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_1565274
_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         '2(C18 H11 N S1.5)'
_chemical_formula_sum            'C36 H22 N2 S3'
_chemical_formula_weight         578.73
_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.cc261rtv
_audit_creation_date             2020-06-12
_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                   28.6595(5)
_cell_length_b                   8.9864(2)
_cell_length_c                   13.6296(2)
_cell_measurement_reflns_used    5286
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      72.7710
_cell_measurement_theta_min      4.9050
_cell_volume                     3510.25(11)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -62.00  32.00   1.00   26.10    --  -41.12  37.00 -90.00   94
  2  \w     21.00  77.00   1.00   26.10    --   41.12  37.00  30.00   56
  3  \w     24.00  75.00   1.00   26.10    --   41.12  57.00 -60.00   51
  4  \w    143.00 169.00   1.00  104.40    --  105.32  61.00 -90.00   26
  5  \w     76.00 177.00   1.00  104.40    --  105.32  61.00  90.00  101
  6  \w    119.00 175.00   1.00  104.40    --  105.32  61.00 -30.00   56
  7  \w     24.00  84.00   1.00  104.40    --  105.32 -94.00 -90.00   60
  8  \w    132.00 171.00   1.00  104.40    --  105.32 125.00 -30.00   39
  9  \w     77.00 104.00   1.00  104.40    --  105.32  61.00 -30.00   27
 10  \w     83.00 108.00   1.00  104.40    --  105.32  45.00   0.00   25
 11  \w    131.00 175.00   1.00  104.40    --  105.32  45.00   0.00   44
 12  \w    107.00 138.00   1.00  104.40    --  105.32  61.00 -90.00   31
;
_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      -0.0720380000
_diffrn_orient_matrix_UB_12      -0.0142761000
_diffrn_orient_matrix_UB_13      -0.1240452000
_diffrn_orient_matrix_UB_21      0.0363948000
_diffrn_orient_matrix_UB_22      -0.0507639000
_diffrn_orient_matrix_UB_23      0.0108431000
_diffrn_orient_matrix_UB_31      -0.0791956000
_diffrn_orient_matrix_UB_32      -0.0103583000
_diffrn_orient_matrix_UB_33      0.1177958000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12006
_diffrn_reflns_point_group_measured_fraction_full 0.926
_diffrn_reflns_point_group_measured_fraction_max 0.926
_diffrn_reflns_theta_full        67.053
_diffrn_reflns_theta_max         67.053
_diffrn_reflns_theta_min         4.629
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76613
_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    1.095
_exptl_crystal_description       block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.243
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
;
 Flack x determined using 1987 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.080(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5935
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0570
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+1.4403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1593
_refine_ls_wR_factor_ref         0.1656
_reflns_Friedel_coverage         0.767
_reflns_Friedel_fraction_full    0.845
_reflns_Friedel_fraction_max     0.845
_reflns_number_gt                5269
_reflns_number_total             5935
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1mh01360b2.cif
_cod_data_source_block           ty-dbt-pe-2-20200610
_cod_original_cell_volume        3510.24(11)
_cod_database_code               1565274
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C36 H22 N2 S3'
_shelx_estimated_absorpt_t_max   0.817
_shelx_estimated_absorpt_t_min   0.643
_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.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C17(H17), C18(H18), C1'(H1'), C2'(H2'), C3'(H3'), C4'(H4'), C9'(H9'),
  C10'(H10'), C11'(H11'), C12'(H12'), C14'(H14'), C15'(H15'), C18'(H18')
;
_shelx_res_checksum              93763
_shelx_fab_checksum              50691
_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 0.748