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_1552200
_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         '2(C26 H20 Ag N8), 2(Cl O4), 2(C8 H10)'
_chemical_formula_sum            'C68 H60 Ag2 Cl2 N16 O8'
_chemical_formula_weight         1515.96
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc21f60q
_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                90
_cell_angle_beta                 97.7230(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.99950(10)
_cell_length_b                   23.1335(3)
_cell_length_c                   20.7862(2)
_cell_measurement_reflns_used    22953
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.8570
_cell_measurement_theta_min      2.8550
_cell_volume                     6670.70(12)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.969
_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     24.00  89.00   0.50    0.50    --    0.00  77.00-150.00  130
  2  \w    -35.00  21.00   0.50    0.50    --    0.00  77.00-150.00  112
  3  \w    -53.00  25.00   0.50    0.50    --    0.00  19.00-180.00  156
  4  \w    -21.00   4.00   0.50    0.50    --    0.00  57.00  60.00   50
  5  \w     67.00 145.00   0.50    0.50    --   95.80  61.00 150.00  156
  6  \w     14.00  83.00   0.50    0.50    --   95.80 -45.00   0.00  138
  7  \w     93.00 152.00   0.50    0.50    --   95.80  45.00-150.00  118
  8  \w      9.00 125.00   0.50    0.50    --   95.80 -61.00   0.00  232
  9  \w     89.00 171.00   0.50    0.50    --   95.80  45.00 -90.00  164
 10  \w     83.00 137.00   0.50    0.50    --   95.80  45.00-180.00  108
 11  \w     78.00 178.00   0.50    0.50    --   95.80  45.00-120.00  200
;
_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      0.0349242000
_diffrn_orient_matrix_UB_12      0.0257614000
_diffrn_orient_matrix_UB_13      -0.0611014000
_diffrn_orient_matrix_UB_21      0.0532873000
_diffrn_orient_matrix_UB_22      0.0481103000
_diffrn_orient_matrix_UB_23      0.0416350000
_diffrn_orient_matrix_UB_31      0.0909170000
_diffrn_orient_matrix_UB_32      -0.0381876000
_diffrn_orient_matrix_UB_33      0.0112867000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0276
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            37953
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.299
_diffrn_reflns_theta_min         2.872
_diffrn_source                   'Rotating-anode X-ray tube (dual wavelength)'
_diffrn_source_type              'Rigaku (Cu) X-ray DW Source'
_exptl_absorpt_coefficient_mu    6.010
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55215
_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    1.509
_exptl_crystal_description       block
_exptl_crystal_F_000             3088
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
TITL lin_a.res in P2(1)/c
CELL   13.9995   23.1335   20.7862     90.00     97.72     90.00
SPGR P21/c
Q101 0.780 0.442 0.278 !      10.74 eA-3
Q102 0.780 0.435 0.346 !       4.23 eA-3
C103 0.017 0.513 0.453 !       3.70 eA-3
C104 0.094 0.553 0.466 !       3.34 eA-3
Q105 0.269 0.935 0.285 !       3.33 eA-3
Q106 0.297 0.302 0.310 !       2.90 eA-3
C107 0.891 0.451 0.465 !       2.90 eA-3
C108 0.055 0.986 0.062 !       2.83 eA-3
C109 0.251 0.894 0.017 !       2.65 eA-3
C110 0.044 0.986 0.037 !       2.59 eA-3
Q111 0.191 0.286 0.190 !       2.57 eA-3
C112 0.810 0.412 0.436 !       2.42 eA-3
C113 0.846 0.083 0.077 !       2.29 eA-3
Q114 0.799 0.488 0.248 !       1.83 eA-3
Q115 0.755 0.113 0.173 !       1.76 eA-3
Q116 0.751 0.250 0.004 !       1.62 eA-3
Q117 0.738 0.159 0.284 !       1.54 eA-3
C118 0.219 0.631 0.470 !       1.42 eA-3
Q119 0.704 0.488 0.233 !       1.38 eA-3
C120 0.205 0.585 0.469 !       1.36 eA-3
Q121 0.778 0.392 0.236 !       1.34 eA-3
Q122 0.720 0.441 0.157 !       1.20 eA-3
Q123 0.674 0.231 0.011 !       1.09 eA-3
Q124 0.932 0.203 0.000 !       1.08 eA-3
Q125 0.468 0.228 0.499 !       1.07 eA-3
Q126 0.279 0.593 0.270 !       1.06 eA-3
Q127 0.723 0.394 0.250 !       1.04 eA-3
Q128 0.937 0.163 0.002 !       1.03 eA-3
Q129 0.982 0.126-0.005 !       1.01 eA-3
Q130 0.189 0.283 0.141 !       1.01 eA-3
Q131 0.826 0.066 0.300 !       0.97 eA-3
Q132 0.885 0.460 0.266 !       0.96 eA-3
Q133 0.667 0.080 0.263 !       0.96 eA-3
Q134 0.391 0.285 0.499 !       0.93 eA-3
Q135 0.405 0.316 0.020 !       0.92 eA-3
C136 0.139 0.964 0.092 !       0.92 eA-3
Q137 0.474 0.914 0.050 !       0.88 eA-3
Q138 0.360 0.204 0.316 !       0.87 eA-3
Q139 0.877 0.706 0.311 !       0.87 eA-3
Q140 0.140 0.048 0.388 !       0.85 eA-3
