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_7713002
_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         'C52 H78 Mg2 O4, 1.33[C4H10O]'
_chemical_formula_sum            'C57.32 H91.3 Mg2 O5.33'
_chemical_formula_weight         914.34
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yc'
_space_group_name_H-M_alt        'P 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-11-19
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2022-09-10 deposited with the CCDC.	2023-04-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.778(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.5905(10)
_cell_length_b                   10.4610(9)
_cell_length_c                   20.3664(17)
_cell_measurement_reflns_used    7705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.456
_cell_measurement_theta_min      2.188
_cell_volume                     2682.2(4)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.1564
_diffrn_reflns_av_unetI/netI     0.1403
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            62305
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.508
_diffrn_reflns_theta_min         1.947
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0865 before and 0.0760 after correction.
The Ratio of minimum to maximum transmission is 0.7700.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_description       block
_exptl_crystal_F_000             1004
_exptl_crystal_recrystallization_method 'slow evaporation in ether'
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.366
_refine_diff_density_rms         0.060
_refine_ls_abs_structure_details
;
 Flack x determined using 1353 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.2(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         9936
_refine_ls_number_restraints     495
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.2148
_refine_ls_R_factor_gt           0.0959
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1634P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2430
_refine_ls_wR_factor_ref         0.3109
_reflns_Friedel_coverage         0.989
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                4058
_reflns_number_total             9936
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00785e2.cif
_cod_data_source_block           sg_883_0m_clw
_cod_original_formula_sum        'C57.32 H91.30 Mg2 O5.33'
_cod_database_code               7713002
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.962
_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
 C53-C50 \\sim C54-C50
 with sigma of 0.005
 C51-C53 \\sim C54-C52
 with sigma of 0.005
 C52-C50 \\sim C51-C50 \\sim C47-C46 \\sim C48-C46 \\sim C52-C54 \\sim C53-C51
\\sim C49-C48
 with sigma of 0.005
 C23-C22 \\sim C24-C23 \\sim C25-C24 \\sim C26-C25 \\sim C27-C26 \\sim C27-C22
\\sim C5-C4 \\sim C6-C5 ~
 C7-C6 \\sim C8-C7 \\sim C9-C8 \\sim C9-C4
 with sigma of 0.005
 C39-C38 \\sim C40-C39 \\sim C41-C40 \\sim C45-C44 \\sim C44-C43 \\sim C43-C42
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.002 within 2A
4. Others
 Sof(H52D)=Sof(H52E)=Sof(H51C)=Sof(H51D)=Sof(H51E)=Sof(C54)=Sof(H54A)=
 Sof(H54B)=Sof(H54C)=1-FVAR(1)
 Sof(H52A)=Sof(H52B)=Sof(H52C)=Sof(H51A)=Sof(H51B)=Sof(C53)=Sof(H53A)=
 Sof(H53B)=Sof(H53C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C36(H36), C33(H33), C18(H18), C12(H12), C46(H46), C30(H30), C50(H50), C14(H14)
5.b Secondary CH2 refined with riding coordinates:
 C32(H32A,H32B), C38(H38A,H38B), C35(H35A,H35B), C34(H34A,H34B), C41(H41A,
 H41B), C13(H13A,H13B), C42(H42A,H42B), C19(H19A,H19B), C31(H31A,H31B),
 C11(H11A,H11B), C29(H29A,H29B), C37(H37A,H37B), C16(H16A,H16B), C17(H17A,H17B),
  C52(H52D,H52E), C43(H43A,H43B), C45(H45A,H45B), C48(H48A,H48B), C39(H39A,
 H39B), C44(H44A,H44B), C51(H51A,H51B), C15(H15A,H15B), C40(H40A,H40B)
5.c Me refined with riding coordinates:
 C52(H52A,H52B,H52C)
5.d Aromatic/amide H refined with riding coordinates:
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C5(H5), C6(H6), C7(H7),
 C8(H8), C9(H9)
5.e Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C51(H51C,H51D,H51E), C49(H49A,H49B,
 H49C), C47(H47A,H47B,H47C), C54(H54A,H54B,H54C), C53(H53A,H53B,H53C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              72730
_shelx_fab_checksum              28600
_olex2_submission_special_instructions 'No special instructions were received'