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_1565275
_publ_section_title
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 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         'C36 H22 N2 O S2, 1(C7 H8)'
_chemical_formula_sum            'C43 H30 N2 O S2'
_chemical_formula_weight         654.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc261rvw
_audit_creation_date             2020-07-27
_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                 107.502(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   28.6573(6)
_cell_length_b                   6.76310(10)
_cell_length_c                   36.8149(7)
_cell_measurement_reflns_used    11949
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.0340
_cell_measurement_theta_min      3.7640
_cell_volume                     6804.9(2)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -108.00 -15.00   1.00   18.97    --  -40.87 -57.00-180.00   93
  2  \w   -111.00 -85.00   1.00   18.97    --  -40.87-137.00 -14.00   26
  3  \w    -65.00  32.00   1.00   18.97    --  -40.87  37.00  90.00   97
  4  \w   -111.00 -18.00   1.00   18.97    --  -40.87 -37.00 -90.00   93
  5  \w     49.00  85.00   1.00   18.97    --   40.87-137.00 -14.00   36
  6  \w     33.00  89.00   1.00   18.97    --   40.87-132.00 162.00   56
  7  \w     56.00 100.00   1.00   75.86    --  105.32 -94.00 150.00   44
  8  \w     25.00  94.00   1.00   75.86    --  105.32 -94.00  60.00   69
  9  \w    106.00 171.00   1.00   75.86    --  105.32  77.00-150.00   65
 10  \w     38.00 119.00   1.00   75.86    --  105.32 -45.00  60.00   81
 11  \w    109.00 134.00   1.00   75.86    --  105.32 -61.00 -90.00   25
 12  \w     36.00 123.00   1.00   75.86    --  105.32 -45.00 150.00   87
 13  \w     69.00 117.00   1.00   75.86    --  105.32-125.00 -90.00   48
 14  \w     40.00 131.00   1.00   75.86    --  105.32 -45.00-120.00   91
 15  \w     59.00 109.00   1.00   75.86    --  105.32 -94.00   0.00   50
 16  \w     60.00 109.00   1.00   75.86    --  105.32 -94.00 -90.00   49
 17  \w     89.00 115.00   1.00   75.86    --  105.32-125.00-180.00   26
 18  \w     18.00 169.00   1.00   75.86    --  105.32   0.00  30.00  151
;
_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      0.0297954000
_diffrn_orient_matrix_UB_12      0.0338297000
_diffrn_orient_matrix_UB_13      0.0419543000
_diffrn_orient_matrix_UB_21      -0.0410046000
_diffrn_orient_matrix_UB_22      -0.0977365000
_diffrn_orient_matrix_UB_23      0.0128361000
_diffrn_orient_matrix_UB_31      0.0247207000
_diffrn_orient_matrix_UB_32      -0.2028073000
_diffrn_orient_matrix_UB_33      0.0008253000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0176
_diffrn_reflns_av_unetI/netI     0.0132
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            21698
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.075
_diffrn_reflns_theta_max         67.075
_diffrn_reflns_theta_min         3.450
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.702
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71320
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       prism
_exptl_crystal_F_000             2736
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6059
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0489
_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^)+(0.0683P)^2^+5.5677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1397
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5348
_reflns_number_total             6059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1mh01360b2.cif
_cod_data_source_block           dptz-dbf-tol-20200721
_cod_database_code               1565275
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H O N S '
_shelx_estimated_absorpt_t_max   0.876
_shelx_estimated_absorpt_t_min   0.784
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C42-C43
 1.53 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C39A) \\sim Ueq, Uanis(C38A) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C43A)
\\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C41) \\sim Ueq, Uanis(C41A) \\sim Ueq,
Uanis(C40A) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C43) = Uanis(C43A)
Uanis(C42) = Uanis(C42A)
Uanis(C41) = Uanis(C41A)
Uanis(C40) = Uanis(C40A)
Uanis(C39) = Uanis(C39A)
Uanis(C38) = Uanis(C38A)
Uanis(C37) = Uanis(C37A)
4. Others
 Sof(C37A)=Sof(H37A)=Sof(C38A)=Sof(H38A)=Sof(C42A)=Sof(C41A)=Sof(H41A)=
 Sof(C40A)=Sof(H40A)=Sof(C39A)=Sof(H39A)=Sof(C43A)=Sof(H43A)=Sof(H43B)=
 Sof(H43C)=1-FVAR(1)
 Sof(C42)=Sof(C37)=Sof(H37)=Sof(C38)=Sof(H38)=Sof(C39)=Sof(H39)=Sof(C40)=
 Sof(H40)=Sof(C41)=Sof(H41)=Sof(C43)=Sof(H43D)=Sof(H43E)=Sof(H43F)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C4(H4), C9(H9), C10(H10), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C26(H26),
  C27(H27), C28(H28), C33(H33), C34(H34), C35(H35), C36(H36), C37A(H37A),
 C38A(H38A), C41A(H41A), C40A(H40A), C39A(H39A), C37(H37), C38(H38), C39(H39),
 C40(H40), C41(H41)
5.b Fitted hexagon refined as free rotating group:
 C37A(C38A,C42A,C41A,C40A,C39A), C42(C37,C38,C39,C40,C41)
5.c Idealised Me refined as rotating group:
 C43(H43D,H43E,H43F), C43A(H43A,H43B,H43C)
;
_shelx_res_checksum              24068
_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 1.367
_oxdiff_exptl_absorpt_empirical_full_min 0.633