Exploring intermolecular interactions and energetics in crystalline substituted thieno[2,3-d]pyrimidines
Deb, Pran Kishore; Menon, Anila M.; PSR, Fathima Nida; Shruti, Ipsha; Nidal, Sara; Venugopala, Katharigatta N.; Chopra, Deepak; CrystEngComm 27 (2025) 2070–2085; doi:10.1039/D5CE00071H

data_7250015
_publ_section_title
;
 Exploring intermolecular interactions and energetics in crystalline
 substituted thieno[2,3-d]pyrimidines
;
_journal_issue                   14
_journal_name_full               CrystEngComm
_journal_page_first              2070
_journal_page_last               2085
_journal_paper_doi               10.1039/D5CE00071H
_journal_volume                  27
_journal_year                    2025
_chemical_formula_moiety         'C9 H11 N3 S'
_chemical_formula_sum            'C9 H11 N3 S'
_chemical_formula_weight         193.27
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-01-09
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-01-18 deposited with the CCDC.	2025-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.293(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.2226(5)
_cell_length_b                   7.7209(5)
_cell_length_c                   14.3343(11)
_cell_measurement_reflns_used    9990
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.09
_cell_measurement_theta_min      2.48
_cell_volume                     907.47(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0786
_diffrn_reflns_av_unetI/netI     0.0364
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            32694
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.131
_diffrn_reflns_theta_min         2.850
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9111
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1257 before and 0.0885 after correction.
The Ratio of minimum to maximum transmission is 0.9111.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_description       needle
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.589
_exptl_crystal_size_mid          0.098
_exptl_crystal_size_min          0.048
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.244
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     129
_refine_ls_number_reflns         2650
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_gt           0.0371
_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^)+(0.0550P)^2^+0.2399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0997
_refine_ls_wR_factor_ref         0.1028
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2161
_reflns_number_total             2650
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00071h2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7250012--7250019.cif.'
_cod_database_code               7250015
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.985
_shelx_estimated_absorpt_t_min   0.839
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C)
;
_shelx_res_checksum              6647
_olex2_submission_special_instructions 'No special instructions were received'