Organic Microporous Crystals Driven by Pure C-H‧‧‧π Interactions with Vapors-Induced Crystal-to-Crystal Transformations
Tian, Yu; Yang, Jie; Gao, Mingxue; Liu, Zhenjiang; Zhao, M.; Fang, Manman; Li, Zhen; Materials Horizons  (2021) –; doi:10.1039/D1MH01360B

data_1565276
_publ_section_title
;
 Organic Microporous Crystals Driven by Pure C-H&#x2027;&#x2027;&#x2027;\p
 Interactions with Vapors-Induced Crystal-to-Crystal Transformations
;
_journal_name_full               'Materials Horizons'
_journal_paper_doi               10.1039/D1MH01360B
_journal_year                    2021
_chemical_formula_moiety         '2(C18 H11 N O0.5 S)'
_chemical_formula_sum            'C36 H22 N2 O S2'
_chemical_formula_weight         562.67
_space_group_crystal_system      orthorhombic
_space_group_IT_number           26
_space_group_name_Hall           'P 2c -2'
_space_group_name_H-M_alt        'P m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc261rxy
_audit_creation_date             2020-05-08
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-09-05 deposited with the CCDC.	2021-11-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.9077(2)
_cell_length_b                   9.23090(10)
_cell_length_c                   12.76950(10)
_cell_measurement_reflns_used    28606
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.7860
_cell_measurement_theta_min      4.5340
_cell_volume                     3525.34(5)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1975
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -110.00 -13.00   1.00    4.45    --  -41.12 -57.00-120.00   97
  2  \w   -107.00 -17.00   1.00    4.45    --  -41.12 -37.00  60.00   90
  3  \w   -115.00 -18.00   1.00    4.45    --  -41.12 -37.00 -60.00   97
  4  \w    -68.00  32.00   1.00    4.45    --  -41.12  57.00  30.00  100
  5  \w     23.00  91.00   1.00    4.45    --   41.12-125.00 -30.00   68
  6  \w     58.00  85.00   1.00    4.45    --   41.12  77.00  60.00   27
  7  \w      2.00  80.00   1.00    4.45    --   41.12 -99.00 120.00   78
  8  \w      9.00  36.00   1.00    4.45    --   41.12  77.00  60.00   27
  9  \w      6.00  32.00   1.00    4.45    --   42.00  88.00 157.77   26
 10  \w     11.00  36.00   1.00    4.45    --   46.00  84.00  -3.40   25
 11  \w     11.00  36.00   1.00    4.45    --   46.00  84.00 129.46   25
 12  \w     11.00  36.00   1.00    4.45    --   46.00  84.00-128.15   25
 13  \w     18.00  45.00   1.00    4.45    --   50.00  82.00  77.53   27
 14  \w     25.00  51.00   1.00    4.45    --   58.00  77.00 -43.48   26
 15  \w     26.00  51.00   1.00    4.45    --   58.00  77.00  -5.91   25
 16  \w     85.00 132.00   1.00    4.45    --   58.00  77.00  -5.91   47
 17  \w     30.00  55.00   1.00    4.45    --   62.00  74.00  21.63   25
 18  \w     30.00  64.00   1.00    4.45    --   62.00  75.00  40.11   34
 19  \w     29.00  56.00   1.00    4.45    --   62.00  77.00 -91.09   27
 20  \w     30.00  56.00   1.00    4.45    --   62.00  75.00-113.50   26
 21  \w    111.00 137.00   1.00    4.45    --   62.00  74.00  21.63   26
 22  \w     89.00 115.00   1.00    4.45    --   62.00  77.00 -91.09   26
 23  \w    110.00 139.00   1.00    4.45    --   66.00  77.00  75.45   29
 24  \w     33.00  76.00   1.00    4.45    --   66.00  77.00 178.74   43
 25  \w     35.00  62.00   1.00    4.45    --   66.00  76.00 100.14   27
 26  \w     33.00  58.00   1.00    4.45    --   66.00  77.00  75.45   25
 27  \w     37.00  79.00   1.00    4.45    --   66.00  62.00 -18.62   42
 28  \w     35.00  65.00   1.00    4.45    --   66.00  75.00-155.19   30
 29  \w     38.00  87.00   1.00    4.45    --   70.00  76.00 133.41   49
 30  \w     50.00  82.00   1.00   17.78    --   82.00  74.00  98.26   32
 31  \w     73.00 100.00   1.00   17.78    --  105.32  77.00-120.00   27
 32  \w     38.00 137.00   1.00   17.78    --  105.32 -77.00  30.00   99
 33  \w     73.00 166.00   1.00   17.78    --  105.32  77.00  30.00   93
 34  \w    121.00 163.00   1.00   17.78    --  105.32  77.00 -30.00   42
 35  \w     23.00 109.00   1.00   17.78    --  105.32 -94.00-120.00   86
