Enhancing the Stability of Photogenerated Benzophenone Triplet Radical Pairs through Supramolecular Assembly.
DeHaven, Baillie A.; Goodlett, Dustin W.; Sindt, Ammon J.; Noll, Niklas; De Vetta, Martina; Smith, Mark D.; Martin, Corey R.; González, Leticia; Shimizu, Linda S.; Journal of the American Chemical Society 140 (2018) 13064–13070; doi:10.1021/jacs.8b08501

data_4133097
_publ_section_title
;
 Enhancing the Stability of Photogenerated Benzophenone Triplet Radical
 Pairs through Supramolecular Assembly.
;
_journal_issue                   40
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13064
_journal_page_last               13070
_journal_paper_doi               10.1021/jacs.8b08501
_journal_volume                  140
_journal_year                    2018
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C31 H28 N2 O3'
_chemical_formula_sum            'C31 H28 N2 O3'
_chemical_formula_weight         476.55
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2018-06-28
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-11 deposited with the CCDC.
2018-07-19 downloaded from the CCDC.
;
_cell_angle_alpha                93.9470(10)
_cell_angle_beta                 90.4050(10)
_cell_angle_gamma                91.1100(10)
_cell_formula_units_Z            2
_cell_length_a                   6.0098(3)
_cell_length_b                   7.2615(3)
_cell_length_c                   27.0654(11)
_cell_measurement_reflns_used    9226
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.969
_cell_measurement_theta_min      2.263
_cell_volume                     1178.07(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'Bruker APEX3 v2016.5-0 (Bruker, 2016)'
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker PHOTON-100 area detector'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            72515
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        30.064
_diffrn_reflns_theta_max         30.064
_diffrn_reflns_theta_min         2.263
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.6948
_exptl_absorpt_correction_T_min  0.6724
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1627 before and 0.0434 after correction.
The Ratio of minimum to maximum transmission is 0.9678.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_description       plate
_exptl_crystal_F_000             504
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.097
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     657
_refine_ls_number_reflns         13721
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0560
_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^)+(0.1041P)^2^+0.1738P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1642
_reflns_Friedel_coverage         0.984
_reflns_Friedel_fraction_full    0.983
_reflns_Friedel_fraction_max     0.983
_reflns_number_gt                10061
_reflns_number_total             13721
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08501_si_002.cif
_cod_data_source_block           bd_bpla_uv
_cod_database_code               4133097
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.955
_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.a Secondary CH2 refined with riding coordinates:
 C2A(H2AA,H2AB), C17A(H17A,H17B), C2B(H2BA,H2BB), C17B(H17C,H17D)
2.b Aromatic/amide H refined with riding coordinates:
 N1A(H1A), N2A(H2A), C4A(H4A), C5A(H5A), C7A(H7A), C8A(H8A), C11A(H11A),
 C12A(H12A), C14A(H14A), C15A(H15A), C19A(H19A), C20A(H20A), C22A(H22A),
 C23A(H23A), C26A(H26A), C27A(H27A), C29A(H29A), C30A(H30A), N1B(H1B), N2B(H2B),
  C4B(H4B), C5B(H5B), C7B(H7B), C8B(H8B), C11B(H11B), C12B(H12B), C14B(H14B),
 C15B(H15B), C19B(H19B), C20B(H20B), C22B(H22B), C23B(H23B), C26B(H26B),
 C27B(H27B), C29B(H29B), C30B(H30B)
2.c Idealised Me refined as rotating group:
 C16A(H16A,H16B,H16C), C31A(H31A,H31B,H31C), C16B(H16D,H16E,H16F), C31B(H31D,
 H31E,H31F)
;
_shelx_res_checksum              30042
_shelx_hkl_checksum              96906
_olex2_submission_special_instructions 'No special instructions were received'