5. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C18 \\sim C29
\\sim C40 \\sim C41 \\sim C42: within 2A with sigma of 0.05 and sigma for
terminal atoms of 0.1
Uanis(O4) \\sim Ueq: with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C21) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.14
Uanis(O5) \\sim Ueq: with sigma of 0.07 and sigma for terminal atoms of 0.14
Uanis(C11) = Uanis(C12) = Uanis(C13) = Uanis(C14) = Uanis(C15) = Uanis(C16)
Uanis(C22) = Uanis(C23) = Uanis(C24) = Uanis(C25) = Uanis(C26) = Uanis(C27)
6. Rigid body (RIGU) restrains
 O1, O2, O3, O4, O5, O6, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12,
 C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28,
  C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39, O5, O6, C40, C41, C42
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
7. Others
 Fixed Sof: H40B(0.5) H40C(0.5) H41B(0.5) H41C(0.5) H42B(0.5) H42C(0.5)
8.a Me refined with riding coordinates:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
8.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C10(H10), C12(H12), C13(H13), C15(H15), C16(H16), C19(H19), C21(H21),
 C23(H23), C24(H24), C26(H26), C27(H27), C30(H30), C32(H32), C34(H34), C35(H35),
  C37(H37), C38(H38)
8.c Fitted hexagon refined as free rotating group:
 C11(C12,C13,C14,C15,C16), C22(C23,C24,C25,C26,C27), C33(C34,C35,C36,C37,C38)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              43848
_shelx_hkl_checksum              49345
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'