Calcium-catalysed ring-opening copolymerisation of epoxides and cyclic anhydrides
Francés-Poveda, Enrique; Martínez de Sarasa Buchaca, Marc; Moya-López, Carmen; Vitorica-Yrezabal, Iñigo J.; López-Solera, Isabel; Castro-Osma, José A.; la Cruz-Martínez, Felipe de; Lara-Sánchez, Agustín; Polymer Chemistry 15 (2024) 3238–3245; doi:10.1039/D4PY00379A

data_1572157
_publ_section_title
;
 Calcium-catalysed ring-opening copolymerisation of epoxides and cyclic
 anhydrides
;
_journal_issue                   32
_journal_name_full               'Polymer Chemistry'
_journal_page_first              3238
_journal_page_last               3245
_journal_paper_doi               10.1039/D4PY00379A
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C44 H58 Ca2 I2 N8 O4, 2(C H2 Cl2), C3 H7'
_chemical_formula_sum            'C49 H69 Ca2 Cl4 I2 N8 O4'
_chemical_formula_weight         1309.88
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-02-13
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-02-13 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.473(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.835(2)
_cell_length_b                   17.351(3)
_cell_length_c                   26.132(5)
_cell_measurement_reflns_used    9622
_cell_measurement_temperature    150.00
_cell_measurement_theta_max      28.40
_cell_measurement_theta_min      2.35
_cell_volume                     5793.1(17)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150.00
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0732
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            67749
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.957
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.495
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.5105
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1420 before and 0.0923 after correction.
The Ratio of minimum to maximum transmission is 0.6845.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.502
_exptl_crystal_description       block
_exptl_crystal_F_000             2660
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.502
_refine_diff_density_min         -1.825
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     619
_refine_ls_number_reflns         10522
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.1283
_refine_ls_R_factor_gt           0.1078
_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^)+(0.0131P)^2^+226.0766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2780
_refine_ls_wR_factor_ref         0.2911
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8391
_reflns_number_total             10522
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py00379a2.cif
_cod_data_source_block           mo_agu345_0m
_cod_depositor_comments
'Adding full bibliography for 1572157--1572158.cif.'
_cod_database_code               1572157
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.796
_shelx_estimated_absorpt_t_min   0.735
_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
 Cl4-C48 = Cl3-C48
 1.771 with sigma of 0.01
 Cl4-Cl3
 2.916 with sigma of 0.03
 C46-C45 \\sim C47-C46
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Cl4 \\sim Cl3 \\sim C48: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 2A
C47 \\sim C45 \\sim C46 \\sim C47 \\sim C46 \\sim C45: within 2A with sigma of
0.02 and sigma for terminal atoms of 0.04 within 2A
C48 \\sim Cl3 \\sim Cl4: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
4. Rigid body (RIGU) restrains
 Cl4, Cl3, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C47, C45, C46, C47, C46, C45
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
5.a Free rotating group:
 Cl4(Cl3,C48)
5.b Ternary CH refined with riding coordinates:
 C1(H1), C19(H19), C20(H20), C2(H2)
5.c Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C44(H44A,H44B), C43(H43A,H43B), C46(H46A,H46B), C40(H40A,
 H40B), C47(H47A,H47B), C49(H49A,H49B), C42(H42A,H42B), C41(H41A,H41B),
 C39(H39A,H39B), C37(H37A,H37B), C48(H48A,H48B)
5.d Me refined with riding coordinates:
 C12(H12A,H12B,H12C), C45(H45A,H45B,H45C), C30(H30A,H30B,H30C), C11(H11A,H11B,
 H11C), C29(H29A,H29B,H29C), C7(H7A,H7B,H7C), C25(H25A,H25B,H25C), C24(H24A,
 H24B,H24C), C6(H6A,H6B,H6C)
5.e Aromatic/amide H refined with riding coordinates:
 C32(H32), C27(H27), C15(H15), C34(H34), C35(H35), C33(H33), C4(H4), C17(H17),
 C22(H22), C16(H16), C36(H36), C18(H18), C9(H9), C14(H14)
;
_shelx_res_checksum              29728
_olex2_submission_special_instructions 'No special instructions were received'