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_2017482
_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 H17 N5 S2 , 0.5C5 H12'
_chemical_formula_moiety         'C17 H17 N5 S2 , 0.5C5 H12'
_chemical_formula_sum            'C19.5 H23 N5 S2'
_chemical_formula_weight         391.57
_chemical_name_systematic
;
2,6-bis(4-methyl-2-pyrimidylthiomethyl)pyridine n-pentane hemisolvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                95.910(10)
_cell_angle_beta                 99.800(10)
_cell_angle_gamma                97.310(10)
_cell_formula_units_Z            2
_cell_length_a                   7.4070(10)
_cell_length_b                   11.1000(10)
_cell_length_c                   12.4280(10)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      2.66
_cell_volume                     990.56(19)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.052
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            33717
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.283
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.898
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2007)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       laminar
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.392
_refine_diff_density_min         -0.517
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     264
_refine_ls_number_reflns         3758
_refine_ls_number_restraints     40
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0505
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0726P)^2^+0.4726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1349
_reflns_number_gt                3265
_reflns_number_total             3758
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ku3018.cif
_cod_data_source_block           III
_cod_original_cell_volume        990.6(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2017482
_cod_database_fobs_code          2017482