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_7060605
_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 O4 S Si'
_chemical_formula_sum            'C15 H20 N2 O4 S Si'
_chemical_formula_weight         352.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     direct
_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
_cell_angle_beta                 95.94(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.937(8)
_cell_length_b                   7.336(4)
_cell_length_c                   15.771(8)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.59
_cell_volume                     1603.8(15)
_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 0.9966
_diffrn_measured_fraction_theta_max 0.9966
_diffrn_measurement_device_type  'Bruker D8 VENTURE PHOTON 100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            49417
_diffrn_reflns_theta_full        27.9972
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.7065
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0919 before and 0.0622 after correction.
The Ratio of minimum to maximum transmission is 0.9471.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.4598
_exptl_crystal_description       prism
_exptl_crystal_F_000             745.1559
_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.138
_refine_diff_density_max         0.3560
_refine_diff_density_min         -0.2854
_refine_diff_density_rms         0.0580
_refine_ls_d_res_high            0.7570
_refine_ls_d_res_low             7.8431
_refine_ls_goodness_of_fit_ref   1.0563
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    32
_refine_ls_number_parameters     208
_refine_ls_number_reflns         3854
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0563
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0285
_refine_ls_shift/su_max          0.0004
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0345P)^2^+0.9123P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0772
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -18
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              20
_reflns_limit_l_min              -12
_reflns_number_gt                3472
_reflns_number_total             3854
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d1nj00793a2.cif
_cod_data_source_block           1c
_cod_depositor_comments
'Adding full bibliography for 7060605--7060606.cif.'
_cod_original_cell_volume        1603.7(15)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7060605
_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:
 C1(H1a,H1b), C15(H15a,H15b), C14(H14a,H14b), C2(H2a,H2b), C5(H5a,H5b), C4(H4a,
 H4b), C6(H6a,H6b), C3(H3a,H3b)
2.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13)
;
_olex2_submission_special_instructions 'No special instructions were received'