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_4134733
_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, 2(C2 H3 N), 4(F6 P)'
_chemical_formula_sum            'C68 H54 F24 N6 P4'
_chemical_formula_weight         1535.05
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.518(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   41.838(6)
_cell_length_b                   12.6590(19)
_cell_length_c                   29.003(4)
_cell_measurement_reflns_used    9997
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.613
_cell_measurement_theta_min      2.218
_cell_volume                     15313(4)
_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      100.02
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'QuazarTM optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0435
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            48267
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        23.533
_diffrn_reflns_theta_max         23.533
_diffrn_reflns_theta_min         0.976
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.199
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0886 before and 0.0553 after correction. The Ratio of minimum to maximum transmission is 0.8128. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_description       block
_exptl_crystal_F_000             6240
_exptl_crystal_size_max          0.149
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.096
_refine_diff_density_max         1.131
_refine_diff_density_min         -0.647
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.573
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     984
_refine_ls_number_reflns         11376
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.586
_refine_ls_R_factor_all          0.1516
_refine_ls_R_factor_gt           0.1223
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3618
_refine_ls_wR_factor_ref         0.3937
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7806
_reflns_number_total             11376
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c02128_si_002.cif
_cod_data_source_block           cx1296
_cod_depositor_comments
'Adding full bibliography for 4134731--4134735.cif.'
_cod_database_code               4134733
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.971
_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
 F15-F13 \\sim F15-F14 \\sim F15-F16 \\sim F13-F16 \\sim F13-F17 \\sim F13-F18
\\sim F14-F16 \\sim F17-F18
 with sigma of 0.04
 P3-F15 \\sim P3-F13 \\sim P3-F14 \\sim P3-F16 \\sim P3-F17 \\sim P3-F18
 with sigma of 0.02
3. Others
 Fixed Sof: P2(0.5) F7(0.5) F8(0.5) F9(0.5) F10(0.5) F11(0.5) F12(0.5) P3(0.5)
 F13(0.5) F14(0.5) F15(0.5) F16(0.5) F17(0.5) F18(0.5)
4.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C32(H32A,H32B), C57(H57A,H57B), C64(H64A,H64B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C12(H12), C14(H14),
 C15(H15), C17(H17), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C27(H27),
  C28(H28), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C37(H37),
 C39(H39), C40(H40), C42(H42), C44(H44), C46(H46), C47(H47), C49(H49), C51(H51),
  C53(H53), C54(H54), C55(H55), C56(H56), C59(H59), C60(H60), C62(H62), C63(H63)
4.c Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C)
;
_shelx_res_checksum              57700
_shelx_hkl_checksum              2557
_shelx_fab_checksum              25086
_olex2_date_sample_data_collection 2018-05-22
_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 cx1296
_olex2_submission_special_instructions 'No special instructions were received'