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_7123063
_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
'C42.5 H64.25 In N2.75 O3.25, F6 P, 0.99(C7 H8)'
_chemical_formula_sum            'C49.2 H71.86 F6 In N2.77 O3.23 P'
_chemical_formula_weight         1013.63
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-05
_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                90
_cell_angle_beta                 100.866(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.279(5)
_cell_length_b                   15.4120(19)
_cell_length_c                   17.904(2)
_cell_measurement_reflns_used    9790
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.37
_cell_volume                     10373(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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 1.000
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Bruker-Nonius Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II 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  0.0772
_diffrn_reflns_av_unetI/netI     0.0701
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            51203
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.608
_diffrn_reflns_theta_min         1.902
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.549
_exptl_absorpt_correction_T_max  0.952
_exptl_absorpt_correction_T_min  0.495
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1595 before and 0.0997 after correction. The Ratio of minimum to maximum transmission is 0.5200. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       needle
_exptl_crystal_F_000             4242
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.119
_exptl_crystal_size_min          0.088
_refine_diff_density_max         2.292
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     714
_refine_ls_number_reflns         11948
_refine_ls_number_restraints     742
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0577
_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^)+(0.0947P)^2^+11.6175P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1536
_refine_ls_wR_factor_ref         0.1675
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9450
_reflns_number_total             11948
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08858f2.cif
_cod_data_source_block           pm182
_cod_original_formula_sum        'C49.20 H71.86 F6 In N2.77 O3.23 P'
_cod_database_code               7123063
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.953
_shelx_estimated_absorpt_t_min   0.908
_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
 C48A-C43A \\sim C44A-C43A \\sim C45A-C44A \\sim C46A-C45A \\sim C44-C43
 with sigma of 0.01
 C48A-C43A \\sim C44A-C43A \\sim C45A-C44A \\sim C46A-C45A \\sim C47A-C46A
\\sim C48A-C47A
 with sigma of 0.01
 O9-C50 \\sim O9-C53 \\sim O3-C42
 with sigma of 0.01
 C50-C51 \\sim C52-C53 \\sim C51-C52
 with sigma of 0.01
 C43-C49 \\sim C43A-C49A \\sim C43B-C49B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N3 \\sim C37 \\sim C38 \\sim C53 \\sim C51 \\sim O9 \\sim C52 \\sim C50: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C49 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C43A
\\sim C48A \\sim C47A \\sim C46A \\sim C45A \\sim C44A \\sim C49A \\sim C46B
\\sim C47B \\sim C48B \\sim C43B \\sim C44B \\sim C45B: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Uanis(C37) = Uanis(C50)
4. Rigid body (RIGU) restrains
 N3, C37, C38, C53, C51, O9, C52, C50
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C49, C43, C44, C45, C46, C47, C48, C43A, C48A, C47A, C46A, C45A, C44A, C49A,
 C46B, C47B, C48B, C43B, C44B, C45B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 1*[Sof(C49)+Sof(H49A)+Sof(H49B)+Sof(H49C)+Sof(C43)+Sof(C44)+Sof(H44)+Sof(C45)+
 Sof(H45)+Sof(C46)+Sof(H46)+Sof(C47)+Sof(H47)+Sof(C48)+Sof(H48)]+1*[Sof(C43A)+
 Sof(C48A)+Sof(H48A)+Sof(C47A)+Sof(H47A)+Sof(C46A)+Sof(H46A)+Sof(C45A)+
 Sof(H45A)+Sof(C44A)+Sof(H44A)+Sof(C49A)+Sof(H49D)+Sof(H49E)+Sof(H49F)]+1*
 [Sof(C46B)+Sof(H46B)+Sof(C47B)+Sof(H47B)+Sof(C48B)+Sof(H48B)+Sof(C43B)+
 Sof(C44B)+Sof(H44B)+Sof(C45B)+Sof(H45B)+Sof(C49B)+Sof(H49G)+Sof(H49H)+
 Sof(H49I)]=1 with esd of 0.005
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(C51)=Sof(H51A)=Sof(H51B)=Sof(O9)=Sof(C52)=
 Sof(H52A)=Sof(H52B)=Sof(C50)=Sof(H50A)=Sof(H50B)=1-FVAR(1)
 Sof(N3)=Sof(C37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=FVAR(1)
 Sof(C49)=Sof(H49A)=Sof(H49B)=Sof(H49C)=Sof(C43)=Sof(C44)=Sof(H44)=Sof(C45)=
 Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=FVAR(2)
 Sof(C43A)=Sof(C48A)=Sof(H48A)=Sof(C47A)=Sof(H47A)=Sof(C46A)=Sof(H46A)=
 Sof(C45A)=Sof(H45A)=Sof(C44A)=Sof(H44A)=Sof(C49A)=Sof(H49D)=Sof(H49E)=
 Sof(H49F)=FVAR(3)
 Sof(C46B)=Sof(H46B)=Sof(C47B)=Sof(H47B)=Sof(C48B)=Sof(H48B)=Sof(C43B)=
 Sof(C44B)=Sof(H44B)=Sof(C45B)=Sof(H45B)=Sof(C49B)=Sof(H49G)=Sof(H49H)=
 Sof(H49I)=FVAR(4)
6.a Free rotating group:
 C49(C43,C44,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), C39(H39A,
 H39B), C40(H40A,H40B), C41(H41A,H41B), C42(H42A,H42B), C53(H53A,H53B),
 C51(H51A,H51B), C52(H52A,H52B), C50(H50A,H50B)
6.d Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C15(H15), C22(H22), C25(H25), C27(H27), C44(H44), C45(H45),
 C46(H46), C47(H47), C48(H48), C48A(H48A), C47A(H47A), C46A(H46A), C45A(H45A),
 C44A(H44A), C46B(H46B), C47B(H47B), C48B(H48B), C44B(H44B), C45B(H45B)
6.e Fitted hexagon refined as free rotating group:
 C43A(C48A,C47A,C46A,C45A,C44A), C46B(C47B,C48B,C43B,C44B,C45B)
6.f Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C12(H12A,H12B,H12C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C30(H30A,H30B,H30C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C38(H38A,H38B,H38C), C49(H49A,H49B,H49C), C49A(H49D,H49E,H49F),
 C49B(H49G,H49H,H49I)
;
_shelx_res_checksum              67807
_olex2_diffrn_ambient_temperature_device Kryoflex
_olex2_submission_special_instructions 'No special instructions were received'