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_7250013
_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         'C19 H21 N3 O S'
_chemical_formula_sum            'C19 H21 N3 O S'
_chemical_formula_weight         339.45
_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             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                90
_cell_angle_beta                 94.478(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.1073(11)
_cell_length_b                   13.0293(10)
_cell_length_c                   9.4999(8)
_cell_measurement_reflns_used    9499
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      30.100
_cell_measurement_theta_min      2.131
_cell_volume                     1740.8(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0932
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            61428
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.100
_diffrn_reflns_theta_min         2.131
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.196
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7457
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1828 before and 0.0789 after correction.
The Ratio of minimum to maximum transmission is 0.7457.
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    1.295
_exptl_crystal_description       needle
_exptl_crystal_F_000             720
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.043
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         5111
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0448P)^2^+0.7565P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1110
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3884
_reflns_number_total             5111
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5ce00071h2.cif
_cod_data_source_block           9
_cod_depositor_comments
'Adding full bibliography for 7250012--7250019.cif.'
_cod_database_code               7250013
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.992
_shelx_estimated_absorpt_t_min   0.892
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C12(H12), C8(H8), C9(H9), C11(H11), C10(H10)
2.b Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C16(H16A,H16B,
 H16C), C17(H17A,H17B,H17C)
;
_shelx_res_checksum              4907
_olex2_submission_original_sample_id 9
_olex2_submission_special_instructions 'No special instructions were received'