Aluminium complexes containing salicylbenzothiazole ligands and their application in the ring-opening polymerisation of rac-lactide and ε-caprolactone
Nakonkhet, Chutakan; Nanok, Tanin; Wattanathana, Worawat; Chuawong, Pitak; Hormnirun, Pimpa; Dalton Trans.  (2017) –; doi:10.1039/C7DT02435E

data_7043720
_publ_section_title
;
 Aluminium complexes containing salicylbenzothiazole ligands and their
 application in the ring-opening polymerisation of rac-lactide and
 \e-caprolactone
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02435E
_journal_year                    2017
_chemical_formula_moiety         'C27 H19 Al N2 O2 S2, 0.5(C7 H8)'
_chemical_formula_sum            'C30.5 H23 Al N2 O2 S2'
_chemical_formula_weight         540.61
_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'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-04-21
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-05-20 deposited with the CCDC.
2017-07-20 downloaded from the CCDC.
;
_cell_angle_alpha                90.0450(10)
_cell_angle_beta                 98.2050(10)
_cell_angle_gamma                94.7900(10)
_cell_formula_units_Z            4
_cell_length_a                   12.8441(6)
_cell_length_b                   13.5123(7)
_cell_length_c                   15.8237(8)
_cell_measurement_reflns_used    9088
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.222
_cell_measurement_theta_min      2.821
_cell_volume                     2708.4(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.988
_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  0.0241
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            46865
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         72.216
_diffrn_reflns_theta_min         4.162
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.344
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.6715
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1309 before and 0.0392 after correction. The Ratio of minimum to maximum transmission is 0.8911. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       block
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         10564
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0350
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0431P)^2^+1.9441P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0896
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10068
_reflns_number_total             10564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02435e2.cif
_cod_data_source_block           1a3_0m
_cod_original_formula_sum        'C30.50 H23 Al N2 O2 S2'
_cod_database_code               7043720
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.799
_shelx_estimated_absorpt_t_min   0.799
_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.a Aromatic/amide H refined with riding coordinates:
 C42(H42), C5(H5), C45(H45), C43(H43), C44(H44), C12(H12), C52(H52), C29(H29),
 C39(H39), C25(H25), C32(H32), C3(H3), C11(H11), C2(H2), C15(H15), C4(H4),
 C24(H24), C18(H18), C9(H9), C30(H30), C23(H23), C22(H22), C31(H31), C10(H10),
 C51(H51), C16(H16), C17(H17), C49(H49), C50(H50), C36(H36), C38(H38), C57(H57),
  C58(H58), C37(H37), C56(H56), C60(H60), C59(H59)
2.b Idealised Me refined as rotating group:
 C27(H27a,H27b,H27c), C54(H54a,H54b,H54c), C61(H61a,H61b,H61c)
;
_olex2_submission_special_instructions 'No special instructions were received'