Mechanical-Bond-Induced Exciplex Fluorescence in an Anthracene-Based Homo[2]catenane.
Garci, Amine; Beldjoudi, Yassine; Kodaimati, Mohamad S.; Hornick, Jessica E.; Nguyen, Minh T.; Cetin, M. Mustafa; Stern, Charlotte L.; Roy, Indranil; Weiss, Emily A.; Stoddart, J. Fraser; Journal of the American Chemical Society 142 (2020) 7956–7967; doi:10.1021/jacs.0c02128

data_4134734
_publ_section_title
;
 Mechanical-Bond-Induced Exciplex Fluorescence in an Anthracene-Based
 Homo[2]catenane.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7956
_journal_page_last               7967
_journal_paper_doi               10.1021/jacs.0c02128
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C64 H48 N4, 4(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C68 H54 F24 N6 P4'
_chemical_formula_weight         1535.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           68
_space_group_name_Hall           '-C 2a 2ac'
_space_group_name_H-M_alt        'C c c a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2019-12-17 # Formatted by publCIF

;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.0098(9)
_cell_length_b                   34.634(3)
_cell_length_c                   39.679(3)
_cell_measurement_reflns_used    9355
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      65.156
_cell_measurement_theta_min      2.227
_cell_volume                     16504(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0505
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       40
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            39705
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        65.429
_diffrn_reflns_theta_max         65.429
_diffrn_reflns_theta_min         2.227
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.680
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1234 before and 0.0684 after correction. The Ratio of minimum to maximum transmission is 0.7141. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       plate
_exptl_crystal_F_000             6240
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.482
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         7007
_refine_ls_number_restraints     261
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0752
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1053P)^2^+47.6391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2040
_refine_ls_wR_factor_ref         0.2162
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5339
_reflns_number_total             7007
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02128_si_004.cif
_cod_data_source_block           cx1296b
_cod_depositor_comments
'Adding full bibliography for 4134731--4134735.cif.'
_cod_original_sg_symbol_Hall     '-C 2b 2bc'
_cod_original_sg_symbol_H-M      'C c c e'
_cod_database_code               4134734
_publcif_datablock.id            {ebd8992c-643b-4272-be2f-9b6d59b2cd84}
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.906
_shelx_estimated_absorpt_t_min   0.607
_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
 F8-F10 \\sim F8-F11 \\sim F8-F12 \\sim F8-F13 \\sim F9-F10 \\sim F9-F11 \\sim
F9-F12 \\sim F9-F13 \\sim F10-
 F11 \\sim F10-F13 \\sim F11-F12 \\sim F12-F13
 with sigma of 0.02
 P3-F8 \\sim P3-F9 \\sim P3-F10 \\sim P3-F11 \\sim P3-F12 \\sim P3-F13
 with sigma of 0.01
 F12A-F8A \\sim F12A-F9A \\sim F12A-F11A \\sim F12A-F13A \\sim F8A-F10A \\sim
F8A-F11A \\sim F8A-F13A
 \\sim F9A-F10A \\sim F9A-F11A \\sim F9A-F13A \\sim F10A-F11A \\sim F10A-F13A
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 P3A, F8A, F9A, F10A, F11A, F12A, F13A, F12, P3, F8, F9, F10, F11, F13
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(P3A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=Sof(F13A)=0.5*(1-
 FVAR(2))
 Sof(P3)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=Sof(F13)=0.5*FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C8(H8A,H8B)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13),
 C15(H15), C16(H16), C18(H18), C20(H20), C22(H22), C23(H23), C25(H25), C27(H27),
  C29(H29), C30(H30), C31(H31), C32(H32)
5.c Idealised Me refined as rotating group:
 C34(H34A,H34B,H34C)
;
_shelx_res_checksum              11248
_shelx_hkl_checksum              41676
_shelx_fab_checksum              71158
_olex2_date_sample_data_collection 2018-05-23
_olex2_date_sample_submission    2018-05-22
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder in Paratone oil'
_olex2_submission_original_sample_id cx1296b
_olex2_submission_special_instructions 'No special instructions were received'
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
_publcif_funding_html
;
;