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_4514283
_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 H111 Cl In2 N4 O5, 3.56(C7 H8)'
_chemical_formula_sum            'C96.95 H139.51 Cl In2 N4 O5'
_chemical_formula_weight         1706.12
_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                86.040(10)
_cell_angle_beta                 73.489(9)
_cell_angle_gamma                64.932(10)
_cell_formula_units_Z            1
_cell_length_a                   12.196(4)
_cell_length_b                   12.295(4)
_cell_length_c                   18.618(6)
_cell_measurement_reflns_used    9832
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.42
_cell_measurement_theta_min      2.28
_cell_volume                     2420.3(14)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0695
_diffrn_reflns_av_unetI/netI     0.0640
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            42504
_diffrn_reflns_point_group_measured_fraction_full 0.915
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_theta_full        22.567
_diffrn_reflns_theta_max         22.567
_diffrn_reflns_theta_min         1.832
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1134 before and 0.0866 after correction. The Ratio of minimum to maximum transmission is 0.7888. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.170
_exptl_crystal_description       irregular
_exptl_crystal_F_000             904
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.332
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.141
_refine_ls_abs_structure_details
;
 Flack x determined using 4194 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.064(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     955
_refine_ls_number_reflns         11685
_refine_ls_number_restraints     1773
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0853
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1371P)^2^+11.8255P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2324
_refine_ls_wR_factor_ref         0.2427
_reflns_Friedel_coverage         0.890
_reflns_Friedel_fraction_full    0.862
_reflns_Friedel_fraction_max     0.862
_reflns_number_gt                10137
_reflns_number_total             11685
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b01939_si_002.cif
_cod_data_source_block           pm195n_2
_cod_original_cell_volume        2420.5(13)
_cod_database_code               4514283
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.874
_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
 C29-C30 \\sim C31-C29 \\sim C29-C32
 with sigma of 0.02
 C31-C29 \\sim C29-C32 \\sim C29-C30
 with sigma of 0.02
 C25-C30 \\sim C32-C31 \\sim C30-C31
 with sigma of 0.02
 C29-C25 \\sim C29-C32 \\sim C29-C30 \\sim C29-C31
 with sigma of 0.01
 C31-C29 \\sim C30A-C29 \\sim C30-C29 \\sim C31A-C29 \\sim C32-C29 \\sim
C32A-C29
 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(C66) = Uanis(C67) = Uanis(C68)
Uanis(C51) = Uanis(C49) = Uanis(C50)
Uanis(C11) = Uanis(C9) = Uanis(C10)
Uanis(C32) = Uanis(C30) = Uanis(C31)
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(C93)=Sof(H93A)=Sof(H93B)=Sof(H93C)=Sof(C87)=Sof(C88)=Sof(H88)=Sof(C89)=
 Sof(H89)=Sof(C90)=Sof(H90)=Sof(C91)=Sof(H91)=Sof(C92)=Sof(H92)=FVAR(1)
 Sof(C100)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C94)=Sof(C95)=Sof(H95)=Sof(C96)=
 Sof(H96)=Sof(C97)=Sof(H97)=Sof(C98)=Sof(H98)=Sof(C99)=Sof(H99)=FVAR(2)
 Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(C30A)=Sof(H30D)=Sof(H30E)=
 Sof(H30F)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=1-FVAR(3)
 Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=
 Sof(C32)=Sof(H32A)=Sof(H32B)=Sof(H32C)=FVAR(3)
6.a Free rotating group:
 C79(C73,C74,C75,C76,C77,C78), C86(C80,C81,C82,C83,C84,C85), C93(C87,C88,C89,
 C90,C91,C92), C100(C94,C95,C96,C97,C98,C99)
6.b Ternary CH refined with riding coordinates:
 N1(H1), N2(H2), N3(H3), N4(H4), C16(H16), C21(H21), C52(H52), C57(H57)
6.c Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B),
 C22(H22A,H22B), C37(H37A,H37B), C54(H54A,H54B), C55(H55A,H55B), C56(H56A,H56B),
  C53(H53A,H53B)
6.d Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C100(H10D,H10E,
 H10F), C31A(H31D,H31E,H31F), C30A(H30D,H30E,H30F), C32A(H32D,H32E,H32F)
6.e Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C24(H24), C26(H26), C39(H39), C41(H41), C58(H58), C60(H60),
 C62(H62), C74(H74), C75(H75), C76(H76), C77(H77), C78(H78), C81(H81), C82(H82),
  C83(H83), C84(H84), C85(H85), C88(H88), C89(H89), C90(H90), C91(H91),
 C92(H92), C95(H95), C96(H96), C97(H97), C98(H98), C99(H99)
6.f Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C45(H45A,H45B,H45C), C46(H46A,H46B,H46C),
 C47(H47A,H47B,H47C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C51(H51A,H51B,
 H51C), C66(H66A,H66B,H66C), C67(H67A,H67B,H67C), C68(H68A,H68B,H68C), C70(H70A,
 H70B,H70C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C79(H79A,H79B,H79C),
 C86(H86A,H86B,H86C), C93(H93A,H93B,H93C)
;
_shelx_res_checksum              57426
_shelx_hkl_checksum              15979
_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-2
_olex2_submission_special_instructions 'No special instructions were received'