Cationic indium complexes for the copolymerization of functionalized epoxides with cyclic ethers and lactide
Diaz, Carlos; Ebrahimi, Tannaz; Mehrkhodavandi, Parisa; Chemical Communications  (2019) –; doi:10.1039/C8CC08858F

data_7123065
_publ_section_title
;
 Cationic indium complexes for the copolymerization of functionalized
 epoxides with cyclic ethers and lactide
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC08858F
_journal_year                    2019
_chemical_formula_moiety         'C44 H68 In N2 O4, B F4, C4 H8 O'
_chemical_formula_sum            'C48 H76 B F4 In N2 O5'
_chemical_formula_weight         962.73
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-10-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-05 deposited with the CCDC.    2019-02-21 downloaded from the CCDC.
;
_cell_angle_alpha                78.475(5)
_cell_angle_beta                 85.242(5)
_cell_angle_gamma                82.119(5)
_cell_formula_units_Z            2
_cell_length_a                   9.2636(12)
_cell_length_b                   15.978(2)
_cell_length_c                   16.814(2)
_cell_measurement_reflns_used    4716
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.38
_cell_measurement_theta_min      2.62
_cell_volume                     2411.5(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device       'Bruker-Nonius Kappa 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  0.0528
_diffrn_reflns_av_unetI/netI     0.0928
_diffrn_reflns_Laue_measured_fraction_full 0.956
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15110
_diffrn_reflns_point_group_measured_fraction_full 0.956
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        23.591
_diffrn_reflns_theta_max         23.591
_diffrn_reflns_theta_min         1.967
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.970
_exptl_absorpt_correction_T_min  0.917
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0844 before and 0.0504 after correction. The Ratio of minimum to maximum transmission is 0.9454. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.326
_exptl_crystal_description       CUBE
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.055
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.093
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         6891
_refine_ls_number_restraints     432
_refine_ls_restrained_S_all      0.999
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1280
_refine_ls_wR_factor_ref         0.1430
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4963
_reflns_number_total             6891
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08858f2.cif
_cod_data_source_block           pm191
_cod_database_code               7123065
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.970
_shelx_estimated_absorpt_t_min   0.917
_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. Restrained distances
 C47A-C48A
 1.5 with sigma of 0.01
 O3-C37 \\sim O3-C40 \\sim O4-C41 \\sim O4-C41A \\sim O4-C44 \\sim O4-C44A
 with sigma of 0.01
 C38-C37 \\sim C39-C38 \\sim C40-C39 \\sim C42-C41 \\sim C42A-C41A \\sim
C44-C43 \\sim C44A-C43A ~
 C43A-C42A \\sim C43-C42
 with sigma of 0.01
 O5A-C48A \\sim O5A-C45A \\sim O3-C37
 with sigma of 0.01
 C46A-C45A \\sim C47A-C46A \\sim C38-C37
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C41A \\sim C42A \\sim C43A \\sim C44A \\sim C41 \\sim C42 \\sim C43 \\sim C44:
within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
O5 \\sim O5A \\sim C45A \\sim C46A \\sim C47A \\sim C48A \\sim C45 \\sim C46
\\sim C47 \\sim C48: within 2A with sigma of 0.04 and sigma for terminal atoms
of 0.08
4. Rigid body (RIGU) restrains
 C41A, C42A, C43A, C44A, C41, C42, C43, C44
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O5, O5A, C45A, C46A, C47A, C48A, C45, C46, C47, C48
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C41A)=Sof(H41A)=Sof(H41B)=Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C43A)=
 Sof(H43A)=Sof(H43B)=Sof(C44A)=Sof(H44A)=Sof(H44B)=1-FVAR(1)
 Sof(C41)=Sof(H41C)=Sof(H41D)=Sof(C42)=Sof(H42C)=Sof(H42D)=Sof(C43)=Sof(H43C)=
 Sof(H43D)=Sof(C44)=Sof(H44C)=Sof(H44D)=FVAR(1)
 Sof(O5A)=Sof(C45A)=Sof(H3)=Sof(H4)=Sof(C46A)=Sof(H5)=Sof(H7)=Sof(C47A)=
 Sof(H9)=Sof(H10)=Sof(C48A)=Sof(H48A)=Sof(H48B)=1-FVAR(2)
 Sof(O5)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(C47)=
 Sof(H47A)=Sof(H47B)=Sof(C48)=Sof(H48C)=Sof(H48D)=FVAR(2)
6.a Free rotating group:
 O5(C45,C46,C47,C48)
6.b Ternary CH refined with riding coordinates:
 C16(H16), C21(H21)
6.c Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41A(H41A,H41B),
 C42A(H42A,H42B), C43A(H43A,H43B), C44A(H44A,H44B), C45(H45A,H45B), C46(H46A,
 H46B), C47(H47A,H47B), C48(H48C,H48D), C45A(H3,H4), C46A(H5,H7), C47A(H9,H10),
 C48A(H48A,H48B), C41(H41C,H41D), C42(H42C,H42D), C43(H43C,H43D), C44(H44C,H44D)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C15(H15), C29(H29), C31(H31), C36(H36)
6.e Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C23(H23A,H23B,
 H23C), C24(H24A,H24B,H24C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C)
;
_shelx_res_checksum              68901
_olex2_diffrn_ambient_temperature_device Kryoflex
_olex2_submission_special_instructions 'No special instructions were received'