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_4129114
_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         'C29.8 H19.44 Al2 O10 S0.36, 0.17(O)'
_chemical_formula_sum            'C29.8 H17.44 Al2 O10.15 S0.36'
_chemical_formula_weight         603.31
_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             2019-04-14
_audit_creation_method
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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                   18.4641(6)
_cell_length_b                   18.4641(6)
_cell_length_c                   37.4193(12)
_cell_measurement_reflns_used    9405
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.81
_cell_volume                     12757.1(7)
_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-2017/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT2014/5 (Sheldrick, 2014)'
_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  0.0608
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            206016
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.176
_diffrn_reflns_theta_min         2.020
_diffrn_source
;
Advanced Light Source, station 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6490
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0707 before and 0.0555 after correction. The Ratio of minimum to maximum transmission is 0.8706. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.628
_exptl_crystal_description       block
_exptl_crystal_F_000             2473
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.515-
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 4915 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.05(2)
_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     420
_refine_ls_number_reflns         13117
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0491
_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^)+(0.1194P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1422
_refine_ls_wR_factor_ref         0.1466
_reflns_Friedel_coverage         0.780
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                11839
_reflns_number_total             13117
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10501_si_015.cif
_cod_data_source_block           delta-MOF-520-27
_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        12757.1(9)
_cod_original_formula_sum        'C29.80 H17.44 Al2 O10.15 S0.36'
_cod_database_code               4129114
_shelx_shelxl_version_number     2017/1
_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
{S1G, C28}
3. Restrained distances
 C5G-C6G \\sim C1G-C6G \\sim C1G-C2G \\sim C3G-C2G \\sim C4G-C3G \\sim C4G-C5G
 with sigma of 0.02
 C6G-C2G \\sim C1G-C3G
 with sigma of 0.02
4. Restrained planarity
 C6G, C1G, C2G, C3G, C5G, C4G
 with sigma of 0.1
5. Uiso/Uaniso restraints and constraints
C4G \\sim C5G \\sim C6G \\sim C1G \\sim C2G \\sim C3G: within 1.7A with sigma
of 0.04 and sigma for terminal atoms of 0.08
Uanis(S1G) = Uanis(C28)
6. Others
 Fixed Sof: S1G(0.35942) C6G(0.35942) H6G(0.35942) C1G(0.35942) C2G(0.35942)
 H2G(0.35942) C3G(0.35942) H3G(0.35942) C4G(0.35942) H4G(0.35942) C5G(0.35942)
 H5G(0.35942) C28(0.64058) H28(0.64058) O2S(0.04339)
7.a Aromatic/amide H refined with riding coordinates:
 O8(H8), O7(H7), C19(H19), C16(H16), C15(H15), C23(H23), C7(H7A), C20(H20),
 C3(H3), C6(H6), C9(H9), C11(H11), C4(H4), C26(H26), C22(H22), C13(H13),
 C27(H27), C6G(H6G), C2G(H2G), C3G(H3G), C4G(H4G), C5G(H5G), C28(H28)
;
_shelx_res_checksum              98035
_shelx_hkl_checksum              61974
_shelx_fab_checksum              56770
_olex2_submission_special_instructions 'No special instructions were received'