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_1545203
_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 O8 S'
_chemical_formula_sum            'C30 H36 N Na O8 S'
_chemical_formula_weight         593.65
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-17
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.232(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6531(9)
_cell_length_b                   11.2507(9)
_cell_length_c                   17.5258(12)
_cell_measurement_reflns_used    4413
_cell_measurement_temperature    289.97(10)
_cell_measurement_theta_max      27.1490
_cell_measurement_theta_min      3.6110
_cell_volume                     2931.5(4)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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      289.97(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -19.00   18.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -17.1479  -99.0000  -30.0000 37

  2 omega   17.00   59.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854  -99.0000  -90.0000 42

  3 omega   -2.00   93.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854   38.0000  -90.0000 95

  4 omega  -49.00   30.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.5854    0.0000  -90.0000 79
;
_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      -0.0111458000
_diffrn_orient_matrix_UB_12      0.0039819000
_diffrn_orient_matrix_UB_13      0.0361529000
_diffrn_orient_matrix_UB_21      0.0043319000
_diffrn_orient_matrix_UB_22      0.0627043000
_diffrn_orient_matrix_UB_23      -0.0006120000
_diffrn_orient_matrix_UB_31      -0.0462018000
_diffrn_orient_matrix_UB_32      0.0049033000
_diffrn_orient_matrix_UB_33      -0.0225483000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_av_unetI/netI     0.0893
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            14661
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.491
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.177
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95857
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
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    1.345
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.500
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.117
_refine_ls_extinction_coef       0.0022(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.149
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     490
_refine_ls_number_reflns         5138
_refine_ls_number_restraints     101
_refine_ls_restrained_S_all      1.139
_refine_ls_R_factor_all          0.1682
_refine_ls_R_factor_gt           0.1572
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+49.8207P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3291
_refine_ls_wR_factor_ref         0.3337
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4300
_reflns_number_total             5138
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b02271_si_004.cif
_cod_data_source_block           chenchj_0513
_cod_database_code               1545203
_reflns_odcompleteness_completeness 99.64
_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', C23', O4', C21', O8', C29', C28', O7', C27', C26', O6', C25', C24'
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8, C29, O4, C21, O5, C23, C24, C25, C26, O7, C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O8, C29, O4, C21, O5, C23, C24, C25, C26, O7, C27, C28
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
O5' \\sim C23' \\sim O4' \\sim C21' \\sim O8' \\sim C29' \\sim C28' \\sim O7'
\\sim C27' \\sim C26' \\sim O6' \\sim C25' \\sim C24': within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(C24')=Sof(H24C)=Sof(H24D)=Sof(O4')=Sof(O5')=Sof(O6')=Sof(O7')=Sof(O8')=
 Sof(C21')=Sof(H21C)=Sof(H21D)=Sof(H22C)=Sof(H22D)=Sof(C23')=Sof(H23C)=
 Sof(H23D)=Sof(C25')=Sof(H25C)=Sof(H25D)=Sof(C26')=Sof(H26C)=Sof(H26D)=
 Sof(C27')=Sof(H27C)=Sof(H27D)=Sof(C28')=Sof(H28C)=Sof(H28D)=Sof(C29')=
 Sof(H29C)=Sof(H29D)=Sof(H30C)=Sof(H30D)=1-FVAR(1)
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(O4)=Sof(O5)=Sof(O6)=Sof(O7)=Sof(O8)=Sof(C21)=
 Sof(H21A)=Sof(H21B)=Sof(H22A)=Sof(H22B)=Sof(C23)=Sof(H23A)=Sof(H23B)=Sof(C25)=
 Sof(H25A)=Sof(H25B)=Sof(C26)=Sof(H26A)=Sof(H26B)=Sof(C27)=Sof(H27A)=Sof(H27B)=
 Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(H30A)=Sof(H30B)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C8(H8)
5.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C24'(H24C,H24D), C21(H21A,H21B), C21'(H21C,H21D), C22(H22C,
 H22D), C22(H22A,H22B), C23(H23A,H23B), C23'(H23C,H23D), C25(H25A,H25B),
 C25'(H25C,H25D), C26(H26A,H26B), C26'(H26C,H26D), C27(H27A,H27B), C27'(H27C,
 H27D), C28(H28A,H28B), C28'(H28C,H28D), C29(H29A,H29B), C29'(H29C,H29D),
 C30(H30A,H30B), C30(H30C,H30D)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C5(H5), C6(H6), C10(H10), C11(H11), C12(H12), C13(H13),
 C16(H16), C17(H17), C18(H18), C19(H19)
5.d Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              89509
_shelx_hkl_checksum              61207
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-05-13
_olex2_submission_special_instructions 'No special instructions were received'