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_1544840
_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         'C37 H60 N Na O7 S, 2.5(C7 H8)'
_chemical_formula_sum            'C54.5 H80 N Na O7 S'
_chemical_formula_weight         916.24
_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     iterative
_audit_creation_date             2016-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_cell_angle_alpha                107.939(9)
_cell_angle_beta                 92.806(8)
_cell_angle_gamma                93.558(8)
_cell_formula_units_Z            2
_cell_length_a                   10.6133(9)
_cell_length_b                   15.1843(17)
_cell_length_c                   17.3640(16)
_cell_measurement_reflns_used    1771
_cell_measurement_temperature    294.59(10)
_cell_measurement_theta_max      21.4960
_cell_measurement_theta_min      3.8820
_cell_volume                     2650.3(5)
_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
;
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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294.59(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0733
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega    2.00   27.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0541   38.0000   60.0000 25

  2 omega    8.00   90.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0541   57.0000   60.0000 82

  3 omega   62.00   88.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0541   38.0000   60.0000 26

  4 omega    0.00   36.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0541   57.0000  -90.0000 36

  5 omega  -47.00  -21.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8354  -38.0000   60.0000 26

  6 omega  -44.00   43.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0541  -38.0000  120.0000 87

  7 omega  -16.00   23.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8354  -99.0000   60.0000 39

  8 omega  -48.00   39.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       21.0541  -57.0000  -90.0000 87

  9 omega  -19.00    7.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -16.8354  -99.0000  150.0000 26
;
_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      0.0252061000
_diffrn_orient_matrix_UB_12      -0.0439712000
_diffrn_orient_matrix_UB_13      -0.0096027000
_diffrn_orient_matrix_UB_21      0.0621527000
_diffrn_orient_matrix_UB_22      0.0221932000
_diffrn_orient_matrix_UB_23      0.0091550000
_diffrn_orient_matrix_UB_31      -0.0029257000
_diffrn_orient_matrix_UB_32      0.0008852000
_diffrn_orient_matrix_UB_33      0.0409513000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.710
_diffrn_reflns_av_R_equivalents  0.0775
_diffrn_reflns_av_unetI/netI     0.1502
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18903
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         3.420
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.119
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94267
_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    1.148
_exptl_crystal_description       block
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.518
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.056
_refine_ls_extinction_coef       0.0005(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   0.972
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     656
_refine_ls_number_reflns         9331
_refine_ls_number_restraints     116
_refine_ls_restrained_S_all      0.973
_refine_ls_R_factor_all          0.1589
_refine_ls_R_factor_gt           0.0770
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0416P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1336
_refine_ls_wR_factor_ref         0.1674
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4664
_reflns_number_total             9331
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma6b02271_si_005.cif
_cod_data_source_block           chenchj_0418_2
_cod_depositor_comments
'Adding full bibliography for 1544839--1544842.cif.'
_cod_original_formula_sum        'C54.50 H80 N Na O7 S'
_cod_database_code               1544840
_reflns_odcompleteness_completeness 99.75
_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
 C3C-C1C \\sim C1C-C7C
 with sigma of 0.02
 C7B-C1B \\sim C1B-C3B
 with sigma of 0.02
3. Rigid bond restraints
 C1D, C2D, C3D, C4D, C5D, C6D, C7D
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C1C, C2C, C3C, C4C, C5C, C6C, C7C
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C1D \\sim C2D \\sim C3D \\sim C4D \\sim C5D \\sim C6D \\sim C7D: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
C1C \\sim C2C \\sim C3C \\sim C4C \\sim C5C \\sim C6C \\sim C7C: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
5. Others
 Sof(C1C)=Sof(HP)=Sof(HQ)=Sof(HR)=Sof(C2C)=Sof(C3C)=Sof(HS)=Sof(C4C)=Sof(HT)=
 Sof(C5C)=Sof(HU)=Sof(C6C)=Sof(HV)=Sof(C7C)=Sof(HW)=1-FVAR(1)
 Sof(C1B)=Sof(HH)=Sof(HI)=Sof(HJ)=Sof(C2B)=Sof(C7B)=Sof(HK)=Sof(C6B)=Sof(HL)=
 Sof(C5B)=Sof(HM)=Sof(C4B)=Sof(HN)=Sof(C3B)=Sof(HO)=FVAR(1)
 Fixed Sof: C1D(0.5) HX(0.5) HY(0.5) HZ(0.5) C2D(0.5) C7D(0.5) H0AA(0.5)
 C6D(0.5) H1AA(0.5) C5D(0.5) H2AA(0.5) C4D(0.5) H3AA(0.5) C3D(0.5) H4AA(0.5)
6.a Ternary CH refined with riding coordinates:
 C7(H7), C10(H10), C13(H13), C22(H22), C25(H25)
6.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,
 H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
 C38(H38A,H38B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C18(H18), C19(H19), C20(H20), C3A(HC), C4A(HD), C5A(HE),
 C6A(HF), C7A(HG), C7B(HK), C6B(HL), C5B(HM), C4B(HN), C3B(HO), C3C(HS),
 C4C(HT), C5C(HU), C6C(HV), C7C(HW), C7D(H0AA), C6D(H1AA), C5D(H2AA), C4D(H3AA),
  C3D(H4AA)
6.d Fitted hexagon refined as free rotating group:
 C2B(C7B,C6B,C5B,C4B,C3B), C2C(C3C,C4C,C5C,C6C,C7C), C2D(C7D,C6D,C5D,C4D,C3D)
6.e Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C),
 C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C23(H23A,H23B,H23C), C24(H24A,H24B,
 H24C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C1A(H,HA,HB), C1B(HH,HI,HJ),
 C1C(HP,HQ,HR), C1D(HX,HY,HZ)
;
_shelx_res_checksum              55691
_shelx_hkl_checksum              2041
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'