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_7234616
_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         'C33 H51 N3 Si2 Zn'
_chemical_formula_sum            'C33 H51 N3 Si2 Zn'
_chemical_formula_weight         611.31
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                90
_cell_angle_beta                 93.00(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.188(4)
_cell_length_b                   10.266(4)
_cell_length_c                   26.260(16)
_cell_measurement_reflns_used    9879
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      52.69
_cell_measurement_theta_min      3.36
_cell_volume                     3550(3)
_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      296.15
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_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  0.0407
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            21684
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        52.869
_diffrn_reflns_theta_max         52.869
_diffrn_reflns_theta_min         3.371
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.774
_exptl_absorpt_correction_T_max  0.7504
_exptl_absorpt_correction_T_min  0.1544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1711 before and 0.0633 after correction.
The Ratio of minimum to maximum transmission is 0.2058.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.144
_exptl_crystal_description       prism
_exptl_crystal_F_000             1312
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: hexane'
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.361
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         4073
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0418
_refine_ls_R_factor_gt           0.0361
_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^)+(0.0519P)^2^+1.9608P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.0989
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3604
_reflns_number_total             4073
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9ra07133d2.cif
_cod_data_source_block           aga3_tip
_cod_database_code               7234616
_shelx_shelxl_version_number     2016/6
_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 Ternary CH refined with riding coordinates:
 C1(H1), C21(H21), C24(H24)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C4(H4), C17(H17), C19(H19), C9(H9), C18(H18), C10(H10),
 C11(H11)
2.c Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C23(H23A,H23B,H23C), C13(H13A,H13B,H13C), C26(H26A,H26B,
 H26C), C14(H14A,H14B,H14C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C), C32(H32A,
 H32B,H32C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C29(H29A,H29B,H29C),
 C30(H30A,H30B,H30C), C28(H28A,H28B,H28C)
;
_shelx_res_checksum              60611
_olex2_submission_special_instructions 'No special instructions were received'