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_4129110
_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         'C31.59 H19.8 Al2 N1.2 O8.8, 0.25(O)'
_chemical_formula_sum            'C31.59 H19.8 Al2 N1.2 O9.05'
_chemical_formula_weight         614.96
_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             2019-06-16
_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                   19.0466(6)
_cell_length_b                   19.0466(6)
_cell_length_c                   36.3890(12)
_cell_measurement_reflns_used    9852
_cell_measurement_temperature    100
_cell_measurement_theta_max      56.766
_cell_measurement_theta_min      3.360
_cell_volume                     13200.9(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      100.0
_diffrn_detector                 'Bruker PHOTON-II detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture with PHOTON-II detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0367
_diffrn_reflns_av_unetI/netI     0.0493
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            34031
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        58.280
_diffrn_reflns_theta_max         58.280
_diffrn_reflns_theta_min         3.359
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.621
_exptl_absorpt_correction_T_max  0.7514
_exptl_absorpt_correction_T_min  0.6707
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0813 before and 0.0435 after correction. The Ratio of minimum to maximum transmission is 0.8926. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    0.619
_exptl_crystal_description       block
_exptl_crystal_F_000             2529
_exptl_crystal_size_max          0.9
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.487
_refine_diff_density_rms         0.176
_refine_ls_abs_structure_details
;
 Flack x determined using 2548 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.230(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.423
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         9065
_refine_ls_number_restraints     134
_refine_ls_restrained_S_all      1.418
_refine_ls_R_factor_all          0.1465
_refine_ls_R_factor_gt           0.1250
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3230
_refine_ls_wR_factor_ref         0.3391
_reflns_Friedel_coverage         0.753
_reflns_Friedel_fraction_full    0.971
_reflns_Friedel_fraction_max     0.971
_reflns_number_gt                7223
_reflns_number_total             9065
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b10501_si_019.cif
_cod_data_source_block           lambda-MOF_520-30-solvated
_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        13200.9(9)
_cod_original_formula_sum        'C31.59 H19.80 Al2 N1.20 O9.05'
_cod_database_code               4129110
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.935
_shelx_estimated_absorpt_t_min   0.605
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H) groups
2. Restrained distances
 O10-C28 \\sim O9-C28
 with sigma of 0.02
 C5GB-C4GB \\sim C4GB-C3G \\sim C5GB-C6GB \\sim C7GB-C6GB \\sim C7GB-C2GB \\sim
C2GB-C3G
 with sigma of 0.02
 C2GA-C1GA \\sim C2GB-C1GB
 with sigma of 0.02
 N1G-C1GA \\sim N1G-C1GB
 with sigma of 0.02
 C5GA-C6GA \\sim C6GA-C7GA \\sim C7GA-C2GA \\sim C2GA-C3G \\sim C4GA-C3G \\sim
C5GA-C4GA
 with sigma of 0.02
 N1G-C1GA \\sim N1G-C1GB \\sim N2G-C3G
 with sigma of 0.02
3. Restrained planarity
 C7GA, C2GA, C3G, C4GA, C5GA, C6GA
 with sigma of 0.1
 C2GB, C7GB, C6GB, C5GB, C4GB, C3G
 with sigma of 0.1
 C7GA, C6GA, C5GA, C4GA, C3G, C2GA
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
O10 \\sim C28 \\sim O9: within 1.7A with sigma of 0.02 and sigma for terminal
atoms of 0.04
C1GB \\sim C2GB \\sim C7GB \\sim C6GB \\sim C5GB \\sim C4GB: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C1GA \\sim C2GA \\sim C7GA \\sim C6GA \\sim C5GA \\sim C4GA: within 1.7A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C1GB \\sim C1GA: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
C2GB \\sim C2GA: within 1.7A with sigma of 0.02 and sigma for terminal atoms of
0.04
Uanis(C2GB) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N2G) = Uanis(N1G)
5. Others
 Fixed Sof: N1G(0.59879) N2G(0.59879) C3G(0.59879) C2GB(0.28234) C1GB(0.28234)
 H1GB(0.28234) C1GA(0.31646) H1GA(0.31646) C2GA(0.31646) C28(0.40121)
 H28(0.40121) O9(0.40121) O10(0.40121) C4GB(0.28234) H4GB(0.28234)
 C5GA(0.31646) H5GA(0.31646) C5GB(0.28234) H5GB(0.28234) C4GA(0.31646)
 H4GA(0.31646) C6GA(0.31646) C6GB(0.28234) C7GA(0.31646) H7GA(0.31646)
 C7GB(0.28234) H7GB(0.28234)
6.a Aromatic/amide H refined with riding coordinates:
 O8(H8), O7(H7), C7(H7A), C4(H4), C3(H3), C19(H19), C20(H20), C16(H16),
 C26(H26), C9(H9), C23(H23), C6(H6), C13(H13), C15(H15), C22(H22), C27(H27),
 C11(H11), C1GB(H1GB), C1GA(H1GA), C28(H28), C4GB(H4GB), C5GA(H5GA), C5GB(H5GB),
  C4GA(H4GA), C7GA(H7GA), C7GB(H7GB)
;
_shelx_res_checksum              58801
_shelx_hkl_checksum              68250
_olex2_submission_special_instructions 'No special instructions were received'