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_7718126
_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         '2(C28 H43 F3 N2 O Si2 Sn)'
_chemical_formula_sum            'C56 H86 F6 N4 O2 Si4 Sn2'
_chemical_formula_weight         1311.02
_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     iterative
_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                90
_cell_angle_beta                 101.530(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.5900(19)
_cell_length_b                   21.3852(17)
_cell_length_c                   14.0681(13)
_cell_measurement_reflns_used    9748
_cell_measurement_temperature    100
_cell_measurement_theta_max      26.42
_cell_measurement_theta_min      2.38
_cell_volume                     6364.3(10)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0473
_diffrn_reflns_av_unetI/netI     0.0147
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            289330
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.022
_diffrn_reflns_theta_min         1.857
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.918
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6422
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1565 before and 0.0601 after correction.
The Ratio of minimum to maximum transmission is 0.8616.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_description       plate
_exptl_crystal_F_000             2704
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.627
_exptl_crystal_size_mid          0.362
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.727
_refine_diff_density_min         -0.899
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     689
_refine_ls_number_reflns         12556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0243
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0233P)^2^+8.9098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0563
_refine_ls_wR_factor_ref         0.0583
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11446
_reflns_number_total             12556
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03514c2.cif
_cod_data_source_block           p21cmono
_cod_depositor_comments
'Adding full bibliography for 7718121--7718126.cif.'
_cod_database_code               7718126
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.931
_shelx_estimated_absorpt_t_min   0.597
_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. Uiso/Uaniso restraints and constraints
Uanis(F6) = Uanis(F6A) = Uanis(F5) = Uanis(F5A) = Uanis(F4) = Uanis(F4A)
3. Others
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(1)
 Sof(F6)=Sof(F5)=Sof(F4)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C35(H35), C31(H31), C33(H33), C45(H45), C46(H46), C48(H48), C49(H49), C7(H7),
 C5(H5), C3(H3), C21(H21), C20(H20), C18(H18), C17(H17)
4.b Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C), C43(H43A,H43B,H43C), C42(H42A,H42B,H42C), C39(H39A,H39B,
 H39C), C40(H40A,H40B,H40C), C38(H38A,H38B,H38C), C55(H55A,H55B,H55C), C56(H56A,
 H56B,H56C), C54(H54A,H54B,H54C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C),
 C51(H51A,H51B,H51C), C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C27(H27A,H27B,
 H27C), C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C), C10(H10A,
 H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C15(H15A,H15B,H15C),
 C14(H14A,H14B,H14C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              4788
_shelx_hkl_checksum              89070
_olex2_submission_special_instructions 'No special instructions were received'