A Self-assembled M2L2 Truncated Square and its Application as a Container for Fullerenes
Yuan, Jun; Lv, Wanqian; Li, Anquan; Zhu, Kelong; Chemical Communications  (2021) –; doi:10.1039/D1CC05581J

data_7129205
_publ_section_title
;
 A Self-assembled M2L2 Truncated Square and its Application as a Container
 for Fullerenes
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D1CC05581J
_journal_year                    2021
_chemical_formula_moiety         '2(C17 H14 N S2)'
_chemical_formula_sum            'C34 H28 N2 S4'
_chemical_formula_weight         592.82
_chemical_name_systematic
4,4'-(4,11-dipropylbenzo[5,6][1,4]dithiino[2,3-b]thianthrene-2,9-diyl)dipyridine
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-10-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-10-01 deposited with the CCDC.	2021-11-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3680(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.02800(10)
_cell_length_b                   10.8723(2)
_cell_length_c                   37.5335(5)
_cell_measurement_reflns_used    7491
_cell_measurement_temperature    223.00(10)
_cell_measurement_theta_max      75.9930
_cell_measurement_theta_min      4.7060
_cell_volume                     3266.51(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (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    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      223.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2913
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.976
_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    -66.00  33.00   1.00    7.50    --  -41.14  38.00  60.00   99
  2  \w    -35.00  71.00   1.00    7.50    --   41.14 -77.00-150.00  106
  3  \w     79.00 175.00   1.00   40.00    --  112.00  77.00 -90.00   96
  4  \w     45.00 145.00   1.00   40.00    --  112.00 -77.00-180.00  100
  5  \w    122.00 178.00   1.00   40.00    --  112.00 111.00  90.00   56
  6  \w     74.00 139.00   1.00   40.00    --  112.00 -30.00 120.00   65
  7  \w     88.00 152.00   1.00   40.00    --  112.00  30.00 150.00   64
  8  \w    126.00 151.00   1.00   40.00    --  112.00 178.00-180.00   25
  9  \w     37.00 110.00   1.00   40.00    --  112.00-107.00-165.00   73
 10  \w     57.00 115.00   1.00   40.00    --  112.00 178.00-180.00   58
;
_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      -0.0168549000
_diffrn_orient_matrix_UB_12      0.0621168000
_diffrn_orient_matrix_UB_13      0.0364483000
_diffrn_orient_matrix_UB_21      0.0593775000
_diffrn_orient_matrix_UB_22      0.1226661000
_diffrn_orient_matrix_UB_23      -0.0152032000
_diffrn_orient_matrix_UB_31      -0.1822703000
_diffrn_orient_matrix_UB_32      0.0342131000
_diffrn_orient_matrix_UB_33      -0.0116361000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            13909
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.008
_diffrn_reflns_theta_min         4.726
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62766
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.205
_exptl_crystal_description       plate
_exptl_crystal_F_000             1240
_exptl_crystal_preparation
'diffusion of hexane into tetrahydrofuran solution'
_exptl_crystal_recrystallization_method
'diffusion of hexane into tetrahydrofuran solution'
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         6639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0526
_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^)+(0.1259P)^2^+0.8110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1681
_refine_ls_wR_factor_ref         0.1738
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5892
_reflns_number_total             6639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cc05581j2.cif
_cod_data_source_block           a20042705a0267
_cod_database_code               7129205
_shelx_shelxl_version_number     2018/1
_chemical_oxdiff_formula         C44H32N2S4
_chemical_oxdiff_usercomment     BINJIPEITI
_reflns_odcompleteness_completeness 98.72
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     74.33
_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.a Secondary CH2 refined with riding coordinates:
 C00O(H00F,H00H), C00U(H00A,H00C), C00X(H00I,H00J), C012(H01A,H01B)
2.b Aromatic/amide H refined with riding coordinates:
 C00A(H00D), C00B(H00B), C00E(H00E), C00G(H00G), C00K(H00K), C00Q(H00Q),
 C00R(H00R), C00T(H00T), C00V(H00V), C00W(H00W), C00Y(H00Y), C00Z(H00Z),
 C010(H010), C011(H011)
2.c Idealised Me refined as rotating group:
 C013(H01F,H01G,H01H), C014(H01C,H01D,H01E)
;
_olex2_submission_original_sample_id L1
_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 1.461
_oxdiff_exptl_absorpt_empirical_full_min 0.548