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_4517709
_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         'C27 H50 In N2 O Si, C4 H10 O, F6 P'
_chemical_formula_sum            'C31 H60 F6 In N2 O2 P Si'
_chemical_formula_weight         780.69
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-03-05
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.750(7)
_cell_length_b                   14.750(7)
_cell_length_c                   35.67(2)
_cell_measurement_reflns_used    9476
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      32.175
_cell_measurement_theta_min      2.986
_cell_volume                     7760(7)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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  (Sheldrick, 2015)'
_diffrn_ambient_temperature      90.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.934
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0232
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.934
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -51
_diffrn_reflns_number            96058
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.933
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         32.597
_diffrn_reflns_theta_min         2.762
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_T_max  0.7464
_exptl_absorpt_correction_T_min  0.6946
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0388 before and 0.0365 after correction. The Ratio of minimum to maximum transmission is 0.9306. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_description       irregular
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.674
_refine_diff_density_min         -0.464
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.358(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.147
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     444
_refine_ls_number_reflns         12991
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0273
_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^)+(0.0189P)^2^+4.3626P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0581
_refine_ls_wR_factor_ref         0.0589
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.932
_reflns_number_gt                12336
_reflns_number_total             12991
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs0c01365_si_002.cif
_cod_data_source_block           pm092(complex4)
_cod_depositor_comments
'Adding full bibliography for 4517706--4517710.cif.'
_cod_original_cell_volume        7762(9)
_cod_database_code               4517709
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.978
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.642(14)
 0.358(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C28-C29 \\sim C30-C31
 with sigma of 0.01
 C29-O3 \\sim C30-O3
 with sigma of 0.01
 C28-O3 \\sim C31-O3
 with sigma of 0.01
 C31B-C30B \\sim C29B-C28B
 with sigma of 0.01
 C30B-O3B \\sim C29B-O3B
 with sigma of 0.01
 C31B-O3B \\sim C28B-O3B
 with sigma of 0.01
4. Others
 Sof(C28B)=Sof(H28D)=Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29C)=Sof(H29D)=
 Sof(O3B)=Sof(C30B)=Sof(H30C)=Sof(H30D)=Sof(C31B)=Sof(H31D)=Sof(H31E)=Sof(H31F)=
 1-FVAR(1)
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(O3)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1), C6(H6), N1(H1A)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C7(H7A,H7B), C24(H24A,
 H24B), C29(H29A,H29B), C30(H30A,H30B), C29B(H29C,H29D), C30B(H30C,H30D)
5.c Me refined with riding coordinates:
 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), C23(H23A,
 H23B,H23C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C),
 C28(H28A,H28B,H28C), C31(H31A,H31B,H31C), C28B(H28D,H28E,H28F), C31B(H31D,H31E,
 H31F)
5.d Aromatic/amide H refined with riding coordinates:
 C10(H10), C12(H12)
;
_shelx_res_checksum              54424
_shelx_hkl_checksum              48524
_olex2_submission_special_instructions 'No special instructions were received'