5,8-Bis[bis(pyridin-2-yl)amino]-1,3,4,6,7,9,9b-heptaazaphenalen-2(1<i>H</i>)-one dimethyl sulfoxide monosolvate dihydrate
Schwarzer, Anke; Kroke, Edwin; Acta Crystallographica Section E 70 (2014) o456–o457; doi:10.1107/S1600536814005698

data_2239244
_publ_section_title
;
 5,8-Bis[bis(pyridin-2-yl)amino]-1,3,4,6,7,9,9b-heptaazaphenalen-2(1<i>H</i>)-one
 dimethyl sulfoxide monosolvate dihydrate
;
_journal_coeditor_code           SU2711
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o456
_journal_page_last               o457
_journal_paper_doi               10.1107/S1600536814005698
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          'C26 H17 N13 O, C2 H6 O S, 2H2 O'
_chemical_formula_moiety         'C26 H17 N13 O, C2 H6 O S, 2(H2 O)'
_chemical_formula_sum            'C28 H27 N13 O4 S'
_chemical_formula_weight         641.69
_chemical_name_common
;
5,8-Bis(dipyridin-2-ylamino)-<i>s</i>-heptazin-2-one dimethyl sulfoxide
monosolvate dihydrate
;
_chemical_name_systematic
'5,8-Bis[bis(pyridin-2-yl)amino]-1,3,4,6,7,9,9b-heptaazaphenalen-2(1<i>H</i>)-one dimethyl sulfoxide monosolvate dihydrate'
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.4880(10)
_cell_angle_beta                 86.5370(10)
_cell_angle_gamma                86.6930(10)
_cell_formula_units_Z            2
_cell_length_a                   10.6534(2)
_cell_length_b                   11.6791(2)
_cell_length_c                   12.5591(2)
_cell_measurement_reflns_used    852
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.18
_cell_measurement_theta_min      2.53
_cell_volume                     1450.06(4)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0415
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22692
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.54
_exptl_absorpt_coefficient_mu    0.173
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.439
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         5662
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.967
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0393
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+0.3491P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1152
_reflns_number_gt                4333
_reflns_number_total             5662
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            su2711sup1.cif
_cod_data_source_block           I
_cod_database_code               2239244
_cod_database_fobs_code          2239244