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_4129312
_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, 1(C24 H12)'
_chemical_formula_sum            'C32 H12 Br4 O3'
_chemical_formula_weight         764.06
_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     direct
_audit_creation_date             2014-12-19
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.28 svn.r3106 for OlexSys, GUI svn.r4959)
;
_cell_angle_alpha                90
_cell_angle_beta                 89.1480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.9540(7)
_cell_length_b                   9.5826(8)
_cell_length_c                   16.2147(14)
_cell_measurement_reflns_used    6859
_cell_measurement_temperature    300
_cell_measurement_theta_max      26.719
_cell_measurement_theta_min      2.469
_cell_volume                     1235.75(18)
_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      300
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0249
_diffrn_reflns_av_unetI/netI     0.0157
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17910
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.580
_diffrn_reflns_theta_min         2.469
_diffrn_source                   'rotating-anode X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.550
_exptl_absorpt_correction_T_max  0.2439
_exptl_absorpt_correction_T_min  0.0922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/4 (Bruker,2014/4) was used for absorption correction. wR2(int) was 0.0939 before and 0.0350 after correction. The Ratio of minimum to maximum transmission is 0.3780. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.053
_exptl_crystal_description       plate
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     306
_refine_ls_number_reflns         2866
_refine_ls_number_restraints     307
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0404
_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^)+(0.0586P)^2^+1.0998P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1082
_refine_ls_wR_factor_ref         0.1173
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2262
_reflns_number_total             2866
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b00412_si_002.cif
_cod_data_source_block           coronene_TBPA_300K
_cod_database_code               4129312
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.420
_shelx_estimated_absorpt_t_min   0.121
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Shared sites
{Br1, Br1D}
{Br2, Br2D}
3. Restrained distances
 C1A-C7 \\sim C1B-C8
 with sigma of 0.02
 C2A-C8 \\sim C2B-C3
 with sigma of 0.02
 O1A-C7 \\sim O1B-C8
 with sigma of 0.02
 O2A-C8 \\sim O2B-C3
 with sigma of 0.02
 C2A-C7 \\sim C2B-C8
 with sigma of 0.02
 C1A-C8 \\sim C1B-C3
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
Uanis(Br1) = Uanis(Br1D)
Uanis(Br2) = Uanis(Br2D)
5. 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
6. Others
 1*[Sof(C19A)+Sof(C9A)+Sof(H9A)+Sof(C10A)+Sof(H10A)+Sof(C11A)+Sof(H11A)+
 Sof(C12A)+Sof(H12A)+Sof(C13A)+Sof(H13A)+Sof(C14A)+Sof(H14A)+Sof(C15A)+
 Sof(C16A)+Sof(C17A)+Sof(C18A)+Sof(C20A)]+1*[Sof(C19B)+Sof(C9B)+Sof(H9B)+
 Sof(C10B)+Sof(H10B)+Sof(C11B)+Sof(H11B)+Sof(C12B)+Sof(H12B)+Sof(C13B)+
 Sof(H13B)+Sof(C14B)+Sof(H14B)+Sof(C15B)+Sof(C16B)+Sof(C17B)+Sof(C18B)+
 Sof(C20B)]+1*[Sof(C19C)+Sof(C9C)+Sof(H9C)+Sof(C10C)+Sof(H10C)+Sof(C11C)+
 Sof(H11C)+Sof(C12C)+Sof(H12C)+Sof(C13C)+Sof(H13C)+Sof(C14C)+Sof(H14C)+
 Sof(C15C)+Sof(C16C)+Sof(C17C)+Sof(C18C)+Sof(C20C)]=1 with esd of 0.001
 Sof(O3B)=Sof(O1B)=Sof(O2B)=Sof(C1B)=Sof(C2B)=Sof(Br2)=0.5*(1-FVAR(2))
 Sof(O3A)=Sof(O1A)=Sof(O2A)=Sof(C1A)=Sof(C2A)=Sof(Br1)=0.5*FVAR(2)
 Sof(C19A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C12A)=
 Sof(H12A)=Sof(C13A)=Sof(H13A)=Sof(C14A)=Sof(H14A)=Sof(C15A)=Sof(C16A)=
 Sof(C17A)=Sof(C18A)=Sof(C20A)=FVAR(2)
 Sof(C19B)=Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11B)=Sof(C12B)=
 Sof(H12B)=Sof(C13B)=Sof(H13B)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(C16B)=
 Sof(C17B)=Sof(C18B)=Sof(C20B)=FVAR(3)
 Sof(C19C)=Sof(C9C)=Sof(H9C)=Sof(C10C)=Sof(H10C)=Sof(C11C)=Sof(H11C)=Sof(C12C)=
 Sof(H12C)=Sof(C13C)=Sof(H13C)=Sof(C14C)=Sof(H14C)=Sof(C15C)=Sof(C16C)=
 Sof(C17C)=Sof(C18C)=Sof(C20C)=FVAR(4)
 Uiso(O3A)=Uiso(O1A)=Uiso(O2A)=Uiso(C1A)=Uiso(C2A)=Uiso(O3B)=Uiso(O1B)=
 Uiso(O2B)=Uiso(C1B)=Uiso(C2B)=FVAR(5)
 Fixed Sof: Br3(0.5) Br1D(0.5) Br2D(0.5)
7.a Free rotating group:
 O3A(O1A,O2A,C1A,C2A), O3B(O1B,O2B,C1B,C2B), C19A(C9A,C10A,C11A,C12A,C13A,C14A,
 C15A,C16A,C17A,C18A,C20A), C19B(C9B,C10B,C11B,C12B,C13B,C14B,C15B,C16B,C17B,
 C18B,C20B), C19C(C9C,C10C,C11C,C12C,C13C,C14C,C15C,C16C,C17C,C18C,C20C)
7.b Aromatic/amide H refined with riding coordinates:
 C9A(H9A), C10A(H10A), C11A(H11A), C12A(H12A), C13A(H13A), C14A(H14A),
 C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B), C13B(H13B), C14B(H14B), C9C(H9C),
  C10C(H10C), C11C(H11C), C12C(H12C), C13C(H13C), C14C(H14C)
;
_shelx_res_checksum              64579
_shelx_hkl_checksum              31348
_olex2_submission_special_instructions 'No special instructions were received'