Enhancement of Electron-donating Character in Alkylated Monopyrrolo-tetrathiafultvalene Derivatives
Korsching, Kai R.; Schäfer, Hannes; Schönborn, Josefine; Nimthong-Roldán, Arunpatcha; Zeller, Matthias; Azov, Vladimir A.; RSC Adv.  (2015) –; doi:10.1039/C5RA19012F

data_7222287
_publ_section_title
;
 Enhancement of Electron-donating Character in Alkylated
 Monopyrrolo-tetrathiafultvalene Derivatives
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA19012F
_journal_year                    2015
_chemical_formula_moiety         'C17 H15 N O2 S5'
_chemical_formula_sum            'C17 H15 N O2 S5'
_chemical_formula_weight         425.60
_chemical_melting_point          513
_chemical_name_systematic
11,12-Dimethyl-5-(4-methylbenzenesulfonyl)-2,8,10,13-tetrathia-5-azatricyclo[7.4.0.03,7]trideca-1(9),3,6,11-tetraen
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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
_atom_sites_solution_primary     patt
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-07-24 deposited with the CCDC.
2015-09-23 downloaded from the CCDC.
;
_cell_angle_alpha                107.566(2)
_cell_angle_beta                 103.414(2)
_cell_angle_gamma                92.688(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9673(14)
_cell_length_b                   9.3214(15)
_cell_length_c                   11.9354(19)
_cell_measurement_reflns_used    8553
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.3245
_cell_measurement_theta_min      2.3099
_cell_volume                     917.8(3)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 1998)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrea, 2008)'
_computing_publication_material
;
        SHELXL97 (Sheldrick, 2008)
;
_computing_structure_refinement
;  
SHELXL-2012 (Sheldrick, 2012), 
SHELXLE Rev609 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker AXS Smart Apex CCD Diffractometer'
_diffrn_measurement_method       'Phi and Omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0264
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10464
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.331
_diffrn_reflns_theta_min         2.354
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_correction_T_min  0.6529
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V 2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane/cyclohexane'
_exptl_crystal_size_max          0.550
_exptl_crystal_size_mid          0.520
_exptl_crystal_size_min          0.390
_refine_diff_density_max         0.534
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     230
_refine_ls_number_reflns         5416
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0303
_refine_ls_R_factor_gt           0.0290
_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^)+(0.0459P)^2^+0.4251P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0828
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5133
_reflns_number_total             5416
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ra19012f2.cif
_cod_data_source_block           13RN078_0m
_cod_database_code               7222287
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.719
_shelx_estimated_absorpt_t_max   0.788
_shelx_res_checksum              22633
_shelx_hkl_checksum              56449