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_7718125
_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         'C33 H56 N2 O Si2 Sn'
_chemical_formula_sum            'C33 H56 N2 O Si2 Sn'
_chemical_formula_weight         671.66
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2021-05-21
_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                90
_cell_angle_beta                 99.493(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6210(13)
_cell_length_b                   18.034(2)
_cell_length_c                   18.943(2)
_cell_measurement_reflns_used    9277
_cell_measurement_temperature    100
_cell_measurement_theta_max      30.56
_cell_measurement_theta_min      2.35
_cell_volume                     3578.6(7)
_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 1.000
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker D8 venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_unetI/netI     0.0108
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            233627
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.627
_diffrn_reflns_theta_min         2.066
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.807
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6597
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1486 before and 0.0687 after correction.
The Ratio of minimum to maximum transmission is 0.8842.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_description       rhombic
_exptl_crystal_F_000             1416
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.262
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     399
_refine_ls_number_reflns         11018
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0178
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+1.4195P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10242
_reflns_number_total             11018
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03514c2.cif
_cod_data_source_block           p21_n
_cod_depositor_comments
'Adding full bibliography for 7718121--7718126.cif.'
_cod_original_cell_volume        3578.7(7)
_cod_database_code               7718125
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.942
_shelx_estimated_absorpt_t_min   0.693
_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
 Sof(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(H12D)=Sof(H12E)=
 Sof(H12F)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=1-FVAR(1)
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C12)=Sof(H12A)=Sof(H12B)=Sof(H12C)=
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C23(H23), C22(H22)
3.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C5(H5), C3(H3), C20(H20), C19(H19), C18(H18)
3.c Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C28(H28A,H28B,
 H28C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C26(H26A,H26B,H26C), C27(H27A,
 H27B,H27C), C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C),
 C24(H24A,H24B,H24C), C33(H33A,H33B,H33C), C10(H10A,H10B,H10C), C12(H12A,H12B,
 H12C), C11(H11A,H11B,H11C), C11A(H11D,H11E,H11F), C12A(H12D,H12E,H12F),
 C10A(H10D,H10E,H10F)
;
_shelx_res_checksum              65032
_shelx_hkl_checksum              37240
_olex2_submission_special_instructions 'No special instructions were received'