Thermo-enhanced ring-opening polymerization of ε-caprolactone: The synthesis, characterization and catalytic behavior of aluminum hydroquinolin-8-olates
Zhang, Qiurui; Zhang, Wenjuan; Rajendran, Natesan Mannangatti; Liang, Tongling; Sun, Wen Hua; Dalton Trans.  (2017) –; doi:10.1039/C7DT01720K

data_7043121
_publ_section_title
;
 Thermo-enhanced ring-opening polymerization of \e-caprolactone: The
 synthesis, characterization and catalytic behavior of aluminum
 hydroquinolin-8-olates
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT01720K
_journal_year                    2017
_chemical_formula_moiety         'C22 H30 Al2 Cl2 N2 O2'
_chemical_formula_sum            'C22 H30 Al2 Cl2 N2 O2'
_chemical_formula_weight         479.34
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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_creation_date             2016-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2017-04-01 deposited with the CCDC.
2017-05-25 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.11(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.829(3)
_cell_length_b                   9.976(2)
_cell_length_c                   17.574(4)
_cell_measurement_reflns_used    4271
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4839
_cell_measurement_theta_min      1.2507
_cell_volume                     2408.6(10)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2007)'
_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
;
????
;
_diffrn_ambient_temperature      173.1500
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 270.0000
                 XTD: 39.9931
              2theta: -20.1391
scan:
    Number of images: 360
               Slice: -110.0000 - 70.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 39.9931
              2theta: -20.1391
scan:
    Number of images: 328
               Slice: -110.0000 - 54.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 39.9931
              2theta: -20.1391
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0278
_diffrn_orient_matrix_UB_12      0.0062
_diffrn_orient_matrix_UB_13      -0.0670
_diffrn_orient_matrix_UB_21      0.0628
_diffrn_orient_matrix_UB_22      0.0758
_diffrn_orient_matrix_UB_23      -0.0191
_diffrn_orient_matrix_UB_31      0.0299
_diffrn_orient_matrix_UB_32      -0.0350
_diffrn_orient_matrix_UB_33      -0.0407
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0323
_diffrn_reflns_av_unetI/netI     0.0176
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14604
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.52
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.364
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4118
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.322
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1008
_refine_diff_density_max         0.407
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.116
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     166
_refine_ls_number_reflns         2748
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.116
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0704P)^2^+1.3363P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1198
_reflns_number_gt                2722
_reflns_number_total             2748
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01720k2.cif
_cod_data_source_block           C5
_cod_original_cell_volume        2408.4(8)
_cod_database_code               7043121
_diffrn_number_total             2907
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H5BD)=Sof(H5BC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=
 Sof(C8A)=Sof(H8A)=1-FVAR(1)
 Sof(H5AA)=Sof(H5AB)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C7)=Sof(H7A)=Sof(H7B)=
 Sof(C8)=Sof(H8)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C8(H8), C8A(H8A)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5AA,H5AB), C5(H5BD,H5BC), C6(H6A,H6B), C7(H7A,H7B), C6A(H6AA,H6AB),
 C7A(H7AA,H7AB)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2)
3.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'