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_1570874
_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         'C51 H46 O, C H2 Cl2'
_chemical_formula_sum            'C52 H48 Cl2 O'
_chemical_formula_weight         759.80
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2019-11-15
_audit_creation_method
; 
Olex2 1.2 
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) 
;
_audit_update_record
;
2022-06-20 deposited with the CCDC.	2024-02-01 downloaded from the CCDC.
;
_cell_angle_alpha                93.696(5)
_cell_angle_beta                 114.031(4)
_cell_angle_gamma                108.413(5)
_cell_formula_units_Z            2
_cell_length_a                   12.819(3)
_cell_length_b                   13.093(3)
_cell_length_c                   14.822(3)
_cell_measurement_reflns_used    4142
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.21
_cell_volume                     2101.6(8)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1221
_diffrn_reflns_av_unetI/netI     0.0988
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            29916
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.543
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.192
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5558
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2008/1 (Bruker,2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_description       plate
_exptl_crystal_F_000             804
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         7408
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.1634
_refine_ls_R_factor_gt           0.0812
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2050
_refine_ls_wR_factor_ref         0.2373
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3306
_reflns_number_total             7408
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sc05533g4.cif
_cod_data_source_block           t
_cod_depositor_comments
'Adding full bibliography for 1570870--1570891.cif.'
_cod_database_code               1570874
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.981
_olex2_refinement_description
; 
1. Fixed Uiso 
 At 1.2 times of: 
  All C(H) groups, All C(H,H) groups 
 At 1.5 times of: 
  All C(H,H,H) groups 
2. Restrained distances 
 Cl2-C1S' = Cl1'-C1S' 
 1.73 with sigma of 0.01 
 Cl2-C1S' \\sim Cl2'-C1S 
 with sigma of 0.02 
 Cl1'-C1S' \\sim Cl1-C1S 
 with sigma of 0.02 
 Cl2-Cl1' \\sim Cl2'-Cl1 
 with sigma of 0.04 
 Cl1'-C1S' \\sim Cl1-C1S \\sim Cl2-C1S' \\sim Cl2'-C1S 
 with sigma of 0.01 
 Cl2'-Cl1 \\sim Cl1'-Cl2 
 with sigma of 0.01 
3. Uiso/Uaniso restraints and constraints 
Uanis(Cl1) \\sim Ueq, Uanis(C1S) \\sim Ueq, Uanis(Cl2') \\sim Ueq, Uanis(C1S') 
\\sim Ueq, Uanis(Cl1') \\sim Ueq, Uanis(Cl2) \\sim Ueq, Uanis(C15) \\sim Ueq: 
with sigma of 0.01 and sigma for terminal atoms of 0.02 
4. Others 
 Sof(C1S)=Sof(H1SC)=Sof(H1SD)=Sof(Cl1)=Sof(Cl2')=1-FVAR(1) 
 Sof(C1S')=Sof(H1SA)=Sof(H1SB)=Sof(Cl1')=Sof(Cl2)=FVAR(1) 
5.a Secondary CH2 refined with riding coordinates: 
 C1S'(H1SA,H1SB), C1S(H1SC,H1SD) 
5.b Aromatic/amide H refined with riding coordinates: 
 C2(H2), C6(H6), C11(H11), C13(H13), C26(H26), C27(H27), C28(H28), C29(H29), 
 C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C40(H40), C41(H41), C42(H42), 
  C43(H43), C45(H45), C48(H48), C49(H49), C50(H50), C51(H51) 
5.c Idealised Me refined as rotating group: 
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B, 
 H18C), C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A, 
 H23B,H23C) 
;
_shelx_res_checksum              38780
_olex2_submission_special_instructions 'No special instructions were received'