Orthogonal Di-Spiro Skeleton Engineering on Suppressing π-π Stacking and Spectral Broadening for High-Performance Narrowband Electroluminescence
Li, Hao-Ze; Yang, Yu-Tao; Zhao, Yi-Cheng; Xie, Feng-Ming; Tang, Jianxin; Li, Yanqing; Materials Horizons  (2025) –; doi:10.1039/D5MH01864A

data_1576313
_publ_section_title
;
 Orthogonal Di-Spiro Skeleton Engineering on Suppressing \p-\p Stacking
 and Spectral Broadening for High-Performance Narrowband
 Electroluminescence
;
_journal_name_full               'Materials Horizons'
_journal_paper_doi               10.1039/D5MH01864A
_journal_year                    2025
_chemical_formula_moiety         'C72 H63 B N2, 4[C2H6O]'
_chemical_formula_sum            'C80 H87 B N2 O4'
_chemical_formula_weight         1151.418
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2025-10-14
_audit_creation_method
;
Olex2 1.5-dev
(compiled 2025.10.02 svn.r20e3d319 for OlexSys, GUI svn.r7233)
;
_audit_update_record
;
2025-11-11 deposited with the CCDC.	2025-11-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.416(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.2644(4)
_cell_length_b                   17.5784(5)
_cell_length_c                   26.3039(7)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    170
_cell_measurement_theta_max      26.32
_cell_measurement_theta_min      2.45
_cell_volume                     6524.6(3)
_computing_cell_refinement       'SAINT V8.41 (?, 2016)'
_computing_data_collection       'Bruker APEX III'
_computing_data_reduction        'SAINT V8.41 (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5-dev (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.9973
_diffrn_measured_fraction_theta_max 0.9965
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0736
_diffrn_reflns_av_unetI/netI     0.0664
_diffrn_reflns_Laue_measured_fraction_full 0.9973
_diffrn_reflns_Laue_measured_fraction_max 0.9965
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            50332
_diffrn_reflns_point_group_measured_fraction_full 0.9973
_diffrn_reflns_point_group_measured_fraction_max 0.9965
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.40
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5193
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1580 before and 0.0752 after correction.
The Ratio of minimum to maximum transmission is 0.6967.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_description       needle
_exptl_crystal_F_000             2473.344
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.3187
_refine_diff_density_min         -0.3021
_refine_diff_density_rms         0.0553
_refine_ls_d_res_high            0.7992
_refine_ls_d_res_low             10.5773
_refine_ls_goodness_of_fit_ref   1.0461
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    102
_refine_ls_number_parameters     688
_refine_ls_number_reflns         13328
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0461
_refine_ls_R_factor_all          0.0709
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          -0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0563P)^2^+0.4022P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1126
_refine_ls_wR_factor_ref         0.1262
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                9325
_reflns_number_total             13328
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5mh01864a2.cif
_cod_data_source_block           dsbn1_0m
_cod_original_formula_sum        'C80 H87 B1 N2 O4'
_cod_database_code               1576313
_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:
 C20(H20), C14(H14), C28(H28), C35(H35), C22(H22), C15(H15), C52(H52),
 C29(H29), C54(H54), C68(H68), C5(H5), C46(H46), C17(H17), C44(H44), C16(H16),
 C69(H69), C72(H72), C38(H38), C37(H37), C8(H8), C6(H6), C71(H71), C7(H7),
 C75(H75), C70(H70), C73(H73), C74(H74)
2.b Idealised Me refined as rotating group:
 C41(H41a,H41b,H41c), C65(H65a,H65b,H65c), C61(H61a,H61b,H61c), C67(H67a,H67b,
 H67c), C66(H66a,H66b,H66c), C63(H63a,H63b,H63c), C43(H43a,H43b,H43c), C42(H42a,
 H42b,H42c), C56(H56a,H56b,H56c), C62(H62a,H62b,H62c), C58(H58a,H58b,H58c),
 C57(H57a,H57b,H57c)
;
_olex2_refine_details
;
Refinement using NoSpherA2, an implementation of
NOn-SPHERical Atom-form-factors in Olex2.
Please cite:
F. Kleemiss et al. Chem. Sci. DOI 10.1039/D0SC05526C - 2021
NoSpherA2 implementation of HAR makes use of
tailor-made aspherical atomic form factors calculated
on-the-fly from a Hirshfeld-partitioned electron density (ED) - not from
spherical-atom form factors.

The ED is calculated from a gaussian basis set single determinant SCF
wavefunction - either Hartree-Fock or DFT using selected funtionals
- for a fragment of the crystal.
This fragment can be embedded in an electrostatic crystal field by employing cluster charges
or modelled using implicit solvation models, depending on the software used.
The following options were used:
   SOFTWARE:       ORCA 6.1
   PARTITIONING:   NoSpherA2
   INT ACCURACY:   Low
   METHOD:         r2SCAN
   BASIS SET:      cc-pVDZ
   CHARGE:         0
   MULTIPLICITY:   1
   DATE:           2025-10-14_14-20-49
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 405 electrons were 
found in a volume of 1946\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
4 EtOH per Formula Unit which account for 416 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'