Suppressing Cyclic Polymerization for Isoselective Synthesis of High-Molecular-Weight Linear Polylactide Catalyzed by Sodium/Potassium Sulfonamidate Complexes
Chen, Changjuan; Cui, Yaqin; Mao, Xiaoyang; Pan, Xiaobo; Wu, Jincai; Macromolecules 50 (2017) 83–; doi:10.1021/acs.macromol.6b02271

data_1544841
_publ_section_title
;
 Suppressing Cyclic Polymerization for Isoselective Synthesis of
 High-Molecular-Weight Linear Polylactide Catalyzed by Sodium/Potassium
 Sulfonamidate Complexes
;
_journal_issue                   1
_journal_name_full               Macromolecules
_journal_page_first              83
_journal_paper_doi               10.1021/acs.macromol.6b02271
_journal_volume                  50
_journal_year                    2017
_chemical_formula_moiety         'C40 H55 K N O9 S, 1(C7 H8)'
_chemical_formula_sum            'C47 H63 K N O9 S'
_chemical_formula_weight         857.14
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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     direct
_audit_creation_date             2016-04-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                76.475(5)
_cell_angle_beta                 86.282(5)
_cell_angle_gamma                88.815(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9876(5)
_cell_length_b                   12.4673(7)
_cell_length_c                   18.4805(12)
_cell_measurement_reflns_used    3392
_cell_measurement_temperature    291.23(10)
_cell_measurement_theta_max      26.7070
_cell_measurement_theta_min      3.6860
_cell_volume                     2456.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.23(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega   -9.00   82.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   77.0000    0.0000 91

  2 omega   21.00   54.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   57.0000   90.0000 33

  3 omega   -5.00   85.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   38.0000  -90.0000 90

  4 omega  -12.00   14.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000   90.0000 26

  5 omega   41.00   69.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  178.0000   30.0000 28

  6 omega  -52.00   46.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -38.0000   90.0000 98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0029878000
_diffrn_orient_matrix_UB_12      -0.0222484000
_diffrn_orient_matrix_UB_13      -0.0318248000
_diffrn_orient_matrix_UB_21      -0.0059629000
_diffrn_orient_matrix_UB_22      -0.0537485000
_diffrn_orient_matrix_UB_23      0.0234175000
_diffrn_orient_matrix_UB_31      -0.0643470000
_diffrn_orient_matrix_UB_32      0.0063480000
_diffrn_orient_matrix_UB_33      0.0017625000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_unetI/netI     0.0604
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15012
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         3.361
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.201
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73777
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.159
_exptl_crystal_description       block
_exptl_crystal_F_000             918
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     631
_refine_ls_number_reflns         8518
_refine_ls_number_restraints     177
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0912
_refine_ls_R_factor_gt           0.0627
_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^)+(0.0948P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1611
_refine_ls_wR_factor_ref         0.1816
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5991
_reflns_number_total             8518
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b02271_si_006.cif
_cod_data_source_block           wujc_0415
_cod_depositor_comments
'Adding full bibliography for 1544839--1544842.cif.'
_cod_database_code               1544841
_reflns_odcompleteness_completeness 98.57
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 C7B-C1B \\sim C1B-C3B
 with sigma of 0.02
 C7C-C1C \\sim C1C-C3C
 with sigma of 0.02
3. Restrained planarity
 C1B, C2B, C3B, C4B, C5B, C6B, C7B
 with sigma of 0.1
4. Rigid bond restraints
 C2C, C3C, C4C, C5C, C6C, C7C, C1C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1B, C2B, C3B, C4B, C5B, C6B, C7B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1A, C2A, C7A, C6A, C5A, C4A, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
C2C \\sim C3C \\sim C4C \\sim C5C \\sim C6C \\sim C7C \\sim C1C: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C1B \\sim C2B \\sim C3B \\sim C4B \\sim C5B \\sim C6B \\sim C7B: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
C1A \\sim C2A \\sim C7A \\sim C6A \\sim C5A \\sim C4A \\sim C3A: within 2A with
sigma of 0.04 and sigma for terminal atoms of 0.08
6. Others
 Fixed Sof: C1B(0.33333) H1BA(0.33333) H1BB(0.33333) H1BC(0.33333)
 C2B(0.33333) C3B(0.33333) H3B(0.33333) C4B(0.33333) H4B(0.33333) C5B(0.33333)
 H5B(0.33333) C6B(0.33333) H6B(0.33333) C7B(0.33333) H7B(0.33333) C2C(0.33333)
 C3C(0.33333) H3C(0.33333) C4C(0.33333) H4C(0.33333) C5C(0.33333) H5C(0.33333)
 C6C(0.33333) H6C(0.33333) C7C(0.33333) H7C(0.33333) C1C(0.33333) H1CA(0.33333)
 H1CB(0.33333) H1CC(0.33333) C1A(0.33333) H1AA(0.33333) H1AB(0.33333)
 H1AC(0.33333) C2A(0.33333) C7A(0.33333) H7A(0.33333) C6A(0.33333) H6A(0.33333)
 C5A(0.33333) H5A(0.33333) C4A(0.33333) H4A(0.33333) C3A(0.33333) H3A(0.33333)
7.a Ternary CH refined with riding coordinates:
 C16(H16), C7(H7), C13(H13), C10(H10)
7.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C40(H40A,H40B), C39(H39A,
 H39B), C37(H37A,H37B), C35(H35A,H35B), C36(H36A,H36B), C34(H34A,H34B),
 C38(H38A,H38B), C33(H33A,H33B)
7.c Aromatic/amide H refined with riding coordinates:
 C27(H27), C25(H25), C24(H24), C3(H3), C26(H26), C18(H18), C21(H21), C5(H5),
 C31(H31), C20(H20), C19(H19), C3B(H3B), C4B(H4B), C5B(H5B), C6B(H6B), C7B(H7B),
  C3C(H3C), C4C(H4C), C5C(H5C), C6C(H6C), C7C(H7C), C7A(H7A), C6A(H6A),
 C5A(H5A), C4A(H4A), C3A(H3A)
7.d Fitted hexagon refined as free rotating group:
 C2B(C3B,C4B,C5B,C6B,C7B), C2C(C3C,C4C,C5C,C6C,C7C), C2A(C7A,C6A,C5A,C4A,C3A)
7.e Idealised Me refined as rotating group:
 C9(H9A,H9B,H9C), C8(H8A,H8B,H8C), C15(H15A,H15B,H15C), C12(H12A,H12B,H12C),
 C11(H11A,H11B,H11C), C14(H14A,H14B,H14C), C1B(H1BA,H1BB,H1BC), C1C(H1CA,H1CB,
 H1CC), C1A(H1AA,H1AB,H1AC)
;
_shelx_res_checksum              39486
_shelx_hkl_checksum              91930
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'