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_7250016
_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         'C15 H15 N3 S'
_chemical_formula_sum            'C15 H15 N3 S'
_chemical_formula_weight         269.36
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-14
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-23 deposited with the CCDC.	2025-02-25 downloaded from the CCDC.
;
_cell_angle_alpha                86.364(3)
_cell_angle_beta                 69.904(3)
_cell_angle_gamma                88.495(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7760(7)
_cell_length_b                   8.2126(7)
_cell_length_c                   10.8516(10)
_cell_measurement_reflns_used    8992
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.023
_cell_measurement_theta_min      3.746
_cell_volume                     649.49(10)
_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)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.988
_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  0.0514
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            53844
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.110
_diffrn_reflns_theta_min         2.002
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.238
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9506
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1423 before and 0.0586 after correction.
The Ratio of minimum to maximum transmission is 0.9506.
The \l/2 correction factor is Not present.
;
_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    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.195
_exptl_crystal_size_min          0.117
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.319
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3783
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0519P)^2^+0.2885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1002
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3608
_reflns_number_total             3783
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00071h2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7250012--7250019.cif.'
_cod_database_code               7250016
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.923
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C9(H9), C12(H12), C11(H11), C10(H10)
2.c Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C14(H14A,H14B,H14C)
;
_shelx_res_checksum              75936
_olex2_submission_original_sample_id 6
_olex2_submission_special_instructions 'No special instructions were received'