Lithium anthraquinoids as catalysts in the ROP of lactide and caprolactone into cyclic polymers
Ruiz Martínez, Cristina; Pérez, Juana M.; Arrabal-Campos, Francisco M.; Rodríguez-Diéguez, Antonio; Choquesillo-Lazarte, Duane; Martínez-Lao, Juan A.; Ortuño, Manuel A.; Fernández, Ignacio; Polymer Chemistry 14 (2023) 452–461; doi:10.1039/D2PY01076C

data_1568216
_publ_section_title
;
 Lithium anthraquinoids as catalysts in the ROP of lactide and
 caprolactone into cyclic polymers
;
_journal_issue                   4
_journal_name_full               'Polymer Chemistry'
_journal_page_first              452
_journal_page_last               461
_journal_paper_doi               10.1039/D2PY01076C
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C17 H14 N2 O2'
_chemical_formula_sum            'C17 H14 N2 O2'
_chemical_formula_weight         278.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-03-02
_audit_creation_method
;
Olex2 1.5
(compiled 2021.12.09 svn.r5202d8cf for OlexSys, GUI svn.r6439)
;
_audit_update_record
;
2022-07-28 deposited with the CCDC.	2022-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.966(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.1707(15)
_cell_length_b                   3.8686(5)
_cell_length_c                   30.877(4)
_cell_measurement_reflns_used    5043
_cell_measurement_temperature    130.00
_cell_measurement_theta_max      25.114
_cell_measurement_theta_min      2.211
_cell_volume                     1333.6(3)
_computing_cell_refinement       'SAINT V8.40B (Bruker, 2016)'
_computing_data_collection       'Bruker Apex3, 2019'
_computing_data_reduction        'SAINT V8.40B (Bruker, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      130.00
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1081
_diffrn_reflns_av_unetI/netI     0.0884
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       3
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            11079
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        20.813
_diffrn_reflns_theta_max         20.813
_diffrn_reflns_theta_min         2.215
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.0261
_exptl_absorpt_correction_T_min  0.0082
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1358 before and 0.0914 after correction.
The Ratio of minimum to maximum transmission is 0.3142.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             584
_refine_diff_density_max         0.230
_refine_diff_density_min         -0.245
_refine_diff_density_rms         0.056
_refine_ls_abs_structure_details
;
 Flack x determined using 793 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.4(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.163
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         2769
_refine_ls_number_restraints     338
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0771
_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^)+(0.0432P)^2^+2.2789P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1618
_refine_ls_wR_factor_ref         0.1699
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.992
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                2246
_reflns_number_total             2769
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2py01076c2.cif
_cod_data_source_block           compound1d
_cod_depositor_comments
;
Adding full bibliography for 1568216--1568217.cif.

2025-06-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C34 H28 N4 O4'
_cod_original_formula_weight         556.60
_cod_original_formula_moiety         '2(C17 H14 N2 O2)'
_cod_original_formula_units_Z            2
_cod_original_sg_symbol_H-M      Pc
_cod_database_code               1568216
_shelx_shelxl_version_number     2019/1
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 C18, C19, C20, C21, C22, C23, C24, C25, C26, C27, C28, C29, C30, C31, C32,
 C33, C34, N3, N4, O3, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11, C12, C13, C14, C15, C16, C17,
 N1, N2, O1, O2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C14(H14), C15(H15), C16(H16), C17(H17), N1(H1),
 C22(H22), C23(H23), C24(H24), C31(H31), C32(H32), C33(H33), C34(H34), N3(H3)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_olex2_submission_special_instructions 'No special instructions were received'