Synthesis and properties of an <i>O</i>-doped aromatic belt.
Han, Ying; Guo, Wei-Chen; Du, Xu-Sheng; Chen, Chuan-Feng; Chemical communications (Cambridge, England) 60 (2024) 5719–5722; doi:10.1039/d4cc01667j

data_7133009
_publ_section_title
;
 Synthesis and properties of an <i>O</i>-doped aromatic belt.
;
_journal_issue                   44
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              5719
_journal_page_last               5722
_journal_paper_doi               10.1039/d4cc01667j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C45 H36 O9'
_chemical_formula_sum            'C45 H36 O9'
_chemical_formula_weight         720.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           57
_space_group_name_Hall           '-P 2c 2b'
_space_group_name_H-M_alt        'P b c m'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-07-05 deposited with the CCDC.	2024-05-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.1779(3)
_cell_length_b                   7.77835(17)
_cell_length_c                   27.1947(7)
_cell_measurement_reflns_used    6535
_cell_measurement_temperature    169.99(10)
_cell_measurement_theta_max      75.1700
_cell_measurement_theta_min      2.7210
_cell_volume                     3422.11(13)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      169.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.979
_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     34.00  78.00   0.50    1.70    --  103.25 -94.00 -60.00   88
  2  \w     35.00  85.00   0.50    1.70    --  103.25 -69.00  -4.00  100
  3  \w     40.00  66.00   0.50    1.70    --  103.25 -61.00  30.00   52
  4  \w     33.00  60.00   0.50    1.70    --  103.25 -51.00 170.00   54
  5  \w     92.00 178.00   0.50    1.70    --  103.25  30.00   0.00  172
  6  \w     72.00 112.00   0.50    0.42    --   46.95 137.00   4.00   80
  7  \w   -165.00-112.00   0.50    1.70    -- -104.50 -30.00  90.00  106
  8  \w   -173.00-135.00   0.50    1.70    -- -104.50 -51.00 170.00   76
  9  \w   -144.00 -97.00   0.50    1.70    -- -104.50-132.00 118.00   94
 10  \w   -117.00 -74.00   0.50    0.42    --  -46.95-137.00 -59.00   86
 11  \w   -107.00 -81.00   0.50    0.42    --  -46.95-125.00-150.00   52
 12  \w    -11.00  27.00   0.50    0.42    --  -46.95  19.00 -60.00   76
 13  \w    -23.00  28.00   0.50    0.42    --  -46.95  19.00-150.00  102
 14  \w    -68.00 -43.00   0.50    1.70    -- -104.50  61.00-150.00   50
 15  \w    -62.00 -33.00   0.50    1.70    -- -104.50  61.00  60.00   58
 16  \w    -68.00 -43.00   0.50    1.70    -- -104.50  61.00  90.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0354262000
_diffrn_orient_matrix_UB_12      0.0536607000
_diffrn_orient_matrix_UB_13      0.0502918000
_diffrn_orient_matrix_UB_21      0.0662651000
_diffrn_orient_matrix_UB_22      0.1091092000
_diffrn_orient_matrix_UB_23      -0.0260324000
_diffrn_orient_matrix_UB_31      -0.0585169000
_diffrn_orient_matrix_UB_32      0.1563609000
_diffrn_orient_matrix_UB_33      0.0009387000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0636
_diffrn_reflns_av_unetI/netI     0.0584
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            13451
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.317
_diffrn_reflns_theta_min         2.731
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'PhotonJet R (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.795
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    1.399
_exptl_crystal_description       cube
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       0.00052(13)
_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   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0557P)^2^+1.0956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1158
_refine_ls_wR_factor_ref         0.1194
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3156
_reflns_number_total             3546
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc01667j2.cif
_cod_data_source_block           tx12270_auto
_cod_depositor_comments
'Adding full bibliography for 7133009--7133010.cif.'
_cod_original_cell_volume        3422.12(13)
_cod_database_code               7133009
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O S'
_chemical_oxdiff_usercomment     'C H N O S'
_diffrn_oxdiff_digest_frames
;
01c7e923695be6c0b6054cdedd8d2f694400028e6ca
;
_diffrn_oxdiff_digest_hkl
;
01ce527c72f1a66a3cde1149d7f950c34ad15e
;
_reflns_odcompleteness_completeness 99.86
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_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:
 C28(H28A,H28B), C14(H14A,H14B)
2.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C18(H18), C16(H16), C7(H7), C13(H13), C10(H10)
2.c Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              71058
_shelx_hkl_checksum              19181
_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 3.903
_oxdiff_exptl_absorpt_empirical_full_min 0.248