Air- and Moisture-Stable Indium Salan Catalysts for Living Multiblock PLA Formation in Air
Ebrahimi, Tannaz; Aluthge, Dinesh C.; Patrick, Brian O.; Hatzikiriakos, Savvas G.; Mehrkhodavandi, Parisa; ACS Catalysis 7 (2017) 6413–; doi:10.1021/acscatal.7b01939

data_4514284
_publ_section_title
;
 Air- and Moisture-Stable Indium Salan Catalysts for Living Multiblock PLA
 Formation in Air
;
_journal_issue                   10
_journal_name_full               'ACS Catalysis'
_journal_page_first              6413
_journal_paper_doi               10.1021/acscatal.7b01939
_journal_volume                  7
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C72 H112 In2 N4 O6, 2(C7 H8)'
_chemical_formula_sum            'C86 H128 In2 N4 O6'
_chemical_formula_weight         1543.56
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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             2017-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_cell_angle_alpha                74.0920(10)
_cell_angle_beta                 87.9700(10)
_cell_angle_gamma                65.2360(10)
_cell_formula_units_Z            1
_cell_length_a                   12.0666(5)
_cell_length_b                   12.3213(6)
_cell_length_c                   18.3525(8)
_cell_measurement_reflns_used    5732
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.11
_cell_measurement_theta_min      2.32
_cell_volume                     2372.91(19)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 0.943
_diffrn_measured_fraction_theta_max 0.936
_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  0.0564
_diffrn_reflns_av_unetI/netI     0.1565
_diffrn_reflns_Laue_measured_fraction_full 0.943
_diffrn_reflns_Laue_measured_fraction_max 0.936
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            16202
_diffrn_reflns_point_group_measured_fraction_full 0.797
_diffrn_reflns_point_group_measured_fraction_max 0.776
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.234
_diffrn_reflns_theta_min         1.866
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.531
_exptl_absorpt_correction_T_max  0.979
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0744 before and 0.0617 after correction. The Ratio of minimum to maximum transmission is 0.9109. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.080
_exptl_crystal_description       BLADE
_exptl_crystal_F_000             818
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.077
_refine_diff_density_min         -0.619
_refine_diff_density_rms         0.079
_refine_ls_abs_structure_details
;
 Flack x determined using 2887 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.07(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.830
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     957
_refine_ls_number_reflns         14819
_refine_ls_number_restraints     1774
_refine_ls_restrained_S_all      0.796
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0533
_refine_ls_shift/su_max          0.027
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0948
_refine_ls_wR_factor_ref         0.1020
_reflns_Friedel_coverage         0.656
_reflns_Friedel_fraction_full    0.651
_reflns_Friedel_fraction_max     0.615
_reflns_number_gt                9961
_reflns_number_total             14819
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b01939_si_002.cif
_cod_data_source_block           pm194_sq_3
_cod_original_cell_volume        2372.91(18)
_cod_database_code               4514284
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.979
_shelx_estimated_absorpt_t_min   0.816
_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
 C30-C29 \\sim C29-C32 \\sim C31-C29
 with sigma of 0.01
