Phenothiazine cyclic hexamers: synthesis, properties, and complexation behavior with C<sub>60</sub>.
Yamamoto, Koji; Tsutsui, Kanta; Tanuma, Miho; Ito, Kaname; Wakamatsu, Kan; Yamamoto, Koji; Nakamura, Yosuke; Chemical communications (Cambridge, England) 60 (2024) 2220–2223; doi:10.1039/d3cc06206f

data_7132661
_publ_section_title
;
 Phenothiazine cyclic hexamers: synthesis, properties, and complexation
 behavior with C<sub>60</sub>.
;
_journal_issue                   16
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              2220
_journal_page_last               2223
_journal_paper_doi               10.1039/d3cc06206f
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C126 H102 N6 S6'
_chemical_formula_sum            'C126 H102 N6 S6'
_chemical_formula_weight         1892.49
_space_group_crystal_system      cubic
_space_group_IT_number           206
_space_group_name_Hall           '-I 2b 2c 3'
_space_group_name_H-M_alt        'I a -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-12-17
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-12-15 deposited with the CCDC.	2024-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   33.0600(2)
_cell_length_b                   33.0600(2)
_cell_length_c                   33.0600(2)
_cell_measurement_reflns_used    65631
_cell_measurement_temperature    130.15
_cell_measurement_theta_max      27.1920
_cell_measurement_theta_min      2.5020
_cell_volume                     36133.4(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      130.15
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -103.00  77.00   0.25    5.00    --  -13.00  55.00 108.00  720
  2  \w     14.00  77.00   0.25    5.00    --  -13.00  55.00 -36.00  252
  3  \w    -71.00  35.00   0.25    5.00    --  -13.00  27.00-180.00  424
  4  \w      0.00  60.00   0.25    5.00    --  -13.00  55.00-108.00  240
  5  \w    -10.00  50.00   0.25    5.00    --  -13.00  55.00  36.00  240
  6  \w   -103.00  77.00   0.25    5.00    --  -13.00  55.00-180.00  720
  7  \w    -19.50  40.50   0.25    5.00    --  -13.00  27.00  36.00  240
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0105173000
_diffrn_orient_matrix_UB_12      0.0028435000
_diffrn_orient_matrix_UB_13      -0.0184903000
_diffrn_orient_matrix_UB_21      0.0090670000
_diffrn_orient_matrix_UB_22      -0.0193205000
_diffrn_orient_matrix_UB_23      0.0021977000
_diffrn_orient_matrix_UB_31      -0.0163658000
_diffrn_orient_matrix_UB_32      -0.0088706000
_diffrn_orient_matrix_UB_33      -0.0106538000
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            266714
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.346
_diffrn_reflns_theta_min         2.305
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69178
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear dark yellow'
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.696
_exptl_crystal_description       block
_exptl_crystal_F_000             7968
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.446
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         5514
_refine_ls_number_restraints     183
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0574
_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^)+(0.1245P)^2^+11.7322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.1938
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4293
_reflns_number_total             5514
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06206f2.cif
_cod_data_source_block           tnm_mesptz_6mer_chcl3_ea
_cod_depositor_comments          'Adding full bibliography for 7132661.cif.'
_cod_original_cell_volume        36133.4(7)
_cod_database_code               7132661
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C126H102N6S6
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.984
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_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
 C16-C15 \\sim C15-C14 \\sim C14-C13 \\sim C18-C13 \\sim C17-C18 \\sim C16-C17
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
N1 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18: within 1.7A
with sigma of 0.04 and sigma for terminal atoms of 0.08 within 1.7A
Uanis(C16) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C13)
\\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(C21) \\sim Ueq, Uanis(C20) \\sim Ueq: with sigma of 0.05 and sigma for
terminal atoms of 0.05
4. Rigid body (RIGU) restrains
 C19, C14
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C16, C20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C21, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C19, C14, C13, C21, C18, C17, C16, C15, C20, N1
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Aromatic/amide H refined with riding coordinates:
 C6(H6), C3(H3), C4(H4), C10(H10), C12(H12), C9(H9), C17(H17), C15(H15)
5.b Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_smtbx_masks_special_details
;

The asymmetric unit cell contains 3 ethyl acetate molecules which have been treated
as a diffuse contribution to the overall scattering without specific atom positions
by Solvent Mask program in Olex2.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              35732
_shelx_hkl_checksum              98863
_shelx_fab_checksum              53624
_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 1.404
_oxdiff_exptl_absorpt_empirical_full_min 0.787