Molecular motion, dielectric response, and phase transition of charge-transfer crystals: acquired dynamic and dielectric properties of polar molecules in crystals.
Harada, Jun; Ohtani, Masaki; Takahashi, Yukihiro; Inabe, Tamotsu; Journal of the American Chemical Society 137 (2015) 4477–4486; doi:10.1021/jacs.5b00412

data_4129315
_publ_section_title
;
 Molecular motion, dielectric response, and phase transition of
 charge-transfer crystals: acquired dynamic and dielectric properties of
 polar molecules in crystals.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4477
_journal_page_last               4486
_journal_paper_doi               10.1021/jacs.5b00412
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'Br4 C8 O3, 2(C10 H6)'
_chemical_formula_sum            'C28 H12 Br4 O3'
_chemical_formula_weight         716.02
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2014-12-18
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                85.0856(13)
_cell_angle_beta                 73.6923(12)
_cell_angle_gamma                69.0129(12)
_cell_formula_units_Z            2
_cell_length_a                   10.0091(8)
_cell_length_b                   10.0755(8)
_cell_length_c                   12.5454(10)
_cell_measurement_reflns_used    9947
_cell_measurement_temperature    265
_cell_measurement_theta_max      27.342
_cell_measurement_theta_min      2.263
_cell_volume                     1133.55(16)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'Bruker APEX2 2014.1-1 (Bruker, 2014)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2008)'
_diffrn_ambient_temperature      265
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0334
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            21564
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.378
_diffrn_reflns_theta_min         1.691
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.133
_exptl_absorpt_correction_T_max  0.2176
_exptl_absorpt_correction_T_min  0.0685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.1037 before and 0.0458 after correction. The Ratio of minimum to maximum transmission is 0.3148. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.098
_exptl_crystal_description       block
_exptl_crystal_F_000             688
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.576
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5118
_refine_ls_number_restraints     142
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0389
_refine_ls_R_factor_gt           0.0318
_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^)+(0.0473P)^2^+0.8194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0912
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4369
_reflns_number_total             5118
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00412_si_002.cif
_cod_data_source_block           perylene_TBPA_265K
_cod_database_code               4129315
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.360
_shelx_estimated_absorpt_t_min   0.125
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Restrained distances
 C7-C1A \\sim C4-C1B \\sim C8-C2A \\sim C5-C2B
 with sigma of 0.02
 C4-Br2A \\sim C7-Br2B \\sim C5-Br3A \\sim C8-Br3B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(Br2A) = Uanis(Br2B)
Uanis(Br3A) = Uanis(Br3B)
Uanis(O1A) = Uanis(O1B)
Uanis(O2A) = Uanis(O2B)
Uanis(O3A) = Uanis(O3B)
Uanis(C1A) = Uanis(C1B)
Uanis(C2A) = Uanis(C2B)
4. Rigid body (RIGU) restrains
 O3A, O1A, O2A, Br1, Br2A, Br3A, Br4, C1A, C2A, C3, C4, C5, C6, C7, C8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Same fragment restrains
{O3A, O1A, O2A, C1A, C2A} sigma for 1-2: 0.02, 1-3: 0.04
as
{O3B, O1B, O2B, C1B, C2B}
6. Others
 Sof(O3B)=Sof(O1B)=Sof(O2B)=Sof(C1B)=Sof(C2B)=Sof(Br2B)=Sof(Br3B)=1-FVAR(1)
 Sof(O3A)=Sof(O1A)=Sof(O2A)=Sof(Br2A)=Sof(Br3A)=Sof(C1A)=Sof(C2A)=FVAR(1)
7.a Free rotating group:
 O3A(O1A,O2A,Br1,Br2A,Br3A,Br4,C1A,C2A,C3,C4,C5,C6,C7,C8)
7.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C19(H19), C20(H20),
 C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              9955
_shelx_hkl_checksum              62421
_olex2_submission_special_instructions 'No special instructions were received'