Indium alkoxide complexes supported by constrained Schiff-base ligands for the ring-opening (co)polymerization of cyclic esters
Piyawongsiri, Thitirat; Chumsaeng, Phongnarin; Phomphrai, Khamphee; Dalton Transactions  (2025) –; doi:10.1039/D5DT02356D

data_7719885
_publ_section_title
;
 Indium alkoxide complexes supported by constrained Schiff-base ligands
 for the ring-opening (co)polymerization of cyclic esters
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D5DT02356D
_journal_year                    2025
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C40 H59 In N2 O3'
_chemical_formula_sum            'C40 H59 In N2 O3'
_chemical_formula_weight         730.71
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2025-09-18 deposited with the CCDC.	2025-11-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.0190(3)
_cell_length_b                   17.8022(6)
_cell_length_c                   24.8113(7)
_cell_measurement_reflns_used    9275
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      70.22
_cell_measurement_theta_min      4.34
_cell_volume                     4425.3(2)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0559
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            33547
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.242
_diffrn_reflns_theta_min         3.055
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.510
_exptl_absorpt_correction_T_max  0.7533
_exptl_absorpt_correction_T_min  0.4164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1519 before and 0.1043 after correction.
The Ratio of minimum to maximum transmission is 0.5528.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_description       needle
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.049
_refine_diff_density_max         2.048
_refine_diff_density_min         -1.365
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.305(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     450
_refine_ls_number_reflns         7932
_refine_ls_number_restraints     92
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0729
_refine_ls_R_factor_gt           0.0697
_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^)+(0.0725P)^2^+24.4701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1734
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.756
_reflns_Friedel_fraction_full    0.959
_reflns_Friedel_fraction_max     0.958
_reflns_number_gt                7551
_reflns_number_total             7932
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt02356d2.cif
_cod_data_source_block           p212121
_cod_database_code               7719885
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.301
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.695(17)
 0.305(17)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1-C18 \\sim N1-C18A
 with sigma of 0.02
 N2-C18 \\sim N2-C18A
 with sigma of 0.04
 N1-C19 \\sim N1-C19A
 with sigma of 0.04
 N2-C19 \\sim N2-C19A
 with sigma of 0.02
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
4. Rigid body (RIGU) restrains
 C11, C8, C9, C10
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C38, C37, C39, C40
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 C28, C26, C25, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C15, C16, C14, C17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 N2, C19A, C18A, N1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=1-FVAR(1)
 Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B), C18(H18A,H18B), C5(H5A,H5B), C21(H21A,H21B), C4(H4A,H4B),
 C19(H19A,H19B), C18A(H18C,H18D), C19A(H19C,H19D)
6.b Aromatic/amide H refined with riding coordinates:
 C29(H29), C12(H12)
6.c Idealised Me refined as rotating group:
 C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C17(H17A,H17B,H17C), C15(H15A,H15B,
 H15C), C26(H26A,H26B,H26C), C34(H34A,H34B,H34C), C16(H16A,H16B,H16C), C28(H28A,
 H28B,H28C), C39(H39A,H39B,H39C), C38(H38A,H38B,H38C), C27(H27A,H27B,H27C),
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C40(H40A,H40B,H40C), C11(H11A,H11B,H11C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              74147
_shelx_fab_checksum              4758
_olex2_submission_special_instructions 'No special instructions were received'