Q141 0.092 0.327 0.498 !       0.85 eA-3
Q142 0.858 0.166 0.002 !       0.83 eA-3
Q143 0.607 0.331-0.003 !       0.79 eA-3
Q144 0.138 0.759 0.343 !       0.77 eA-3
Q145 0.311 0.446 0.443 !       0.76 eA-3
Q146 0.596 0.275 0.017 !       0.76 eA-3
Q147 0.211 0.266 0.162 !       0.75 eA-3
Q148 0.373 0.433 0.425 !       0.75 eA-3
Q149 0.373 0.058 0.919 !       0.75 eA-3
C150 0.954 0.082 0.012 !       0.75 eA-3
C151 0.035 0.923 0.999 !       0.74 eA-3
Q152 0.437 0.115 0.500 !       0.74 eA-3
Q153 0.749 0.924 0.328 !       0.72 eA-3
Q154 0.580 0.560 0.485 !       0.71 eA-3
Q155 0.860 0.936 0.439 !       0.71 eA-3
Q156 0.299 0.642 0.020 !       0.68 eA-3
Q157 0.404 0.353 0.000 !       0.67 eA-3
Q158 0.313 0.289 0.375 !       0.67 eA-3
Q159 0.907 0.488 0.377 !       0.67 eA-3
Q160 0.516 0.372 0.009 !       0.67 eA-3
Q161 0.676 0.937 0.155 !       0.67 eA-3
Q162 0.199 0.588 0.233 !       0.66 eA-3
Q163 0.996 0.415 0.061 !       0.65 eA-3
Q164 0.158 0.943 0.188 !       0.65 eA-3
C165 0.852 0.128 0.048 !       0.64 eA-3
Q166 0.054 0.112 0.000 !       0.63 eA-3
C167 0.029 0.033 0.015 !       0.62 eA-3
Q168 0.363 0.042 0.096 !       0.62 eA-3
Q169 0.338 0.979 0.234 !       0.61 eA-3
C170 0.840 0.138 0.076 !       0.61 eA-3
Q171 0.240 0.899 0.483 !       0.60 eA-3
Q172 0.813 0.406 0.312 !       0.60 eA-3
Q173 0.013 0.286 0.155 !       0.60 eA-3
Q174 0.825 0.927 0.343 !       0.60 eA-3
Q175 0.252 0.172 0.247 !       0.60 eA-3
C176 0.813 0.290 0.501 !       0.59 eA-3
Q177 0.830 0.072 0.238 !       0.59 eA-3
Q178 0.748 0.115 0.329 !       0.58 eA-3
Q179 0.112 0.261 0.330 !       0.57 eA-3
Q180 0.911 0.563 0.016 !       0.57 eA-3
Q181 1.001 0.644 0.340 !       0.57 eA-3
Q182 0.358 0.953 0.394 !       0.56 eA-3
Q183 0.979 0.673 0.330 !       0.56 eA-3
Q184 0.247 0.022 0.252 !       0.56 eA-3
Q185 0.342 0.892 0.217 !       0.55 eA-3
Q186 0.619 0.766 0.328 !       0.55 eA-3
Q187 0.832 0.971 0.154 !       0.55 eA-3
Q188 0.155 0.892 0.279 !       0.54 eA-3
Q189 0.684 0.404 0.202 !       0.54 eA-3
Q190 0.578 0.351 0.364 !       0.53 eA-3
Q191 0.235 0.233 0.019 !       0.53 eA-3
Q192 0.308 0.587 0.027 !       0.52 eA-3
Q193 0.172 0.014 0.265 !       0.52 eA-3
Q194 0.335 0.131 0.323 !       0.52 eA-3
Q195 0.044 0.211 0.000 !       0.51 eA-3
Q196 0.133 0.789 0.360 !       0.51 eA-3
C197 0.860 0.042 0.064 !       0.51 eA-3
Q198 0.101 0.370 0.301 !       0.51 eA-3
Q199 0.578 0.603 0.192 !       0.51 eA-3
;
_refine_diff_density_max         1.886
_refine_diff_density_min         -1.585
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         13191
_refine_ls_number_restraints     46
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0785
_refine_ls_R_factor_gt           0.0750
_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^)+(0.0997P)^2^+31.8068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2077
_refine_ls_wR_factor_ref         0.2104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12107
_reflns_number_total             13191
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02621e2.cif
_cod_data_source_block           o-xylene@M_sq
_cod_database_code               1552200
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.889
_shelx_estimated_absorpt_t_min   0.840
_reflns_odcompleteness_completeness 99.89
_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
 C64-C65
 1.45 with sigma of 0.02
 O1-O3
 2.4 with sigma of 0.02
 O1-O2
 2.4 with sigma of 0.02
 O1-Cl1
 1.47 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C62 \\sim C63 \\sim C64 \\sim C65 \\sim C66 \\sim C67: within 1.7A with sigma
of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Others
 Fixed Sof: Cl1(0.6) Cl1A(0.4)
5.a Secondary CH2 refined with riding coordinates:
 C35(H35A,H35B), C44(H44A,H44B), C9(H9A,H9B), C18(H18A,H18B)
5.b Aromatic/amide H refined with riding coordinates:
 C27(H27), C28(H28), C29(H29), C30(H30), C33(H33), C34(H34), C38(H38),
 C39(H39), C40(H40), C42(H42), C45(H45), C46(H46), C49(H49), C50(H50), C51(H51),
  C52(H52), C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C12(H12), C13(H13),
 C14(H14), C15(H15), C19(H19), C20(H20), C23(H23), C24(H24), C25(H25), C26(H26),
  C55(H55), C56(H56), C57(H57), C58(H58), C63(H63), C64(H64), C65(H65), C66(H66)
5.c Idealised Me refined as rotating group:
 C53(H53A,H53B,H53C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C68(H68A,H68B,
 H68C)
;
_platon_squeeze_void_probe_radius 1.20
_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 1.375
_oxdiff_exptl_absorpt_empirical_full_min 0.767