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_4517710
_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 H56 In N2 O2 Si, B C24 F20, C7 H8'
_chemical_formula_sum            'C62 H64 B F20 In N2 O2 Si'
_chemical_formula_weight         1402.87
_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   geom
_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                 106.494(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6691(8)
_cell_length_b                   25.0259(13)
_cell_length_c                   17.6496(9)
_cell_measurement_reflns_used    9424
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      25.44
_cell_measurement_theta_min      2.28
_cell_volume                     6212.7(6)
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_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  0.0298
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            65966
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.478
_diffrn_reflns_theta_min         1.453
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.504
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0442 before and 0.0391 after correction.
The Ratio of minimum to maximum transmission is 0.8888.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_description       block
_exptl_crystal_F_000             2856
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.940
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     889
_refine_ls_number_reflns         11436
_refine_ls_number_restraints     1653
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0309P)^2^+15.1872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0851
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9853
_reflns_number_total             11436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c01365_si_002.cif
_cod_data_source_block           pm209(complex5)
_cod_depositor_comments
'Adding full bibliography for 4517706--4517710.cif.'
_cod_database_code               4517710
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.956
_shelx_estimated_absorpt_t_min   0.897
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1B-C24 \\sim Si1A-C24 \\sim Si1A-C26A \\sim Si1A-C27A \\sim Si1B-C26B \\sim
Si1B-C25B \\sim Si1A-
 C25A \\sim Si1B-C27B
 with sigma of 0.01
3. Restrained planarity
 C56A, C57A, C58A, C59A, C60A, C61A, C62A
 with sigma of 0.1
 C56B, C57B, C58B, C59B, C60B, C61B, C62B
 with sigma of 0.1
4. 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(C62B) = Uanis(C59A)
5. 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
6. Others
 Sof(C56A)=Sof(C57A)=Sof(H57A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(H59A)=
 Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(H62A)=Sof(H62B)=
 Sof(H62C)=1-FVAR(1)
 Sof(C56B)=Sof(C57B)=Sof(H57B)=Sof(C58B)=Sof(H58B)=Sof(C59B)=Sof(H59B)=
 Sof(C60B)=Sof(H60B)=Sof(C61B)=Sof(H61B)=Sof(C62B)=Sof(H62D)=Sof(H62E)=
 Sof(H62F)=FVAR(1)
 Sof(Si1A)=Sof(H24A)=Sof(H24B)=Sof(C25A)=Sof(H25A)=Sof(H25B)=Sof(H25C)=
 Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=Sof(C27A)=Sof(H27A)=Sof(H27B)=
 Sof(H27C)=1-FVAR(2)
 Sof(Si1B)=Sof(H24C)=Sof(H24D)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=
 Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C27B)=Sof(H27D)=Sof(H27E)=
 Sof(H27F)=FVAR(2)
7.a Ternary CH refined with riding coordinates:
 C1(H1), C2(H2)
7.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C24(H24A,H24B), C24(H24C,
 H24D), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B)
7.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C10(H10), C12(H12), C57A(H57A), C58A(H58A), C59A(H59A), C60A(H60A),
 C61A(H61A), C57B(H57B), C58B(H58B), C59B(H59B), C60B(H60B), C61B(H61B)
7.d Fitted hexagon refined as free rotating group:
 C56A(C57A,C58A,C59A,C60A,C61A), C56B(C57B,C58B,C59B,C60B,C61B)
7.e Idealised Me refined as rotating group:
 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), C25A(H25A,H25B,H25C), C25B(H25D,H25E,H25F), C26A(H26A,H26B,H26C),
 C26B(H26D,H26E,H26F), C27A(H27A,H27B,H27C), C27B(H27D,H27E,H27F), C62A(H62A,
 H62B,H62C), C62B(H62D,H62E,H62F)
;
_shelx_res_checksum              36402
_shelx_hkl_checksum              63877
_olex2_submission_special_instructions 'No special instructions were received'