Indium-Catalyzed Block Copolymerization of Lactide and Methyl Methacrylate by Sequential Addition
Jung, Hyuk-Joon; Yu, Insun; Nyamayaro, Kudzanai; Mehrkhodavandi, Parisa; ACS Catalysis  (2020) 6488–6496; doi:10.1021/acscatal.0c01365

data_4517708
_publ_section_title
;
 Indium-Catalyzed Block Copolymerization of Lactide and Methyl
 Methacrylate by Sequential Addition
;
_journal_name_full               'ACS Catalysis'
_journal_page_first              6488
_journal_page_last               6496
_journal_paper_doi               10.1021/acscatal.0c01365
_journal_year                    2020
_chemical_formula_moiety
'C31 H58 In N2 O2 Si, C27 H50 In N2 O Si, 2(B C24 F20), C5 H12'
_chemical_formula_sum            'C111 H120 B2 F40 In2 N4 O3 Si2'
_chemical_formula_weight         2625.54
_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             2020-03-06
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                91.0320(10)
_cell_angle_beta                 101.5490(10)
_cell_angle_gamma                91.7730(10)
_cell_formula_units_Z            2
_cell_length_a                   13.9210(5)
_cell_length_b                   16.0270(6)
_cell_length_c                   26.4150(9)
_cell_measurement_reflns_used    7859
_cell_measurement_temperature    90.15
_cell_measurement_theta_max      29.317
_cell_measurement_theta_min      2.644
_cell_volume                     5769.7(4)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2017/1 (Sheldrick, 2015)'
_diffrn_ambient_temperature      90.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0381
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            157070
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.571
_diffrn_reflns_theta_min         1.479
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.537
_exptl_absorpt_correction_T_max  0.9528
_exptl_absorpt_correction_T_min  0.8172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2668
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.421
_refine_diff_density_min         -0.793
_refine_diff_density_rms         0.077
_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     1515
_refine_ls_number_reflns         32341
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0543
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0447P)^2^+3.4571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0936
_reflns_Friedel_coverage         0.000
_reflns_number_gt                25393
_reflns_number_total             32341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c01365_si_002.cif
_cod_data_source_block           pm089(complex3)
_cod_depositor_comments
'Adding full bibliography for 4517706--4517710.cif.'
_cod_database_code               4517708
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.900
_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
 C113-C112 \\sim C114-C113 \\sim C115-C114 \\sim C116-C115 \\sim C111-C110
\\sim C110-C109 \\sim C109-
 C108 \\sim C108-C107
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C110) = Uanis(C115)
Uanis(C107) = Uanis(C112)
Uanis(C111) = Uanis(C116)
4. Others
 Sof(C112)=Sof(H11F)=Sof(H11G)=Sof(H11H)=Sof(C113)=Sof(H11I)=Sof(H11J)=
 Sof(C114)=Sof(H11K)=Sof(H11L)=Sof(C115)=Sof(H11M)=Sof(H11N)=Sof(C116)=
 Sof(H11O)=Sof(H11P)=Sof(H11Q)=1-FVAR(1)
 Sof(C107)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C108)=Sof(H10D)=Sof(H10E)=
 Sof(C109)=Sof(H10F)=Sof(H10G)=Sof(C110)=Sof(H11A)=Sof(H11B)=Sof(C111)=
 Sof(H11C)=Sof(H11D)=Sof(H11E)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C32(H32), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C24(H24A,
 H24B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B),
 C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B), C38(H38A,H38B),
  C55(H55A,H55B), C108(H10D,H10E), C109(H10F,H10G), C110(H11A,H11B), C113(H11I,
 H11J), C114(H11K,H11L), C115(H11M,H11N)
5.c Me refined with riding coordinates:
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C53(H53A,H53B,H53C), C54(H54A,
 H54B,H54C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C),
 C107(H10A,H10B,H10C), C112(H11F,H11G,H11H)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12), C41(H41), C43(H43)
5.e Idealised Me refined as rotating group:
 C111(H11C,H11D,H11E), C116(H11O,H11P,H11Q)
;
_shelx_res_checksum              2054
_shelx_hkl_checksum              6218
_olex2_submission_special_instructions 'No special instructions were received'