Single-crystal X-ray diffraction and NMR crystallography of a 1:1 cocrystal of dithianon and pyrimethanil
Pöppler, Ann-Christin; Corlett, Emily K.; Pearce, Harriet; Seymour, Mark P.; Reid, Matthew; Montgomery, Mark G.; Brown, Steven P.; Acta Crystallographica Section C 73 (2017) 149–156; doi:10.1107/S2053229617000870

data_2020784
_publ_section_title
;
 Single-crystal X-ray diffraction and NMR crystallography of a 1:1
 cocrystal of dithianon and pyrimethanil
;
_journal_coeditor_code           DF3006
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              149
_journal_page_last               156
_journal_paper_doi               10.1107/S2053229617000870
_journal_volume                  73
_journal_year                    2017
_chemical_formula_iupac          'C14 H4 N2 O2 S2, C12 H13 N3'
_chemical_formula_moiety         'C14 H4 N2 O2 S2, C12 H13 N3'
_chemical_formula_sum            'C26 H17 N5 O2 S2'
_chemical_formula_weight         495.59
_chemical_name_common
;
Dithianon--pyrimethanil (1/1)
;
_chemical_name_systematic
'5,10-Dioxo-5<i>H</i>,10<i>H</i>-naphtho[2,3-<i>b</i>][1,4]dithiine-2,3-dicarbonitrile--4,6-dimethyl-<i>N</i>-phenylpyrimidin-2-amine (1/1)'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     other
_cell_angle_alpha                90
_cell_angle_beta                 97.047(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.1707(2)
_cell_length_b                   22.8006(6)
_cell_length_c                   13.8237(4)
_cell_measurement_reflns_used    2711
_cell_measurement_temperature    100
_cell_measurement_theta_max      62.5720
_cell_measurement_theta_min      5.0250
_cell_volume                     2243.05(11)
_computing_cell_refinement
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_collection
;
CrysAlis PRO (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlis PRO (Agilent, 2014)
;
_computing_molecular_graphics
;
CAMERON (Watkin <i>et al.</i>,  1996) and
Mercury (Macrae <i>et al.</i>,  2006)
;
_computing_publication_material
;
CRYSTALS (Betteridge <i>et al.</i>,  2003)
;
_computing_structure_refinement
;
CRYSTALS (Betteridge <i>et al.</i>,  2003)
;
_computing_structure_solution
;
SUPERFLIP (Palatinus & Chapuis, 2007)
;
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.9781
_diffrn_measured_fraction_theta_max 0.9781
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur Onyx Ultra'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.035
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            5143
_diffrn_reflns_theta_full        58.8557
_diffrn_reflns_theta_max         58.9342
_diffrn_reflns_theta_min         3.2213
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.454
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59641
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Agilent, 2014)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.600
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.37
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9756
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         3141
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.0007021
_refine_ls_shift/su_mean         0.0000978
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
0.138E+04 0.207E+04 0.111E+04 326.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0935
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0935
_reflns_number_gt                2667
_reflns_number_total             3160
_reflns_threshold_expression     I>2.0\s(I)
_cod_data_source_file            df3006sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        2243.04(7)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2020784
_cod_database_fobs_code          2020784