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_7043120
_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 H32 Al2 N2 O2'
_chemical_formula_sum            'C22 H32 Al2 N2 O2'
_chemical_formula_weight         410.46
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 116.14(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.670(3)
_cell_length_b                   8.2200(16)
_cell_length_c                   9.0500(18)
_cell_measurement_reflns_used    1938
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4596
_cell_measurement_theta_min      2.7628
_cell_volume                     1113.3(5)
_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 0.934
_diffrn_measured_fraction_theta_max 0.937
_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: 44.9825
              2theta: -20.2715
scan:
    Number of images: 356
               Slice: -110.0000 - 68.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9825
              2theta: -20.2715
scan:
    Number of images: 150
               Slice: -110.0000 - -35.0000
         Image width: 0.5000
            Exp time: 3.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9825
              2theta: -20.2715
;
_diffrn_measurement_device
;
Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_device_details
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_method       dtprofit.ref
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.0489
_diffrn_orient_matrix_UB_12      -0.0446
_diffrn_orient_matrix_UB_13      -0.0109
_diffrn_orient_matrix_UB_21      0.0735
_diffrn_orient_matrix_UB_22      -0.0897
_diffrn_orient_matrix_UB_23      0.0365
_diffrn_orient_matrix_UB_31      -0.0757
_diffrn_orient_matrix_UB_32      -0.0235
_diffrn_orient_matrix_UB_33      0.0948
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4852
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         2.72
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0000
_diffrn_source_power             1.2000
_diffrn_source_voltage           50.0000
_exptl_absorpt_coefficient_mu    0.150
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4389
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             440
_refine_diff_density_max         0.702
_refine_diff_density_min         -0.348
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1274
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0588
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0928P)^2^+1.0769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1592
_refine_ls_wR_factor_ref         0.1612
_reflns_number_gt                1256
_reflns_number_total             1274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7dt01720k2.cif
_cod_data_source_block           C1
_cod_original_cell_volume        1113.3(4)
_cod_database_code               7043120
_diffrn_number_total             1317
_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. Others
 Fixed Sof: H5A(0.5) H5B(0.5) H7B(0.5) H7A(0.5) H6B(0.5) H6A(0.5) C8(0.5)
 H8(0.5)
3.a Riding coordinates:
 C7(H7B,H7A), C8(H8)
3.b Secondary CH2 refined with riding coordinates:
 C5(H5A,H5B), C6(H6B,H6A)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2), C1(H1)
3.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
_olex2_submission_special_instructions 'No special instructions were received'