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_4129117
_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         'C27.45 H18.55 Al2 O10.55 P0.55, 0.48(O)'
_chemical_formula_sum            'C27.45 H18.55 Al2 O11.03 P0.55'
_chemical_formula_weight         595.89
_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             2019-06-09
_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                   18.1702(6)
_cell_length_b                   18.1702(6)
_cell_length_c                   37.8430(14)
_cell_measurement_reflns_used    9198
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.30
_cell_volume                     12494.1(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-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_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  0.0590
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            245782
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         26.108
_diffrn_reflns_theta_min         2.320
_diffrn_source
;
Advanced Light Source, station 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6540
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1246 before and 0.0595 after correction. The Ratio of minimum to maximum transmission is 0.8775. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.634
_exptl_crystal_description       block
_exptl_crystal_F_000             2446
_exptl_crystal_size_max          0.071
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.374
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.034
_refine_ls_abs_structure_details
;
 Flack x determined using 4204 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.08(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     402
_refine_ls_number_reflns         11482
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      0.993
_refine_ls_R_factor_all          0.0367
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0689P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0871
_refine_ls_wR_factor_ref         0.0890
_reflns_Friedel_coverage         0.773
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                10317
_reflns_number_total             11482
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10501_si_010.cif
_cod_data_source_block           delta-MOF-520-23
_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        12494.1(9)
_cod_database_code               4129117
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7 of O7, H8 of O8, All P(H) groups
 At 1.5 times of:
  H1GC of O1GA, H1GD of O1GB
2. Restrained distances
 O10-C28 = O9-C28
 1.27 with sigma of 0.02
 P1GB-O10 \\sim P1GA-O10 \\sim P1GB-O9 \\sim P1GA-O9
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C28) \\sim Ueq, Uanis(O1GB) \\sim Ueq, Uanis(O1GA) \\sim Ueq: with sigma
of 0.002 and sigma for terminal atoms of 0.004
4. Rigid body (RIGU) restrains
 P1GB, C28, P1GA, O1GB, O1GA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C28(0.45016) H28(0.45016) O1S(0.48335) P1GB(0.23339) H1GB(0.23339)
 P1GA(0.31632) H1GA(0.31632) O1GA(0.31632) H1GC(0.31632) O1GB(0.23339)
 H1GD(0.23339)
6.a Ternary CH refined with riding coordinates:
 P1GB(H1GB), P1GA(H1GA)
6.b Aromatic/amide H refined with riding coordinates:
 O8(H8), O7(H7), C16(H16), C19(H19), C15(H15), C20(H20), C7(H7A), C3(H3),
 C26(H26), C11(H11), C6(H6), C27(H27), C9(H9), C4(H4), C23(H23), C22(H22),
 C13(H13), C28(H28)
6.c Tetrahedral OH refined with riding coordinates:
 O1GA(H1GC), O1GB(H1GD)
;
_shelx_res_checksum              7242
_shelx_hkl_checksum              22604
_shelx_fab_checksum              86981
_olex2_submission_special_instructions 'No special instructions were received'