Benchmark selectivity p-xylene separation by a non-porous molecular solid through liquid or vapor extraction
Sun, Na; Wang, Shi-Qiang; Zou, Ruqiang; Cui, Wen-Gang; Zhang, Anqi; Zhang, Tianzhen; Li, Qi; Zhuang, Zhan-Zhong; Zhang, Ying-Hui; Xu, Jialiang; Zaworotko, Michael J.; Bu, Xian-He; Chemical Science  (2019) –; doi:10.1039/C9SC02621E

data_1552199
_publ_section_title
;
 Benchmark selectivity p-xylene separation by a non-porous molecular solid
 through liquid or vapor extraction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02621E
_journal_year                    2019
_chemical_formula_moiety         'C26 H20 Ag N8, Cl O4, 0.5(C8 H10)'
_chemical_formula_sum            'C30 H25 Ag Cl N8 O4'
_chemical_formula_weight         704.90
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc21f5zn
_audit_creation_date             2018-10-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-01-25 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                67.1420(10)
_cell_angle_beta                 76.6260(10)
_cell_angle_gamma                86.6820(10)
_cell_formula_units_Z            2
_cell_length_a                   10.73870(10)
_cell_length_b                   11.8558(2)
_cell_length_c                   12.6250(2)
_cell_measurement_reflns_used    12643
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.9700
_cell_measurement_theta_min      5.0430
_cell_volume                     1440.05(4)
_computing_cell_refinement       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.33c (Rigaku OD, 2017)'
_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_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -53.00  29.00   0.50    0.50    --    0.00 -57.00 120.00  164
  2  \w    -88.00 -56.00   0.50    0.50    --    0.00 -57.00 120.00   64
  3  \w    -37.00 -10.00   0.50    0.50    --    0.00 -38.00-120.00   54
  4  \w    -32.00  21.00   0.50    0.50    --    0.00  38.00 120.00  106
  5  \w     31.00  87.00   0.50    0.50    --    0.00  38.00 120.00  112
  6  \w     -5.00  21.00   0.50    0.50    --    0.00 -38.00-120.00   52
  7  \w     65.00 183.00   0.50    0.50    --   95.80  45.00 -60.00  236
  8  \w    108.00 184.00   0.50    0.50    --   95.80  45.00  30.00  152
  9  \w      6.00  50.00   0.50    0.50    --   95.80 -82.00  90.00   88
 10  \w     49.00 122.00   0.50    0.50    --   95.80 -61.00-180.00  146
 11  \w     90.00 183.00   0.50    0.50    --   95.80  45.00 -30.00  186
 12  \w     11.00 105.00   0.50    0.50    --   95.80 -61.00  90.00  188
 13  \w     51.00 126.00   0.50    0.50    --   95.80 -61.00 -60.00  150
 14  \w     72.00  99.00   0.50    0.50    --   95.80 -82.00  30.00   54
 15  \w     59.00 132.00   0.50    0.50    --   95.80 -82.00-180.00  146
 16  \w     54.00 132.00   0.50    0.50    --   95.80 -82.00  90.00  156
 17  \w     78.00 103.00   0.50    0.50    --   95.80 -82.00-120.00   50
 18  \w    100.00 168.00   0.50    0.50    --   95.80  61.00-120.00  136
 19  \w     10.00 132.00   0.50    0.50    --   95.80 -82.00 -60.00  244
 20  \w    112.00 180.00   0.50    0.50    --   95.80  45.00   0.00  136
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0102852000
_diffrn_orient_matrix_UB_12      -0.0708245000
_diffrn_orient_matrix_UB_13      -0.0811850000
_diffrn_orient_matrix_UB_21      0.1211071000
_diffrn_orient_matrix_UB_22      -0.0609098000
_diffrn_orient_matrix_UB_23      0.0395176000
_diffrn_orient_matrix_UB_31      -0.0836598000
_diffrn_orient_matrix_UB_32      -0.1057576000
_diffrn_orient_matrix_UB_33      0.1016665000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0175
_diffrn_reflns_av_unetI/netI     0.0171
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14307
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.078
_diffrn_reflns_theta_min         3.902
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    6.910
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.33c (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.626
_exptl_crystal_description       block
_exptl_crystal_F_000             714
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.164
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         5659
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0639P)^2^+2.3401P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1044
_refine_ls_wR_factor_ref         0.1047
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5584
_reflns_number_total             5659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02621e2.cif
_cod_data_source_block           m-xylene@M
_cod_database_code               1552199
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.874
_shelx_estimated_absorpt_t_min   0.724
_reflns_odcompleteness_completeness 99.73
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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
 C34-C30
 1.55 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34:
within 1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.003 and sigma for
terminal atoms of 0.006
4. Others
 Fixed Sof: C32(0.5) C27(0.5) H27(0.5) C28(0.5) H28(0.5) C29(0.5) H29(0.5)
 C30(0.5) C31(0.5) H31(0.5) C33(0.5) H33A(0.5) H33B(0.5) H33C(0.5) C34(0.5)
 H34A(0.5) H34B(0.5) H34C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C18(H18A,H18B)
5.b Me refined with riding coordinates:
 C33(H33A,H33B,H33C), C34(H34A,H34B,H34C)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C6(H6), C9(H9), C10(H10), C13(H13), C14(H14),
 C15(H15), C16(H16), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C29(H29), C31(H31)
5.d Fitted hexagon refined as free rotating group:
 C32(C27,C28,C29,C30,C31)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.895
_oxdiff_exptl_absorpt_empirical_full_min 0.689