Hierarchical supramolecular co-assembly formation employing multi-component light-harvesting charge transfer interactions giving rise to long-wavelength emitting luminescent microspheres.
Gorai, Tumpa; Lovitt, June I.; Umadevi, Deivasigamani; McManus, Gavin; Gunnlaugsson, Thorfinnur; Chemical science 13 (2022) 7805–7813; doi:10.1039/d2sc02097a

data_1567048
_publ_section_title
;
 Hierarchical supramolecular co-assembly formation employing
 multi-component light-harvesting charge transfer interactions giving rise
 to long-wavelength emitting luminescent microspheres.
;
_journal_issue                   26
_journal_name_full               'Chemical science'
_journal_page_first              7805
_journal_page_last               7813
_journal_paper_doi               10.1039/d2sc02097a
_journal_volume                  13
_journal_year                    2022
_chemical_absolute_configuration syn
_chemical_formula_moiety         '2(C10 H2 N4), C31 H27 N3 O3, C2 H6 O'
_chemical_formula_sum            'C53 H37 N11 O4'
_chemical_formula_weight         891.93
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2022-02-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-02-28 deposited with the CCDC.	2022-05-30 downloaded from the CCDC.
;
_cell_angle_alpha                93.3946(13)
_cell_angle_beta                 99.9779(14)
_cell_angle_gamma                107.9484(13)
_cell_formula_units_Z            1
_cell_length_a                   10.1334(4)
_cell_length_b                   10.2002(3)
_cell_length_c                   11.4807(4)
_cell_measurement_reflns_used    1362
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.56
_cell_measurement_theta_min      2.52
_cell_volume                     1103.79(7)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX 3 (Bruker, 2017) '
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CMOS area detector'
_diffrn_detector_area_resol_mean 5.12
_diffrn_detector_type            'Bruker PHOTON 50'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Quest ECO'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    '0.5 mm double-pinhole'
_diffrn_radiation_detector       'Bruker PHOTON 50'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_unetI/netI     0.0686
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            45138
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.755
_diffrn_reflns_theta_min         2.484
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           20.0
_diffrn_source_power             1.0
_diffrn_source_type              'Siemens, KFF Mo 2K -90 C'
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.089
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0587 before and 0.0517 after correction.
The Ratio of minimum to maximum transmission is 0.9434.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear yellowish yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.342
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             464
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.379
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details
;
 Flack x determined using 3658 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.6(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         13673
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0934
_refine_ls_R_factor_gt           0.0551
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+0.3529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1136
_refine_ls_wR_factor_ref         0.1315
_reflns_Friedel_coverage         0.990
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.987
_reflns_number_gt                9700
_reflns_number_total             13673
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc02097a2.cif
_cod_data_source_block           DPA-TCNB
_cod_depositor_comments          'Adding full bibliography for 1567048.cif.'
_cod_database_code               1567048
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.990
_shelx_estimated_absorpt_t_min   0.970
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O7-H7
 0.9 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C11(H11), C26(H26)
3.b Secondary CH2 refined with riding coordinates:
 C67(H67A,H67B)
3.c Aromatic/amide H refined with riding coordinates:
 C38(H38), C41(H41), C3(H3), C5(H5), N10(H10), C14(H14), C15(H15), C17(H17),
 C18(H18), C19(H19), C20(H20), C22(H22), N25(H25), C29(H29), C31(H31), C32(H32),
  C33(H33), C34(H34), C36(H36), C37(H37), C52(H52), C55(H55)
3.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C27(H27A,H27B,H27C), C68(H68A,H68B,H68C)
3.e Idealised tetrahedral OH refined as rotating group:
 O66(H66)
;
_shelx_res_checksum              63663
_shelx_hkl_checksum              68296
_olex2_submission_special_instructions 'No special instructions were received'