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_1557865
_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         'C44 H59 In N2 O2'
_chemical_formula_sum            'C44 H59 In N2 O2'
_chemical_formula_weight         762.75
_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             2019-11-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-03-02 deposited with the CCDC.	2020-04-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 117.891(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.5732(15)
_cell_length_b                   13.8493(11)
_cell_length_c                   18.4226(15)
_cell_measurement_reflns_used    9858
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.63
_cell_measurement_theta_min      2.22
_cell_volume                     3962.8(6)
_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      296.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            63957
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.627
_diffrn_reflns_theta_min         1.930
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7005
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0531 before and 0.0467 after correction.
The Ratio of minimum to maximum transmission is 0.9389.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.201
_refine_diff_density_min         -1.115
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     481
_refine_ls_number_reflns         12154
_refine_ls_number_restraints     860
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0292P)^2^+5.6646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0887
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9833
_reflns_number_total             12154
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc01291b2.cif
_cod_data_source_block           Complex1b
_cod_depositor_comments
;Adding full bibliography for 1557864--1557868.cif.

 Adding full bibliography for 1557864--1557868.cif.
;
_cod_database_code               1557865
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.838
_olex2_refinement_description
;
1. 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
2. Restrained distances
 O2B-C41 \\sim O2A-C41
 with sigma of 0.01
 C41-C42B \\sim C42A-C41
 with sigma of 0.01
 O2B-C44B \\sim O2A-C44A
 with sigma of 0.01
 C43B-C42B \\sim C42A-C43A
 with sigma of 0.01
 C44A-C43A \\sim C43B-C44B
 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
Uanis(C42B) = Uanis(O2A)
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(O2A)=Sof(C42A)=Sof(H42A)=Sof(C43A)=Sof(H43A)=Sof(C44A)=Sof(H44A)=1-FVAR(1)
 Sof(O2B)=Sof(C42B)=Sof(H42B)=Sof(C43B)=Sof(H43B)=Sof(C44B)=Sof(H44B)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 N1(H1), C26(H26), C31(H31), C33(H33), C37(H37)
6.b Secondary CH2 refined with riding coordinates:
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,
 H32B), C36(H36A,H36B), C40(H40A,H40B)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1A), C2(H2), C3(H3), C5(H5), C6(H6), C11(H11), C13(H13), C16(H16),
 C17(H17), C18(H18), C20(H20), C21(H21), C25(H25), C42A(H42A), C42B(H42B),
 C43A(H43A), C43B(H43B), C44A(H44A), C44B(H44B)
6.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), C38(H38A,H38B,H38C), C39(H39A,H39B,
 H39C)
;
_olex2_submission_special_instructions 'No special instructions were received'