Coordinative Alignment in the Pores of MOFs for the Structural Determination of N-, S-, and P-Containing Organic Compounds Including Complex Chiral Molecules.
Pei, Xiaokun; Bürgi, Hans-Beat; Kapustin, Eugene A.; Liu, Yuzhong; Yaghi, Omar M.; Journal of the American Chemical Society 141 (2019) 18862–18869; doi:10.1021/jacs.9b10501

data_4129126
_publ_section_title
;
 Coordinative Alignment in the Pores of MOFs for the Structural
 Determination of N-, S-, and P-Containing Organic Compounds Including
 Complex Chiral Molecules.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              18862
_journal_page_last               18869
_journal_paper_doi               10.1021/jacs.9b10501
_journal_volume                  141
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety
'C32.5 H22.5 Al2 N1.5 O9.7, 0.3(C15 H15 N O3), 0.25(O)'
_chemical_formula_sum            'C37 H27 Al2 N1.8 O10.85'
_chemical_formula_weight         724.36
_space_group_crystal_system      tetragonal
_space_group_IT_number           94
_space_group_name_Hall           'P 4n 2n'
_space_group_name_H-M_alt        'P 42 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-04-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.4248(7)
_cell_length_b                   19.4248(7)
_cell_length_c                   35.7345(13)
_cell_measurement_reflns_used    9417
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      3.45
_cell_volume                     13483.4(8)
_computing_cell_refinement       'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_data_collection       'Bruker APEX3 Bruker-AXS, Madison WI'
_computing_data_reduction        'SAINT V8.38A Bruker-AXS, Madison WI'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-2008 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            171051
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.411
_diffrn_reflns_theta_max         25.411
_diffrn_reflns_theta_min         2.150
_diffrn_source
;
Advanced Light Source, station 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1266 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.9032. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.714
_exptl_crystal_description       block
_exptl_crystal_F_000             2995
_exptl_crystal_size_max          0.079
_exptl_crystal_size_mid          0.068
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details
;
 Flack x determined using 4330 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     708
_refine_ls_number_reflns         11493
_refine_ls_number_restraints     272
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0795
_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^)+(0.1482P)^2^+3.7013P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2190
_refine_ls_wR_factor_ref         0.2223
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    0.995
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                10685
_reflns_number_total             11493
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10501_si_023.cif
_cod_data_source_block           delta-MOF-520-S-32
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_atom_sites_solution_secondary' value 'diffmap' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 

 Adding full bibliography for 4129110--4129131.cif.
;
_cod_original_cell_volume        13483.4(11)
_cod_original_formula_sum        'C37 H27 Al2 N1.80 O10.85'
