Ring opening polymerization of d,l-lactide and ε-caprolactone catalysed by (pyrazol-1-yl)copper(ii) carboxylate complexes
Appavoo, Divambal; Spencer, Lara C.; Guzei, Ilia A.; Gómez-García, Carlos J.; van Wyk, Juanita L.; Darkwa, James; RSC Advances 11 (2021) 13475–13485; doi:10.1039/D1RA00339A

data_7242645
_publ_section_title
;
 Ring opening polymerization of d,l-lactide and \e-caprolactone catalysed
 by (pyrazol-1-yl)copper(ii) carboxylate complexes
;
_journal_issue                   22
_journal_name_full               'RSC Advances'
_journal_page_first              13475
_journal_page_last               13485
_journal_paper_doi               10.1039/D1RA00339A
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C64 H64 Cu2 N8 O12, 7.074(H2 O)'
_chemical_formula_sum            'C64 H78.15 Cu2 N8 O19.07'
_chemical_formula_weight         1391.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2020-12-07
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2020-12-17 deposited with the CCDC.	2021-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.485(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.7157(3)
_cell_length_b                   21.1150(6)
_cell_length_c                   17.2695(5)
_cell_measurement_reflns_used    8793
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      29.3689
_cell_measurement_theta_min      2.8809
_cell_volume                     3471.85(18)
_computing_cell_refinement       'SAINT Ver. 7.24A (Bruker-AXS, 2007)'
_computing_data_collection       'APEX2 Ver. 2.1-4 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT Ver. 7.24A'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '0.60\% \w and 0.6\% \f scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0511
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            57515
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         30.575
_diffrn_reflns_theta_min         2.881
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  0.9470
_exptl_absorpt_correction_T_min  0.9281
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
SADABS  (Bruker-AXS, 2007)
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1458
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.738
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     460
_refine_ls_number_reflns         10630
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0457
_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^)+(0.0602P)^2^+2.9809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8216
_reflns_number_total             10630
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ra00339a2.cif
_cod_data_source_block           darkwa136
_cod_database_code               7242645
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.947
_shelx_estimated_absorpt_t_min   0.928
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O7-H7A = O7-H7B = O8-H8B = O8-H8A = O9-H9A = O9-H9B = O10-H10A = O10-H10B
 0.9584 with sigma of 0.002
 H10A-O9 = O9-H10B
 3.355 with sigma of 0.003
 H7A-H7B = H8B-H8A = H9A-H9B = H10A-H10B
 1.515 with sigma of 0.005
 O3-H3 = O6-H6
 0.84 with sigma of 0.01
3. Others
 Sof(O10)=Sof(H10A)=Sof(H10B)=FVAR(1)
 Sof(O7)=Sof(H7A)=Sof(H7B)=FVAR(2)
 Sof(O8)=Sof(H8A)=Sof(H8B)=FVAR(3)
 Sof(O9)=Sof(H9A)=Sof(H9B)=FVAR(4)
 Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(5)
 Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(5)
4.a Secondary CH2 refined with riding coordinates:
 C20(H20A,H20B), C27(H27A,H27B)
4.b Me refined with riding coordinates:
 C15(H15A,H15B,H15C), C19(H19A,H19B,H19C), C28(H28A,H28B,H28C)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C4(H4), C6(H6A), C7(H7), C10(H10), C11(H11), C13(H13), C14(H14),
 C17(H17), C22(H22), C23(H23), C24(H24), C25(H25), C30(H30)
4.d Disordered Me refined as rotating group:
 C32(H32A,H32B,H32C,H32D,H32E,H32F)
;
_shelx_res_checksum              68712
_olex2_submission_special_instructions 'No special instructions were received'