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_7061778
_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         'C22 H32 N2 O3 Si2'
_chemical_formula_sum            'C22 H32 N2 O3 Si2'
_chemical_formula_weight         428.67
_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
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;
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
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_cell_angle_gamma                90
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_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD area detector'
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_diffrn_measured_fraction_theta_full 0.999
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_diffrn_measurement_device
'Rayonix SX 165 area detector and Marexperts dtb goniostat'
_diffrn_measurement_device_type  'Marexperts dtb goniostat'
_diffrn_measurement_method       '/f scans'
_diffrn_radiation_monochromator  'Silicon 111'
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_diffrn_reflns_av_R_equivalents  0.1065
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_diffrn_reflns_Laue_measured_fraction_full 0.999
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_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7991
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_source                   synchrotron
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'Belok station, Kurchatov Center for Synchrotron Radiation and Nanotechnology, Moscow'
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_exptl_crystal_colour            colourless
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_exptl_crystal_description       prism
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_exptl_crystal_size_mid          0.05
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.1119
_refine_ls_R_factor_gt           0.0721
_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^)+(0.0767P)^2^+0.9681P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1572
_refine_ls_wR_factor_ref         0.1772
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1580
_reflns_number_total             2342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2nj03872b4.cif
_cod_data_source_block           108
_cod_depositor_comments
'Adding full bibliography for 7061778--7061786.cif.'
_cod_database_code               7061778
_shelxl_version_number           2014/6
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.986
_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. Others
 Fixed Sof: O1(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6)
3.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              58907
_olex2_submission_special_instructions 'No special instructions were received'