Bisphthalonitrile with a Disulfide-Based Linker and its Dimethylene Analogue: Comparative Structural Insights
Alpugan, Serkan; Ekineker, Gülçin; Ahsen, Vefa; Berber, Savaş; Önal, Emel; Dumoulin, Fabienne; Crystals 6 (2016) 89–; doi:10.3390/cryst6080089

data_1544035
_publ_section_title
;
 Bisphthalonitrile with a Disulfide-Based Linker and its Dimethylene
 Analogue: Comparative Structural Insights
;
_journal_issue                   8
_journal_name_full               Crystals
_journal_page_first              89
_journal_paper_doi               10.3390/cryst6080089
_journal_volume                  6
_journal_year                    2016
_chemical_formula_moiety         'C20 H14 N4 O2 S2'
_chemical_formula_sum            'C20 H14 N4 O2 S2'
_chemical_formula_weight         406.47
_chemical_name_common            phthalonitrile
_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
_cell_angle_alpha                73.857(3)
_cell_angle_beta                 79.443(4)
_cell_angle_gamma                83.488(3)
_cell_formula_units_Z            1
_cell_length_a                   5.3047(3)
_cell_length_b                   9.4281(5)
_cell_length_c                   10.3733(6)
_cell_measurement_reflns_used    42
_cell_measurement_temperature    299.(2)
_cell_measurement_theta_max      21.7092
_cell_measurement_theta_min      5.0672
_cell_volume                     488.84(5)
_computing_cell_refinement       'APEX2 v2014.11-0 (Bruker AXS)'
_computing_data_collection
'Bruker Instrument Service v2013.12.0.0 (Bruker AXS)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS)'
_computing_molecular_graphics    'MERCURY (Macrae et al., 2006)'
_computing_publication_material
'PLATON V1.16 (Spek, 2009), SHELXTL V6.14 (Bruker AXS)'
_computing_structure_refinement  'SHELXTL V6.14 (Bruker AXS)'
_computing_structure_solution    'SHELXTL V6.14 (Bruker AXS)'
_diffrn_ambient_temperature      299.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type
'Bruker APEX II QUAZAR three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer QUAZAR mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_unetI/netI     0.0309
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7730
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.44
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_type              ImuS
_exptl_absorpt_coefficient_mu    0.296
_exptl_absorpt_correction_T_max  0.97
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             210
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.143
_refine_ls_abs_structure_details
;
Flack x determined using 1405 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.28(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     253
_refine_ls_number_reflns         3697
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0403
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0522P)^2^+0.0507P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                3371
_reflns_number_total             3697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            CCDC-1061336.cif
_cod_data_source_block           I
_cod_database_code               1544035
_shelx_res_checksum              72855
_shelx_hkl_checksum              21038