Hydrogen-bonded supramolecular structures in co-crystals of ??- or ??-diketone enols with 2,6-diaminopyridine or 2,4-diaminopyrimidine
Bertolasi, Valerio; Pretto, Loretta; Gilli, Paola; Ferretti, Valeria; Gilli, Gastone; New Journal of Chemistry 26 (2002) 1559–; doi:10.1039/b205705k

data_7050970
_publ_section_title
;
 Hydrogen-bonded supramolecular structures in co-crystals of ??- or
 ??-diketone enols with 2,6-diaminopyridine or 2,4-diaminopyrimidine
;
_journal_issue                   11
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1559
_journal_paper_doi               10.1039/b205705k
_journal_volume                  26
_journal_year                    2002
_chemical_formula_moiety         'C7 H10 O2, (C7 H9 O2)-, (C5 H8 N3)+'
_chemical_formula_sum            'C19 H27 N3 O4'
_chemical_formula_weight         361.44
_chemical_name_systematic
;
5-Methyl-1,3-cyclohexanedionate, 2,6-diaminopyridinium,
5-methyl-1,3-cyclohexanedione enol
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.420(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.474(2)
_cell_length_b                   5.270(2)
_cell_length_c                   22.478(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      ?12
_cell_measurement_theta_min      7
_cell_volume                     1939.9(8)
_computing_cell_refinement       'CAD4 Enraf-Nonius, 1984'
_computing_data_collection       'CAD4 Enraf-Nonius, 1984'
_computing_data_reduction        'MolEN (Fair, Enraf-Nonius, 1990)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material
;
SHELXL-97 (Sheldrick, 1997), PARST (Nardelli, 1995)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      296
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_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  0.022
_diffrn_reflns_av_sigmaI/netI    0.0723
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            4348
_diffrn_reflns_theta_full        27.01
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.234
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         4231
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1412
_refine_ls_R_factor_gt           0.0622
_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^)+(0.0865P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1450
_refine_ls_wR_factor_ref         0.1739
_reflns_number_gt                2124
_reflns_number_total             4231
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            b205705k.txt
_cod_data_source_block           (4)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' tag value 'Mononlinic' was replaced with
'monoclinic' value as specified in the replacement file
'/home/robertas/cod-tools/perl-scripts/inputs/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 2/c'
_cod_database_code               7050970