_cod_database_code               4129126
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.994
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4GA-C3GA = C3GB-C4GB = C4GB-C5GB = C5GA-C4GA = C5GA-C10A = C10B-C5GB
 1.52 with sigma of 0.02
 N3GA-C7GA = N3GB-C7GB
 1.46 with sigma of 0.02
 N3GB-C5GB = N3GA-C5GA
 1.47 with sigma of 0.02
 C9GB-C8GB = C9GA-C8GA = C7GB-C8GB = C7GA-C8GA
 1.5 with sigma of 0.02
 O2GA-C12A = O2GB-C12B = O3GA-C13A = O3GB-C13B
 1.36 with sigma of 0.02
 O2GA-C15A = O3GA-C16A = O2GB-C15B = O3GB-C16B
 1.41 with sigma of 0.02
 O9-C28 = O10-C28
 1.29 with sigma of 0.02
 N3GA-C6GA = N3GB-C6GB
 1.35 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C3GB) \\sim Ueq, Uanis(C2GB) \\sim Ueq, Uanis(C4GB) \\sim Ueq,
Uanis(C5GB) \\sim Ueq, Uanis(N3GA) \\sim Ueq, Uanis(O1GB) \\sim Ueq,
Uanis(N3GB) \\sim Ueq, Uanis(C10B) \\sim Ueq, Uanis(C11B) \\sim Ueq,
Uanis(C12B) \\sim Ueq, Uanis(C13B) \\sim Ueq, Uanis(C14B) \\sim Ueq,
Uanis(C9GB) \\sim Ueq, Uanis(C9GA) \\sim Ueq, Uanis(C10A) \\sim Ueq,
Uanis(C11A) \\sim Ueq, Uanis(C12A) \\sim Ueq, Uanis(C13A) \\sim Ueq,
Uanis(C14A) \\sim Ueq, Uanis(C7GB) \\sim Ueq, Uanis(C5GA) \\sim Ueq,
Uanis(C4GA) \\sim Ueq, Uanis(C3GA) \\sim Ueq, Uanis(C8GA) \\sim Ueq,
Uanis(C7GA) \\sim Ueq, Uanis(C8GB) \\sim Ueq, Uanis(C6GA) \\sim Ueq,
Uanis(C2GA) \\sim Ueq, Uanis(C6GB) \\sim Ueq, Uanis(C1G) \\sim Ueq, Uanis(O1GA)
\\sim Ueq, Uanis(O2GA) \\sim Ueq, Uanis(O3GA) \\sim Ueq, Uanis(C16B) \\sim Ueq,
Uanis(O3GB) \\sim Ueq, Uanis(C15B) \\sim Ueq, Uanis(O2GB) \\sim Ueq,
Uanis(C15A) \\sim Ueq, Uanis(C16A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N1G, O10, N2G, C28, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: N1G(0.6) O10(0.4) C3GB(0.3) C2GB(0.3) C4GB(0.3) H4GC(0.3)
 H4GD(0.3) C5GB(0.3) H5GB(0.3) N3GA(0.3) O1GB(0.3) N3GB(0.3) N2G(0.6) C10B(0.3)
 C11B(0.3) H11B(0.3) C12B(0.3) C13B(0.3) C14B(0.3) H14B(0.3) C9GB(0.3)
 C9GA(0.3) C10A(0.3) C11A(0.3) H11A(0.3) C12A(0.3) C13A(0.3) C14A(0.3)
 H14A(0.3) C7GB(0.3) H7GC(0.3) H7GD(0.3) C5GA(0.3) H5GA(0.3) C4GA(0.3)
 H4GA(0.3) H4GB(0.3) C3GA(0.3) C28(0.4) H28(0.4) O9(0.4) C8GA(0.3) H8GA(0.3)
 H8GB(0.3) C7GA(0.3) H7GA(0.3) H7GB(0.3) C8GB(0.3) H8GC(0.3) H8GD(0.3)
 C6GA(0.3) C2GA(0.3) C6GB(0.3) C1G(0.6) H1G(0.6) O1GA(0.3) O2GA(0.3) O3GA(0.3)
 C16B(0.3) H16D(0.3) H16E(0.3) H16F(0.3) O3GB(0.3) C15B(0.3) H15D(0.3)
 H15E(0.3) H15F(0.3) O2GB(0.3) C15A(0.3) H15A(0.3) H15B(0.3) H15C(0.3)
 C16A(0.3) H16A(0.3) H16B(0.3) H16C(0.3)
6.a Ternary CH refined with riding coordinates:
 C5GB(H5GB), C5GA(H5GA)
6.b Secondary CH2 refined with riding coordinates:
 C4GB(H4GC,H4GD), C7GB(H7GC,H7GD), C4GA(H4GA,H4GB), C8GA(H8GA,H8GB), C7GA(H7GA,
 H7GB), C8GB(H8GC,H8GD)
6.c Me refined with riding coordinates:
 C16B(H16D,H16E,H16F), C15B(H15D,H15E,H15F), C15A(H15A,H15B,H15C), C16A(H16A,
 H16B,H16C)
6.d Aromatic/amide H refined with riding coordinates:
 O8(H8), O7(H7), C7(H7A), C23(H23), C4(H4), C16(H16), C15(H15), C3(H3),
 C26(H26), C9(H9), C20(H20), C19(H19), C11(H11), C22(H22), C13(H13), C6(H6),
 C27(H27), C11B(H11B), C14B(H14B), C11A(H11A), C14A(H14A), C28(H28), C1G(H1G)
6.e Fitted hexagon refined as free rotating group:
 C10B(C11B,C12B,C13B,C14B,C9GB), C9GA(C10A,C11A,C12A,C13A,C14A)
;
_shelx_res_checksum              85477
_shelx_hkl_checksum              71000
_olex2_submission_special_instructions 'No special instructions were received'