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_4129131
_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
'C33.76 H22.72 Al2 N1.83 O9.74, 0.23(O), C0.69 O0.5'
_chemical_formula_sum            'C34.45 H22.72 Al2 N1.83 O10.47'
_chemical_formula_weight         683.81
_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
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Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
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_cell_length_b                   19.079(3)
_cell_length_c                   36.683(5)
_cell_measurement_reflns_used    9538
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.19
_cell_measurement_theta_min      5.18
_cell_volume                     13353(3)
_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-2018/03 (Sheldrick, 2018)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 7.39
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.994
_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  0.0562
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_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       49
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            146105
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        28.500
_diffrn_reflns_theta_max         29.341
_diffrn_reflns_theta_min         1.922
_diffrn_source
;
Advanced Light Source, station 12.2.1
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_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8051
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.680
_exptl_crystal_description       block
_exptl_crystal_F_000             2816
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.104
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details
;
 Flack x determined using 6177 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.126(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         16935
_refine_ls_number_restraints     391
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0532
_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^)+(0.1135P)^2^+0.1333P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1504
_reflns_Friedel_coverage         0.797
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                15030
_reflns_number_total             16935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10501_si_020.cif
_cod_data_source_block           delta-MOF-520-31-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        13353(4)
_cod_database_code               4129131
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.989
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
2. Restrained distances
 C21A-C20A
 1.54 with sigma of 0.02
 C22A-C21A \\sim C22B-C21B
 with sigma of 0.02
 O9A-C22A \\sim O9B-C22B \\sim O9A-C21A \\sim O9B-C21B
 with sigma of 0.02
 C23A-C21A \\sim C22A-C20A
 with sigma of 0.02
 C23B-C22B \\sim C20B-C21B \\sim C21A-C20A \\sim C23A-C22A
 with sigma of 0.02
 C22B-C20B \\sim C23B-C21B
 with sigma of 0.02
 C23B-C20B \\sim C22B-C21B
 with sigma of 0.04
 N7GA-C17A \\sim N7GB-C17B
 with sigma of 0.02
 N7GA-C23A \\sim N7GB-C23B \\sim N7GA-C20A \\sim N7GB-C20B
 with sigma of 0.02
3. Restrained planarity
 N7GA, C18A, C17A, C16A
 with sigma of 0.1
 C9GB, N3GB, C10B, C11B, N4GB, C12B, C13B, N5GB, C8GB
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
Uanis(C7GA) \\sim Ueq, Uanis(C7GB) \\sim Ueq, Uanis(C6GB) \\sim Ueq,
Uanis(C6GA) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(N6GA) \\sim Ueq, Uanis(N6GB) \\sim Ueq, Uanis(C14A) \\sim Ueq,
Uanis(C14B) \\sim Ueq, Uanis(C15A) \\sim Ueq, Uanis(C15B) \\sim Ueq,
