Cationic indium catalysts for ring opening polymerization: tuning reactivity with hemilabile ligands
Goonesinghe, Chatura; Roshandel, Hootan; Diaz, Carlos; Jung, Hyuk-Joon; Nyamayaro, Kudzanai; Ezhova, Maria; Mehrkhodavandi, Parisa; Chemical Science 11 (2020) 6485–6491; doi:10.1039/D0SC01291B

data_1557868
_publ_section_title
;
 Cationic indium catalysts for ring opening polymerization: tuning
 reactivity with hemilabile ligands
;
_journal_issue                   25
_journal_name_full               'Chemical Science'
_journal_page_first              6485
_journal_page_last               6491
_journal_paper_doi               10.1039/D0SC01291B
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C48 H64 In N2 O4, C32 H12 B F24, 2(C4 H8 O)'
_chemical_formula_sum            'C88 H92 B F24 In N2 O6'
_chemical_formula_weight         1855.26
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-29
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2020-03-02 deposited with the CCDC.	2020-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                80.163(3)
_cell_angle_beta                 76.369(3)
_cell_angle_gamma                85.869(3)
_cell_formula_units_Z            2
_cell_length_a                   12.616(3)
_cell_length_b                   13.343(3)
_cell_length_c                   26.255(5)
_cell_measurement_reflns_used    9841
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.25
_cell_measurement_theta_min      2.23
_cell_volume                     4229.7(16)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_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
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.988
_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  0.1605
_diffrn_reflns_av_unetI/netI     0.0668
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_number            18759
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.280
_diffrn_reflns_theta_min         1.550
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           0.99
_diffrn_source_power             0.0495
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.387
_exptl_absorpt_correction_T_max  0.9977
_exptl_absorpt_correction_T_min  0.9887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 180047 reflections, Rint = 0.2262
 (72648 with I > 3sig(I), Rint = 0.1951)
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.457
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.028
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.006
_refine_diff_density_max         2.236
_refine_diff_density_min         -1.203
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1163
_refine_ls_number_reflns         18759
_refine_ls_number_restraints     100
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0983
_refine_ls_R_factor_gt           0.0794
_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^)+(0.0854P)^2^+20.1133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2047
_refine_ls_wR_factor_ref         0.2140
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14576
_reflns_number_total             18759
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01291b2.cif
_cod_data_source_block           Complex2bTHF
_cod_depositor_comments
;Adding full bibliography for 1557864--1557868.cif.

 Adding full bibliography for 1557864--1557868.cif.
;
_cod_original_cell_volume        4229.9(14)
_cod_database_code               1557868
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.998
_shelx_estimated_absorpt_t_min   0.989
_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
 N1-C40B \\sim N1-C40A
 with sigma of 0.02
 C41-C40B \\sim C41-C40A
 with sigma of 0.02
 C28-C29A \\sim C28-C29B
 with sigma of 0.02
 C30-C29A \\sim C30-C29B
 with sigma of 0.02
 N2-C26B \\sim N2-C26A
 with sigma of 0.02
 C27-C26B \\sim C27-C26A
 with sigma of 0.02
 C31-C26B \\sim C31-C26A
 with sigma of 0.02
 F24A-C80 \\sim F24B-C80
 with sigma of 0.02
 F22A-C80 \\sim F22B-C80
 with sigma of 0.02
 C80-F23A \\sim C80-F23B
 with sigma of 0.02
 F22A-F23A \\sim F22A-F24A \\sim F22B-F23B \\sim F22B-F24B \\sim F23A-F24A
\\sim F23B-F24B
 with sigma of 0.04
 C80-F22A \\sim C80-F22B \\sim C80-F23A \\sim C80-F23B \\sim C80-F24A \\sim
C80-F24B \\sim C80-C75
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 F22A, F23A, F24A, C75, C80
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F22B, F23B, F24B, C75, C80
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C40A)=Sof(H40A)=Sof(H40B)=1-FVAR(1)
 Sof(C40B)=Sof(H40C)=Sof(H40D)=FVAR(1)
 Sof(H28C)=Sof(H28D)=Sof(C29B)=Sof(H29C)=Sof(H29D)=Sof(H30C)=Sof(H30D)=1-FVAR(2)
 Sof(H28A)=Sof(H28B)=Sof(C29A)=Sof(H29A)=Sof(H29B)=Sof(H30A)=Sof(H30B)=FVAR(2)
 Sof(C26A)=Sof(H26A)=Sof(H27C)=Sof(H27D)=1-FVAR(3)
 Sof(C26B)=Sof(H26B)=Sof(H27A)=Sof(H27B)=FVAR(3)
 Sof(F22B)=Sof(F23B)=Sof(F24B)=1-FVAR(4)
 Sof(F22A)=Sof(F23A)=Sof(F24A)=FVAR(4)
5.a Ternary CH refined with riding coordinates:
 C26A(H26A), C26B(H26B), C33(H33)
5.b Secondary CH2 refined with riding coordinates:
 C0AA(H0AA,H0AB), C1AA(H1AA,H1AB), C2AA(H2AA,H2AB), C3AA(H3AA,H3AB), C27(H27A,
 H27B), C27(H27C,H27D), C28(H28A,H28B), C28(H28C,H28D), C29A(H29A,H29B),
 C29B(H29C,H29D), C30(H30A,H30B), C30(H30C,H30D), C32(H32A,H32B), C40A(H40A,
 H40B), C40B(H40C,H40D), C45(H45A,H45B), C46(H46A,H46B), C47(H47A,H47B),
 C48(H48A,H48B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B),
  C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C11(H11), C13(H13), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C25(H25), C42(H42), C43(H43), C44(H44),
  C50(H50), C52(H52), C54(H54), C58(H58), C60(H60), C62(H62), C66(H66),
 C68(H68), C70(H70), C74(H74), C76(H76), C78(H78)
5.d Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C)
;
_shelx_res_checksum              6045
_olex2_submission_special_instructions 'No special instructions were received'