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_1572158
_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         'C36 H46 Ca2 I2 N8 O4, 2(C H2 Cl2)'
_chemical_formula_sum            'C38 H50 Ca2 Cl4 I2 N8 O4'
_chemical_formula_weight         1158.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2024-02-24
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-03-18 deposited with the CCDC.	2024-07-08 downloaded from the CCDC.
;
_cell_angle_alpha                106.384(11)
_cell_angle_beta                 100.446(11)
_cell_angle_gamma                93.892(10)
_cell_formula_units_Z            1
_cell_length_a                   9.505(3)
_cell_length_b                   10.990(3)
_cell_length_c                   12.918(5)
_cell_measurement_reflns_used    6171
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      25.864
_cell_measurement_theta_min      2.196
_cell_volume                     1263.0(7)
_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  'SHELXL 2014/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.994
_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  0.0762
_diffrn_reflns_av_unetI/netI     0.0415
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            29978
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.465
_diffrn_reflns_theta_min         2.157
_exptl_absorpt_coefficient_mu    1.703
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0979 before and 0.0603 after correction.
The Ratio of minimum to maximum transmission is 0.8735.
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    1.523
_exptl_crystal_description       block
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.852
_refine_diff_density_min         -1.149
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     270
_refine_ls_number_reflns         5188
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0444
_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^)+(0.0738P)^2^+0.9607P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1230
_refine_ls_wR_factor_ref         0.1348
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4033
_reflns_number_total             5188
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4py00379a2.cif
_cod_data_source_block           mo_phocai_0m_a
_cod_depositor_comments
'Adding full bibliography for 1572157--1572158.cif.'
_cod_database_code               1572158
_shelxl_version_number           2014-3
_shelx_estimated_absorpt_t_max   0.848
_shelx_estimated_absorpt_t_min   0.749
_olex2_refinement_description
;
1.a Rotating group:
 O2(H2A,H2B)
1.b Ternary CH refined with riding coordinates:
 C12(H12), C11(H11)
1.c Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
1.d Aromatic/amide H refined with riding coordinates:
 C18(H18), C2(H2), C14(H14), C17(H17), C16(H16), C15(H15)
1.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C)
;
_shelx_res_checksum              49896
_olex2_submission_special_instructions 'No special instructions were received'