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_4514285
_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_formula_moiety         'C72 H104 In2 N4 O6'
_chemical_formula_sum            'C72 H104 In2 N4 O6'
_chemical_formula_weight         1351.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-15
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_cell_angle_alpha                90
_cell_angle_beta                 99.726(8)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   17.557(6)
_cell_length_b                   19.409(8)
_cell_length_c                   12.845(4)
_cell_measurement_reflns_used    5313
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.50
_cell_measurement_theta_min      2.65
_cell_volume                     4314(3)
_computing_cell_refinement       'SAINT v7.60A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.60A (Bruker, 2009)'
_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    'SIR2002 (Burla et al., 2007)'
_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 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.106
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5700
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_theta_full        22.728
_diffrn_reflns_theta_max         22.728
_diffrn_reflns_theta_min         2.406
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.236
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/2 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.1222 before and 0.0813 after correction.
 The Ratio of minimum to maximum transmission is 0.25.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.1525 before and 0.0930 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present

Final HKLF 4 output contains 69975 reflections, Rint = 0.1056
 (28189 with I > 3sig(I), Rint = 0.0842)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1420
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.285
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         5700
_refine_ls_number_restraints     1962
_refine_ls_restrained_S_all      0.932
_refine_ls_R_factor_all          0.1051
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0960P)^2^+15.8194P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1893
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3785
_reflns_number_total             5700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b01939_si_002.cif
_cod_data_source_block           pm077_sq_4
_cod_database_code               4514285
_shelx_shelxl_version_number     2017/1
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.681(5)
 0.319(5)
2. 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
3. Restrained distances
 C16-C21 \\sim C21-C20 \\sim C20-C19 \\sim C19-C18 \\sim C18-C17 \\sim C17-C16
 with sigma of 0.01
 C16A-C21A \\sim C21A-C20A \\sim C20A-C19A \\sim C19A-C18A \\sim C18A-C17A
\\sim C17A-C16A
 with sigma of 0.01
 C9-C10 \\sim C10-C11 \\sim C11-C9 \\sim C9A-C11A
 with sigma of 0.01
 C1-C2 \\sim C1A-C2A
 with sigma of 0.01
 C29-C31 \\sim C29A-C31A \\sim C29-C32 \\sim C29A-C32A
 with sigma of 0.01
 C27-C33 \\sim C27A-C33A
 with sigma of 0.01
 C25-C29 \\sim C25A-C29A
 with sigma of 0.01
4. 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(C1) = Uanis(C1A)
Uanis(C8) = Uanis(C8A)
Uanis(C17) = Uanis(C17A)
Uanis(C7) = Uanis(C7A)
Uanis(C6) = Uanis(C6A)
Uanis(C29) = Uanis(C29A)
Uanis(C31) = Uanis(C31A)
Uanis(C32) = Uanis(C32A)
Uanis(C5) = Uanis(C5A)
Uanis(C4) = Uanis(C4A)
Uanis(C3) = Uanis(C3A)
Uanis(C2) = Uanis(C2A)
Uanis(C28) = Uanis(C28A)
Uanis(C23) = Uanis(C23A)
Uanis(C24) = Uanis(C24A)
