Controllable π-π coupling of intramolecular dimer models in aggregated states.
Liao, Qiuyan; Li, Aisen; Huang, Arui; Wang, Jiaqiang; Chang, Kai; Li, Hehua; Yao, Pengfei; Zhong, Cheng; Xie, Peidong; Wang, Jinfeng; Li, Zhen; Li, Qianqian; Chemical science 15 (2024) 4364–4373; doi:10.1039/d3sc05533g

data_1570873
_publ_section_title
;
 Controllable &#x3c0;-&#x3c0; coupling of intramolecular dimer models in
 aggregated states.
;
_journal_issue                   12
_journal_name_full               'Chemical science'
_journal_page_first              4364
_journal_page_last               4373
_journal_paper_doi               10.1039/d3sc05533g
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C35 H38 O'
_chemical_formula_sum            'C35 H38 O'
_chemical_formula_weight         474.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-06-20
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2022-06-20 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.519(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6293(12)
_cell_length_b                   12.4614(17)
_cell_length_c                   26.146(4)
_cell_measurement_reflns_used    9996
_cell_measurement_temperature    293
_cell_measurement_theta_max      31.51
_cell_measurement_theta_min      2.26
_cell_volume                     2802.8(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0331
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            20821
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.371
_diffrn_reflns_theta_min         1.563
_diffrn_source_current           0.0
_diffrn_source_power             0.0
_diffrn_source_voltage           0.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.065
_exptl_absorpt_correction_T_max  0.7463
_exptl_absorpt_correction_T_min  0.6355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction.'
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       block
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.198
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     404
_refine_ls_number_reflns         5698
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0553
_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^)+(0.0539P)^2^+1.4106P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1499
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4484
_reflns_number_total             5698
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05533g4.cif
_cod_data_source_block           mo_190719c
_cod_depositor_comments
'Adding full bibliography for 1570870--1570891.cif.'
_cod_database_code               1570873
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.990
_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. Restrained distances
 C10-C1AA \\sim C10-C21A
 with sigma of 0.02
 C1AA-C34A \\sim C21A-C34
 with sigma of 0.02
 C1AA-C33A \\sim C21A-C33
 with sigma of 0.02
 C1AA-C32A \\sim C21A-C32
 with sigma of 0.02
 C10-C34A \\sim C10-C34
 with sigma of 0.04
 C10-C33A \\sim C10-C33
 with sigma of 0.04
 C10-C32A \\sim C10-C32
 with sigma of 0.04
 C34A-C33A \\sim C34-C33
 with sigma of 0.04
 C34A-C32A \\sim C34-C32
 with sigma of 0.04
 C33A-C32A \\sim C33-C32
 with sigma of 0.04
 C28-C31A \\sim C28-C31
 with sigma of 0.02
 C28-C29A \\sim C28-C29
 with sigma of 0.02
 C28-C30A \\sim C28-C30
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C30) \\sim Ueq, Uanis(C30A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C33A) \\sim Ueq, Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
4. Others
 Sof(C32)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C34)=Sof(H34D)=Sof(H34E)=Sof(H34F)=
 Sof(C33)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C21A)=1-FVAR(1)
 Sof(C1AA)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=Sof(C33A)=Sof(H33A)=
 Sof(H33B)=Sof(H33C)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(1)
 Sof(C29)=Sof(H29D)=Sof(H29E)=Sof(H29F)=Sof(C31)=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 Sof(C30)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(2)
 Sof(C31A)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C29A)=Sof(H29A)=Sof(H29B)=
 Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C9(H9), C3(H3), C11(H11), C5(H5), C15(H15), C21(H21), C19(H19), C16(H16),
 C25(H25), C23(H23), C22(H22), C17(H17), C18(H18), C24(H24)
5.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C26(H26A,H26B,H26C), C31A(H31A,H31B,H31C), C29A(H29A,
 H29B,H29C), C30A(H30A,H30B,H30C), C34A(H34A,H34B,H34C), C33A(H33A,H33B,H33C),
 C32A(H32A,H32B,H32C), C32(H32D,H32E,H32F), C34(H34D,H34E,H34F), C33(H33D,H33E,
 H33F), C29(H29D,H29E,H29F), C31(H31D,H31E,H31F), C30(H30D,H30E,H30F)
;
_olex2_submission_special_instructions 'No special instructions were received'