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_4129120
_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 H19.54 Al2 O10.51 P0.51, 0.65(C3 H7 N O)'
_chemical_formula_sum            'C30.06 H24.02 Al2 N0.69 O11.09 P0.41'
_chemical_formula_weight         638.75
_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             2019-05-17
_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                   18.6051(8)
_cell_length_b                   18.6051(8)
_cell_length_c                   37.3840(18)
_cell_measurement_reflns_used    9896
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.666
_cell_measurement_theta_min      2.245
_cell_volume                     12940.5(10)
_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 0.996
_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  0.0752
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            88734
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         27.192
_diffrn_reflns_theta_min         1.584
_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  0.6124
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0799 before and 0.0676 after correction. The Ratio of minimum to maximum transmission is 0.8215. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.656
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.021
_refine_ls_abs_structure_details
;
 Flack x determined using 4260 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.16(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     428
_refine_ls_number_reflns         13310
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      0.912
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0319P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0610
_refine_ls_wR_factor_ref         0.0631
_reflns_Friedel_coverage         0.781
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                11066
_reflns_number_total             13310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10501_si_012.cif
_cod_data_source_block           lambda-MOF-520-24
_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        12940.5(13)
_cod_database_code               4129120
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.991
_shelx_estimated_absorpt_t_min   0.991
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, H7 of O7, H8 of O8
 At 1.5 times of:
  All C(H,H,H) groups, H1G of O1G
2. Shared sites
{P1G, C28}
3. Uiso/Uaniso restraints and constraints
P1G \\sim O1G \\sim C1G: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
Uanis(P1G) = Uanis(C28)
4. Rigid body (RIGU) restrains
 O1S, C1S, N1S, C2S, C3S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C28)=Sof(H28)=1-FVAR(1)
 Sof(P1G)=Sof(O1G)=Sof(H1G)=Sof(C1G)=Sof(H1GA)=Sof(H1GB)=Sof(H1GC)=FVAR(1)
 Sof(O1S)=Sof(C1S)=Sof(H1S)=Sof(N1S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(H2SC)=
 Sof(C3S)=Sof(H3SA)=Sof(H3SB)=Sof(H3SC)=FVAR(2)
6.a Me refined with riding coordinates:
 C1G(H1GA,H1GB,H1GC), C2S(H2SA,H2SB,H2SC), C3S(H3SA,H3SB,H3SC)
6.b Aromatic/amide H refined with riding coordinates:
 O8(H8), O7(H7), C19(H19), C23(H23), C15(H15), C16(H16), C26(H26), C20(H20),
 C11(H11), C7(H7A), C3(H3), C9(H9), C13(H13), C6(H6), C4(H4), C22(H22),
 C27(H27), C28(H28), C1S(H1S)
6.c Idealised tetrahedral OH refined as rotating group:
 O1G(H1G)
;
_shelx_res_checksum              21498
_shelx_hkl_checksum              80491
_shelx_fab_checksum              26337
_olex2_submission_special_instructions 'No special instructions were received'