Homoleptic Magnesium and Calcium Complexes Supported by Constrained Reduced Schiff Base Ligand for Lactide Polymerisation: DFT Analysis of Lactide/Ligand Interactions
Quek, Timothy; Saeteaw, Thonthun; Pongpanit, Tanyawan; Namuangruk, Supawadee; Phomphrai, Khamphee; Physical Chemistry Chemical Physics  (2025) –; doi:10.1039/D5CP02229K

data_7250791
_publ_section_title
;
 Homoleptic Magnesium and Calcium Complexes Supported by Constrained
 Reduced Schiff Base Ligand for Lactide Polymerisation: DFT Analysis of
 Lactide/Ligand Interactions
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D5CP02229K
_journal_year                    2025
_chemical_formula_moiety         'C42 H70 Mg N4 O2, C7 H8, 2[C7H8]'
_chemical_formula_sum            'C63 H94 Mg N4 O2'
_chemical_formula_weight         963.73
_chemical_properties_physical    Air-sensitive
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-10-23 deposited with the CCDC.	2025-08-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.4474(4)
_cell_length_b                   20.5344(5)
_cell_length_c                   22.8703(7)
_cell_measurement_reflns_used    3505
_cell_measurement_temperature    200
_cell_measurement_theta_max      54.694
_cell_measurement_theta_min      3.865
_cell_volume                     5845.6(3)
_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      200
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            97311
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         79.435
_diffrn_reflns_theta_min         3.865
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.591
_exptl_absorpt_correction_T_max  0.7542
_exptl_absorpt_correction_T_min  0.6759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1036 before and 0.0884 after correction.
The Ratio of minimum to maximum transmission is 0.8962.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.095
_exptl_crystal_description       needle
_exptl_crystal_F_000             2112
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Toluene'
_exptl_crystal_size_max          0.206
_exptl_crystal_size_mid          0.054
_exptl_crystal_size_min          0.052
_refine_diff_density_max         0.254
_refine_diff_density_min         -0.203
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.00139(19)
_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   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         6325
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.1037
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.037
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1182P)^2^+3.2897P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1902
_refine_ls_wR_factor_ref         0.2595
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3939
_reflns_number_total             6325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cp02229k3.cif
_cod_data_source_block           cu_mp7_0m
_cod_database_code               7250791
_shelx_shelxl_version_number     2019/1
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.888
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H4(0.5) HF(0.5) HG(0.5)
3.a Ternary CH refined with riding coordinates:
 N003(H003), C007(H007)
3.b Secondary CH2 refined with riding coordinates:
 C00C(H00A,H00C), C00E(H00D,H00E), C00F(H00F,H00G), C00H(H00H,H00I)
3.c Aromatic/amide H refined with riding coordinates:
 C00B(H00B), C00R(H1), C00S(H2), C00T(H3)
3.d Idealised Me refined as rotating group:
 C00I(H00J,H00K,H00L), C00J(H00M,H00N,H00O), C00K(H00P,H00Q,H00R), C00L(H00S,
 H00T,H00U), C00M(H00V,H00W,H00X), C00O(H00Y,H,HA), C00P(H00Z,HB,HC), C00Q(H00,
 HD,HE), C00X(H4,HF,HG)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              57125
_shelx_fab_checksum              5869
_olex2_submission_special_instructions 'No special instructions were received'