Contrasting crystal packing arrangements in triiodide salts of radical cations of chiral bis(pyrrolo[3,4-d])tetrathiafulvalenes
Martin, Lee; Yang, Songjie; Brooks, Andrew C.; Horton, Peter N.; Male, Louise; Moulfi, Ourida; Harmand, Lydie; Day, Peter; Clegg, William; Harrington, Ross W.; Wallis, John D.; CrystEngComm 17 (2015) 7354–; doi:10.1039/C5CE01430A

data_7221844
_publ_section_title
;
 Contrasting crystal packing arrangements in triiodide salts of radical
 cations of chiral bis(pyrrolo[3,4-d])tetrathiafulvalenes
;
_journal_issue                   38
_journal_name_full               CrystEngComm
_journal_page_first              7354
_journal_paper_doi               10.1039/C5CE01430A
_journal_volume                  17
_journal_year                    2015
_chemical_absolute_configuration ad
_chemical_formula_sum            'C26 H22 I3 N2 S4'
_chemical_formula_weight         871.39
_chemical_name_systematic
'Bis(S-N-(1-phenylethyl)-2,5-dihydropyrrolo)tetrathiafulvalene triiodide 13.I3'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2015-07-19 deposited with the CCDC.
2015-08-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   9.484(10)
_cell_length_b                   19.551(14)
_cell_length_c                   30.639(3)
_cell_measurement_temperature    120(2)
_cell_volume                     5681(7)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXs
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.923
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type
;
Bruker-Nonius APEX II CCD camera on \k-goniostat
;
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1394
_diffrn_reflns_av_unetI/netI     0.2841
_diffrn_reflns_laue_measured_fraction_full 0.923
_diffrn_reflns_laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            23205
_diffrn_reflns_point_group_measured_fraction_full 0.848
_diffrn_reflns_point_group_measured_fraction_max 0.771
_diffrn_reflns_theta_full        23.000
_diffrn_reflns_theta_max         27.873
_diffrn_reflns_theta_min         2.931
_exptl_absorpt_coefficient_mu    3.615
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    2.038
_exptl_crystal_description       'cut needles'
_exptl_crystal_F_000             3320
_exptl_crystal_recrystallization_method electrocrystallisation
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.050
_refine_diff_density_min         -1.848
_refine_diff_density_rms         0.354
_refine_ls_abs_structure_details
;
 Flack x determined using 1233 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.12(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         10456
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.2909
_refine_ls_R_factor_gt           0.1588
_refine_ls_shift/su_max          0.336
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+595.3403P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2564
_refine_ls_wR_factor_ref         0.3222
_reflns_Friedel_coverage         0.630
_reflns_friedel_fraction_full    0.753
_reflns_friedel_fraction_max     0.665
_reflns_number_gt                4940
_reflns_number_total             10456
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01430a1.cif
_cod_data_source_block           castle
_cod_depositor_comments
'Adding full bibliography for 7221839--7221844.cif.'
_cod_database_code               7221844
_shelxl_version_number           2013-4
_shelx_res_checksum              10369