Uanis(C16A) \\sim Ueq, Uanis(C16B) \\sim Ueq, Uanis(C17A) \\sim Ueq,
Uanis(C17B) \\sim Ueq, Uanis(C19A) \\sim Ueq, Uanis(C19B) \\sim Ueq,
Uanis(C18A) \\sim Ueq, Uanis(C18B) \\sim Ueq: with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C23B) \\sim Ueq, Uanis(C23A) \\sim Ueq, Uanis(N7GB) \\sim Ueq,
Uanis(N7GA) \\sim Ueq, Uanis(C20A) \\sim Ueq, Uanis(C20B) \\sim Ueq,
Uanis(C21A) \\sim Ueq, Uanis(C21B) \\sim Ueq, Uanis(O9A) \\sim Ueq, Uanis(O9B)
\\sim Ueq, Uanis(C22B) \\sim Ueq, Uanis(C22A) \\sim Ueq: with sigma of 0.02 and
sigma for terminal atoms of 0.04
Uanis(C9GB) \\sim Ueq, Uanis(C9GA) \\sim Ueq, Uanis(C8GA) \\sim Ueq,
Uanis(C8GB) \\sim Ueq, Uanis(N5GB) \\sim Ueq, Uanis(N5GA) \\sim Ueq,
Uanis(C13B) \\sim Ueq, Uanis(C13A) \\sim Ueq, Uanis(C12B) \\sim Ueq,
Uanis(N3GB) \\sim Ueq, Uanis(N3GA) \\sim Ueq, Uanis(C12A) \\sim Ueq,
Uanis(C10B) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C11A) \\sim Ueq,
Uanis(C11B) \\sim Ueq, Uanis(N4GB) \\sim Ueq, Uanis(N4GA) \\sim Ueq: with sigma
of 0.02 and sigma for terminal atoms of 0.04
5. Rigid body (RIGU) restrains
 C23B, N7GB, C20B, C21B, O9B, C22B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C22A, C23A, N7GA, C20A, C21A, O9A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
 Fixed Sof: O10(0.73804) N1G(0.26196) C28(0.73804) H28(0.73804) C3G(0.26196)
 C2G(0.26196) C1G(0.26196) H1G(0.26196) C4G(0.26196) H4G(0.26196) O9(0.73804)
 N2G(0.26196) C13B(0.13098) N5GB(0.13098) C8GB(0.13098) C9GB(0.13098)
 H9GB(0.13098) O9A(0.13098) C21A(0.13098) H21A(0.13098) H21B(0.13098)
 C20B(0.13098) H20A(0.13098) H20B(0.13098) C22B(0.13098) H22A(0.13098)
 H22B(0.13098) O1S(0.22775) O2S(0.50423) C7GB(0.13098) H7GB(0.13098)
 C7GA(0.13098) H7GA(0.13098) C6GA(0.13098) H6GA(0.13098) C6GB(0.13098)
 H6GB(0.13098) C5G(0.26196) C8GA(0.13098) C9GA(0.13098) H9GA(0.13098)
 N3GA(0.13098) C12A(0.13098) C13A(0.13098) N5GA(0.13098) C11B(0.13098)
 H11B(0.13098) N4GB(0.13098) C12B(0.13098) N3GB(0.13098) C10B(0.13098)
 H10B(0.13098) C10A(0.13098) H10A(0.13098) C11A(0.13098) H11A(0.13098)
 N4GA(0.13098) N6GA(0.13098) N6GB(0.13098) C19A(0.13098) H19A(0.13098)
 C14A(0.13098) C15A(0.13098) H15A(0.13098) C16A(0.13098) H16A(0.13098)
 C17A(0.13098) C18A(0.13098) H18A(0.13098) C19B(0.13098) H19B(0.13098)
 C14B(0.13098) C15B(0.13098) H15B(0.13098) C16B(0.13098) H16B(0.13098)
 C17B(0.13098) C18B(0.13098) H18B(0.13098) C1S(0.38748) C2S(0.29929)
 N7GB(0.13098) C23A(0.13098) H23A(0.13098) H23B(0.13098) C22A(0.13098)
 H22C(0.13098) H22D(0.13098) C21B(0.13098) H21C(0.13098) H21D(0.13098)
 O9B(0.13098) C20A(0.13098) H20C(0.13098) H20D(0.13098) C23B(0.13098)
 H23C(0.13098) H23D(0.13098) N7GA(0.13098)
7.a Secondary CH2 refined with riding coordinates:
 C21A(H21A,H21B), C20B(H20A,H20B), C22B(H22A,H22B), C23A(H23A,H23B), C22A(H22C,
 H22D), C21B(H21C,H21D), C20A(H20C,H20D), C23B(H23C,H23D)
7.b Aromatic/amide H refined with riding coordinates:
 O8(H8), O7(H7), C7(H7A), C13(H13), C3(H3), C4(H4), C19(H19), C22(H22),
 C27(H27), C26(H26), C23(H23), C6(H6), C20(H20), C9(H9), C16(H16), C15(H15),
 C11(H11), C28(H28), C1G(H1G), C4G(H4G), C9GB(H9GB), C7GB(H7GB), C7GA(H7GA),
 C6GA(H6GA), C6GB(H6GB), C9GA(H9GA), C11B(H11B), C10B(H10B), C10A(H10A),
 C11A(H11A), C19A(H19A), C15A(H15A), C16A(H16A), C18A(H18A), C19B(H19B),
 C15B(H15B), C16B(H16B), C18B(H18B)
7.c Fitted pentagon refined as free rotating group:
 C11B(N4GB,C12B,N3GB,C10B)
7.d Fitted hexagon refined as free rotating group:
 C8GA(C9GA,N3GA,C12A,C13A,N5GA), C19A(C14A,C15A,C16A,C17A,C18A), C19B(C14B,
 C15B,C16B,C17B,C18B)
;
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_olex2_submission_special_instructions 'No special instructions were received'