The synthesis, characterization, and theoretical analysis of novel Si-substituted silylethyl derivatives of 2-mercaptobenzoxazole and 2-mercaptobenzothiazole
Trofimova, Olga; Grebneva, Ekaterina; Bolgova, Yuliya; Belogolova, Elena; Emel’yanov, Artem; Albanov, Alexander; Borodina, Tat’yana; Ivanova, Anastasiya; Korzhova, Svetlana; Pozdnyakov, Alexander; New Journal of Chemistry 45 (2021) 9416–9426; doi:10.1039/D1NJ00793A

data_7060606
_publ_section_title
;
 The synthesis, characterization, and theoretical analysis of novel
 Si-substituted silylethyl derivatives of 2-mercaptobenzoxazole and
 2-mercaptobenzothiazole
;
_journal_issue                   21
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              9416
_journal_page_last               9426
_journal_paper_doi               10.1039/D1NJ00793A
_journal_volume                  45
_journal_year                    2021
_chemical_formula_moiety         'C15 H20 N2 O3 S2 Si'
_chemical_formula_sum            'C15 H20 N2 O3 S2 Si'
_chemical_formula_weight         368.54
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2021-04-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-04-16 deposited with the CCDC.	2021-04-21 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.361(16)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.187(5)
_cell_length_b                   10.587(4)
_cell_length_c                   13.213(5)
_cell_measurement_reflns_used    9731
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.05
_cell_measurement_theta_min      3.09
_cell_volume                     1638.3(11)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      293.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Bruker APEX2'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0295
_diffrn_reflns_av_unetI/netI     0.0130
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            47504
_diffrn_reflns_theta_full        27.99
_diffrn_reflns_theta_max         27.99
_diffrn_reflns_theta_min         2.59
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.414
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6681
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0902 before and 0.0478 after correction.
The Ratio of minimum to maximum transmission is 0.8956.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedron
_exptl_crystal_F_000             776
_exptl_crystal_size_max          0.428
_exptl_crystal_size_mid          0.337
_exptl_crystal_size_min          0.239
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.280
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3929
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0253
_refine_ls_R_factor_gt           0.0239
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0288P)^2^+1.0236P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0638
_reflns_number_gt                3715
_reflns_number_total             3929
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d1nj00793a2.cif
_cod_data_source_block           2c
_cod_depositor_comments
'Adding full bibliography for 7060605--7060606.cif.'
_cod_original_cell_volume        1638.4(10)
_cod_database_code               7060606
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C3(H3A,H3B), C6(H6A,H6B), C5(H5A,H5B), C2(H2A,
 H2B), C1(H1A,H1B), C4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C10(H10), C13(H13), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'