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_4129115
_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
'C33.29 H23.81 Al2 B0.51 N1.01 O10, 0.21(O), 0.46(C)'
_chemical_formula_sum            'C33.75 H23.81 Al2 B0.51 N1.02 O10.21'
_chemical_formula_weight         666.40
_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             2019-06-17
_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                   19.2915(5)
_cell_length_b                   19.2915(5)
_cell_length_c                   36.0810(11)
_cell_measurement_reflns_used    9683
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.78
_cell_volume                     13428.0(6)
_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 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_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 0.995
_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_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0942
_diffrn_reflns_av_unetI/netI     0.0471
_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       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            128287
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        23.605
_diffrn_reflns_theta_max         23.605
_diffrn_reflns_theta_min         1.919
_diffrn_source                   'Advanced Light Source, station 12.2.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1922 before and 0.0942 after correction. The Ratio of minimum to maximum transmission is 0.8863. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.659
_exptl_crystal_description       block
_exptl_crystal_F_000             2749
_exptl_crystal_size_max          0.057
_exptl_crystal_size_mid          0.057
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Flack x determined using 3726 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.06(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     600
_refine_ls_number_reflns         9297
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0544
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1026P)^2^+2.6675P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1434
_refine_ls_wR_factor_ref         0.1479
_reflns_Friedel_coverage         0.762
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                8804
_reflns_number_total             9297
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10501_si_018.cif
_cod_data_source_block           delta-MOF-520-30-activated
_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        13428.0(8)
_cod_database_code               4129115
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.996
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C13B-C9B
 1.54 with sigma of 0.02
 O9-C28 \\sim O10-C28
 with sigma of 0.02
 O2GB-B1GB \\sim O2GA-B1GA \\sim O1GB-B1GB \\sim O1GA-B1GA
 with sigma of 0.02
 C10B-C10A \\sim C11B-C11A \\sim C13A-C12A
 with sigma of 0.02
 O2GB-C9B \\sim O2GA-C9A \\sim O1GB-C8B \\sim O1GA-C8A
 with sigma of 0.02
 C8A-C9A \\sim C8B-C9B
 with sigma of 0.02
 C13B-C9B \\sim C13A-C9A \\sim C9A-C12A \\sim C8B-C11B \\sim C8B-C10B \\sim
C11A-C8A \\sim C8A-C10A ~
 C9B-C12B
 with sigma of 0.02
3. Restrained planarity
 O2GC, O1GC, B1GC, C6GB, C5GB, C4GB, C3GB, C2GB, C7GB
 with sigma of 0.1
4. Rigid body (RIGU) restrains
 O10, N2G, C28, N1G, O9
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C2GA(0.30759) C1GA(0.30759) H1GA(0.30759) C3GA(0.30759)
 N1G(0.50749) O9(0.49251) O10(0.49251) N2G(0.50749) C28(0.49251) H28(0.49251)
 C2GB(0.1999) C4GA(0.30759) H4GA(0.30759) C5GA(0.30759) H5GA(0.30759)
 C7GA(0.30759) H7GA(0.30759) C6GA(0.30759) C4GB(0.1999) H4GB(0.1999)
 C6GB(0.1999) C7GB(0.1999) H7GB(0.1999) C5GB(0.1999) H5GB(0.1999) C1GB(0.1999)
 H1GB(0.1999) C3GB(0.1999) O1GA(0.1538) O2GA(0.1538) B1GB(0.1538) O2GC(0.1999)
 O1GC(0.1999) C8GB(0.1999) B1GC(0.1999) O1S(0.21465) O2GB(0.1538) C9A(0.1538)
 C13A(0.1538) H13A(0.1538) H13B(0.1538) H13C(0.1538) C12A(0.1538) H12A(0.1538)
 H12B(0.1538) H12C(0.1538) O1GB(0.1538) C11A(0.1538) H11A(0.1538) H11B(0.1538)
 H11C(0.1538) C8B(0.1538) C10A(0.1538) H10A(0.1538) H10B(0.1538) H10C(0.1538)
 B1GA(0.1538) C9GB(0.1999) H9GA(0.1999) H9GB(0.1999) H9GC(0.1999) C9B(0.1538)
 C8A(0.1538) C1S(0.45596) C10B(0.1538) H10D(0.1538) H10E(0.1538) H10F(0.1538)
 C11B(0.1538) H11D(0.1538) H11E(0.1538) H11F(0.1538) C13B(0.1538) H13D(0.1538)
 H13E(0.1538) H13F(0.1538) C12B(0.1538) H12D(0.1538) H12E(0.1538) H12F(0.1538)
 Fixed Uiso: C12A(0.15) C8B(0.15) C11B(0.15) C13B(0.15)
6.a Me refined with riding coordinates:
 C13A(H13A,H13B,H13C), C12A(H12A,H12B,H12C), C11A(H11A,H11B,H11C), C10A(H10A,
 H10B,H10C), C9GB(H9GA,H9GB,H9GC), C10B(H10D,H10E,H10F), C11B(H11D,H11E,H11F),
 C13B(H13D,H13E,H13F), C12B(H12D,H12E,H12F)
6.b Aromatic/amide H refined with riding coordinates:
 O8(H8), O7(H7), C3(H3), C19(H19), C7(H7A), C26(H26), C23(H23), C20(H20),
 C13(H13), C6(H6), C11(H11), C4(H4), C15(H15), C27(H27), C22(H22), C16(H16),
 C9(H9), C1GA(H1GA), C28(H28), C4GA(H4GA), C5GA(H5GA), C7GA(H7GA), C4GB(H4GB),
 C7GB(H7GB), C5GB(H5GB), C1GB(H1GB)
;
_shelx_res_checksum              85997
_shelx_hkl_checksum              89074
_olex2_submission_special_instructions 'No special instructions were received'