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_1544842
_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         'C29 H32 N2 Na O10 S'
_chemical_formula_sum            'C29 H32 N2 Na O10 S'
_chemical_formula_weight         623.61
_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             2016-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.924(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.7318(8)
_cell_length_b                   16.8460(15)
_cell_length_c                   16.1244(13)
_cell_measurement_reflns_used    2591
_cell_measurement_temperature    293.00(10)
_cell_measurement_theta_max      28.1080
_cell_measurement_theta_min      3.9330
_cell_volume                     2913.5(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.00(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 0.996
_diffrn_measurement_details
;
  1 omega  -28.00   -3.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2104  -38.0000   60.0000 25

  2 omega  -11.00   25.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.6791  -99.0000    0.0000 36

  3 omega  -11.00   39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2104  -57.0000  -30.0000 50

  4 omega  -48.00   43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2104  -57.0000 -150.0000 91

  5 omega   -1.00   39.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       21.2104  -99.0000  150.0000 40
;
_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      0.0028047000
_diffrn_orient_matrix_UB_12      0.0037740000
_diffrn_orient_matrix_UB_13      0.0438203000
_diffrn_orient_matrix_UB_21      0.0316122000
_diffrn_orient_matrix_UB_22      -0.0368946000
_diffrn_orient_matrix_UB_23      0.0032827000
_diffrn_orient_matrix_UB_31      0.0580255000
_diffrn_orient_matrix_UB_32      0.0199572000
_diffrn_orient_matrix_UB_33      -0.0022091000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0383
_diffrn_reflns_av_unetI/netI     0.0599
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            11368
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         3.301
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.187
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86293
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_description       prism
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.531
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         5113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0534
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1452
_refine_ls_wR_factor_ref         0.1687
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3714
_reflns_number_total             5113
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b02271_si_007.cif
_cod_data_source_block           wujc_0426_1
_cod_depositor_comments
'Adding full bibliography for 1544839--1544842.cif.'
_cod_database_code               1544842
_reflns_odcompleteness_completeness 99.74
_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
2.a Ternary CH refined with riding coordinates:
 C7(H7)
2.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C21(H21A,H21B), C20(H20A,H20B), C27(H27A,
 H27B), C26(H26A,H26B), C25(H25A,H25B), C22(H22A,H22B), C23(H23A,H23B)
2.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C9(H9), C15(H15), C2(H2), C18(H18), C10(H10), C5(H5), C12(H12),
 C17(H17), C11(H11), C16(H16), C3(H3), C24(H24)
;
_shelx_res_checksum              36375
_shelx_hkl_checksum              94664
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'