Intramolecular exciplex featuring a bis-sp<sup>3</sup> C-locked acceptor-donor-acceptor sandwich.
Xie, Feng-Ming; Wang, Han-Yang; Li, Hao-Ze; Zhang, Kai; Shen, Yang; Zou, Jianhua; Li, Yan-Qing; Tang, Jian-Xin; Materials horizons 11 (2024) 3921–3927; doi:10.1039/d4mh00400k

data_1571729
_publ_section_title
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 Intramolecular exciplex featuring a bis-sp<sup>3</sup> C-locked
 acceptor-donor-acceptor sandwich.
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_journal_issue                   16
_journal_name_full               'Materials horizons'
_journal_page_first              3921
_journal_page_last               3927
_journal_paper_doi               10.1039/d4mh00400k
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C98 H58 N8 O2, CH2Cl2, 0.5[C2H6O], CH2Cl2'
_chemical_formula_sum            'C101.5 H65 Cl4 N8 O2.5'
_chemical_formula_weight         1575.39
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_audit_creation_date             2024-05-17
_audit_creation_method
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Olex2 1.5-dev
(compiled 2024.05.14 svn.rc2abdb5a for OlexSys, GUI svn.r6697)
;
_audit_update_record
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2024-05-24 deposited with the CCDC.	2024-05-29 downloaded from the CCDC.
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_cell_angle_alpha                97.833(2)
_cell_angle_beta                 93.512(2)
_cell_angle_gamma                99.176(2)
_cell_formula_units_Z            2
_cell_length_a                   14.2142(8)
_cell_length_b                   14.3406(7)
_cell_length_c                   19.3048(9)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      26.348
_cell_measurement_theta_min      2.204
_cell_volume                     3834.6(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       APEX-III
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.9972
_diffrn_measured_fraction_theta_max 0.9962
_diffrn_measurement_device_type  'Bruker 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  0.0560
_diffrn_reflns_av_unetI/netI     0.0671
_diffrn_reflns_Laue_measured_fraction_full 0.9972
_diffrn_reflns_Laue_measured_fraction_max 0.9962
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45300
_diffrn_reflns_point_group_measured_fraction_full 0.9972
_diffrn_reflns_point_group_measured_fraction_max 0.9962
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.88
_exptl_absorpt_coefficient_mu    0.216
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0718 before and 0.0565 after correction.
The Ratio of minimum to maximum transmission is 0.9424.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             1624.052
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.5164
_refine_diff_density_min         -0.4148
_refine_diff_density_rms         0.1046
_refine_ls_d_res_high            0.8107
_refine_ls_d_res_low             10.8574
_refine_ls_extinction_coef       0.0113(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_goodness_of_fit_ref   1.0895
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    116
_refine_ls_number_parameters     974
_refine_ls_number_reflns         15041
_refine_ls_number_restraints     1456
_refine_ls_restrained_S_all      1.0372
_refine_ls_R_factor_all          0.1103
_refine_ls_R_factor_gt           0.0830
_refine_ls_shift/su_max          -0.0005
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+11.0168P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1789
_refine_ls_wR_factor_ref         0.1942
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              17
_reflns_limit_h_min              -17
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                11025
_reflns_number_total             15041
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4mh00400k2.cif
_cod_data_source_block           2trz_0m
_cod_depositor_comments
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          Adding full bibliography for 1571729.cif.

2025-07-10
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
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_cod_original_formula_sum            'C203 H130 Cl8 N16 O5'
_cod_original_formula_weight         3150.79
_cod_original_formula_moiety
'2(C98 H58 N8 O2), 2[CH2Cl2], 1[C2H6O], 2[CH2Cl2]'
_cod_original_formula_units_Z            1
_cod_database_code               1571729
_olex2_refinement_description
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1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.008 and sigma for 1-3 distances of 8
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.008 and sigma
for terminal atoms of 8 within 2A
4.a Aromatic/amide H refined with riding coordinates:
 C36(H36), C43(H43), C38(H38), C45(H45), C44(H44), C32(H32), C79(H79),
 C24(H24), C88(H88), C80(H80), C54(H54), C23(H23), C74(H74), C75(H75), C20(H20),
  C28(H28), C90(H90), C61(H61), C67(H67), C21(H21), C30(H30), C25(H25),
 C63(H63), C89(H89), C83(H83), C18(H18), C62(H62), C82(H82), C73(H73), C17(H17),
  C29(H29), C91(H91), C52(H52), C94(H94), C57(H57), C92(H92), C49(H49),
 C70(H70), C95(H95), C51(H51), C55(H55), C69(H69), C98(H98), C68(H68), C50(H50),
  C96(H96), C56(H56), C14(H14), C10(H10), C97(H97), C6(H6), C13(H13), C11(H11),
 C12(H12), C3(H3), C7(H7), C5(H5), C4(H4)
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_smtbx_masks_special_details
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A solvent mask was calculated and 181 electrons were 
found in a volume of 624\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 2[CH2Cl2], 1[CH4O], 2[CH2Cl2] per Formula Unit 
which account for 186 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'