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_4517707
_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 H59 In N2 O Si2'
_chemical_formula_sum            'C31 H59 In N2 O Si2'
_chemical_formula_weight         646.80
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-06
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.103(2)
_cell_angle_gamma                90
_cell_formula_units_Z            16
_cell_length_a                   16.279(3)
_cell_length_b                   23.517(4)
_cell_length_c                   37.715(6)
_cell_measurement_reflns_used    9842
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      27.366
_cell_measurement_theta_min      2.33
_cell_volume                     14328(4)
_computing_cell_refinement       'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS, 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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0880
_diffrn_reflns_av_unetI/netI     0.0846
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_number            143702
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.166
_diffrn_reflns_theta_min         1.023
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5586
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0811 before and 0.0665 after correction. The Ratio of minimum to maximum transmission is 0.7492. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       prism
_exptl_crystal_F_000             5504
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.019
_refine_diff_density_max         0.991
_refine_diff_density_min         -1.261
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1389
_refine_ls_number_reflns         31616
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0227P)^2^+18.1805P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0859
_refine_ls_wR_factor_ref         0.0981
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21465
_reflns_number_total             31616
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c01365_si_002.cif
_cod_data_source_block           pm203(complex2)
_cod_depositor_comments
'Adding full bibliography for 4517706--4517710.cif.'
_cod_database_code               4517707
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.986
_shelx_estimated_absorpt_t_min   0.909
_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.a Ternary CH refined with riding coordinates:
 C1A(H1A), C2A(H2A), C1C(H1C), C2C(H2C), C1D(H1D), C2D(H2D), C1B(H1B), C2B(H2B)
2.b Secondary CH2 refined with riding coordinates:
 C3A(H3AA,H3AB), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C24A(H24A,
 H24B), C25A(H25A,H25B), C3C(H3CA,H3CB), C4C(H4CA,H4CB), C5C(H5CA,H5CB),
 C6C(H6CA,H6CB), C24C(H24C,H24D), C25C(H25C,H25D), C3D(H3DA,H3DB), C4D(H4DA,
 H4DB), C5D(H5DA,H5DB), C6D(H6DA,H6DB), C24D(H24E,H24F), C25D(H25E,H25F),
 C3B(H3BA,H3BB), C4B(H4BA,H4BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C24B(H24G,
 H24H), C25B(H25G,H25H)
2.c Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C10A(H10A), C12A(H12A), C7C(H7C), C10C(H10C), C12C(H12C), C7D(H7D),
 C10D(H10D), C12D(H12D), C7B(H7B), C10B(H10B), C12B(H12B)
2.d Idealised Me refined as rotating group:
 C16A(H16A,H16B,H16C), C17A(H17A,H17B,H17C), C18A(H18A,H18B,H18C), C19A(H19A,
 H19B,H19C), C20A(H20A,H20B,H20C), C21A(H21A,H21B,H21C), C22A(H22A,H22B,H22C),
 C23A(H23A,H23B,H23C), C26A(H26A,H26B,H26C), C27A(H27A,H27B,H27C), C28A(H28A,
 H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C31A(H31A,H31B,H31C),
 C16C(H16D,H16E,H16F), C17C(H17D,H17E,H17F), C18C(H18D,H18E,H18F), C19C(H19D,
 H19E,H19F), C20C(H20D,H20E,H20F), C21C(H21D,H21E,H21F), C22C(H22D,H22E,H22F),
 C23C(H23D,H23E,H23F), C26C(H26D,H26E,H26F), C27C(H27D,H27E,H27F), C28C(H28D,
 H28E,H28F), C29C(H29D,H29E,H29F), C30C(H30D,H30E,H30F), C31C(H31D,H31E,H31F),
 C16D(H16G,H16H,H16I), C17D(H17G,H17H,H17I), C18D(H18G,H18H,H18I), C19D(H19G,
 H19H,H19I), C20D(H20G,H20H,H20I), C21D(H21G,H21H,H21I), C22D(H22G,H22H,H22I),
 C23D(H23G,H23H,H23I), C26D(H26G,H26H,H26I), C27D(H27G,H27H,H27I), C28D(H28G,
 H28H,H28I), C29D(H29G,H29H,H29I), C30D(H30G,H30H,H30I), C31D(H31G,H31H,H31I),
 C16B(H16J,H16K,H16L), C17B(H17J,H17K,H17L), C18B(H18J,H18K,H18L), C19B(H19J,
 H19K,H19L), C20B(H20J,H20K,H20L), C21B(H21J,H21K,H21L), C22B(H22J,H22K,H22L),
 C23B(H23J,H23K,H23L), C26B(H26J,H26K,H26L), C27B(H27J,H27K,H27L), C28B(H28J,
 H28K,H28L), C29B(H29J,H29K,H29L), C30B(H30J,H30K,H30L), C31B(H31J,H31K,H31L)
;
_shelx_res_checksum              27024
_shelx_hkl_checksum              31521
_olex2_submission_special_instructions 'No special instructions were received'