 36  \w     73.00  99.00   1.00   17.78    --  105.32  77.00 -30.00   26
 37  \w     76.00 103.00   1.00   17.78    --  105.32  61.00  30.00   27
 38  \w     77.00 102.00   1.00   17.78    --  105.32  61.00-150.00   25
 39  \w     76.00 135.00   1.00   17.78    --  105.32  61.00   0.00   59
 40  \w     76.00 160.00   1.00   17.78    --  105.32  61.00  90.00   84
 41  \w    112.00 173.00   1.00   17.78    --  105.32  77.00-150.00   61
 42  \w     78.00 107.00   1.00   17.78    --  105.32  61.00-120.00   29
 43  \w     73.00  99.00   1.00   17.78    --  105.32  77.00-150.00   26
 44  \w    125.00 150.00   1.00   17.78    --  105.32  61.00  60.00   25
 45  \w     76.00 103.00   1.00   17.78    --  105.32  61.00  60.00   27
 46  \w     73.00 150.00   1.00   17.78    --  105.32  77.00 120.00   77
 47  \w     73.00 169.00   1.00   17.78    --  105.32  77.00 150.00   96
 48  \w     73.00 178.00   1.00   17.78    --  105.32  77.00 -60.00  105
 49  \w    107.00 159.00   1.00   17.78    --  105.32  77.00-180.00   52
 50  \w     63.00 117.00   1.00   17.78    --  105.32-125.00  30.00   54
 51  \w     73.00  99.00   1.00   17.78    --  105.32  77.00-180.00   26
 52  \w     73.00 143.00   1.00   17.78    --  105.32  77.00   0.00   70
 53  \w     73.00 167.00   1.00   17.78    --  105.32  77.00 -90.00   94
 54  \w     76.00 102.00   1.00   17.78    --  105.32  61.00 120.00   26
 55  \w     76.00 112.00   1.00   17.78    --  105.32  61.00 -90.00   36
 56  \w    116.00 171.00   1.00   17.78    --  105.32  77.00-120.00   55
 57  \w    140.00 172.00   1.00   17.78    --  105.32 125.00 -60.00   32
 58  \w     91.00 117.00   1.00   17.78    --  105.32-125.00-180.00   26
 59  \w     33.00 114.00   1.00   17.78    --  105.32 -45.00-120.00   81
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0035665000
_diffrn_orient_matrix_UB_12      -0.0472009000
_diffrn_orient_matrix_UB_13      0.0667046000
_diffrn_orient_matrix_UB_21      -0.0095790000
_diffrn_orient_matrix_UB_22      -0.0206456000
_diffrn_orient_matrix_UB_23      -0.1524547000
_diffrn_orient_matrix_UB_31      0.1201057000
_diffrn_orient_matrix_UB_32      -0.0002432000
_diffrn_orient_matrix_UB_33      -0.0141257000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0103
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            57365
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.074
_diffrn_reflns_theta_max         67.074
_diffrn_reflns_theta_min         4.435
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.570
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50435
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.060
_exptl_crystal_description       prism
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.095
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.035
_refine_ls_abs_structure_details
;
 Flack x determined using 2364 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.008(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         6210
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0312
_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^)+(0.0567P)^2^+0.1171P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0883
_refine_ls_wR_factor_ref         0.0915
_reflns_Friedel_coverage         0.845
_reflns_Friedel_fraction_full    0.935
_reflns_Friedel_fraction_max     0.935
_reflns_number_gt                5596
_reflns_number_total             6210
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1mh01360b2.cif
_cod_data_source_block           ty-ml-6-0520
_cod_database_code               1565276
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C36 H22 O1 N2 S2'
_shelx_estimated_absorpt_t_max   0.885
_shelx_estimated_absorpt_t_min   0.810
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(S1') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16),
 C17(H17), C18(H18), C2'(H2'), C4'(H4'), C5'(H5'), C7'(H7'), C8'(H8'), C9'(H9'),
  C10'(H10'), C15'(H15'), C16'(H16'), C17'(H17'), C18'(H18')
;
_shelx_res_checksum              80873
_shelx_fab_checksum              66093
_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 2.043
_oxdiff_exptl_absorpt_empirical_full_min 0.580