Bimetallic constrained aluminum alkoxide complexes for ring-opening polymerization of cyclic esters: activity enhancement <i>via</i> cationic activation.
Kanhanond, Narongchai; Chumsaeng, Phongnarin; Namuangruk, Supawadee; Phomphrai, Khamphee; Dalton transactions (Cambridge, England : 2003) 54 (2025) 3246–3255; doi:10.1039/d4dt02849j

data_7717792
_publ_section_title
;
 Bimetallic constrained aluminum alkoxide complexes for ring-opening
 polymerization of cyclic esters: activity enhancement <i>via</i> cationic
 activation.
;
_journal_issue                   8
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3246
_journal_page_last               3255
_journal_paper_doi               10.1039/d4dt02849j
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C74 H106 Al2 N4 O6'
_chemical_formula_sum            'C74 H106 Al2 N4 O6'
_chemical_formula_weight         1201.58
_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             2024-03-27
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-09-27 deposited with the CCDC.	2024-12-27 downloaded from the CCDC.
;
_cell_angle_alpha                84.610(3)
_cell_angle_beta                 68.229(2)
_cell_angle_gamma                60.173(2)
_cell_formula_units_Z            2
_cell_length_a                   14.8016(11)
_cell_length_b                   14.8762(11)
_cell_length_c                   19.8231(14)
_cell_measurement_reflns_used    9751
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      72.12
_cell_measurement_theta_min      2.42
_cell_volume                     3494.3(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_unetI/netI     0.0282
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            107461
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.068
_diffrn_reflns_theta_min         2.415
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.783
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0913 before and 0.0606 after correction.
The Ratio of minimum to maximum transmission is 0.9161.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.142
_exptl_crystal_description       Flake
_exptl_crystal_F_000             1304
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: DCM, Hexane'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.833
_refine_diff_density_min         -0.365
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         13234
_refine_ls_number_restraints     292
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0656
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0812P)^2^+2.9870P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1666
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11813
_reflns_number_total             13234
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt02849j3.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 7717792--7717793.cif.'
_cod_original_cell_volume        3494.3(4)
_cod_database_code               7717792
_shelx_shelxl_version_number     2019/2
_shelx_estimated_absorpt_t_max   0.877
_shelx_estimated_absorpt_t_min   0.735
_olex2_refinement_description
;
1. 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
2. Restrained distances
 C69-C70 \\sim C69A-C70A
 with sigma of 0.02
 C69-C71 \\sim C69A-C71A
 with sigma of 0.02
 C72-C74 \\sim C72A-C74A
 with sigma of 0.02
 C72-C73 \\sim C72A-C73A
 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C71 \\sim C71A \\sim C73 \\sim C73A: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 1.7A
C70 \\sim C70A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C74 \\sim C74A: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
Uanis(C74A) = Uanis(C72A)
Uanis(C71) = Uanis(C69)
5. Others
 Sof(C69A)=Sof(H69A)=Sof(C70A)=Sof(H70D)=Sof(H70E)=Sof(H70F)=Sof(C71A)=
 Sof(H71D)=Sof(H71E)=Sof(H71F)=1-FVAR(1)
 Sof(C69)=Sof(H69)=Sof(C70)=Sof(H70A)=Sof(H70B)=Sof(H70C)=Sof(C71)=Sof(H71A)=
 Sof(H71B)=Sof(H71C)=FVAR(1)
 Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=Sof(C72A)=Sof(H72A)=Sof(C73A)=
 Sof(H73D)=Sof(H73E)=Sof(H73F)=1-FVAR(2)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(H73C)=Sof(C72)=Sof(H72)=Sof(C74)=Sof(H74A)=
 Sof(H74B)=Sof(H74C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C69(H69), C72(H72), C69A(H69A), C72A(H72A)
6.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C21(H21A,H21B), C4(H4A,H4B), C55(H55A,H55B), C22(H22A,H22B),
 C39(H39A,H39B), C56(H56A,H56B), C5(H5A,H5B)
6.c Aromatic/amide H refined with riding coordinates:
 C25(H25), C42(H42), C59(H59), C8(H8)
6.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C28(H28A,H28B,H28C), C32(H32A,H32B,H32C), C51(H51A,H51B,
 H51C), C47(H47A,H47B,H47C), C30(H30A,H30B,H30C), C11(H11A,H11B,H11C), C62(H62A,
 H62B,H62C), C29(H29A,H29B,H29C), C45(H45A,H45B,H45C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C64(H64A,H64B,H64C), C17(H17A,H17B,H17C), C66(H66A,H66B,
 H66C), C63(H63A,H63B,H63C), C67(H67A,H67B,H67C), C16(H16A,H16B,H16C), C50(H50A,
 H50B,H50C), C34(H34A,H34B,H34C), C68(H68A,H68B,H68C), C15(H15A,H15B,H15C),
 C33(H33A,H33B,H33C), C49(H49A,H49B,H49C), C73(H73A,H73B,H73C), C70(H70A,H70B,
 H70C), C74(H74A,H74B,H74C), C71(H71A,H71B,H71C), C70A(H70D,H70E,H70F),
 C71A(H71D,H71E,H71F), C74A(H74D,H74E,H74F), C73A(H73D,H73E,H73F)
;
_shelx_res_checksum              46791
_olex2_submission_special_instructions 'No special instructions were received'