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_4129125
_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         'C28.72 H18.68 Al2 N2.16 O8.56'
_chemical_formula_sum            'C28.72 H18.69 Al2 N2.15 O8.57'
_chemical_formula_weight         584.89
_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             2019-04-08
_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                   18.9000(10)
_cell_length_b                   18.9000(10)
_cell_length_c                   36.682(2)
_cell_measurement_reflns_used    4387
_cell_measurement_temperature    100
_cell_measurement_theta_max      13.159
_cell_measurement_theta_min      2.287
_cell_volume                     13103.2(12)
_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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker PHOTON-II detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'CMOS detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_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       48
_diffrn_reflns_limit_l_min       -48
_diffrn_reflns_number            216133
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         29.069
_diffrn_reflns_theta_min         1.586
_diffrn_source
;
Advanced Light Source, station 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1090 before and 0.0598 after correction. The Ratio of minimum to maximum transmission is 0.9083. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.593
_exptl_crystal_description       block
_exptl_crystal_F_000             2405
_exptl_crystal_size_max          0.082
_exptl_crystal_size_mid          0.073
_exptl_crystal_size_min          0.051
_refine_diff_density_max         0.145
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.022
_refine_ls_abs_structure_details
;
 Flack x determined using 5505 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.06(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         16251
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0495P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0741
_reflns_Friedel_coverage         0.796
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                13746
_reflns_number_total             16251
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10501_si_004.cif
_cod_data_source_block           delta-MOF-520-18
_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        13103.0(16)
_cod_database_code               4129125
_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 O(H) groups
2. Shared sites
{N1GA, N2GB}
{N2GA, N1GB}
{C1GA, N3GB}
{C2GB, N3GA}
{C2GA, C1GB}
3. Rigid bond restraints
 O9, C28, O10
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C28 \\sim O9 \\sim O10: within 1.7A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(N1GA) = Uanis(N2GB)
Uanis(N2GA) = Uanis(N1GB)
Uanis(C1GA) = Uanis(N3GB)
Uanis(C2GB) = Uanis(N3GA)
Uanis(C2GA) = Uanis(C1GB)
5. Others
 1*[Sof(O9)+Sof(O10)+Sof(C28)+Sof(H28)]+1*[Sof(N3GA)+Sof(C2GA)+Sof(H2GA)+
 Sof(N1GA)+Sof(N2GA)+Sof(C1GA)+Sof(H1GA)]+1*[Sof(N2GB)+Sof(N1GB)+Sof(N3GB)+
 Sof(C1GB)+Sof(C2GB)+Sof(H2GB)]=1 with esd of 0.0001
 Sof(O9)=Sof(O10)=Sof(C28)=Sof(H28)=FVAR(1)
 Sof(N3GA)=Sof(C2GA)=Sof(H2GA)=Sof(N1GA)=Sof(N2GA)=Sof(C1GA)=Sof(H1GA)=FVAR(2)
 Sof(N2GB)=Sof(N1GB)=Sof(N3GB)=Sof(C1GB)=Sof(C2GB)=Sof(H2GB)=FVAR(3)
6.a Aromatic/amide H refined with riding coordinates:
 O8(H8), O7(H7), C26(H26), C7(H7A), C19(H19), C11(H11), C23(H23), C27(H27),
 C4(H4), C3(H3), C9(H9), C13(H13), C6(H6), C20(H20), C22(H22), C16(H16),
 C15(H15), C2GA(H2GA), C1GA(H1GA), C28(H28), C2GB(H2GB)
;
_shelx_res_checksum              76144
_shelx_hkl_checksum              18256
_shelx_fab_checksum              6189
_olex2_submission_special_instructions 'No special instructions were received'