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_4517706
_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 H61 In N2 O Si2'
_chemical_formula_sum            'C31 H61 In N2 O Si2'
_chemical_formula_weight         648.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_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                90
_cell_angle_beta                 106.121(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.5173(5)
_cell_length_b                   22.1551(9)
_cell_length_c                   11.8658(4)
_cell_measurement_reflns_used    9933
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.7
_cell_measurement_theta_min      2.6
_cell_volume                     3666.4(2)
_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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0378
_diffrn_reflns_av_unetI/netI     0.0384
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            36740
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.764
_diffrn_reflns_theta_min         1.725
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_T_max  0.9293
_exptl_absorpt_correction_T_min  0.8438
_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    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.524
_refine_diff_density_min         -0.922
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         9488
_refine_ls_number_restraints     951
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0446
_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^)+4.7072P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0741
_refine_ls_wR_factor_ref         0.0771
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7891
_reflns_number_total             9488
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c01365_si_002.cif
_cod_data_source_block           pm080(complex1)
_cod_depositor_comments
'Adding full bibliography for 4517706--4517710.cif.'
_cod_database_code               4517706
_shelx_shelxl_version_number     2017/1
_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
 C16-C14 \\sim C16A-C14A \\sim C17-C14 \\sim C15A-C14A \\sim C17A-C14A \\sim
C15-C14
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08 within 2A
Uanis(C17) = Uanis(C15A)
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C22A)=Sof(H22D)=Sof(H22E)=Sof(H22F)=Sof(C2A)=Sof(H2A)=Sof(C3A)=Sof(H3AA)=
 Sof(H3AB)=Sof(N2A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=
 Sof(C1A)=Sof(H1AA)=Sof(C4A)=Sof(H4AA)=Sof(H4AB)=Sof(C23)=Sof(H23D)=Sof(H23E)=
 Sof(H23F)=1-FVAR(1)
 Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=
 Sof(H4B)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(C22)=
 Sof(H22A)=Sof(H22B)=Sof(H22C)=Sof(C23A)=Sof(H23A)=Sof(H23B)=Sof(H23C)=Sof(N2)=
 FVAR(1)
 Sof(C14A)=Sof(C16A)=Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=
 Sof(H17E)=Sof(H17F)=Sof(C15A)=Sof(H15D)=Sof(H15E)=Sof(H15F)=1-FVAR(2)
 Sof(C14)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=Sof(C16)=Sof(H16A)=Sof(H16B)=
 Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2), C2A(H2A), C1A(H1AA)
6.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), C3A(H3AA,H3AB), C5A(H5AA,H5AB), C6A(H6AA,H6AB),
 C4A(H4AA,H4AB)
6.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12)
6.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C),
 C23A(H23A,H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,
 H27C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C),
 C22A(H22D,H22E,H22F), C23(H23D,H23E,H23F), C16A(H16D,H16E,H16F), C17A(H17D,
 H17E,H17F), C15A(H15D,H15E,H15F)
;
_shelx_res_checksum              35769
_shelx_hkl_checksum              96037
_olex2_submission_special_instructions 'No special instructions were received'