Novel melamine – salicylic salt solvates and co-crystals; an analysis of the energetic parameters of the intermolecular hydrogen bonds stabilizing the crystal structure
Wzgarda-Raj, Kinga; Rybarczyk-Pirek, Agnieszka; Wojtulewski, Sławomir; Palusiak, Marcin; CrystEngComm  (2022) –; doi:10.1039/D2CE00684G

data_7245100
_publ_section_title
;
 &#x000D; Novel melamine -- salicylic salt solvates and co-crystals; an
 analysis of the energetic parameters of the intermolecular hydrogen bonds
 stabilizing the crystal structure&#x000D;
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D2CE00684G
_journal_year                    2022
_chemical_formula_moiety         'C7 H5 O3, C3 H7 N6, 0.5(C2 H6 O)'
_chemical_formula_sum            'C11 H15 N6 O3.5'
_chemical_formula_weight         287.29
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-06-23 deposited with the CCDC.	2022-06-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.6800(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.8757(2)
_cell_length_b                   9.57340(10)
_cell_length_c                   18.7224(2)
_cell_measurement_reflns_used    14929
_cell_measurement_temperature    100
_cell_measurement_theta_max      76.2950
_cell_measurement_theta_min      3.4430
_cell_volume                     2611.07(5)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.4052
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31470
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.489
_diffrn_reflns_theta_min         3.472
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.950
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_description       plate
_exptl_crystal_F_000             1208
_exptl_crystal_size_max          0.288
_exptl_crystal_size_mid          0.155
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.219
_refine_diff_density_min         -0.325
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         4806
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0683P)^2^+0.8060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4323
_reflns_number_total             4806
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2ce00684g1.cif
_cod_data_source_block           structure_II
_cod_depositor_comments
;

2024-09-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C22 H30 N12 O7'
_cod_original_formula_weight         574.58
_cod_original_formula_moiety         '2(C7 H5 O3), 2(C3 H7 N6), C2 H6 O'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7245100
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              9737
_shelx_hkl_checksum              18026