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_1552198
_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), C4'
_chemical_formula_sum            'C72 H60 Ag2 Cl2 N16 O8'
_chemical_formula_weight         1564.00
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_block_doi                 10.5517/ccdc.csd.cc21f5ym
_audit_creation_date             2019-05-07
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-15 deposited with the CCDC.    2019-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9420(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.20450(10)
_cell_length_b                   23.0696(2)
_cell_length_c                   20.6652(2)
_cell_measurement_reflns_used    20371
_cell_measurement_temperature    169(6)
_cell_measurement_theta_max      73.1650
_cell_measurement_theta_min      3.6990
_cell_volume                     6706.87(10)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169(6)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.971
_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     63.00  89.00   0.50    0.50    --    0.00  57.00-120.00   52
  2  \w    -29.00  85.00   0.50    0.50    --    0.00  57.00 -60.00  228
  3  \w     34.00  82.00   0.50    0.50    --    0.00  77.00-180.00   96
  4  \w    -22.00   4.00   0.50    0.50    --    0.00  77.00-180.00   52
  5  \w    -23.00   3.00   0.50    0.50    --    0.00  57.00-120.00   52
  6  \w     92.00 118.00   0.50    0.95    --   98.20 -82.00-120.00   52
  7  \w      9.00  45.00   0.50    0.95    --   98.20 -82.00-120.00   72
  8  \w      9.00 137.00   0.50    0.95    --   98.20 -82.00  90.00  256
  9  \w     40.00  70.00   0.50    0.95    --   98.20 -82.00  30.00   60
 10  \w     68.00 132.00   0.50    0.95    --   98.20  61.00 -90.00  128
 11  \w     82.00 136.00   0.50    0.95    --   98.20 -82.00  30.00  108
 12  \w    163.00 188.00   0.50    0.95    --   98.20  30.00-150.00   50
 13  \w     61.00 102.00   0.50    0.95    --   98.20 -82.00-180.00   82
 14  \w     83.00 188.00   0.50    0.95    --   98.20  61.00 120.00  210
 15  \w     68.00 177.00   0.50    0.95    --   98.20  61.00-180.00  218
 16  \w     50.00 112.00   0.50    0.95    --   98.20 -61.00 150.00  124
;
_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      0.0300180000
_diffrn_orient_matrix_UB_12      0.0640182000
_diffrn_orient_matrix_UB_13      0.0082660000
_diffrn_orient_matrix_UB_21      0.1020038000
_diffrn_orient_matrix_UB_22      -0.0189307000
_diffrn_orient_matrix_UB_23      0.0266114000
_diffrn_orient_matrix_UB_31      0.0261197000
_diffrn_orient_matrix_UB_32      0.0003949000
_diffrn_orient_matrix_UB_33      -0.0699523000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0214
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            40500
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.402
_diffrn_reflns_theta_min         3.680
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.999
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.397
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     936
_refine_ls_number_reflns         13112
_refine_ls_number_restraints     155
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0703P)^2^+12.8583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11713
_reflns_number_total             13112
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02621e2.cif
_cod_data_source_block           p-xylene@M
_cod_database_code               1552198
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.841
_shelx_estimated_absorpt_t_min   0.754
_reflns_odcompleteness_completeness 99.33
_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
 C4-C6A
 2.2 with sigma of 0.02
 C3-C7A
 2.3 with sigma of 0.02
 C6-C4
 2.3 with sigma of 0.02
 C4A-C5
 1.2 with sigma of 0.02
 C11-C9
 2.4 with sigma of 0.02
 C14_$1-C13_$1
 1.25 with sigma of 0.02
 C11-C15_$1
 1.25 with sigma of 0.02
 C15_$1-C14_$1
 1.25 with sigma of 0.02
 C15_$1-C12
 2.75 with sigma of 0.02
 C14-C12
 2.3 with sigma of 0.02
 C15-C13
 2.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6A \\sim C7A: within 1.7A with sigma of
0.001 and sigma for terminal atoms of 0.002
C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 1.7A
with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.0001 and sigma for
terminal atoms of 0.0002
Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C12) \\sim Ueq:
with sigma of 0.0001 and sigma for terminal atoms of 0.0002
4. Others
 Fixed Sof: C3(0.5) H3(0.5) C3A(0.5) H3A(0.5) C4A(0.5) H4A(0.5) C6(0.5)
 H6(0.5) C7(0.5) H7(0.5) C4(0.5) H4(0.5) C6A(0.5) H6A(0.5) C7A(0.5) H7A(0.5)
 C9(0.5) C10(0.5) C11(0.5) C12(0.5) C14(0.5) C15(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C41(H41A,H41B), C58(H58A,H58B), C67(H67A,H67B)
5.b Aromatic/amide H refined with riding coordinates:
 C24(H24), C25(H25), C26(H26), C27(H27), C30(H30), C31(H31), C35(H35),
 C36(H36), C37(H37), C38(H38), C42(H42), C43(H43), C46(H46), C47(H47), C48(H48),
  C49(H49), C50(H50), C51(H51), C52(H52), C53(H53), C56(H56), C57(H57),
 C61(H61), C62(H62), C63(H63), C64(H64), C68(H68), C69(H69), C72(H72), C73(H73),
  C74(H74), C75(H75), C3(H3), C3A(H3A), C4A(H4A), C6(H6), C7(H7), C4(H4),
 C6A(H6A), C7A(H7A), C18(H18), C19(H19), C20(H20), C21(H21)
5.c Fitted hexagon refined as free rotating group:
 C3A(C4A,C5,C6,C7,C2)
5.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C), C23(H23A,H23B,H23C)
;
_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 1.200
_oxdiff_exptl_absorpt_empirical_full_min 0.880