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_7221840
_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-phenyl)ethylpyrrolo)tetrathiafulvalenetriiodide  11.I3'
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_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                89.206(5)
_cell_angle_beta                 87.608(3)
_cell_angle_gamma                60.661(5)
_cell_formula_units_Z            6
_cell_length_a                   9.4562(16)
_cell_length_b                   9.5572(14)
_cell_length_c                   53.944(9)
_cell_measurement_reflns_used    6126
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      2.910
_cell_volume                     4246.0(12)
_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-97 (Sheldrick, 1997a)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9.091
_diffrn_measured_fraction_theta_full 0.842
_diffrn_measured_fraction_theta_max 0.825
_diffrn_measurement_device_type
'Bruker-Nonius 95mm CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1058
_diffrn_reflns_av_unetI/netI     0.2212
_diffrn_reflns_laue_measured_fraction_full 0.842
_diffrn_reflns_laue_measured_fraction_max 0.825
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            41220
_diffrn_reflns_point_group_measured_fraction_full 0.672
_diffrn_reflns_point_group_measured_fraction_max 0.650
_diffrn_reflns_theta_full        24.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.288
_exptl_absorpt_coefficient_mu    3.627
_exptl_absorpt_correction_T_max  0.9646
_exptl_absorpt_correction_T_min  0.5025
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.10 (Sheldrick, G.M., 2003)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    2.045
_exptl_crystal_description       Sheet
_exptl_crystal_F_000             2490
_exptl_crystal_recrystallization_method electrocrystallisation
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.034
_refine_diff_density_min         -1.613
_refine_diff_density_rms         0.298
_refine_ls_abs_structure_details
;
 Flack x determined using 3137 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.12(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1891
_refine_ls_number_reflns         19478
_refine_ls_number_restraints     2930
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1848
_refine_ls_R_factor_gt           0.0846
_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^)+165.2835P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1534
_refine_ls_wR_factor_ref         0.1872
_reflns_Friedel_coverage         0.575
_reflns_friedel_fraction_full    0.503
_reflns_friedel_fraction_max     0.475
_reflns_number_gt                10434
_reflns_number_total             19478
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01430a1.cif
_cod_data_source_block           1570post
_cod_depositor_comments
'Adding full bibliography for 7221839--7221844.cif.'
_cod_database_code               7221840
_shelx_estimated_absorpt_t_min   0.502
_shelx_estimated_absorpt_t_max   0.965
_shelxl_version_number           2013-4
_shelx_res_checksum              44605