Probing Distance Dependent Charge-Transfer Character in Excimers of Extended Viologen Cyclophanes Using Femtosecond Vibrational Spectroscopy.
Wu, Yilei; Zhou, Jiawang; Phelan, Brian T.; Mauck, Catherine M.; Stoddart, J. Fraser; Young, Ryan M.; Wasielewski, Michael R.; Journal of the American Chemical Society 139 (2017) 14265–14276; doi:10.1021/jacs.7b08275

data_4131660
_publ_section_title
;
 Probing Distance Dependent Charge-Transfer Character in Excimers of
 Extended Viologen Cyclophanes Using Femtosecond Vibrational Spectroscopy.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14265
_journal_page_last               14276
_journal_paper_doi               10.1021/jacs.7b08275
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C48 H40 N4, 4(F6 P), C2 H3 N'
_chemical_formula_sum            'C50 H43 F24 N5 P4'
_chemical_formula_weight         1293.77
_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
_audit_creation_date             2016-01-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                83.000(3)
_cell_angle_beta                 73.214(2)
_cell_angle_gamma                71.465(2)
_cell_formula_units_Z            1
_cell_length_a                   9.6412(3)
_cell_length_b                   11.9525(4)
_cell_length_c                   13.9387(4)
_cell_measurement_reflns_used    3215
_cell_measurement_temperature    250(2)
_cell_measurement_theta_max      63.409
_cell_measurement_theta_min      3.313
_cell_volume                     1457.24(8)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2013)'
_computing_data_collection       'APEX2 V2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT'
_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      250.03
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Quazar optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0222
_diffrn_reflns_av_unetI/netI     0.0244
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10403
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         63.666
_diffrn_reflns_theta_min         3.313
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    2.255
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6474
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0471 before and 0.0366 after correction.
The Ratio of minimum to maximum transmission is 0.8602.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_description       block
_exptl_crystal_F_000             654
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.216
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.143
_refine_diff_density_max         1.152
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.437
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         4751
_refine_ls_number_restraints     602
_refine_ls_restrained_S_all      1.509
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0968
_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          0.3130
_refine_ls_wR_factor_ref         0.3339
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3702
_reflns_number_total             4751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08275_si_002.cif
_cod_data_source_block           cx0661a
_cod_database_code               4131660
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.739
_shelx_estimated_absorpt_t_min   0.642
_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
 P2-F9 \\sim P2-F8A \\sim P2-F8 \\sim P2-F12A \\sim P2-F12 \\sim P2-F11A \\sim
P2-F11 \\sim P2-F7A \\sim P2-
 F9A \\sim P2-F10 \\sim P2-F10A
 with sigma of 0.01
 F11-F10 \\sim F9-F7 \\sim F12-F8 \\sim F11A-F7A \\sim F12A-F8A \\sim F9A-F10A
\\sim F11A-F10A \\sim F9A-
 F7A \\sim F12A-F8A \\sim F11-F7 \\sim F12-F8 \\sim F9-F10 \\sim F7A-F10A \\sim
F11A-F8A \\sim F6A-F1 \\sim F2-
 F3A
 with sigma of 0.01
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-FVAR(1)
 Sof(F7)=Sof(F8)=Sof(F9)=Sof(F10)=Sof(F11)=Sof(F12)=FVAR(1)
 Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(2)
 Sof(F3)=Sof(F4)=Sof(F5)=Sof(F6)=FVAR(2)
 Fixed Sof: N3(0.5) C25(0.5) C26(0.5) H26A(0.5) H26B(0.5) H26C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C18(H18A,H18B)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C24(H24)
5.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C)
;
_shelx_res_checksum              56158
_shelx_hkl_checksum              49395
_olex2_date_sample_submission    2016-01-19
_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 cx0661a
_olex2_submission_special_instructions 'No special instructions were received'