Synthesis of Zigzag- and Fjord-Edged Nanographene with Dual Amplified Spontaneous Emission
Xu, Xiushang; Serra, Gianluca; Villa, Andrea; Muñoz-Mármol, Rafael; Vasylevskyi, Serhii; Gadea, Marcos; Lucotti, Andrea; Lin, Zesen; Boj, Pedro G.; Kabe, Ryota; Tommasini, Matteo; Diaz-Garcia, Maria Angeles; Scotognella, Francesco; Paternò, Giuseppe Maria; Narita, Akimitsu; Chemical Science  (2022) –; doi:10.1039/D2SC04208H

data_1567797
_publ_section_title
;
 Synthesis of Zigzag- and Fjord-Edged Nanographene with Dual Amplified
 Spontaneous Emission
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC04208H
_journal_year                    2022
_chemical_formula_moiety         'C72 H58, 0.5(C6 H6)'
_chemical_formula_sum            'C75 H61'
_chemical_formula_weight         962.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-08
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-04-18 deposited with the CCDC.	2022-10-17 downloaded from the CCDC.
;
_cell_angle_alpha                114.665(5)
_cell_angle_beta                 95.802(3)
_cell_angle_gamma                90.221(3)
_cell_formula_units_Z            4
_cell_length_a                   18.1166(5)
_cell_length_b                   19.1083(9)
_cell_length_c                   19.7848(10)
_cell_measurement_reflns_used    12203
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      30.9720
_cell_measurement_theta_min      2.0860
_cell_volume                     6184.2(5)
_computing_cell_refinement       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.115a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -339.92  20.48   1.70   34.00  19.67  -0.86 -59.25    --   212
  2  \w    -63.36 -19.16   1.70   34.00    --  -22.05  94.56   1.16   26
;
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0045697000
_diffrn_orient_matrix_UB_12      0.0172650000
_diffrn_orient_matrix_UB_13      -0.0255884000
_diffrn_orient_matrix_UB_21      0.0050733000
_diffrn_orient_matrix_UB_22      0.0370707000
_diffrn_orient_matrix_UB_23      0.0302637000
_diffrn_orient_matrix_UB_31      0.0388087000
_diffrn_orient_matrix_UB_32      -0.0006984000
_diffrn_orient_matrix_UB_33      -0.0024135000
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_unetI/netI     0.1030
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88875
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.950
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76783
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.115a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic dark blue'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.033
_exptl_crystal_description       block
_exptl_crystal_F_000             2044
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.135
_exptl_crystal_size_min          0.112
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1375
_refine_ls_number_reflns         24548
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1181
_refine_ls_R_factor_gt           0.0771
_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^)+(0.0558P)^2^+2.8615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1518
_refine_ls_wR_factor_ref         0.1729
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15877
_reflns_number_total             24548
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc04208h2.cif
_cod_data_source_block           mo_xxs_dbdnc_pl3_a
_cod_depositor_comments
;

2025-05-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C150 H122'
_cod_original_formula_weight         1924.47
_cod_original_formula_moiety         '2(C72 H58), C6 H6'
_cod_original_formula_units_Z            2
_cod_database_code               1567797
_shelx_shelxl_version_number     2019/1
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.987
_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.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C15(H15), C19(H19), C22(H22), C23(H23), C42(H42), C43(H43), C47(H47),
 C58(H58), C59(H59), C89(H89), C91(H91), C97(H97), C99(H99), C100(H100),
 C106(H106), C113(H113), C125(H125), C130(H130), C143(H143), C144(H144),
 C145(H145), C20(H20), C25(H25), C33(H33), C34(H34), C57(H57), C61(H61),
 C67(H67), C76(H76), C92(H92), C98(H98), C109(H109), C110(H110), C116(H116),
 C118(H118), C122(H122), C128(H128), C131(H131), C136(H136), C137(H137),
 C140(H140), C142(H142), C148(H148), C35(H35), C69(H69), C73(H73), C127(H127),
 C139(H139), C147(H147)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C21(H21A,H21B,H21C),
 C51(H51A,H51B,H51C), C53(H53A,H53B,H53C), C103(H10A,H10B,H10C), C111(H11A,H11B,
 H11C), C115(H11D,H11E,H11F), C121(H12A,H12B,H12C), C129(H12D,H12E,H12F),
 C133(H13A,H13B,H13C), C9(H9A,H9B,H9C), C17(H17A,H17B,H17C), C29(H29A,H29B,
 H29C), C31(H31A,H31B,H31C), C37(H37A,H37B,H37C), C65(H65A,H65B,H65C), C71(H71A,
 H71B,H71C), C117(H11G,H11H,H11I), C119(H11J,H11K,H11L), C123(H12G,H12H,H12I),
 C141(H14A,H14B,H14C), C149(H14D,H14E,H14F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              40739
_shelx_hkl_checksum              11274
_shelx_fab_checksum              24661
_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 1.322
_oxdiff_exptl_absorpt_empirical_full_min 0.702