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_4125674
_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+), (Y6 (O H2)2 (C69 H42 O12)2 (C7 H4 F O2)2 (O H)8)4-'
_chemical_formula_sum            'C160 H136 F2 N4 O38 Y6'
_chemical_formula_weight         3294.18
_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
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-10-10
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 115.009(8)
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   18.998(1)
_cell_length_b                   17.5118(7)
_cell_length_c                   19.567(1)
_cell_measurement_reflns_used    7876
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      67.5990
_cell_measurement_theta_min      2.5060
_cell_volume                     5899.4(6)
_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      100.0(1)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0917
_diffrn_reflns_av_unetI/netI     0.0837
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29971
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        65.088
_diffrn_reflns_theta_max         65.088
_diffrn_reflns_theta_min         2.523
_diffrn_source                   'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    2.331
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5473
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.086 before and 0.076 after correction.
The Ratio of minimum to maximum transmission is 0.7270.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.927
_exptl_crystal_description       'truncated rectangular pyramid'
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.673
_refine_diff_density_min         -1.577
_refine_diff_density_rms         0.184
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.410
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     527
_refine_ls_number_reflns         10377
_refine_ls_number_restraints     381
_refine_ls_restrained_S_all      1.405
_refine_ls_R_factor_all          0.1597
_refine_ls_R_factor_gt           0.1342
_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          0.3634
_refine_ls_wR_factor_ref         0.3841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6986
_reflns_number_total             10377
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00219_si_006.cif
_cod_data_source_block           kme_935c
_cod_original_cell_volume        5899.3(7)
_cod_database_code               4125674
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.845
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.960(1) 0.040(1)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C1-C2 = C2-C3 = C3-C4 = C4-C5 = C5-C6 = C6-C1
 1.39 with sigma of 0.001
 C1-C3 = C2-C4 = C3-C5 = C4-C6 = C5-C1 = C6-C2
 2.408 with sigma of 0.02
 C1-C4 = C2-C5 = C3-C6
 2.78 with sigma of 0.02
 C7-C8 = C8-C9 = C9-C10
 1.39 with sigma of 0.001
 C7-C9 = C8-C10 = C8-C8_$1 = C9-C9_$1
 2.408 with sigma of 0.02
 C7-C10 = C8-C9_$1
 2.78 with sigma of 0.02
 C18-C19 = C19-C20 = C20-C21
 1.39 with sigma of 0.001
 C18-C20 = C19-C21 = C19-C19_$1 = C20-C20_$1
 2.408 with sigma of 0.02
 C18-C21 = C19-C20_$1
 2.78 with sigma of 0.02
 C29-C30 = C30-C31 = C31-C32
 1.39 with sigma of 0.001
 C29-C31 = C30-C32 = C30-C30_$1 = C31-C31_$1
 2.408 with sigma of 0.02
 C29-C32 = C30-C31_$1
 2.78 with sigma of 0.02
 C33-C34 = C34-C35
 1.39 with sigma of 0.001
 C35-C36A = C36A-C37A = C37A-C38A = C38A-C33
 1.39 with sigma of 0.001
 C35-C36B = C36B-C37B = C37B-C38B = C38B-C33
 1.39 with sigma of 0.001
 C33-C35 = C34-C36A = C34-C36B = C35-C37A = C35-C37B
 2.408 with sigma of 0.02
 C36A-C38A = C36B-C38B = C37A-C33 = C37B-C33
 2.408 with sigma of 0.02
 C33-C36A = C33-C36B = C34-C37A = C34-C37B = C35-C38A = C35-C38B
 2.78 with sigma of 0.02
 C1-C7 = C3-C18 = C5-C29
 1.5 with sigma of 0.01
 C14-C17 = C25-C28
 1.5 with sigma of 0.01
 C36A-C39A = C36B-C39B
 1.5 with sigma of 0.02
 O5-C39A = O6A-C39A = O5-C39B = O6B-C39B
 1.23 with sigma of 0.02
 O11-C43
 1.23 with sigma of 0.02
 O4-C28 = O3-C28
 1.23 with sigma of 0.02
 C45-F1A \\sim C49-F1B
 with sigma of 0.01
4. Restrained planarity
 C36A, C39A, O6A, O5
 with sigma of 0.01
 C36B, C39B, O6B, O5
 with sigma of 0.01
 C43, C44, C45, C46, C47, C48, C49, F1A, F1B
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
C36A \\sim C36B \\sim C37A \\sim C37B \\sim C38A \\sim C38B: within 2A with
sigma of 0.02 and sigma for terminal atoms of 0.04
O6A \\sim O6B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim F1A \\sim
F1B: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O7) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O11) \\sim Ueq: with sigma of
0.006 and sigma for terminal atoms of 0.012
Uanis(F1A) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C43)
\\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47) \\sim Ueq: with sigma of 0.03 and
sigma for terminal atoms of 0.06
Uanis(F1A) = Uanis(F1B)
6. Rigid body (RIGU) restrains
 C33, C34, C35, C36A, C36B, C37A, C37B, C38A, C38B, C39A, C39B, O6A, O6B, O5
 with sigma for 1-2 distances of 0.003 and sigma for 1-3 distances of 0.003
7. Others
 Fixed Sof: O6A(0.5) O6B(0.5) H35(0.5) H35A(0.5) C36A(0.5) C37A(0.5) H37A(0.5)
 C38A(0.5) H38A(0.5) C39A(0.5) C36B(0.5) C37B(0.5) H37B(0.5) C38B(0.5)
 H38B(0.5) C39B(0.5) H40A(0.5) H40B(0.5) H40C(0.5) H41A(0.5) H41B(0.5)
 H41C(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C43(0.5) C44(0.5) C45(0.5) H45(0.25)
 C46(0.5) H46(0.5) C47(0.5) H47(0.5) C48(0.5) H48(0.5) C49(0.5) H49(0.25)
 F1A(0.25) F1B(0.25)
8.a 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),
  C35(H35A), C37A(H37A), C38A(H38A), C37B(H37B), C38B(H38B), C45(H45), C46(H46),
  C47(H47), C48(H48), C49(H49)
8.b Fitted hexagon refined as free rotating group:
 C11(C12,C13,C14,C15,C16), C22(C23,C24,C25,C26,C27), C44(C45,C46,C47,C48,C49)
8.c Idealised Me refined as rotating group:
 C40(H40A,H40B,H40C), C41(H41A,H41B,H41C), C42(H42A,H42B,H42C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              95889
_shelx_hkl_checksum              61935
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'