 C29-C32 \\sim C30-C29 \\sim C31-C29
 with sigma of 0.01
 C29-C30A \\sim C29-C32A \\sim C29-C31A
 with sigma of 0.01
 C29-C32 \\sim C29-C30A \\sim C30-C29 \\sim C29-C32A \\sim C31-C29 \\sim
C29-C31A
 with sigma of 0.01
 C68-C67 \\sim C68-C66 \\sim C67-C66 \\sim C67A-C66A \\sim C67A-C68A \\sim
C66A-C68A
 with sigma of 0.04
 C65-C61 \\sim C65-C68 \\sim C65-C67 \\sim C65-C66 \\sim C65-C67A \\sim
C65-C66A \\sim C65-C68A
 with sigma of 0.02
 C31-C30 \\sim C31-C32 \\sim C30-C32 \\sim C30A-C32A \\sim C31A-C32A
 with sigma of 0.04
 C29-C31 \\sim C29-C30 \\sim C29-C30A \\sim C29-C31A \\sim C29-C32 \\sim
C29-C25 \\sim C29-C32A
 with sigma of 0.02
 C67A-C66A \\sim C67A-C68A \\sim C66A-C68A
 with sigma of 0.04
 C65-C61 \\sim C65-C67A \\sim C65-C66A \\sim C65-C68A
 with sigma of 0.02
 C30A-C32A \\sim C31A-C32A
 with sigma of 0.04
 C29-C30A \\sim C29-C31A \\sim C29-C32A \\sim C29-C25
 with sigma of 0.02
 C68-C67 \\sim C68-C66 \\sim C67-C66
 with sigma of 0.04
 C65-C61 \\sim C65-C68 \\sim C65-C67 \\sim C65-C66
 with sigma of 0.02
 C31-C30 \\sim C31-C32 \\sim C30-C32
 with sigma of 0.04
 C29-C31 \\sim C29-C30 \\sim C29-C32 \\sim C29-C25
 with sigma of 0.02
 C30-C31 \\sim C30-C32 \\sim C31-C32 \\sim C32A-C30A \\sim C32A-C31A
 with sigma of 0.04
 C29-C25 \\sim C29-C30 \\sim C29-C31 \\sim C29-C32 \\sim C29-C32A \\sim
C29-C30A \\sim C29-C31A
 with sigma of 0.02
 C31-C29 \\sim C29-C31A \\sim C29-C32 \\sim C29-C30A \\sim C30-C29 \\sim
C29-C32A
 with sigma of 0.01
 C65-C66 \\sim C65-C66A \\sim C65-C67 \\sim C65-C67A \\sim C68-C65 \\sim
C68A-C65
 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(C31) = Uanis(C32) = Uanis(C30)
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(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=1-FVAR(1)
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(C67A)=Sof(H67D)=Sof(H67E)=Sof(H67F)=Sof(C66A)=Sof(H66D)=Sof(H66E)=
 Sof(H66F)=Sof(C68A)=Sof(H68D)=Sof(H68E)=Sof(H68F)=1-FVAR(2)
 Sof(C67)=Sof(H67A)=Sof(H67B)=Sof(H67C)=Sof(C66)=Sof(H66A)=Sof(H66B)=Sof(H66C)=
 Sof(C68)=Sof(H68A)=Sof(H68B)=Sof(H68C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C57(H57), C52(H52), C21(H21), C16(H16)
6.b Secondary CH2 refined with riding coordinates:
 C54(H54A,H54B), C53(H53A,H53B), C55(H55A,H55B), C56(H56A,H56B), C58(H58A,
 H58B), C22(H22A,H22B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C1(H1A,H1B), C37(H37A,H37B)
6.c Me refined with riding coordinates:
 C68(H68A,H68B,H68C), C68A(H68D,H68E,H68F)
6.d Aromatic/amide H refined with riding coordinates:
 C41(H41), C39(H39), C60(H60), C62(H62), C5(H5), C3(H3A), C26(H26), C24(H24),
 C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C81(H81), C82(H82), C83(H83),
  C84(H84), C85(H85)
6.e Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C50(H50A,H50B,
 H50C), C51(H51A,H51B,H51C), C49(H49A,H49B,H49C), C67(H67A,H67B,H67C),
 C67A(H67D,H67E,H67F), C66(H66A,H66B,H66C), C66A(H66D,H66E,H66F), C70(H70A,H70B,
 H70C), C72(H72A,H72B,H72C), C71(H71A,H71B,H71C), C13(H13A,H13B,H13C), C14(H14A,
 H14B,H14C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C),
 C9(H9A,H9B,H9C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C),
  C32(H32A,H32B,H32C), C32A(H32D,H32E,H32F), C31(H31A,H31B,H31C), C31A(H31D,
 H31E,H31F), C30(H30A,H30B,H30C), C30A(H30D,H30E,H30F), C79(H79A,H79B,H79C),
 C86(H86A,H86B,H86C)
;
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              86036
_shelx_hkl_checksum              16314
_shelx_fab_checksum              57150
_olex2_diffrn_ambient_temperature_device Kryoflex
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in oil'
_olex2_submission_original_sample_id RR/RR-3
_olex2_submission_special_instructions 'No special instructions were received'