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_4514282
_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         'C74 H117 Cl In2 N4 O5, 4(C7 H8)'
_chemical_formula_sum            'C102 H149 Cl In2 N4 O5'
_chemical_formula_weight         1776.33
_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   mixed
_atom_sites_solution_primary     direct
_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                85.3880(10)
_cell_angle_beta                 74.1760(10)
_cell_angle_gamma                65.3920(10)
_cell_formula_units_Z            1
_cell_length_a                   12.1349(8)
_cell_length_b                   12.2766(8)
_cell_length_c                   18.6225(12)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.47
_cell_volume                     2425.0(3)
_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    '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 1.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  X8
_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  0.0225
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44492
_diffrn_reflns_point_group_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         27.544
_diffrn_reflns_theta_min         1.137
_diffrn_source                   microsource
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0462 before and 0.0419 after correction. The Ratio of minimum to maximum transmission is 0.9079. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       RECTANGULAR
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.468
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.108
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.233
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 9185 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.005(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1133
_refine_ls_number_reflns         21442
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0227
_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^)+(0.0201P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0463
_refine_ls_wR_factor_ref         0.0473
_reflns_Friedel_coverage         0.932
_reflns_Friedel_fraction_full    0.952
_reflns_Friedel_fraction_max     0.926
_reflns_number_gt                20241
_reflns_number_total             21442
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs7b01939_si_002.cif
_cod_data_source_block           pm177_1
_cod_database_code               4514282
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.781
_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
 C88-C82 \\sim C81-C75
 with sigma of 0.01
 C88A-C82A \\sim C81-C75
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C73 \\sim C73A \\sim C74 \\sim C74A: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
4. Rigid body (RIGU) restrains
 C73, C74A, C73A, C74
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C73A)=Sof(H73C)=Sof(H73D)=Sof(C74A)=Sof(H74D)=Sof(H74E)=Sof(H74F)=1-FVAR(1)
 Sof(C73)=Sof(H73A)=Sof(H73B)=Sof(C74)=Sof(H74A)=Sof(H74B)=Sof(H74C)=FVAR(1)
 Sof(C82A)=Sof(C83A)=Sof(H83A)=Sof(C84A)=Sof(H84A)=Sof(C85A)=Sof(H85A)=
 Sof(C86A)=Sof(H86A)=Sof(C87A)=Sof(H87A)=Sof(C88A)=Sof(H88D)=Sof(H88E)=
 Sof(H88F)=1-FVAR(2)
 Sof(C82)=Sof(C87)=Sof(H87)=Sof(C86)=Sof(H86)=Sof(C85)=Sof(H85)=Sof(C84)=
 Sof(H84)=Sof(C83)=Sof(H83)=Sof(C88)=Sof(H88A)=Sof(H88B)=Sof(H88C)=FVAR(2)
6.a Ternary CH refined with riding coordinates:
 C16(H16), C21(H21), C52(H52), C57(H57)
6.b 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), C53(H53A,H53B), C54(H54A,H54B), C55(H55A,H55B),
  C56(H56A,H56B), C58(H58A,H58B), C73(H73A,H73B), C73A(H73C,H73D)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C24(H24), C26(H26), C39(H39), C41(H41), C60(H60), C62(H62),
 C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C87(H87), C86(H86), C85(H85),
  C84(H84), C83(H83), C83A(H83A), C84A(H84A), C85A(H85A), C86A(H86A),
 C87A(H87A), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C97(H97),
 C98(H98), C99(H99), C100(H100), C101(H101)
6.d Fitted hexagon refined as free rotating group:
 C82(C87,C86,C85,C84,C83), C82A(C83A,C84A,C85A,C86A,C87A)
6.e 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), C30(H30A,H30B,H30C), C31(H31A,
 H31B,H31C), C32(H32A,H32B,H32C), 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), C74(H74A,H74B,H74C), C74A(H74D,H74E,
 H74F), C81(H81A,H81B,H81C), C88(H88A,H88B,H88C), C88A(H88D,H88E,H88F),
 C95(H95A,H95B,H95C), C102(H10D,H10E,H10F)
;
_shelx_res_checksum              79650
_shelx_hkl_checksum              91114
_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-1
_olex2_submission_special_instructions 'No special instructions were received'