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_1568217
_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         'C24 H15 N3 O2, C H Cl3'
_chemical_formula_sum            'C25 H16 Cl3 N3 O2'
_chemical_formula_weight         496.76
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-02-01
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2022-07-28 deposited with the CCDC.	2022-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.062(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3458(8)
_cell_length_b                   15.7608(7)
_cell_length_c                   9.4437(4)
_cell_measurement_reflns_used    3574
_cell_measurement_temperature    295.0
_cell_measurement_theta_max      66.71
_cell_measurement_theta_min      2.88
_cell_volume                     2280.81(18)
_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 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      295.0
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker D8 Venture'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  multilayer
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0489
_diffrn_reflns_av_unetI/netI     0.0468
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            15183
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        66.794
_diffrn_reflns_theta_max         66.794
_diffrn_reflns_theta_min         2.884
_diffrn_source                   'high brilliance microfocus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.877
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.5743
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0756 before and 0.0382 after correction.
The Ratio of minimum to maximum transmission is 0.7157.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.447
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.447
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.046
_refine_ls_extinction_coef       0.0015(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/1 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     327
_refine_ls_number_reflns         3995
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.417
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0635
_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^)+(0.1025P)^2^+0.5112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1785
_refine_ls_wR_factor_ref         0.1973
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2914
_reflns_number_total             3995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2py01076c2.cif
_cod_data_source_block           compound1b
_cod_depositor_comments
'Adding full bibliography for 1568216--1568217.cif.'
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1568217
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.722
_shelx_estimated_absorpt_t_min   0.675
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
2. Restrained distances
 Cl3A-Cl2A \\sim Cl3A-Cl1A \\sim Cl2A-Cl1A \\sim Cl3B-Cl1B \\sim Cl3B-Cl2B
\\sim Cl1B-Cl2B
 with sigma of 0.04
 C25-Cl3A \\sim C25-Cl2A \\sim C25-Cl1A \\sim C25-Cl3B \\sim C25-Cl1B \\sim
C25-Cl2B
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 Cl2A, Cl3A, Cl1A, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl1B, Cl3B, Cl2B, C25
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H25A)=Sof(Cl1B)=Sof(Cl2B)=Sof(Cl3B)=1-FVAR(1)
 Sof(H25)=Sof(Cl1A)=Sof(Cl2A)=Sof(Cl3A)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C25(H25), C25(H25A)
5.b Aromatic/amide H refined with riding coordinates:
 N1(H1), C2(H2), C3(H3), C4(H4), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C17(H17), C18(H18), C21(H21), C22(H22), C23(H23), C24(H24)
;
_shelx_res_checksum              54650
_olex2_submission_special_instructions 'No special instructions were received'