Tailor-made block copolymers of l-, d- and rac-lactides and ε-caprolactone via one-pot sequential ring opening polymerization by pyridylamidozinc(ii) catalysts
D'Auria, Ilaria; D'Alterio, Massimo Christian; Tedesco, Consiglia; Pellecchia, Claudio; RSC Advances 9 (2019) 32771–; doi:10.1039/C9RA07133D

data_7234617
_publ_section_title
;
 Tailor-made block copolymers of l-, d- and rac-lactides and
 \e-caprolactone via one-pot sequential ring opening polymerization by
 pyridylamidozinc(ii) catalysts
;
_journal_issue                   56
_journal_name_full               'RSC Advances'
_journal_page_first              32771
_journal_paper_doi               10.1039/C9RA07133D
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety         'C28 H36 N2 Zn'
_chemical_formula_sum            'C28 H36 N2 Zn'
_chemical_formula_weight         465.96
_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     direct
_audit_creation_date             2019-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-05-17 deposited with the CCDC.    2019-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                78.79(3)
_cell_angle_beta                 84.49(4)
_cell_angle_gamma                67.01(3)
_cell_formula_units_Z            2
_cell_length_a                   8.671(4)
_cell_length_b                   8.736(3)
_cell_length_c                   19.457(10)
_cell_measurement_reflns_used    2402
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.1345
_cell_measurement_theta_min      28.0369
_cell_volume                     1330.6(11)
_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    'SIR2014 (Burla et al. 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Rigaku AFC7S'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1245
_diffrn_reflns_av_unetI/netI     0.2804
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.881
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            11078
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.881
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.685
_diffrn_reflns_theta_min         1.067
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.3372
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_description       prism
_exptl_crystal_F_000             496
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         6042
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.3627
_refine_ls_R_factor_gt           0.1157
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1422P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2698
_refine_ls_wR_factor_ref         0.4085
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1535
_reflns_number_total             6042
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra07133d2.cif
_cod_data_source_block           trig2_ref
_cod_database_code               7234617
_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:
 C24(H24), C21(H21)
2.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C27(H27A,H27B)
2.c Me refined with riding coordinates:
 C28(H28A,H28B,H28C)
2.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C19(H19), C4(H4), C17(H17), C3(H3), C5(H5), C11(H11), C9(H9),
 C10(H10)
2.e Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C22(H22A,H22B,
 H22C), C25(H25A,H25B,H25C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              9946
_olex2_submission_special_instructions 'No special instructions were received'