Uanis(C25) = Uanis(C25A)
Uanis(C26) = Uanis(C26A)
Uanis(C27) = Uanis(C27A)
5. 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
6. Others
 Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(C1A)=Sof(H1A)=Sof(C7A)=Sof(C2A)=Sof(C3A)=
 Sof(H3A)=Sof(C4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(C8A)=Sof(C9A)=Sof(H9AA)=
 Sof(H9AB)=Sof(H9AC)=Sof(C10A)=Sof(H10D)=Sof(H10E)=Sof(H10F)=Sof(C11A)=
 Sof(H11D)=Sof(H11E)=Sof(H11F)=Sof(C12A)=Sof(C15A)=Sof(H15A)=Sof(H15B)=
 Sof(H15C)=Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C13A)=Sof(H13D)=
 Sof(H13E)=Sof(H13F)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17C)=Sof(H17D)=
 Sof(C18A)=Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C20A)=
 Sof(H20C)=Sof(H20D)=Sof(C21A)=Sof(H21A)=Sof(H22A)=Sof(C28A)=Sof(C23A)=
 Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(C26A)=Sof(H26A)=Sof(C27A)=Sof(C29A)=
 Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=
 Sof(H31F)=Sof(C32A)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33A)=Sof(C34A)=
 Sof(H34D)=Sof(H34E)=Sof(H34F)=Sof(C35A)=Sof(H35D)=Sof(H35E)=Sof(H35F)=
 Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H36F)=1-FVAR(1)
 Sof(O1)=Sof(O2)=Sof(O3)=Sof(C1)=Sof(H1)=Sof(C7)=Sof(C2)=Sof(C3)=Sof(H3)=
 Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(C8)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=
 Sof(C10)=Sof(H10A)=Sof(H10B)=Sof(H10C)=Sof(C11)=Sof(H11A)=Sof(H11B)=Sof(H11C)=
 Sof(C12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=Sof(H14A)=Sof(H14B)=
 Sof(H14C)=Sof(C15)=Sof(H15D)=Sof(H15E)=Sof(H15F)=Sof(C16)=Sof(H16)=Sof(C17)=
 Sof(H17A)=Sof(H17B)=Sof(C18)=Sof(H18A)=Sof(H18B)=Sof(C19)=Sof(H19A)=Sof(H19B)=
 Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21)=Sof(H22)=Sof(C28)=Sof(C23)=
 Sof(C24)=Sof(H24)=Sof(C25)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(C29)=Sof(C30)=
 Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C32)=
 Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33)=Sof(C34)=Sof(H34A)=Sof(H34B)=Sof(H34C)=
 Sof(C35)=Sof(H35A)=Sof(H35B)=Sof(H35C)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(H36C)=
 FVAR(1)
7.a Ternary CH refined with riding coordinates:
 C16(H16), C16A(H16A), C21(H21), C21A(H21A)
7.b Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C17A(H17C,H17D), C18(H18A,H18B), C18A(H18C,H18D), C19(H19A,
 H19B), C19A(H19C,H19D), C20(H20A,H20B), C20A(H20C,H20D)
7.c Me refined with riding coordinates:
 C9(H9A,H9B,H9C), C15(H15D,H15E,H15F), C30A(H30D,H30E,H30F)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C1A(H1A), C3(H3), C5(H5), C3A(H3A), C5A(H5A), C22(H22), C22(H22A),
 C24(H24), C26(H26), C24A(H24A), C26A(H26A)
7.e Fitted hexagon refined as free rotating group:
 C7(C2,C3,C4,C5,C6), C7A(C2A,C3A,C4A,C5A,C6A), C28(C23,C24,C25,C26,C27),
 C28A(C23A,C24A,C25A,C26A,C27A)
7.f Idealised Me refined as rotating group:
 C9A(H9AA,H9AB,H9AC), C10(H10A,H10B,H10C), C10A(H10D,H10E,H10F), C11(H11A,H11B,
 H11C), C11A(H11D,H11E,H11F), C13(H13A,H13B,H13C), C15A(H15A,H15B,H15C),
 C14(H14A,H14B,H14C), C14A(H14D,H14E,H14F), C13A(H13D,H13E,H13F), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F), C32(H32A,H32B,H32C),
 C32A(H32D,H32E,H32F), C34(H34A,H34B,H34C), C34A(H34D,H34E,H34F), C35(H35A,H35B,
 H35C), C35A(H35D,H35E,H35F), C36(H36A,H36B,H36C), C36A(H36D,H36E,H36F)
;
_shelx_res_checksum              52594
_shelx_hkl_checksum              29044
_shelx_fab_checksum              80521
_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 +/-4
_olex2_submission_special_instructions 'No special instructions were received'