Separation of Xylene Isomers through Multiple Metal Site Interactions in Metal-Organic Frameworks.
Gonzalez, Miguel I.; Kapelewski, Matthew T.; Bloch, Eric D.; Milner, Phillip J.; Reed, Douglas A.; Hudson, Matthew R.; Mason, Jarad A.; Barin, Gokhan; Brown, Craig M.; Long, Jeffrey R.; Journal of the American Chemical Society  (2018) –; doi:10.1021/jacs.7b13825

data_4127188
_publ_section_title
;
 Separation of Xylene Isomers through Multiple Metal Site Interactions in
 Metal-Organic Frameworks.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b13825
_journal_year                    2018
_chemical_formula_moiety         '(C8 H2 Co2 O6), 0.63(C8 H10), 0.61(H2 O)'
_chemical_formula_sum            'C14.15 H10.91 Co2 O6.61'
_chemical_formula_weight         404.56
_chemical_name_common            Co2(m-dobdc)(EB)0.63(H2O)0.61
_space_group_crystal_system      trigonal
_space_group_IT_number           160
_space_group_name_Hall           'R 3 -2"'
_space_group_name_H-M_alt        'R 3 m :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'intrinsic phasing'
_atom_sites_solution_secondary   difmap
_audit_creation_date             2017-09-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            9
_cell_length_a                   25.8977(9)
_cell_length_b                   25.8977(9)
_cell_length_c                   6.7599(3)
_cell_measurement_reflns_used    8536
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      34.271
_cell_measurement_theta_min      3.921
_cell_volume                     3926.4(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.42
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 with PHOTON100 CMOS detector'
_diffrn_measurement_method       '\f and \w shutterless scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.8856
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_av_unetI/netI     0.0339
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            15913
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        32.097
_diffrn_reflns_theta_max         34.484
_diffrn_reflns_theta_min         3.396
_diffrn_source                   'Advanced Light Source station 11.3.1'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.494
_exptl_absorpt_correction_T_max  0.940
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.1367 before and 0.0651 after correction.
The Ratio of minimum to maximum transmission is 0.9119.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1813
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.018
_exptl_crystal_size_min          0.018
_refine_diff_density_max         1.068
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 810 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.069(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2004
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0749P)^2^+1.7444P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1099
_reflns_Friedel_coverage         0.951
_reflns_Friedel_fraction_full    0.966
_reflns_Friedel_fraction_max     0.964
_reflns_number_gt                1853
_reflns_number_total             2004
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b13825_si_007.cif
_cod_data_source_block           mk011s_0m
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-07-04

The following automatic conversions were performed:

'_atom_sites_solution_secondary' value 'diffmap' was changed to
'difmap'.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 
;
_cod_database_code               4127188
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.940
_shelx_estimated_absorpt_t_min   0.572
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C6-C12
 1.512 with sigma of 0.02
 C13-C12
 1.523 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C6, C7, C8, C9, C10, C11, C12, C13
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Fixed Sof: O4(0.29773) C9(0.31384) H9(0.31384) C10(0.31384) H10(0.31384)
 C11(0.31384) H11(0.31384) C6(0.31384) C7(0.31384) H7(0.31384) C8(0.31384)
 H8(0.31384) C12(0.31384) H12A(0.31384) H12B(0.31384) C13(0.31384)
 H13A(0.31384) H13B(0.31384) H13C(0.31384)
5.a Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C7(H7), C8(H8)
5.c Fitted hexagon refined as free rotating group:
 C9(C10,C11,C6,C7,C8)
5.d Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C)
;
_shelx_res_checksum              45871
_shelx_hkl_checksum              96787
_olex2_submission_special_instructions 'No special instructions were received'