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_4129121
_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_formula_moiety         'C30.61 H21.53 Al2 O10 S0.52, 0.25(O)'
_chemical_formula_sum            'C30.61 H21.53 Al2 O10.25 S0.52'
_chemical_formula_weight         623.98
_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                   18.6986(11)
_cell_length_b                   18.6986(11)
_cell_length_c                   37.201(3)
_cell_measurement_reflns_used    9436
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.12
_cell_measurement_theta_min      2.23
_cell_volume                     13006.9(15)
_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 0.997
_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  0.0993
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            132943
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        23.886
_diffrn_reflns_theta_max         23.886
_diffrn_reflns_theta_min         2.021
_diffrn_source
;
Advanced Light Source, station 12.2.1
;
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.6502
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1261 before and 0.0741 after correction. The Ratio of minimum to maximum transmission is 0.8728. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.637
_exptl_crystal_description       block
_exptl_crystal_F_000             2572
_exptl_crystal_size_max          0.095
_exptl_crystal_size_mid          0.069
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details
;
 Flack x determined using 2926 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         9350
_refine_ls_number_restraints     159
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0646
_refine_ls_R_factor_gt           0.0541
_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^)+(0.1123P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1465
_refine_ls_wR_factor_ref         0.1560
_reflns_Friedel_coverage         0.760
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                7700
_reflns_number_total             9350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10501_si_017.cif
_cod_data_source_block           lambda-MOF-520-29
_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        13006.8(18)
_cod_database_code               4129121
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.991
_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
 C4GB-C3GB = C3GB-C2GB = C1GB-C2GB = C1GB-C6GB = C5GB-C6GB = C4GB-C5GB
 1.54 with sigma of 0.005
 O9-C28 = O10-C28
 1.27 with sigma of 0.005
 C2GA-C3GA \\sim C1GA-C2GA \\sim C1GA-C6GA \\sim C6GA-C5GA \\sim C4GA-C5GA
\\sim C4GA-C3GA
 with sigma of 0.02
 C2GB-C4GB \\sim C4GB-C6GB \\sim C6GB-C2GB
 with sigma of 0.02
 C1GB-C3GB \\sim C3GB-C5GB \\sim C5GB-C1GB
 with sigma of 0.02
 C1GB-C3GB \\sim C2GB-C4GB
 with sigma of 0.02
 S1GA-C1GA \\sim S1GB-C1GB
 with sigma of 0.02
3. Rigid bond restraints
 C2GA, C3GA, C4GA, C5GA, C6GA, C1GA
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C2GB, C1GB, C6GB, C3GB, C5GB, C4GB
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1GA \\sim C6GA \\sim C5GA \\sim C4GA \\sim C3GA \\sim C2GA: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C3GB \\sim C2GB \\sim C1GB \\sim C6GB \\sim C5GB \\sim C4GB: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C5GB) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.03
Uanis(S1GA) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(S1GB) \\sim Ueq: with sigma
of 0.004 and sigma for terminal atoms of 0.008
5. Others
 Fixed Sof: S1GB(0.29196) S1GA(0.22986) C28(0.47819) H28(0.47819)
 C1GA(0.22986) C6GA(0.22986) H6GA(0.22986) H6GB(0.22986) C6GB(0.29196)
 H6GC(0.29196) H6GD(0.29196) C2GB(0.29196) H2GA(0.29196) H2GB(0.29196)
 C3GA(0.22986) H3GA(0.22986) H3GB(0.22986) C1GB(0.29196) C2GA(0.22986)
 H2GC(0.22986) H2GD(0.22986) C5GA(0.22986) H5GA(0.22986) H5GB(0.22986)
 C4GA(0.22986) H4GA(0.22986) H4GB(0.22986) C3GB(0.29196) H3GC(0.29196)
 H3GD(0.29196) C5GB(0.29196) C4GB(0.29196)
6.a Secondary CH2 refined with riding coordinates:
 C6GA(H6GA,H6GB), C6GB(H6GC,H6GD), C2GB(H2GA,H2GB), C3GA(H3GA,H3GB), C2GA(H2GC,
 H2GD), C5GA(H5GA,H5GB), C4GA(H4GA,H4GB), C3GB(H3GC,H3GD)
6.b Aromatic/amide H refined with riding coordinates:
 O8(H8), O7(H7), C7(H7A), C16(H16), C19(H19), C6(H6), C15(H15), C11(H11),
 C3(H3), C20(H20), C23(H23), C13(H13), C9(H9), C26(H26), C22(H22), C4(H4),
 C27(H27), C28(H28)
;
_shelx_res_checksum              29795
_shelx_hkl_checksum              43374
_shelx_fab_checksum              7296
_olex2_submission_special_instructions 'No special instructions were received'