Homoleptic phenoxy-imine pyridine zinc complexes: efficient catalysts for solvent free synthesis and chemical degradation of polyesters
D'Aniello, Sara; Laviéville, Sidonie; Santulli, Federica; Simon, Malaury; Sellitto, Michele; Tedesco, Consiglia; Thomas, Christophe M.; Mazzeo, Mina; Catalysis Science & Technology 12 (2022) 6142–6154; doi:10.1039/D2CY01092E

data_1567536
_publ_section_title
;
 Homoleptic phenoxy-imine pyridine zinc complexes: efficient catalysts for
 solvent free synthesis and chemical degradation of polyesters
;
_journal_issue                   20
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              6142
_journal_page_last               6154
_journal_paper_doi               10.1039/D2CY01092E
_journal_volume                  12
_journal_year                    2022
_chemical_formula_moiety         'C30 H30 N4 O2 Zn, C6 H6'
_chemical_formula_sum            'C36 H36 N4 O2 Zn'
_chemical_formula_weight         622.06
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2022-05-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2022-05-10 deposited with the CCDC.	2022-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.877(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.911(3)
_cell_length_b                   6.0729(9)
_cell_length_c                   27.229(4)
_cell_measurement_reflns_used    10252
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      65.461
_cell_measurement_theta_min      6.401
_cell_volume                     1635.1(6)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0650
_diffrn_reflns_av_unetI/netI     0.0585
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            10252
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        65.461
_diffrn_reflns_theta_max         65.461
_diffrn_reflns_theta_min         6.401
_exptl_absorpt_coefficient_mu    1.327
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.5797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1575 before and 0.0711 after correction.
The Ratio of minimum to maximum transmission is 0.7703.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_description       needle
_exptl_crystal_F_000             652
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: benzene, pentane'
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.460
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2767
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0710
_refine_ls_R_factor_gt           0.0564
_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^)+(0.0985P)^2^+0.4918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1526
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2236
_reflns_number_total             2767
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2cy01092e2.cif
_cod_data_source_block           sl_c2_dis_prev
_cod_depositor_comments
'Adding full bibliography for 1567535--1567537.cif.'
_cod_original_cell_volume        1635.1(7)
_cod_database_code               1567536
_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. Restrained distances
 C18A-C16B \\sim C18A-C18B
 with sigma of 0.02
 C16A-C17A \\sim C16A-C18B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C16A \\sim C17A \\sim C17B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C18A \\sim C16B \\sim C18B: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
4. Rigid body (RIGU) restrains
 C16A, C17A, C17B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C18A, C16B, C18B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C16A(0.5) H16A(0.5) C17A(0.5) H17A(0.5) C18A(0.5) H18A(0.5)
 C16B(0.5) H16B(0.5) C17B(0.5) H17B(0.5) C18B(0.5) H18B(0.5)
6.a Free rotating group:
 C16A(C17A,C18A), C16B(C17B,C18B)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
6.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C8(H8), C4(H4), C10(H10), C7(H7), C12(H12), C6(H6), C5(H5),
 C16A(H16A), C17A(H17A), C18A(H18A), C16B(H16B), C17B(H17B), C18B(H18B)
6.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C)
;
_shelx_res_checksum              86509
_olex2_submission_special_instructions 'No special instructions were received'