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_7221842
_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            'C40 H31 Cl I3 N2 S4'
_chemical_formula_weight         1084.06
_chemical_name_systematic
'Bis(R-N-(1-naphthyl)ethylpyrrolo)tetrathiafulvalenetriiodide chlorobenzene solvate 12.I3.PhCl'
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 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                90
_cell_angle_beta                 123.371(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.3842(14)
_cell_length_b                   9.0879(2)
_cell_length_c                   19.4801(9)
_cell_measurement_reflns_used    6624
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.9122
_cell_measurement_theta_min      2.9468
_cell_volume                     3900.8(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET)
(compiled Aug  2 2010,13:00:58)   
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELX-s
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 15.9832
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0174
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_laue_measured_fraction_full 0.983
_diffrn_reflns_laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9095
_diffrn_reflns_point_group_measured_fraction_full 0.725
_diffrn_reflns_point_group_measured_fraction_max 0.624
_diffrn_reflns_theta_full        27.000
_diffrn_reflns_theta_max         28.980
_diffrn_reflns_theta_min         2.953
_exptl_absorpt_coefficient_mu    2.719
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.313
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.846
_exptl_crystal_description       plate
_exptl_crystal_F_000             2100
_exptl_crystal_recrystallization_method electrocrystallisation
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.45
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.871
_refine_diff_density_min         -0.862
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6467
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0325
_refine_ls_R_factor_gt           0.0280
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0376P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0662
_refine_ls_wR_factor_ref         0.0675
_reflns_Friedel_coverage         0.366
_reflns_friedel_fraction_full    0.433
_reflns_friedel_fraction_max     0.356
_reflns_number_gt                5804
_reflns_number_total             6467
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce01430a1.cif
_cod_data_source_block           OU1JWC
_cod_depositor_comments
'Adding full bibliography for 7221839--7221844.cif.'
_cod_database_code               7221842
_shelxl_version_number           2013-4
_shelx_res_checksum              5553