Bis(melaminium) <small>DL</small>-malate tetrahydrate
Jan Janczak; Genivaldo Julio Perpétuo; Acta Crystallographica Section C 59 (2003) o349–o352; doi:10.1107/S0108270103010047

data_2013336
_publ_section_title
;
 Bis(melaminium) <small>DL</small>-malate tetrahydrate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o349
_journal_page_last               o352
_journal_paper_doi               10.1107/S0108270103010047
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '2C3 H7 N6 1+, C4 H4 O5 2-, 4H2 O'
_chemical_formula_moiety         '2C3 H7 N6 1+, C4 H4 O5 2-, 4H2 O'
_chemical_formula_sum            'C10 H26 N12 O9'
_chemical_formula_weight         458.43
_chemical_melting_point          decomposition
_chemical_name_common
;
Bis(melaminium) DL-malate tetrahydrate'
;
_chemical_name_systematic
;
Bis(1,3,5-triamine-2,4,6-trianine-1-ium) DL-malate tetrahydrate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 110.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   26.533(5)
_cell_length_b                   12.297(2)
_cell_length_c                   13.079(3)
_cell_measurement_reflns_used    3878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      3.16
_cell_volume                     4010.0(16)
_computing_cell_refinement
;
KM-4 Software
;
_computing_data_collection
;
KM-4 Software (Kuma, 2000)
;
_computing_data_reduction
;
KM-4 Software
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1990)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2'
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       '\w scan'
_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  0.0336
_diffrn_reflns_av_sigmaI/netI    0.0364
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15560
_diffrn_reflns_theta_full        28.39
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         3.16
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.9681
_exptl_absorpt_correction_T_min  0.9614
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
face-indexed, SHEXLTL (Sheldrick, 1990)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_meas      1.52
_exptl_crystal_density_method    floatation
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1936
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.362
_refine_diff_density_min         -0.276
_refine_ls_extinction_coef       0.000227(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4986
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0061P)^2^+0.0402P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0324
_refine_ls_wR_factor_ref         0.0410
_reflns_number_gt                3878
_reflns_number_total             4986
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1613.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2013336
_cod_database_fobs_code          2013336