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_1544839
_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         'C30 H36 N Na O9 S, C6 H6'
_chemical_formula_sum            'C36 H42 N Na O9 S'
_chemical_formula_weight         687.75
_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             2016-06-16
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                94.526(4)
_cell_angle_beta                 92.174(4)
_cell_angle_gamma                117.703(5)
_cell_formula_units_Z            2
_cell_length_a                   9.6525(4)
_cell_length_b                   10.0128(5)
_cell_length_c                   20.1980(10)
_cell_measurement_reflns_used    3582
_cell_measurement_temperature    293.26(10)
_cell_measurement_theta_max      28.2150
_cell_measurement_theta_min      3.7060
_cell_volume                     1716.78(16)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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      293.26(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.879
_diffrn_measurement_details
;
  1 omega   35.00   86.45   1.0500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7086  -19.0000   60.0000 49

  2 omega    3.00   66.00   1.0500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7086  -99.0000  -90.0000 60

  3 omega  -19.00   21.95   1.0500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3492  -99.0000   60.0000 39

  4 omega  -51.00   93.90   1.0500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7086    0.0000 -180.0000 138

  5 omega   -9.00   72.90   1.0500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7086   77.0000   30.0000 78

  6 omega   62.00   88.25   1.0500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.7086  178.0000 -180.0000 25

  7 omega -101.00  -55.85   1.0500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.3492  178.0000   60.0000 43
;
_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      -0.0136088000
_diffrn_orient_matrix_UB_12      -0.0688166000
_diffrn_orient_matrix_UB_13      -0.0184962000
_diffrn_orient_matrix_UB_21      -0.0411945000
_diffrn_orient_matrix_UB_22      0.0141144000
_diffrn_orient_matrix_UB_23      -0.0260533000
_diffrn_orient_matrix_UB_31      0.0711057000
_diffrn_orient_matrix_UB_32      0.0392933000
_diffrn_orient_matrix_UB_33      -0.0151329000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0528
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.879
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14094
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.879
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.656
_diffrn_reflns_theta_min         3.266
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.163
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69745
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
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    1.330
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         7762
_refine_ls_number_restraints     220
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0741
_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^)+(0.0655P)^2^+2.5662P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1714
_refine_ls_wR_factor_ref         0.1929
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5628
_reflns_number_total             7762
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b02271_si_003.cif
_cod_data_source_block           chenchj_0614_2
_cod_depositor_comments
'Adding full bibliography for 1544839--1544842.cif.'
_cod_database_code               1544839
_reflns_odcompleteness_completeness 99.76
_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, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O5', O6', O7', O8', O9', C22, C23', C24', C25', C26', C27', C28, C29', C30, C31
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O5, O6, O7, O8, O9, C23, C24, C25, C26, C27, C29, C31'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O3, C16, C17, C18, C19
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O3 \\sim C16 \\sim C17 \\sim C18 \\sim C19: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
O5 \\sim O6 \\sim O7 \\sim O8 \\sim O9 \\sim C23 \\sim C24 \\sim C25 \\sim C26
\\sim C27 \\sim C29 \\sim C31': within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O5' \\sim O6' \\sim O7' \\sim O8' \\sim O9' \\sim C22 \\sim C23' \\sim C24'
\\sim C25' \\sim C26' \\sim C27' \\sim C28 \\sim C29' \\sim C30 \\sim C31:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O5')=Sof(O6')=Sof(O7')=Sof(O8')=Sof(O9')=Sof(H22C)=Sof(H22D)=Sof(C23')=
 Sof(H23C)=Sof(H23D)=Sof(C24')=Sof(H24C)=Sof(H24D)=Sof(C25')=Sof(H25C)=
 Sof(H25D)=Sof(C26')=Sof(H26C)=Sof(H26D)=Sof(C27')=Sof(H27C)=Sof(H27D)=
 Sof(H28C)=Sof(H28D)=Sof(C29')=Sof(H29C)=Sof(H29D)=Sof(H30C)=Sof(H30D)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=1-FVAR(1)
 Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(O9)=Sof(H22A)=Sof(H22B)=Sof(C23)=
 Sof(H23A)=Sof(H23B)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(C25)=Sof(H25A)=Sof(H25B)=
 Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=Sof(H28A)=Sof(H28B)=
 Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H30A)=Sof(H30B)=Sof(C31')=Sof(H31C)=Sof(H31D)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C22(H22C,H22D), C22(H22A,H22B), C23(H23A,H23B), C23'(H23C,H23D), C24(H24A,
 H24B), C24'(H24C,H24D), C25(H25A,H25B), C25'(H25C,H25D), C26(H26A,H26B),
 C26'(H26C,H26D), C27(H27A,H27B), C27'(H27C,H27D), C28(H28C,H28D), C28(H28A,
 H28B), C29(H29A,H29B), C29'(H29C,H29D), C30(H30C,H30D), C30(H30A,H30B),
 C31(H31A,H31B), C31'(H31C,H31D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C11(H11), C12(H12), C13(H13), C14(H14),
 C17(H17), C18(H18), C19(H19), C20(H20), C32(H32), C33(H33), C34(H34), C35(H35),
  C36(H36), C37(H37)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              16610
_shelx_hkl_checksum              6886
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-06-14
_olex2_submission_special_instructions 'No special instructions were received'