Coordinating Effect in Ring-opening Polymerization of ε-Caprolactone Using Aluminum Complexes Bearing Bisphenolate as Catalysts
Chen, Hsing-Yin; Lee, Ying Hsien; Chiang, Michael, Y.; Lu, Wei-Yi; Tseng, Hsi-Ching; Chen, Yu-Hsieh; Lai, Yi-Chun; Lin, Chu-Chieh; Chen, Hsuan-Ying; RSC Adv.  (2015) –; doi:10.1039/C5RA10753A

data_7222143
_publ_section_title
;
 Coordinating Effect in Ring-opening Polymerization of \e-Caprolactone
 Using Aluminum Complexes Bearing Bisphenolate as Catalysts
;
_journal_name_full               'RSC Adv.'
_journal_paper_doi               10.1039/C5RA10753A
_journal_year                    2015
_chemical_formula_moiety         'C78 H106 Al2 O8, 2(O1 C4 H8)'
_chemical_formula_sum            'C86 H122 Al2 O10'
_chemical_formula_weight         1369.80
_chemical_name_common            aloophohme
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/cc13n1d6
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-09-03 deposited with the CCDC.
2015-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 126.648(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   34.0176(19)
_cell_length_b                   14.8864(4)
_cell_length_c                   22.9056(12)
_cell_measurement_reflns_used    7044
_cell_measurement_temperature    150.00(14)
_cell_measurement_theta_max      29.1884
_cell_measurement_theta_min      2.8435
_cell_volume                     9306.4(12)
_computing_cell_refinement
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_computing_data_collection
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_computing_data_reduction
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.00(14)
_diffrn_detector_area_resol_mean 16.0690
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_sigmaI/netI    0.0557
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            45262
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    0.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) 
(compiled Jan 23 2012,18:06:46) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       crystal
_exptl_crystal_F_000             2976
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_platon_squeeze_details
; 
The reaction was set in THF and 1H NMR 
spectrum revealed that THF was observed 
in the crystal. The voids in the SQUEEZE 
loop should be occupies by THF. 
;
_refine_diff_density_max         0.917
_refine_diff_density_min         -0.276
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         9129
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0783
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1599P)^2^+5.6017P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2330
_refine_ls_wR_factor_ref         0.2563
_reflns_number_gt                6242
_reflns_number_total             9129
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5ra10753a2.cif
_cod_data_source_block           aloophohme
_cod_original_cell_volume        9306.4(8)
_cod_database_code               7222143