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_7123064
_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         'F6 Sb, C44 H68 In N2 O4'
_chemical_formula_sum            'C44 H68 F6 In N2 O4 Sb'
_chemical_formula_weight         1039.57
_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             2018-10-31
_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                 102.098(6)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   27.115(3)
_cell_length_b                   10.3591(9)
_cell_length_c                   41.932(4)
_cell_measurement_reflns_used    9937
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.53
_cell_measurement_theta_min      2.67
_cell_volume                     11517(2)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker-Nonius Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0354
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            60629
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        22.478
_diffrn_reflns_theta_max         22.478
_diffrn_reflns_theta_min         1.645
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.922
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1736 before and 0.0532 after correction. The Ratio of minimum to maximum transmission is 0.8941. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.199
_exptl_crystal_description       needle
_exptl_crystal_F_000             4256
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.821
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     643
_refine_ls_number_reflns         7517
_refine_ls_number_restraints     1285
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.0869
_refine_ls_R_factor_gt           0.0621
_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^)+(0.0851P)^2^+38.0158P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.1796
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5277
_reflns_number_total             7517
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc08858f2.cif
_cod_data_source_block           pm193mc_sq_sq_sq
_cod_database_code               7123064
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.973
_shelx_estimated_absorpt_t_min   0.656
_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
 C13-C12 \\sim C14-C12 \\sim C11-C12 \\sim C11A-C12 \\sim C13A-C12 \\sim
C14A-C12
 with sigma of 0.02
 C14A-C11A \\sim C11A-C13A \\sim C13A-C14A
 with sigma of 0.01
 C42A-C41A \\sim C42-C41 \\sim C43-C42A \\sim C43A-C42 \\sim C44-C43A \\sim
C44A-C43
 with sigma of 0.01
 O3-C44A \\sim O3-C44 \\sim O3-C41A \\sim O3-C41
 with sigma of 0.01
 C36-C34 \\sim C35-C34 \\sim C34-C33 \\sim C36A-C34A \\sim C35A-C34A \\sim
C34A-C33A
 with sigma of 0.01
 C27-C34 \\sim C27-C34A
 with sigma of 0.01
 Sb1-F4 \\sim Sb1-F6 \\sim Sb1-F5 \\sim Sb1-F1 \\sim Sb1-F3 \\sim Sb1-F2
 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
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(C11A)=Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C13A)=Sof(H13D)=Sof(H13E)=
 Sof(H13F)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=1-FVAR(1)
 Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=
 Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(1)
 Sof(C42A)=Sof(H42C)=Sof(H42D)=Sof(C43)=Sof(H43C)=Sof(H43D)=1-FVAR(2)
 Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=FVAR(2)
 Sof(C33A)=Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34A)=Sof(C35A)=Sof(H35D)=
 Sof(H35E)=Sof(H35F)=Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(3)
 Sof(C33)=Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34)=Sof(C35)=Sof(H35A)=Sof(H35B)=
 Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=FVAR(3)
 Fixed Sof: C41(0.5) H41A(0.5) H41B(0.5) C44(0.5) H44A(0.5) H44B(0.5)
 C41A(0.5) H41C(0.5) H41D(0.5) C44A(0.5) H44C(0.5) H44D(0.5)
6.a Ternary CH refined with riding coordinates:
 C15(H15), C20(H20)
6.b Secondary CH2 refined with riding coordinates:
 C16(H16A,H16B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C37(H37A,
 H37B), C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B), C41(H41A,H41B),
 C42(H42A,H42B), C43A(H43A,H43B), C44(H44A,H44B), C41A(H41C,H41D), C42A(H42C,
 H42D), C43(H43C,H43D), C44A(H44C,H44D)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C8(H8), C21(H21), C22(H22), C24(H24), C26(H26)
6.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C11(H11A,H11B,H11C),
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C29(H29A,H29B,H29C), C31(H31A,H31B,
 H31C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C11A(H11D,H11E,H11F), C13A(H13D,H13E,H13F), C14A(H14D,H14E,H14F),
 C33A(H33D,H33E,H33F), C35A(H35D,H35E,H35F), C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              80108
_shelx_fab_checksum              38772
_platon_squeeze_void_probe_radius 1.20
_olex2_diffrn_ambient_temperature_device Kryoflex
_olex2_submission_original_sample_id CD-1-154-11
_olex2_submission_special_instructions 'No special instructions were received'