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_1565273
_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         'C Cl2, 2(C36 H22 N2 O S2)'
_chemical_formula_sum            'C73 H46 Cl2 N4 O2 S4'
_chemical_formula_weight         1210.28
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc261rwx
_audit_creation_date             2020-04-25
_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                 103.7910(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3600(2)
_cell_length_b                   14.8334(2)
_cell_length_c                   14.02980(10)
_cell_measurement_reflns_used    12696
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.0670
_cell_measurement_theta_min      4.3480
_cell_volume                     2902.30(6)
_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    -30.00  32.00   1.00    4.07    --  -41.12  57.00  30.00   62
  2  \w    -82.00  36.00   1.00    4.07    --  -41.12  19.00   0.00  118
  3  \w    -89.00  -6.00   1.00    4.07    --  -41.12 125.00  60.00   83
  4  \w     47.00  83.00   1.00    4.07    --   41.12-122.00 -38.00   36
  5  \w     21.00  92.00   1.00    4.07    --   41.12  37.00  30.00   71
  6  \w    101.00 173.00   1.00   16.27    --  105.32 125.00  60.00   72
  7  \w     58.00 178.00   1.00   16.27    --  105.32  15.00 150.00  120
  8  \w     33.00  59.00   1.00   16.27    --  105.32 -30.00 -90.00   26
  9  \w    127.00 173.00   1.00   16.27    --  105.32 125.00 -60.00   46
 10  \w     24.00  88.00   1.00   16.27    --  105.32 -94.00-150.00   64
 11  \w     95.00 123.00   1.00   16.27    --  105.32 125.00 -60.00   28
 12  \w     33.00  98.00   1.00   16.27    --  105.32 -94.00  60.00   65
 13  \w    125.00 176.00   1.00   16.27    --  105.32 125.00   0.00   51
 14  \w     69.00 115.00   1.00   16.27    --  105.32-125.00-180.00   46
 15  \w     64.00 114.00   1.00   16.27    --  105.32-122.00 -38.00   50
 16  \w     77.00 126.00   1.00   16.27    --  105.32 -30.00 -90.00   49
 17  \w     34.00 117.00   1.00   16.27    --  105.32 -45.00  30.00   83
 18  \w     82.00 178.00   1.00   16.27    --  105.32  45.00 -60.00   96
 19  \w     29.00  97.00   1.00   16.27    --  105.32 -94.00   0.00   68
;
_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      0.0036870000
_diffrn_orient_matrix_UB_12      0.1031953000
_diffrn_orient_matrix_UB_13      0.0127848000
_diffrn_orient_matrix_UB_21      -0.1103788000
_diffrn_orient_matrix_UB_22      0.0032495000
_diffrn_orient_matrix_UB_23      -0.0248434000
_diffrn_orient_matrix_UB_31      0.0016929000
_diffrn_orient_matrix_UB_32      -0.0113375000
_diffrn_orient_matrix_UB_33      0.1095575000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_unetI/netI     0.0248
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            20229
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.047
_diffrn_reflns_theta_max         67.047
_diffrn_reflns_theta_min         4.351
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.18615
_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            gray
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       prism
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.560
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.0096(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         5182
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0576
_refine_ls_R_factor_gt           0.0538
_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^)+(0.0804P)^2^+1.5001P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1495
_refine_ls_wR_factor_ref         0.1540
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4674
_reflns_number_total             5182
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1mh01360b2.cif
_cod_data_source_block           ty-ml-yelow-20190517
_cod_database_code               1565273
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C36 H22 O1 N2 S2'
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.681
_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
2. Restrained distances
 Cl1-C37
 1.76 with sigma of 0.02
3. Others
 Fixed Sof: C37(0.5)
4.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)
;
_shelx_res_checksum              29285
_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 3.508
_oxdiff_exptl_absorpt_empirical_full_min 0.468