Probing Atomistic Behavior To Unravel Dielectric Phenomena in Charge Transfer Cocrystals
Bhowal, Rohit; Balaraman, Anina Anju; Ghosh, Manasi; Dutta, Soma; Dey, Krishna Kishor; Chopra, Deepak; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11459

data_4135452
_publ_section_title
;
 Probing Atomistic Behavior To Unravel Dielectric Phenomena in Charge
 Transfer Cocrystals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11459
_journal_year                    2020
_chemical_formula_moiety         'C24 H21 N3, C12 H5 N O5'
_chemical_formula_sum            'C36 H26 N4 O5'
_chemical_formula_weight         594.61
_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   mixed
_audit_creation_date             2020-10-21
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                90
_cell_angle_beta                 100.908(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.030(3)
_cell_length_b                   7.6625(9)
_cell_length_c                   25.365(4)
_cell_measurement_reflns_used    470
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      12.41
_cell_measurement_theta_min      2.76
_cell_volume                     2868.4(8)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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  0.3936
_diffrn_reflns_av_unetI/netI     0.8650
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            35113
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.264
_diffrn_reflns_theta_min         1.635
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6281
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1062 before and 0.0749 after correction.
The Ratio of minimum to maximum transmission is 0.8420.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       needle
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       0.026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         8450
_refine_ls_number_restraints     151
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.5832
_refine_ls_R_factor_gt           0.1698
_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^)+(0.0764P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2369
_refine_ls_wR_factor_ref         0.3806
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1425
_reflns_number_total             8450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CC1_300K.cif
_cod_data_source_block           cc1_300k
_cod_original_cell_volume        2868.5(8)
_cod_database_code               4135452
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.977
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
2. Shared sites
{C1, C10B}
{C2, C11B}
{H2, H11B}
{C3, C12B}
{H3, H12B}
{C4, C7B}
{C5, C6B}
{O3, O5B}
{O4, O4B}
{C6, C5B}
{O5, O3B}
{C7, C4B}
{C12, C3B}
{H12, H3BA}
{C11, C2B}
{H11, H2BA}
{C10, C1B}
{C9, C9B}
{C8, C8B}
3. Restrained distances
 N1B-C1B
 1.517 with sigma of 0.01
4. Uiso/Uaniso restraints and constraints
O4 \\sim O3 \\sim O5 \\sim C7 \\sim C8 \\sim C4 \\sim C9 \\sim C6 \\sim C1
\\sim C10 \\sim C12 \\sim C3 \\sim C5 \\sim C11 \\sim C2 \\sim O1 \\sim N1
\\sim O2 \\sim O1B \\sim N1B \\sim O2B: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
Uanis(C1) = Uanis(C1B)
Uanis(C1) = Uanis(C2B)
Uanis(C3) = Uanis(C3B)
Uanis(C4) = Uanis(C4B)
Uanis(C8) = Uanis(C8B)
Uanis(C7) = Uanis(C7B)
Uanis(C12) = Uanis(C12B)
Uanis(C11) = Uanis(C11B)
Uanis(C10) = Uanis(C10B)
Uanis(C9) = Uanis(C9B)
Uanis(O4) = Uanis(O4B)
Uanis(O3) = Uanis(O3B)
Uanis(O5) = Uanis(O5B)
5. Others
 Sof(O1B)=Sof(N1B)=Sof(O2B)=Sof(C1B)=Sof(C2B)=Sof(H2BA)=Sof(C3B)=Sof(H3BA)=
 Sof(C4B)=Sof(C5B)=Sof(O3B)=Sof(O4B)=Sof(C6B)=Sof(O5B)=Sof(C7B)=Sof(C12B)=
 Sof(H12B)=Sof(C11B)=Sof(H11B)=Sof(C10B)=Sof(H10B)=Sof(C9B)=Sof(C8B)=1-FVAR(1)
 Sof(O1)=Sof(N1)=Sof(O2)=Sof(C1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3)=Sof(C4)=
 Sof(C5)=Sof(O3)=Sof(O4)=Sof(C6)=Sof(O5)=Sof(C7)=Sof(C12)=Sof(H12)=Sof(C11)=
 Sof(H11)=Sof(C10)=Sof(H10)=Sof(C9)=Sof(C8)=FVAR(1)
6.a Rotating group:
 N4(H4A,H4B), N2(H2A,H2B), N3(H3A,H3B)
6.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C16(H16), C36(H36), C24(H24), C18(H18), C32(H32), C30(H30),
 C33(H33), C35(H35), C23(H23), C29(H29), C26(H26), C21(H21), C14(H14), C27(H27),
  C2(H2), C3(H3), C12(H12), C11(H11), C10(H10), C2B(H2BA), C3B(H3BA),
 C12B(H12B), C11B(H11B), C10B(H10B)
;
_shelx_res_checksum              15213
_shelx_hkl_checksum              63683
_olex2_submission_special_instructions 'No special instructions were received'