Supramolecular salts assembled by melamine and two organic hydroxyl acids: synthesis, structure, hydrogen bonds, and luminescent property
Li, Fengcai; Xu, Hao; Xu, Xinwei; Cang, Hui; Xu, Jiaying; Chen, Song; CrystEngComm 23 (2021) 2235–2248; doi:10.1039/D0CE01647K

data_7242200
_publ_section_title
;
 Supramolecular salts assembled by melamine and two organic hydroxyl
 acids: synthesis, structure, hydrogen bonds, and luminescent property
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              2235
_journal_page_last               2248
_journal_paper_doi               10.1039/D0CE01647K
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C11 H7 O3, C3 H7 N6, C3 H7 N O'
_chemical_formula_sum            'C17 H21 N7 O4'
_chemical_formula_weight         387.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-21 deposited with the CCDC.	2021-01-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.150(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.0401(2)
_cell_length_b                   21.0320(8)
_cell_length_c                   12.0394(5)
_cell_measurement_reflns_used    5025
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.282
_cell_measurement_theta_min      2.571
_cell_volume                     1782.64(11)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      110.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.938
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.938
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.298
_diffrn_reflns_theta_min         2.572
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.107
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1408 before and 0.0732 after correction. The Ratio of minimum to maximum transmission is 0.9421. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             816
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         5012
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.1197
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0501P)^2^+0.9017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1435
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3056
_reflns_number_total             5012
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce01647k2.cif
_cod_data_source_block           zz_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7242199--7242200.cif.'
_cod_database_code               7242200
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.995
_shelx_estimated_absorpt_t_min   0.987
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 N7-C16 \\sim N7-C17 \\sim N7-C18 \\sim N7-C19
 with sigma of 0.02
 N7-C15 \\sim N7-C20
 with sigma of 0.02
 O4-C20 \\sim O4-C15
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
Uanis(C20) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C18) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C15(0.85) H15(0.85) C19(0.85) H19A(0.85) H19B(0.85) H19C(0.85)
 C17(0.85) H17A(0.85) H17B(0.85) H17C(0.85) C20(0.15) H20(0.15) C16(0.15)
 H16A(0.15) H16B(0.15) H16C(0.15) C18(0.15) H18A(0.15) H18B(0.15) H18C(0.15)
5.a Aromatic/amide H refined with riding coordinates:
 N3(H3B), C10(H10), C3(H3A), C5(H5), C8(H8), C7(H7), C6(H6), C15(H15), C20(H20)
5.b X=CH2 refined with riding coordinates:
 N5(H5A,H5B), N6(H6A,H6B), N1(H1A,H1B)
5.c Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C)
5.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'