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_7718123
_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         'C29 H48 N2 O Si2 Sn'
_chemical_formula_sum            'C29 H48 N2 O Si2 Sn'
_chemical_formula_weight         615.56
_chemical_name_systematic        C29H48ON2Si2Sn
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-22
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-08-21 deposited with the CCDC.	2025-02-24 downloaded from the CCDC.
;
_cell_angle_alpha                100.519(3)
_cell_angle_beta                 103.382(4)
_cell_angle_gamma                105.443(3)
_cell_formula_units_Z            2
_cell_length_a                   10.5871(13)
_cell_length_b                   12.1261(14)
_cell_length_c                   13.7342(17)
_cell_measurement_reflns_used    9369
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.55
_cell_measurement_theta_min      2.97
_cell_volume                     1596.4(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_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  0.0275
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            65884
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.033
_diffrn_reflns_theta_min         2.065
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.898
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6821
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0864 before and 0.0492 after correction.
The Ratio of minimum to maximum transmission is 0.9142.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_description       needle
_exptl_crystal_F_000             644
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.405
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         9325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.115
_refine_ls_R_factor_all          0.0184
_refine_ls_R_factor_gt           0.0172
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0180P)^2^+0.6625P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0455
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8958
_reflns_number_total             9325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03514c2.cif
_cod_data_source_block           p-1_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7718121--7718126.cif.'
_cod_database_code               7718123
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.807
_shelx_estimated_absorpt_t_min   0.744
_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:
 C5(H5), C3(H3), C7(H7), C20(H20), C19(H19), C18(H18)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C11(H11A,H11B,
 H11C), C12(H12A,H12B,H12C), C10(H10A,H10B,H10C), C23(H23A,H23B,H23C), C22(H22A,
 H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C),
 C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_res_checksum              5100
_shelx_hkl_checksum              86123
_olex2_submission_special_instructions 'No special instructions were received'