ppm-Level Thermally Switchable Yttrium Phenoxide Catalysts for Moisture-Insensitive and Controllably Immortal Polymerization of rac-Lactide
Chen, Changjuan; Bai, Zhiyong; Cui, Yaqin; Cong, Yong; Pan, Xiaobo; Wu, Jincai; Macromolecules 51 (2018) 6800–; doi:10.1021/acs.macromol.8b01229

data_1552822
_publ_section_title
;
 ppm-Level Thermally Switchable Yttrium Phenoxide Catalysts for
 Moisture-Insensitive and Controllably Immortal Polymerization of
 rac-Lactide
;
_journal_issue                   17
_journal_name_full               Macromolecules
_journal_page_first              6800
_journal_paper_doi               10.1021/acs.macromol.8b01229
_journal_volume                  51
_journal_year                    2018
_chemical_formula_moiety         'C174 H256 O26 Y4, 4(C H2 Cl2)'
_chemical_formula_sum            'C178 H264 Cl8 O26 Y4'
_chemical_formula_weight         3459.12
_space_group_crystal_system      tetragonal
_space_group_IT_number           120
_space_group_name_Hall           'I -4 -2c'
_space_group_name_H-M_alt        'I -4 c 2'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.8909(4)
_cell_length_b                   25.8909(4)
_cell_length_c                   59.130(4)
_cell_measurement_reflns_used    7511
_cell_measurement_temperature    173.01(10)
_cell_measurement_theta_max      69.6270
_cell_measurement_theta_min      4.4050
_cell_volume                     39637(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_temperature      173.01(10)
_diffrn_detector_area_resol_mean 16.0733
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega  -50.00  -21.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  -77.0000   90.0000 29

  2 omega  -17.00   23.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  -77.0000   90.0000 40

  3 omega  -23.00   16.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       -8.5000  -63.0000  -60.0000 39

  4 omega   32.00   67.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   57.0000    0.0000 35

  5 omega   53.00   79.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000 -129.0000   61.0000 26

  6 omega   28.00  127.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       54.0000   38.0000  -30.0000 99

  7 omega  125.00  151.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -150.0000 26

  8 omega   38.00  103.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -50.0000 -180.0000 65

  9 omega  148.00  177.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000  -90.0000 29

 10 omega   90.00  145.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   25.0000  -90.0000 55

 11 omega  140.00  165.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  132.0000   42.0000 25

 12 omega   91.00  175.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   63.0000  -30.0000 84

 13 omega   39.00  108.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 69

 14 omega  131.00  174.00   1.0000   30.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -120.0000 43
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0005934000
_diffrn_orient_matrix_UB_12      0.0080657000
_diffrn_orient_matrix_UB_13      -0.0258230000
_diffrn_orient_matrix_UB_21      -0.0023677000
_diffrn_orient_matrix_UB_22      -0.0588743000
_diffrn_orient_matrix_UB_23      -0.0035053000
_diffrn_orient_matrix_UB_31      -0.0594649000
_diffrn_orient_matrix_UB_32      0.0022565000
_diffrn_orient_matrix_UB_33      0.0004122000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_av_unetI/netI     0.0791
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -67
_diffrn_reflns_number            54607
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.214
_diffrn_reflns_theta_max         25.639
_diffrn_reflns_theta_min         1.769
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88080
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             14656
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.609
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details
;
 Flack x determined using 4985 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.009(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1014
_refine_ls_number_reflns         18153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0859
_refine_ls_R_factor_gt           0.0539
_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^)+(0.0580P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1214
_refine_ls_wR_factor_ref         0.1419
_reflns_Friedel_coverage         0.916
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.988
_reflns_number_gt                13077
_reflns_number_total             18153
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma8b01229_si_003.cif
_cod_data_source_block           chchj_0322_3
_cod_database_code               1552822
_shelxl_version_number           2013-4
_shelx_estimated_absorpt_t_max   0.816
_shelx_estimated_absorpt_t_min   0.759
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.748(6)
 0.252(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H89A of C89, H34 of C34, H32 of C32, H5 of C5, H11 of
  C11, H3A of C3, H9 of C9, H55 of C55, H49 of C49, H47 of C47, H53 of C53, H76
  of C76
 At 1.5 times of:
  All C(H,H,H) groups, H78 of C78, H89B of C89, All O(H) groups, All O(H,H)
  groups
3.a Riding coordinates:
 O6(H6), O7(H7A,H7B), O13(H13A,H13B), O14(H14)
3.b Secondary CH2 refined with riding coordinates:
 C89(H89A,H89B), C90(H90A,H90B)
3.c Aromatic/amide H refined with riding coordinates:
 C3(H3A), C5(H5), C9(H9), C11(H11), C32(H32), C34(H34), C47(H47), C49(H49),
 C53(H53), C55(H55), C76(H76), C78(H78)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,
 H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C),
 C29(H29A,H29B,H29C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,
 H40C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C59(H59A,
 H59B,H59C), C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C63(H63A,H63B,H63C),
 C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C67(H67A,H67B,H67C), C68(H68A,H68B,
 H68C), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C73(H73A,
 H73B,H73C), C82(H82A,H82B,H82C), C83(H83A,H83B,H83C), C84(H84A,H84B,H84C),
 C86(H86A,H86B,H86C), C87(H87A,H87B,H87C), C88(H88A,H88B,H88C)
3.e Idealised tetrahedral OH refined as rotating group:
 O3(H3), O10(H10)
;
_shelx_res_checksum              35875
_shelx_hkl_checksum              61211
_olex2_date_sample_data_collection 2018-03-22
_olex2_submission_special_instructions 'No special instructions were received'