Simple magnesium alkoxides: synthesis, molecular structure, and catalytic behaviour in the ring-opening polymerization of lactide and macrolactones and for copolymerization of maleic anhydride and propylene oxide
Wannipurage, Duleeka; D'Aniello, Sara; Pappalardo, Daniela; Kulathungage, Lakshani Wathsala; Ward, Cassandra L.; Anderson, Danni P.; Groysman, Stanislav; Mazzeo, Mina; Dalton Transactions  (2023) –; doi:10.1039/D3DT00785E

data_7713000
_publ_section_title
;
 Simple magnesium alkoxides: synthesis, molecular structure, and catalytic
 behaviour in the ring-opening polymerization of lactide and macrolactones
 and for copolymerization of maleic anhydride and propylene oxide
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00785E
_journal_year                    2023
_chemical_formula_moiety         'C50 H74 Mg O4, C1 H2 Cl2'
_chemical_formula_sum            'C51 H76 Cl2 Mg O4'
_chemical_formula_weight         848.32
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-08-17 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                67.339(13)
_cell_angle_beta                 83.200(15)
_cell_angle_gamma                82.150(14)
_cell_formula_units_Z            2
_cell_length_a                   12.352(6)
_cell_length_b                   13.519(6)
_cell_length_c                   15.032(7)
_cell_measurement_reflns_used    3690
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.403
_cell_measurement_theta_min      2.144
_cell_volume                     2288.7(19)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.1145
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8442
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.556
_diffrn_reflns_theta_min         1.472
_exptl_absorpt_coefficient_mu    0.200
_exptl_absorpt_correction_T_max  0.745210
_exptl_absorpt_correction_T_min  0.338895
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 37824 reflections, Rint = 0.1132
 (11429 with I > 3sig(I), Rint = 0.0886)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.896
_refine_diff_density_min         -0.517
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     558
_refine_ls_number_reflns         8442
_refine_ls_number_restraints     426
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.1295
_refine_ls_R_factor_gt           0.0830
_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^)+(0.1251P)^2^+2.6153P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2068
_refine_ls_wR_factor_ref         0.2400
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5791
_reflns_number_total             8442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00785e2.cif
_cod_data_source_block           mg1_twin_p1bar
_cod_original_cell_volume        2288.8(18)
_cod_database_code               7713000
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.928
_shelx_estimated_absorpt_t_min   0.907
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.577(2)
 0.423(2)
2. 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
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.002 and sigma
for terminal atoms of 0.002
4. Others
 Sof(Cl4S)=Sof(C2S)=Sof(H2SA)=Sof(H2SB)=Sof(Cl3S)=1-FVAR(1)
 Sof(Cl1S)=Sof(Cl2S)=Sof(C1S)=Sof(H1SA)=Sof(H1SB)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C18(H18), C20(H20), C16(H16), C37(H37), C39(H39), C41(H41)
5.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C21(H21A,H21B), C19(H19A,H19B), C43(H43A,H43B), C14(H14A,
 H14B), C17(H17A,H17B), C15(H15A,H15B), C35(H35A,H35B), C34(H34A,H34B),
 C48(H48A,H48B), C47(H47A,H47B), C38(H38A,H38B), C46(H46A,H46B), C49(H49A,H49B),
  C36(H36A,H36B), C45(H45A,H45B), C40(H40A,H40B), C42(H42A,H42B), C50(H50A,
 H50B), C44(H44A,H44B), C1S(H1SA,H1SB), C2S(H2SA,H2SB)
5.c Aromatic/amide H refined with riding coordinates:
 C8(H8), C31(H31), C11(H11), C7(H7), C32(H32), C30(H30), C28(H28), C9(H9),
 C29(H29), C10(H10)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C4(H4A,H4B,
 H4C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C)
;
_shelx_res_checksum              69079
_olex2_exptl_crystal_mounting_method
'mounted on a MicroMount (MiTeGen) with paratone oil (Parabar 10312, Hampton Research)'
_olex2_submission_special_instructions 'No special instructions were received'