Heteroleptic phenoxyimino tin(ii) bis(trimethylsilyl)amides for the synthesis of poly(diester-alt-ethers) from cyclohexene oxide and succinic anhydride
Quek, Timothy; Chumsaeng, Phongnarin; Phomphrai, Khamphee; Dalton Transactions 54 (2025) 5143–5152; doi:10.1039/D4DT03514C

data_7718124
_publ_section_title
;
 Heteroleptic phenoxyimino tin(ii) bis(trimethylsilyl)amides for the
 synthesis of poly(diester-alt-ethers) from cyclohexene oxide and succinic
 anhydride
;
_journal_issue                   12
_journal_name_full               'Dalton Transactions'
_journal_page_first              5143
_journal_page_last               5152
_journal_paper_doi               10.1039/D4DT03514C
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C31 H52 N2 O Si2 Sn'
_chemical_formula_sum            'C31 H52 N2 O Si2 Sn'
_chemical_formula_weight         643.61
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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     dual
_audit_creation_date             2024-02-28
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-21 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.057(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9746(13)
_cell_length_b                   27.777(3)
_cell_length_c                   12.2977(15)
_cell_measurement_reflns_used    9805
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.322
_cell_measurement_theta_min      2.212
_cell_volume                     3407.3(7)
_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)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0847
_diffrn_reflns_av_unetI/netI     0.0467
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            60650
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.551
_diffrn_reflns_theta_min         1.811
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.844
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1240 before and 0.0818 after correction.
The Ratio of minimum to maximum transmission is 0.8898.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_description       plate
_exptl_crystal_F_000             1352
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.183
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.039
_refine_diff_density_max         2.147
_refine_diff_density_min         -1.084
_refine_diff_density_rms         0.143
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.331
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         7850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.331
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0083P)^2^+8.7962P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0755
_refine_ls_wR_factor_ref         0.1104
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5614
_reflns_number_total             7850
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03514c2.cif
_cod_data_source_block           p21c
_cod_depositor_comments
'Adding full bibliography for 7718121--7718126.cif.'
_cod_original_cell_volume        3407.2(7)
_cod_database_code               7718124
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.861
_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:
 C3(H3), C18(H18), C17(H17), C7(H7), C5(H5), C20(H20), C21(H21)
2.b Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C28(H28A,H28B,
 H28C), C31(H31A,H31B,H31C), C27(H27A,H27B,H27C), C13(H13A,H13B,H13C), C25(H25A,
 H25B,H25C), C14(H14A,H14B,H14C), C23(H23A,H23B,H23C), C26(H26A,H26B,H26C),
 C24(H24A,H24B,H24C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              91690
_shelx_hkl_checksum              67874
_olex2_submission_special_instructions 'No special instructions were received'