Ternary assembly of pyrazine 2,3-dicarboxylic acid with a ditopic amine
Singh, Abhay Pratap; Baruah, Jubaraj Bikash; CrystEngComm 27 (2025) 4498–4507; doi:10.1039/D5CE00391A

data_7250454
_publ_section_title
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 Ternary assembly of pyrazine 2,3-dicarboxylic acid with a ditopic amine
;
_journal_issue                   26
_journal_name_full               CrystEngComm
_journal_page_first              4498
_journal_page_last               4507
_journal_paper_doi               10.1039/D5CE00391A
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C21 H23 N3, C6 H2 N2 O4, C H4 O, 2(H2 O)'
_chemical_formula_sum            'C28 H33 N5 O7'
_chemical_formula_weight         551.59
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2025-05-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.07.19 svn.r715e62df for OlexSys, GUI svn.r6380)
;
_audit_update_record
;
2025-05-22 deposited with the CCDC.	2025-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                72.607(8)
_cell_angle_beta                 81.828(9)
_cell_angle_gamma                87.451(9)
_cell_formula_units_Z            2
_cell_length_a                   10.504(3)
_cell_length_b                   11.035(3)
_cell_length_c                   12.357(4)
_cell_measurement_reflns_used    9899
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      27.07
_cell_measurement_theta_min      2.19
_cell_volume                     1352.9(7)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      299.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.993
_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  0.0519
_diffrn_reflns_av_unetI/netI     0.0334
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34997
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.115
_diffrn_reflns_theta_min         1.959
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.099
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.5744
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1622 before and 0.0749 after correction.
The Ratio of minimum to maximum transmission is 0.7705.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       Block
_exptl_crystal_F_000             584
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         5932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0813
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0581P)^2^+0.9582P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1456
_refine_ls_wR_factor_ref         0.1629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4570
_reflns_number_total             5932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00391a2.cif
_cod_data_source_block           hanthraimmida_23pyzdc_2h2o_ch3oh
_cod_depositor_comments
'Adding full bibliography for 7250453--7250454.cif.'
_cod_original_cell_volume        1353.0(7)
_cod_database_code               7250454
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,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, All O(H,H) groups
2.a Free rotating group:
 O5(H5C,H5D), O6(H6C,H6D)
2.b Secondary CH2 refined with riding coordinates:
 N3(H3A,H3B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C4(H4A,H4B)
2.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C1(H1A), C2(H2), C3(H3), C10(H10), C11(H11), C12(H12), C13(H13),
 C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C26(H26), C27(H27)
2.d Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C)
2.e Idealised tetrahedral OH refined as rotating group:
 O7(H7)
;
_shelx_res_checksum              23314
_olex2_submission_special_instructions 'No special instructions were received'