Siloxane-containing derivatives of benzoic acid: chemical transformation of the carboxyl group
Goncharova, Irina K.; Ulianova, Eva A.; Novikov, Roman A.; Volodin, Alexander D.; Korlyukov, Alexander A.; Arzumanyan, Ashot V.; New Journal of Chemistry 46 (2022) 18041–18047; doi:10.1039/D2NJ03872B

data_7061782
_publ_section_title
;
 Siloxane-containing derivatives of benzoic acid: chemical transformation
 of the carboxyl group
;
_journal_issue                   37
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              18041
_journal_page_last               18047
_journal_paper_doi               10.1039/D2NJ03872B
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C20 H28 N2 O3 Si2, C10 H15 N O2 Si'
_chemical_formula_sum            'C30 H43 N3 O5 Si3'
_chemical_formula_weight         609.94
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-08-27
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-08-27 deposited with the CCDC.	2022-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.806(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6295(8)
_cell_length_b                   14.8131(8)
_cell_length_c                   17.2611(9)
_cell_measurement_reflns_used    4391
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.848
_cell_measurement_theta_min      2.333
_cell_volume                     3278.8(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_collection       'APEX3 v2019.11-0 (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.00
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'APEX QUEST'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.0827
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            20592
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.861
_exptl_absorpt_coefficient_mu    0.186
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1063 before and 0.0658 after correction.
The Ratio of minimum to maximum transmission is 0.7392.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       block
_exptl_crystal_F_000             1304
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.217
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         6426
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.1534
_refine_ls_R_factor_gt           0.1288
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0002P)^2^+37.1785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2798
_refine_ls_wR_factor_ref         0.2902
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4962
_reflns_number_total             6426
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03872b4.cif
_cod_data_source_block           ye105
_cod_depositor_comments
'Adding full bibliography for 7061778--7061786.cif.'
_cod_database_code               7061782
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.959
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C27) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
3. Others
 Fixed Sof: C27A(0.5) H27A(0.5) C14(0.5) H14(0.5) C15A(0.5) H15A(0.5) C9A(0.5)
 H9A(0.5) C6A(0.5) H6A(0.5) C28A(0.5) H28A(0.5) C27(0.5) H27(0.5) C25(0.5)
 H25(0.5) C10(0.5) H10(0.5) C25A(0.5) H25A(0.5) C24(0.5) H24(0.5) C9(0.5)
 H9(0.5) C24A(0.5) H24A(0.5) C17(0.5) H17(0.5) C18A(0.5) H18A(0.5) C18(0.5)
 H18(0.5) C15(0.5) H15(0.5) C10A(0.5) H10A(0.5) C7(0.5) H7(0.5) C17A(0.5)
 H17A(0.5) C14A(0.5) H14A(0.5) C28(0.5) H28(0.5) C7A(0.5) H7A(0.5) C6(0.5)
 H6(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N3(H3), N1(H1), C27A(H27A), C14(H14), C15A(H15A), C9A(H9A), C6A(H6A),
 C28A(H28A), C27(H27), C25(H25), C10(H10), C25A(H25A), C24(H24), C9(H9),
 C24A(H24A), C17(H17), C18A(H18A), C18(H18), C15(H15), C10A(H10A), C7(H7),
 C17A(H17A), C14A(H14A), C28(H28), C7A(H7A), C6(H6)
4.b Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C2(H2A,H2B,H2C), C20(H20A,H20B,H20C), C30(H30A,H30B,
 H30C), C22(H22A,H22B,H22C), C3(H3A,H3B,H3C), C21(H21A,H21B,H21C), C1(H1A,H1B,
 H1C), C4(H4A,H4B,H4C)
4.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_shelx_res_checksum              25307
_olex2_submission_special_instructions 'No special instructions were received'