Dithioether ligands containing a 2,6-disubstituted pyridine linker with two thioether-heterocycle arms
Rotondo, Archimede; Bruno, Giuseppe; Nicoló, Francesco; Tresoldi, Giuseppe; Di Pietro, Santo; Acta Crystallographica Section C 66 (2010) o15–o19; doi:10.1107/S0108270109051543

data_2017480
_publ_section_title
;
 Dithioether ligands containing a 2,6-disubstituted pyridine linker
 with two thioether-heterocycle arms
;
_journal_coeditor_code           KU3018
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o15
_journal_page_last               o19
_journal_paper_doi               10.1107/S0108270109051543
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C17 H15 N3 S2'
_chemical_formula_moiety         'C17 H15 N3 S2'
_chemical_formula_sum            'C17 H15 N3 S2'
_chemical_formula_weight         325.44
_chemical_name_systematic
;
2,6-bis(2-pyridylthiomethyl)pyridine
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 110.39(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6960(10)
_cell_length_b                   9.2810(10)
_cell_length_c                   16.7410(10)
_cell_measurement_reflns_used    9457
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.61
_cell_measurement_theta_min      2.55
_cell_volume                     1557.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'APEX2 (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics
;
XP (Bruker, 2007), ORTEP-3 for Windows (Farrugia, 1997) and
Mercury
(Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
WinGX (Farrugia, 1999), PARST (Nardelli, 1995), enCIFer (Allen
<i>et al.</i>,  2004)
and PLATON (Spek, 2009)
;
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            46596
_diffrn_reflns_theta_full        26.36
_diffrn_reflns_theta_max         26.36
_diffrn_reflns_theta_min         2.55
_exptl_absorpt_coefficient_mu    0.341
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.856
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.388
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             680
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.261
_refine_ls_extinction_coef       0.0249(13)
_refine_ls_extinction_method     'SHELXL97 (Sheldrick, 2008)'
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     200
_refine_ls_number_reflns         3188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.08
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0282
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0370P)^2^+0.4485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0804
_reflns_number_gt                2886
_reflns_number_total             3188
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ku3018.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               2017480
_cod_database_fobs_code          2017480