Singlet Fission in Quaterrylenediimide Thin Films
Chen, Michelle; Powers-Riggs, Natalia E.; Coleman, Adam F.; Young, Ryan M.; Wasielewski, Michael R.; The Journal of Physical Chemistry C  (2020) –; doi:10.1021/acs.jpcc.9b10397

data_1557141
_publ_section_title
;
 Singlet Fission in Quaterrylenediimide Thin Films
;
_journal_name_full               'The Journal of Physical Chemistry C'
_journal_paper_doi               10.1021/acs.jpcc.9b10397
_journal_year                    2020
_chemical_formula_moiety         'C68 H50 N2 O4'
_chemical_formula_sum            'C68 H50 N2 O4'
_chemical_formula_weight         959.10
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 107.438(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   13.949(3)
_cell_length_b                   15.719(3)
_cell_length_c                   15.272(3)
_cell_measurement_reflns_used    2281
_cell_measurement_temperature    100
_cell_measurement_theta_max      64.195
_cell_measurement_theta_min      4.137
_cell_volume                     3194.7(11)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0424
_diffrn_reflns_av_unetI/netI     0.1498
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9798
_diffrn_reflns_point_group_measured_fraction_full 0.698
_diffrn_reflns_point_group_measured_fraction_max 0.698
_diffrn_reflns_theta_full        58.923
_diffrn_reflns_theta_max         58.923
_diffrn_reflns_theta_min         4.137
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  0.7524
_exptl_absorpt_correction_T_min  0.5675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1021 before and 0.0616 after correction. The Ratio of minimum to maximum transmission is 0.7543. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    0.997
_exptl_crystal_description       block
_exptl_crystal_F_000             1008
_exptl_crystal_recrystallization_method
'compound was crystallized through the slow diffusion of methanol into a toluene solution.'
_exptl_crystal_size_max          0.166
_exptl_crystal_size_mid          0.058
_exptl_crystal_size_min          0.057
_refine_diff_density_max         0.644
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.3(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     675
_refine_ls_number_reflns         6414
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.1661
_refine_ls_R_factor_gt           0.1205
_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          0.3002
_refine_ls_wR_factor_ref         0.3549
_reflns_Friedel_coverage         0.399
_reflns_Friedel_fraction_full    0.416
_reflns_Friedel_fraction_max     0.416
_reflns_number_gt                3538
_reflns_number_total             6414
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jp9b10397_si_002.cif
_cod_data_source_block           new_unit
_cod_original_cell_volume        3194.9(10)
_cod_database_code               1557141
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.924
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C55, C54, C56, C52, C53, C51, C64, C65, C63, C67, C68, C66
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
3.a Ternary CH refined with riding coordinates:
 C51(H51), C54(H54), C63(H63), C66(H66)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C12(H12), C3(H3), C13(H13), C17(H17), C18(H18), C22(H22),
 C23(H23), C27(H27), C28(H28), C32(H32), C33(H33), C38(H38), C37(H37), C42(H42),
  C48(H48), C47(H47), C49(H49), C59(H59), C60(H60), C61(H61)
3.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C55(H55A,H55B,H55C), C56(H56A,H56B,
 H56C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,
 H68B,H68C)
;
_shelx_res_checksum              26378
_shelx_hkl_checksum              59592
_shelx_fab_checksum              3320
_olex2_exptl_crystal_mounting_method
'Appropriate crystal was selected and added to a microsource loop affixed with paratone oil. '
_olex2_submission_original_sample_id (iPr2Ph)2QDI
_olex2_submission_special_instructions 'No special instructions were received'