Dialkylaluminum 2-substituted 6,6-dimethylcyclopentylpyridin-7-oxylates toward structural-differentiation of the ring-opening polymerization of ε-caprolactone and l-lactides.
Zhu, Dongzhi; Guo, Liwei; Zhang, Wenjuan; Hu, Xinquan; Nomura, Kotohiro; Vignesh, Arumugam; Hao, Xiang; Zhang, Qiuyue; Sun, Wen-Hua; Dalton transactions (Cambridge, England : 2003) 48 (2019) 4157–4167; doi:10.1039/c9dt00137a

data_7049012
_publ_section_title
;
 Dialkylaluminum 2-substituted 6,6-dimethylcyclopentylpyridin-7-oxylates
 toward structural-differentiation of the ring-opening polymerization of
 \e-caprolactone and l-lactides.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4157
_journal_page_last               4167
_journal_paper_doi               10.1039/c9dt00137a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C12 H17 Al Cl N O'
_chemical_formula_sum            'C12 H17 Al Cl N O'
_chemical_formula_weight         253.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yac'
_space_group_name_H-M_alt        'P 1 2/n 1'
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-06-20
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-12-26 deposited with the CCDC.    2019-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.05(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.156(2)
_cell_length_b                   9.5875(19)
_cell_length_c                   13.196(3)
_cell_measurement_reflns_used    4420
_cell_measurement_temperature    173.1500
_cell_measurement_theta_max      27.4755
_cell_measurement_theta_min      1.5550
_cell_volume                     1275.2(5)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.1500
_diffrn_measured_fraction_theta_full 0.978
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0706
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15208
_diffrn_reflns_point_group_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_min         2.633
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.47470
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_description       block
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.427
_exptl_crystal_size_mid          0.419
_exptl_crystal_size_min          0.293
_refine_diff_density_max         0.425
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2881
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0477
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+0.7560P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1433
_refine_ls_wR_factor_ref         0.1528
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2743
_reflns_number_total             2881
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt00137a2.cif
_cod_data_source_block           a
_cod_depositor_comments          'Adding full bibliography for 7049012.cif.'
_cod_original_cell_volume        1275.2(4)
_cod_database_code               7049012
_shelx_shelxl_version_number     2016/6
_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.a Ternary CH refined with riding coordinates:
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C5(H5a,H5b)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C2(H2)
2.d Idealised Me refined as rotating group:
 C11(H11a,H11b,H11c), C12(H12a,H12b,H12c), C9(H9a,H9b,H9c), C10(H10a,H10b,H10c)
;
_shelx_res_checksum              76253
_olex2_submission_special_instructions 'No special instructions were received'