Coexistence of Parallel and Rotary Stackings in the Lamellar Crystals of a Perylene Bisimide Dyad for Temperature-Sensitive Bicomponent Emission.
Chen, Jiehuan; Tang, Ningning; Zhou, Jiadong; Wang, Liangxuan; Jiang, Nianqiang; Zheng, Nan; Liu, Linlin; Xie, Zengqi; The journal of physical chemistry letters  (2021) 3373–3378; doi:10.1021/acs.jpclett.1c00674

data_8000491
_publ_section_title
;
 Coexistence of Parallel and Rotary Stackings in the Lamellar Crystals of
 a Perylene Bisimide Dyad for Temperature-Sensitive Bicomponent Emission.
;
_journal_name_full               'The journal of physical chemistry letters'
_journal_page_first              3373
_journal_page_last               3378
_journal_paper_doi               10.1021/acs.jpclett.1c00674
_journal_year                    2021
_chemical_formula_moiety         'C52 H16 N4 O8'
_chemical_formula_sum            'C52 H16 N4 O8'
_chemical_formula_weight         824.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.074(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.786(8)
_cell_length_b                   38.640(5)
_cell_length_c                   9.0207(7)
_cell_measurement_reflns_used    1840
_cell_measurement_temperature    149.99(10)
_cell_measurement_theta_max      59.2160
_cell_measurement_theta_min      3.5620
_cell_volume                     8638(3)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_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    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      149.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.933
_diffrn_measured_fraction_theta_max 0.933
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w     32.00  66.00   0.50   15.00    --    0.00  37.00-124.00   68
  2  \w    -57.00 -32.00   0.50   60.00    --    5.00 -37.00  79.00   50
  3  \w     18.00  43.00   0.50   60.00    --    5.00  37.00-124.00   50
  4  \w    -92.00 -47.00   0.50   60.00    --  -98.80  37.00-124.00   90
  5  \w   -161.00-136.00   0.50   60.00    --  -98.80 -37.00  79.00   50
  6  \w     26.00  56.00   0.50   15.00    --    0.00  19.00   0.00   60
  7  \w    -88.00   9.00   0.50   15.00    --    0.00 -57.00   0.00  194
  8  \w    -92.00 -10.00   0.50   60.00    --  -98.80  72.00  30.00  164
  9  \w   -111.00 -36.00   0.50   60.00    --  -98.80  19.00 -90.00  150
 10  \w   -132.00 -95.00   0.50   60.00    --  -98.80 -19.00-150.00   74
 11  \w   -187.00 -97.00   0.50   60.00    --  -98.80 -19.00 120.00  180
 12  \w   -112.00 -46.00   0.50   60.00    --  -98.80  38.00  60.00  132
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0300310000
_diffrn_orient_matrix_UB_12      0.0174989000
_diffrn_orient_matrix_UB_13      0.1307620000
_diffrn_orient_matrix_UB_21      0.0541417000
_diffrn_orient_matrix_UB_22      -0.0070382000
_diffrn_orient_matrix_UB_23      -0.0749318000
_diffrn_orient_matrix_UB_31      -0.0041330000
_diffrn_orient_matrix_UB_32      0.0352042000
_diffrn_orient_matrix_UB_33      -0.0806973000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1189
_diffrn_reflns_av_unetI/netI     0.2759
_diffrn_reflns_Laue_measured_fraction_full 0.933
_diffrn_reflns_Laue_measured_fraction_max 0.933
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            28714
_diffrn_reflns_point_group_measured_fraction_full 0.933
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        67.080
_diffrn_reflns_theta_max         67.080
_diffrn_reflns_theta_min         2.900
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.362
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.00074
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.634
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.796
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.272
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         14392
_refine_ls_number_restraints     219
_refine_ls_restrained_S_all      1.294
_refine_ls_R_factor_all          0.3702
_refine_ls_R_factor_gt           0.2234
_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          0.5168
_refine_ls_wR_factor_ref         0.5841
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3433
_reflns_number_total             14392
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jz1c00674_si_002.cif
_cod_data_source_block           dpbi
_cod_database_code               8000491
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 93.14
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C067-O105
 1.22 with sigma of 0.01
 N046-C082
 1.5 with sigma of 0.01
 C082-C071
 1.5 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C067) \\sim Ueq, Uanis(C050) \\sim Ueq, Uanis(C033) \\sim Ueq,
Uanis(C043) \\sim Ueq, Uanis(C049) \\sim Ueq, Uanis(C057) \\sim Ueq,
Uanis(C058) \\sim Ueq, Uanis(C045) \\sim Ueq, Uanis(C010) \\sim Ueq,
Uanis(C024) \\sim Ueq, Uanis(C038) \\sim Ueq, Uanis(C044) \\sim Ueq,
Uanis(C008) \\sim Ueq, Uanis(C021) \\sim Ueq, Uanis(C025) \\sim Ueq,
Uanis(C034) \\sim Ueq, Uanis(C015) \\sim Ueq, Uanis(C027) \\sim Ueq,
Uanis(C039) \\sim Ueq, Uanis(C023) \\sim Ueq, Uanis(C032) \\sim Ueq,
Uanis(C051) \\sim Ueq, Uanis(N046) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C041) \\sim Ueq, Uanis(C018) \\sim Ueq, Uanis(C001) \\sim Ueq,
Uanis(C002) \\sim Ueq, Uanis(C013) \\sim Ueq, Uanis(C006) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C047) \\sim Ueq, Uanis(C052) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C019) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C082) \\sim Ueq, Uanis(C071) \\sim Ueq, Uanis(C060) \\sim Ueq,
Uanis(C069) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C008) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4.a Aromatic/amide H refined with riding coordinates:
 C013(H013), C014(H014), C015(H015), C020(H020), C027(H027), C031(H031),
 C034(H034), C035(H035), C037(H037), C040(H040), C041(H041), C044(H044),
 C045(H045), C051(H051), C057(H057), C058(H058)
4.b Fitted hexagon refined as free rotating group:
 C001(C003,C017,C006,C004,C002), C005(C011,C019,N026,C022,C016), C032(C023,
 C039,C052,N029,C047), C036(N007,C030,C009,C018,C028), C038(C024,C010,C008,C021,
 C025), C049(N046,C067,C050,C033,C043)
;
_shelx_res_checksum              88175
_shelx_hkl_checksum              98896
_shelx_fab_checksum              65342
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 743.218
_oxdiff_exptl_absorpt_empirical_full_min 0.201